data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Warren Piers' _publ_contact_author_address ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'wpiers@ucalgary.ca' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Morgan, Matthew' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; 'Piers, Warren' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_MM1507_0m_a _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C24 B F20 C29 H24 N Zr' _chemical_formula_sum 'C53 H24 B F20 N Zr' _chemical_formula_weight 1156.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system tetragonal _space_group_IT_number 78 _space_group_name_H-M_alt 'P 43' _space_group_name_Hall 'P 4cw' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 11.57510(10) _cell_length_b 11.57510(10) _cell_length_c 34.2480(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4588.65(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9923 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 66.59 _exptl_crystal_description 'block' _exptl_crystal_colour 'Orange' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.674 _exptl_crystal_F_000 2296 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_absorpt_coefficient_mu 3.073 _shelx_estimated_absorpt_T_min 0.491 _shelx_estimated_absorpt_T_max 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20967 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.819 _diffrn_reflns_theta_max 66.626 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_point_group_measured_fraction_full 0.934 _reflns_number_total 7737 _reflns_number_gt 7629 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.874 _reflns_Friedel_fraction_max 0.906 _reflns_Friedel_fraction_full 0.886 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.1.7' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+4.6891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3443 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.018(8) _chemical_absolute_configuration ? _refine_ls_number_reflns 7737 _refine_ls_number_parameters 685 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.71262(3) 0.01573(3) 0.63443(2) 0.02254(10) Uani 1 1 d . . . . . F15 F 0.6433(3) 0.4579(3) 0.50298(9) 0.0324(7) Uani 1 1 d . . . . . F6 F 0.7317(3) 0.4408(3) 0.42738(10) 0.0315(7) Uani 1 1 d . . . . . F5 F 0.2446(3) 0.2572(3) 0.43088(10) 0.0321(7) Uani 1 1 d . . . . . F16 F 0.2514(3) 0.4785(3) 0.46226(9) 0.0303(7) Uani 1 1 d . . . . . F11 F 0.3831(3) 0.6080(3) 0.40875(10) 0.0332(7) Uani 1 1 d . . . . . F20 F 0.5370(3) 0.2356(3) 0.51853(9) 0.0316(7) Uani 1 1 d . . . . . F10 F 0.4657(3) 0.1346(3) 0.44567(10) 0.0335(7) Uani 1 1 d . . . . . F1 F 0.5503(3) 0.4615(3) 0.37039(9) 0.0317(7) Uani 1 1 d . . . . . F14 F 0.6926(3) 0.6708(3) 0.52563(11) 0.0441(9) Uani 1 1 d . . . . . F2 F 0.4424(3) 0.4429(3) 0.30245(10) 0.0442(9) Uani 1 1 d . . . . . F17 F 0.1238(3) 0.4555(3) 0.52591(11) 0.0413(8) Uani 1 1 d . . . . . F19 F 0.4097(3) 0.2213(3) 0.58247(10) 0.0368(7) Uani 1 1 d . . . . . F18 F 0.2022(3) 0.3299(3) 0.58771(10) 0.0433(8) Uani 1 1 d . . . . . F7 F 0.8951(3) 0.2896(3) 0.41239(13) 0.0464(9) Uani 1 1 d . . . . . F3 F 0.2359(4) 0.3310(4) 0.29722(11) 0.0510(10) Uani 1 1 d . . . . . F13 F 0.5831(4) 0.8555(3) 0.49209(12) 0.0581(12) Uani 1 1 d . . . . . F9 F 0.6311(4) -0.0154(3) 0.42554(13) 0.0492(10) Uani 1 1 d . . . . . F4 F 0.1403(3) 0.2406(3) 0.36316(11) 0.0440(9) Uani 1 1 d . . . . . F12 F 0.4277(4) 0.8172(3) 0.43371(12) 0.0534(11) Uani 1 1 d . . . . . F8 F 0.8487(4) 0.0597(3) 0.41062(14) 0.0555(11) Uani 1 1 d . . . . . N1 N 0.7510(4) 0.1897(4) 0.60634(14) 0.0288(10) Uani 1 1 d . . . . . C7 C 0.6869(5) 0.2863(5) 0.6108(2) 0.0337(13) Uani 1 1 d . . . . . H7 H 0.6162 0.2811 0.6248 0.040 Uiso 1 1 calc R U . . . C48 C 0.4002(4) 0.3549(4) 0.48581(15) 0.0217(10) Uani 1 1 d . . . . . C31 C 0.4474(4) 0.4055(4) 0.37018(15) 0.0234(10) Uani 1 1 d . . . . . C47 C 0.5907(4) 0.5442(4) 0.48401(16) 0.0248(11) Uani 1 1 d . . . . . C32 C 0.3949(5) 0.3964(5) 0.33438(17) 0.0282(11) Uani 1 1 d . . . . . C46 C 0.6162(5) 0.6548(5) 0.49644(16) 0.0299(11) Uani 1 1 d . . . . . C49 C 0.2937(4) 0.4098(4) 0.49089(15) 0.0240(10) Uani 1 1 d . . . . . C50 C 0.2269(5) 0.4010(5) 0.52399(17) 0.0283(11) Uani 1 1 d . . . . . C6 C 0.7189(5) 0.3910(5) 0.5961(2) 0.0385(14) Uani 1 1 d . . . . . H6 H 0.6712 0.4569 0.5995 0.046 Uiso 1 1 calc R U . . . C52 C 0.3710(5) 0.2832(4) 0.55222(16) 0.0283(11) Uani 1 1 d . . . . . C51 C 0.2654(5) 0.3377(5) 0.55499(17) 0.0288(11) Uani 1 1 d . . . . . C53 C 0.4344(4) 0.2925(4) 0.51822(16) 0.0246(11) Uani 1 1 d . . . . . C36 C 0.5898(4) 0.2959(4) 0.43907(14) 0.0205(10) Uani 1 1 d . . . . . C35 C 0.2988(4) 0.3060(4) 0.40031(16) 0.0240(10) Uani 1 1 d . . . . . C37 C 0.7008(4) 0.3284(4) 0.42971(16) 0.0252(11) Uani 1 1 d . . . . . C30 C 0.4028(4) 0.3642(4) 0.40518(16) 0.0219(10) Uani 1 1 d . . . . . C5 C 0.8225(5) 0.3992(5) 0.5761(2) 0.0414(15) Uani 1 1 d . . . . . H5 H 0.8478 0.4712 0.5659 0.050 Uiso 1 1 calc R U . . . C38 C 0.7884(5) 0.2511(5) 0.42089(18) 0.0322(12) Uani 1 1 d . . . . . C44 C 0.4833(5) 0.7284(5) 0.45017(18) 0.0351(13) Uani 1 1 d . . . . . C41 C 0.5717(4) 0.1770(4) 0.43763(16) 0.0256(11) Uani 1 1 d . . . . . C42 C 0.5131(4) 0.5193(4) 0.45418(15) 0.0221(10) Uani 1 1 d . . . . . C15 C 0.9600(4) -0.1896(5) 0.63081(19) 0.0311(11) Uani 1 1 d . . . . . H15 H 0.9467 -0.1576 0.6559 0.037 Uiso 1 1 calc R U . . . C40 C 0.6554(5) 0.0977(5) 0.42794(18) 0.0324(12) Uani 1 1 d . . . . . C22 C 0.5559(5) -0.1278(5) 0.62700(18) 0.0347(13) Uani 1 1 d . . . . . H22 H 0.5284 -0.1663 0.6497 0.042 Uiso 1 1 calc R U . . . C43 C 0.4620(4) 0.6166(4) 0.43799(16) 0.0253(11) Uani 1 1 d . . . . . C1 C 0.8825(4) -0.0072(4) 0.60205(17) 0.0265(11) Uani 1 1 d . . . . . C45 C 0.5618(6) 0.7479(5) 0.47981(18) 0.0360(13) Uani 1 1 d . . . . . C34 C 0.2422(5) 0.2944(4) 0.36485(18) 0.0284(11) Uani 1 1 d . . . . . C39 C 0.7661(5) 0.1350(5) 0.42009(18) 0.0343(13) Uani 1 1 d . . . . . C13 C 0.9971(5) 0.1166(5) 0.5137(2) 0.0382(13) Uani 1 1 d . . . . . H13 H 0.9228 0.1412 0.5054 0.046 Uiso 1 1 calc R U . . . C2 C 0.9159(4) 0.0864(5) 0.58125(17) 0.0285(11) Uani 1 1 d . . . . . C11 C 1.1934(6) 0.0723(5) 0.4990(2) 0.0410(15) Uani 1 1 d . . . . . H11 H 1.2536 0.0643 0.4803 0.049 Uiso 1 1 calc R U . . . C8 C 1.0149(5) 0.0855(4) 0.55263(17) 0.0296(12) Uani 1 1 d . . . . . C3 C 0.8515(4) 0.1956(5) 0.58567(17) 0.0279(11) Uani 1 1 d . . . . . C33 C 0.2899(5) 0.3403(5) 0.33173(17) 0.0321(12) Uani 1 1 d . . . . . C16 C 1.0036(5) -0.3010(5) 0.6279(2) 0.0356(13) Uani 1 1 d . . . . . H16 H 1.0199 -0.3440 0.6509 0.043 Uiso 1 1 calc R U . . . C19 C 0.9537(6) -0.1762(5) 0.56146(18) 0.0361(13) Uani 1 1 d . . . . . H19 H 0.9361 -0.1347 0.5383 0.043 Uiso 1 1 calc R U . . . C25 C 0.6454(6) -0.0035(6) 0.70297(18) 0.0429(15) Uani 1 1 d . . . . . H25 H 0.5723 -0.0382 0.7074 0.051 Uiso 1 1 calc R U . . . C12 C 1.0865(6) 0.1118(5) 0.4873(2) 0.0414(14) Uani 1 1 d . . . . . H12 H 1.0746 0.1356 0.4610 0.050 Uiso 1 1 calc R U . . . C28 C 0.8379(5) 0.0216(6) 0.69420(18) 0.0378(14) Uani 1 1 d . . . . . H28 H 0.9183 0.0069 0.6919 0.045 Uiso 1 1 calc R U . . . C20 C 0.6596(5) -0.0849(5) 0.57283(18) 0.0339(13) Uani 1 1 d . . . . . H20 H 0.7150 -0.0889 0.5524 0.041 Uiso 1 1 calc R U . . . B1 B 0.4765(5) 0.3825(5) 0.44600(18) 0.0217(11) Uani 1 1 d . . . . . C24 C 0.5776(5) 0.0034(5) 0.57814(18) 0.0318(12) Uani 1 1 d . . . . . H24 H 0.5672 0.0690 0.5618 0.038 Uiso 1 1 calc R U . . . C21 C 0.5140(5) -0.0228(5) 0.61180(19) 0.0345(13) Uani 1 1 d . . . . . H21 H 0.4531 0.0223 0.6225 0.041 Uiso 1 1 calc R U . . . C14 C 0.9354(4) -0.1238(4) 0.59802(17) 0.0255(11) Uani 1 1 d . . . . . C9 C 1.1242(5) 0.0518(5) 0.56433(19) 0.0336(13) Uani 1 1 d . . . . . H9 H 1.1384 0.0334 0.5909 0.040 Uiso 1 1 calc R U . . . C27 C 0.7853(5) 0.1290(5) 0.69196(19) 0.0370(13) Uani 1 1 d . . . . . H27 H 0.8234 0.2003 0.6873 0.044 Uiso 1 1 calc R U . . . C18 C 0.9969(6) -0.2869(5) 0.5588(2) 0.0426(15) Uani 1 1 d . . . . . H18 H 1.0088 -0.3208 0.5339 0.051 Uiso 1 1 calc R U . . . C29 C 0.7516(7) -0.0618(6) 0.70046(18) 0.0444(15) Uani 1 1 d . . . . . H29 H 0.7630 -0.1428 0.7026 0.053 Uiso 1 1 calc R U . . . C10 C 1.2135(5) 0.0447(5) 0.5370(2) 0.0412(15) Uani 1 1 d . . . . . H10 H 1.2883 0.0206 0.5450 0.049 Uiso 1 1 calc R U . . . C26 C 0.6661(6) 0.1143(6) 0.69775(19) 0.0388(14) Uani 1 1 d . . . . . H26 H 0.6097 0.1738 0.6981 0.047 Uiso 1 1 calc R U . . . C4 C 0.8891(5) 0.3004(5) 0.5711(2) 0.0371(14) Uani 1 1 d . . . . . H4 H 0.9606 0.3049 0.5576 0.044 Uiso 1 1 calc R U . . . C17 C 1.0229(5) -0.3488(5) 0.5920(2) 0.0388(15) Uani 1 1 d . . . . . H17 H 1.0542 -0.4244 0.5899 0.047 Uiso 1 1 calc R U . . . C23 C 0.6457(5) -0.1652(5) 0.60259(19) 0.0333(13) Uani 1 1 d . . . . . H23 H 0.6896 -0.2338 0.6058 0.040 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0226(2) 0.0242(2) 0.0208(2) -0.00015(18) 0.00136(17) -0.00461(15) F15 0.0352(16) 0.0343(16) 0.0276(18) -0.0022(13) -0.0088(13) 0.0049(13) F6 0.0271(15) 0.0267(15) 0.041(2) -0.0003(13) 0.0054(14) -0.0040(12) F5 0.0302(15) 0.0374(16) 0.0286(18) 0.0060(14) 0.0016(13) -0.0108(13) F16 0.0289(15) 0.0393(17) 0.0226(17) 0.0095(13) 0.0010(12) 0.0103(13) F11 0.0381(17) 0.0265(15) 0.0351(19) 0.0045(13) -0.0137(14) 0.0016(12) F20 0.0305(15) 0.0372(16) 0.0271(18) 0.0085(13) 0.0001(13) 0.0092(12) F10 0.0317(16) 0.0265(15) 0.042(2) 0.0010(14) 0.0020(14) -0.0049(12) F1 0.0288(15) 0.0411(17) 0.0253(17) 0.0068(13) 0.0054(12) -0.0085(13) F14 0.054(2) 0.046(2) 0.033(2) -0.0111(16) -0.0155(17) -0.0088(16) F2 0.051(2) 0.060(2) 0.0215(18) 0.0120(16) 0.0042(15) 0.0064(17) F17 0.0329(17) 0.054(2) 0.037(2) 0.0067(16) 0.0120(15) 0.0169(15) F19 0.0491(19) 0.0398(18) 0.0216(17) 0.0107(14) -0.0018(15) 0.0071(14) F18 0.050(2) 0.055(2) 0.0248(19) 0.0077(16) 0.0165(16) 0.0056(16) F7 0.0260(16) 0.049(2) 0.064(3) 0.0089(19) 0.0144(16) 0.0055(15) F3 0.058(2) 0.068(3) 0.028(2) 0.0000(18) -0.0213(17) -0.0035(19) F13 0.102(3) 0.0288(18) 0.043(2) -0.0063(16) -0.020(2) -0.0149(19) F9 0.060(2) 0.0226(16) 0.065(3) 0.0005(17) 0.012(2) 0.0047(15) F4 0.0379(18) 0.0446(19) 0.050(2) -0.0018(17) -0.0172(17) -0.0140(15) F12 0.086(3) 0.0218(16) 0.053(3) 0.0044(16) -0.024(2) 0.0064(17) F8 0.051(2) 0.042(2) 0.074(3) 0.007(2) 0.022(2) 0.0247(17) N1 0.027(2) 0.027(2) 0.033(3) 0.0021(19) 0.0002(19) -0.0022(17) C7 0.029(3) 0.030(3) 0.042(4) 0.005(3) 0.004(3) 0.005(2) C48 0.024(2) 0.021(2) 0.020(3) 0.0014(19) -0.002(2) -0.0016(18) C31 0.025(2) 0.022(2) 0.023(3) 0.0023(19) 0.002(2) 0.0017(18) C47 0.023(2) 0.029(3) 0.023(3) 0.000(2) 0.002(2) 0.0009(19) C32 0.033(3) 0.031(3) 0.020(3) 0.004(2) 0.006(2) 0.006(2) C46 0.034(3) 0.037(3) 0.019(3) -0.006(2) -0.001(2) -0.006(2) C49 0.027(3) 0.027(2) 0.018(3) 0.004(2) -0.002(2) 0.0014(19) C50 0.028(3) 0.030(3) 0.027(3) -0.001(2) 0.005(2) 0.003(2) C6 0.039(3) 0.027(3) 0.050(4) 0.002(3) 0.004(3) 0.005(2) C52 0.040(3) 0.024(2) 0.021(3) 0.006(2) -0.001(2) -0.001(2) C51 0.038(3) 0.029(3) 0.019(3) 0.001(2) 0.007(2) -0.003(2) C53 0.024(2) 0.024(2) 0.025(3) 0.001(2) -0.002(2) 0.0011(19) C36 0.022(2) 0.026(2) 0.014(2) 0.0009(19) -0.0014(18) 0.0017(18) C35 0.026(2) 0.022(2) 0.023(3) 0.003(2) 0.000(2) -0.0010(19) C37 0.030(3) 0.026(2) 0.020(3) 0.001(2) 0.001(2) 0.001(2) C30 0.024(2) 0.018(2) 0.024(3) 0.000(2) 0.002(2) 0.0034(18) C5 0.037(3) 0.027(3) 0.060(5) 0.009(3) 0.003(3) -0.006(2) C38 0.028(3) 0.036(3) 0.032(3) 0.008(2) 0.006(2) 0.003(2) C44 0.049(3) 0.026(3) 0.031(3) 0.003(2) 0.000(3) -0.003(2) C41 0.026(2) 0.028(3) 0.023(3) 0.003(2) -0.001(2) 0.0012(19) C42 0.021(2) 0.025(2) 0.020(3) 0.001(2) 0.0050(19) -0.0014(18) C15 0.030(2) 0.033(3) 0.030(3) 0.003(3) 0.000(2) 0.003(2) C40 0.046(3) 0.023(3) 0.028(3) 0.004(2) 0.002(3) 0.004(2) C22 0.035(3) 0.038(3) 0.031(3) 0.008(2) -0.009(2) -0.016(2) C43 0.027(2) 0.027(2) 0.022(3) 0.001(2) 0.000(2) -0.0008(19) C1 0.022(2) 0.031(3) 0.027(3) 0.001(2) 0.000(2) -0.0028(19) C45 0.054(4) 0.027(3) 0.027(3) -0.006(2) 0.003(3) -0.008(2) C34 0.027(3) 0.026(3) 0.032(3) -0.004(2) -0.006(2) 0.000(2) C39 0.035(3) 0.033(3) 0.035(3) 0.005(2) 0.010(2) 0.013(2) C13 0.036(3) 0.039(3) 0.040(4) 0.009(3) -0.002(3) -0.006(2) C2 0.026(3) 0.030(3) 0.029(3) 0.002(2) -0.002(2) -0.002(2) C11 0.043(3) 0.040(3) 0.040(4) -0.002(3) 0.020(3) 0.000(3) C8 0.030(3) 0.026(2) 0.033(3) 0.002(2) 0.004(2) -0.002(2) C3 0.026(2) 0.029(3) 0.029(3) 0.001(2) -0.002(2) 0.000(2) C33 0.039(3) 0.034(3) 0.023(3) -0.001(2) -0.009(2) 0.008(2) C16 0.034(3) 0.032(3) 0.041(4) 0.009(3) -0.001(3) 0.005(2) C19 0.049(3) 0.034(3) 0.025(3) 0.002(2) 0.002(3) -0.001(3) C25 0.042(3) 0.063(4) 0.023(3) -0.005(3) 0.008(3) -0.012(3) C12 0.054(4) 0.039(3) 0.031(3) 0.003(3) 0.010(3) -0.012(3) C28 0.035(3) 0.053(4) 0.026(3) -0.008(3) -0.011(2) 0.006(3) C20 0.034(3) 0.038(3) 0.030(3) -0.008(3) -0.004(2) -0.003(2) B1 0.024(3) 0.020(2) 0.021(3) 0.001(2) -0.003(2) 0.000(2) C24 0.035(3) 0.030(3) 0.031(3) 0.005(2) -0.011(2) -0.004(2) C21 0.028(3) 0.039(3) 0.037(3) -0.001(3) -0.002(2) -0.001(2) C14 0.021(2) 0.025(2) 0.031(3) 0.003(2) 0.005(2) -0.0011(18) C9 0.033(3) 0.028(3) 0.041(4) 0.008(2) 0.000(3) 0.000(2) C27 0.042(3) 0.035(3) 0.034(3) -0.012(3) -0.006(3) -0.004(2) C18 0.057(4) 0.036(3) 0.035(4) -0.010(3) 0.005(3) 0.002(3) C29 0.072(4) 0.038(3) 0.024(3) 0.004(3) -0.001(3) 0.005(3) C10 0.029(3) 0.032(3) 0.063(5) 0.002(3) 0.012(3) -0.001(2) C26 0.042(3) 0.048(3) 0.027(3) -0.016(3) -0.003(3) 0.011(3) C4 0.028(3) 0.035(3) 0.048(4) 0.006(3) 0.005(3) -0.004(2) C17 0.036(3) 0.026(3) 0.054(4) -0.001(3) 0.005(3) 0.005(2) C23 0.035(3) 0.025(3) 0.040(4) 0.001(2) -0.011(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C1 2.274(5) . ? Zr1 N1 2.276(4) . ? Zr1 C21 2.467(6) . ? Zr1 C22 2.473(5) . ? Zr1 C29 2.474(6) . ? Zr1 C25 2.483(6) . ? Zr1 C23 2.485(5) . ? Zr1 C24 2.486(6) . ? Zr1 C20 2.487(6) . ? Zr1 C26 2.509(6) . ? Zr1 C28 2.509(6) . ? Zr1 C27 2.511(6) . ? F15 C47 1.338(6) . ? F6 C37 1.351(6) . ? F5 C35 1.345(6) . ? F16 C49 1.355(6) . ? F11 C43 1.359(6) . ? F20 C53 1.357(6) . ? F10 C41 1.351(6) . ? F1 C31 1.356(6) . ? F14 C46 1.348(6) . ? F2 C32 1.337(7) . ? F17 C50 1.352(6) . ? F19 C52 1.337(6) . ? F18 C51 1.341(6) . ? F7 C38 1.345(7) . ? F3 C33 1.342(7) . ? F13 C45 1.337(7) . ? F9 C40 1.342(7) . ? F4 C34 1.336(6) . ? F12 C44 1.337(7) . ? F8 C39 1.334(6) . ? N1 C7 1.350(7) . ? N1 C3 1.364(7) . ? C7 C6 1.364(8) . ? C7 H7 0.9500 . ? C48 C53 1.382(7) . ? C48 C49 1.397(7) . ? C48 B1 1.656(8) . ? C31 C32 1.372(8) . ? C31 C30 1.390(7) . ? C47 C46 1.381(8) . ? C47 C42 1.391(8) . ? C32 C33 1.381(8) . ? C46 C45 1.373(9) . ? C49 C50 1.376(8) . ? C50 C51 1.365(8) . ? C6 C5 1.384(9) . ? C6 H6 0.9500 . ? C52 C51 1.379(8) . ? C52 C53 1.381(8) . ? C36 C37 1.376(7) . ? C36 C41 1.393(7) . ? C36 B1 1.668(7) . ? C35 C34 1.386(8) . ? C35 C30 1.390(7) . ? C37 C38 1.386(8) . ? C30 B1 1.651(7) . ? C5 C4 1.389(8) . ? C5 H5 0.9500 . ? C38 C39 1.368(8) . ? C44 C45 1.380(9) . ? C44 C43 1.382(8) . ? C41 C40 1.375(8) . ? C42 C43 1.388(7) . ? C42 B1 1.663(7) . ? C15 C14 1.387(8) . ? C15 C16 1.388(8) . ? C15 H15 0.9500 . ? C40 C39 1.378(9) . ? C22 C23 1.402(9) . ? C22 C21 1.409(8) . ? C22 H22 0.9500 . ? C1 C2 1.353(8) . ? C1 C14 1.488(7) . ? C34 C33 1.368(8) . ? C13 C12 1.376(9) . ? C13 C8 1.397(9) . ? C13 H13 0.9500 . ? C2 C3 1.476(7) . ? C2 C8 1.508(8) . ? C11 C10 1.362(10) . ? C11 C12 1.379(10) . ? C11 H11 0.9500 . ? C8 C9 1.383(8) . ? C3 C4 1.382(8) . ? C16 C17 1.367(10) . ? C16 H16 0.9500 . ? C19 C18 1.379(9) . ? C19 C14 1.407(8) . ? C19 H19 0.9500 . ? C25 C26 1.395(10) . ? C25 C29 1.405(10) . ? C25 H25 0.9500 . ? C12 H12 0.9500 . ? C28 C27 1.386(9) . ? C28 C29 1.405(10) . ? C28 H28 0.9500 . ? C20 C23 1.388(9) . ? C20 C24 1.407(8) . ? C20 H20 0.9500 . ? C24 C21 1.401(9) . ? C24 H24 0.9500 . ? C21 H21 0.9500 . ? C9 C10 1.396(9) . ? C9 H9 0.9500 . ? C27 C26 1.404(9) . ? C27 H27 0.9500 . ? C18 C17 1.376(10) . ? C18 H18 0.9500 . ? C29 H29 0.9500 . ? C10 H10 0.9500 . ? C26 H26 0.9500 . ? C4 H4 0.9500 . ? C17 H17 0.9500 . ? C23 H23 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zr1 N1 74.25(17) . . ? C1 Zr1 C21 129.2(2) . . ? N1 Zr1 C21 102.08(18) . . ? C1 Zr1 C22 120.4(2) . . ? N1 Zr1 C22 133.98(18) . . ? C21 Zr1 C22 33.13(19) . . ? C1 Zr1 C29 104.2(2) . . ? N1 Zr1 C29 132.2(2) . . ? C21 Zr1 C29 113.0(2) . . ? C22 Zr1 C29 89.1(2) . . ? C1 Zr1 C25 136.2(2) . . ? N1 Zr1 C25 122.7(2) . . ? C21 Zr1 C25 89.4(2) . . ? C22 Zr1 C25 78.9(2) . . ? C29 Zr1 C25 32.9(2) . . ? C1 Zr1 C23 87.54(19) . . ? N1 Zr1 C23 128.40(19) . . ? C21 Zr1 C23 54.49(19) . . ? C22 Zr1 C23 32.9(2) . . ? C29 Zr1 C23 98.8(2) . . ? C25 Zr1 C23 104.0(2) . . ? C1 Zr1 C24 99.1(2) . . ? N1 Zr1 C24 81.12(18) . . ? C21 Zr1 C24 32.9(2) . . ? C22 Zr1 C24 54.59(19) . . ? C29 Zr1 C24 143.4(2) . . ? C25 Zr1 C24 122.1(2) . . ? C23 Zr1 C24 54.22(18) . . ? C1 Zr1 C20 75.2(2) . . ? N1 Zr1 C20 95.97(19) . . ? C21 Zr1 C20 54.5(2) . . ? C22 Zr1 C20 54.3(2) . . ? C29 Zr1 C20 130.6(2) . . ? C25 Zr1 C20 133.1(2) . . ? C23 Zr1 C20 32.4(2) . . ? C24 Zr1 C20 32.9(2) . . ? C1 Zr1 C26 131.3(2) . . ? N1 Zr1 C26 90.3(2) . . ? C21 Zr1 C26 98.8(2) . . ? C22 Zr1 C26 103.7(2) . . ? C29 Zr1 C26 54.1(2) . . ? C25 Zr1 C26 32.5(2) . . ? C23 Zr1 C26 134.1(2) . . ? C24 Zr1 C26 124.2(2) . . ? C20 Zr1 C26 153.3(2) . . ? C1 Zr1 C28 84.3(2) . . ? N1 Zr1 C28 102.0(2) . . ? C21 Zr1 C28 143.1(2) . . ? C22 Zr1 C28 121.7(2) . . ? C29 Zr1 C28 32.7(2) . . ? C25 Zr1 C28 54.0(2) . . ? C23 Zr1 C28 124.1(2) . . ? C24 Zr1 C28 175.9(2) . . ? C20 Zr1 C28 147.9(2) . . ? C26 Zr1 C28 53.6(2) . . ? C1 Zr1 C27 98.9(2) . . ? N1 Zr1 C27 78.7(2) . . ? C21 Zr1 C27 130.8(2) . . ? C22 Zr1 C27 132.6(2) . . ? C29 Zr1 C27 53.9(2) . . ? C25 Zr1 C27 53.8(2) . . ? C23 Zr1 C27 152.7(2) . . ? C24 Zr1 C27 148.1(2) . . ? C20 Zr1 C27 173.1(2) . . ? C26 Zr1 C27 32.5(2) . . ? C28 Zr1 C27 32.1(2) . . ? C7 N1 C3 119.1(5) . . ? C7 N1 Zr1 125.3(4) . . ? C3 N1 Zr1 115.5(3) . . ? N1 C7 C6 122.9(6) . . ? N1 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C53 C48 C49 113.0(5) . . ? C53 C48 B1 127.5(5) . . ? C49 C48 B1 119.0(4) . . ? F1 C31 C32 115.5(4) . . ? F1 C31 C30 119.1(4) . . ? C32 C31 C30 125.4(5) . . ? F15 C47 C46 116.4(5) . . ? F15 C47 C42 119.7(4) . . ? C46 C47 C42 123.8(5) . . ? F2 C32 C31 121.2(5) . . ? F2 C32 C33 119.8(5) . . ? C31 C32 C33 119.0(5) . . ? F14 C46 C45 120.1(5) . . ? F14 C46 C47 119.8(5) . . ? C45 C46 C47 120.1(5) . . ? F16 C49 C50 115.9(4) . . ? F16 C49 C48 119.8(5) . . ? C50 C49 C48 124.4(5) . . ? F17 C50 C51 120.1(5) . . ? F17 C50 C49 120.1(5) . . ? C51 C50 C49 119.8(5) . . ? C7 C6 C5 118.7(5) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? F19 C52 C51 119.3(5) . . ? F19 C52 C53 121.1(5) . . ? C51 C52 C53 119.6(5) . . ? F18 C51 C50 120.5(5) . . ? F18 C51 C52 120.7(5) . . ? C50 C51 C52 118.8(5) . . ? F20 C53 C52 114.9(5) . . ? F20 C53 C48 120.7(5) . . ? C52 C53 C48 124.4(5) . . ? C37 C36 C41 113.7(5) . . ? C37 C36 B1 127.0(4) . . ? C41 C36 B1 118.8(4) . . ? F5 C35 C34 114.9(4) . . ? F5 C35 C30 121.0(5) . . ? C34 C35 C30 124.1(5) . . ? F6 C37 C36 121.6(5) . . ? F6 C37 C38 114.5(5) . . ? C36 C37 C38 123.9(5) . . ? C31 C30 C35 112.6(5) . . ? C31 C30 B1 119.6(4) . . ? C35 C30 B1 127.7(5) . . ? C6 C5 C4 119.0(5) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? F7 C38 C39 119.7(5) . . ? F7 C38 C37 120.3(5) . . ? C39 C38 C37 120.0(5) . . ? F12 C44 C45 120.0(5) . . ? F12 C44 C43 120.4(5) . . ? C45 C44 C43 119.5(5) . . ? F10 C41 C40 116.5(5) . . ? F10 C41 C36 119.2(4) . . ? C40 C41 C36 124.2(5) . . ? C43 C42 C47 113.6(5) . . ? C43 C42 B1 126.7(5) . . ? C47 C42 B1 119.0(4) . . ? C14 C15 C16 121.8(6) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? F9 C40 C41 121.2(5) . . ? F9 C40 C39 119.3(5) . . ? C41 C40 C39 119.5(5) . . ? C23 C22 C21 107.5(5) . . ? C23 C22 Zr1 74.0(3) . . ? C21 C22 Zr1 73.2(3) . . ? C23 C22 H22 126.2 . . ? C21 C22 H22 126.2 . . ? Zr1 C22 H22 118.5 . . ? F11 C43 C44 114.3(5) . . ? F11 C43 C42 121.4(5) . . ? C44 C43 C42 124.3(5) . . ? C2 C1 C14 124.0(5) . . ? C2 C1 Zr1 114.2(4) . . ? C14 C1 Zr1 120.5(3) . . ? F13 C45 C46 121.1(6) . . ? F13 C45 C44 120.4(6) . . ? C46 C45 C44 118.6(5) . . ? F4 C34 C33 120.1(5) . . ? F4 C34 C35 120.0(5) . . ? C33 C34 C35 119.9(5) . . ? F8 C39 C38 120.8(5) . . ? F8 C39 C40 120.5(5) . . ? C38 C39 C40 118.7(5) . . ? C12 C13 C8 120.5(6) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C1 C2 C3 119.2(5) . . ? C1 C2 C8 123.7(5) . . ? C3 C2 C8 117.1(5) . . ? C10 C11 C12 120.7(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C9 C8 C13 119.0(5) . . ? C9 C8 C2 120.6(5) . . ? C13 C8 C2 120.5(5) . . ? N1 C3 C4 120.0(5) . . ? N1 C3 C2 116.2(5) . . ? C4 C3 C2 123.8(5) . . ? F3 C33 C34 120.7(5) . . ? F3 C33 C32 120.4(5) . . ? C34 C33 C32 118.9(5) . . ? C17 C16 C15 120.0(6) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C19 C14 120.9(6) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C26 C25 C29 108.2(6) . . ? C26 C25 Zr1 74.8(4) . . ? C29 C25 Zr1 73.2(4) . . ? C26 C25 H25 125.9 . . ? C29 C25 H25 125.9 . . ? Zr1 C25 H25 118.0 . . ? C13 C12 C11 119.7(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C27 C28 C29 108.2(6) . . ? C27 C28 Zr1 74.0(3) . . ? C29 C28 Zr1 72.3(3) . . ? C27 C28 H28 125.9 . . ? C29 C28 H28 125.9 . . ? Zr1 C28 H28 119.6 . . ? C23 C20 C24 108.3(5) . . ? C23 C20 Zr1 73.7(3) . . ? C24 C20 Zr1 73.5(3) . . ? C23 C20 H20 125.9 . . ? C24 C20 H20 125.9 . . ? Zr1 C20 H20 118.8 . . ? C30 B1 C48 113.4(4) . . ? C30 B1 C42 113.3(4) . . ? C48 B1 C42 100.4(4) . . ? C30 B1 C36 102.0(4) . . ? C48 B1 C36 114.9(4) . . ? C42 B1 C36 113.4(4) . . ? C21 C24 C20 107.7(5) . . ? C21 C24 Zr1 72.8(3) . . ? C20 C24 Zr1 73.6(3) . . ? C21 C24 H24 126.2 . . ? C20 C24 H24 126.2 . . ? Zr1 C24 H24 119.3 . . ? C24 C21 C22 108.1(5) . . ? C24 C21 Zr1 74.3(3) . . ? C22 C21 Zr1 73.7(3) . . ? C24 C21 H21 126.0 . . ? C22 C21 H21 126.0 . . ? Zr1 C21 H21 118.0 . . ? C15 C14 C19 116.9(5) . . ? C15 C14 C1 120.5(5) . . ? C19 C14 C1 122.4(5) . . ? C8 C9 C10 120.0(6) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C28 C27 C26 108.4(6) . . ? C28 C27 Zr1 73.9(3) . . ? C26 C27 Zr1 73.7(3) . . ? C28 C27 H27 125.8 . . ? C26 C27 H27 125.8 . . ? Zr1 C27 H27 118.5 . . ? C17 C18 C19 120.6(6) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C25 C29 C28 107.5(6) . . ? C25 C29 Zr1 73.9(4) . . ? C28 C29 Zr1 75.0(4) . . ? C25 C29 H29 126.2 . . ? C28 C29 H29 126.2 . . ? Zr1 C29 H29 117.0 . . ? C11 C10 C9 120.0(6) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C25 C26 C27 107.7(6) . . ? C25 C26 Zr1 72.8(3) . . ? C27 C26 Zr1 73.9(3) . . ? C25 C26 H26 126.1 . . ? C27 C26 H26 126.1 . . ? Zr1 C26 H26 119.2 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C20 C23 C22 108.5(5) . . ? C20 C23 Zr1 73.9(3) . . ? C22 C23 Zr1 73.1(3) . . ? C20 C23 H23 125.7 . . ? C22 C23 H23 125.7 . . ? Zr1 C23 H23 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C7 C6 -1.2(9) . . . . ? Zr1 N1 C7 C6 174.2(5) . . . . ? F1 C31 C32 F2 -1.7(7) . . . . ? C30 C31 C32 F2 177.3(5) . . . . ? F1 C31 C32 C33 179.8(5) . . . . ? C30 C31 C32 C33 -1.2(8) . . . . ? F15 C47 C46 F14 1.5(8) . . . . ? C42 C47 C46 F14 180.0(5) . . . . ? F15 C47 C46 C45 -176.9(5) . . . . ? C42 C47 C46 C45 1.6(9) . . . . ? C53 C48 C49 F16 177.0(4) . . . . ? B1 C48 C49 F16 4.2(7) . . . . ? C53 C48 C49 C50 -1.9(8) . . . . ? B1 C48 C49 C50 -174.6(5) . . . . ? F16 C49 C50 F17 2.5(7) . . . . ? C48 C49 C50 F17 -178.6(5) . . . . ? F16 C49 C50 C51 -177.1(5) . . . . ? C48 C49 C50 C51 1.8(9) . . . . ? N1 C7 C6 C5 -0.8(10) . . . . ? F17 C50 C51 F18 -0.7(8) . . . . ? C49 C50 C51 F18 178.9(5) . . . . ? F17 C50 C51 C52 -179.9(5) . . . . ? C49 C50 C51 C52 -0.3(8) . . . . ? F19 C52 C51 F18 0.6(8) . . . . ? C53 C52 C51 F18 180.0(5) . . . . ? F19 C52 C51 C50 179.8(5) . . . . ? C53 C52 C51 C50 -0.8(8) . . . . ? F19 C52 C53 F20 -0.6(7) . . . . ? C51 C52 C53 F20 -180.0(5) . . . . ? F19 C52 C53 C48 -180.0(5) . . . . ? C51 C52 C53 C48 0.6(8) . . . . ? C49 C48 C53 F20 -178.7(4) . . . . ? B1 C48 C53 F20 -6.7(8) . . . . ? C49 C48 C53 C52 0.7(8) . . . . ? B1 C48 C53 C52 172.7(5) . . . . ? C41 C36 C37 F6 176.0(5) . . . . ? B1 C36 C37 F6 4.2(8) . . . . ? C41 C36 C37 C38 -2.1(8) . . . . ? B1 C36 C37 C38 -173.9(5) . . . . ? F1 C31 C30 C35 -178.2(4) . . . . ? C32 C31 C30 C35 2.8(7) . . . . ? F1 C31 C30 B1 -0.8(7) . . . . ? C32 C31 C30 B1 -179.8(5) . . . . ? F5 C35 C30 C31 178.1(4) . . . . ? C34 C35 C30 C31 -2.8(7) . . . . ? F5 C35 C30 B1 1.0(8) . . . . ? C34 C35 C30 B1 -180.0(5) . . . . ? C7 C6 C5 C4 1.2(11) . . . . ? F6 C37 C38 F7 2.4(8) . . . . ? C36 C37 C38 F7 -179.3(5) . . . . ? F6 C37 C38 C39 -176.3(5) . . . . ? C36 C37 C38 C39 1.9(9) . . . . ? C37 C36 C41 F10 -179.0(5) . . . . ? B1 C36 C41 F10 -6.5(7) . . . . ? C37 C36 C41 C40 0.1(8) . . . . ? B1 C36 C41 C40 172.7(5) . . . . ? F15 C47 C42 C43 177.9(5) . . . . ? C46 C47 C42 C43 -0.6(8) . . . . ? F15 C47 C42 B1 6.6(7) . . . . ? C46 C47 C42 B1 -171.8(5) . . . . ? F10 C41 C40 F9 2.0(8) . . . . ? C36 C41 C40 F9 -177.2(5) . . . . ? F10 C41 C40 C39 -178.8(5) . . . . ? C36 C41 C40 C39 2.0(9) . . . . ? F12 C44 C43 F11 0.5(8) . . . . ? C45 C44 C43 F11 179.8(5) . . . . ? F12 C44 C43 C42 -178.0(5) . . . . ? C45 C44 C43 C42 1.3(9) . . . . ? C47 C42 C43 F11 -179.3(4) . . . . ? B1 C42 C43 F11 -8.9(8) . . . . ? C47 C42 C43 C44 -0.9(8) . . . . ? B1 C42 C43 C44 169.5(5) . . . . ? F14 C46 C45 F13 0.0(9) . . . . ? C47 C46 C45 F13 178.3(6) . . . . ? F14 C46 C45 C44 -179.5(5) . . . . ? C47 C46 C45 C44 -1.2(9) . . . . ? F12 C44 C45 F13 -0.4(9) . . . . ? C43 C44 C45 F13 -179.7(6) . . . . ? F12 C44 C45 C46 179.2(6) . . . . ? C43 C44 C45 C46 -0.2(9) . . . . ? F5 C35 C34 F4 1.7(7) . . . . ? C30 C35 C34 F4 -177.5(5) . . . . ? F5 C35 C34 C33 -179.7(5) . . . . ? C30 C35 C34 C33 1.2(8) . . . . ? F7 C38 C39 F8 -0.6(9) . . . . ? C37 C38 C39 F8 178.2(6) . . . . ? F7 C38 C39 C40 -178.4(6) . . . . ? C37 C38 C39 C40 0.4(9) . . . . ? F9 C40 C39 F8 -0.8(9) . . . . ? C41 C40 C39 F8 -180.0(6) . . . . ? F9 C40 C39 C38 177.0(5) . . . . ? C41 C40 C39 C38 -2.2(9) . . . . ? C14 C1 C2 C3 175.6(5) . . . . ? Zr1 C1 C2 C3 8.5(7) . . . . ? C14 C1 C2 C8 -3.0(9) . . . . ? Zr1 C1 C2 C8 -170.1(4) . . . . ? C12 C13 C8 C9 1.1(9) . . . . ? C12 C13 C8 C2 -177.6(5) . . . . ? C1 C2 C8 C9 -56.1(8) . . . . ? C3 C2 C8 C9 125.3(6) . . . . ? C1 C2 C8 C13 122.5(6) . . . . ? C3 C2 C8 C13 -56.1(7) . . . . ? C7 N1 C3 C4 2.8(9) . . . . ? Zr1 N1 C3 C4 -173.0(5) . . . . ? C7 N1 C3 C2 -178.7(5) . . . . ? Zr1 N1 C3 C2 5.5(6) . . . . ? C1 C2 C3 N1 -9.5(8) . . . . ? C8 C2 C3 N1 169.1(5) . . . . ? C1 C2 C3 C4 168.8(6) . . . . ? C8 C2 C3 C4 -12.5(8) . . . . ? F4 C34 C33 F3 -0.6(8) . . . . ? C35 C34 C33 F3 -179.3(5) . . . . ? F4 C34 C33 C32 179.4(5) . . . . ? C35 C34 C33 C32 0.7(8) . . . . ? F2 C32 C33 F3 0.7(8) . . . . ? C31 C32 C33 F3 179.3(5) . . . . ? F2 C32 C33 C34 -179.3(5) . . . . ? C31 C32 C33 C34 -0.7(8) . . . . ? C14 C15 C16 C17 -0.2(8) . . . . ? C8 C13 C12 C11 2.2(9) . . . . ? C10 C11 C12 C13 -4.1(10) . . . . ? C31 C30 B1 C48 167.3(4) . . . . ? C35 C30 B1 C48 -15.7(7) . . . . ? C31 C30 B1 C42 53.7(6) . . . . ? C35 C30 B1 C42 -129.3(5) . . . . ? C31 C30 B1 C36 -68.5(5) . . . . ? C35 C30 B1 C36 108.4(5) . . . . ? C53 C48 B1 C30 135.6(5) . . . . ? C49 C48 B1 C30 -52.9(6) . . . . ? C53 C48 B1 C42 -103.3(5) . . . . ? C49 C48 B1 C42 68.3(5) . . . . ? C53 C48 B1 C36 18.7(7) . . . . ? C49 C48 B1 C36 -169.7(4) . . . . ? C43 C42 B1 C30 20.3(7) . . . . ? C47 C42 B1 C30 -169.8(4) . . . . ? C43 C42 B1 C48 -101.0(6) . . . . ? C47 C42 B1 C48 69.0(5) . . . . ? C43 C42 B1 C36 136.0(5) . . . . ? C47 C42 B1 C36 -54.0(6) . . . . ? C37 C36 B1 C30 104.4(6) . . . . ? C41 C36 B1 C30 -67.0(6) . . . . ? C37 C36 B1 C48 -132.5(5) . . . . ? C41 C36 B1 C48 56.0(6) . . . . ? C37 C36 B1 C42 -17.8(7) . . . . ? C41 C36 B1 C42 170.7(5) . . . . ? C23 C20 C24 C21 0.7(6) . . . . ? Zr1 C20 C24 C21 -65.4(4) . . . . ? C23 C20 C24 Zr1 66.1(4) . . . . ? C20 C24 C21 C22 -0.6(6) . . . . ? Zr1 C24 C21 C22 -66.5(4) . . . . ? C20 C24 C21 Zr1 65.9(4) . . . . ? C23 C22 C21 C24 0.3(6) . . . . ? Zr1 C22 C21 C24 66.9(4) . . . . ? C23 C22 C21 Zr1 -66.6(4) . . . . ? C16 C15 C14 C19 1.6(8) . . . . ? C16 C15 C14 C1 176.5(5) . . . . ? C18 C19 C14 C15 -1.6(8) . . . . ? C18 C19 C14 C1 -176.3(6) . . . . ? C2 C1 C14 C15 137.2(6) . . . . ? Zr1 C1 C14 C15 -56.5(6) . . . . ? C2 C1 C14 C19 -48.3(8) . . . . ? Zr1 C1 C14 C19 118.1(5) . . . . ? C13 C8 C9 C10 -2.5(8) . . . . ? C2 C8 C9 C10 176.1(5) . . . . ? C29 C28 C27 C26 1.5(7) . . . . ? Zr1 C28 C27 C26 66.1(4) . . . . ? C29 C28 C27 Zr1 -64.7(4) . . . . ? C14 C19 C18 C17 0.1(10) . . . . ? C26 C25 C29 C28 0.8(7) . . . . ? Zr1 C25 C29 C28 68.0(4) . . . . ? C26 C25 C29 Zr1 -67.2(5) . . . . ? C27 C28 C29 C25 -1.4(7) . . . . ? Zr1 C28 C29 C25 -67.3(4) . . . . ? C27 C28 C29 Zr1 65.9(5) . . . . ? C12 C11 C10 C9 2.6(10) . . . . ? C8 C9 C10 C11 0.7(9) . . . . ? C29 C25 C26 C27 0.1(7) . . . . ? Zr1 C25 C26 C27 -66.1(5) . . . . ? C29 C25 C26 Zr1 66.2(4) . . . . ? C28 C27 C26 C25 -0.9(7) . . . . ? Zr1 C27 C26 C25 65.4(4) . . . . ? C28 C27 C26 Zr1 -66.3(4) . . . . ? N1 C3 C4 C5 -2.5(10) . . . . ? C2 C3 C4 C5 179.2(6) . . . . ? C6 C5 C4 C3 0.5(10) . . . . ? C15 C16 C17 C18 -1.3(9) . . . . ? C19 C18 C17 C16 1.3(10) . . . . ? C24 C20 C23 C22 -0.5(6) . . . . ? Zr1 C20 C23 C22 65.4(4) . . . . ? C24 C20 C23 Zr1 -66.0(4) . . . . ? C21 C22 C23 C20 0.2(6) . . . . ? Zr1 C22 C23 C20 -65.9(4) . . . . ? C21 C22 C23 Zr1 66.1(4) . . . . ? _refine_diff_density_max 0.621 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.053 _shelxl_version_number 2013-4 _shelx_res_file ; TITL MM1507_0m_a.res in P4(3) CELL 1.54178 11.5751 11.5751 34.2480 90.000 90.000 90.000 ZERR 4.000 0.0001 0.0001 0.0005 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 1/2+Z SYMM -Y, X, 3/4+Z SYMM Y, -X, 1/4+Z SFAC C H N B F Zr UNIT 212 96 4 4 80 4 L.S. 20 HTAB CONF ACTA PLAN 0 BOND $H WPDB -1 FMAP 2 LIST 6 SIZE 0.150 0.150 0.270 TEMP -99.960 WGHT 0.022400 4.689100 FVAR 0.38811 ZR1 6 0.712622 0.015730 0.634429 11.00000 0.02261 0.02421 = 0.02082 -0.00015 0.00136 -0.00461 F15 5 0.643319 0.457887 0.502975 11.00000 0.03524 0.03429 = 0.02763 -0.00220 -0.00882 0.00487 F6 5 0.731664 0.440759 0.427383 11.00000 0.02706 0.02674 = 0.04070 -0.00026 0.00543 -0.00400 F5 5 0.244618 0.257175 0.430882 11.00000 0.03020 0.03738 = 0.02859 0.00601 0.00155 -0.01077 F16 5 0.251383 0.478543 0.462263 11.00000 0.02889 0.03934 = 0.02257 0.00950 0.00102 0.01031 F11 5 0.383068 0.607959 0.408752 11.00000 0.03813 0.02648 = 0.03507 0.00454 -0.01375 0.00164 F20 5 0.536982 0.235617 0.518532 11.00000 0.03051 0.03720 = 0.02712 0.00850 0.00009 0.00920 F10 5 0.465702 0.134551 0.445674 11.00000 0.03171 0.02652 = 0.04225 0.00100 0.00201 -0.00486 F1 5 0.550315 0.461459 0.370386 11.00000 0.02882 0.04112 = 0.02527 0.00685 0.00538 -0.00850 F14 5 0.692647 0.670826 0.525626 11.00000 0.05382 0.04566 = 0.03273 -0.01107 -0.01549 -0.00881 F2 5 0.442387 0.442906 0.302447 11.00000 0.05093 0.06014 = 0.02151 0.01200 0.00416 0.00643 F17 5 0.123800 0.455541 0.525909 11.00000 0.03294 0.05370 = 0.03728 0.00669 0.01199 0.01688 F19 5 0.409727 0.221278 0.582466 11.00000 0.04915 0.03977 = 0.02160 0.01072 -0.00177 0.00715 F18 5 0.202215 0.329915 0.587707 11.00000 0.04979 0.05548 = 0.02478 0.00775 0.01652 0.00560 F7 5 0.895147 0.289645 0.412392 11.00000 0.02595 0.04885 = 0.06449 0.00892 0.01443 0.00551 F3 5 0.235852 0.331045 0.297221 11.00000 0.05788 0.06753 = 0.02760 0.00002 -0.02128 -0.00354 F13 5 0.583103 0.855451 0.492087 11.00000 0.10215 0.02884 = 0.04329 -0.00635 -0.01970 -0.01487 F9 5 0.631093 -0.015449 0.425540 11.00000 0.05999 0.02263 = 0.06505 0.00049 0.01169 0.00471 F4 5 0.140264 0.240630 0.363159 11.00000 0.03787 0.04462 = 0.04962 -0.00176 -0.01716 -0.01400 F12 5 0.427746 0.817155 0.433706 11.00000 0.08563 0.02177 = 0.05267 0.00441 -0.02352 0.00644 F8 5 0.848709 0.059655 0.410620 11.00000 0.05062 0.04202 = 0.07386 0.00654 0.02159 0.02470 N1 3 0.750993 0.189744 0.606339 11.00000 0.02686 0.02676 = 0.03265 0.00206 0.00018 -0.00224 C7 1 0.686856 0.286313 0.610788 11.00000 0.02943 0.03003 = 0.04153 0.00493 0.00439 0.00477 AFIX 43 H7 2 0.616222 0.281105 0.624803 11.00000 -1.20000 AFIX 0 C48 1 0.400175 0.354866 0.485811 11.00000 0.02379 0.02070 = 0.02047 0.00142 -0.00155 -0.00165 C31 1 0.447395 0.405532 0.370178 11.00000 0.02512 0.02198 = 0.02299 0.00233 0.00230 0.00173 C47 1 0.590691 0.544196 0.484011 11.00000 0.02285 0.02880 = 0.02264 -0.00017 0.00209 0.00095 C32 1 0.394911 0.396389 0.334380 11.00000 0.03344 0.03150 = 0.01959 0.00434 0.00591 0.00616 C46 1 0.616238 0.654766 0.496438 11.00000 0.03352 0.03706 = 0.01926 -0.00610 -0.00052 -0.00639 C49 1 0.293742 0.409813 0.490893 11.00000 0.02692 0.02664 = 0.01832 0.00393 -0.00151 0.00143 C50 1 0.226934 0.401026 0.523993 11.00000 0.02754 0.03025 = 0.02715 -0.00091 0.00471 0.00261 C6 1 0.718944 0.390978 0.596062 11.00000 0.03863 0.02656 = 0.05038 0.00245 0.00376 0.00517 AFIX 43 H6 2 0.671155 0.456941 0.599458 11.00000 -1.20000 AFIX 0 C52 1 0.371028 0.283204 0.552215 11.00000 0.03961 0.02430 = 0.02090 0.00612 -0.00116 -0.00148 C51 1 0.265426 0.337695 0.554993 11.00000 0.03763 0.02942 = 0.01927 0.00063 0.00719 -0.00330 C53 1 0.434447 0.292520 0.518219 11.00000 0.02447 0.02403 = 0.02515 0.00106 -0.00196 0.00111 C36 1 0.589819 0.295853 0.439068 11.00000 0.02156 0.02618 = 0.01362 0.00091 -0.00137 0.00171 C35 1 0.298826 0.305962 0.400314 11.00000 0.02647 0.02210 = 0.02333 0.00257 -0.00011 -0.00098 C37 1 0.700786 0.328392 0.429713 11.00000 0.02955 0.02570 = 0.02033 0.00127 0.00085 0.00115 C30 1 0.402842 0.364229 0.405182 11.00000 0.02417 0.01770 = 0.02373 -0.00024 0.00156 0.00337 C5 1 0.822534 0.399152 0.576070 11.00000 0.03703 0.02671 = 0.06035 0.00863 0.00325 -0.00561 AFIX 43 H5 2 0.847751 0.471248 0.565918 11.00000 -1.20000 AFIX 0 C38 1 0.788449 0.251095 0.420888 11.00000 0.02761 0.03645 = 0.03245 0.00796 0.00600 0.00261 C44 1 0.483329 0.728374 0.450173 11.00000 0.04862 0.02608 = 0.03061 0.00252 -0.00041 -0.00348 C41 1 0.571748 0.176981 0.437628 11.00000 0.02601 0.02792 = 0.02299 0.00320 -0.00087 0.00120 C42 1 0.513059 0.519280 0.454175 11.00000 0.02146 0.02493 = 0.01976 0.00122 0.00501 -0.00142 C15 1 0.960020 -0.189597 0.630806 11.00000 0.02975 0.03303 = 0.03043 0.00292 -0.00044 0.00350 AFIX 43 H15 2 0.946717 -0.157561 0.655945 11.00000 -1.20000 AFIX 0 C40 1 0.655446 0.097660 0.427944 11.00000 0.04571 0.02341 = 0.02815 0.00374 0.00237 0.00363 C22 1 0.555924 -0.127839 0.627005 11.00000 0.03486 0.03825 = 0.03109 0.00761 -0.00910 -0.01636 AFIX 43 H22 2 0.528416 -0.166338 0.649669 11.00000 -1.20000 AFIX 0 C43 1 0.461972 0.616600 0.437993 11.00000 0.02686 0.02725 = 0.02168 0.00063 0.00035 -0.00084 C1 1 0.882543 -0.007240 0.602048 11.00000 0.02186 0.03057 = 0.02709 0.00099 0.00014 -0.00276 C45 1 0.561751 0.747901 0.479810 11.00000 0.05402 0.02736 = 0.02652 -0.00617 0.00282 -0.00838 C34 1 0.242248 0.294424 0.364846 11.00000 0.02734 0.02610 = 0.03176 -0.00396 -0.00569 0.00048 C39 1 0.766104 0.135034 0.420089 11.00000 0.03534 0.03270 = 0.03495 0.00547 0.00967 0.01318 C13 1 0.997144 0.116606 0.513691 11.00000 0.03569 0.03891 = 0.04010 0.00861 -0.00173 -0.00601 AFIX 43 H13 2 0.922806 0.141250 0.505395 11.00000 -1.20000 AFIX 0 C2 1 0.915943 0.086364 0.581245 11.00000 0.02593 0.03005 = 0.02948 0.00210 -0.00202 -0.00203 C11 1 1.193395 0.072313 0.498995 11.00000 0.04316 0.04025 = 0.03955 -0.00234 0.02001 0.00050 AFIX 43 H11 2 1.253628 0.064304 0.480349 11.00000 -1.20000 AFIX 0 C8 1 1.014923 0.085537 0.552632 11.00000 0.03001 0.02553 = 0.03319 0.00160 0.00389 -0.00187 C3 1 0.851523 0.195621 0.585670 11.00000 0.02588 0.02874 = 0.02921 0.00094 -0.00229 0.00004 C33 1 0.289943 0.340266 0.331731 11.00000 0.03921 0.03397 = 0.02307 -0.00141 -0.00938 0.00764 C16 1 1.003566 -0.301008 0.627915 11.00000 0.03432 0.03191 = 0.04069 0.00922 -0.00122 0.00529 AFIX 43 H16 2 1.019930 -0.344030 0.650881 11.00000 -1.20000 AFIX 0 C19 1 0.953714 -0.176212 0.561460 11.00000 0.04945 0.03406 = 0.02493 0.00188 0.00194 -0.00052 AFIX 43 H19 2 0.936073 -0.134735 0.538279 11.00000 -1.20000 AFIX 0 C25 1 0.645434 -0.003469 0.702970 11.00000 0.04245 0.06289 = 0.02331 -0.00547 0.00838 -0.01212 AFIX 43 H25 2 0.572252 -0.038181 0.707447 11.00000 -1.20000 AFIX 0 C12 1 1.086524 0.111781 0.487252 11.00000 0.05383 0.03949 = 0.03099 0.00320 0.01043 -0.01169 AFIX 43 H12 2 1.074637 0.135554 0.461008 11.00000 -1.20000 AFIX 0 C28 1 0.837879 0.021594 0.694199 11.00000 0.03454 0.05274 = 0.02601 -0.00785 -0.01077 0.00560 AFIX 43 H28 2 0.918343 0.006923 0.691902 11.00000 -1.20000 AFIX 0 C20 1 0.659604 -0.084885 0.572832 11.00000 0.03353 0.03829 = 0.02982 -0.00811 -0.00417 -0.00331 AFIX 43 H20 2 0.714983 -0.088895 0.552405 11.00000 -1.20000 AFIX 0 B1 4 0.476539 0.382485 0.446002 11.00000 0.02364 0.02034 = 0.02104 0.00093 -0.00307 -0.00043 C24 1 0.577570 0.003425 0.578136 11.00000 0.03451 0.02995 = 0.03093 0.00460 -0.01147 -0.00371 AFIX 43 H24 2 0.567183 0.069020 0.561838 11.00000 -1.20000 AFIX 0 C21 1 0.513953 -0.022837 0.611796 11.00000 0.02758 0.03888 = 0.03693 -0.00147 -0.00223 -0.00083 AFIX 43 H21 2 0.453140 0.022288 0.622492 11.00000 -1.20000 AFIX 0 C14 1 0.935399 -0.123768 0.598016 11.00000 0.02099 0.02484 = 0.03080 0.00285 0.00479 -0.00106 C9 1 1.124167 0.051763 0.564326 11.00000 0.03257 0.02754 = 0.04067 0.00801 -0.00038 -0.00026 AFIX 43 H9 2 1.138421 0.033371 0.590927 11.00000 -1.20000 AFIX 0 C27 1 0.785260 0.128952 0.691956 11.00000 0.04167 0.03503 = 0.03427 -0.01180 -0.00575 -0.00387 AFIX 43 H27 2 0.823354 0.200326 0.687291 11.00000 -1.20000 AFIX 0 C18 1 0.996895 -0.286927 0.558826 11.00000 0.05655 0.03579 = 0.03550 -0.00978 0.00473 0.00239 AFIX 43 H18 2 1.008814 -0.320823 0.533886 11.00000 -1.20000 AFIX 0 C29 1 0.751617 -0.061793 0.700458 11.00000 0.07184 0.03756 = 0.02381 0.00377 -0.00149 0.00493 AFIX 43 H29 2 0.763019 -0.142822 0.702601 11.00000 -1.20000 AFIX 0 C10 1 1.213524 0.044687 0.537045 11.00000 0.02859 0.03178 = 0.06309 0.00214 0.01214 -0.00098 AFIX 43 H10 2 1.288349 0.020606 0.545023 11.00000 -1.20000 AFIX 0 C26 1 0.666105 0.114274 0.697749 11.00000 0.04160 0.04793 = 0.02681 -0.01624 -0.00278 0.01077 AFIX 43 H26 2 0.609652 0.173840 0.698059 11.00000 -1.20000 AFIX 0 C4 1 0.889076 0.300420 0.571066 11.00000 0.02792 0.03548 = 0.04784 0.00606 0.00525 -0.00402 AFIX 43 H4 2 0.960629 0.304923 0.557565 11.00000 -1.20000 AFIX 0 C17 1 1.022891 -0.348788 0.591990 11.00000 0.03612 0.02639 = 0.05384 -0.00057 0.00456 0.00461 AFIX 43 H17 2 1.054156 -0.424429 0.589935 11.00000 -1.20000 AFIX 0 C23 1 0.645708 -0.165160 0.602585 11.00000 0.03494 0.02467 = 0.04023 0.00091 -0.01081 -0.00300 AFIX 43 H23 2 0.689633 -0.233813 0.605850 11.00000 -1.20000 AFIX 0 HKLF 4 REM MM1507_0m_a.res in P4(3) REM R1 = 0.0338 for 7629 Fo > 4sig(Fo) and 0.0343 for all 7737 data REM 685 parameters refined using 1 restraints END WGHT 0.0222 4.6894 REM Instructions for potential hydrogen bonds EQIV $1 y, -x+1, z+1/4 HTAB C6 F1_$1 REM Highest difference peak 0.621, deepest hole -0.383, 1-sigma level 0.053 Q1 1 0.7555 -0.0366 0.6437 11.00000 0.05 0.62 Q2 1 0.7118 -0.0435 0.6144 11.00000 0.05 0.40 Q3 1 0.7767 0.0394 0.6203 11.00000 0.05 0.40 Q4 1 0.6974 0.0993 0.6452 11.00000 0.05 0.31 Q5 1 1.1625 0.0130 0.5053 11.00000 0.05 0.30 Q6 1 0.8417 0.1243 0.5085 11.00000 0.05 0.26 Q7 1 0.7146 0.1018 0.6222 11.00000 0.05 0.26 Q8 1 0.6330 0.0353 0.6137 11.00000 0.05 0.23 Q9 1 0.2977 0.2843 0.3484 11.00000 0.05 0.20 Q10 1 0.8784 -0.1014 0.6223 11.00000 0.05 0.20 Q11 1 0.4893 0.4655 0.4533 11.00000 0.05 0.20 Q12 1 1.2038 0.0998 0.5158 11.00000 0.05 0.19 Q13 1 0.8808 0.3127 0.5152 11.00000 0.05 0.19 Q14 1 0.3951 0.4230 0.3940 11.00000 0.05 0.18 Q15 1 0.6753 -0.0016 0.4437 11.00000 0.05 0.18 Q16 1 0.6863 -0.0215 0.5770 11.00000 0.05 0.18 Q17 1 0.4346 0.3503 0.4689 11.00000 0.05 0.18 Q18 1 0.5204 0.1619 0.5021 11.00000 0.05 0.17 Q19 1 0.8656 -0.1763 0.6137 11.00000 0.05 0.17 Q20 1 0.8985 -0.2544 0.6326 11.00000 0.05 0.17 ; _shelx_res_checksum 78543 _shelx_hkl_file ; -1 0 0 1777.62 117.49 1 0 0 1715.53 118.99 -2 0 0 176.58 13.60 -2 0 0 173.78 13.90 2 0 0 172.88 14.20 -3 0 0 3815.12 239.18 -3 0 0 3734.73 254.47 3 0 0 3764.22 258.07 -4 0 0 1253.17 87.79 -4 0 0 1278.47 83.59 4 0 0 1221.08 89.09 -5 0 0 13.80 5.20 -5 0 0 12.90 4.80 5 0 0 15.40 5.30 -6 0 0 14.30 5.60 -6 0 0 11.20 5.50 6 0 0 14.20 5.70 -7 0 0 4054.19 263.77 -8 0 0 273.87 27.80 -9 0 0 128.29 6.80 -9 0 0 119.29 9.20 -10 0 0 185.58 9.10 -10 0 0 195.88 12.50 -11 0 0 253.57 11.50 -11 0 0 267.17 15.60 -12 0 0 115.69 6.40 -12 0 0 120.29 8.80 -13 0 0 55.89 4.00 -13 0 0 60.99 5.50 -13 1 0 10.60 2.10 -13 1 0 13.10 2.90 -12 1 0 16.40 2.60 -12 1 0 14.00 3.60 -11 1 0 205.88 13.00 -11 1 0 204.38 9.70 -10 1 0 190.98 12.10 -10 1 0 169.78 8.80 -9 1 0 37.60 5.30 -9 1 0 34.70 3.80 -8 1 0 6.70 5.70 7 -1 0 74.19 13.30 -7 1 0 78.29 12.70 6 -1 0 296.47 28.20 -6 1 0 291.87 26.60 5 -1 0 257.47 24.00 -5 1 0 250.47 20.90 -5 1 0 234.48 21.90 4 -1 0 1326.47 95.79 -4 1 0 1324.17 88.49 -4 1 0 1341.97 92.09 3 -1 0 332.37 27.50 -3 1 0 346.47 25.20 -3 1 0 338.47 24.90 -2 1 0 325.47 23.50 -2 1 0 342.07 23.50 1 -1 0 3411.66 226.88 -1 1 0 3344.87 230.98 -1 1 0 3404.96 213.18 0 -1 0 1863.61 123.59 0 1 0 1816.82 124.89 0 1 0 1823.92 115.59 -1 -1 0 3394.36 226.88 1 1 0 3339.07 212.18 -2 -1 0 982.10 71.19 -2 -1 0 1035.60 66.69 2 1 0 1036.20 70.29 -3 -1 0 12.40 4.10 -3 -1 0 16.10 4.40 3 1 0 13.60 3.20 -4 -1 0 297.97 24.50 4 1 0 279.07 22.80 -5 -1 0 4434.66 288.57 -5 -1 0 4531.95 307.47 5 1 0 4560.84 309.17 -6 -1 0 219.28 21.70 -6 -1 0 199.58 20.80 -7 -1 0 24.10 8.00 -7 -1 0 18.40 7.30 8 1 0 1749.22 122.09 -9 -1 0 164.38 8.10 -9 -1 0 163.08 11.00 -10 -1 0 7.20 2.20 -10 -1 0 6.10 3.00 -11 -1 0 135.09 9.90 -11 -1 0 138.59 7.30 -12 -1 0 151.58 7.60 -12 -1 0 154.98 10.40 -13 -1 0 88.89 6.70 -13 -1 0 86.49 4.90 -13 2 0 103.59 5.30 -13 2 0 94.99 6.90 -12 2 0 264.27 11.20 -12 2 0 249.38 14.60 -11 2 0 63.59 5.00 -11 2 0 71.39 6.90 -10 2 0 43.60 6.00 -10 2 0 50.49 4.50 -9 2 0 482.15 25.30 -9 2 0 493.55 19.20 8 -2 0 11.20 7.40 -8 2 0 9.40 6.40 7 -2 0 107.59 17.50 -7 2 0 151.38 17.70 6 -2 0 10.70 6.20 -6 2 0 18.10 6.60 5 -2 0 2680.33 192.08 -5 2 0 2743.03 176.88 4 -2 0 42.80 5.10 4 -2 0 43.50 8.50 -4 2 0 43.90 7.60 3 -2 0 382.76 27.50 3 -2 0 380.36 31.80 -3 2 0 395.16 28.50 2 -2 0 3442.36 234.48 -2 2 0 3540.35 240.28 -2 2 0 3508.55 221.38 1 -2 0 1063.79 72.79 -1 2 0 1045.10 74.99 -1 2 0 1073.99 69.09 0 -2 0 174.68 14.50 0 2 0 181.18 13.70 0 2 0 180.98 14.40 -1 -2 0 341.57 25.60 1 2 0 341.07 23.60 1 2 0 319.77 23.60 -2 -2 0 3459.55 231.98 2 2 0 3368.66 216.68 -3 -2 0 4581.24 315.27 3 2 0 4710.03 295.07 -4 -2 0 2383.36 169.88 4 2 0 2397.46 167.18 4 2 0 2581.74 159.68 -5 -2 0 341.97 30.70 5 2 0 351.56 29.30 -6 -2 0 165.28 19.40 6 2 0 169.98 18.90 -7 -2 0 2.90 4.70 7 2 0 15.60 7.20 8 2 0 9.20 6.70 -9 -2 0 716.83 35.70 -9 -2 0 729.03 26.90 -10 -2 0 46.10 4.30 -10 -2 0 36.40 5.40 -11 -2 0 300.47 12.70 -11 -2 0 289.47 17.00 -12 -2 0 349.27 19.20 -12 -2 0 359.66 14.30 -13 -2 0 7.60 2.60 -13 -2 0 6.10 1.70 -13 3 0 37.30 4.30 -13 3 0 40.60 3.30 -12 3 0 398.46 20.80 -12 3 0 405.16 15.90 -11 3 0 190.98 9.40 -11 3 0 206.58 12.70 -10 3 0 603.64 30.30 -10 3 0 586.44 22.80 -9 3 0 575.84 29.20 -9 3 0 570.44 22.00 8 -3 0 505.15 48.30 -8 3 0 492.85 43.60 7 -3 0 949.21 76.29 -7 3 0 910.01 69.19 6 -3 0 298.87 30.80 -6 3 0 286.27 26.90 5 -3 0 9.10 6.00 -5 3 0 22.20 6.80 4 -3 0 43.40 9.90 -4 3 0 58.99 9.20 3 -3 0 3025.80 214.28 3 -3 0 3050.59 206.28 -3 3 0 3119.09 196.68 2 -3 0 4648.94 310.77 -2 3 0 4601.04 292.77 1 -3 0 9.50 3.10 -1 3 0 17.80 4.70 -1 3 0 14.10 3.80 0 -3 0 3700.03 261.27 0 3 0 3976.20 264.17 0 3 0 3918.41 244.78 -1 -3 0 309.57 25.90 1 3 0 326.87 24.00 1 3 0 325.37 23.90 -2 -3 0 393.06 31.70 2 3 0 390.96 29.20 -3 -3 0 2988.30 205.38 3 3 0 2961.50 191.48 -4 -3 0 208.78 21.50 4 3 0 208.88 19.80 -5 -3 0 863.71 64.39 5 3 0 774.82 59.49 -6 -3 0 1015.90 77.49 6 3 0 991.90 73.09 -7 -3 0 593.44 50.89 7 3 0 560.44 47.50 -8 -3 0 677.63 59.89 8 3 0 726.33 57.59 -9 -3 0 323.37 13.30 -9 -3 0 306.57 17.60 -10 -3 0 1921.11 89.69 -10 -3 0 1955.00 67.79 -11 -3 0 217.88 10.00 -11 -3 0 212.58 13.30 -12 -3 0 48.00 3.80 -12 -3 0 41.80 5.10 -13 -3 0 10.50 1.90 -13 -3 0 10.20 2.60 -13 4 0 58.79 3.60 -12 4 0 13.90 2.40 -11 4 0 11.40 2.40 -10 4 0 162.98 11.60 -10 4 0 168.08 8.50 -10 4 0 173.88 11.40 -9 4 0 265.27 16.10 -9 4 0 255.27 11.60 8 -4 0 122.89 21.60 -8 4 0 119.29 9.50 -8 4 0 135.69 19.50 -8 4 0 120.29 6.70 7 -4 0 509.45 48.90 -7 4 0 520.65 44.00 6 -4 0 419.86 39.70 -6 4 0 369.66 33.80 5 -4 0 109.49 16.90 -5 4 0 104.39 13.90 4 -4 0 43.90 11.30 -4 4 0 38.30 8.30 3 -4 0 180.38 21.10 -3 4 0 216.18 18.80 2 -4 0 2461.75 166.28 2 -4 0 2377.26 172.28 -2 4 0 2485.95 158.08 1 -4 0 265.37 22.70 -1 4 0 287.97 22.50 -1 4 0 292.57 24.50 0 -4 0 1210.58 87.09 0 4 0 1261.67 87.69 0 4 0 1218.98 81.59 -1 -4 0 1343.27 95.99 1 4 0 1348.17 89.19 -2 -4 0 51.49 9.20 2 4 0 52.69 8.20 -3 -4 0 65.79 11.40 3 4 0 68.99 10.40 -4 -4 0 43.80 10.50 4 4 0 36.40 9.00 -5 -4 0 1874.01 138.59 5 4 0 1958.10 129.79 -6 -4 0 2.00 5.60 6 4 0 3.50 4.90 -7 -4 0 603.34 53.29 7 4 0 586.44 49.50 -8 -4 0 234.88 10.30 -8 -4 0 212.88 13.00 -8 -4 0 198.38 27.20 8 4 0 184.38 24.80 -9 -4 0 429.26 22.30 -9 -4 0 403.76 16.60 -10 -4 0 39.40 4.10 -10 -4 0 26.20 4.50 -11 -4 0 14.70 2.60 -11 -4 0 14.20 3.40 -12 -4 0 81.69 6.60 -12 -4 0 74.19 4.70 -13 -4 0 100.39 6.80 -12 5 0 77.49 4.70 -11 5 0 24.70 4.20 -11 5 0 24.30 3.10 -10 5 0 114.39 9.10 -10 5 0 99.49 6.30 -9 5 0 538.55 28.50 -9 5 0 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6 6 22 208.18 9.70 7 6 22 33.50 3.70 8 6 22 60.19 4.30 9 6 22 54.69 3.70 -9 7 22 88.39 6.50 -8 7 22 197.38 12.30 -7 7 22 174.08 11.70 -6 7 22 38.90 5.70 -5 7 22 607.04 32.60 -4 7 22 106.09 9.20 -3 7 22 70.19 7.30 -2 7 22 443.86 24.80 -1 7 22 714.53 37.30 0 7 22 103.59 8.80 1 7 22 474.35 26.00 4 7 22 32.00 3.90 5 7 22 954.90 34.70 6 7 22 354.66 14.40 7 7 22 172.08 8.00 8 7 22 116.59 5.90 9 7 22 48.70 3.30 -8 8 22 103.89 7.40 -7 8 22 102.79 8.00 -6 8 22 63.69 6.50 -5 8 22 78.29 7.50 -4 8 22 20.10 4.20 -3 8 22 223.18 14.60 -2 8 22 137.79 10.40 -1 8 22 125.59 9.80 0 8 22 209.38 13.60 3 8 22 136.89 7.20 4 8 22 223.48 10.10 5 8 22 27.30 3.30 6 8 22 5.80 1.90 7 8 22 217.48 9.40 8 8 22 92.59 4.80 -7 9 22 70.49 5.90 -6 9 22 54.49 5.60 -5 9 22 53.89 5.80 -4 9 22 207.88 13.40 -3 9 22 446.16 24.50 -2 9 22 90.39 8.00 -1 9 22 4.40 2.90 1 9 22 441.56 17.40 2 9 22 17.90 2.90 3 9 22 91.69 5.50 4 9 22 393.56 15.50 5 9 22 65.69 4.40 6 9 22 79.29 4.60 7 9 22 94.89 4.80 -5 10 22 215.58 12.70 -4 10 22 3.90 2.50 -3 10 22 0.80 2.00 -2 10 22 29.70 4.50 0 10 22 82.19 5.10 1 10 22 5.00 2.00 2 10 22 419.36 16.30 3 10 22 162.58 7.60 4 10 22 22.90 2.80 5 10 22 118.89 5.70 -3 11 22 21.10 3.40 0 11 22 31.60 3.00 1 11 22 72.39 4.30 2 11 22 125.29 6.00 3 11 22 10.50 1.90 2 11 -23 35.60 3.90 1 11 -23 58.19 5.10 0 11 -23 219.08 12.10 -1 11 -23 31.60 4.00 -2 11 -23 98.99 6.70 5 10 -23 260.87 14.00 4 10 -23 1.70 2.00 3 10 -23 141.19 9.20 2 10 -23 57.29 5.60 1 10 -23 76.09 6.40 0 10 -23 81.19 6.70 -1 10 -23 91.09 7.00 -2 10 -23 161.08 10.10 -3 10 -23 20.40 3.60 -4 10 -23 325.27 17.00 -5 10 -23 24.50 3.60 6 9 -23 31.10 4.20 5 9 -23 117.69 8.30 4 9 -23 129.29 9.10 3 9 -23 47.80 5.70 2 9 -23 4.80 2.70 1 9 -23 85.19 7.40 0 9 -23 105.99 8.20 -1 9 -23 77.69 7.00 -2 9 -23 253.57 14.60 -3 9 -23 12.70 3.50 -4 9 -23 111.19 8.20 -5 9 -23 7.90 2.60 -6 9 -23 37.50 4.30 6 -9 23 38.70 4.60 8 8 -23 50.19 4.50 4 8 -23 97.89 8.10 3 8 -23 933.81 45.30 2 8 -23 137.99 10.10 1 8 -23 436.96 23.40 0 8 -23 106.39 8.60 -1 8 -23 271.47 15.70 -2 8 -23 3.30 2.70 -3 8 -23 116.49 8.80 -4 8 -23 531.05 26.80 4 -8 23 506.15 28.00 -5 8 -23 84.59 7.30 5 -8 23 99.99 8.20 -6 8 -23 357.16 19.40 6 -8 23 378.46 20.80 -7 8 -23 30.60 4.10 7 -8 23 31.70 4.70 -8 8 -23 62.39 5.10 8 -8 23 69.59 5.70 3 7 -23 703.43 35.20 2 7 -23 348.47 19.50 1 7 -23 329.27 18.60 0 7 -23 218.68 13.60 -1 7 -23 136.79 9.80 -2 7 -23 564.94 28.80 -3 7 -23 110.39 8.70 3 -7 23 118.79 10.00 -4 7 -23 234.78 14.40 4 -7 23 237.18 15.50 -5 7 -23 14.50 3.80 5 -7 23 19.30 4.40 -6 7 -23 54.29 5.90 6 -7 23 63.09 6.90 -7 7 -23 13.70 3.30 7 -7 23 21.90 4.30 -8 7 -23 16.30 3.10 8 -7 23 11.40 3.10 2 6 -23 329.57 18.60 1 6 -23 453.95 24.00 0 6 -23 205.28 12.90 -1 6 -23 261.57 15.30 -2 6 -23 795.72 38.90 -3 6 -23 129.49 9.40 3 -6 23 135.59 10.80 -4 6 -23 143.19 11.00 4 -6 23 206.78 13.00 -5 6 -23 99.49 8.70 5 -6 23 148.19 10.80 -6 6 -23 145.59 9.70 6 -6 23 113.99 10.20 -7 6 -23 259.37 14.50 7 -6 23 228.28 15.40 -8 6 -23 29.70 4.30 8 -6 23 24.80 4.50 -9 6 -23 42.00 4.50 9 -6 23 54.69 5.40 1 5 -23 523.45 26.90 0 5 -23 146.69 10.10 -1 5 -23 128.19 9.20 -2 5 -23 203.28 11.70 2 -5 23 157.78 12.60 -3 5 -23 253.57 14.20 3 -5 23 217.28 15.30 -4 5 -23 125.89 9.50 4 -5 23 142.49 10.90 -5 5 -23 111.39 9.30 5 -5 23 160.78 11.40 -6 5 -23 244.38 14.80 6 -5 23 254.17 16.40 -7 5 -23 689.13 32.90 7 -5 23 619.64 34.80 -8 5 -23 258.57 14.70 8 -5 23 248.38 15.90 -9 5 -23 110.49 7.80 9 -5 23 111.69 8.60 -10 5 -23 243.28 13.20 10 -5 23 248.88 14.00 2 4 -23 78.89 17.10 1 -4 23 334.27 36.70 -2 4 -23 172.18 10.70 2 -4 23 164.18 11.80 2 -4 23 152.18 23.90 -3 4 -23 105.69 7.60 3 -4 23 79.59 8.30 -4 4 -23 431.76 23.20 4 -4 23 450.45 25.10 -5 4 -23 380.96 20.00 5 -4 23 343.17 21.30 -6 4 -23 33.50 5.00 6 -4 23 13.80 4.20 -7 4 -23 102.89 8.30 7 -4 23 109.29 9.50 -8 4 -23 107.39 8.20 8 -4 23 103.99 9.10 -9 4 -23 128.99 8.70 9 -4 23 120.09 9.30 -10 4 -23 3.20 2.00 10 -4 23 4.60 2.40 3 3 -23 1021.90 83.39 2 3 -23 51.89 14.00 1 3 -23 287.27 30.90 0 -3 23 48.80 13.70 1 -3 23 249.58 30.30 2 -3 23 288.77 33.60 3 -3 23 999.50 50.49 3 -3 23 979.80 83.19 -4 3 -23 327.37 17.40 4 -3 23 294.87 18.80 -5 3 -23 656.53 32.20 5 -3 23 628.44 34.40 -6 3 -23 118.69 8.90 -7 3 -23 699.63 36.20 7 -3 23 778.32 39.20 -8 3 -23 870.81 41.80 8 -3 23 847.52 44.30 -9 3 -23 51.79 5.30 9 -3 23 42.50 5.60 -10 3 -23 188.88 11.10 10 -3 23 190.68 11.80 4 2 -23 116.79 20.60 3 2 -23 224.48 28.00 2 2 -23 308.07 33.10 1 2 -23 385.96 37.80 -1 -2 23 403.16 39.30 0 2 -23 62.29 13.10 0 -2 23 50.19 13.50 1 -2 23 859.11 72.39 2 -2 23 345.57 37.00 3 -2 23 25.10 10.50 4 -2 23 135.39 10.30 4 -2 23 113.59 21.50 -5 2 -23 37.20 5.20 5 -2 23 31.60 5.50 -6 2 -23 347.77 17.60 6 -2 23 264.97 18.40 -7 2 -23 322.77 18.00 7 -2 23 323.97 19.60 -8 2 -23 124.19 9.20 8 -2 23 144.49 10.60 -9 2 -23 0.30 2.00 9 -2 23 1.30 2.40 -10 2 -23 46.70 5.00 10 -2 23 59.69 5.80 -11 2 -23 33.50 3.70 4 1 -23 319.17 35.70 3 1 -23 177.98 24.10 2 1 -23 836.52 69.59 -2 -1 23 858.01 70.29 1 1 -23 784.52 67.19 -1 -1 23 861.81 69.49 0 1 -23 122.59 18.80 0 -1 23 184.48 22.80 -1 1 -23 806.62 66.89 1 -1 23 868.11 70.89 2 -1 23 414.06 41.80 3 -1 23 280.07 32.70 4 -1 23 266.57 16.60 4 -1 23 245.28 31.00 5 -1 23 637.24 33.90 -6 1 -23 435.36 22.00 6 -1 23 392.66 23.50 -7 1 -23 275.47 15.30 7 -1 23 243.58 16.20 -8 1 -23 496.05 24.80 8 -1 23 461.45 26.30 -9 1 -23 83.19 7.00 9 -1 23 82.49 7.60 -10 1 -23 69.89 5.90 -11 1 -23 84.29 5.90 4 0 -23 165.88 23.70 3 0 -23 50.99 13.40 -3 0 23 33.40 11.40 2 0 -23 78.89 15.40 -2 0 23 68.99 14.40 1 0 -23 121.69 19.20 -1 0 23 191.58 23.10 0 0 -23 3.60 5.20 0 0 23 4.50 5.90 -1 0 -23 165.38 21.60 1 0 23 193.78 24.50 2 0 23 62.19 14.10 3 0 23 53.29 14.70 4 0 23 207.28 28.00 5 0 23 135.79 10.40 6 0 23 189.28 13.00 7 0 23 266.37 16.60 -8 0 -23 83.19 7.00 8 0 23 72.99 7.70 -9 0 -23 99.69 7.60 -10 0 -23 88.99 6.70 -11 0 -23 221.88 11.80 4 -1 -23 217.18 29.80 -4 1 23 327.27 33.20 3 -1 -23 321.67 33.90 -3 1 23 278.77 32.50 2 -1 -23 404.26 38.20 -2 1 23 340.17 37.30 1 -1 -23 706.73 61.99 -1 1 23 778.02 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33.70 1 3 23 288.07 33.90 -2 -3 -23 24.50 10.80 2 3 23 58.89 15.50 -3 -3 -23 953.90 77.59 3 3 23 940.31 79.79 4 3 23 61.39 6.70 5 3 23 271.67 16.70 -8 -3 -23 152.88 8.00 10 3 23 36.20 3.30 -8 4 23 121.49 9.20 -7 4 23 116.79 9.50 -6 4 23 8.40 3.50 -5 4 23 276.07 16.90 -4 4 23 430.66 24.20 -3 4 23 67.99 7.20 2 -4 -23 126.69 20.40 -2 4 23 106.29 8.90 -2 4 23 90.59 18.90 1 -4 -23 310.37 33.10 -1 4 23 243.08 31.60 -1 4 23 276.87 17.10 0 -4 -23 157.78 22.80 0 4 23 179.88 24.80 -1 -4 -23 207.78 28.10 1 4 23 304.57 32.70 -2 -4 -23 99.49 18.40 2 4 23 91.59 18.50 2 4 23 93.69 8.20 3 4 23 290.17 17.40 4 4 23 488.25 26.70 8 4 23 494.15 19.20 9 4 23 126.79 6.50 10 4 23 301.07 11.80 -8 5 23 211.98 13.20 -7 5 23 689.13 36.00 -6 5 23 364.36 21.30 -5 5 23 127.59 10.20 -4 5 23 137.99 10.50 -3 5 23 289.67 17.70 -1 5 23 85.49 8.00 0 5 23 144.29 10.70 1 5 23 686.63 35.90 2 5 23 44.50 5.80 3 5 23 664.63 34.80 7 5 23 17.60 2.90 8 5 23 87.99 5.30 9 5 23 7.50 1.80 10 5 23 25.10 2.40 -9 6 23 64.69 5.60 -8 6 23 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8.40 4 -4 27 99.19 9.10 -5 4 -27 424.46 22.00 5 -4 27 398.56 23.60 -6 4 -27 225.18 13.00 6 -4 27 193.98 13.90 -7 4 -27 117.99 8.40 7 -4 27 112.49 9.20 -8 4 -27 42.70 4.70 8 -4 27 36.60 5.10 -9 4 -27 85.89 6.20 9 -4 27 80.99 6.90 0 -3 27 393.06 22.30 1 -3 27 130.19 10.20 -2 3 -27 281.37 14.60 2 -3 27 196.38 15.00 -3 3 -27 206.98 12.90 3 -3 27 213.48 14.30 -4 3 -27 575.94 27.70 4 -3 27 500.15 29.40 -5 3 -27 160.38 10.80 5 -3 27 174.88 12.40 -6 3 -27 275.87 16.40 6 -3 27 320.67 18.50 -7 3 -27 113.19 8.20 7 -3 27 106.69 9.10 -8 3 -27 277.87 15.20 8 -3 27 278.27 16.70 -9 3 -27 119.09 8.10 9 -3 27 139.89 9.30 -1 -2 27 260.47 16.30 0 -2 27 189.18 12.90 1 -2 27 59.79 6.60 2 -2 27 74.79 7.70 3 -2 27 58.59 7.10 4 -2 27 100.39 9.10 -5 2 -27 48.00 5.90 5 -2 27 50.39 6.50 -6 2 -27 125.49 9.30 6 -2 27 150.78 11.00 -7 2 -27 50.39 5.70 7 -2 27 66.29 7.00 -8 2 -27 208.68 12.30 8 -2 27 210.18 13.60 -9 2 -27 22.70 3.60 9 -2 27 17.50 3.50 -10 2 -27 54.89 4.40 10 -2 27 56.99 4.90 -2 -1 27 64.89 7.20 -1 -1 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13.10 3 6 27 354.96 20.30 -7 7 27 74.19 6.20 -6 7 27 41.20 5.10 -5 7 27 109.19 8.70 -4 7 27 113.19 9.10 -3 7 27 112.89 9.20 -2 7 27 52.59 6.20 -1 7 27 113.29 9.10 0 7 27 13.00 3.50 1 7 27 112.09 9.00 2 7 27 37.10 5.40 -6 8 27 109.59 7.80 -5 8 27 174.98 11.30 -4 8 27 141.29 10.00 -3 8 27 6.40 2.90 -2 8 27 105.19 8.50 -1 8 27 82.59 7.30 0 8 27 154.58 10.70 1 8 27 246.48 14.80 -5 9 27 57.29 5.10 -4 9 27 4.30 2.30 -3 9 27 40.70 4.80 -2 9 27 43.40 5.10 -1 9 27 86.09 7.10 0 9 27 85.39 6.90 -2 10 27 137.69 8.50 0 10 -28 62.39 5.10 4 9 -28 10.80 2.50 3 9 -28 30.30 3.90 2 9 -28 206.08 11.80 1 9 -28 20.50 3.70 0 9 -28 14.10 3.10 -1 9 -28 184.08 11.00 -2 9 -28 142.49 9.10 -3 9 -28 24.10 3.60 -4 9 -28 93.89 6.50 6 8 -28 221.48 11.90 5 8 -28 50.49 4.80 4 8 -28 80.29 6.40 3 8 -28 104.79 7.60 2 8 -28 63.29 6.00 1 8 -28 -0.70 2.10 0 8 -28 93.99 7.40 -1 8 -28 241.78 13.90 -2 8 -28 25.50 4.20 -3 8 -28 193.38 11.70 -4 8 -28 38.60 4.60 -5 8 -28 52.59 4.80 5 -8 28 34.90 4.70 -6 8 -28 107.19 7.00 6 -8 28 114.59 7.50 7 7 -28 134.39 8.00 6 7 -28 19.50 3.20 5 7 -28 22.50 3.70 4 7 -28 250.07 14.30 3 7 -28 18.30 3.80 2 7 -28 77.69 6.90 1 7 -28 193.08 12.00 0 7 -28 247.68 14.40 -1 7 -28 11.50 3.40 -2 7 -28 72.49 6.60 -3 7 -28 975.10 46.70 -4 7 -28 35.80 4.70 4 -7 28 20.40 4.20 -5 7 -28 13.70 3.20 5 -7 28 14.60 3.50 -6 7 -28 62.19 5.50 6 -7 28 63.99 6.10 -7 7 -28 141.19 8.60 7 -7 28 150.28 9.60 7 6 -28 67.89 5.50 6 6 -28 41.40 4.70 5 6 -28 9.00 3.00 4 6 -28 119.99 8.80 3 6 -28 145.89 10.10 2 6 -28 187.98 12.10 1 6 -28 150.08 10.30 0 6 -28 169.38 11.10 -1 6 -28 215.08 13.20 -2 6 -28 56.19 6.00 -3 6 -28 59.19 6.20 3 -6 28 54.19 6.80 -4 6 -28 64.19 6.60 4 -6 28 91.29 7.90 -5 6 -28 182.88 11.60 5 -6 28 197.48 12.80 -6 6 -28 31.00 4.30 6 -6 28 27.80 4.70 -7 6 -28 12.80 2.90 7 -6 28 11.00 3.10 -8 6 -28 224.08 12.00 8 -6 28 225.18 13.10 6 5 -28 186.78 11.30 5 5 -28 440.76 22.80 4 5 -28 94.09 7.70 3 5 -28 81.39 7.30 2 5 -28 1066.59 50.89 1 5 -28 13.40 3.60 0 5 -28 142.29 9.80 -1 5 -28 366.66 19.90 -2 5 -28 906.01 42.70 2 -5 28 854.21 45.20 -3 5 -28 26.50 4.50 3 -5 28 24.20 4.90 -4 5 -28 1.00 2.50 4 -5 28 4.80 3.20 -5 5 -28 449.06 22.90 5 -5 28 419.96 24.50 -6 5 -28 8.20 2.90 6 -5 28 12.30 3.40 -7 5 -28 10.90 2.90 7 -5 28 10.90 3.20 -8 5 -28 62.89 5.10 8 -5 28 50.19 5.50 1 4 -28 147.49 10.10 0 4 -28 382.26 20.30 -1 4 -28 92.09 7.80 1 -4 28 105.09 8.60 -2 4 -28 4.00 2.50 2 -4 28 1.20 2.90 -3 4 -28 245.88 14.80 3 -4 28 260.17 16.40 -4 4 -28 260.77 16.10 4 -4 28 322.17 18.30 -5 4 -28 108.09 8.30 5 -4 28 114.19 9.60 -6 4 -28 103.39 7.70 6 -4 28 88.29 8.40 -7 4 -28 234.88 14.00 7 -4 28 266.47 15.70 -8 4 -28 67.19 5.60 8 -4 28 73.39 6.70 -9 4 -28 4.20 2.00 9 -4 28 5.00 2.30 0 -3 28 505.55 27.70 1 -3 28 28.10 4.80 2 -3 28 136.69 10.70 -3 3 -28 399.06 21.00 3 -3 28 387.96 23.00 -4 3 -28 28.50 4.40 4 -3 28 15.00 4.20 -5 3 -28 81.89 7.50 5 -3 28 116.59 9.30 -6 3 -28 162.48 10.50 6 -3 28 159.78 11.80 -7 3 -28 32.90 4.40 7 -3 28 18.20 4.30 -8 3 -28 105.69 7.40 8 -3 28 104.79 8.50 -9 3 -28 31.90 3.70 9 -3 28 23.10 3.90 -1 -2 28 270.47 16.60 0 -2 28 184.58 12.80 1 -2 28 218.38 14.10 2 -2 28 1198.78 60.09 3 -2 28 34.40 5.70 4 -2 28 120.09 10.30 5 -2 28 1086.19 55.19 -6 2 -28 233.38 12.90 6 -2 28 179.98 13.70 -7 2 -28 99.39 7.50 7 -2 28 106.59 9.00 -8 2 -28 73.19 6.10 8 -2 28 79.69 7.10 -9 2 -28 213.08 11.80 9 -2 28 219.68 12.80 -2 -1 28 194.18 13.10 -1 -1 28 392.16 22.30 0 -1 28 693.63 36.40 1 -1 28 446.06 25.00 2 -1 28 273.97 16.80 3 -1 28 111.39 9.40 4 -1 28 138.79 10.80 5 -1 28 27.70 5.40 6 -1 28 108.89 9.40 7 -1 28 204.78 13.50 8 -1 28 5.80 2.60 9 -1 28 16.30 3.30 -3 0 28 472.65 25.90 -2 0 28 206.78 13.70 -1 0 28 763.82 39.70 0 0 28 1266.27 62.99 1 0 28 661.33 35.10 2 0 28 169.78 12.20 3 0 28 513.45 28.10 4 0 28 395.66 22.70 5 0 28 153.58 11.30 6 0 28 240.28 15.20 7 0 28 224.18 14.10 8 0 28 95.39 7.90 9 0 28 12.60 3.00 -4 1 28 137.59 10.40 -3 1 28 90.59 8.30 -2 1 28 262.97 16.30 -1 1 28 466.65 26.00 0 1 28 769.92 40.10 1 1 28 520.95 28.60 2 1 28 220.88 14.60 3 1 28 40.70 6.00 4 1 28 123.99 10.10 5 1 28 239.88 15.50 6 1 28 194.88 13.20 7 1 28 19.40 4.10 8 1 28 251.27 14.90 -5 2 28 1016.40 51.09 -4 2 28 118.29 9.60 -3 2 28 47.40 6.30 -2 2 28 1200.68 60.09 -1 2 28 244.48 15.60 0 2 28 193.28 13.30 1 2 28 304.97 18.50 2 2 28 1292.87 64.49 3 2 28 140.59 10.80 4 2 28 3.60 3.10 5 2 28 888.11 45.60 6 2 28 56.89 6.60 7 2 28 70.89 6.90 -6 3 28 145.99 10.50 -5 3 28 102.09 8.60 -4 3 28 6.10 3.20 -3 3 28 360.06 21.10 -2 3 28 133.59 10.50 -1 3 28 29.90 5.20 1 3 28 96.79 8.60 2 3 28 40.50 6.20 3 3 28 421.76 24.00 4 3 28 232.58 15.10 5 3 28 26.60 4.90 6 3 28 79.39 7.40 -7 4 28 247.08 14.70 -6 4 28 95.99 8.20 -5 4 28 77.79 7.50 -4 4 28 340.97 20.00 -3 4 28 247.78 15.90 -2 4 28 4.70 2.90 -1 4 28 80.99 7.90 1 4 28 140.29 10.70 2 4 28 118.39 9.70 3 4 28 4.90 2.90 4 4 28 299.87 18.00 5 4 28 6.30 3.20 -8 5 28 38.40 4.50 -7 5 28 22.40 3.80 -6 5 28 15.00 3.60 -5 5 28 418.76 23.50 -4 5 28 3.60 2.80 -3 5 28 18.70 4.30 -2 5 28 821.02 42.60 -1 5 28 256.27 16.30 0 5 28 128.59 10.30 1 5 28 42.70 6.00 2 5 28 1116.49 56.09 3 5 28 92.29 8.10 4 5 28 82.09 7.60 -8 6 28 218.78 12.20 -7 6 28 22.70 3.70 -6 6 28 38.40 5.00 -5 6 28 216.08 14.00 -4 6 28 33.00 5.40 -3 6 28 67.39 7.00 -2 6 28 59.09 6.60 -1 6 28 240.28 15.40 0 6 28 228.98 14.80 1 6 28 143.99 10.70 2 6 28 169.28 11.80 3 6 28 140.39 10.20 -7 7 28 158.88 9.80 -6 7 28 66.39 6.10 -5 7 28 24.00 4.20 -4 7 28 13.60 3.80 -3 7 28 984.60 49.70 -2 7 28 62.69 6.60 -1 7 28 18.00 3.80 0 7 28 217.18 13.80 1 7 28 197.08 12.90 2 7 28 122.09 9.20 -6 8 28 93.29 6.80 -5 8 28 38.60 4.70 -4 8 28 47.30 5.40 -3 8 28 147.39 10.30 -2 8 28 20.30 4.00 -1 8 28 214.78 13.40 0 8 28 95.29 7.80 1 8 28 4.30 2.60 -4 9 28 119.29 8.10 -3 9 28 33.20 4.20 -2 9 28 116.99 8.30 -1 9 28 201.18 12.20 0 9 28 8.90 2.80 3 9 -29 134.99 8.20 2 9 -29 34.20 4.10 1 9 -29 43.10 4.60 0 9 -29 81.49 6.30 -1 9 -29 105.79 7.40 -2 9 -29 147.29 9.20 -3 9 -29 8.90 2.40 5 8 -29 153.58 9.00 4 8 -29 4.60 2.20 3 8 -29 77.29 6.20 2 8 -29 20.20 3.50 1 8 -29 324.77 17.40 0 8 -29 111.49 8.10 -1 8 -29 23.90 4.00 -2 8 -29 164.18 10.40 -3 8 -29 66.99 5.90 -4 8 -29 286.97 15.40 -5 8 -29 117.79 7.70 6 7 -29 191.78 10.70 5 7 -29 39.50 4.40 4 7 -29 67.39 6.00 3 7 -29 79.49 6.70 2 7 -29 10.60 3.20 1 7 -29 136.09 9.30 0 7 -29 127.49 9.10 -1 7 -29 257.07 14.80 -2 7 -29 35.10 4.80 -3 7 -29 8.80 3.00 -4 7 -29 192.58 11.80 4 -7 29 200.18 12.50 -5 7 -29 127.89 8.50 5 -7 29 129.29 9.20 -6 7 -29 167.38 10.10 6 -7 29 185.68 11.10 7 6 -29 173.38 9.80 6 6 -29 148.19 9.10 5 6 -29 71.89 6.20 4 6 -29 4.90 2.70 3 6 -29 194.98 12.10 2 6 -29 224.58 13.50 1 6 -29 63.99 6.20 0 6 -29 101.39 8.00 -1 6 -29 157.78 10.60 -2 6 -29 361.76 19.50 -3 6 -29 90.19 7.20 3 -6 29 67.99 7.30 -4 6 -29 434.86 22.40 4 -6 29 419.96 23.90 -5 6 -29 35.30 4.50 5 -6 29 28.00 4.70 -6 6 -29 135.99 9.10 6 -6 29 154.38 10.40 -7 6 -29 206.98 11.20 7 -6 29 188.68 12.10 5 5 -29 200.88 12.00 4 5 -29 38.20 5.30 3 5 -29 20.30 3.90 2 5 -29 17.90 3.90 1 5 -29 279.27 15.90 0 5 -29 346.77 18.80 -1 5 -29 150.78 10.30 -2 5 -29 232.28 13.80 2 -5 29 226.28 14.80 -3 5 -29 62.49 6.50 3 -5 29 80.39 7.90 -4 5 -29 83.29 7.10 4 -5 29 82.99 8.10 -5 5 -29 155.38 9.90 5 -5 29 141.39 10.90 -6 5 -29 80.19 6.80 6 -5 29 105.89 8.30 -7 5 -29 34.70 4.40 7 -5 29 56.19 5.80 -8 5 -29 151.08 8.30 8 -5 29 117.29 8.80 0 4 -29 175.38 11.20 -1 4 -29 189.78 12.30 1 -4 29 215.78 13.60 -2 4 -29 1.00 2.40 2 -4 29 15.00 4.20 -3 4 -29 356.66 19.90 3 -4 29 382.56 21.90 -4 4 -29 543.05 28.00 4 -4 29 563.64 30.40 -5 4 -29 58.99 6.10 5 -4 29 72.89 7.40 -6 4 -29 20.30 3.60 6 -4 29 2.90 2.80 -7 4 -29 80.39 6.30 7 -4 29 75.29 7.30 -8 4 -29 3.20 2.00 8 -4 29 0.60 2.30 0 -3 29 26.80 5.00 1 -3 29 588.94 31.60 2 -3 29 278.17 17.30 3 -3 29 238.88 15.80 -4 3 -29 323.67 17.10 4 -3 29 280.27 18.60 -5 3 -29 26.30 4.60 5 -3 29 40.70 6.00 -6 3 -29 185.28 11.40 6 -3 29 184.28 12.90 -7 3 -29 83.99 6.70 7 -3 29 85.29 7.80 -8 3 -29 100.09 7.30 8 -3 29 122.69 8.60 -9 3 -29 137.09 8.40 9 -3 29 157.78 9.30 -1 -2 29 601.44 32.00 0 -2 29 824.02 42.50 1 -2 29 326.97 19.50 2 -2 29 181.18 12.60 3 -2 29 55.99 6.80 4 -2 29 100.99 9.20 5 -2 29 5.20 3.30 6 -2 29 272.37 17.10 7 -2 29 13.40 3.70 -8 2 -29 28.50 3.80 8 -2 29 13.40 3.30 9 -2 29 17.70 3.20 -2 -1 29 304.47 18.30 -1 -1 29 383.56 22.00 0 -1 29 676.23 35.70 1 -1 29 419.76 24.00 2 -1 29 577.94 31.30 3 -1 29 847.42 43.70 4 -1 29 554.14 30.20 5 -1 29 325.37 19.60 6 -1 29 42.20 5.80 7 -1 29 180.68 12.10 8 -1 29 292.87 16.80 9 -1 29 49.30 5.10 -3 0 29 36.20 5.70 -2 0 29 803.32 41.40 -1 0 29 550.34 29.90 0 0 29 2.70 2.90 1 0 29 656.63 35.00 2 0 29 830.32 43.20 3 0 29 27.80 5.20 4 0 29 215.98 14.30 5 0 29 367.56 21.30 6 0 29 99.59 8.60 7 0 29 168.48 11.50 8 0 29 110.19 8.50 9 0 29 88.99 6.80 -4 1 29 576.14 30.80 -3 1 29 845.02 43.50 -2 1 29 576.34 31.00 -1 1 29 440.96 24.80 0 1 29 604.94 32.50 1 1 29 443.16 25.00 2 1 29 357.06 21.10 3 1 29 594.14 32.20 4 1 29 220.38 14.80 5 1 29 168.88 12.20 6 1 29 231.08 15.00 7 1 29 247.48 15.20 8 1 29 23.00 3.90 -5 2 29 23.70 4.60 -4 2 29 100.69 8.70 -3 2 29 87.49 8.20 -2 2 29 108.49 9.20 -1 2 29 377.16 21.90 0 2 29 798.72 41.60 1 2 29 596.44 32.20 2 2 29 152.18 11.50 3 2 29 275.97 17.30 4 2 29 11.40 3.70 5 2 29 190.58 13.10 6 2 29 441.56 24.50 7 2 29 39.20 5.30 -6 3 29 204.58 13.20 -5 3 29 45.60 5.90 -4 3 29 246.68 15.70 -3 3 29 368.66 21.60 -2 3 29 257.77 16.40 0 3 29 46.70 6.20 1 3 29 923.41 47.40 2 3 29 61.69 7.00 3 3 29 320.97 19.40 4 3 29 375.86 21.80 5 3 29 95.29 8.40 6 3 29 74.79 7.10 -7 4 29 52.19 5.50 -6 4 29 4.10 2.60 -5 4 29 49.20 6.10 -4 4 29 525.75 28.60 -3 4 29 341.17 20.30 -2 4 29 11.10 3.60 -1 4 29 243.48 15.80 0 4 29 190.38 13.20 1 4 29 577.54 31.30 2 4 29 136.89 10.60 3 4 29 282.27 17.30 4 4 29 519.15 28.20 5 4 29 95.89 8.10 -7 5 29 55.19 5.50 -6 5 29 103.39 8.30 -5 5 29 194.28 12.90 -4 5 29 108.29 9.00 -3 5 29 104.19 8.90 -2 5 29 143.59 11.00 -1 5 29 190.78 13.20 0 5 29 392.96 22.70 1 5 29 329.57 19.60 2 5 29 11.70 3.60 3 5 29 53.79 6.30 4 5 29 64.79 6.60 -7 6 29 208.88 12.30 -6 6 29 154.28 10.30 -5 6 29 17.20 3.80 -4 6 29 408.26 22.90 -3 6 29 84.49 7.80 -2 6 29 430.56 24.10 -1 6 29 212.08 14.00 0 6 29 132.39 10.20 1 6 29 44.80 5.90 2 6 29 247.68 15.40 3 6 29 182.58 12.00 -6 7 29 207.28 12.40 -5 7 29 131.59 9.40 -4 7 29 200.48 12.90 -3 7 29 12.70 3.40 -2 7 29 46.90 5.80 -1 7 29 227.28 14.20 0 7 29 145.49 10.30 1 7 29 179.98 11.90 2 7 29 14.30 3.40 -5 8 29 112.39 7.90 -4 8 29 333.77 18.50 -3 8 29 58.89 5.90 -2 8 29 121.89 9.00 -1 8 29 41.80 5.20 0 8 29 93.39 7.50 1 8 29 273.17 15.70 -3 9 29 2.30 1.90 -2 9 29 97.99 7.10 -1 9 29 137.99 9.00 0 9 29 84.59 6.60 2 9 -30 43.60 4.30 1 9 -30 49.20 4.50 0 9 -30 100.99 6.90 -1 9 -30 35.70 4.10 -2 9 -30 58.29 5.00 4 8 -30 79.79 5.80 3 8 -30 26.50 3.70 2 8 -30 31.00 4.10 1 8 -30 209.28 12.10 0 8 -30 19.60 3.40 -1 8 -30 56.69 5.40 -2 8 -30 23.70 3.80 -3 8 -30 98.09 7.10 -4 8 -30 203.48 11.40 6 7 -30 193.28 10.50 5 7 -30 81.99 6.10 4 7 -30 11.40 2.90 3 7 -30 23.90 3.80 2 7 -30 299.77 16.30 1 7 -30 15.70 3.50 0 7 -30 10.80 3.00 -1 7 -30 213.48 12.60 -2 7 -30 52.59 5.70 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50.09 5.60 4 -4 30 44.70 6.30 -5 4 -30 415.36 22.20 5 -4 30 440.46 24.30 -6 4 -30 68.09 6.00 6 -4 30 69.79 7.00 -7 4 -30 10.90 2.70 7 -4 30 7.20 3.10 -8 4 -30 90.99 6.20 0 -3 30 25.80 5.00 1 -3 30 272.77 17.10 2 -3 30 269.07 16.70 3 -3 30 190.98 13.30 4 -3 30 34.40 5.60 -5 3 -30 261.87 15.00 5 -3 30 272.07 16.90 -6 3 -30 47.90 5.10 6 -3 30 42.90 6.00 -7 3 -30 21.20 3.50 7 -3 30 18.70 3.80 -8 3 -30 23.20 3.60 8 -3 30 31.90 4.20 -1 -2 30 24.70 4.60 0 -2 30 1530.15 75.39 1 -2 30 318.27 19.30 2 -2 30 186.08 13.00 3 -2 30 328.07 19.50 4 -2 30 298.77 18.30 5 -2 30 16.10 4.00 6 -2 30 115.29 9.40 7 -2 30 327.27 18.80 8 -2 30 28.00 4.20 9 -2 30 53.19 4.90 -2 -1 30 371.66 21.30 -1 -1 30 358.66 21.00 0 -1 30 433.76 24.50 1 -1 30 382.86 22.30 2 -1 30 19.50 4.40 3 -1 30 6.70 3.00 4 -1 30 23.90 4.70 5 -1 30 109.79 9.10 6 -1 30 7.60 3.10 7 -1 30 29.50 4.70 8 -1 30 212.38 13.00 9 -1 30 55.79 5.00 -3 0 30 36.40 5.60 -2 0 30 1615.74 79.19 -1 0 30 392.46 22.60 0 0 30 0.90 2.70 1 0 30 486.95 27.10 2 0 30 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4.30 -5 6 33 52.99 5.10 -4 6 33 327.37 18.20 -3 6 33 108.79 8.20 -2 6 33 147.79 10.10 -1 6 33 20.60 3.90 0 6 33 193.58 12.40 1 6 33 246.18 14.80 2 6 33 96.29 7.60 3 6 33 155.28 10.00 -4 7 33 75.29 6.10 -3 7 33 2.80 2.20 -2 7 33 107.59 7.90 -1 7 33 162.58 10.50 0 7 33 47.20 5.10 1 7 33 105.59 7.60 2 7 33 1.30 1.90 -1 8 33 64.99 5.40 0 8 33 101.49 7.00 1 8 33 107.19 7.20 2 7 -34 296.57 15.00 1 7 -34 49.90 4.50 0 7 -34 47.10 4.60 -1 7 -34 289.47 15.00 -2 7 -34 339.67 17.20 1 6 -34 48.10 5.00 0 6 -34 110.89 7.60 -1 6 -34 71.99 5.90 -2 6 -34 9.00 2.70 -3 6 -34 163.18 9.50 -4 6 -34 1.20 1.90 4 -6 34 2.20 2.00 -3 5 -34 123.69 7.70 3 -5 34 91.49 7.80 -4 5 -34 185.48 10.70 4 -5 34 196.68 12.00 -5 5 -34 16.80 2.80 5 -5 34 8.20 2.70 1 -4 34 177.68 12.20 2 -4 34 301.47 17.60 3 -4 34 43.40 5.50 4 -4 34 117.49 8.90 5 -4 34 163.58 10.90 6 -4 34 66.99 6.00 0 -3 34 21.40 4.30 1 -3 34 214.28 13.80 2 -3 34 267.17 16.40 3 -3 34 185.78 12.50 4 -3 34 19.60 3.90 5 -3 34 229.38 14.20 6 -3 34 16.20 3.30 -1 -2 34 201.68 13.20 0 -2 34 550.94 29.60 1 -2 34 15.20 4.00 2 -2 34 73.19 7.40 3 -2 34 110.19 9.10 4 -2 34 198.78 13.20 5 -2 34 10.80 3.10 6 -2 34 47.10 5.30 7 -2 34 334.77 18.20 -2 -1 34 17.40 3.80 -1 -1 34 23.40 4.50 0 -1 34 458.65 25.50 1 -1 34 10.80 3.40 2 -1 34 157.18 11.40 3 -1 34 173.08 12.20 4 -1 34 4.50 2.80 5 -1 34 94.29 8.00 6 -1 34 56.89 5.80 7 -1 34 42.40 4.70 -3 0 34 16.60 4.00 -2 0 34 552.24 29.60 -1 0 34 381.86 21.80 0 0 34 1.10 2.50 1 0 34 494.25 27.30 2 0 34 542.05 29.50 3 0 34 10.40 3.60 4 0 34 60.29 6.60 5 0 34 345.07 19.70 6 0 34 131.99 9.40 7 0 34 47.50 5.00 -4 1 34 18.80 3.80 -3 1 34 141.39 10.30 -2 1 34 208.58 13.60 -1 1 34 24.90 4.70 0 1 34 423.56 23.90 1 1 34 17.40 4.10 2 1 34 24.60 4.70 3 1 34 220.78 14.40 4 1 34 152.48 11.00 5 1 34 33.80 5.00 6 1 34 95.69 7.60 7 1 34 303.07 16.50 -4 2 34 235.58 14.30 -3 2 34 82.59 7.50 -2 2 34 92.99 8.20 -1 2 34 26.30 4.90 0 2 34 540.45 29.30 1 2 34 172.58 12.10 2 2 34 77.49 7.50 3 2 34 281.87 17.10 4 2 34 273.77 16.50 5 2 34 53.49 5.80 6 2 34 14.60 3.10 7 2 34 354.26 18.50 -5 3 34 212.38 12.80 -4 3 34 31.40 4.50 -3 3 34 180.28 12.10 -2 3 34 267.57 16.40 -1 3 34 193.38 13.10 0 3 34 13.10 3.70 1 3 34 181.28 12.40 2 3 34 96.69 8.30 3 3 34 206.68 13.40 4 3 34 53.39 5.80 5 3 34 99.89 7.70 6 3 34 126.69 8.40 -6 4 34 80.89 6.10 -5 4 34 149.39 9.90 -4 4 34 105.89 8.10 -3 4 34 44.00 5.30 -2 4 34 299.57 17.70 -1 4 34 161.58 11.40 0 4 34 49.99 6.10 1 4 34 15.10 3.80 2 4 34 232.98 14.50 3 4 34 27.50 4.50 4 4 34 104.89 7.90 5 4 34 250.37 14.30 -5 5 34 5.10 2.30 -4 5 34 245.48 14.50 -3 5 34 86.19 7.20 -2 5 34 35.70 4.90 -1 5 34 30.80 4.80 0 5 34 347.17 19.80 1 5 34 111.29 8.70 2 5 34 8.60 2.90 3 5 34 228.98 13.70 4 5 34 162.78 10.20 -4 6 34 6.20 2.30 -3 6 34 142.69 9.60 -2 6 34 20.90 3.70 -1 6 34 83.29 6.90 0 6 34 154.58 10.30 1 6 34 57.39 5.70 2 6 34 39.00 4.70 3 6 34 7.50 2.40 -2 7 34 371.56 19.90 -1 7 34 303.37 16.70 0 7 34 49.60 5.00 1 7 34 40.00 4.40 2 7 34 315.17 16.70 0 7 -35 17.50 2.80 -2 6 -35 41.60 4.20 -3 6 -35 159.08 9.10 3 -5 35 10.60 2.80 4 -5 35 275.27 15.50 2 -4 35 29.00 4.70 3 -4 35 133.99 9.50 4 -4 35 29.40 4.50 5 -4 35 44.80 4.90 1 -3 35 496.55 26.80 2 -3 35 190.08 12.50 3 -3 35 185.98 12.30 4 -3 35 88.59 7.50 5 -3 35 75.99 6.70 6 -3 35 146.49 9.50 0 -2 35 76.79 7.30 1 -2 35 73.29 7.20 2 -2 35 33.30 5.30 3 -2 35 105.79 8.60 4 -2 35 48.80 5.80 5 -2 35 15.20 3.50 6 -2 35 100.59 7.60 -1 -1 35 441.06 24.30 0 -1 35 41.90 5.70 1 -1 35 456.85 25.30 2 -1 35 32.80 5.20 3 -1 35 88.29 7.80 4 -1 35 344.97 19.80 5 -1 35 42.20 5.30 6 -1 35 466.45 24.70 -2 0 35 49.99 6.00 -1 0 35 47.40 6.00 0 0 35 2.40 2.70 1 0 35 35.30 5.40 2 0 35 55.69 6.60 3 0 35 36.30 5.40 4 0 35 130.19 9.80 5 0 35 30.70 4.70 6 0 35 133.49 9.20 7 0 35 10.40 2.50 -3 1 35 114.99 8.80 -2 1 35 24.90 4.50 -1 1 35 428.26 23.80 0 1 35 51.59 6.10 1 1 35 458.05 25.40 2 1 35 60.29 6.70 3 1 35 528.75 28.60 4 1 35 14.90 3.70 5 1 35 53.19 5.70 6 1 35 147.89 9.70 -4 2 35 49.00 5.30 -3 2 35 139.79 10.00 -2 2 35 51.59 6.00 -1 2 35 66.49 6.90 0 2 35 34.10 5.40 1 2 35 37.10 5.40 2 2 35 55.39 6.30 3 2 35 163.58 11.30 4 2 35 31.50 4.80 5 2 35 26.80 4.20 6 2 35 52.19 5.00 -5 3 35 74.89 6.20 -4 3 35 72.89 6.40 -3 3 35 194.08 12.40 -2 3 35 151.78 10.60 -1 3 35 585.24 31.10 0 3 35 37.40 5.50 1 3 35 92.09 8.10 2 3 35 124.49 9.40 3 3 35 209.58 13.30 4 3 35 159.68 10.60 5 3 35 11.40 2.80 6 3 35 185.88 10.80 -5 4 35 71.39 5.90 -4 4 35 24.70 3.90 -3 4 35 170.18 11.10 -2 4 35 23.10 4.10 -1 4 35 11.50 3.20 0 4 35 149.09 10.60 1 4 35 358.06 20.30 2 4 35 49.20 5.70 3 4 35 96.99 7.70 4 4 35 29.30 4.20 5 4 35 269.97 14.90 -5 5 35 53.39 4.90 -4 5 35 326.87 17.90 -3 5 35 20.70 3.70 -2 5 35 12.80 3.10 -1 5 35 50.79 5.60 0 5 35 27.00 4.50 1 5 35 43.30 5.20 2 5 35 14.60 3.30 3 5 35 60.69 5.60 4 5 35 65.19 5.50 -3 6 35 173.48 10.80 -2 6 35 41.70 4.80 -1 6 35 171.88 10.80 0 6 35 102.39 7.60 1 6 35 476.35 24.80 2 6 35 118.29 8.00 3 6 35 142.49 8.70 -1 7 35 49.30 4.70 0 7 35 14.50 2.70 3 -5 36 14.90 3.00 4 -5 36 27.00 3.70 2 -4 36 55.29 5.60 3 -4 36 200.68 12.30 4 -4 36 83.79 6.70 5 -4 36 3.20 2.00 1 -3 36 37.90 5.10 2 -3 36 59.89 6.10 3 -3 36 96.79 7.80 4 -3 36 147.89 10.10 5 -3 36 77.09 6.30 0 -2 36 23.60 4.20 1 -2 36 147.39 10.50 2 -2 36 335.27 19.30 3 -2 36 9.00 3.00 4 -2 36 18.00 3.60 5 -2 36 436.66 23.30 6 -2 36 61.89 5.50 -1 -1 36 43.20 5.40 0 -1 36 32.50 5.10 1 -1 36 59.99 6.40 2 -1 36 15.40 3.70 3 -1 36 3.00 2.70 4 -1 36 231.58 14.20 5 -1 36 67.79 6.30 6 -1 36 67.69 5.90 -2 0 36 27.90 4.50 -1 0 36 55.99 6.10 0 0 36 1055.39 52.79 1 0 36 47.00 5.80 2 0 36 12.20 3.40 3 0 36 221.58 14.00 4 0 36 70.79 6.70 5 0 36 24.00 4.00 6 0 36 63.19 5.60 -3 1 36 5.40 2.60 -2 1 36 15.40 3.40 -1 1 36 37.20 5.20 0 1 36 48.40 5.80 1 1 36 53.59 6.10 2 1 36 138.59 10.20 3 1 36 25.60 4.40 4 1 36 75.59 6.80 5 1 36 229.28 13.70 6 1 36 173.38 10.50 -4 2 36 11.00 2.80 -3 2 36 16.30 3.50 -2 2 36 319.47 18.40 -1 2 36 135.49 9.90 0 2 36 15.00 3.80 1 2 36 12.20 3.50 2 2 36 331.37 19.10 3 2 36 67.99 6.50 4 2 36 49.30 5.40 5 2 36 81.79 6.60 6 2 36 103.99 7.10 -5 3 36 85.29 6.40 -4 3 36 166.68 10.50 -3 3 36 77.39 6.60 -2 3 36 69.79 6.60 -1 3 36 16.10 3.60 0 3 36 269.87 16.20 1 3 36 3.60 2.50 2 3 36 12.50 3.30 3 3 36 92.19 7.50 4 3 36 183.08 11.40 5 3 36 16.80 3.10 -5 4 36 2.80 2.00 -4 4 36 81.19 6.50 -3 4 36 191.38 11.80 -2 4 36 38.70 4.80 -1 4 36 74.59 6.80 0 4 36 89.09 7.50 1 4 36 211.38 13.20 2 4 36 14.50 3.20 3 4 36 187.28 11.70 4 4 36 87.59 6.60 5 4 36 36.40 3.90 -4 5 36 27.60 3.80 -3 5 36 18.60 3.20 -2 5 36 95.29 7.30 -1 5 36 201.28 12.30 0 5 36 25.00 4.20 1 5 36 88.69 7.10 2 5 36 438.36 23.20 3 5 36 89.99 6.70 4 5 36 7.10 2.20 -2 6 36 125.29 8.30 -1 6 36 192.18 11.50 0 6 36 52.59 5.00 1 6 36 84.79 6.40 2 6 36 73.69 5.70 2 -4 37 44.70 4.80 3 -4 37 69.19 5.80 4 -4 37 253.97 14.20 1 -3 37 350.46 19.30 2 -3 37 50.89 5.50 3 -3 37 3.30 2.30 4 -3 37 261.37 15.00 0 -2 37 76.49 6.70 1 -2 37 25.80 4.40 2 -2 37 50.29 5.70 3 -2 37 27.60 4.30 4 -2 37 57.69 5.70 5 -2 37 28.50 4.10 -1 -1 37 158.28 10.60 0 -1 37 191.58 12.30 1 -1 37 150.18 10.40 2 -1 37 93.59 7.80 3 -1 37 184.68 12.00 4 -1 37 81.59 7.00 5 -1 37 111.29 8.00 -2 0 37 67.99 6.30 -1 0 37 174.98 11.50 0 0 37 4.90 2.60 1 0 37 166.38 11.30 2 0 37 90.89 7.70 3 0 37 77.39 7.00 4 0 37 75.29 6.70 5 0 37 55.19 5.40 -3 1 37 161.78 10.40 -2 1 37 102.99 8.10 -1 1 37 178.78 11.70 0 1 37 148.79 10.40 1 1 37 150.78 10.60 2 1 37 27.50 4.50 3 1 37 322.47 18.30 4 1 37 110.89 8.20 5 1 37 155.78 9.90 -4 2 37 49.20 4.90 -3 2 37 31.90 4.30 -2 2 37 29.80 4.50 -1 2 37 44.30 5.30 0 2 37 74.29 6.90 1 2 37 106.29 8.40 2 2 37 39.40 5.00 3 2 37 54.69 5.70 4 2 37 50.99 5.30 5 2 37 130.99 8.60 -4 3 37 271.57 15.00 -3 3 37 15.20 3.10 -2 3 37 39.90 4.80 -1 3 37 320.57 18.20 0 3 37 74.79 6.70 1 3 37 166.08 11.10 2 3 37 34.60 4.70 3 3 37 7.70 2.70 4 3 37 94.89 7.00 -4 4 37 214.88 12.30 -3 4 37 73.39 6.10 -2 4 37 39.60 4.70 -1 4 37 124.59 8.90 0 4 37 69.09 6.30 1 4 37 74.09 6.60 2 4 37 62.89 5.80 3 4 37 271.57 15.20 4 4 37 227.18 12.70 -2 5 37 129.99 8.60 -1 5 37 172.98 10.70 0 5 37 40.80 4.60 1 5 37 120.19 8.20 2 5 37 17.50 3.10 1 -3 38 134.99 9.00 2 -3 38 29.00 4.10 3 -3 38 12.00 2.80 0 -2 38 284.07 16.10 1 -2 38 6.00 2.70 2 -2 38 31.20 4.50 3 -2 38 286.97 16.30 4 -2 38 73.49 6.10 -1 -1 38 11.20 3.00 0 -1 38 100.69 7.70 1 -1 38 10.30 2.90 2 -1 38 87.29 7.20 3 -1 38 79.89 6.80 4 -1 38 47.10 5.10 -2 0 38 285.57 16.10 -1 0 38 91.79 7.30 0 0 38 0.70 2.20 1 0 38 109.59 8.30 2 0 38 264.37 15.60 3 0 38 6.10 2.60 4 0 38 28.80 4.10 -3 1 38 73.99 6.00 -2 1 38 109.09 8.00 -1 1 38 5.00 2.40 0 1 38 92.59 7.50 1 1 38 3.70 2.30 2 1 38 2.50 2.30 3 1 38 134.49 9.20 4 1 38 176.88 10.90 -3 2 38 273.17 15.20 -2 2 38 28.20 4.20 -1 2 38 6.40 2.60 0 2 38 298.47 17.10 1 2 38 93.09 7.50 2 2 38 28.00 4.30 3 2 38 45.40 4.90 4 2 38 101.59 7.30 -4 3 38 31.60 3.80 -3 3 38 10.70 2.60 -2 3 38 36.80 4.40 -1 3 38 106.19 7.90 0 3 38 6.30 2.60 1 3 38 68.69 6.20 2 3 38 304.57 17.10 3 3 38 14.60 3.00 -3 4 38 31.10 3.80 -2 4 38 92.39 6.80 -1 4 38 186.78 11.40 0 4 38 17.40 3.20 1 4 38 74.39 6.20 2 4 38 74.59 6.10 2 -3 39 26.60 3.70 0 -2 39 54.99 5.20 1 -2 39 96.49 7.20 2 -2 39 133.09 8.80 3 -2 39 3.50 2.20 -1 -1 39 97.89 7.20 0 -1 39 16.90 3.20 1 -1 39 96.59 7.30 2 -1 39 279.37 15.80 3 -1 39 51.69 5.00 -2 0 39 53.59 5.10 -1 0 39 19.60 3.40 0 0 39 -0.70 1.70 1 0 39 23.60 3.90 2 0 39 44.20 4.90 3 0 39 53.19 5.10 4 0 39 35.20 4.10 -2 1 39 251.57 14.30 -1 1 39 92.39 7.10 0 1 39 35.70 4.50 1 1 39 83.19 6.80 2 1 39 87.99 6.90 3 1 39 87.99 6.80 -3 2 39 6.70 2.20 -2 2 39 137.99 8.90 -1 2 39 103.99 7.60 0 2 39 35.60 4.50 1 2 39 276.67 15.70 2 2 39 135.79 9.10 3 2 39 22.60 3.60 -2 3 39 23.30 3.50 -1 3 39 124.79 8.40 0 3 39 39.10 4.50 1 3 39 57.79 5.40 2 3 39 4.30 2.20 0 4 39 42.30 4.40 1 -2 40 147.79 9.10 0 -1 40 76.29 6.00 1 -1 40 3.40 2.00 2 -1 40 35.50 4.10 -1 0 40 81.39 6.20 0 0 40 414.96 21.80 1 0 40 70.09 5.80 2 0 40 3.70 1.90 -2 1 40 29.90 3.60 -1 1 40 -0.40 1.70 0 1 40 77.39 6.10 1 1 40 4.70 2.10 2 1 40 137.09 8.90 -1 2 40 136.59 8.80 0 2 40 3.70 2.00 1 2 40 37.70 4.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' ; _shelx_hkl_checksum 62254 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Warren Piers' _publ_contact_author_address ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Morgan, Matthew' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; 'Piers, Warren' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_MM1511 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C29 H24 Cl N Zr' _chemical_formula_sum 'C29 H24 Cl N Zr' _chemical_formula_weight 513.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.7014(7) _cell_length_b 20.2371(15) _cell_length_c 7.7474(4) _cell_angle_alpha 90 _cell_angle_beta 104.290(4) _cell_angle_gamma 90 _cell_volume 2233.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4539 _cell_measurement_theta_min 35.81 _cell_measurement_theta_max 72.45 _exptl_crystal_description 'block' _exptl_crystal_colour 'Colourless' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_F_000 1048 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 5.253 _shelx_estimated_absorpt_T_min 0.622 _shelx_estimated_absorpt_T_max 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.628 _exptl_absorpt_correction_T_max 0.725 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15564 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.102 _diffrn_reflns_theta_max 72.564 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 4307 _reflns_number_gt 3806 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.1.7' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0723P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4307 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.25638(17) 0.48071(12) 0.1486(3) 0.0107(5) Uani 1 1 d . . . . . C2 C 0.17929(18) 0.47474(12) 0.2125(3) 0.0103(5) Uani 1 1 d . . . . . C3 C 0.12966(17) 0.53471(13) 0.2428(3) 0.0105(5) Uani 1 1 d . . . . . C4 C 0.05001(18) 0.53295(13) 0.3119(3) 0.0140(5) Uani 1 1 d . . . . . H4 H 0.0215 0.4918 0.3260 0.017 Uiso 1 1 calc R U . . . C5 C 0.0132(2) 0.59089(14) 0.3594(4) 0.0173(6) Uani 1 1 d . . . . . H5 H -0.0412 0.5903 0.4050 0.021 Uiso 1 1 calc R U . . . C6 C 0.0566(2) 0.64953(14) 0.3394(4) 0.0178(5) Uani 1 1 d . . . . . H6 H 0.0352 0.6899 0.3781 0.021 Uiso 1 1 calc R U . . . C7 C 0.1319(2) 0.64880(13) 0.2618(4) 0.0169(5) Uani 1 1 d . . . . . H7 H 0.1600 0.6898 0.2449 0.020 Uiso 1 1 calc R U . . . C8 C 0.14349(18) 0.41073(12) 0.2660(4) 0.0114(5) Uani 1 1 d . . . . . C9 C 0.06103(19) 0.38252(13) 0.1636(4) 0.0152(5) Uani 1 1 d . . . . . H9 H 0.0273 0.4043 0.0586 0.018 Uiso 1 1 calc R U . . . C10 C 0.0276(2) 0.32295(14) 0.2133(4) 0.0188(6) Uani 1 1 d . . . . . H10 H -0.0291 0.3047 0.1434 0.023 Uiso 1 1 calc R U . . . C11 C 0.0772(2) 0.29019(14) 0.3649(4) 0.0212(6) Uani 1 1 d . . . . . H11 H 0.0554 0.2490 0.3977 0.025 Uiso 1 1 calc R U . . . C12 C 0.1588(2) 0.31811(14) 0.4682(4) 0.0206(6) Uani 1 1 d . . . . . H12 H 0.1926 0.2960 0.5727 0.025 Uiso 1 1 calc R U . . . C13 C 0.19143(19) 0.37813(14) 0.4202(4) 0.0155(5) Uani 1 1 d . . . . . H13 H 0.2468 0.3971 0.4931 0.019 Uiso 1 1 calc R U . . . C14 C 0.30624(18) 0.41720(13) 0.1320(4) 0.0119(5) Uani 1 1 d . . . . . C15 C 0.27234(19) 0.37400(14) -0.0107(4) 0.0178(5) Uani 1 1 d . . . . . H15 H 0.2187 0.3863 -0.1013 0.021 Uiso 1 1 calc R U . . . C16 C 0.3152(2) 0.31363(14) -0.0230(4) 0.0201(6) Uani 1 1 d . . . . . H16 H 0.2913 0.2856 -0.1222 0.024 Uiso 1 1 calc R U . . . C17 C 0.3925(2) 0.29413(14) 0.1087(4) 0.0206(6) Uani 1 1 d . . . . . H17 H 0.4217 0.2528 0.1009 0.025 Uiso 1 1 calc R U . . . C18 C 0.42655(19) 0.33572(14) 0.2520(4) 0.0188(6) Uani 1 1 d . . . . . H18 H 0.4790 0.3226 0.3440 0.023 Uiso 1 1 calc R U . . . C19 C 0.38425(19) 0.39689(14) 0.2619(4) 0.0157(5) Uani 1 1 d . . . . . H19 H 0.4094 0.4253 0.3597 0.019 Uiso 1 1 calc R U . . . C20 C 0.1948(2) 0.58729(16) -0.2594(4) 0.0262(7) Uani 1 1 d . . . . . H20 H 0.1339 0.6062 -0.2809 0.031 Uiso 1 1 calc R U . . . C21 C 0.2780(3) 0.62098(16) -0.2662(4) 0.0290(7) Uani 1 1 d . . . . . H21 H 0.2830 0.6664 -0.2930 0.035 Uiso 1 1 calc R U . . . C22 C 0.3517(2) 0.57529(17) -0.2263(4) 0.0269(7) Uani 1 1 d . . . . . H22 H 0.4154 0.5843 -0.2237 0.032 Uiso 1 1 calc R U . . . C23 C 0.3155(2) 0.51390(14) -0.1909(4) 0.0205(6) Uani 1 1 d . . . . . H23 H 0.3506 0.4746 -0.1564 0.025 Uiso 1 1 calc R U . . . C24 C 0.2176(2) 0.52123(16) -0.2158(4) 0.0213(6) Uani 1 1 d . . . . . H24 H 0.1747 0.4873 -0.2048 0.026 Uiso 1 1 calc R U . . . C25 C 0.4284(2) 0.66194(17) 0.2175(5) 0.0364(9) Uani 1 1 d . . . . . H25 H 0.4287 0.7069 0.1825 0.044 Uiso 1 1 calc R U . . . C26 C 0.3854(2) 0.63707(17) 0.3480(4) 0.0294(7) Uani 1 1 d . . . . . H26 H 0.3514 0.6619 0.4153 0.035 Uiso 1 1 calc R U . . . C27 C 0.4022(2) 0.56852(16) 0.3599(4) 0.0221(6) Uani 1 1 d . . . . . H27 H 0.3825 0.5389 0.4387 0.027 Uiso 1 1 calc R U . . . C28 C 0.45321(19) 0.55147(16) 0.2343(4) 0.0234(6) Uani 1 1 d . . . . . H28 H 0.4726 0.5082 0.2118 0.028 Uiso 1 1 calc R U . . . C29 C 0.4704(2) 0.60981(19) 0.1482(5) 0.0307(7) Uani 1 1 d . . . . . H29 H 0.5045 0.6130 0.0590 0.037 Uiso 1 1 calc R U . . . Cl1 Cl 0.23522(5) 0.71035(3) 0.00741(9) 0.02046(16) Uani 1 1 d . . . . . N1 N 0.16774(16) 0.59321(11) 0.2090(3) 0.0115(4) Uani 1 1 d . . . . . Zr1 Zr 0.29512(2) 0.58843(2) 0.05722(3) 0.00956(10) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0094(11) 0.0096(12) 0.0122(11) 0.0022(9) 0.0008(9) -0.0010(9) C2 0.0104(11) 0.0082(11) 0.0117(11) 0.0005(9) 0.0017(9) -0.0017(9) C3 0.0111(11) 0.0093(12) 0.0092(11) 0.0005(9) -0.0013(9) 0.0004(9) C4 0.0139(12) 0.0121(12) 0.0174(13) 0.0030(10) 0.0067(10) 0.0005(10) C5 0.0158(13) 0.0189(14) 0.0185(14) 0.0032(10) 0.0068(11) 0.0038(10) C6 0.0231(14) 0.0135(13) 0.0191(13) -0.0009(10) 0.0094(11) 0.0070(11) C7 0.0247(14) 0.0086(12) 0.0177(13) -0.0001(9) 0.0061(11) -0.0003(11) C8 0.0109(12) 0.0080(12) 0.0172(13) -0.0001(9) 0.0072(10) 0.0020(9) C9 0.0146(12) 0.0131(13) 0.0168(12) 0.0014(10) 0.0021(10) 0.0006(10) C10 0.0188(13) 0.0143(13) 0.0239(14) -0.0036(11) 0.0067(11) -0.0042(11) C11 0.0318(16) 0.0096(12) 0.0274(15) 0.0026(10) 0.0171(13) -0.0017(11) C12 0.0264(15) 0.0170(14) 0.0202(14) 0.0072(11) 0.0091(12) 0.0060(12) C13 0.0146(12) 0.0158(13) 0.0168(13) -0.0005(10) 0.0049(10) 0.0013(10) C14 0.0106(12) 0.0106(12) 0.0154(13) 0.0024(9) 0.0053(10) 0.0014(9) C15 0.0160(12) 0.0145(13) 0.0212(14) -0.0011(10) 0.0014(11) 0.0014(11) C16 0.0257(14) 0.0116(13) 0.0228(14) -0.0042(11) 0.0059(12) -0.0006(11) C17 0.0200(14) 0.0123(13) 0.0313(15) 0.0020(11) 0.0096(12) 0.0043(11) C18 0.0134(12) 0.0178(14) 0.0245(14) 0.0058(11) 0.0035(11) 0.0041(10) C19 0.0142(12) 0.0169(13) 0.0162(13) -0.0002(10) 0.0040(10) -0.0008(10) C20 0.0302(17) 0.0327(18) 0.0115(13) -0.0019(11) -0.0029(12) 0.0096(13) C21 0.054(2) 0.0220(16) 0.0138(13) 0.0034(11) 0.0144(14) 0.0055(15) C22 0.0346(18) 0.0283(17) 0.0251(16) -0.0006(12) 0.0214(14) -0.0038(14) C23 0.0287(15) 0.0161(13) 0.0193(13) -0.0006(11) 0.0110(12) 0.0026(12) C24 0.0228(14) 0.0274(16) 0.0122(12) -0.0069(11) 0.0010(11) -0.0027(12) C25 0.0252(16) 0.0253(16) 0.047(2) 0.0101(15) -0.0143(15) -0.0201(14) C26 0.0257(16) 0.0310(17) 0.0229(15) -0.0107(13) -0.0104(13) -0.0063(14) C27 0.0167(13) 0.0297(16) 0.0142(13) 0.0030(11) -0.0072(11) -0.0084(12) C28 0.0088(12) 0.0308(17) 0.0269(15) 0.0069(13) -0.0025(11) 0.0012(11) C29 0.0113(13) 0.046(2) 0.0313(17) 0.0110(15) -0.0012(12) -0.0107(14) Cl1 0.0310(4) 0.0112(3) 0.0214(3) 0.0031(2) 0.0109(3) 0.0011(3) N1 0.0124(10) 0.0117(11) 0.0114(10) 0.0000(8) 0.0045(9) 0.0000(8) Zr1 0.00883(14) 0.00966(14) 0.01016(14) 0.00059(7) 0.00230(9) -0.00194(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.350(4) . ? C1 C14 1.501(3) . ? C1 Zr1 2.403(2) . ? C2 C3 1.465(3) . ? C2 C8 1.495(3) . ? C3 N1 1.362(3) . ? C3 C4 1.403(3) . ? C4 C5 1.379(4) . ? C4 H4 0.9500 . ? C5 C6 1.374(4) . ? C5 H5 0.9500 . ? C6 C7 1.385(4) . ? C6 H6 0.9500 . ? C7 N1 1.348(3) . ? C7 H7 0.9500 . ? C8 C13 1.395(4) . ? C8 C9 1.396(4) . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(5) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.388(4) . ? C14 C15 1.401(4) . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.384(4) . ? C16 H16 0.9500 . ? C17 C18 1.385(4) . ? C17 H17 0.9500 . ? C18 C19 1.396(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C24 1.399(4) . ? C20 C21 1.412(5) . ? C20 Zr1 2.531(3) . ? C20 H20 0.9500 . ? C21 C22 1.400(5) . ? C21 Zr1 2.542(3) . ? C21 H21 0.9500 . ? C22 C23 1.405(4) . ? C22 Zr1 2.548(3) . ? C22 H22 0.9500 . ? C23 C24 1.413(4) . ? C23 Zr1 2.519(3) . ? C23 H23 0.9500 . ? C24 Zr1 2.536(3) . ? C24 H24 0.9500 . ? C25 C29 1.396(6) . ? C25 C26 1.411(5) . ? C25 Zr1 2.529(3) . ? C25 H25 0.9500 . ? C26 C27 1.408(5) . ? C26 Zr1 2.516(3) . ? C26 H26 0.9500 . ? C27 C28 1.410(4) . ? C27 Zr1 2.513(3) . ? C27 H27 0.9500 . ? C28 C29 1.410(5) . ? C28 Zr1 2.504(3) . ? C28 H28 0.9500 . ? C29 Zr1 2.535(3) . ? C29 H29 0.9500 . ? Cl1 Zr1 2.6163(7) . ? N1 Zr1 2.447(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C14 115.3(2) . . ? C2 C1 Zr1 118.09(18) . . ? C14 C1 Zr1 126.54(17) . . ? C1 C2 C3 118.8(2) . . ? C1 C2 C8 124.4(2) . . ? C3 C2 C8 116.8(2) . . ? N1 C3 C4 121.1(2) . . ? N1 C3 C2 116.4(2) . . ? C4 C3 C2 122.4(2) . . ? C5 C4 C3 120.0(2) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 118.7(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? N1 C7 C6 123.7(3) . . ? N1 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? C13 C8 C9 118.5(2) . . ? C13 C8 C2 120.6(2) . . ? C9 C8 C2 120.8(2) . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.5(3) . . ? C12 C13 H13 119.7 . . ? C8 C13 H13 119.7 . . ? C19 C14 C15 117.2(2) . . ? C19 C14 C1 121.7(2) . . ? C15 C14 C1 121.0(2) . . ? C16 C15 C14 121.6(3) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.1(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C17 C18 C19 120.3(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 121.5(3) . . ? C14 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C24 C20 C21 108.2(3) . . ? C24 C20 Zr1 74.17(17) . . ? C21 C20 Zr1 74.28(18) . . ? C24 C20 H20 125.9 . . ? C21 C20 H20 125.9 . . ? Zr1 C20 H20 117.6 . . ? C22 C21 C20 107.6(3) . . ? C22 C21 Zr1 74.24(17) . . ? C20 C21 Zr1 73.41(17) . . ? C22 C21 H21 126.2 . . ? C20 C21 H21 126.2 . . ? Zr1 C21 H21 118.2 . . ? C21 C22 C23 108.5(3) . . ? C21 C22 Zr1 73.84(17) . . ? C23 C22 Zr1 72.78(16) . . ? C21 C22 H22 125.7 . . ? C23 C22 H22 125.7 . . ? Zr1 C22 H22 119.5 . . ? C22 C23 C24 107.6(3) . . ? C22 C23 Zr1 75.03(17) . . ? C24 C23 Zr1 74.45(16) . . ? C22 C23 H23 126.2 . . ? C24 C23 H23 126.2 . . ? Zr1 C23 H23 116.5 . . ? C20 C24 C23 107.9(3) . . ? C20 C24 Zr1 73.78(17) . . ? C23 C24 Zr1 73.09(16) . . ? C20 C24 H24 126.0 . . ? C23 C24 H24 126.0 . . ? Zr1 C24 H24 119.0 . . ? C29 C25 C26 109.0(3) . . ? C29 C25 Zr1 74.28(18) . . ? C26 C25 Zr1 73.27(17) . . ? C29 C25 H25 125.5 . . ? C26 C25 H25 125.5 . . ? Zr1 C25 H25 118.8 . . ? C27 C26 C25 107.2(3) . . ? C27 C26 Zr1 73.63(16) . . ? C25 C26 Zr1 74.25(18) . . ? C27 C26 H26 126.4 . . ? C25 C26 H26 126.4 . . ? Zr1 C26 H26 117.8 . . ? C26 C27 C28 108.1(3) . . ? C26 C27 Zr1 73.85(16) . . ? C28 C27 Zr1 73.31(16) . . ? C26 C27 H27 126.0 . . ? C28 C27 H27 126.0 . . ? Zr1 C27 H27 118.8 . . ? C29 C28 C27 108.1(3) . . ? C29 C28 Zr1 74.99(17) . . ? C27 C28 Zr1 74.04(16) . . ? C29 C28 H28 126.0 . . ? C27 C28 H28 126.0 . . ? Zr1 C28 H28 117.0 . . ? C25 C29 C28 107.6(3) . . ? C25 C29 Zr1 73.73(18) . . ? C28 C29 Zr1 72.53(16) . . ? C25 C29 H29 126.2 . . ? C28 C29 H29 126.2 . . ? Zr1 C29 H29 119.4 . . ? C7 N1 C3 117.2(2) . . ? C7 N1 Zr1 125.55(18) . . ? C3 N1 Zr1 117.23(16) . . ? C1 Zr1 N1 68.23(8) . . ? C1 Zr1 C28 79.81(9) . . ? N1 Zr1 C28 117.74(9) . . ? C1 Zr1 C27 73.69(9) . . ? N1 Zr1 C27 86.28(9) . . ? C28 Zr1 C27 32.65(10) . . ? C1 Zr1 C26 101.66(10) . . ? N1 Zr1 C26 81.44(10) . . ? C28 Zr1 C26 54.06(11) . . ? C27 Zr1 C26 32.52(11) . . ? C1 Zr1 C23 76.30(9) . . ? N1 Zr1 C23 129.79(9) . . ? C28 Zr1 C23 88.28(11) . . ? C27 Zr1 C23 116.80(10) . . ? C26 Zr1 C23 141.42(11) . . ? C1 Zr1 C25 126.89(10) . . ? N1 Zr1 C25 109.44(11) . . ? C28 Zr1 C25 53.46(11) . . ? C27 Zr1 C25 53.50(11) . . ? C26 Zr1 C25 32.49(12) . . ? C23 Zr1 C25 120.22(12) . . ? C1 Zr1 C20 98.83(10) . . ? N1 Zr1 C20 97.73(10) . . ? C28 Zr1 C20 140.20(11) . . ? C27 Zr1 C20 169.63(11) . . ? C26 Zr1 C20 157.48(11) . . ? C23 Zr1 C20 53.53(10) . . ? C25 Zr1 C20 132.59(11) . . ? C1 Zr1 C29 111.81(10) . . ? N1 Zr1 C29 134.89(10) . . ? C28 Zr1 C29 32.48(11) . . ? C27 Zr1 C29 53.75(10) . . ? C26 Zr1 C29 53.78(12) . . ? C23 Zr1 C29 90.56(12) . . ? C25 Zr1 C29 31.99(13) . . ? C20 Zr1 C29 125.43(12) . . ? C1 Zr1 C24 70.66(9) . . ? N1 Zr1 C24 100.50(9) . . ? C28 Zr1 C24 117.53(11) . . ? C27 Zr1 C24 137.84(10) . . ? C26 Zr1 C24 170.32(11) . . ? C23 Zr1 C24 32.46(10) . . ? C25 Zr1 C24 149.25(12) . . ? C20 Zr1 C24 32.05(10) . . ? C29 Zr1 C24 122.69(11) . . ? C1 Zr1 C21 123.52(10) . . ? N1 Zr1 C21 124.20(10) . . ? C28 Zr1 C21 118.05(11) . . ? C27 Zr1 C21 147.99(11) . . ? C26 Zr1 C21 133.09(12) . . ? C23 Zr1 C21 53.45(10) . . ? C25 Zr1 C21 102.00(12) . . ? C20 Zr1 C21 32.32(12) . . ? C29 Zr1 C21 94.37(12) . . ? C24 Zr1 C21 53.29(11) . . ? C1 Zr1 C22 108.11(10) . . ? N1 Zr1 C22 150.47(10) . . ? C28 Zr1 C22 89.14(11) . . ? C27 Zr1 C22 121.69(11) . . ? C26 Zr1 C22 126.92(12) . . ? C23 Zr1 C22 32.19(10) . . ? C25 Zr1 C22 96.12(13) . . ? C20 Zr1 C22 53.08(11) . . ? C29 Zr1 C22 74.43(12) . . ? C24 Zr1 C22 53.14(10) . . ? C21 Zr1 C22 31.92(11) . . ? _refine_diff_density_max 0.667 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.105 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mm1511 in P2(1)/c CELL 1.54178 14.7014 20.2371 7.7474 90.000 104.290 90.000 ZERR 4.00 0.0007 0.0015 0.0004 0.000 0.004 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N Cl Zr UNIT 116 96 4 4 4 L.S. 4 ACTA BOND $H FMAP 2 PLAN -3 SIZE 0.060 0.080 0.100 TEMP -99.960 WGHT 0.072300 FVAR 0.13489 C1 1 0.256379 0.480711 0.148567 11.00000 0.00942 0.00960 = 0.01217 0.00225 0.00082 -0.00101 C2 1 0.179286 0.474740 0.212505 11.00000 0.01041 0.00822 = 0.01169 0.00046 0.00174 -0.00174 C3 1 0.129662 0.534709 0.242813 11.00000 0.01105 0.00933 = 0.00920 0.00046 -0.00126 0.00042 C4 1 0.050011 0.532948 0.311897 11.00000 0.01386 0.01212 = 0.01741 0.00296 0.00670 0.00046 AFIX 43 H4 2 0.021466 0.491846 0.325985 11.00000 -1.20000 AFIX 0 C5 1 0.013155 0.590890 0.359354 11.00000 0.01578 0.01887 = 0.01850 0.00318 0.00681 0.00384 AFIX 43 H5 2 -0.041184 0.590271 0.404960 11.00000 -1.20000 AFIX 0 C6 1 0.056552 0.649528 0.339394 11.00000 0.02311 0.01349 = 0.01909 -0.00093 0.00938 0.00697 AFIX 43 H6 2 0.035211 0.689897 0.378150 11.00000 -1.20000 AFIX 0 C7 1 0.131940 0.648795 0.261817 11.00000 0.02472 0.00863 = 0.01772 -0.00013 0.00607 -0.00028 AFIX 43 H7 2 0.159994 0.689795 0.244875 11.00000 -1.20000 AFIX 0 C8 1 0.143486 0.410731 0.265969 11.00000 0.01094 0.00796 = 0.01723 -0.00006 0.00721 0.00197 C9 1 0.061032 0.382523 0.163595 11.00000 0.01458 0.01314 = 0.01682 0.00141 0.00209 0.00062 AFIX 43 H9 2 0.027284 0.404296 0.058624 11.00000 -1.20000 AFIX 0 C10 1 0.027641 0.322948 0.213286 11.00000 0.01883 0.01426 = 0.02393 -0.00360 0.00671 -0.00418 AFIX 43 H10 2 -0.029097 0.304676 0.143435 11.00000 -1.20000 AFIX 0 C11 1 0.077210 0.290187 0.364931 11.00000 0.03175 0.00956 = 0.02742 0.00257 0.01714 -0.00166 AFIX 43 H11 2 0.055435 0.248972 0.397653 11.00000 -1.20000 AFIX 0 C12 1 0.158762 0.318110 0.468248 11.00000 0.02640 0.01697 = 0.02018 0.00722 0.00909 0.00602 AFIX 43 H12 2 0.192572 0.296039 0.572666 11.00000 -1.20000 AFIX 0 C13 1 0.191429 0.378132 0.420248 11.00000 0.01455 0.01581 = 0.01677 -0.00053 0.00493 0.00127 AFIX 43 H13 2 0.246843 0.397090 0.493111 11.00000 -1.20000 AFIX 0 C14 1 0.306240 0.417198 0.132039 11.00000 0.01064 0.01065 = 0.01539 0.00237 0.00532 0.00137 C15 1 0.272343 0.374002 -0.010698 11.00000 0.01604 0.01449 = 0.02116 -0.00106 0.00138 0.00140 AFIX 43 H15 2 0.218748 0.386323 -0.101279 11.00000 -1.20000 AFIX 0 C16 1 0.315174 0.313629 -0.022978 11.00000 0.02572 0.01158 = 0.02281 -0.00425 0.00589 -0.00064 AFIX 43 H16 2 0.291326 0.285591 -0.122177 11.00000 -1.20000 AFIX 0 C17 1 0.392458 0.294131 0.108689 11.00000 0.02002 0.01228 = 0.03133 0.00205 0.00961 0.00432 AFIX 43 H17 2 0.421729 0.252765 0.100877 11.00000 -1.20000 AFIX 0 C18 1 0.426551 0.335721 0.251962 11.00000 0.01337 0.01778 = 0.02455 0.00584 0.00347 0.00412 AFIX 43 H18 2 0.479001 0.322561 0.343996 11.00000 -1.20000 AFIX 0 C19 1 0.384250 0.396886 0.261865 11.00000 0.01415 0.01689 = 0.01621 -0.00024 0.00397 -0.00083 AFIX 43 H19 2 0.409425 0.425256 0.359686 11.00000 -1.20000 AFIX 0 C20 1 0.194837 0.587288 -0.259448 11.00000 0.03025 0.03270 = 0.01151 -0.00192 -0.00294 0.00959 AFIX 43 H20 2 0.133939 0.606218 -0.280854 11.00000 -1.20000 AFIX 0 C21 1 0.277999 0.620975 -0.266199 11.00000 0.05436 0.02205 = 0.01379 0.00340 0.01440 0.00550 AFIX 43 H21 2 0.283021 0.666439 -0.292965 11.00000 -1.20000 AFIX 0 C22 1 0.351695 0.575287 -0.226336 11.00000 0.03462 0.02826 = 0.02512 -0.00062 0.02143 -0.00384 AFIX 43 H22 2 0.415447 0.584280 -0.223695 11.00000 -1.20000 AFIX 0 C23 1 0.315547 0.513895 -0.190888 11.00000 0.02871 0.01611 = 0.01933 -0.00060 0.01101 0.00258 AFIX 43 H23 2 0.350618 0.474571 -0.156410 11.00000 -1.20000 AFIX 0 C24 1 0.217572 0.521227 -0.215801 11.00000 0.02276 0.02738 = 0.01215 -0.00691 0.00097 -0.00269 AFIX 43 H24 2 0.174703 0.487289 -0.204848 11.00000 -1.20000 AFIX 0 C25 1 0.428397 0.661939 0.217532 11.00000 0.02522 0.02530 = 0.04662 0.01009 -0.01431 -0.02007 AFIX 43 H25 2 0.428705 0.706914 0.182544 11.00000 -1.20000 AFIX 0 C26 1 0.385381 0.637071 0.348032 11.00000 0.02575 0.03096 = 0.02290 -0.01074 -0.01039 -0.00634 AFIX 43 H26 2 0.351435 0.661936 0.415323 11.00000 -1.20000 AFIX 0 C27 1 0.402162 0.568523 0.359900 11.00000 0.01666 0.02967 = 0.01423 0.00303 -0.00721 -0.00841 AFIX 43 H27 2 0.382521 0.538919 0.438745 11.00000 -1.20000 AFIX 0 C28 1 0.453209 0.551471 0.234347 11.00000 0.00877 0.03082 = 0.02689 0.00691 -0.00253 0.00121 AFIX 43 H28 2 0.472610 0.508222 0.211796 11.00000 -1.20000 AFIX 0 C29 1 0.470416 0.609805 0.148156 11.00000 0.01134 0.04604 = 0.03133 0.01102 -0.00118 -0.01066 AFIX 43 H29 2 0.504452 0.613044 0.058991 11.00000 -1.20000 AFIX 0 CL1 4 0.235218 0.710355 0.007410 11.00000 0.03102 0.01125 = 0.02145 0.00313 0.01093 0.00113 N1 3 0.167736 0.593206 0.209018 11.00000 0.01235 0.01175 = 0.01138 0.00001 0.00452 0.00003 ZR1 5 0.295121 0.588425 0.057220 11.00000 0.00883 0.00966 = 0.01016 0.00059 0.00230 -0.00194 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mm1511 in P2(1)/c REM R1 = 0.0370 for 3806 Fo > 4sig(Fo) and 0.0422 for all 4307 data REM 289 parameters refined using 0 restraints END WGHT 0.0725 0.0000 REM Highest difference peak 0.667, deepest hole -0.631, 1-sigma level 0.105 Q1 1 0.2749 0.6505 0.0326 11.00000 0.05 0.67 Q2 1 0.2959 0.6102 -0.1008 11.00000 0.05 0.61 Q3 1 0.2119 0.5723 0.0597 11.00000 0.05 0.54 ; _shelx_res_checksum 5994 _shelx_hkl_file ; 0 0 1 -0.18 0.18 0 0 -1 -0.36 0.27 0 0 1 -0.30 0.19 0 0 2 181.64 5.82 0 0 -2 185.29 6.79 0 0 2 192.42 5.84 0 0 3 0.51 0.39 0 0 3 0.01 0.38 0 0 -3 0.30 0.64 0 0 -4 178.52 7.83 0 0 4 179.92 6.46 0 0 -4 183.52 7.13 0 0 5 -0.28 0.63 0 0 6 18.58 1.44 0 0 6 19.42 1.50 0 0 7 -0.59 0.50 0 0 7 -0.55 0.61 0 0 8 1.98 0.62 0 0 -8 2.19 0.87 0 0 9 -0.28 0.35 0 1 0 -0.20 0.11 0 1 0 -0.25 0.11 0 -1 0 0.10 0.11 0 1 1 432.74 12.55 0 1 -1 436.75 14.10 0 1 1 444.52 12.38 0 -1 1 441.81 12.41 0 -1 -1 430.67 13.81 0 -1 1 437.64 12.37 0 1 2 11.56 0.93 0 1 -2 14.32 1.39 0 1 2 13.94 0.96 0 -1 2 13.12 0.97 0 -1 -2 12.41 1.15 0 -1 2 12.50 0.82 0 1 3 15.54 1.25 0 1 -3 13.28 1.67 0 1 3 16.65 1.26 0 -1 3 16.15 1.14 0 -1 -3 14.47 1.55 0 -1 3 15.66 1.22 0 1 4 129.43 4.99 0 1 -4 125.25 6.26 0 1 -4 126.17 5.38 0 -1 -4 126.08 5.66 0 -1 4 130.63 5.00 0 -1 -4 123.47 5.92 0 1 5 12.51 1.61 0 1 -5 13.75 2.55 0 -1 5 14.53 1.70 0 1 6 94.78 3.58 0 1 6 101.72 3.85 0 -1 6 94.17 3.60 0 1 7 67.94 2.96 0 1 7 61.02 2.74 0 -1 7 59.48 2.70 0 1 -8 0.86 0.74 0 1 8 2.29 0.60 0 -1 8 3.08 0.71 0 -1 -8 1.26 0.85 0 1 9 18.72 1.11 0 -1 9 18.79 1.10 0 2 0 267.77 8.67 0 2 0 274.74 7.83 0 -2 0 266.40 7.84 0 2 -1 2.70 0.67 0 2 1 1.27 0.34 0 2 1 1.73 0.36 0 -2 1 1.61 0.21 0 -2 1 1.28 0.35 0 -2 -1 1.63 0.30 0 2 2 317.09 9.65 0 2 2 324.52 9.49 0 2 -2 318.43 11.14 0 -2 2 312.26 9.49 0 -2 -2 311.19 10.52 0 -2 2 316.70 9.26 0 2 3 316.49 9.92 0 2 -3 319.75 11.83 0 -2 3 325.96 9.97 0 -2 -3 321.38 11.21 0 -2 3 311.45 9.67 0 2 -4 -0.36 0.89 0 2 4 0.36 0.49 0 -2 4 -0.23 0.51 0 -2 -4 -0.39 0.78 0 2 -5 29.69 3.37 0 2 5 32.65 2.44 0 -2 -5 33.69 3.07 0 -2 5 26.84 2.25 0 2 6 35.25 2.00 0 2 6 43.29 2.24 0 -2 6 40.69 2.06 0 -2 6 39.43 2.14 0 2 7 90.10 3.62 0 2 7 82.54 3.34 0 -2 7 83.44 3.38 0 2 8 34.13 1.79 0 -2 -8 33.83 2.26 0 -2 8 31.17 1.77 0 2 9 0.20 0.41 0 -2 -9 0.35 0.57 0 -2 9 0.15 0.38 0 3 0 -0.07 0.31 0 3 0 -0.01 0.34 0 -3 0 -0.31 0.27 0 3 -1 20.29 1.55 0 3 1 22.49 1.20 0 -3 1 19.72 0.77 0 -3 -1 20.33 0.99 0 -3 1 22.23 1.26 0 3 2 16.57 1.14 0 3 -2 16.49 1.68 0 3 2 16.57 1.17 0 -3 2 17.24 1.18 0 -3 -2 16.31 1.11 0 -3 2 15.28 0.80 0 3 -3 128.17 5.78 0 3 3 122.57 4.51 0 -3 3 118.95 4.07 0 -3 -3 125.43 5.21 0 -3 3 119.47 4.52 0 -3 -3 119.38 4.90 0 3 -4 234.05 10.04 0 3 4 239.72 8.11 0 -3 4 225.12 8.04 0 -3 -4 237.73 9.08 0 3 5 1.96 0.91 0 3 -5 1.03 1.53 0 -3 -5 1.10 1.25 0 -3 5 3.91 1.06 0 3 6 157.43 5.43 0 3 6 156.58 5.16 0 -3 6 153.37 5.17 0 3 7 7.63 1.14 0 3 7 7.60 1.04 0 -3 7 8.38 1.13 0 3 8 7.80 0.99 0 -3 8 8.02 1.00 0 -3 -8 6.21 1.22 0 3 9 0.08 0.38 0 -3 9 -0.04 0.33 0 -3 -9 1.22 0.61 0 4 0 724.99 23.28 0 4 0 750.33 21.01 0 -4 0 731.89 21.08 0 4 -1 20.46 1.69 0 4 1 19.23 1.27 0 -4 1 20.22 1.31 0 -4 1 18.31 0.81 0 -4 -1 20.88 1.52 0 4 2 0.84 0.51 0 4 -2 1.18 0.75 0 -4 -2 -0.26 0.29 0 -4 2 0.09 0.20 0 -4 2 0.66 0.46 0 4 -3 205.34 8.60 0 4 3 205.98 6.96 0 -4 3 203.99 6.96 0 -4 -3 206.55 7.77 0 4 4 3.44 0.94 0 4 -4 1.59 1.31 0 -4 4 2.84 0.84 0 -4 -4 3.53 1.27 0 4 5 32.84 2.64 0 4 -5 39.82 3.95 0 -4 -5 32.90 3.34 0 -4 5 39.49 2.71 0 4 6 45.23 2.40 0 4 6 46.56 2.22 0 4 -6 43.70 2.79 0 -4 6 44.90 2.23 0 4 7 15.74 1.53 0 4 7 16.53 1.38 0 -4 7 16.20 1.44 0 4 8 13.25 1.14 0 -4 -8 11.39 1.63 0 -4 8 12.60 1.20 0 4 9 2.18 0.51 0 -4 -9 2.32 0.67 0 -4 9 1.15 0.42 0 5 0 -0.48 0.56 0 5 0 -0.36 0.55 0 -5 0 -0.89 0.46 0 5 1 44.38 1.86 0 5 -1 43.42 2.62 0 5 1 43.97 2.12 0 -5 1 44.15 1.62 0 -5 -1 41.11 2.30 0 5 -2 0.56 0.82 0 5 2 1.44 0.67 0 -5 -2 -0.20 0.62 0 -5 2 0.09 0.18 0 -5 -2 0.20 0.28 0 -5 2 0.06 0.48 0 5 3 28.51 2.03 0 5 -3 26.13 2.63 0 -5 3 25.73 1.86 0 -5 -3 26.61 2.34 0 5 -4 17.14 2.50 0 5 4 16.37 1.73 0 -5 4 16.77 1.64 0 -5 -4 20.98 2.30 0 5 -5 45.68 4.45 0 5 5 46.41 3.22 0 -5 -5 49.90 3.97 0 -5 5 43.65 3.01 0 5 6 3.22 0.73 0 5 -6 4.42 1.16 0 5 6 6.96 1.11 0 5 6 6.08 0.95 0 -5 6 4.93 0.89 0 5 7 51.20 2.45 0 5 7 57.33 2.75 0 -5 7 52.06 2.56 0 5 8 1.91 0.62 0 -5 8 2.37 0.65 0 -5 -8 -0.06 0.77 0 5 9 95.09 3.06 0 -5 -9 94.25 3.35 0 -5 9 98.35 3.08 0 6 0 250.94 8.62 0 6 0 239.30 7.89 0 -6 0 239.65 7.73 0 6 1 7.46 0.85 0 6 1 6.80 1.06 0 6 -1 7.83 1.32 0 -6 -1 7.97 1.17 0 -6 1 8.10 0.74 0 6 2 151.36 5.42 0 6 -2 151.99 6.57 0 -6 2 137.15 5.38 0 -6 -2 148.64 5.87 0 6 3 35.58 2.39 0 6 -3 33.78 3.05 0 -6 3 37.07 2.30 0 -6 -3 34.73 2.76 0 6 4 2.43 1.13 0 6 -4 0.77 1.28 0 -6 -4 0.86 0.98 0 -6 4 1.16 0.85 0 6 -5 5.72 2.21 0 6 5 9.07 1.91 0 -6 -5 8.21 2.03 0 -6 5 10.19 1.77 0 6 6 60.06 2.64 0 6 6 60.68 2.89 0 6 -6 55.63 3.26 0 6 6 62.42 2.69 0 -6 6 65.34 2.82 0 6 -7 2.77 1.02 0 6 7 3.52 0.81 0 6 7 3.79 0.94 0 -6 7 2.55 0.75 0 6 8 31.07 1.66 0 -6 8 26.40 1.60 0 -6 -8 26.74 2.08 0 7 0 -0.06 0.58 0 7 0 -0.18 0.48 0 -7 0 0.09 0.47 0 7 -1 302.31 10.93 0 7 1 307.12 9.59 0 7 1 297.75 9.98 0 -7 1 284.14 8.90 0 -7 -1 295.47 9.83 0 7 -2 148.94 6.69 0 7 2 148.26 5.51 0 -7 -2 141.24 5.92 0 -7 2 143.90 5.62 0 7 -3 118.64 6.15 0 7 3 112.21 4.90 0 -7 -3 112.78 5.45 0 -7 3 113.26 4.90 0 7 -4 15.92 2.69 0 7 4 8.71 1.55 0 -7 -4 11.92 2.05 0 -7 4 11.12 1.53 0 7 -5 -0.87 1.38 0 7 5 -0.88 1.18 0 -7 -5 -1.70 1.14 0 -7 5 0.42 0.96 0 7 6 82.17 3.33 0 7 6 91.09 3.69 0 7 -6 89.77 4.18 0 7 6 86.14 3.41 0 -7 6 88.99 3.54 0 7 7 14.72 1.39 0 7 -7 14.73 1.81 0 7 7 15.77 1.33 0 7 7 20.03 1.61 0 -7 7 18.27 1.50 0 7 8 5.58 0.84 0 -7 8 6.25 0.89 0 -7 -8 5.11 1.09 0 8 0 49.96 2.73 0 8 0 50.73 2.77 0 -8 0 43.33 2.33 0 8 1 5.18 0.89 0 8 1 1.75 0.82 0 8 -1 3.06 1.03 0 -8 -1 4.13 1.07 0 -8 1 3.00 0.64 0 8 -2 38.86 3.06 0 8 2 37.47 2.45 0 -8 -2 33.41 2.63 0 -8 2 34.49 2.46 0 8 3 242.84 8.65 0 8 -3 233.58 10.33 0 -8 3 240.03 8.81 0 -8 -3 242.80 9.39 0 8 -4 15.09 2.76 0 8 4 13.01 1.94 0 -8 4 15.14 1.82 0 -8 -4 13.05 2.38 0 8 -5 82.76 3.81 0 8 5 81.36 3.10 0 8 -5 67.62 5.56 0 8 5 86.79 3.32 0 8 5 66.65 4.45 0 8 5 88.86 3.16 0 -8 5 68.24 4.35 0 -8 -5 60.24 4.87 0 8 6 3.50 0.88 0 8 6 4.52 0.85 0 8 -6 4.15 1.17 0 8 6 3.25 0.84 0 -8 6 3.00 0.80 0 8 -7 90.80 4.00 0 8 7 82.18 3.50 0 8 7 82.07 3.18 0 8 7 86.01 3.34 0 -8 7 82.34 3.42 0 8 8 0.62 0.51 0 -8 -8 -0.13 0.60 0 -8 8 0.44 0.49 0 9 0 0.11 0.70 0 9 0 0.80 0.74 0 -9 0 0.50 0.58 0 9 -1 159.27 6.89 0 9 1 163.98 6.19 0 -9 -1 150.74 6.15 0 9 -2 145.63 7.01 0 9 2 153.01 5.92 0 -9 -2 154.38 6.39 0 -9 2 134.22 5.96 0 9 3 11.80 1.77 0 9 -3 10.54 2.14 0 -9 3 7.00 1.48 0 -9 -3 7.01 1.63 0 9 4 47.15 3.26 0 9 -4 37.09 3.83 0 -9 4 46.60 3.26 0 -9 -4 38.93 3.44 0 9 5 7.00 1.02 0 9 -5 7.38 1.32 0 9 5 5.45 0.90 0 9 5 8.27 1.15 0 9 6 168.91 5.56 0 9 6 165.38 5.60 0 9 -6 174.30 6.54 0 9 6 172.04 5.88 0 -9 6 171.09 5.83 0 9 7 6.87 0.96 0 9 7 7.94 1.09 0 9 -7 7.79 1.28 0 9 7 9.18 1.16 0 -9 7 7.46 1.12 0 9 8 6.87 0.92 0 9 -8 7.50 1.11 0 -9 -8 6.34 1.06 0 -9 8 8.05 0.92 0 10 0 570.22 19.33 0 10 0 580.84 17.91 0 -10 0 564.34 17.36 0 10 1 16.96 1.86 0 10 -1 15.62 2.04 0 -10 -1 17.09 1.82 0 10 -2 143.37 7.22 0 10 2 161.12 6.34 0 -10 -2 153.41 6.64 0 -10 2 149.38 6.43 0 10 3 93.51 4.59 0 10 -3 83.77 5.42 0 -10 3 81.13 4.61 0 -10 -3 87.75 5.00 0 10 4 7.07 1.63 0 10 -4 5.99 1.85 0 -10 -4 7.75 1.96 0 -10 4 6.14 1.56 0 10 -5 19.07 2.04 0 10 -5 13.07 1.77 0 10 5 16.09 1.47 0 10 5 18.50 1.44 0 10 5 16.91 1.44 0 10 6 2.90 0.78 0 10 -6 2.66 1.05 0 10 6 1.78 0.79 0 10 6 1.75 0.75 0 -10 6 2.27 0.82 0 10 7 13.34 1.19 0 10 7 12.51 1.33 0 10 7 12.63 1.29 0 10 -7 14.73 1.61 0 -10 7 15.12 1.32 0 10 -8 9.08 1.12 0 10 8 9.12 0.99 0 -10 -8 10.68 1.17 0 -10 8 10.09 0.95 0 11 0 0.54 0.79 0 -11 0 -0.58 0.55 0 11 -1 155.89 7.14 0 11 1 171.24 6.64 0 -11 -1 150.53 6.33 0 -11 1 149.67 6.47 0 11 -2 -0.34 0.86 0 11 2 0.53 0.85 0 -11 -2 0.14 0.78 0 -11 2 -0.37 0.76 0 11 -3 0.61 1.11 0 11 3 0.45 0.95 0 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3.08 0.82 0 12 -7 3.31 0.88 0 12 7 2.85 0.69 0 -12 7 2.44 0.66 0 12 8 58.35 2.13 0 -12 8 61.23 2.11 0 -12 -8 55.41 2.28 0 13 0 -0.20 0.81 0 13 1 22.69 2.35 0 -13 -1 21.42 2.24 0 -13 1 18.03 2.13 0 13 -2 21.38 2.85 0 13 2 25.77 2.58 0 -13 2 16.88 2.29 0 -13 -2 20.77 2.50 0 13 3 10.12 2.01 0 13 -3 18.93 3.08 0 -13 3 13.30 2.19 0 -13 -3 15.23 2.49 0 13 4 90.74 3.74 0 13 -4 87.32 4.12 0 13 -4 89.95 4.12 0 13 5 6.76 1.17 0 13 -5 9.61 1.58 0 13 5 6.64 1.02 0 13 -5 5.39 1.19 0 13 6 29.05 2.00 0 13 6 33.47 1.89 0 13 6 27.31 1.73 0 13 -6 30.48 2.22 0 -13 6 28.25 1.86 0 13 7 39.63 1.98 0 13 7 37.96 1.77 0 13 -7 38.21 2.18 0 -13 7 40.94 1.91 0 -13 -7 36.74 2.06 0 14 0 3.69 1.38 0 14 1 2.25 1.15 0 -14 1 2.15 1.24 0 14 2 33.99 3.14 0 14 -2 25.41 3.30 0 -14 -2 31.37 3.08 0 -14 2 32.95 3.07 0 14 3 181.70 5.79 0 14 -3 185.19 6.62 0 14 -3 179.17 6.42 0 14 -3 184.60 6.66 0 14 3 172.49 6.01 0 14 4 1.88 0.88 0 14 -4 2.75 1.24 0 14 4 3.09 0.81 0 14 -4 1.50 0.95 0 14 -4 3.25 1.06 0 14 -5 55.79 3.19 0 14 -5 58.01 3.35 0 14 5 59.39 2.68 0 14 5 62.92 2.98 0 14 6 12.33 1.22 0 14 6 13.56 1.43 0 14 -6 10.47 1.44 0 -14 6 12.73 1.25 0 14 -7 23.78 1.64 0 14 7 25.60 1.46 0 14 7 22.39 1.29 0 -14 7 27.40 1.42 0 -14 -7 24.88 1.50 0 15 1 5.95 1.61 0 -15 1 7.95 1.80 0 15 -2 5.31 1.24 0 15 2 5.77 0.94 0 15 -2 5.36 1.08 0 15 2 4.50 0.96 0 15 3 7.65 1.20 0 15 -3 8.14 1.46 0 15 3 8.31 1.14 0 15 -3 8.28 1.43 0 15 -3 7.76 1.35 0 15 -4 100.38 4.44 0 15 -4 99.55 4.45 0 15 4 103.03 3.82 0 15 -4 100.30 4.63 0 15 4 95.00 3.99 0 15 5 8.73 1.17 0 15 5 7.14 1.17 0 15 -5 11.93 1.57 0 15 -5 12.98 1.80 0 15 6 39.11 2.08 0 15 6 40.15 1.94 0 15 -6 33.66 2.21 0 -15 6 37.20 1.94 0 15 -7 23.25 1.50 0 15 7 21.26 1.19 0 15 7 24.59 1.33 0 -15 7 22.58 1.21 0 16 0 295.58 9.26 0 16 0 280.27 8.78 0 16 1 0.11 0.63 0 16 1 1.11 0.82 0 16 1 0.56 0.70 0 16 -1 0.46 0.70 0 16 -1 -0.48 0.83 0 16 -2 4.01 1.16 0 16 2 4.95 1.06 0 16 2 2.87 0.81 0 16 -2 2.63 0.86 0 16 3 24.10 1.90 0 16 -3 26.58 2.18 0 16 -3 29.23 2.39 0 16 3 27.61 1.81 0 16 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3.55 0.94 0 18 -3 3.78 1.18 0 18 3 4.64 0.93 0 18 -3 2.99 1.05 0 18 -4 0.21 0.69 0 18 -4 -0.97 0.86 0 18 4 0.84 0.60 0 18 -4 -0.46 0.72 0 18 4 0.14 0.64 0 18 -5 29.76 1.96 0 18 5 29.93 1.75 0 18 5 30.57 1.65 0 18 -6 10.35 1.02 0 18 6 10.59 0.91 0 18 6 10.09 0.90 0 -18 6 11.81 0.83 0 19 0 -0.27 0.63 0 19 0 -0.11 0.83 0 19 1 1.78 0.93 0 19 -1 1.92 0.99 0 19 -1 0.98 0.77 0 19 1 1.45 0.79 0 19 2 23.78 1.89 0 19 -2 29.26 2.37 0 19 2 26.89 1.75 0 19 -2 29.70 2.10 0 19 3 2.44 0.80 0 19 -3 4.40 1.02 0 19 -3 3.25 1.14 0 19 3 2.44 0.74 0 19 4 27.04 1.60 0 19 -4 24.55 1.93 0 19 -4 26.69 1.82 0 19 4 25.79 1.69 0 19 -4 27.70 2.13 0 19 5 2.65 0.65 0 19 -5 2.00 0.67 0 19 5 3.32 0.70 0 -19 5 2.40 0.51 0 19 6 42.14 1.62 0 -19 6 41.87 1.55 0 20 0 0.44 0.87 0 20 0 0.18 0.65 0 20 1 45.88 2.46 0 20 -1 47.09 2.58 0 20 1 47.98 2.78 0 20 -1 47.84 2.91 0 20 2 1.77 0.72 0 20 2 2.99 0.81 0 20 -2 2.35 0.85 0 20 -2 1.65 1.01 0 20 3 50.81 2.46 0 20 3 49.23 2.27 0 20 -3 48.37 2.85 0 20 -3 49.74 2.62 0 20 -4 0.64 0.81 0 20 4 0.31 0.51 0 20 4 0.63 0.55 0 20 -4 -0.25 0.59 0 20 5 29.17 1.43 0 20 5 30.08 1.50 0 20 -5 28.89 1.55 0 -20 5 31.23 1.37 0 21 0 0.09 0.81 0 21 0 -0.20 0.61 0 21 -1 2.32 0.85 0 21 -1 2.36 0.99 0 21 1 1.44 0.87 0 21 1 1.86 0.71 0 21 2 19.37 1.52 0 21 -2 19.07 1.66 0 21 2 21.46 1.57 0 21 -2 19.21 1.91 0 21 -3 5.78 0.99 0 21 3 6.14 0.86 0 21 3 4.91 0.84 0 21 -3 5.54 1.13 0 21 4 46.78 1.91 0 21 4 45.88 2.03 0 21 -4 46.63 2.36 0 21 -4 47.73 2.27 0 -21 5 18.56 0.91 0 22 0 22.95 1.93 0 22 0 21.63 1.61 0 22 -1 1.65 0.71 0 22 1 1.62 0.84 0 22 -1 2.65 0.92 0 22 1 1.58 0.64 0 22 -2 24.65 1.75 0 22 -2 27.25 2.04 0 22 2 29.12 1.68 0 22 -3 6.10 0.91 0 22 3 5.60 0.78 0 22 -3 6.85 1.13 0 22 3 7.51 0.91 0 22 4 1.11 0.47 0 22 4 1.08 0.41 0 23 0 0.12 0.54 0 23 0 0.31 0.66 0 23 -1 71.42 3.21 0 23 -1 69.07 2.86 0 23 1 69.54 3.03 0 23 1 69.27 2.78 0 23 2 1.91 0.58 0 23 -2 0.85 0.73 0 23 -2 0.48 0.55 0 23 3 30.99 1.47 0 23 -3 30.13 1.60 0 23 -3 29.61 1.73 0 24 0 82.65 3.20 0 24 0 76.67 2.91 0 24 1 1.06 0.70 0 24 1 2.23 0.57 0 24 -1 2.70 0.80 0 24 -1 1.99 0.59 0 24 -2 40.40 2.01 0 24 -2 41.10 1.82 0 24 2 40.90 1.72 0 25 0 0.42 0.44 -1 0 9 0.38 0.37 1 0 -8 6.35 1.17 -1 0 8 9.05 1.04 -1 0 7 -0.24 0.50 -1 0 7 0.69 0.64 -1 0 6 141.77 4.93 -1 0 6 141.23 4.77 -1 0 5 0.11 0.68 1 0 -5 -1.44 0.88 -1 0 4 139.56 5.22 1 0 -4 141.50 6.53 -1 0 4 131.11 5.04 1 0 -3 -0.06 0.57 -1 0 3 0.20 0.37 -1 0 3 0.18 0.35 1 0 -2 13.66 1.28 -1 0 2 14.67 0.90 -1 0 2 15.10 0.99 1 0 -1 -1.11 0.29 -1 0 1 -0.80 0.23 -1 0 1 -0.91 0.16 1 0 0 2.44 0.23 -1 0 0 3.06 0.35 -1 0 0 2.65 0.28 1 0 1 -0.29 0.25 -1 0 -1 -0.57 0.27 -1 0 -1 -0.04 0.35 -1 0 -2 194.61 7.13 1 0 2 204.84 6.27 -1 0 -2 189.85 6.45 -1 0 -3 0.35 0.59 1 0 3 -0.21 0.38 -1 0 -3 0.95 0.72 -1 0 -4 129.22 5.53 1 0 4 125.58 5.09 -1 0 -4 128.82 6.10 1 0 5 -0.39 0.68 1 0 6 24.46 1.65 1 0 6 25.56 1.74 1 0 7 0.50 0.57 -1 0 -7 0.77 0.92 -1 0 -8 1.03 0.74 1 0 8 0.71 0.54 1 0 9 0.00 0.36 -1 1 9 9.09 0.84 -1 -1 9 8.29 0.80 1 -1 -9 9.41 1.05 -1 1 8 4.13 0.75 -1 -1 8 5.27 0.83 -1 1 7 34.32 1.94 -1 -1 7 34.25 1.93 -1 -1 7 36.99 2.10 -1 1 6 4.58 0.83 -1 1 6 6.15 0.97 -1 -1 6 5.03 0.91 -1 -1 6 6.50 0.95 1 1 -5 62.29 4.58 -1 1 5 62.09 3.30 1 -1 -5 60.14 4.05 -1 -1 5 67.54 3.42 1 1 -4 27.91 2.65 -1 1 4 26.51 1.81 -1 1 4 28.92 1.97 1 -1 -4 26.54 2.46 -1 -1 4 27.07 1.82 -1 -1 4 27.07 1.83 1 1 -3 240.46 9.04 -1 1 3 230.63 7.39 -1 1 3 233.41 7.62 1 -1 -3 235.07 8.79 -1 -1 3 229.40 7.44 -1 -1 3 239.36 7.42 1 1 -2 21.28 1.65 -1 1 2 19.61 1.17 -1 1 2 20.98 1.07 -1 -1 2 19.43 1.07 1 -1 -2 20.37 1.45 -1 -1 2 21.38 1.10 -1 1 1 62.18 2.14 -1 1 1 60.61 1.96 1 1 -1 63.94 2.59 1 -1 -1 60.90 2.46 -1 -1 1 62.48 2.01 -1 -1 1 64.77 2.07 -1 1 0 194.11 6.29 1 1 0 188.27 6.15 1 1 0 190.01 5.49 -1 1 0 189.38 5.50 -1 -1 0 194.62 5.67 1 -1 0 198.79 5.52 1 1 1 684.91 18.87 -1 1 -1 664.11 18.95 -1 1 -1 651.91 21.31 1 -1 1 678.97 18.89 -1 -1 -1 674.98 19.31 -1 -1 -1 661.51 20.94 -1 1 -2 4.86 1.03 -1 1 -2 3.53 0.65 1 1 2 2.75 0.57 -1 -1 -2 2.84 0.75 1 -1 2 3.37 0.61 -1 -1 -2 3.20 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2.91 0.87 -2 12 6 2.94 0.83 -2 12 6 3.58 0.80 2 12 -6 2.48 1.02 -2 -12 6 3.15 0.83 2 12 -5 23.14 2.17 -2 12 5 23.23 1.80 -2 12 5 22.40 1.67 2 12 -5 25.47 2.17 -2 12 5 24.34 1.70 2 12 -4 4.78 1.14 -2 12 4 3.18 0.90 -2 12 4 3.09 0.77 2 12 -4 3.03 1.03 2 12 -3 15.88 2.82 -2 12 3 20.90 2.45 -2 -12 3 18.52 2.41 2 -12 -3 19.15 2.78 -2 12 2 15.53 2.00 2 12 -2 12.95 2.33 -2 -12 2 15.70 2.11 2 -12 -2 10.66 1.88 2 12 -1 3.13 1.25 -2 12 1 2.97 1.19 2 12 0 29.30 2.60 -2 12 0 29.65 2.84 -2 -12 0 26.18 2.24 2 -12 0 34.68 2.75 -2 12 -1 1.26 1.10 2 12 1 1.97 1.05 -2 -12 -1 2.96 1.13 2 -12 1 2.35 1.11 -2 12 -2 0.59 1.11 2 12 2 0.89 0.99 2 -12 2 -0.20 0.80 -2 -12 -2 0.02 0.95 2 12 3 3.56 1.32 -2 12 -3 5.02 1.90 -2 -12 -3 3.22 1.47 2 -12 3 2.93 1.40 -2 12 -4 86.48 4.23 2 12 4 86.63 3.40 -2 12 -4 89.48 4.19 -2 12 -4 88.24 4.05 2 12 4 86.88 3.55 2 12 5 5.30 0.90 2 12 5 4.35 0.99 -2 12 -5 3.55 1.01 2 12 6 81.13 3.44 -2 12 -6 87.66 3.87 2 12 6 84.44 3.20 -2 -12 -6 84.72 3.66 2 -12 6 81.36 3.41 2 12 7 0.50 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118.91 4.85 -2 16 2 118.40 4.43 2 16 -2 128.21 4.72 -2 16 1 4.54 1.02 2 16 -1 5.83 1.16 2 16 -1 5.05 1.03 -2 16 1 4.73 1.17 2 16 0 83.66 3.73 -2 16 0 87.89 3.93 -2 16 0 81.78 3.50 2 16 0 89.42 3.61 2 16 0 85.95 3.35 -2 16 -1 -0.46 0.81 -2 16 -1 -1.06 0.61 2 16 1 0.84 0.70 2 16 1 -0.20 0.65 2 16 1 0.83 0.81 2 16 2 0.54 0.78 -2 16 -2 0.59 0.95 -2 16 -2 0.51 0.78 2 16 2 1.01 0.68 -2 16 -2 1.99 1.17 2 16 2 0.91 0.86 2 16 3 70.58 3.03 -2 16 -3 70.28 3.56 2 16 3 71.65 3.24 -2 16 -3 74.54 3.55 -2 16 -3 69.70 3.82 2 16 4 0.91 0.65 -2 16 -4 -0.90 0.68 -2 16 -4 -0.46 0.76 -2 16 -4 0.93 1.00 2 16 4 -0.48 0.68 -2 16 -5 30.55 2.14 2 16 5 28.42 1.71 2 16 5 29.95 1.89 2 -16 5 28.54 1.69 2 16 6 16.73 1.16 2 16 6 14.25 1.17 -2 16 -6 13.69 1.31 2 -16 6 14.97 1.07 -2 17 7 0.44 0.38 2 17 -6 0.11 0.58 -2 17 6 -0.26 0.38 -2 17 6 0.25 0.51 -2 -17 6 0.20 0.35 2 17 -5 35.99 2.33 2 17 -5 35.86 2.24 -2 17 5 34.71 1.99 -2 17 5 33.37 1.87 -2 17 4 0.24 0.71 -2 17 4 0.37 0.60 2 17 -4 -0.10 0.73 2 17 -4 -0.24 0.88 2 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4.09 1.17 4 6 5 2.27 0.74 -4 -6 -5 1.82 0.99 4 -6 5 0.71 0.58 4 6 6 62.36 2.79 4 -6 6 69.09 2.89 -4 -6 -6 69.80 3.53 4 6 7 1.49 0.60 -4 -6 -7 1.14 0.85 4 -6 7 1.36 0.55 4 6 8 26.71 1.38 4 -6 8 29.93 1.38 -4 -6 -8 27.74 1.58 4 7 -8 28.87 2.04 -4 7 8 26.60 1.58 -4 7 8 22.61 1.74 4 7 -7 5.33 1.28 -4 7 7 5.70 1.06 -4 7 7 4.75 0.87 -4 -7 7 5.02 0.85 -4 7 6 106.28 3.87 -4 7 6 104.17 4.12 4 7 -6 103.18 4.66 -4 -7 6 101.07 3.77 4 7 -5 76.96 5.70 -4 7 4 0.28 0.71 4 7 -4 0.52 1.04 4 7 -3 240.99 10.34 -4 7 3 252.40 8.73 -4 -7 3 246.59 8.46 4 -7 -3 250.01 10.14 -4 7 2 22.31 1.69 4 7 -2 21.15 2.22 -4 7 2 23.87 1.79 -4 -7 2 21.64 1.68 4 -7 -2 21.17 2.30 -4 7 1 138.09 4.88 -4 7 1 134.84 6.21 4 7 -1 136.79 5.85 4 7 -1 136.87 5.22 -4 -7 1 139.50 5.32 -4 7 0 32.16 2.61 -4 7 0 29.13 1.47 4 7 0 34.30 2.15 -4 -7 0 32.47 2.27 4 -7 0 31.41 1.97 -4 7 -1 3.74 1.36 4 7 1 4.26 1.12 -4 -7 -1 2.60 0.94 4 -7 1 4.22 0.93 -4 7 -2 162.66 7.74 4 7 2 166.38 6.57 -4 -7 -2 165.82 6.87 4 -7 2 165.68 6.35 4 7 3 -0.84 0.84 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35.37 2.38 4 10 -4 85.32 5.98 4 -10 -4 91.49 5.62 4 10 -3 19.74 2.72 4 10 -2 139.00 6.77 -4 10 2 129.44 5.69 4 -10 -2 137.61 6.82 -4 -10 2 136.23 5.43 -4 -10 2 134.05 5.86 4 10 -1 17.17 1.96 -4 10 1 14.09 2.13 -4 -10 1 11.82 1.60 4 -10 -1 15.58 1.75 4 10 0 93.21 4.53 -4 10 0 94.61 5.32 -4 -10 0 89.89 4.46 4 -10 0 88.61 4.31 -4 10 -1 128.89 6.76 4 10 1 138.42 5.87 4 -10 1 125.19 5.64 -4 -10 -1 132.41 5.93 4 10 2 -0.04 0.88 -4 10 -2 0.59 1.07 -4 -10 -2 1.02 1.02 4 -10 2 -0.72 0.81 4 10 3 20.81 2.52 -4 10 -3 21.88 3.45 4 -10 3 16.23 2.10 -4 -10 -3 20.91 2.60 4 10 4 30.62 1.89 -4 10 -4 28.94 2.62 4 10 4 28.75 1.81 -4 10 -4 34.78 2.44 -4 -10 -4 31.81 2.25 4 10 5 4.47 0.94 -4 10 -5 3.72 1.11 4 10 5 4.46 0.90 4 -10 5 4.13 0.85 -4 -10 -5 3.53 1.02 -4 10 -6 17.07 1.75 4 10 6 18.63 1.53 -4 -10 -6 17.85 1.68 4 -10 6 18.49 1.40 -4 10 -7 11.70 1.24 4 10 7 10.59 1.13 4 -10 7 12.28 1.03 -4 -10 -7 13.14 1.27 -4 11 8 1.63 0.56 4 11 -8 1.11 0.66 -4 11 8 2.70 0.61 4 11 -7 8.71 1.34 -4 11 7 10.69 1.15 -4 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0.78 0.44 15 -5 2 0.97 0.52 -15 6 6 29.92 1.52 -15 6 6 28.68 1.67 15 6 -6 29.71 1.69 -15 -6 6 32.37 1.43 15 6 -5 5.16 0.96 -15 6 5 5.12 0.93 -15 6 5 4.51 0.77 -15 -6 5 5.30 0.73 -15 6 4 26.12 1.90 -15 6 4 25.37 1.63 -15 -6 4 26.95 1.49 -15 6 3 -1.15 0.57 -15 6 3 -0.97 0.45 -15 -6 3 -0.54 0.40 15 6 -2 32.88 1.97 -15 6 2 35.60 2.00 -15 6 2 33.80 2.22 -15 6 1 1.40 0.63 -15 6 1 0.45 0.71 15 6 -1 0.32 0.65 15 -6 -1 1.26 0.76 -15 6 0 42.61 2.36 15 6 0 39.87 2.25 -15 6 0 42.25 2.15 15 -6 0 42.74 2.32 15 6 1 3.17 0.76 -15 6 -1 3.44 0.70 15 -6 1 10.39 1.23 15 6 2 49.18 2.14 -15 6 -2 49.15 1.98 -15 -6 -2 46.60 1.87 15 -6 2 50.25 2.18 -15 7 6 10.13 0.87 -15 7 6 10.31 0.99 15 7 -6 7.41 0.92 -15 -7 6 8.87 0.75 -15 7 5 0.58 0.60 15 7 -5 0.98 0.65 -15 7 5 0.26 0.45 -15 -7 5 0.01 0.35 -15 7 4 13.85 1.21 -15 7 4 11.17 1.40 -15 -7 4 14.98 1.09 -15 7 3 0.41 0.71 -15 7 3 0.71 0.57 -15 -7 3 0.36 0.46 -15 7 2 11.28 1.21 -15 7 2 10.86 1.44 15 7 -2 10.21 1.23 -15 7 1 37.07 2.01 -15 7 1 36.13 2.29 15 7 -1 40.83 2.19 15 -7 -1 39.33 2.16 -15 7 0 22.26 1.47 15 7 0 22.99 1.65 -15 7 0 22.03 1.72 -15 7 -1 103.81 3.52 -15 7 -1 95.51 3.64 15 7 1 102.64 3.74 15 -7 1 92.46 3.66 -15 7 -2 2.30 0.48 15 7 2 2.43 0.59 15 -7 2 2.96 0.60 -15 8 6 0.21 0.36 -15 -8 6 -0.24 0.29 -15 8 5 57.24 2.65 -15 8 5 61.99 2.41 -15 -8 5 58.42 2.23 -15 8 4 0.67 0.49 -15 8 4 0.77 0.66 -15 -8 4 1.48 0.49 -15 8 3 34.50 2.19 -15 8 3 35.98 1.89 -15 -8 3 34.81 1.69 15 8 -2 11.09 1.24 -15 8 2 12.94 1.43 -15 8 2 9.79 1.11 -15 8 1 67.17 3.17 15 8 -1 67.32 2.95 -15 8 1 70.91 2.83 15 -8 -1 69.16 2.92 -15 8 0 27.84 1.87 15 8 0 28.33 1.73 -15 8 0 26.55 1.56 -15 8 -1 5.99 0.92 -15 8 -1 8.04 0.84 15 8 1 6.65 0.95 15 -8 1 8.64 1.12 15 8 2 2.87 0.59 15 -8 2 3.29 0.62 -15 9 6 36.51 1.57 -15 -9 6 37.22 1.53 -15 9 5 2.03 0.61 -15 9 5 1.17 0.45 -15 -9 5 1.47 0.45 -15 9 4 53.51 2.58 -15 9 4 51.67 2.23 -15 -9 4 50.55 2.07 -15 9 3 7.57 0.95 -15 9 3 10.19 1.31 -15 -9 3 9.10 0.88 15 9 -2 54.62 2.48 -15 9 2 58.55 2.83 -15 9 2 55.08 2.40 -15 9 1 7.59 0.94 -15 9 1 10.06 1.31 15 9 -1 7.89 1.09 -15 9 0 19.96 1.57 -15 9 0 19.33 1.25 15 9 0 23.04 1.54 15 9 1 5.99 0.85 -15 9 -1 4.81 0.82 -15 9 -1 4.83 0.67 15 -9 1 4.17 0.79 15 -9 2 1.83 0.50 -15 10 5 29.39 1.57 -15 10 5 30.46 1.43 -15 -10 5 31.23 1.37 -15 10 4 -0.65 0.46 -15 10 4 0.27 0.38 -15 -10 4 -0.31 0.33 -15 10 3 38.61 1.84 -15 10 3 38.18 2.15 -15 -10 3 39.13 1.72 15 10 -2 25.97 1.59 -15 10 2 26.91 1.49 -15 10 2 25.11 1.78 -15 -10 2 26.03 1.34 -15 10 1 10.54 0.96 -15 10 1 10.99 1.31 15 10 -1 10.55 1.14 -15 10 0 46.86 2.28 -15 10 0 43.02 1.85 15 10 0 43.69 2.10 15 10 1 1.94 0.56 -15 10 -1 2.44 0.64 15 -10 1 2.00 0.62 -15 11 5 23.89 1.14 -15 -11 5 20.62 1.04 -15 11 4 0.62 0.51 -15 11 4 0.91 0.42 -15 -11 4 0.61 0.37 -15 11 3 0.28 0.56 -15 11 3 0.73 0.46 -15 -11 3 0.91 0.41 -15 11 2 7.95 0.83 -15 11 2 9.94 1.15 15 11 -2 10.38 1.02 -15 -11 2 8.50 0.79 15 11 -1 3.13 0.69 -15 11 1 3.01 0.55 -15 11 1 4.83 0.91 15 11 0 2.35 0.60 -15 11 0 3.97 0.82 15 11 1 95.35 3.16 -15 11 -1 91.81 3.32 15 -11 1 88.43 3.13 -15 12 4 12.04 1.00 -15 12 4 11.84 0.83 -15 -12 4 13.26 0.84 -15 12 3 7.04 0.73 -15 12 3 7.21 0.96 -15 -12 3 7.52 0.71 -15 12 2 0.49 0.55 -15 12 2 0.21 0.40 15 12 -2 0.34 0.49 -15 -12 2 0.00 0.33 -15 12 1 18.10 1.36 15 12 -1 19.07 1.23 -15 12 0 69.20 2.72 15 12 0 66.99 2.57 -15 13 3 0.21 0.45 -15 -13 3 -0.13 0.28 -15 13 2 25.46 1.46 -15 -13 2 25.49 1.13 15 13 -1 8.06 0.83 -15 13 1 7.46 0.90 15 13 0 21.91 1.22 -15 13 0 22.67 1.31 16 0 -6 29.55 1.66 -16 0 5 -0.02 0.46 -16 0 5 0.35 0.56 -16 0 4 76.69 2.91 -16 0 4 73.44 3.23 -16 0 3 -0.13 0.52 -16 0 3 -0.24 0.57 -16 0 2 101.73 3.83 -16 0 2 93.48 3.64 16 0 -1 -0.18 0.53 -16 0 1 -0.31 0.50 16 0 0 1.69 0.67 -16 0 0 1.68 0.61 16 0 1 -0.92 0.43 -16 0 -1 -0.41 0.42 16 0 2 14.32 1.03 -16 0 -2 14.92 0.98 16 1 -6 -0.47 0.47 16 -1 -6 -0.40 0.41 -16 1 5 33.61 1.93 -16 1 5 35.54 1.67 -16 -1 5 36.00 1.99 -16 1 4 7.03 0.95 -16 1 4 7.44 1.10 -16 -1 4 6.54 0.88 -16 -1 4 5.55 0.93 -16 1 3 59.65 2.61 -16 1 3 58.41 2.81 -16 -1 3 58.09 2.52 -16 -1 3 59.01 2.74 -16 1 2 17.06 1.45 -16 1 2 20.72 1.50 -16 -1 2 19.32 1.41 -16 1 1 7.21 1.05 16 1 -1 9.44 1.18 16 -1 -1 6.38 0.97 -16 -1 1 8.36 1.03 16 1 0 52.29 2.42 -16 1 0 49.21 2.31 16 -1 0 52.23 2.39 -16 -1 0 51.73 2.30 16 1 1 0.67 0.56 -16 1 -1 0.62 0.51 -16 -1 -1 0.07 0.45 16 -1 1 1.78 0.61 -16 1 -2 31.76 1.45 16 1 2 31.02 1.52 16 -1 2 30.51 1.50 -16 -1 -2 31.40 1.44 16 2 -6 3.86 0.72 16 -2 -6 4.03 0.74 -16 2 5 0.41 0.58 -16 2 5 -0.23 0.40 -16 2 4 14.51 1.22 -16 2 4 17.70 1.52 -16 -2 4 13.37 1.31 -16 2 3 5.73 1.01 -16 2 3 3.41 0.77 -16 -2 3 2.90 0.66 -16 -2 3 3.05 0.77 -16 2 2 16.06 1.36 -16 2 2 16.15 1.48 -16 -2 2 17.32 1.30 -16 2 1 61.82 2.70 16 2 -1 61.63 2.74 16 -2 -1 60.46 2.68 -16 -2 1 63.04 2.63 -16 2 0 0.39 0.50 16 2 0 0.16 0.56 16 -2 0 0.63 0.56 -16 -2 0 1.01 0.52 16 2 1 89.10 3.31 -16 2 -1 87.99 3.17 -16 -2 -1 84.54 3.09 16 -2 1 87.04 3.28 16 2 2 1.02 0.45 -16 2 -2 0.73 0.38 16 -2 2 1.22 0.47 -16 -2 -2 1.01 0.40 16 3 -6 37.12 1.82 -16 3 5 2.53 0.57 -16 3 5 2.68 0.72 16 3 -5 2.40 0.73 -16 -3 5 1.90 0.50 -16 3 4 3.57 0.89 -16 3 4 4.03 0.76 -16 -3 4 3.26 0.79 -16 3 3 3.37 0.84 -16 3 3 3.50 0.78 -16 3 2 3.70 0.88 -16 3 2 3.61 0.76 -16 -3 2 3.55 0.71 -16 3 1 0.69 0.61 16 3 -1 1.17 0.64 -16 3 1 1.49 0.61 16 -3 -1 1.39 0.63 -16 -3 1 0.96 0.54 -16 3 0 42.12 2.02 16 3 0 40.50 2.10 16 -3 0 38.83 2.04 -16 -3 0 41.71 1.95 -16 3 -1 1.00 0.47 16 3 1 -0.06 0.47 -16 -3 -1 0.27 0.40 16 -3 1 0.66 0.52 16 3 2 40.75 1.74 -16 3 -2 42.06 1.66 16 -3 2 39.11 1.73 16 4 -6 11.64 0.98 -16 4 5 16.39 1.37 16 4 -5 17.40 1.36 -16 4 5 18.27 1.20 -16 -4 5 16.25 0.99 -16 4 4 26.64 1.82 -16 4 4 24.04 1.52 16 4 -4 27.45 1.72 -16 4 3 0.23 0.62 -16 4 3 0.00 0.48 -16 4 2 35.69 1.94 -16 4 2 36.25 2.13 -16 4 1 2.00 0.73 -16 4 1 2.78 0.71 16 4 -1 3.39 0.79 16 -4 -1 2.93 0.74 -16 -4 1 4.52 0.77 16 4 0 1.09 0.61 -16 4 0 1.53 0.58 16 -4 0 1.16 0.57 -16 -4 0 0.92 0.50 -16 4 -1 38.61 1.79 16 4 1 39.34 1.90 16 -4 1 39.43 1.89 -16 -4 -1 37.92 1.66 -16 4 -2 13.70 0.95 16 4 2 13.34 0.93 16 -4 2 12.83 0.91 -16 5 5 31.84 1.56 16 5 -5 27.49 1.65 -16 5 5 31.87 1.80 -16 -5 5 30.51 1.36 -16 5 4 0.19 0.41 -16 5 4 -0.33 0.49 -16 5 3 92.67 3.48 -16 5 3 95.09 3.81 -16 5 2 5.86 0.90 -16 5 2 7.40 1.11 16 5 -1 21.70 1.53 -16 5 1 20.59 1.55 -16 5 1 21.38 1.47 16 -5 -1 24.42 1.50 16 5 0 8.42 1.05 -16 5 0 10.00 0.98 16 -5 0 7.61 0.98 16 5 1 0.61 0.51 -16 5 -1 0.40 0.39 16 -5 1 1.23 0.53 -16 -5 -1 1.82 0.52 -16 6 5 4.43 0.80 -16 6 5 4.27 0.67 -16 -6 5 4.78 0.61 -16 6 4 56.09 2.26 -16 6 4 51.51 2.50 -16 -6 4 46.46 1.89 -16 6 3 8.35 0.97 -16 6 3 9.19 1.17 -16 6 2 47.89 2.25 -16 6 2 51.23 2.51 -16 6 1 1.07 0.53 -16 6 1 1.84 0.68 16 6 -1 0.89 0.57 16 -6 -1 1.55 0.60 16 6 0 7.31 0.97 -16 6 0 8.03 0.99 -16 6 0 9.09 0.92 16 -6 0 9.97 1.04 16 6 1 1.96 0.54 -16 6 -1 1.64 0.46 16 -6 1 1.82 0.56 -16 7 5 33.74 1.54 -16 7 5 34.17 1.76 -16 -7 5 34.02 1.40 -16 7 4 11.37 1.21 -16 7 4 13.25 1.04 -16 -7 4 14.42 0.93 -16 7 3 33.34 2.00 -16 7 3 35.92 1.76 -16 7 2 -0.01 0.44 -16 7 2 0.38 0.55 -16 7 1 0.17 0.43 -16 7 1 -0.11 0.51 16 7 -1 0.02 0.51 16 7 0 34.53 1.79 -16 7 0 35.18 1.67 -16 7 0 34.78 1.77 16 -7 0 37.30 1.76 -16 7 -1 1.04 0.40 16 7 1 0.68 0.45 16 -7 1 0.68 0.47 -16 8 5 -0.22 0.34 -16 8 5 0.01 0.29 -16 -8 5 1.07 0.39 -16 8 4 1.50 0.48 -16 8 4 1.56 0.61 -16 -8 4 2.90 0.48 -16 8 3 14.28 1.33 -16 8 3 13.27 1.04 -16 8 2 0.06 0.38 -16 8 2 0.56 0.61 -16 8 1 40.74 2.05 -16 8 1 42.19 1.86 16 8 -1 39.35 1.92 -16 8 0 3.30 0.55 -16 8 0 1.45 0.54 16 8 0 3.13 0.66 16 -8 0 2.75 0.63 16 8 1 103.07 3.41 16 -8 1 103.74 3.45 -16 9 4 3.92 0.59 -16 9 4 2.47 0.64 -16 -9 4 3.10 0.48 -16 9 3 5.61 0.87 -16 9 3 6.01 0.73 -16 9 2 20.35 1.21 -16 9 2 21.46 1.48 16 9 -1 3.03 0.64 -16 9 1 2.24 0.49 -16 9 1 3.61 0.71 -16 9 0 81.90 2.98 16 9 0 82.20 2.92 -16 9 0 79.62 2.71 16 -9 0 85.04 2.87 -16 10 4 20.92 1.08 -16 10 4 21.49 1.30 -16 10 3 0.25 0.50 -16 10 3 -0.08 0.31 -16 10 2 22.85 1.45 -16 10 2 21.65 1.17 -16 10 1 23.39 1.37 -16 10 1 17.05 1.00 16 10 -1 16.99 1.11 16 10 0 5.35 0.70 -16 11 3 30.08 1.55 -16 11 2 -0.48 0.41 -16 11 1 8.74 0.89 17 0 -5 0.04 0.39 -17 0 4 0.76 0.45 -17 0 4 1.82 0.60 -17 0 3 0.22 0.45 -17 0 3 -1.22 0.41 -17 0 2 59.66 2.40 17 0 -1 0.25 0.49 -17 0 1 0.26 0.44 17 0 0 75.92 2.82 -17 0 0 77.04 2.74 17 0 1 -0.16 0.35 17 1 -5 -0.30 0.46 -17 1 4 17.05 1.09 -17 1 4 15.78 1.22 -17 -1 4 15.22 1.20 -17 1 3 15.71 1.25 -17 1 3 13.25 1.07 -17 -1 3 14.46 1.05 -17 1 2 1.72 0.57 -17 -1 2 1.93 0.55 -17 1 1 61.85 2.42 17 1 -1 58.95 2.40 -17 -1 1 61.49 2.37 17 -1 -1 58.31 2.39 -17 1 0 0.32 0.46 17 1 0 0.76 0.49 17 -1 0 0.09 0.42 -17 -1 0 0.13 0.39 -17 1 -1 20.03 1.11 17 1 1 21.50 1.25 17 -1 1 24.75 1.37 -17 2 5 59.50 2.42 -17 2 4 1.30 0.48 -17 2 4 2.16 0.62 -17 2 3 21.31 1.44 -17 2 3 17.59 1.19 -17 2 2 7.92 0.99 -17 2 2 6.34 0.86 -17 -2 2 8.23 0.87 -17 2 1 14.86 1.09 17 2 -1 13.32 1.08 17 -2 -1 11.50 1.05 -17 -2 1 14.10 1.01 -17 2 0 12.20 0.94 17 2 0 10.65 0.98 17 -2 0 9.42 0.94 -17 -2 0 10.34 0.86 -17 2 -1 19.87 1.07 -17 3 5 0.95 0.49 -17 3 4 53.19 2.36 -17 3 4 53.69 2.12 -17 3 3 0.99 0.57 -17 3 3 1.04 0.50 -17 3 2 8.23 0.90 -17 3 2 7.78 0.97 17 3 -1 10.44 0.99 -17 3 1 8.64 0.90 -17 -3 1 10.46 0.85 17 3 0 1.15 0.51 -17 3 0 1.39 0.47 -17 -3 0 0.93 0.43 17 -3 0 1.53 0.50 -17 4 4 5.18 0.70 -17 4 4 4.38 0.79 -17 4 3 6.65 0.92 -17 4 3 6.70 0.78 -17 4 2 5.48 0.78 -17 4 2 5.75 0.84 17 4 -1 4.10 0.69 -17 4 1 5.36 0.75 -17 4 0 14.57 0.98 17 4 0 15.33 1.05 17 -4 0 13.46 1.01 -17 5 4 11.60 1.06 -17 5 4 11.38 0.89 -17 5 3 4.83 0.82 -17 5 3 6.04 0.76 -17 5 2 0.64 0.46 -17 5 2 0.28 0.50 -17 5 1 32.09 1.63 -17 5 1 36.16 1.64 17 5 -1 36.12 1.65 -17 5 0 1.31 0.41 17 5 0 0.44 0.42 -17 6 4 3.44 0.57 -17 6 4 2.73 0.65 -17 6 3 2.96 0.68 -17 6 3 2.45 0.53 -17 6 2 33.81 1.56 -17 6 2 33.99 1.74 17 6 -1 -0.47 0.40 -17 6 1 0.39 0.39 -17 6 1 -0.27 0.45 -17 6 0 67.42 2.34 -17 7 4 25.29 1.40 -17 7 4 25.57 1.22 -17 7 3 32.53 1.67 -17 7 3 31.39 1.45 -17 7 2 12.93 1.08 -17 7 2 11.22 0.87 -17 7 1 28.53 1.33 -17 8 3 18.37 1.02 -17 8 3 17.82 1.19 -17 8 2 7.46 0.86 -17 8 2 7.59 0.67 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 429 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Warren Piers' _publ_contact_author_address ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Morgan, Matthew' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; 'Piers, Warren' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_MM1516_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 B Cl N' _chemical_formula_sum 'C25 H19 B Cl N' _chemical_formula_weight 379.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5793(5) _cell_length_b 20.7341(11) _cell_length_c 12.3247(5) _cell_angle_alpha 90 _cell_angle_beta 94.596(4) _cell_angle_gamma 90 _cell_volume 1930.60(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 893 _cell_measurement_theta_min 8.31 _cell_measurement_theta_max 72.19 _exptl_crystal_description 'plate' _exptl_crystal_colour 'Yellow' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.306 _exptl_crystal_F_000 792 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.806 _shelx_estimated_absorpt_T_min 0.840 _shelx_estimated_absorpt_T_max 0.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10726 _diffrn_reflns_av_unetI/netI 0.0524 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.183 _diffrn_reflns_theta_max 66.453 _diffrn_reflns_theta_full 66.500 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_point_group_measured_fraction_full 0.975 _reflns_number_total 3317 _reflns_number_gt 2521 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.2.4' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+0.4990P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3317 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.05877(8) 0.37525(3) 0.41631(5) 0.02978(18) Uani 1 1 d . . . . . N1 N 0.2915(3) 0.40916(10) 0.48499(16) 0.0250(5) Uani 1 1 d . . . . . C17 C 0.0913(4) 0.13971(13) 0.2113(2) 0.0330(6) Uani 1 1 d . . . . . H17 H 0.0499 0.1032 0.1702 0.040 Uiso 1 1 calc R U . . . C16 C 0.1871(4) 0.13179(13) 0.3109(2) 0.0340(6) Uani 1 1 d . . . . . H16 H 0.2122 0.0895 0.3377 0.041 Uiso 1 1 calc R U . . . C1 C 0.2733(3) 0.30495(12) 0.39579(19) 0.0247(5) Uani 1 1 d . . . . . C2 C 0.4148(3) 0.30738(12) 0.47057(19) 0.0249(5) Uani 1 1 d . . . . . C8 C 0.2069(3) 0.41412(12) 0.27357(19) 0.0256(6) Uani 1 1 d . . . . . C25 C 0.5858(3) 0.23193(13) 0.6006(2) 0.0282(6) Uani 1 1 d . . . . . H25 H 0.5180 0.2463 0.6575 0.034 Uiso 1 1 calc R U . . . C6 C 0.3747(4) 0.49021(13) 0.6136(2) 0.0315(6) Uani 1 1 d . . . . . H6 H 0.3548 0.5314 0.6441 0.038 Uiso 1 1 calc R U . . . C9 C 0.3529(4) 0.40153(13) 0.2153(2) 0.0324(6) Uani 1 1 d . . . . . H9 H 0.4351 0.3694 0.2416 0.039 Uiso 1 1 calc R U . . . C24 C 0.7158(4) 0.18525(13) 0.6215(2) 0.0331(6) Uani 1 1 d . . . . . H24 H 0.7368 0.1681 0.6929 0.040 Uiso 1 1 calc R U . . . C20 C 0.5545(3) 0.25771(12) 0.49648(19) 0.0240(5) Uani 1 1 d . . . . . B1 B 0.1814(4) 0.37516(14) 0.3846(2) 0.0258(6) Uani 1 1 d . . . . . C19 C 0.1176(4) 0.25420(13) 0.2325(2) 0.0301(6) Uani 1 1 d . . . . . H19 H 0.0924 0.2962 0.2047 0.036 Uiso 1 1 calc R U . . . C14 C 0.2150(3) 0.24740(12) 0.3328(2) 0.0253(5) Uani 1 1 d . . . . . C23 C 0.8152(4) 0.16357(14) 0.5391(2) 0.0343(6) Uani 1 1 d . . . . . H23 H 0.9028 0.1312 0.5534 0.041 Uiso 1 1 calc R U . . . C15 C 0.2465(4) 0.18430(13) 0.3715(2) 0.0301(6) Uani 1 1 d . . . . . H15 H 0.3096 0.1779 0.4404 0.036 Uiso 1 1 calc R U . . . C22 C 0.7852(4) 0.18960(14) 0.4359(2) 0.0344(6) Uani 1 1 d . . . . . H22 H 0.8533 0.1753 0.3790 0.041 Uiso 1 1 calc R U . . . C13 C 0.0910(4) 0.46230(13) 0.2317(2) 0.0324(6) Uani 1 1 d . . . . . H13 H -0.0110 0.4723 0.2685 0.039 Uiso 1 1 calc R U . . . C7 C 0.2681(4) 0.46809(12) 0.5259(2) 0.0282(6) Uani 1 1 d . . . . . H7 H 0.1766 0.4950 0.4939 0.034 Uiso 1 1 calc R U . . . C21 C 0.6570(4) 0.23626(13) 0.4150(2) 0.0304(6) Uani 1 1 d . . . . . H21 H 0.6385 0.2540 0.3439 0.037 Uiso 1 1 calc R U . . . C10 C 0.3829(4) 0.43425(14) 0.1200(2) 0.0387(7) Uani 1 1 d . . . . . H10 H 0.4825 0.4236 0.0814 0.046 Uiso 1 1 calc R U . . . C3 C 0.4234(3) 0.36988(12) 0.52648(19) 0.0257(5) Uani 1 1 d . . . . . C12 C 0.1222(4) 0.49572(15) 0.1376(2) 0.0372(7) Uani 1 1 d . . . . . H12 H 0.0419 0.5284 0.1114 0.045 Uiso 1 1 calc R U . . . C4 C 0.5388(4) 0.39100(13) 0.6123(2) 0.0301(6) Uani 1 1 d . . . . . H4 H 0.6343 0.3646 0.6401 0.036 Uiso 1 1 calc R U . . . C18 C 0.0568(4) 0.20084(14) 0.1723(2) 0.0345(6) Uani 1 1 d . . . . . H18 H -0.0089 0.2067 0.1041 0.041 Uiso 1 1 calc R U . . . C5 C 0.5121(4) 0.45121(13) 0.6566(2) 0.0331(6) Uani 1 1 d . . . . . H5 H 0.5879 0.4659 0.7167 0.040 Uiso 1 1 calc R U . . . C11 C 0.2682(4) 0.48214(15) 0.0813(2) 0.0390(7) Uani 1 1 d . . . . . H11 H 0.2893 0.5054 0.0172 0.047 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0242(3) 0.0330(3) 0.0320(3) 0.0019(2) 0.0015(2) 0.0000(2) N1 0.0235(12) 0.0255(11) 0.0262(10) 0.0008(8) 0.0033(9) -0.0013(8) C17 0.0311(16) 0.0314(15) 0.0371(14) -0.0114(11) 0.0065(12) -0.0009(11) C16 0.0312(16) 0.0248(14) 0.0464(16) -0.0001(12) 0.0061(13) 0.0016(11) C1 0.0241(14) 0.0258(13) 0.0241(11) 0.0020(10) 0.0015(10) -0.0002(10) C2 0.0242(14) 0.0267(13) 0.0239(11) 0.0007(10) 0.0026(10) -0.0006(10) C8 0.0281(15) 0.0223(13) 0.0260(12) -0.0024(10) -0.0011(10) -0.0015(10) C25 0.0252(15) 0.0332(14) 0.0262(12) 0.0005(10) 0.0028(11) 0.0011(10) C6 0.0352(16) 0.0286(15) 0.0316(13) -0.0037(11) 0.0075(11) -0.0038(11) C9 0.0341(16) 0.0296(14) 0.0339(14) 0.0006(11) 0.0041(12) 0.0027(11) C24 0.0326(17) 0.0336(15) 0.0322(13) 0.0083(11) -0.0039(12) -0.0006(11) C20 0.0192(14) 0.0258(13) 0.0264(12) 0.0004(10) -0.0009(10) -0.0007(9) B1 0.0241(16) 0.0268(15) 0.0260(13) -0.0038(12) -0.0016(11) -0.0005(11) C19 0.0335(16) 0.0282(14) 0.0282(12) -0.0015(11) -0.0006(11) 0.0005(11) C14 0.0213(14) 0.0270(13) 0.0281(12) -0.0016(10) 0.0039(10) 0.0006(9) C23 0.0244(15) 0.0340(16) 0.0434(15) -0.0010(12) -0.0044(12) 0.0033(11) C15 0.0258(15) 0.0308(15) 0.0332(13) 0.0031(11) 0.0001(11) -0.0010(10) C22 0.0258(16) 0.0396(16) 0.0387(15) -0.0064(12) 0.0083(12) 0.0020(11) C13 0.0290(16) 0.0372(16) 0.0308(13) 0.0012(11) 0.0013(11) 0.0028(11) C7 0.0265(15) 0.0266(14) 0.0322(13) 0.0003(10) 0.0067(11) -0.0001(10) C21 0.0289(16) 0.0365(15) 0.0260(12) 0.0013(11) 0.0025(11) -0.0007(11) C10 0.0444(19) 0.0377(17) 0.0358(15) -0.0021(12) 0.0143(13) 0.0004(13) C3 0.0241(14) 0.0292(14) 0.0239(12) 0.0016(10) 0.0032(10) -0.0021(10) C12 0.0381(18) 0.0383(16) 0.0341(14) 0.0054(12) -0.0030(12) 0.0059(12) C4 0.0254(15) 0.0335(15) 0.0313(13) 0.0012(11) 0.0003(11) -0.0010(10) C18 0.0349(17) 0.0405(16) 0.0276(12) -0.0065(12) -0.0002(12) -0.0004(12) C5 0.0338(17) 0.0346(15) 0.0304(13) -0.0055(11) 0.0006(11) -0.0102(11) C11 0.051(2) 0.0390(17) 0.0268(13) 0.0042(12) 0.0026(13) -0.0037(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.892(3) . ? N1 C7 1.339(3) . ? N1 C3 1.357(3) . ? N1 B1 1.599(3) . ? C17 C18 1.373(4) . ? C17 C16 1.386(4) . ? C17 H17 0.9500 . ? C16 C15 1.375(4) . ? C16 H16 0.9500 . ? C1 C2 1.358(3) . ? C1 C14 1.472(3) . ? C1 B1 1.615(4) . ? C2 C3 1.467(3) . ? C2 C20 1.493(3) . ? C8 C9 1.392(4) . ? C8 C13 1.401(4) . ? C8 B1 1.614(4) . ? C25 C24 1.391(4) . ? C25 C20 1.392(3) . ? C25 H25 0.9500 . ? C6 C7 1.376(4) . ? C6 C5 1.390(4) . ? C6 H6 0.9500 . ? C9 C10 1.391(4) . ? C9 H9 0.9500 . ? C24 C23 1.387(4) . ? C24 H24 0.9500 . ? C20 C21 1.391(4) . ? C19 C18 1.390(4) . ? C19 C14 1.395(3) . ? C19 H19 0.9500 . ? C14 C15 1.406(4) . ? C23 C22 1.384(4) . ? C23 H23 0.9500 . ? C15 H15 0.9500 . ? C22 C21 1.381(4) . ? C22 H22 0.9500 . ? C13 C12 1.388(4) . ? C13 H13 0.9500 . ? C7 H7 0.9500 . ? C21 H21 0.9500 . ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C3 C4 1.388(4) . ? C12 C11 1.381(4) . ? C12 H12 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C18 H18 0.9500 . ? C5 H5 0.9500 . ? C11 H11 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 N1 C3 121.4(2) . . ? C7 N1 B1 128.1(2) . . ? C3 N1 B1 110.5(2) . . ? C18 C17 C16 119.4(3) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C15 C16 C17 120.9(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C2 C1 C14 125.1(2) . . ? C2 C1 B1 109.6(2) . . ? C14 C1 B1 125.2(2) . . ? C1 C2 C3 110.8(2) . . ? C1 C2 C20 128.9(2) . . ? C3 C2 C20 120.3(2) . . ? C9 C8 C13 116.4(2) . . ? C9 C8 B1 119.8(2) . . ? C13 C8 B1 123.7(2) . . ? C24 C25 C20 120.3(2) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C7 C6 C5 118.8(2) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C10 C9 C8 122.3(3) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C23 C24 C25 120.5(2) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C21 C20 C25 118.6(2) . . ? C21 C20 C2 119.6(2) . . ? C25 C20 C2 121.8(2) . . ? N1 B1 C8 110.2(2) . . ? N1 B1 C1 97.85(19) . . ? C8 B1 C1 116.3(2) . . ? N1 B1 Cl1 106.89(18) . . ? C8 B1 Cl1 110.91(18) . . ? C1 B1 Cl1 113.49(19) . . ? C18 C19 C14 121.4(3) . . ? C18 C19 H19 119.3 . . ? C14 C19 H19 119.3 . . ? C19 C14 C15 117.2(2) . . ? C19 C14 C1 120.0(2) . . ? C15 C14 C1 122.7(2) . . ? C22 C23 C24 119.2(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C16 C15 C14 120.9(2) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C12 C13 C8 121.3(3) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? N1 C7 C6 120.8(2) . . ? N1 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C22 C21 C20 121.0(2) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? N1 C3 C4 119.8(2) . . ? N1 C3 C2 110.5(2) . . ? C4 C3 C2 129.7(2) . . ? C11 C12 C13 121.0(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C4 C5 C6 120.2(2) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? _refine_diff_density_max 0.345 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.055 _shelxl_version_number 2013-4 _shelx_res_file ; TITL matrix_0m_a.res in P2(1)/c CELL 1.54178 7.5793 20.7341 12.3247 90.000 94.596 90.000 ZERR 4.000 0.0005 0.0011 0.0005 0.000 0.004 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N B Cl UNIT 100 76 4 4 4 L.S. 10 ACTA 133 OMIT -4 133 BOND $H FMAP 2 PLAN 20 LIST 6 SIZE 0.050 0.100 0.100 TEMP -100.150 WGHT 0.059700 0.499000 FVAR 0.20464 CL1 5 -0.058774 0.375254 0.416310 11.00000 0.02420 0.03302 = 0.03199 0.00194 0.00151 -0.00001 N1 3 0.291464 0.409163 0.484987 11.00000 0.02353 0.02547 = 0.02624 0.00082 0.00328 -0.00128 C17 1 0.091317 0.139710 0.211258 11.00000 0.03114 0.03139 = 0.03713 -0.01140 0.00651 -0.00087 AFIX 43 H17 2 0.049897 0.103173 0.170247 11.00000 -1.20000 AFIX 0 C16 1 0.187137 0.131793 0.310911 11.00000 0.03124 0.02485 = 0.04642 -0.00012 0.00610 0.00159 AFIX 43 H16 2 0.212161 0.089547 0.337735 11.00000 -1.20000 AFIX 0 C1 1 0.273291 0.304952 0.395789 11.00000 0.02412 0.02584 = 0.02406 0.00198 0.00150 -0.00018 C2 1 0.414755 0.307379 0.470569 11.00000 0.02418 0.02667 = 0.02392 0.00067 0.00257 -0.00058 C8 1 0.206857 0.414125 0.273565 11.00000 0.02806 0.02226 = 0.02602 -0.00240 -0.00112 -0.00153 C25 1 0.585772 0.231928 0.600558 11.00000 0.02519 0.03320 = 0.02624 0.00050 0.00284 0.00107 AFIX 43 H25 2 0.518002 0.246284 0.657487 11.00000 -1.20000 AFIX 0 C6 1 0.374717 0.490211 0.613581 11.00000 0.03518 0.02863 = 0.03158 -0.00370 0.00754 -0.00376 AFIX 43 H6 2 0.354824 0.531383 0.644147 11.00000 -1.20000 AFIX 0 C9 1 0.352947 0.401527 0.215299 11.00000 0.03410 0.02959 = 0.03385 0.00061 0.00413 0.00272 AFIX 43 H9 2 0.435101 0.369449 0.241555 11.00000 -1.20000 AFIX 0 C24 1 0.715825 0.185254 0.621546 11.00000 0.03256 0.03357 = 0.03223 0.00834 -0.00387 -0.00055 AFIX 43 H24 2 0.736757 0.168088 0.692884 11.00000 -1.20000 AFIX 0 C20 1 0.554455 0.257706 0.496483 11.00000 0.01923 0.02575 = 0.02644 0.00041 -0.00092 -0.00074 B1 4 0.181414 0.375165 0.384596 11.00000 0.02414 0.02677 = 0.02601 -0.00377 -0.00157 -0.00045 C19 1 0.117642 0.254204 0.232481 11.00000 0.03346 0.02818 = 0.02817 -0.00149 -0.00062 0.00050 AFIX 43 H19 2 0.092442 0.296225 0.204680 11.00000 -1.20000 AFIX 0 C14 1 0.214951 0.247396 0.332820 11.00000 0.02127 0.02702 = 0.02806 -0.00164 0.00395 0.00057 C23 1 0.815216 0.163572 0.539120 11.00000 0.02443 0.03397 = 0.04335 -0.00097 -0.00437 0.00329 AFIX 43 H23 2 0.902828 0.131240 0.553366 11.00000 -1.20000 AFIX 0 C15 1 0.246476 0.184299 0.371484 11.00000 0.02580 0.03081 = 0.03324 0.00312 0.00013 -0.00100 AFIX 43 H15 2 0.309611 0.177860 0.440370 11.00000 -1.20000 AFIX 0 C22 1 0.785229 0.189604 0.435860 11.00000 0.02583 0.03963 = 0.03875 -0.00643 0.00833 0.00203 AFIX 43 H22 2 0.853263 0.175292 0.379026 11.00000 -1.20000 AFIX 0 C13 1 0.090951 0.462301 0.231713 11.00000 0.02900 0.03725 = 0.03078 0.00123 0.00135 0.00278 AFIX 43 H13 2 -0.011044 0.472296 0.268517 11.00000 -1.20000 AFIX 0 C7 1 0.268058 0.468086 0.525857 11.00000 0.02653 0.02663 = 0.03223 0.00032 0.00673 -0.00007 AFIX 43 H7 2 0.176625 0.494968 0.493876 11.00000 -1.20000 AFIX 0 C21 1 0.656975 0.236259 0.415012 11.00000 0.02887 0.03646 = 0.02603 0.00129 0.00248 -0.00073 AFIX 43 H21 2 0.638471 0.253983 0.343930 11.00000 -1.20000 AFIX 0 C10 1 0.382872 0.434248 0.119998 11.00000 0.04445 0.03772 = 0.03581 -0.00206 0.01432 0.00044 AFIX 43 H10 2 0.482515 0.423591 0.081442 11.00000 -1.20000 AFIX 0 C3 1 0.423370 0.369875 0.526479 11.00000 0.02414 0.02922 = 0.02385 0.00161 0.00321 -0.00207 C12 1 0.122158 0.495720 0.137551 11.00000 0.03814 0.03829 = 0.03413 0.00540 -0.00300 0.00588 AFIX 43 H12 2 0.041871 0.528419 0.111386 11.00000 -1.20000 AFIX 0 C4 1 0.538758 0.391003 0.612324 11.00000 0.02539 0.03345 = 0.03127 0.00120 0.00035 -0.00105 AFIX 43 H4 2 0.634338 0.364590 0.640147 11.00000 -1.20000 AFIX 0 C18 1 0.056776 0.200837 0.172320 11.00000 0.03491 0.04047 = 0.02759 -0.00646 -0.00018 -0.00043 AFIX 43 H18 2 -0.008891 0.206674 0.104086 11.00000 -1.20000 AFIX 0 C5 1 0.512106 0.451207 0.656649 11.00000 0.03384 0.03463 = 0.03040 -0.00547 0.00057 -0.01017 AFIX 43 H5 2 0.587929 0.465914 0.716679 11.00000 -1.20000 AFIX 0 C11 1 0.268187 0.482136 0.081348 11.00000 0.05102 0.03899 = 0.02680 0.00421 0.00260 -0.00373 AFIX 43 H11 2 0.289269 0.505362 0.017212 11.00000 -1.20000 AFIX 0 HKLF 4 REM matrix_0m_a.res in P2(1)/c REM R1 = 0.0478 for 2521 Fo > 4sig(Fo) and 0.0671 for all 3317 data REM 253 parameters refined using 0 restraints END WGHT 0.0587 0.2748 REM Highest difference peak 0.345, deepest hole -0.247, 1-sigma level 0.055 Q1 1 -0.0320 0.3753 0.4927 11.00000 0.05 0.35 Q2 1 -0.0534 0.4217 0.3928 11.00000 0.05 0.30 Q3 1 -0.0972 0.3765 0.3337 11.00000 0.05 0.27 Q4 1 -0.1999 0.3933 0.4147 11.00000 0.05 0.27 Q5 1 0.5307 0.3894 0.5419 11.00000 0.05 0.24 Q6 1 0.2108 0.4006 0.3335 11.00000 0.05 0.24 Q7 1 0.2388 0.3415 0.3712 11.00000 0.05 0.23 Q8 1 0.2597 0.3979 0.4260 11.00000 0.05 0.22 Q9 1 0.1133 0.2540 0.2954 11.00000 0.05 0.21 Q10 1 0.5350 0.2568 0.4248 11.00000 0.05 0.20 Q11 1 0.7212 0.1574 0.5647 11.00000 0.05 0.20 Q12 1 0.0642 0.3904 0.3824 11.00000 0.05 0.20 Q13 1 0.2877 0.4004 0.1492 11.00000 0.05 0.20 Q14 1 0.6214 0.2669 0.5586 11.00000 0.05 0.20 Q15 1 0.6661 0.3944 0.4952 11.00000 0.05 0.19 Q16 1 0.2334 0.2563 0.2537 11.00000 0.05 0.19 Q17 1 0.3614 0.3047 0.4268 11.00000 0.05 0.19 Q18 1 0.6671 0.3515 0.4609 11.00000 0.05 0.18 Q19 1 0.3623 0.1642 0.5465 11.00000 0.05 0.18 Q20 1 -0.0123 0.3344 0.3816 11.00000 0.05 0.18 ; _shelx_res_checksum 59680 _shelx_hkl_file ; -1 0 0 1.08 0.34 1 0 0 -0.03 0.29 -1 0 0 1.69 0.39 -2 0 0 73.29 2.13 2 0 0 80.42 3.21 -2 0 0 74.04 2.17 -3 0 0 1.74 0.64 3 0 0 -0.06 0.76 -3 0 0 1.33 0.66 4 0 0 2.26 1.31 -4 0 0 1.66 0.69 5 0 0 -0.92 1.04 6 0 0 89.22 4.01 7 0 0 15.43 1.97 8 0 0 26.63 2.15 9 0 0 9.71 1.05 0 1 0 -0.08 0.09 0 1 0 -0.11 0.12 0 1 0 -0.04 0.12 -1 -1 0 196.58 3.00 -1 -1 0 195.26 2.36 1 1 0 183.21 3.73 -1 1 0 197.09 2.41 -1 1 0 196.65 3.09 -2 -1 0 53.41 1.99 -2 -1 0 49.98 1.57 -2 1 0 50.74 1.99 -2 1 0 50.24 1.65 2 1 0 51.58 2.65 -3 -1 0 42.93 2.11 -3 -1 0 43.94 1.78 3 -1 0 48.69 3.51 -3 1 0 44.27 1.86 -3 1 0 49.50 2.21 3 1 0 45.67 3.15 -4 -1 0 2.61 0.85 4 -1 0 1.42 1.23 -4 1 0 2.13 0.86 -4 1 0 2.61 0.76 4 1 0 1.93 1.27 -5 -1 0 2.63 0.98 5 -1 0 3.62 1.62 5 1 0 2.88 1.48 6 -1 0 0.92 0.87 6 1 0 1.18 0.83 7 -1 0 32.58 2.59 7 1 0 36.41 2.70 8 -1 0 0.71 0.74 8 1 0 0.99 0.78 9 -1 0 0.72 0.49 9 1 0 0.60 0.48 0 2 0 108.54 2.20 0 2 0 103.20 1.47 0 2 0 103.82 1.77 -1 -2 0 0.63 0.71 -1 -2 0 -0.13 0.22 1 -2 0 -0.01 0.35 -1 2 0 0.10 0.17 -1 2 0 -0.28 0.42 1 2 0 0.36 0.44 -2 -2 0 6.06 0.64 -2 -2 0 6.62 0.96 -2 2 0 5.31 0.68 -2 2 0 5.41 0.94 2 2 0 5.92 1.11 -3 -2 0 10.07 1.31 -3 -2 0 9.65 0.90 3 2 0 10.62 1.88 -3 2 0 10.30 0.98 -3 2 0 6.89 1.17 4 -2 0 1.19 1.37 -4 -2 0 2.55 0.86 4 2 0 2.59 1.22 -4 2 0 1.70 0.88 5 -2 0 21.20 3.46 -5 -2 0 23.32 2.13 5 2 0 21.30 3.44 6 -2 0 6.79 1.37 6 2 0 5.95 1.33 7 -2 0 0.29 0.75 7 2 0 1.23 0.87 8 -2 0 13.11 1.65 8 2 0 11.44 1.63 9 -2 0 4.29 0.85 9 2 0 4.79 0.87 0 3 0 -0.01 0.24 0 3 0 0.24 0.36 0 3 0 0.02 0.34 -1 -3 0 398.94 5.97 1 -3 0 413.81 6.51 -1 -3 0 403.05 4.15 -1 3 0 397.84 5.77 1 3 0 409.63 6.68 -2 -3 0 351.75 5.94 -2 3 0 350.23 4.06 -2 3 0 364.70 6.20 2 3 0 366.26 7.57 -3 -3 0 22.00 1.76 -3 3 0 20.16 1.15 3 3 0 17.19 2.22 -3 3 0 16.71 1.68 4 -3 0 39.22 4.06 -4 -3 0 28.23 2.13 4 3 0 33.59 3.33 -4 3 0 28.68 2.22 5 -3 0 31.31 3.91 -5 -3 0 40.27 2.74 5 3 0 38.38 4.06 6 -3 0 1.21 0.86 6 3 0 1.89 0.93 7 -3 0 1.78 0.93 7 3 0 1.08 0.91 8 -3 0 -0.19 0.61 8 3 0 -0.17 0.61 9 -3 0 5.58 0.87 9 3 0 5.37 0.87 0 4 0 1.98 0.57 0 4 0 1.10 0.58 -1 -4 0 171.30 3.44 -1 -4 0 167.21 3.75 1 -4 0 163.49 4.02 -1 4 0 168.47 3.72 1 4 0 160.67 4.08 1 4 0 165.06 2.29 2 -4 0 31.34 2.46 -2 -4 0 30.36 1.88 2 4 0 28.51 2.30 -2 4 0 32.93 2.02 -3 -4 0 1.20 0.67 3 -4 0 -0.90 0.75 -3 4 0 0.63 0.78 3 4 0 0.04 0.83 -4 -4 0 6.87 1.30 4 -4 0 5.09 1.90 4 4 0 4.59 1.53 -4 4 0 6.98 1.43 5 -4 0 0.37 1.38 -5 -4 0 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0.48 1 10 0 0.42 0.49 1 10 0 0.90 0.74 -1 10 0 0.04 0.63 -2 -10 0 46.56 2.65 2 -10 0 43.37 3.26 -2 10 0 52.34 3.05 2 10 0 50.04 3.49 -3 -10 0 46.50 2.97 3 -10 0 35.08 3.64 3 10 0 46.12 3.70 -3 10 0 39.10 2.94 -4 -10 0 6.41 1.47 4 10 0 9.72 2.19 -4 10 0 9.87 1.95 5 -10 0 0.74 0.64 5 10 0 0.42 0.78 5 10 0 0.13 0.66 -5 10 0 0.67 0.54 6 -10 0 -0.83 0.53 6 10 0 1.10 0.75 -6 10 0 0.98 0.59 6 10 0 0.63 0.78 7 -10 0 1.87 0.80 7 10 0 3.11 0.81 7 10 0 2.37 0.97 8 -10 0 -0.28 0.48 8 10 0 0.65 0.52 0 11 0 0.34 0.60 0 11 0 0.42 0.67 -1 -11 0 34.08 2.05 1 -11 0 38.63 3.09 1 11 0 30.39 2.76 -1 11 0 31.04 2.33 2 -11 0 39.56 3.26 -2 -11 0 42.39 2.59 2 11 0 37.57 3.18 -2 11 0 40.37 2.81 3 -11 0 5.61 1.76 -3 -11 0 7.33 1.45 3 11 0 5.59 1.58 -3 11 0 5.99 1.53 4 -11 0 0.67 1.27 -4 -11 0 6.44 1.63 -4 11 0 8.44 1.88 4 11 0 7.03 1.96 5 -11 0 2.69 0.89 5 11 0 1.58 0.89 -5 11 0 -5.25 1.77 5 11 0 2.96 0.93 -5 11 0 1.67 0.63 6 -11 0 7.83 1.41 -6 11 0 9.51 1.08 6 11 0 9.06 1.43 6 11 0 9.37 1.68 7 -11 0 0.36 0.65 7 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2.68 0.40 -1 0 14 18.13 1.12 1 0 -14 17.60 1.23 0 0 14 0.22 0.43 0 0 -14 -0.25 0.46 1 0 14 0.16 0.38 -1 0 -14 0.30 0.46 2 0 14 3.39 0.55 -2 0 -14 3.35 0.58 -2 -1 14 0.00 0.36 1 -1 -14 1.76 0.60 -1 -1 14 2.49 0.57 1 1 -14 1.58 0.57 -1 1 14 1.64 0.50 0 -1 14 3.92 0.68 0 -1 -14 3.11 0.70 0 1 14 3.65 0.66 0 1 -14 4.14 0.72 -1 -1 -14 2.32 0.61 1 -1 14 2.42 0.53 1 1 14 2.63 0.57 -1 1 -14 2.41 0.62 -2 -1 -14 0.38 0.41 2 -1 14 0.34 0.34 -2 1 -14 -0.38 0.32 2 1 14 -0.78 0.25 -2 -2 14 -0.50 0.34 1 -2 -14 0.13 0.50 -1 -2 14 -0.07 0.39 -1 2 14 0.45 0.44 0 -2 14 2.79 0.59 0 -2 -14 3.01 0.70 0 2 -14 2.32 0.64 0 2 14 3.53 0.62 -1 -2 -14 2.24 0.62 1 -2 14 2.21 0.51 -1 2 -14 3.01 0.61 1 2 14 2.08 0.53 -2 -2 -14 1.25 0.45 2 -2 14 0.75 0.39 -2 2 -14 0.30 0.34 2 2 14 1.03 0.39 -2 -3 14 0.07 0.38 -1 -3 14 10.95 0.95 0 -3 -14 1.03 0.54 0 -3 14 2.72 0.58 0 3 14 2.37 0.54 0 3 -14 0.92 0.49 -1 -3 -14 1.06 0.51 1 -3 14 0.95 0.45 1 3 14 0.92 0.43 -1 3 -14 1.02 0.48 -2 -3 -14 2.79 0.56 2 -3 14 2.95 0.52 -2 3 -14 3.30 0.53 2 3 14 3.34 0.54 -3 -4 14 23.37 1.00 -2 -4 14 1.78 0.48 -1 -4 14 3.32 0.63 0 -4 -14 0.32 0.49 0 -4 14 0.60 0.44 0 4 14 -0.06 0.36 0 4 -14 0.27 0.43 1 -4 14 1.37 0.46 -1 -4 -14 1.04 0.50 -1 4 -14 1.48 0.44 1 4 14 1.61 0.44 -2 -4 -14 0.49 0.39 2 -4 14 1.14 0.40 2 4 14 1.18 0.37 -2 4 -14 0.59 0.34 -3 -5 14 0.17 0.32 -2 -5 14 4.40 0.68 -2 5 14 5.01 0.55 -1 -5 14 7.04 0.80 -1 5 14 7.74 0.70 0 -5 14 4.62 0.68 0 5 14 1.93 0.48 -1 -5 -14 3.96 0.65 1 -5 14 5.56 0.70 -1 5 -14 4.44 0.63 1 5 14 4.03 0.56 -2 -5 -14 10.02 0.80 2 -5 14 10.00 0.71 2 5 14 8.62 0.66 -2 5 -14 8.87 0.68 -3 -6 14 12.81 0.78 -2 -6 14 0.09 0.36 -2 6 14 0.06 0.27 -1 -6 14 9.10 0.83 -1 6 14 8.80 0.73 0 -6 14 1.48 0.45 -1 -6 -14 0.37 0.42 1 -6 14 1.26 0.42 1 6 14 1.04 0.37 -1 6 -14 1.38 0.39 -2 -6 -14 -0.14 0.34 2 6 14 -0.32 0.29 -2 6 -14 0.17 0.30 -2 -7 14 3.43 0.56 -2 7 14 4.80 0.53 -1 -7 14 2.88 0.56 -1 7 14 2.18 0.44 0 -7 14 11.88 0.85 -1 -7 -14 1.08 0.44 1 -7 14 0.48 0.35 -2 -8 14 2.31 0.47 -2 8 14 3.64 0.46 -1 -8 14 11.58 0.83 -1 8 14 10.75 0.71 0 -8 14 2.68 0.46 1 -8 14 0.06 0.28 -1 -8 -14 0.43 0.38 -2 -9 14 3.63 0.55 -1 -9 14 1.87 0.41 -1 9 14 1.58 0.35 0 -9 14 1.75 0.38 -1 -10 14 0.15 0.29 -1 10 14 0.30 0.26 0 0 15 -0.47 0.28 0 -1 15 6.62 0.61 0 -2 -15 5.11 0.71 0 -2 15 5.44 0.55 0 -3 15 1.45 0.36 0 -4 15 1.25 0.36 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55416 #===END data_MM1531_0m_a _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H19 B F6 N2 O4 S2 ' _chemical_formula_sum 'C54 H38 B2 F12 N4 O8 S4' _chemical_formula_weight 1248.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0900(3) _cell_length_b 15.4860(4) _cell_length_c 18.2577(5) _cell_angle_alpha 75.063(2) _cell_angle_beta 80.627(2) _cell_angle_gamma 89.752(2) _cell_volume 2717.51(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6132 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 70.02 _exptl_crystal_description 'block' _exptl_crystal_colour 'Yellow' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_F_000 1272 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 2.498 _shelx_estimated_absorpt_T_min 0.635 _shelx_estimated_absorpt_T_max 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6385 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17539 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.540 _diffrn_reflns_theta_max 64.483 _diffrn_reflns_theta_full 64.500 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measured_fraction_theta_full 0.960 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_Laue_measured_fraction_full 0.960 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_point_group_measured_fraction_full 0.960 _reflns_number_total 8769 _reflns_number_gt 6196 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.4.9' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1562P)^2^+2.1471P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8769 _refine_ls_number_parameters 943 _refine_ls_number_restraints 399 _refine_ls_R_factor_all 0.1091 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2509 _refine_ls_wR_factor_gt 0.2189 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.7814(5) 0.5728(4) 0.2200(3) 0.0427(11) Uani 1 1 d . . . . . B2 B 0.2701(5) 0.1010(3) 0.2284(3) 0.0413(10) Uani 1 1 d . . . . . C1 C 0.6922(4) 0.6548(3) 0.2357(2) 0.0390(9) Uani 1 1 d . . . . . C2 C 0.6751(4) 0.6507(3) 0.3118(2) 0.0413(9) Uani 1 1 d . . . . . C3 C 0.7276(4) 0.5687(3) 0.3550(2) 0.0399(9) Uani 1 1 d . . . . . C4 C 0.7281(5) 0.5358(3) 0.4334(3) 0.0480(10) Uani 1 1 d . . . . . H4 H 0.6901 0.5690 0.4682 0.058 Uiso 1 1 calc R U . . . C5 C 0.7838(5) 0.4551(4) 0.4605(3) 0.0514(11) Uani 1 1 d . . . . . H5 H 0.7835 0.4323 0.5141 0.062 Uiso 1 1 calc R U . . . C6 C 0.8412(5) 0.4062(3) 0.4093(3) 0.0528(11) Uani 1 1 d . . . . . H6 H 0.8794 0.3502 0.4276 0.063 Uiso 1 1 calc R U . . . C7 C 0.8409(5) 0.4411(3) 0.3323(3) 0.0469(10) Uani 1 1 d . . . . . H7 H 0.8810 0.4095 0.2966 0.056 Uiso 1 1 calc R U . . . C8 C 0.9295(5) 0.5958(3) 0.1730(3) 0.0504(11) Uani 1 1 d . . . . . C9 C 1.0105(6) 0.6567(4) 0.1902(4) 0.0675(15) Uani 1 1 d . . . . . H9 H 0.9754 0.6843 0.2297 0.081 Uiso 1 1 calc R U . . . C10 C 1.1414(7) 0.6793(5) 0.1521(5) 0.087(2) Uani 1 1 d . . . . . H10 H 1.1955 0.7207 0.1659 0.104 Uiso 1 1 calc R U . . . C11 C 1.1909(8) 0.6403(7) 0.0939(5) 0.111(4) Uani 1 1 d . . . . . H11 H 1.2793 0.6561 0.0662 0.133 Uiso 1 1 calc R U . . . C12 C 1.1140(10) 0.5793(8) 0.0757(5) 0.114(4) Uani 1 1 d . . . . . H12 H 1.1496 0.5530 0.0354 0.137 Uiso 1 1 calc R U . . . C13 C 0.9849(7) 0.5551(5) 0.1149(4) 0.0801(19) Uani 1 1 d . . . . . H13 H 0.9336 0.5111 0.1027 0.096 Uiso 1 1 calc R U . . . C14 C 0.6399(4) 0.7219(3) 0.1755(2) 0.0409(9) Uani 1 1 d . . . . . C15 C 0.5156(5) 0.7583(3) 0.1900(3) 0.0500(11) Uani 1 1 d . . . . . H15 H 0.4650 0.7418 0.2406 0.060 Uiso 1 1 calc R U . . . C16 C 0.4641(5) 0.8180(4) 0.1323(3) 0.0551(12) Uani 1 1 d . . . . . H16 H 0.3780 0.8413 0.1432 0.066 Uiso 1 1 calc R U . . . C17 C 0.5372(5) 0.8442(4) 0.0586(3) 0.0564(12) Uani 1 1 d . . . . . H17 H 0.5031 0.8868 0.0193 0.068 Uiso 1 1 calc R U . . . C18 C 0.6607(6) 0.8075(4) 0.0429(3) 0.0601(13) Uani 1 1 d . . . . . H18 H 0.7108 0.8240 -0.0077 0.072 Uiso 1 1 calc R U . . . C19 C 0.7110(5) 0.7473(3) 0.1003(3) 0.0503(11) Uani 1 1 d . . . . . H19 H 0.7957 0.7226 0.0887 0.060 Uiso 1 1 calc R U . . . C20 C 0.6151(5) 0.7183(3) 0.3509(3) 0.0439(9) Uani 1 1 d . . . . . C21 C 0.5097(5) 0.6951(4) 0.4138(3) 0.0559(12) Uani 1 1 d . . . . . H21 H 0.4768 0.6348 0.4333 0.067 Uiso 1 1 calc R U . . . C22 C 0.4538(6) 0.7607(5) 0.4475(3) 0.0691(15) Uani 1 1 d . . . . . H22 H 0.3826 0.7447 0.4902 0.083 Uiso 1 1 calc R U . . . C23 C 0.4996(7) 0.8472(5) 0.4204(3) 0.0694(16) Uani 1 1 d . . . . . H23 H 0.4592 0.8916 0.4432 0.083 Uiso 1 1 calc R U . . . C24 C 0.6047(7) 0.8707(4) 0.3595(3) 0.0660(15) Uani 1 1 d . . . . . H24 H 0.6376 0.9311 0.3411 0.079 Uiso 1 1 calc R U . . . C25 C 0.6629(5) 0.8063(4) 0.3250(3) 0.0544(11) Uani 1 1 d . . . . . H25 H 0.7358 0.8228 0.2834 0.065 Uiso 1 1 calc R U . . . C26 C 0.5275(7) 0.4921(6) 0.1073(4) 0.081(2) Uani 1 1 d . . . . . C27 C 0.1873(4) 0.0088(3) 0.2430(2) 0.0407(9) Uani 1 1 d . . . . . C28 C 0.1707(4) -0.0347(3) 0.3190(2) 0.0397(9) Uani 1 1 d . . . . . C29 C 0.2213(4) 0.0216(3) 0.3628(2) 0.0410(9) Uani 1 1 d . . . . . C30 C 0.2237(5) 0.0049(3) 0.4414(3) 0.0473(10) Uani 1 1 d . . . . . H30 H 0.1883 -0.0502 0.4757 0.057 Uiso 1 1 calc R U . . . C31 C 0.2782(5) 0.0696(4) 0.4686(3) 0.0543(12) Uani 1 1 d . . . . . H31 H 0.2794 0.0593 0.5221 0.065 Uiso 1 1 calc R U . . . C32 C 0.3312(5) 0.1495(4) 0.4183(3) 0.0518(11) Uani 1 1 d . . . . . H32 H 0.3688 0.1942 0.4368 0.062 Uiso 1 1 calc R U . . . C33 C 0.3283(4) 0.1627(3) 0.3419(3) 0.0451(10) Uani 1 1 d . . . . . H33 H 0.3660 0.2167 0.3067 0.054 Uiso 1 1 calc R U . . . C34 C 0.4205(4) 0.1115(3) 0.1826(2) 0.0445(10) Uani 1 1 d . . . . . C35 C 0.5009(5) 0.0383(4) 0.1902(3) 0.0586(12) Uani 1 1 d . . . . . H35 H 0.4640 -0.0185 0.2205 0.070 Uiso 1 1 calc R U . . . C36 C 0.6342(6) 0.0458(6) 0.1547(4) 0.081(2) Uani 1 1 d . . . . . H36 H 0.6869 -0.0058 0.1599 0.097 Uiso 1 1 calc R U . . . C37 C 0.6900(6) 0.1270(6) 0.1124(4) 0.083(2) Uani 1 1 d . . . . . H37 H 0.7817 0.1326 0.0887 0.100 Uiso 1 1 calc R U . . . C38 C 0.6128(7) 0.1997(5) 0.1045(4) 0.0778(19) Uani 1 1 d . . . . . H38 H 0.6522 0.2561 0.0750 0.093 Uiso 1 1 calc R U . . . C39 C 0.4787(6) 0.1945(4) 0.1381(3) 0.0589(13) Uani 1 1 d . . . . . H39 H 0.4268 0.2464 0.1310 0.071 Uiso 1 1 calc R U . . . C40 C 0.1389(4) -0.0243(3) 0.1831(2) 0.0414(9) Uani 1 1 d . . . . . C41 C 0.2153(5) -0.0088(3) 0.1097(3) 0.0469(10) Uani 1 1 d . . . . . H41 H 0.2992 0.0235 0.0987 0.056 Uiso 1 1 calc R U . . . C42 C 0.1715(5) -0.0395(4) 0.0527(3) 0.0551(12) Uani 1 1 d . . . . . H42 H 0.2254 -0.0291 0.0033 0.066 Uiso 1 1 calc R U . . . C43 C 0.0492(6) -0.0853(4) 0.0680(3) 0.0564(12) Uani 1 1 d . . . . . H43 H 0.0191 -0.1070 0.0291 0.068 Uiso 1 1 calc R U . . . C44 C -0.0295(5) -0.0997(4) 0.1394(3) 0.0549(11) Uani 1 1 d . . . . . H44 H -0.1145 -0.1304 0.1494 0.066 Uiso 1 1 calc R U . . . C45 C 0.0147(5) -0.0697(3) 0.1968(3) 0.0493(10) Uani 1 1 d . . . . . H45 H -0.0401 -0.0801 0.2460 0.059 Uiso 1 1 calc R U . . . C46 C 0.1174(5) -0.1274(3) 0.3565(3) 0.0444(10) Uani 1 1 d . . . . . C47 C 0.1718(6) -0.1977(3) 0.3290(3) 0.0537(11) Uani 1 1 d . . . . . H47 H 0.2457 -0.1864 0.2879 0.064 Uiso 1 1 calc R U . . . C48 C 0.1193(7) -0.2840(4) 0.3609(4) 0.0675(15) Uani 1 1 d . . . . . H48 H 0.1573 -0.3314 0.3412 0.081 Uiso 1 1 calc R U . . . C49 C 0.0137(7) -0.3022(4) 0.4204(4) 0.0724(17) Uani 1 1 d . . . . . H49 H -0.0229 -0.3615 0.4413 0.087 Uiso 1 1 calc R U . . . C50 C -0.0403(6) -0.2323(4) 0.4503(4) 0.0737(17) Uani 1 1 d . . . . . H50 H -0.1127 -0.2446 0.4924 0.088 Uiso 1 1 calc R U . . . C51 C 0.0110(5) -0.1458(4) 0.4190(3) 0.0581(13) Uani 1 1 d . . . . . H51 H -0.0256 -0.0988 0.4396 0.070 Uiso 1 1 calc R U . . . F1 F 0.5238(5) 0.5791(3) 0.0819(3) 0.1002(14) Uani 1 1 d . . . . . F2 F 0.6130(5) 0.4622(5) 0.0598(3) 0.125(2) Uani 1 1 d . . . . . F3 F 0.4082(5) 0.4540(4) 0.1129(3) 0.1041(15) Uani 1 1 d . . . . . N1 N 0.7845(3) 0.5195(2) 0.3067(2) 0.0401(8) Uani 1 1 d . . . . . N2 N 0.2728(3) 0.1004(3) 0.3155(2) 0.0408(8) Uani 1 1 d . . . . . N3 N 0.4797(6) 0.5095(4) 0.2488(3) 0.0743(14) Uani 1 1 d . . . . . N4 N -0.0468(5) 0.1456(3) 0.2446(3) 0.0623(11) Uani 1 1 d D . . . . O1 O 0.7117(4) 0.5091(3) 0.1824(2) 0.0557(8) Uani 1 1 d . . . . . O5 O 0.1961(3) 0.1864(2) 0.19245(19) 0.0518(8) Uani 1 1 d . . . . . S1 S 0.57815(15) 0.46149(9) 0.20235(7) 0.0588(4) Uani 1 1 d D . . . . C53 C -0.2692(5) 0.1761(4) 0.3338(3) 0.0595(13) Uani 1 1 d D . . . . S5A S 0.3941(5) 0.4875(6) 0.3308(4) 0.0780(17) Uani 0.533(8) 1 d D . P A 1 O4A O 0.4608(11) 0.4198(9) 0.3802(6) 0.103(3) Uani 0.533(8) 1 d D U P A 1 O3A O 0.3470(13) 0.5632(10) 0.3532(7) 0.104(3) Uani 0.533(8) 1 d . U P A 1 C27A C 0.2481(15) 0.4234(10) 0.3067(9) 0.063(3) Uani 0.533(8) 1 d . U P A 1 F5A F 0.2757(9) 0.3740(6) 0.2589(6) 0.092(2) Uani 0.533(8) 1 d . U P A 1 F4A F 0.1756(18) 0.4780(12) 0.2751(11) 0.087(3) Uani 0.533(8) 1 d . U P A 1 F6A F 0.1771(9) 0.3710(7) 0.3714(6) 0.090(2) Uani 0.533(8) 1 d . U P A 1 F4B F 0.1645(11) 0.4182(10) 0.4009(7) 0.110(4) Uani 0.467(8) 1 d . U P A 2 F6B F 0.186(2) 0.4981(14) 0.2905(13) 0.105(5) Uani 0.467(8) 1 d . U P A 2 F5B F 0.2572(13) 0.3613(9) 0.3147(10) 0.117(3) Uani 0.467(8) 1 d . U P A 2 C27B C 0.2348(16) 0.4342(10) 0.3349(9) 0.061(3) Uani 0.467(8) 1 d . U P A 2 O3B O 0.3906(15) 0.5064(11) 0.3818(8) 0.099(3) Uani 0.467(8) 1 d . U P A 2 O4B O 0.4630(11) 0.3596(6) 0.3658(6) 0.088(3) Uani 0.467(8) 1 d D U P A 2 S5B S 0.4105(7) 0.4458(4) 0.3362(4) 0.0626(15) Uani 0.467(8) 1 d D . P A 2 O7A O -0.0433(6) 0.1292(6) 0.3837(3) 0.0753(19) Uani 0.664(9) 1 d D U P B 1 S4A S -0.1186(3) 0.1079(2) 0.33050(13) 0.0465(8) Uani 0.664(9) 1 d D U P B 1 O8A O -0.1687(7) 0.0185(3) 0.3407(4) 0.0693(18) Uani 0.664(9) 1 d D U P B 1 O7B O -0.045(2) 0.1859(14) 0.3820(10) 0.109(5) Uani 0.336(9) 1 d D U P B 2 O8B O -0.1103(17) 0.0497(7) 0.3623(9) 0.080(3) Uani 0.336(9) 1 d D U P B 2 S4B S -0.0960(7) 0.1445(6) 0.3302(3) 0.0738(18) Uani 0.336(9) 1 d D U P B 2 F10A F -0.3364(5) 0.1648(5) 0.2823(4) 0.0748(17) Uani 0.688(16) 1 d D U P B 1 F11A F -0.3445(6) 0.1372(6) 0.4048(3) 0.079(2) Uani 0.688(16) 1 d D U P B 1 F12A F -0.2459(7) 0.2583(4) 0.3300(6) 0.090(2) Uani 0.688(16) 1 d D U P B 1 F11B F -0.3139(14) 0.1782(13) 0.4002(7) 0.088(3) Uani 0.312(16) 1 d D U P B 2 F12B F -0.2443(12) 0.2626(7) 0.2901(11) 0.087(3) Uani 0.312(16) 1 d D U P B 2 F10B F -0.3534(8) 0.1431(9) 0.3015(9) 0.082(3) Uani 0.312(16) 1 d D U P B 2 O2A O 0.597(3) 0.3682(7) 0.2129(16) 0.083(4) Uani 0.67(6) 1 d D U P C 1 O2B O 0.560(4) 0.3686(13) 0.239(3) 0.083(5) Uani 0.33(6) 1 d D U P C 2 S3A S 0.06064(15) 0.22125(12) 0.21214(9) 0.0483(5) Uani 0.819(5) 1 d . U P B 1 O6A O 0.0598(6) 0.2934(4) 0.2473(4) 0.0843(17) Uani 0.819(5) 1 d . U P B 1 S3B S 0.0488(7) 0.1845(5) 0.1828(6) 0.0550(19) Uani 0.181(5) 1 d D U P B 2 O6B O -0.041(2) 0.1216(15) 0.1812(17) 0.086(8) Uani 0.181(5) 1 d D U P B 2 C52A C 0.0274(5) 0.2701(3) 0.1138(4) 0.0648(18) Uani 0.834(7) 1 d D U P B 1 F9A F -0.0904(6) 0.3075(7) 0.1190(4) 0.090(2) Uani 0.834(7) 1 d D U P B 1 F8A F 0.0302(5) 0.2059(4) 0.0778(2) 0.0899(16) Uani 0.834(7) 1 d D U P B 1 F7A F 0.1210(5) 0.3338(4) 0.0792(3) 0.0965(19) Uani 0.834(7) 1 d D U P B 1 F9B F -0.085(3) 0.323(4) 0.143(2) 0.085(7) Uani 0.166(7) 1 d D U P B 2 F7B F 0.124(3) 0.3592(15) 0.1458(17) 0.101(6) Uani 0.166(7) 1 d D U P B 2 F8B F 0.078(3) 0.289(2) 0.0632(13) 0.093(4) Uani 0.166(7) 1 d D U P B 2 C52B C 0.042(3) 0.300(2) 0.1330(15) 0.058(3) Uani 0.166(7) 1 d D U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.041(3) 0.052(3) 0.035(2) -0.011(2) -0.0084(19) 0.006(2) B2 0.038(3) 0.048(3) 0.036(2) -0.0056(19) -0.0093(18) 0.0022(19) C1 0.028(2) 0.050(2) 0.039(2) -0.0115(17) -0.0038(15) 0.0009(16) C2 0.031(2) 0.054(2) 0.038(2) -0.0126(18) -0.0037(15) -0.0014(17) C3 0.027(2) 0.048(2) 0.043(2) -0.0108(18) -0.0043(15) -0.0040(16) C4 0.040(2) 0.066(3) 0.036(2) -0.012(2) -0.0037(17) -0.002(2) C5 0.041(2) 0.066(3) 0.039(2) 0.001(2) -0.0075(18) 0.002(2) C6 0.045(3) 0.053(3) 0.053(3) -0.001(2) -0.008(2) 0.003(2) C7 0.039(2) 0.050(2) 0.051(2) -0.011(2) -0.0068(18) 0.0050(18) C8 0.044(3) 0.060(3) 0.038(2) -0.0003(19) 0.0003(18) 0.016(2) C9 0.041(3) 0.075(4) 0.077(4) -0.010(3) 0.001(2) 0.001(2) C10 0.047(3) 0.090(5) 0.104(5) 0.003(4) -0.001(3) 0.006(3) C11 0.060(5) 0.137(8) 0.087(5) 0.033(5) 0.026(4) 0.024(5) C12 0.096(7) 0.157(9) 0.068(4) -0.019(5) 0.028(4) 0.047(6) C13 0.072(4) 0.106(5) 0.059(3) -0.028(3) 0.007(3) 0.022(4) C14 0.040(2) 0.041(2) 0.042(2) -0.0104(17) -0.0075(17) 0.0023(17) C15 0.044(3) 0.062(3) 0.043(2) -0.013(2) -0.0061(18) 0.007(2) C16 0.046(3) 0.061(3) 0.057(3) -0.011(2) -0.013(2) 0.012(2) C17 0.056(3) 0.055(3) 0.054(3) -0.001(2) -0.018(2) 0.009(2) C18 0.054(3) 0.072(3) 0.045(2) -0.001(2) -0.003(2) 0.005(2) C19 0.044(3) 0.059(3) 0.044(2) -0.008(2) -0.0044(18) 0.011(2) C20 0.040(2) 0.054(3) 0.041(2) -0.0155(19) -0.0090(17) 0.0092(18) C21 0.047(3) 0.070(3) 0.051(3) -0.022(2) 0.000(2) 0.003(2) C22 0.058(3) 0.095(5) 0.058(3) -0.033(3) -0.003(2) 0.012(3) C23 0.077(4) 0.088(4) 0.060(3) -0.041(3) -0.026(3) 0.034(3) C24 0.093(4) 0.051(3) 0.065(3) -0.022(2) -0.032(3) 0.012(3) C25 0.057(3) 0.060(3) 0.048(3) -0.017(2) -0.010(2) 0.001(2) C26 0.065(4) 0.128(6) 0.064(4) -0.043(4) -0.025(3) 0.017(4) C27 0.030(2) 0.049(2) 0.039(2) -0.0031(17) -0.0047(15) 0.0007(16) C28 0.029(2) 0.046(2) 0.040(2) -0.0052(17) -0.0044(15) 0.0048(16) C29 0.031(2) 0.051(2) 0.038(2) -0.0074(18) -0.0034(15) 0.0087(17) C30 0.042(2) 0.059(3) 0.038(2) -0.0094(19) -0.0033(17) 0.0065(19) C31 0.045(3) 0.081(3) 0.039(2) -0.020(2) -0.0069(18) 0.010(2) C32 0.040(2) 0.065(3) 0.056(3) -0.027(2) -0.0085(19) 0.005(2) C33 0.036(2) 0.050(2) 0.050(2) -0.0134(19) -0.0076(17) 0.0034(18) C34 0.036(2) 0.062(3) 0.035(2) -0.0124(19) -0.0058(16) -0.0041(19) C35 0.040(3) 0.072(3) 0.067(3) -0.027(3) -0.006(2) 0.004(2) C36 0.041(3) 0.124(6) 0.092(4) -0.059(4) -0.004(3) 0.007(3) C37 0.040(3) 0.152(7) 0.068(4) -0.062(4) 0.015(3) -0.028(4) C38 0.057(4) 0.108(5) 0.059(3) -0.017(3) 0.010(3) -0.032(4) C39 0.052(3) 0.071(3) 0.048(3) -0.005(2) -0.007(2) -0.014(2) C40 0.040(2) 0.041(2) 0.040(2) -0.0028(17) -0.0114(17) 0.0007(17) C41 0.040(2) 0.053(3) 0.044(2) -0.0030(19) -0.0101(17) -0.0001(18) C42 0.059(3) 0.068(3) 0.037(2) -0.011(2) -0.008(2) 0.000(2) C43 0.061(3) 0.064(3) 0.049(3) -0.015(2) -0.023(2) 0.002(2) C44 0.048(3) 0.061(3) 0.058(3) -0.015(2) -0.016(2) -0.006(2) C45 0.043(3) 0.061(3) 0.042(2) -0.010(2) -0.0076(18) -0.004(2) C46 0.039(2) 0.049(2) 0.041(2) -0.0023(18) -0.0098(17) 0.0002(18) C47 0.058(3) 0.052(3) 0.048(2) -0.011(2) -0.007(2) 0.002(2) C48 0.088(4) 0.049(3) 0.067(3) -0.008(2) -0.029(3) 0.003(3) C49 0.074(4) 0.054(3) 0.079(4) 0.014(3) -0.034(3) -0.017(3) C50 0.048(3) 0.071(4) 0.076(4) 0.021(3) 0.000(3) -0.006(3) C51 0.047(3) 0.056(3) 0.054(3) 0.010(2) 0.001(2) 0.006(2) F1 0.102(3) 0.109(3) 0.080(3) 0.007(2) -0.039(2) 0.006(3) F2 0.091(3) 0.232(7) 0.085(3) -0.100(4) -0.019(2) 0.028(4) F3 0.078(3) 0.160(4) 0.094(3) -0.054(3) -0.038(2) -0.005(3) N1 0.0338(18) 0.0472(19) 0.0374(18) -0.0078(15) -0.0062(13) 0.0010(14) N2 0.0327(18) 0.052(2) 0.0370(18) -0.0110(15) -0.0048(13) 0.0065(15) N3 0.080(4) 0.073(3) 0.068(3) -0.028(2) 0.009(2) -0.024(3) N4 0.063(3) 0.058(3) 0.062(3) -0.012(2) -0.005(2) 0.006(2) O1 0.056(2) 0.068(2) 0.0539(19) -0.0294(17) -0.0200(15) 0.0137(16) O5 0.0432(18) 0.0509(18) 0.0542(18) 0.0019(14) -0.0122(14) -0.0015(14) S1 0.0719(9) 0.0584(7) 0.0520(7) -0.0163(5) -0.0247(6) 0.0025(6) C53 0.045(3) 0.081(4) 0.064(3) -0.035(3) -0.016(2) 0.021(2) S5A 0.0435(19) 0.135(5) 0.053(2) -0.023(3) -0.0024(13) -0.025(3) O4A 0.075(5) 0.137(6) 0.077(5) 0.007(5) -0.015(4) -0.004(5) O3A 0.096(6) 0.131(7) 0.093(6) -0.064(5) 0.021(4) -0.012(5) C27A 0.059(4) 0.059(4) 0.068(5) -0.011(4) -0.007(4) 0.002(3) F5A 0.083(5) 0.103(5) 0.092(5) -0.025(4) -0.024(4) -0.025(4) F4A 0.067(4) 0.095(7) 0.101(6) -0.008(5) -0.045(4) -0.005(4) F6A 0.072(4) 0.094(5) 0.085(5) 0.004(4) 0.001(4) -0.028(4) F4B 0.076(6) 0.145(9) 0.088(6) -0.004(6) 0.004(5) -0.037(6) F6B 0.085(8) 0.107(10) 0.110(9) -0.004(7) -0.015(7) 0.029(7) F5B 0.101(6) 0.101(6) 0.145(7) -0.028(6) -0.015(6) -0.014(5) C27B 0.059(4) 0.060(4) 0.063(5) -0.015(4) -0.010(4) 0.002(3) O3B 0.103(6) 0.120(6) 0.073(5) -0.041(5) 0.013(4) -0.030(5) O4B 0.069(5) 0.102(6) 0.076(5) 0.009(5) -0.012(4) 0.001(5) S5B 0.058(3) 0.077(3) 0.047(2) -0.012(3) -0.0027(16) -0.020(2) O7A 0.062(3) 0.098(5) 0.062(3) -0.020(3) 0.000(3) 0.006(3) S4A 0.0374(11) 0.0500(18) 0.0445(10) -0.0015(10) -0.0022(7) 0.0051(10) O8A 0.057(4) 0.066(3) 0.069(4) -0.001(3) 0.007(3) 0.006(3) O7B 0.085(7) 0.118(8) 0.119(7) -0.013(7) -0.029(6) 0.007(7) O8B 0.078(6) 0.074(6) 0.069(5) 0.002(5) 0.006(5) 0.021(5) S4B 0.046(2) 0.069(3) 0.086(3) 0.017(2) -0.010(2) 0.009(2) F10A 0.068(3) 0.101(4) 0.062(3) -0.026(3) -0.023(2) 0.005(3) F11A 0.050(3) 0.113(5) 0.065(3) -0.021(3) 0.009(2) 0.011(3) F12A 0.097(4) 0.081(3) 0.107(5) -0.043(3) -0.028(3) 0.012(3) F11B 0.080(6) 0.106(6) 0.085(5) -0.051(5) 0.004(4) 0.010(5) F12B 0.083(5) 0.086(5) 0.099(6) -0.034(5) -0.020(5) 0.023(4) F10B 0.060(5) 0.111(6) 0.073(6) -0.024(5) -0.004(4) -0.004(5) O2A 0.098(11) 0.063(4) 0.102(11) -0.034(4) -0.033(8) 0.017(4) O2B 0.097(14) 0.053(6) 0.107(14) -0.024(8) -0.030(10) 0.030(8) S3A 0.0473(8) 0.0493(9) 0.0484(8) -0.0096(7) -0.0133(6) 0.0047(6) O6A 0.084(4) 0.079(3) 0.106(4) -0.055(3) -0.015(3) -0.007(3) S3B 0.047(3) 0.044(3) 0.079(3) -0.015(3) -0.027(2) 0.001(2) O6B 0.085(11) 0.091(11) 0.089(11) -0.035(9) -0.020(8) 0.006(8) C52A 0.055(3) 0.068(3) 0.062(3) 0.003(3) -0.015(3) 0.001(3) F9A 0.065(3) 0.114(5) 0.077(5) 0.009(4) -0.024(3) 0.026(3) F8A 0.070(3) 0.147(5) 0.055(2) -0.032(3) -0.0086(19) -0.012(3) F7A 0.069(3) 0.088(3) 0.095(3) 0.040(3) -0.012(3) -0.009(2) F9B 0.069(8) 0.104(10) 0.067(12) 0.004(10) -0.018(9) 0.037(8) F7B 0.079(9) 0.076(9) 0.109(10) 0.036(9) -0.006(9) -0.004(8) F8B 0.072(6) 0.119(6) 0.073(6) 0.003(6) -0.009(6) 0.005(6) C52B 0.054(4) 0.060(5) 0.057(5) -0.006(4) -0.012(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O1 1.565(6) . ? B1 C8 1.589(7) . ? B1 N1 1.590(6) . ? B1 C1 1.613(6) . ? B2 O5 1.563(6) . ? B2 N2 1.593(6) . ? B2 C34 1.595(6) . ? B2 C27 1.596(6) . ? C1 C2 1.357(6) . ? C1 C14 1.470(6) . ? C2 C3 1.459(6) . ? C2 C20 1.487(6) . ? C3 N1 1.365(6) . ? C3 C4 1.392(6) . ? C4 C5 1.374(7) . ? C4 H4 0.9500 . ? C5 C6 1.402(8) . ? C5 H5 0.9500 . ? C6 C7 1.371(7) . ? C6 H6 0.9500 . ? C7 N1 1.344(6) . ? C7 H7 0.9500 . ? C8 C9 1.378(9) . ? C8 C13 1.408(8) . ? C9 C10 1.390(9) . ? C9 H9 0.9500 . ? C10 C11 1.379(14) . ? C10 H10 0.9500 . ? C11 C12 1.363(15) . ? C11 H11 0.9500 . ? C12 C13 1.383(12) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.387(7) . ? C14 C19 1.399(6) . ? C15 C16 1.382(7) . ? C15 H15 0.9500 . ? C16 C17 1.384(8) . ? C16 H16 0.9500 . ? C17 C18 1.385(8) . ? C17 H17 0.9500 . ? C18 C19 1.375(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.382(7) . ? C20 C21 1.404(7) . ? C21 C22 1.390(8) . ? C21 H21 0.9500 . ? C22 C23 1.358(10) . ? C22 H22 0.9500 . ? C23 C24 1.380(10) . ? C23 H23 0.9500 . ? C24 C25 1.391(8) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 F2 1.293(8) . ? C26 F1 1.310(10) . ? C26 F3 1.321(9) . ? C26 S1 1.833(6) . ? C27 C28 1.360(6) . ? C27 C40 1.471(6) . ? C28 C29 1.469(7) . ? C28 C46 1.482(6) . ? C29 N2 1.350(6) . ? C29 C30 1.395(6) . ? C30 C31 1.379(8) . ? C30 H30 0.9500 . ? C31 C32 1.386(8) . ? C31 H31 0.9500 . ? C32 C33 1.363(7) . ? C32 H32 0.9500 . ? C33 N2 1.344(6) . ? C33 H33 0.9500 . ? C34 C35 1.382(8) . ? C34 C39 1.405(7) . ? C35 C36 1.386(8) . ? C35 H35 0.9500 . ? C36 C37 1.363(11) . ? C36 H36 0.9500 . ? C37 C38 1.356(11) . ? C37 H37 0.9500 . ? C38 C39 1.385(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.393(7) . ? C40 C41 1.395(7) . ? C41 C42 1.383(7) . ? C41 H41 0.9500 . ? C42 C43 1.377(8) . ? C42 H42 0.9500 . ? C43 C44 1.376(8) . ? C43 H43 0.9500 . ? C44 C45 1.386(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.387(7) . ? C46 C51 1.404(7) . ? C47 C48 1.383(8) . ? C47 H47 0.9500 . ? C48 C49 1.364(10) . ? C48 H48 0.9500 . ? C49 C50 1.404(10) . ? C49 H49 0.9500 . ? C50 C51 1.380(8) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? N3 S1 1.518(6) . ? N3 S5A 1.555(8) . ? N3 S5B 1.684(8) . ? N4 S3B 1.366(10) . ? N4 S3A 1.531(5) . ? N4 S4B 1.557(5) . ? N4 S4A 1.577(5) . ? O1 S1 1.484(4) . ? O5 S3A 1.490(4) . ? O5 S3B 1.526(7) . ? S1 O2B 1.419(18) . ? S1 O2A 1.425(10) . ? C53 F11B 1.233(11) . ? C53 F12A 1.277(7) . ? C53 F10B 1.286(11) . ? C53 F10A 1.291(7) . ? C53 F12B 1.371(11) . ? C53 F11A 1.379(7) . ? C53 S4B 1.808(8) . ? C53 S4A 1.848(6) . ? S5A O3A 1.396(14) . ? S5A O4A 1.438(5) . ? S5A C27A 1.948(17) . ? C27A F4A 1.21(2) . ? C27A F5A 1.298(19) . ? C27A F6A 1.342(17) . ? F4B C27B 1.261(19) . ? F6B C27B 1.26(3) . ? F5B C27B 1.28(2) . ? C27B S5B 1.787(18) . ? O3B S5B 1.401(16) . ? O4B S5B 1.439(5) . ? O7A S4A 1.428(5) . ? S4A O8A 1.431(4) . ? O7B S4B 1.430(5) . ? O8B S4B 1.432(5) . ? S3A O6A 1.424(5) . ? S3A C52A 1.845(7) . ? S3B O6B 1.345(5) . ? S3B C52B 1.80(3) . ? C52A F9A 1.321(5) . ? C52A F8A 1.323(5) . ? C52A F7A 1.325(4) . ? F9B C52B 1.322(5) . ? F7B C52B 1.321(5) . ? F8B C52B 1.323(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 B1 C8 107.2(4) . . ? O1 B1 N1 107.2(4) . . ? C8 B1 N1 110.9(4) . . ? O1 B1 C1 114.4(4) . . ? C8 B1 C1 117.7(4) . . ? N1 B1 C1 98.8(3) . . ? O5 B2 N2 107.0(4) . . ? O5 B2 C34 107.2(4) . . ? N2 B2 C34 109.1(3) . . ? O5 B2 C27 114.9(4) . . ? N2 B2 C27 98.8(3) . . ? C34 B2 C27 119.0(4) . . ? C2 C1 C14 127.0(4) . . ? C2 C1 B1 108.9(4) . . ? C14 C1 B1 124.0(4) . . ? C1 C2 C3 111.2(4) . . ? C1 C2 C20 127.8(4) . . ? C3 C2 C20 121.0(4) . . ? N1 C3 C4 118.5(4) . . ? N1 C3 C2 110.7(4) . . ? C4 C3 C2 130.9(4) . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 118.5(4) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? N1 C7 C6 120.6(4) . . ? N1 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C13 117.4(6) . . ? C9 C8 B1 119.5(5) . . ? C13 C8 B1 123.2(6) . . ? C8 C9 C10 122.6(7) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 118.4(9) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C12 C11 C10 120.5(7) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.0(8) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 120.0(9) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 117.8(4) . . ? C15 C14 C1 121.4(4) . . ? C19 C14 C1 120.8(4) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 119.1(5) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.3(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C14 121.2(5) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? C25 C20 C21 118.7(5) . . ? C25 C20 C2 119.7(4) . . ? C21 C20 C2 121.5(4) . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 120.8(6) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.3(6) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 120.3(5) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? F2 C26 F1 109.1(7) . . ? F2 C26 F3 108.7(6) . . ? F1 C26 F3 110.6(6) . . ? F2 C26 S1 109.2(5) . . ? F1 C26 S1 110.7(5) . . ? F3 C26 S1 108.5(5) . . ? C28 C27 C40 125.5(4) . . ? C28 C27 B2 109.5(4) . . ? C40 C27 B2 125.0(4) . . ? C27 C28 C29 110.5(4) . . ? C27 C28 C46 127.9(4) . . ? C29 C28 C46 121.5(4) . . ? N2 C29 C30 119.1(4) . . ? N2 C29 C28 110.6(4) . . ? C30 C29 C28 130.3(4) . . ? C31 C30 C29 119.1(5) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 118.8(5) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? N2 C33 C32 120.9(4) . . ? N2 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C39 117.7(5) . . ? C35 C34 B2 119.9(4) . . ? C39 C34 B2 122.3(5) . . ? C34 C35 C36 121.5(6) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 119.2(6) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 122.3(6) . . ? C37 C38 H38 118.8 . . ? C39 C38 H38 118.8 . . ? C38 C39 C34 119.1(6) . . ? C38 C39 H39 120.5 . . ? C34 C39 H39 120.5 . . ? C45 C40 C41 118.0(4) . . ? C45 C40 C27 121.5(4) . . ? C41 C40 C27 120.5(4) . . ? C42 C41 C40 121.3(5) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C43 C42 C41 119.7(5) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.2(5) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.3(5) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.6(4) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C47 C46 C51 118.9(5) . . ? C47 C46 C28 119.8(4) . . ? C51 C46 C28 121.4(4) . . ? C48 C47 C46 120.6(5) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C49 C48 C47 120.9(6) . . ? C49 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? C48 C49 C50 119.3(5) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C51 C50 C49 120.4(6) . . ? C51 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C50 C51 C46 119.9(6) . . ? C50 C51 H51 120.1 . . ? C46 C51 H51 120.1 . . ? C7 N1 C3 122.3(4) . . ? C7 N1 B1 127.8(4) . . ? C3 N1 B1 109.7(3) . . ? C33 N2 C29 121.9(4) . . ? C33 N2 B2 127.9(4) . . ? C29 N2 B2 110.0(4) . . ? S1 N3 S5A 136.9(5) . . ? S1 N3 S5B 114.3(4) . . ? S3B N4 S4B 141.7(7) . . ? S3A N4 S4A 128.3(3) . . ? S1 O1 B1 132.9(3) . . ? S3A O5 B2 134.2(3) . . ? S3B O5 B2 123.2(4) . . ? O2B S1 O1 123.0(17) . . ? O2A S1 O1 108.8(12) . . ? O2B S1 N3 107(2) . . ? O2A S1 N3 129.7(14) . . ? O1 S1 N3 109.7(2) . . ? O2B S1 C26 113(2) . . ? O2A S1 C26 101.4(9) . . ? O1 S1 C26 99.1(3) . . ? N3 S1 C26 103.2(3) . . ? F11B C53 F10B 113.7(7) . . ? F12A C53 F10A 113.5(5) . . ? F11B C53 F12B 107.9(7) . . ? F10B C53 F12B 104.6(6) . . ? F12A C53 F11A 108.0(4) . . ? F10A C53 F11A 107.4(5) . . ? F11B C53 S4B 107.9(7) . . ? F10B C53 S4B 123.2(5) . . ? F12B C53 S4B 97.1(7) . . ? F12A C53 S4A 115.0(5) . . ? F10A C53 S4A 108.4(4) . . ? F11A C53 S4A 103.9(4) . . ? O3A S5A O4A 121.1(9) . . ? O3A S5A N3 113.4(7) . . ? O4A S5A N3 107.8(7) . . ? O3A S5A C27A 110.4(8) . . ? O4A S5A C27A 104.9(8) . . ? N3 S5A C27A 96.0(6) . . ? F4A C27A F5A 102.6(14) . . ? F4A C27A F6A 109.4(15) . . ? F5A C27A F6A 106.8(13) . . ? F4A C27A S5A 108.1(12) . . ? F5A C27A S5A 119.2(10) . . ? F6A C27A S5A 110.3(10) . . ? F4B C27B F6B 109.1(17) . . ? F4B C27B F5B 110.3(15) . . ? F6B C27B F5B 119.0(17) . . ? F4B C27B S5B 112.9(12) . . ? F6B C27B S5B 115.6(15) . . ? F5B C27B S5B 88.7(11) . . ? O3B S5B O4B 120.0(10) . . ? O3B S5B N3 103.9(7) . . ? O4B S5B N3 119.7(7) . . ? O3B S5B C27B 92.8(9) . . ? O4B S5B C27B 109.9(8) . . ? N3 S5B C27B 106.6(6) . . ? O7A S4A O8A 121.0(5) . . ? O7A S4A N4 112.0(4) . . ? O8A S4A N4 109.0(3) . . ? O7A S4A C53 105.6(4) . . ? O8A S4A C53 105.3(3) . . ? N4 S4A C53 101.9(3) . . ? O7B S4B O8B 110.0(11) . . ? O7B S4B N4 133.0(10) . . ? O8B S4B N4 98.7(8) . . ? O7B S4B C53 104.9(9) . . ? O8B S4B C53 102.0(8) . . ? N4 S4B C53 104.5(4) . . ? O6A S3A O5 114.8(3) . . ? O6A S3A N4 119.2(3) . . ? O5 S3A N4 111.7(2) . . ? O6A S3A C52A 106.1(3) . . ? O5 S3A C52A 98.7(2) . . ? N4 S3A C52A 103.2(3) . . ? O6B S3B N4 57.1(13) . . ? O6B S3B O5 135.8(14) . . ? N4 S3B O5 119.6(6) . . ? O6B S3B C52B 123.1(16) . . ? N4 S3B C52B 120.9(10) . . ? O5 S3B C52B 97.1(9) . . ? F9A C52A F8A 112.2(6) . . ? F9A C52A F7A 108.2(6) . . ? F8A C52A F7A 111.8(6) . . ? F9A C52A S3A 108.0(5) . . ? F8A C52A S3A 108.7(4) . . ? F7A C52A S3A 107.7(4) . . ? F7B C52B F9B 112(3) . . ? F7B C52B F8B 111(3) . . ? F9B C52B F8B 110(3) . . ? F7B C52B S3B 119(2) . . ? F9B C52B S3B 108(3) . . ? F8B C52B S3B 96(2) . . ? _refine_diff_density_max 1.002 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.090 _shelxl_version_number 2014/6 _shelx_res_file ; TITL MM1531_0m_a.res in P-1 CELL 1.54178 10.0900 15.4860 18.2577 75.063 80.627 89.752 ZERR 2.000 0.0003 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H B N O F S UNIT 108 76 4 8 16 24 8 OMIT -4.00 129.00 L.S. 20 ACTA 129 BOND $H FMAP 2 PLAN 0 LIST 6 DFIX 1.35 0.005 S3B O6B SIMU 0.005 O6A O6B ISOR 0.005 O6A O6B ISOR 0.005 S3A S3B SIMU 0.005 S3A S3B SIMU 0.005 O2A O2B ISOR 0.005 C27A C27B SIMU 0.005 C27A C27B DFIX 1.45 0.005 S4A O7A S4A O8A DANG 2.328 0.05 O7A O8A DANG 2.343 O7B O8B DFIX 1.51 0.005 S4B N4 DFIX 1.435 0.005 S4B O7B S4B O8B SIZE 0.10 0.20 0.20 DFIX 1.45 0.005 S5B O4B DFIX 1.45 0.005 S5A O4A SIMU 0.005 S4A S4B SIMU 0.005 O7A O7B O8A O8B ISOR 0.005 S4A S4B ISOR 0.005 O7A O7B O8A O8B DELU 0.008 F10A F10B F11A F11B F12A F12B F12B F10A ISOR 0.005 F10A F10B F11A F11B F12A F12B F12B F10A SIMU 0.005 F10A F10B F11A F11B F12A F12B F12B F10A SADI 0.02 C53 F10A C53 F11A C53 F12A C53 F10B C53 F11B C53 F12B SADI 0.005 F10B F11B F11B F12B F12B F10B SADI 0.005 F10A F11A F11A F12A F12A F10A FLAT 0.008 F10A F10B F11A F11B F12A F12B SIMU 0.008 F4A F4B F5A F5B F6A F6B ISOR 0.008 F4A F4B F5A F5B F6A F6B SIMU 0.005 O3A O3B O4A O4B ISOR 0.005 O3A O3B O4A O4B DFIX 1.391 S1 O2A S1 O2B DELU 0.005 F7A F7B F8A F8B F9A F9B F9B F7A SIMU 0.005 F7A F7B F8A F8B F9A F9B F9B F7A SADI 0.005 C52A F7A C52A F8A C52A F9A C52B F7B C52B F8B C52B F9B FREE O6B N4 TEMP -100.000 WGHT 0.156200 2.147100 FVAR 0.36844 0.53251 0.66390 0.68831 0.67260 0.81922 0.83401 B1 3 0.781412 0.572767 0.220018 11.00000 0.04143 0.05208 = 0.03513 -0.01118 -0.00844 0.00627 B2 3 0.270143 0.100966 0.228386 11.00000 0.03827 0.04774 = 0.03606 -0.00560 -0.00928 0.00221 C1 1 0.692182 0.654811 0.235683 11.00000 0.02794 0.04977 = 0.03881 -0.01152 -0.00383 0.00089 C2 1 0.675123 0.650726 0.311779 11.00000 0.03061 0.05434 = 0.03849 -0.01264 -0.00375 -0.00140 C3 1 0.727555 0.568660 0.354952 11.00000 0.02744 0.04802 = 0.04302 -0.01076 -0.00426 -0.00404 C4 1 0.728120 0.535779 0.433417 11.00000 0.04044 0.06554 = 0.03636 -0.01194 -0.00367 -0.00246 AFIX 43 H4 2 0.690090 0.569048 0.468159 11.00000 -1.20000 AFIX 0 C5 1 0.783839 0.455068 0.460476 11.00000 0.04116 0.06556 = 0.03923 0.00140 -0.00752 0.00184 AFIX 43 H5 2 0.783480 0.432311 0.514061 11.00000 -1.20000 AFIX 0 C6 1 0.841206 0.406180 0.409319 11.00000 0.04479 0.05295 = 0.05308 -0.00061 -0.00808 0.00337 AFIX 43 H6 2 0.879404 0.350153 0.427609 11.00000 -1.20000 AFIX 0 C7 1 0.840918 0.441090 0.332269 11.00000 0.03865 0.04975 = 0.05091 -0.01136 -0.00678 0.00495 AFIX 43 H7 2 0.880973 0.409510 0.296633 11.00000 -1.20000 AFIX 0 C8 1 0.929510 0.595777 0.173006 11.00000 0.04389 0.05983 = 0.03785 -0.00034 0.00028 0.01608 C9 1 1.010470 0.656671 0.190231 11.00000 0.04108 0.07463 = 0.07744 -0.00984 0.00059 0.00134 AFIX 43 H9 2 0.975387 0.684253 0.229742 11.00000 -1.20000 AFIX 0 C10 1 1.141379 0.679348 0.152117 11.00000 0.04664 0.09031 = 0.10369 0.00262 -0.00099 0.00608 AFIX 43 H10 2 1.195474 0.720750 0.165860 11.00000 -1.20000 AFIX 0 C11 1 1.190896 0.640313 0.093863 11.00000 0.05983 0.13695 = 0.08715 0.03282 0.02616 0.02388 AFIX 43 H11 2 1.279332 0.656084 0.066197 11.00000 -1.20000 AFIX 0 C12 1 1.114006 0.579302 0.075658 11.00000 0.09566 0.15742 = 0.06807 -0.01913 0.02801 0.04719 AFIX 43 H12 2 1.149614 0.552986 0.035402 11.00000 -1.20000 AFIX 0 C13 1 0.984927 0.555141 0.114918 11.00000 0.07229 0.10611 = 0.05933 -0.02806 0.00661 0.02229 AFIX 43 H13 2 0.933619 0.511094 0.102680 11.00000 -1.20000 AFIX 0 C14 1 0.639863 0.721869 0.175476 11.00000 0.04038 0.04071 = 0.04151 -0.01038 -0.00751 0.00233 C15 1 0.515584 0.758266 0.190044 11.00000 0.04354 0.06236 = 0.04304 -0.01266 -0.00605 0.00693 AFIX 43 H15 2 0.465003 0.741843 0.240554 11.00000 -1.20000 AFIX 0 C16 1 0.464132 0.818049 0.132260 11.00000 0.04586 0.06143 = 0.05689 -0.01133 -0.01261 0.01156 AFIX 43 H16 2 0.378043 0.841350 0.143191 11.00000 -1.20000 AFIX 0 C17 1 0.537171 0.844199 0.058585 11.00000 0.05594 0.05452 = 0.05425 -0.00124 -0.01776 0.00902 AFIX 43 H17 2 0.503063 0.886757 0.019277 11.00000 -1.20000 AFIX 0 C18 1 0.660665 0.807505 0.042906 11.00000 0.05405 0.07198 = 0.04466 -0.00134 -0.00320 0.00485 AFIX 43 H18 2 0.710775 0.823985 -0.007723 11.00000 -1.20000 AFIX 0 C19 1 0.711030 0.747333 0.100303 11.00000 0.04356 0.05939 = 0.04373 -0.00805 -0.00437 0.01051 AFIX 43 H19 2 0.795747 0.722586 0.088694 11.00000 -1.20000 AFIX 0 C20 1 0.615078 0.718302 0.350916 11.00000 0.03953 0.05386 = 0.04092 -0.01552 -0.00905 0.00916 C21 1 0.509724 0.695127 0.413826 11.00000 0.04713 0.07032 = 0.05093 -0.02194 0.00012 0.00310 AFIX 43 H21 2 0.476759 0.634810 0.433294 11.00000 -1.20000 AFIX 0 C22 1 0.453786 0.760676 0.447545 11.00000 0.05844 0.09509 = 0.05843 -0.03294 -0.00268 0.01151 AFIX 43 H22 2 0.382605 0.744726 0.490153 11.00000 -1.20000 AFIX 0 C23 1 0.499594 0.847229 0.420354 11.00000 0.07707 0.08791 = 0.05983 -0.04057 -0.02577 0.03412 AFIX 43 H23 2 0.459247 0.891604 0.443228 11.00000 -1.20000 AFIX 0 C24 1 0.604741 0.870692 0.359503 11.00000 0.09292 0.05061 = 0.06493 -0.02235 -0.03209 0.01225 AFIX 43 H24 2 0.637581 0.931110 0.341082 11.00000 -1.20000 AFIX 0 C25 1 0.662875 0.806270 0.325007 11.00000 0.05667 0.06026 = 0.04844 -0.01710 -0.00996 0.00136 AFIX 43 H25 2 0.735791 0.822799 0.283434 11.00000 -1.20000 AFIX 0 C26 1 0.527493 0.492081 0.107305 11.00000 0.06470 0.12774 = 0.06442 -0.04300 -0.02453 0.01652 C27 1 0.187345 0.008779 0.243024 11.00000 0.02964 0.04876 = 0.03882 -0.00305 -0.00472 0.00070 C28 1 0.170723 -0.034735 0.318979 11.00000 0.02949 0.04597 = 0.03969 -0.00524 -0.00438 0.00484 C29 1 0.221293 0.021590 0.362772 11.00000 0.03121 0.05066 = 0.03795 -0.00742 -0.00341 0.00870 C30 1 0.223701 0.004889 0.441382 11.00000 0.04172 0.05948 = 0.03762 -0.00937 -0.00334 0.00654 AFIX 43 H30 2 0.188324 -0.050244 0.475663 11.00000 -1.20000 AFIX 0 C31 1 0.278171 0.069564 0.468608 11.00000 0.04452 0.08127 = 0.03924 -0.01952 -0.00691 0.00967 AFIX 43 H31 2 0.279352 0.059273 0.522088 11.00000 -1.20000 AFIX 0 C32 1 0.331178 0.149473 0.418333 11.00000 0.04041 0.06471 = 0.05645 -0.02677 -0.00852 0.00505 AFIX 43 H32 2 0.368838 0.194193 0.436820 11.00000 -1.20000 AFIX 0 C33 1 0.328278 0.162721 0.341850 11.00000 0.03567 0.05018 = 0.04981 -0.01344 -0.00758 0.00338 AFIX 43 H33 2 0.365954 0.216725 0.306693 11.00000 -1.20000 AFIX 0 C34 1 0.420519 0.111459 0.182650 11.00000 0.03577 0.06206 = 0.03549 -0.01244 -0.00582 -0.00407 C35 1 0.500939 0.038305 0.190242 11.00000 0.03998 0.07228 = 0.06745 -0.02704 -0.00581 0.00401 AFIX 43 H35 2 0.464009 -0.018471 0.220504 11.00000 -1.20000 AFIX 0 C36 1 0.634241 0.045807 0.154741 11.00000 0.04096 0.12362 = 0.09187 -0.05878 -0.00444 0.00671 AFIX 43 H36 2 0.686886 -0.005757 0.159922 11.00000 -1.20000 AFIX 0 C37 1 0.689977 0.127017 0.112405 11.00000 0.04011 0.15236 = 0.06794 -0.06173 0.01487 -0.02759 AFIX 43 H37 2 0.781721 0.132623 0.088711 11.00000 -1.20000 AFIX 0 C38 1 0.612839 0.199665 0.104543 11.00000 0.05735 0.10799 = 0.05867 -0.01680 0.01049 -0.03194 AFIX 43 H38 2 0.652158 0.256101 0.074994 11.00000 -1.20000 AFIX 0 C39 1 0.478725 0.194510 0.138072 11.00000 0.05188 0.07065 = 0.04782 -0.00462 -0.00674 -0.01367 AFIX 43 H39 2 0.426815 0.246437 0.131015 11.00000 -1.20000 AFIX 0 C40 1 0.138913 -0.024319 0.183109 11.00000 0.03999 0.04123 = 0.04032 -0.00276 -0.01141 0.00066 C41 1 0.215349 -0.008804 0.109726 11.00000 0.03961 0.05290 = 0.04382 -0.00295 -0.01011 -0.00009 AFIX 43 H41 2 0.299184 0.023494 0.098696 11.00000 -1.20000 AFIX 0 C42 1 0.171450 -0.039524 0.052741 11.00000 0.05869 0.06756 = 0.03740 -0.01050 -0.00826 0.00025 AFIX 43 H42 2 0.225380 -0.029104 0.003305 11.00000 -1.20000 AFIX 0 C43 1 0.049198 -0.085284 0.068011 11.00000 0.06150 0.06357 = 0.04914 -0.01514 -0.02253 0.00206 AFIX 43 H43 2 0.019068 -0.106957 0.029147 11.00000 -1.20000 AFIX 0 C44 1 -0.029498 -0.099724 0.139412 11.00000 0.04810 0.06097 = 0.05798 -0.01536 -0.01559 -0.00601 AFIX 43 H44 2 -0.114491 -0.130410 0.149375 11.00000 -1.20000 AFIX 0 C45 1 0.014744 -0.069681 0.196842 11.00000 0.04307 0.06059 = 0.04224 -0.00953 -0.00759 -0.00422 AFIX 43 H45 2 -0.040102 -0.080118 0.246013 11.00000 -1.20000 AFIX 0 C46 1 0.117367 -0.127390 0.356491 11.00000 0.03914 0.04919 = 0.04065 -0.00227 -0.00980 0.00024 C47 1 0.171752 -0.197693 0.329013 11.00000 0.05837 0.05243 = 0.04845 -0.01070 -0.00746 0.00181 AFIX 43 H47 2 0.245728 -0.186404 0.287882 11.00000 -1.20000 AFIX 0 C48 1 0.119276 -0.284034 0.360940 11.00000 0.08809 0.04888 = 0.06719 -0.00803 -0.02921 0.00286 AFIX 43 H48 2 0.157272 -0.331354 0.341203 11.00000 -1.20000 AFIX 0 C49 1 0.013685 -0.302204 0.420394 11.00000 0.07402 0.05387 = 0.07927 0.01409 -0.03404 -0.01662 AFIX 43 H49 2 -0.022899 -0.361536 0.441317 11.00000 -1.20000 AFIX 0 C50 1 -0.040340 -0.232297 0.450328 11.00000 0.04830 0.07108 = 0.07577 0.02064 0.00017 -0.00635 AFIX 43 H50 2 -0.112666 -0.244609 0.492420 11.00000 -1.20000 AFIX 0 C51 1 0.010994 -0.145796 0.418973 11.00000 0.04706 0.05559 = 0.05416 0.01050 0.00141 0.00568 AFIX 43 H51 2 -0.025590 -0.098784 0.439636 11.00000 -1.20000 AFIX 0 F1 6 0.523831 0.579130 0.081891 11.00000 0.10186 0.10940 = 0.07972 0.00737 -0.03908 0.00613 F2 6 0.612971 0.462174 0.059778 11.00000 0.09146 0.23235 = 0.08453 -0.09956 -0.01922 0.02763 F3 6 0.408152 0.453971 0.112853 11.00000 0.07800 0.15988 = 0.09443 -0.05432 -0.03755 -0.00498 N1 4 0.784522 0.519544 0.306681 11.00000 0.03380 0.04724 = 0.03740 -0.00778 -0.00622 0.00096 N2 4 0.272847 0.100424 0.315503 11.00000 0.03271 0.05209 = 0.03702 -0.01101 -0.00483 0.00650 N3 4 0.479680 0.509533 0.248838 11.00000 0.07977 0.07292 = 0.06829 -0.02797 0.00908 -0.02410 N4 4 -0.046829 0.145568 0.244606 11.00000 0.06314 0.05845 = 0.06155 -0.01216 -0.00497 0.00613 O1 5 0.711694 0.509148 0.182417 11.00000 0.05640 0.06809 = 0.05390 -0.02939 -0.02000 0.01367 O5 5 0.196072 0.186394 0.192454 11.00000 0.04320 0.05086 = 0.05418 0.00192 -0.01221 -0.00146 S1 7 0.578150 0.461494 0.202354 11.00000 0.07192 0.05842 = 0.05204 -0.01633 -0.02473 0.00247 C53 1 -0.269167 0.176127 0.333755 11.00000 0.04466 0.08065 = 0.06439 -0.03490 -0.01629 0.02063 PART 1 21 S5A 7 0.394109 0.487469 0.330775 21.00000 0.04352 0.13527 = 0.05287 -0.02349 -0.00245 -0.02550 O4A 5 0.460756 0.419810 0.380194 21.00000 0.07548 0.13730 = 0.07694 0.00664 -0.01468 -0.00420 O3A 5 0.346962 0.563163 0.353224 21.00000 0.09559 0.13135 = 0.09346 -0.06398 0.02069 -0.01222 C27A 1 0.248079 0.423422 0.306701 21.00000 0.05866 0.05936 = 0.06760 -0.01122 -0.00735 0.00204 F5A 6 0.275699 0.374037 0.258932 21.00000 0.08332 0.10255 = 0.09241 -0.02509 -0.02405 -0.02550 F4A 6 0.175639 0.478007 0.275149 21.00000 0.06690 0.09494 = 0.10099 -0.00753 -0.04450 -0.00529 F6A 6 0.177121 0.371027 0.371362 21.00000 0.07162 0.09394 = 0.08544 0.00437 0.00077 -0.02807 PART 2 -21 F4B 6 0.164493 0.418215 0.400930 -21.00000 0.07633 0.14528 = 0.08782 -0.00360 0.00436 -0.03652 F6B 6 0.185988 0.498089 0.290462 -21.00000 0.08517 0.10681 = 0.10983 -0.00386 -0.01533 0.02940 F5B 6 0.257231 0.361282 0.314746 -21.00000 0.10120 0.10057 = 0.14479 -0.02780 -0.01538 -0.01414 C27B 1 0.234846 0.434206 0.334861 -21.00000 0.05852 0.05999 = 0.06278 -0.01529 -0.01032 0.00210 O3B 5 0.390577 0.506418 0.381825 -21.00000 0.10266 0.11961 = 0.07303 -0.04059 0.01306 -0.02964 O4B 5 0.462992 0.359607 0.365816 -21.00000 0.06884 0.10215 = 0.07620 0.00945 -0.01227 0.00140 S5B 7 0.410503 0.445823 0.336178 -21.00000 0.05849 0.07714 = 0.04747 -0.01154 -0.00269 -0.02033 PART 1 31 O7A 5 -0.043315 0.129167 0.383738 31.00000 0.06169 0.09847 = 0.06150 -0.01960 0.00017 0.00560 S4A 7 -0.118645 0.107865 0.330502 31.00000 0.03744 0.05003 = 0.04447 -0.00150 -0.00222 0.00515 O8A 5 -0.168731 0.018498 0.340699 31.00000 0.05704 0.06638 = 0.06894 -0.00104 0.00711 0.00558 PART 2 -31 O7B 5 -0.044836 0.185936 0.381983 -31.00000 0.08482 0.11820 = 0.11889 -0.01341 -0.02864 0.00687 O8B 5 -0.110278 0.049723 0.362314 -31.00000 0.07771 0.07389 = 0.06944 0.00166 0.00554 0.02104 S4B 7 -0.096013 0.144500 0.330216 -31.00000 0.04619 0.06853 = 0.08552 0.01725 -0.01042 0.00878 PART 1 41 F10A 6 -0.336450 0.164783 0.282333 41.00000 0.06772 0.10135 = 0.06235 -0.02590 -0.02335 0.00455 F11A 6 -0.344540 0.137171 0.404768 41.00000 0.05009 0.11329 = 0.06510 -0.02146 0.00889 0.01138 F12A 6 -0.245869 0.258261 0.330036 41.00000 0.09694 0.08104 = 0.10676 -0.04257 -0.02819 0.01185 PART 2 -41 F11B 6 -0.313887 0.178245 0.400247 -41.00000 0.07996 0.10622 = 0.08518 -0.05098 0.00384 0.00992 F12B 6 -0.244328 0.262567 0.290060 -41.00000 0.08335 0.08560 = 0.09923 -0.03390 -0.02044 0.02277 F10B 6 -0.353426 0.143054 0.301482 -41.00000 0.05976 0.11070 = 0.07308 -0.02445 -0.00400 -0.00392 PART 1 51 O2A 5 0.597332 0.368163 0.212932 51.00000 0.09830 0.06257 = 0.10170 -0.03402 -0.03270 0.01682 PART 2 -51 O2B 5 0.559678 0.368578 0.238512 -51.00000 0.09672 0.05308 = 0.10669 -0.02433 -0.03032 0.02963 PART 1 61 S3A 7 0.060642 0.221246 0.212145 61.00000 0.04730 0.04926 = 0.04837 -0.00964 -0.01329 0.00468 O6A 5 0.059768 0.293440 0.247259 61.00000 0.08433 0.07930 = 0.10647 -0.05486 -0.01542 -0.00666 PART 2 -61 S3B 7 0.048786 0.184515 0.182818 -61.00000 0.04707 0.04357 = 0.07940 -0.01472 -0.02680 0.00093 O6B 5 -0.041496 0.121622 0.181230 -61.00000 0.08458 0.09144 = 0.08923 -0.03471 -0.01955 0.00560 PART 1 71 ISOR 0.005 C52A C52B SIMU 0.005 C52A C52B C52A 1 0.027430 0.270091 0.113763 71.00000 0.05467 0.06799 = 0.06226 0.00325 -0.01537 0.00072 F9A 6 -0.090448 0.307475 0.119012 71.00000 0.06495 0.11398 = 0.07660 0.00919 -0.02363 0.02610 F8A 6 0.030186 0.205931 0.077758 71.00000 0.07020 0.14702 = 0.05537 -0.03245 -0.00856 -0.01186 F7A 6 0.121021 0.333795 0.079163 71.00000 0.06942 0.08799 = 0.09547 0.04042 -0.01157 -0.00855 PART 2 -71 F9B 6 -0.084533 0.322673 0.142914 -71.00000 0.06906 0.10446 = 0.06719 0.00388 -0.01761 0.03715 F7B 6 0.124368 0.359231 0.145818 -71.00000 0.07924 0.07641 = 0.10931 0.03551 -0.00637 -0.00442 F8B 6 0.078333 0.289134 0.063161 -71.00000 0.07227 0.11861 = 0.07268 0.00302 -0.00905 0.00487 C52B 1 0.042490 0.300422 0.132990 -71.00000 0.05397 0.06000 = 0.05683 -0.00631 -0.01223 0.00294 PART 0 HKLF 4 REM MM1531_0m_a.res in P-1 REM R1 = 0.0812 for 6196 Fo > 4sig(Fo) and 0.1091 for all 8769 data REM 943 parameters refined using 399 restraints END WGHT 0.1499 2.0419 REM Highest difference peak 1.002, deepest hole -0.539, 1-sigma level 0.090 Q1 1 0.5358 0.5166 0.1874 11.00000 0.05 1.00 Q2 1 -0.0987 0.1547 0.3600 11.00000 0.05 0.86 Q3 1 0.4427 0.4637 0.3876 11.00000 0.05 0.81 Q4 1 0.0314 0.3448 0.1971 11.00000 0.05 0.73 Q5 1 0.0634 0.1553 0.1086 11.00000 0.05 0.65 Q6 1 0.0031 0.2167 0.2744 11.00000 0.05 0.62 Q7 1 -0.0598 0.0865 0.3762 11.00000 0.05 0.62 Q8 1 -0.3325 0.2332 0.3624 11.00000 0.05 0.54 Q9 1 0.6058 0.3597 0.1466 11.00000 0.05 0.48 Q10 1 0.0537 0.1963 0.1471 11.00000 0.05 0.47 Q11 1 -0.0893 0.1834 0.4214 11.00000 0.05 0.45 Q12 1 0.4678 0.5774 0.1824 11.00000 0.05 0.44 Q13 1 0.0409 0.2984 0.1643 11.00000 0.05 0.44 Q14 1 0.4282 0.3932 0.1520 11.00000 0.05 0.44 Q15 1 0.0249 0.2857 0.1859 11.00000 0.05 0.43 Q16 1 0.4396 0.3932 0.3605 11.00000 0.05 0.43 Q17 1 0.6182 0.4024 0.1092 11.00000 0.05 0.42 Q18 1 0.5449 0.4245 0.1791 11.00000 0.05 0.40 Q19 1 0.2394 0.4351 0.2481 11.00000 0.05 0.40 Q20 1 0.3556 0.5213 0.3722 11.00000 0.05 0.38 ; _shelx_res_checksum 74891 _shelx_hkl_file ; 1 0 0 0.00 0.90 1 0 0 0.60 1.00 1 0 0 0.90 0.70 2 0 0 208.08 8.50 2 0 0 198.58 10.00 2 0 0 196.48 10.00 3 0 0 0.50 1.70 3 0 0 4.30 3.10 3 0 0 0.20 2.40 4 0 0 116.09 9.90 4 0 0 114.29 7.50 -5 0 0 33.80 6.70 5 0 0 23.60 4.70 5 0 0 29.30 6.90 -6 0 0 69.09 10.00 6 0 0 68.19 10.40 7 0 0 0.70 5.70 8 0 0 -1.20 1.20 9 0 0 16.00 2.30 10 -1 0 26.40 2.60 9 -1 0 3.00 1.50 8 -1 0 12.20 2.10 8 -1 0 10.80 2.50 7 -1 0 3.60 6.30 6 -1 0 448.66 25.80 -6 1 0 472.55 24.10 5 -1 0 14.50 5.60 -5 1 0 14.10 5.10 4 -1 0 456.65 17.50 4 -1 0 397.26 21.20 -4 1 0 440.96 19.90 3 -1 0 75.39 7.80 3 -1 0 80.09 5.00 -3 1 0 82.69 6.30 2 -1 0 1225.68 42.40 2 -1 0 1367.46 45.50 -2 1 0 1262.77 43.90 1 -1 0 2626.34 88.49 1 -1 0 2578.34 86.69 -1 1 0 2881.01 87.79 0 -1 0 361.96 13.00 0 -1 0 378.36 13.20 0 1 0 417.66 13.40 1 1 0 991.10 33.20 1 1 0 962.00 33.00 1 1 0 1002.10 33.40 2 1 0 473.05 18.80 2 1 0 501.95 18.10 2 1 0 462.95 19.00 3 1 0 530.45 22.90 3 1 0 579.94 21.50 3 1 0 550.04 22.90 4 1 0 81.69 8.20 4 1 0 78.49 6.70 4 1 0 99.39 8.90 5 1 0 768.02 34.30 5 1 0 787.92 31.50 5 1 0 829.62 35.20 -6 -1 0 77.29 10.20 6 1 0 76.09 10.40 11 -2 0 9.80 1.70 10 -2 0 13.20 2.20 9 -2 0 16.30 2.20 9 -2 0 13.80 2.20 8 -2 0 15.00 2.20 8 -2 0 14.80 2.20 7 -2 0 113.69 14.70 6 -2 0 4.20 4.80 -6 2 0 8.60 5.00 5 -2 0 607.74 30.40 -5 2 0 663.23 28.50 4 -2 0 213.48 14.50 4 -2 0 248.58 10.50 -4 2 0 223.18 12.70 3 -2 0 2017.10 68.89 3 -2 0 1950.10 63.89 -3 2 0 1853.91 66.39 2 -2 0 2460.35 83.19 2 -2 0 2400.36 79.69 -2 2 0 2513.85 81.99 1 -2 0 2183.68 72.59 1 -2 0 2207.88 70.59 -1 2 0 2132.39 71.89 0 -2 0 498.35 17.10 0 -2 0 458.55 16.60 0 2 0 471.35 17.30 -1 -2 0 20.20 2.30 1 2 0 23.50 3.10 1 2 0 27.10 3.10 2 2 0 664.83 25.00 2 2 0 709.93 25.40 2 2 0 686.53 26.00 3 2 0 1249.57 46.10 3 2 0 1324.67 45.90 3 2 0 1319.17 47.40 4 2 0 171.48 12.40 4 2 0 194.38 11.80 4 2 0 175.08 10.80 5 2 0 673.03 29.60 5 2 0 630.64 30.00 5 2 0 634.64 27.30 11 -3 0 1.00 1.20 10 -3 0 0.50 1.20 10 -3 0 0.40 1.40 9 -3 0 1.80 1.40 9 -3 0 0.00 1.30 8 -3 0 20.50 2.40 8 -3 0 19.70 2.50 7 -3 0 65.49 12.60 6 -3 0 50.49 9.40 -6 3 0 60.89 9.20 5 -3 0 294.37 19.30 -5 3 0 329.37 17.90 4 -3 0 199.88 14.40 -4 3 0 228.18 13.20 3 -3 0 4121.19 131.69 3 -3 0 4094.09 137.29 -3 3 0 3983.50 135.29 2 -3 0 1660.23 59.59 2 -3 0 1731.83 55.89 -2 3 0 1696.63 58.49 1 -3 0 2148.09 70.09 1 -3 0 2075.59 71.99 -1 3 0 2189.48 71.79 0 -3 0 3608.74 115.59 0 -3 0 3323.47 114.79 0 3 0 3677.93 116.09 -1 -3 0 1726.73 58.39 1 3 0 1833.52 60.49 -2 -3 0 13.40 2.80 2 3 0 11.10 3.20 2 3 0 10.60 3.10 -3 -3 0 78.89 6.80 3 3 0 55.79 6.50 3 3 0 63.69 6.10 -4 -3 0 133.49 10.40 4 3 0 130.19 9.50 4 3 0 129.59 10.60 -5 -3 0 342.57 19.40 5 3 0 348.37 20.30 -6 -3 0 287.27 18.90 6 3 0 304.47 20.80 11 -4 0 2.90 1.20 11 -4 0 0.50 1.00 10 -4 0 -0.30 1.30 10 -4 0 -0.60 1.20 9 -4 0 41.20 3.00 9 -4 0 41.40 3.20 8 -4 0 0.30 1.40 8 -4 0 0.20 1.40 7 -4 0 125.19 15.10 6 -4 0 103.89 12.90 -6 4 0 88.49 11.10 5 -4 0 241.28 18.00 -5 4 0 236.58 15.10 4 -4 0 79.79 9.50 -4 4 0 78.49 7.90 3 -4 0 586.44 26.90 3 -4 0 617.54 21.60 -3 4 0 625.34 25.70 2 -4 0 810.52 27.70 2 -4 0 789.32 31.50 -2 4 0 781.12 30.40 1 -4 0 536.45 22.20 1 -4 0 548.25 20.40 -1 4 0 582.94 22.50 0 -4 0 55.09 4.60 0 -4 0 58.19 5.30 0 4 0 60.69 5.70 -1 -4 0 13.40 3.40 -1 -4 0 18.70 2.80 1 4 0 15.30 3.50 -2 -4 0 112.99 6.40 2 4 0 115.09 8.20 -3 -4 0 196.18 10.70 3 4 0 192.98 12.30 4 4 0 37.30 7.20 -5 -4 0 594.44 29.50 5 4 0 667.03 30.70 -6 -4 0 4.20 5.70 6 4 0 16.20 7.80 11 -5 0 8.50 1.50 11 -5 0 11.60 1.70 10 -5 0 48.60 3.00 10 -5 0 46.90 3.20 9 -5 0 1.50 1.40 9 -5 0 0.30 1.20 8 -5 0 47.20 3.30 8 -5 0 43.30 3.20 7 -5 0 150.18 17.00 7 -5 0 157.48 6.50 7 -5 0 150.38 6.40 6 -5 0 310.27 22.20 -6 5 0 270.47 18.90 5 -5 0 474.35 27.00 -5 5 0 485.95 24.60 4 -5 0 667.13 30.60 -4 5 0 600.04 27.80 3 -5 0 208.78 13.70 -3 5 0 211.18 12.90 2 -5 0 194.48 12.30 2 -5 0 205.28 9.50 -2 5 0 207.08 12.10 1 -5 0 17.60 3.80 1 -5 0 13.50 2.90 -1 5 0 12.50 3.70 0 -5 0 1.70 1.90 0 -5 0 4.50 2.70 0 5 0 0.80 2.60 -1 -5 0 16.10 4.00 -1 -5 0 14.90 3.00 1 5 0 16.40 4.00 -2 -5 0 308.97 14.50 -2 -5 0 311.87 16.50 2 5 0 342.37 16.70 -3 -5 0 414.46 21.40 3 5 0 453.75 21.50 -4 -5 0 94.29 10.40 4 5 0 105.49 10.60 -5 -5 0 61.29 9.70 5 5 0 53.89 9.80 -6 -5 0 17.20 7.70 -7 -5 0 20.90 9.40 7 5 0 32.10 2.70 8 5 0 145.39 7.60 11 -6 0 0.40 0.90 11 -6 0 0.20 1.10 10 -6 0 65.79 3.70 10 -6 0 66.69 3.50 9 -6 0 11.60 2.00 9 -6 0 8.00 1.70 8 -6 0 133.09 5.90 8 -6 0 125.79 5.90 7 -6 0 16.60 2.40 7 -6 0 11.40 1.90 6 -6 0 121.29 15.20 -6 6 0 108.59 13.20 5 -6 0 40.40 9.20 -5 6 0 30.10 7.30 4 -6 0 158.08 14.10 -4 6 0 154.18 12.30 3 -6 0 17.30 5.30 -3 6 0 8.10 4.20 2 -6 0 36.50 4.50 2 -6 0 25.50 5.60 -2 6 0 24.40 5.40 1 -6 0 36.80 4.80 1 -6 0 38.60 5.80 -1 6 0 32.70 5.70 0 -6 0 633.14 25.10 0 -6 0 659.43 26.60 0 6 0 669.53 27.70 -1 -6 0 104.69 8.90 1 6 0 115.69 9.50 -2 -6 0 606.34 26.60 2 6 0 593.54 26.80 -3 -6 0 108.39 10.30 3 6 0 141.29 11.10 -4 -6 0 476.15 25.70 4 6 0 568.14 27.30 -5 -6 0 4.40 5.50 5 6 0 10.00 6.90 -6 -6 0 165.88 16.10 7 6 0 84.29 4.20 8 6 0 20.40 2.50 11 -7 0 2.90 0.90 11 -7 0 2.60 1.10 10 -7 0 25.80 2.20 10 -7 0 29.20 2.50 9 -7 0 20.60 2.40 9 -7 0 20.80 2.50 8 -7 0 2.50 1.50 8 -7 0 1.70 1.50 7 -7 0 28.70 2.80 7 -7 0 23.80 2.60 7 -7 0 23.80 2.60 6 -7 0 0.70 6.70 -6 7 0 -5.30 6.00 5 -7 0 6.80 6.40 -5 7 0 9.70 5.80 4 -7 0 12.70 6.00 -4 7 0 13.40 5.70 3 -7 0 186.48 14.10 -3 7 0 170.98 13.10 2 -7 0 4.20 4.00 -2 7 0 1.60 3.50 1 -7 0 0.00 2.80 1 -7 0 -0.50 3.00 -1 7 0 -0.80 3.00 0 -7 0 136.49 10.00 0 7 0 126.99 10.60 -1 -7 0 15.50 4.50 1 7 0 8.90 4.70 -2 -7 0 5.10 4.30 2 7 0 7.40 4.80 -3 -7 0 7.10 4.20 3 7 0 4.40 4.50 -4 -7 0 87.69 10.90 4 7 0 97.99 11.60 -5 -7 0 21.40 7.70 5 7 0 24.40 8.80 -6 -7 0 -3.30 6.80 6 7 0 1.00 1.40 6 7 0 0.30 1.20 7 7 0 2.80 1.30 7 7 0 -0.50 1.30 8 7 0 70.29 4.00 9 7 0 34.60 2.60 11 -8 0 0.90 0.90 11 -8 0 -0.10 0.70 10 -8 0 20.50 2.20 10 -8 0 19.80 2.00 9 -8 0 1.60 1.40 9 -8 0 1.70 1.30 8 -8 0 26.10 2.70 8 -8 0 27.60 2.90 7 -8 0 4.80 1.60 7 -8 0 7.40 1.80 6 -8 0 0.30 1.30 6 -8 0 1.20 1.30 -6 8 0 7.10 8.30 5 -8 0 3.20 6.20 -5 8 0 0.30 5.40 4 -8 0 58.79 11.30 -4 8 0 98.89 11.60 3 -8 0 7.90 5.20 -3 8 0 -4.10 4.00 2 -8 0 316.57 18.00 -2 8 0 284.37 18.00 1 -8 0 294.07 15.50 -1 8 0 311.77 18.20 0 -8 0 1.80 3.50 0 8 0 3.50 3.90 -1 -8 0 118.79 10.90 1 8 0 141.99 12.30 -2 -8 0 23.30 6.10 2 8 0 27.10 7.10 -3 -8 0 9.10 5.00 3 8 0 29.00 7.70 -4 -8 0 82.39 11.00 4 8 0 99.29 13.20 -5 -8 0 14.20 7.70 5 8 0 9.70 8.90 6 8 0 12.10 2.00 6 8 0 15.00 2.20 7 8 0 2.90 1.40 7 8 0 2.10 1.30 8 8 0 19.30 2.40 8 8 0 17.80 2.10 9 8 0 1.80 1.30 10 -9 0 -0.50 0.90 10 -9 0 -1.30 1.20 9 -9 0 2.50 1.30 9 -9 0 1.50 1.30 8 -9 0 -0.70 1.30 8 -9 0 -1.80 1.40 -8 9 0 -0.30 1.60 7 -9 0 10.70 1.90 7 -9 0 11.70 2.00 6 -9 0 122.99 5.70 6 -9 0 121.69 5.70 5 -9 0 -3.10 7.60 5 -9 0 1.90 1.50 -5 9 0 -4.30 5.60 4 -9 0 -7.80 5.90 -4 9 0 4.80 6.00 3 -9 0 47.70 9.70 -3 9 0 52.99 9.40 -2 9 0 0.20 4.90 -1 9 0 27.30 7.40 0 -9 0 69.99 8.60 0 9 0 68.19 9.40 -1 -9 0 171.38 13.90 1 9 0 173.28 14.80 -2 -9 0 0.00 4.50 2 9 0 4.80 5.40 -3 -9 0 16.20 6.50 3 9 0 9.50 6.20 -4 -9 0 -2.40 5.80 4 9 0 18.60 9.60 5 9 0 25.50 2.30 5 9 0 31.30 2.70 6 9 0 31.00 2.60 6 9 0 35.00 2.80 7 9 0 36.90 2.70 7 9 0 30.60 2.70 8 9 0 9.30 1.70 8 9 0 7.60 1.40 9 9 0 5.70 1.30 10 -10 0 -0.90 1.00 10 -10 0 1.70 0.90 9 -10 0 8.30 1.50 9 -10 0 12.80 2.10 8 -10 0 0.10 1.40 8 -10 0 2.40 1.50 -8 10 0 1.00 1.50 7 -10 0 27.60 2.80 7 -10 0 21.50 2.70 -7 10 0 27.60 2.70 6 -10 0 4.30 1.60 6 -10 0 1.90 1.50 -6 10 0 -0.40 1.50 5 -10 0 84.69 4.60 -5 10 0 96.59 4.70 -4 10 0 2.20 6.80 -4 10 0 2.90 1.40 -3 10 0 4.40 7.30 -2 10 0 57.29 10.40 -1 10 0 14.00 6.20 0 -10 0 -2.50 5.20 0 10 0 0.80 4.80 -1 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98.89 4.60 7 11 0 2.50 1.30 7 11 0 1.00 1.20 8 11 0 0.30 1.10 8 11 0 1.00 1.00 9 11 0 1.20 0.90 9 -12 0 -2.10 1.10 9 -12 0 0.30 0.90 8 -12 0 -1.60 1.20 8 -12 0 1.60 2.00 -8 12 0 -0.80 1.30 7 -12 0 2.20 1.40 -7 12 0 3.80 1.60 6 -12 0 36.90 3.10 -6 12 0 34.10 3.00 5 -12 0 16.50 2.60 -5 12 0 20.30 2.80 4 -12 0 130.09 6.10 -4 12 0 136.79 6.10 3 -12 0 1.10 1.70 -3 12 0 -1.10 1.60 -2 12 0 149.99 6.60 -1 12 0 4.70 1.60 -1 12 0 7.70 1.80 0 12 0 7.00 1.70 0 12 0 5.00 1.70 1 12 0 2.60 1.50 1 12 0 2.40 1.60 2 12 0 1.70 1.60 2 12 0 1.60 1.60 2 12 0 2.10 1.40 3 12 0 5.00 1.90 3 12 0 3.60 1.40 3 12 0 1.10 1.50 4 12 0 27.50 2.50 4 12 0 22.80 3.00 4 12 0 23.20 2.60 5 12 0 37.80 3.20 5 12 0 42.20 2.90 5 12 0 35.80 3.00 6 12 0 3.10 1.20 6 12 0 2.00 1.30 7 12 0 2.80 1.10 7 12 0 3.90 1.30 8 12 0 0.40 1.00 8 12 0 -0.70 0.80 8 -13 0 8.20 1.40 -8 13 0 9.70 1.70 7 -13 0 0.90 1.30 -7 13 0 0.50 1.40 6 -13 0 10.70 1.80 -6 13 0 10.50 1.90 5 -13 0 16.10 2.50 -5 13 0 12.90 2.10 4 -13 0 5.90 1.70 -4 13 0 5.90 1.90 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27.30 2.50 8 -10 3 26.30 2.60 8 -10 3 24.80 2.50 -9 10 -3 4.90 1.50 9 -10 3 6.40 1.40 9 -10 3 5.50 1.50 -10 10 -3 0.30 1.20 10 -10 3 1.10 1.00 10 -10 3 1.10 0.80 9 9 -3 9.60 1.20 9 9 -3 9.10 1.40 8 9 -3 1.50 1.20 8 9 -3 0.40 1.10 7 9 -3 5.40 1.50 7 9 -3 8.80 1.50 6 9 -3 8.20 1.60 6 9 -3 6.80 1.60 5 9 -3 105.89 4.80 5 9 -3 105.39 5.00 4 9 -3 -0.80 1.30 4 9 -3 1.00 1.20 -3 -9 3 -8.60 5.70 2 9 -3 4.70 7.10 -2 -9 3 -5.20 6.00 1 9 -3 25.40 8.10 -1 -9 3 18.70 7.00 0 9 -3 9.10 6.30 -1 9 -3 3.60 5.30 -2 9 -3 4.80 5.50 -3 9 -3 10.90 6.60 3 -9 3 14.50 8.00 -4 9 -3 -3.40 5.20 4 -9 3 1.10 7.40 5 -9 3 8.40 1.80 6 -9 3 158.98 6.90 7 -9 3 3.70 1.70 7 -9 3 3.60 1.50 8 -9 3 57.49 3.60 8 -9 3 56.49 3.60 -9 9 -3 -2.00 1.10 9 -9 3 1.00 1.30 9 -9 3 -1.40 1.20 -10 9 -3 1.80 1.10 10 -9 3 0.40 1.00 10 -9 3 -2.10 1.00 9 8 -3 7.20 1.30 9 8 -3 7.00 1.20 8 8 -3 7.30 1.50 8 8 -3 6.40 1.40 7 8 -3 7.50 1.60 7 8 -3 9.70 1.60 6 8 -3 2.60 1.40 6 8 -3 1.60 1.20 5 8 -3 2.10 1.20 5 8 -3 3.30 1.40 -4 -8 3 55.09 10.80 -3 -8 3 11.10 6.20 2 8 -3 15.30 6.60 -2 -8 3 19.10 6.60 1 8 -3 229.38 16.70 -1 -8 3 280.27 17.60 0 8 -3 11.40 5.50 0 -8 3 11.70 5.30 -1 8 -3 10.10 5.60 -2 8 -3 -2.90 4.10 2 -8 3 -4.70 5.10 -3 8 -3 11.00 5.10 3 -8 3 -4.10 5.10 -4 8 -3 5.40 5.50 4 -8 3 9.80 6.60 -5 8 -3 14.60 7.30 5 -8 3 21.30 9.10 6 -8 3 131.99 5.90 6 -8 3 134.39 6.10 6 -8 3 133.49 6.00 7 -8 3 0.90 1.40 7 -8 3 1.10 1.50 7 -8 3 0.80 1.50 8 -8 3 4.30 1.60 8 -8 3 3.10 1.50 9 -8 3 15.10 2.20 9 -8 3 12.20 2.10 -10 8 -3 10.90 1.70 10 -8 3 3.20 1.20 10 -8 3 7.00 1.50 11 -8 3 2.40 1.00 11 -8 3 1.40 1.00 9 7 -3 0.80 1.00 8 7 -3 17.30 2.00 8 7 -3 17.50 2.30 7 7 -3 34.20 2.80 7 7 -3 31.10 2.60 6 7 -3 5.00 1.40 6 7 -3 5.40 1.50 5 7 -3 51.39 3.20 5 7 -3 53.09 3.10 -5 -7 3 40.80 10.70 -4 -7 3 15.30 6.70 3 7 -3 51.69 9.20 -3 -7 3 55.29 9.30 2 7 -3 77.59 9.70 -2 -7 3 115.09 11.40 1 7 -3 3.70 4.30 -1 -7 3 4.70 4.60 0 7 -3 341.97 19.30 0 -7 3 372.16 19.60 0 -7 3 352.26 18.70 -1 7 -3 132.29 11.50 1 -7 3 171.98 13.20 -2 7 -3 17.40 5.10 2 -7 3 14.10 5.30 -3 7 -3 348.87 21.20 3 -7 3 408.76 23.70 -4 7 -3 10.60 5.80 4 -7 3 6.90 6.10 -5 7 -3 93.69 12.20 5 -7 3 52.89 11.30 -6 7 -3 289.27 21.80 6 -7 3 320.97 12.70 6 -7 3 324.97 24.40 6 -7 3 274.77 10.70 6 -7 3 274.67 10.80 7 -7 3 -2.30 1.40 7 -7 3 -0.10 1.40 7 -7 3 -1.40 1.30 8 -7 3 0.50 1.40 8 -7 3 1.90 1.50 8 -7 3 1.30 1.40 9 -7 3 3.00 1.50 9 -7 3 3.10 1.50 10 -7 3 23.30 2.30 10 -7 3 22.70 2.20 11 -7 3 6.70 1.10 11 -7 3 6.00 1.20 9 6 -3 30.90 2.30 8 6 -3 39.50 2.60 8 6 -3 42.90 3.00 7 6 -3 6.00 1.60 7 6 -3 11.10 1.60 6 6 -3 43.50 3.00 6 6 -3 44.70 2.80 -5 -6 3 164.08 16.50 3 6 -3 26.10 6.40 3 6 -3 24.30 6.30 2 6 -3 47.90 7.70 2 6 -3 59.29 7.70 1 6 -3 82.79 8.50 -1 -6 3 97.39 8.90 0 6 -3 153.48 11.10 0 -6 3 152.58 11.10 0 -6 3 147.89 11.40 -1 6 -3 93.19 9.10 1 -6 3 111.09 8.40 1 -6 3 118.99 10.40 -2 6 -3 111.89 10.10 2 -6 3 142.09 12.20 -3 6 -3 221.28 15.10 3 -6 3 272.77 17.90 -4 6 -3 14.10 5.60 4 -6 3 6.80 5.40 -5 6 -3 43.60 8.70 5 -6 3 40.10 9.00 -6 6 -3 6.20 5.70 6 -6 3 1.40 6.00 7 -6 3 0.50 1.30 7 -6 3 0.70 1.30 7 -6 3 -1.10 1.50 8 -6 3 28.50 2.90 8 -6 3 24.10 2.70 8 -6 3 22.90 2.70 9 -6 3 23.90 2.60 9 -6 3 24.10 2.60 9 -6 3 24.60 2.60 10 -6 3 8.10 1.70 10 -6 3 8.90 1.50 11 -6 3 6.10 1.30 11 -6 3 5.20 1.10 8 5 -3 3.80 1.30 7 5 -3 190.88 7.60 7 5 -3 190.68 7.40 6 5 -3 19.80 2.20 5 5 -3 81.89 10.60 4 5 -3 162.88 13.10 3 5 -3 13.90 4.90 3 5 -3 6.30 4.30 2 5 -3 10.40 4.20 2 5 -3 9.50 4.20 -2 -5 3 5.10 4.00 1 5 -3 4.00 3.10 1 5 -3 4.00 3.20 -1 -5 3 5.20 3.60 0 5 -3 58.19 6.20 0 5 -3 42.40 6.10 0 -5 3 60.79 7.10 -1 5 -3 362.86 17.80 1 -5 3 348.57 16.10 1 -5 3 393.76 19.00 -2 5 -3 5.50 3.40 2 -5 3 4.00 3.80 -3 5 -3 134.79 10.90 3 -5 3 152.88 12.70 -4 5 -3 43.60 7.30 4 -5 3 32.90 7.90 -5 5 -3 55.39 9.20 5 -5 3 70.99 11.60 -6 5 -3 61.89 10.20 6 -5 3 88.99 13.00 -7 5 -3 1.70 6.60 7 -5 3 3.50 1.40 7 -5 3 3.40 1.60 7 -5 3 6.20 1.60 8 -5 3 13.00 2.30 8 -5 3 15.00 2.40 8 -5 3 17.30 2.50 9 -5 3 1.10 1.40 9 -5 3 2.20 1.40 9 -5 3 4.50 1.70 10 -5 3 4.60 1.60 10 -5 3 6.30 1.40 10 -5 3 7.20 1.60 11 -5 3 9.10 1.50 8 4 -3 3.00 1.30 7 4 -3 20.30 2.30 6 4 -3 56.29 10.60 5 4 -3 290.57 18.10 4 4 -3 146.89 11.50 -4 -4 3 146.79 12.70 3 4 -3 61.99 7.20 3 4 -3 51.29 7.50 -3 -4 3 51.59 7.80 2 4 -3 552.34 22.80 2 4 -3 525.65 23.60 -2 -4 3 539.95 24.30 1 4 -3 17.80 4.00 1 4 -3 14.00 3.60 -1 -4 3 30.50 5.50 0 4 -3 178.58 9.80 0 4 -3 160.68 9.70 0 -4 3 179.18 11.00 -1 4 -3 307.87 15.00 1 -4 3 310.47 16.20 -2 4 -3 706.83 27.70 2 -4 3 701.73 29.00 2 -4 3 613.44 23.60 -3 4 -3 162.08 11.10 3 -4 3 159.98 12.40 -4 4 -3 169.28 12.20 4 -4 3 154.18 13.20 -5 4 -3 6.50 4.20 5 -4 3 2.00 4.30 -6 4 -3 11.80 5.70 6 -4 3 10.70 5.80 -7 4 -3 43.20 10.20 7 -4 3 51.49 12.00 8 -4 3 7.10 1.60 8 -4 3 9.20 1.80 8 -4 3 3.40 1.50 9 -4 3 1.10 1.40 9 -4 3 3.70 1.50 9 -4 3 3.80 1.60 10 -4 3 28.90 2.60 10 -4 3 27.40 2.40 10 -4 3 27.70 2.60 11 -4 3 2.40 1.30 12 -4 3 0.30 0.80 7 3 -3 4.80 1.40 6 3 -3 3.40 5.30 5 3 -3 105.99 10.50 -5 -3 3 86.79 11.50 4 3 -3 116.69 10.00 -4 -3 3 127.39 11.70 3 3 -3 82.99 7.50 3 3 -3 67.39 7.30 -3 -3 3 95.59 9.10 2 3 -3 79.49 6.40 2 3 -3 90.09 7.50 -2 -3 3 91.79 8.20 1 3 -3 38.90 4.80 1 3 -3 47.60 4.70 -1 -3 3 52.29 6.00 0 3 -3 425.86 17.40 0 3 -3 419.36 17.10 0 -3 3 440.06 19.10 -1 3 -3 189.28 8.80 -1 3 -3 193.28 10.20 1 -3 3 190.98 11.20 -2 3 -3 472.75 20.40 2 -3 3 486.45 21.90 -3 3 -3 199.68 12.40 3 -3 3 223.48 13.90 -4 3 -3 79.29 8.40 4 -3 3 68.89 8.90 -5 3 -3 382.66 21.10 5 -3 3 382.66 22.30 -6 3 -3 7.20 5.50 6 -3 3 10.00 5.40 -7 3 -3 11.20 6.90 7 -3 3 1.70 6.30 8 -3 3 89.79 4.70 8 -3 3 98.59 4.80 8 -3 3 91.99 4.70 9 -3 3 5.40 1.70 9 -3 3 2.90 1.40 9 -3 3 2.40 1.50 10 -3 3 6.90 1.60 10 -3 3 8.60 1.80 11 -3 3 16.60 2.00 12 -3 3 1.30 0.90 6 2 -3 15.10 6.10 -6 -2 3 17.00 7.50 5 2 -3 227.28 15.30 -5 -2 3 266.47 18.00 4 2 -3 38.60 6.10 -4 -2 3 50.89 8.20 3 2 -3 67.59 6.70 3 2 -3 63.49 6.50 -3 -2 3 67.19 8.00 2 2 -3 366.06 16.70 2 2 -3 359.76 15.20 -2 -2 3 408.06 18.30 1 2 -3 1058.29 37.70 1 2 -3 1062.79 36.40 -1 -2 3 1043.20 38.90 0 2 -3 6.70 2.10 0 2 -3 5.90 2.10 0 -2 3 12.40 3.50 -1 2 -3 685.43 25.40 -1 2 -3 669.93 23.70 1 -2 3 694.43 26.90 -2 2 -3 257.87 12.80 2 -2 3 266.47 13.90 -3 2 -3 406.86 18.60 3 -2 3 415.26 20.00 -4 2 -3 3.60 3.40 4 -2 3 -2.30 2.80 -5 2 -3 28.70 6.60 5 -2 3 33.60 7.10 -6 2 -3 11.50 5.50 6 -2 3 21.90 6.80 -7 2 -3 28.70 8.30 7 -2 3 10.80 6.80 8 -2 3 3.70 1.50 8 -2 3 0.90 1.40 9 -2 3 8.50 1.70 9 -2 3 10.60 2.00 10 -2 3 14.90 2.20 10 -2 3 17.20 2.60 11 -2 3 0.30 1.20 12 -2 3 -0.40 0.90 -7 -1 3 9.40 8.40 -6 -1 3 31.10 9.50 5 1 -3 3.60 3.30 -5 -1 3 4.90 5.20 4 1 -3 47.70 6.30 -4 -1 3 60.49 8.90 3 1 -3 5.30 2.80 3 1 -3 1.60 2.40 -3 -1 3 5.70 3.80 2 1 -3 726.63 26.30 2 1 -3 752.52 28.10 -2 -1 3 754.92 29.70 1 1 -3 413.26 14.70 1 1 -3 388.06 16.40 -1 -1 3 432.86 17.90 0 1 -3 583.44 20.50 0 1 -3 566.44 21.00 0 -1 3 601.34 22.90 -1 1 -3 87.89 4.50 -1 1 -3 88.59 5.60 1 -1 3 94.89 6.90 -2 1 -3 3161.78 104.29 2 -1 3 3101.29 105.29 -3 1 -3 321.37 15.40 3 -1 3 308.37 16.00 -4 1 -3 1398.46 52.99 4 -1 3 1450.25 54.29 -5 1 -3 476.05 23.80 5 -1 3 445.16 23.70 -6 1 -3 33.60 8.10 6 -1 3 45.40 8.90 -7 1 -3 4.90 5.60 7 -1 3 7.20 6.40 8 -1 3 -2.30 1.30 8 -1 3 0.80 1.40 9 -1 3 10.90 1.90 9 -1 3 15.10 2.30 10 -1 3 24.30 2.50 11 -1 3 -1.00 1.20 12 -1 3 0.80 1.10 9 0 -3 -0.10 1.30 8 0 -3 4.10 1.40 6 0 -3 -3.50 3.90 -6 0 3 -1.00 5.70 5 0 -3 21.90 4.90 -5 0 3 19.20 7.10 4 0 -3 1935.91 66.39 -4 0 3 1844.02 69.79 -4 0 3 1820.52 64.19 3 0 -3 12.30 3.30 -3 0 3 7.20 3.70 -3 0 3 8.70 3.00 2 0 -3 3317.37 109.49 -2 0 3 3287.17 111.79 1 0 -3 -1.20 1.60 -1 0 3 0.40 2.20 0 0 -3 108.89 5.60 0 0 -3 111.19 4.80 0 0 3 110.19 6.80 -1 0 -3 2.30 1.60 1 0 3 3.50 2.60 1 0 3 -0.30 2.30 -2 0 -3 3464.85 114.89 2 0 3 3687.23 118.69 2 0 3 3525.75 118.09 -3 0 -3 174.48 7.70 3 0 3 189.18 10.90 3 0 3 187.48 11.80 -4 0 -3 157.88 7.90 4 0 3 148.49 11.20 -5 0 -3 3.70 4.10 5 0 3 4.70 4.00 -6 0 -3 6.40 5.60 6 0 3 8.70 5.20 -7 0 -3 9.80 6.50 7 0 3 3.90 6.00 -8 0 -3 78.39 17.80 8 0 3 70.89 3.90 8 0 3 69.89 3.90 9 0 3 9.60 1.80 9 0 3 10.00 1.90 10 0 3 103.69 4.90 11 0 3 0.20 1.20 10 -1 -3 6.50 1.40 9 -1 -3 17.20 2.30 8 -1 -3 30.40 2.50 -7 1 3 14.00 9.00 5 -1 -3 50.69 7.20 5 -1 -3 42.70 8.50 4 -1 -3 55.79 8.30 4 -1 -3 61.29 6.30 -4 1 3 34.40 5.40 3 -1 -3 518.45 21.00 3 -1 -3 497.25 23.60 -3 1 3 515.85 19.40 2 -1 -3 97.69 6.20 -2 1 3 80.79 4.40 1 -1 -3 9.90 2.30 -1 1 3 15.50 3.50 0 -1 -3 646.24 21.80 0 1 3 578.24 22.50 0 1 3 606.14 21.10 -1 -1 -3 798.62 27.80 1 1 3 766.22 28.90 1 1 3 851.41 29.00 -2 -1 -3 2065.79 67.69 2 1 3 2050.19 69.19 2 1 3 2021.00 70.39 -3 -1 -3 236.48 10.80 3 1 3 235.98 13.90 3 1 3 247.98 12.70 -4 -1 -3 270.87 12.90 4 1 3 272.47 14.80 4 1 3 264.87 16.60 5 1 3 147.99 11.50 5 1 3 132.29 12.70 -6 -1 -3 34.90 7.90 6 1 3 35.10 7.70 -7 -1 -3 4.20 5.40 8 1 3 0.90 1.40 8 1 3 0.70 1.30 9 1 3 7.30 1.60 9 1 3 7.80 1.70 10 1 3 2.80 1.40 10 -2 -3 -0.60 1.10 10 -2 -3 2.50 1.80 9 -2 -3 69.59 3.80 9 -2 -3 68.29 3.90 8 -2 -3 24.40 2.50 8 -2 -3 23.10 2.60 -7 2 3 33.60 11.00 6 -2 -3 126.49 14.60 5 -2 -3 60.79 9.30 5 -2 -3 54.29 7.10 4 -2 -3 14.50 4.90 4 -2 -3 7.20 3.00 -4 2 3 15.70 3.70 3 -2 -3 1134.19 41.10 3 -2 -3 1147.79 44.70 -3 2 3 1151.68 39.90 2 -2 -3 1.30 2.00 2 -2 -3 3.50 2.90 -2 2 3 5.50 1.90 1 -2 -3 15.80 2.90 -1 2 3 16.80 2.40 0 -2 -3 474.35 16.50 0 2 3 390.56 15.80 0 2 3 429.26 16.80 -1 -2 -3 1806.52 58.79 1 2 3 1802.82 58.59 1 2 3 1656.73 59.59 -2 -2 -3 1740.23 57.89 2 2 3 1648.83 57.39 2 2 3 1738.53 59.99 -3 -2 -3 569.44 22.60 3 2 3 588.54 25.60 3 2 3 570.14 22.90 -4 -2 -3 666.13 26.10 4 2 3 613.14 26.30 4 2 3 660.33 29.70 -5 -2 -3 158.38 11.10 5 2 3 167.58 12.40 5 2 3 179.48 14.90 6 2 3 100.29 12.40 6 2 3 83.09 12.10 -7 -2 -3 14.20 6.90 8 2 3 -2.30 1.30 9 2 3 0.30 1.30 11 -3 -3 1.30 1.00 10 -3 -3 3.10 1.20 10 -3 -3 1.90 1.40 9 -3 -3 6.70 1.50 9 -3 -3 9.50 1.80 8 -3 -3 10.90 1.90 8 -3 -3 17.60 2.20 6 -3 -3 10.60 6.50 5 -3 -3 156.68 14.30 4 -3 -3 101.99 7.70 4 -3 -3 101.19 10.80 -4 3 3 101.19 7.80 3 -3 -3 1448.85 53.29 3 -3 -3 1368.36 48.60 -3 3 3 1345.57 48.20 2 -3 -3 25.50 3.70 2 -3 -3 13.90 4.20 -2 3 3 24.30 3.50 1 -3 -3 627.94 24.30 1 -3 -3 597.84 22.70 -1 3 3 611.14 22.40 0 -3 -3 777.92 26.70 0 3 3 699.93 26.30 0 3 3 711.13 26.30 -1 -3 -3 1864.61 62.39 1 3 3 1819.12 62.89 1 3 3 1850.11 60.59 -2 -3 -3 790.52 29.10 2 3 3 814.22 30.70 2 3 3 734.93 26.80 -3 -3 -3 40.80 5.80 3 3 3 45.40 4.50 3 3 3 56.99 7.00 -4 -3 -3 1608.24 56.99 4 3 3 1585.74 55.89 4 3 3 1521.25 59.69 -5 -3 -3 215.88 13.80 5 3 3 210.48 16.30 6 3 3 116.79 13.60 8 3 3 14.30 2.30 9 3 3 8.80 1.80 11 -4 -3 2.60 1.20 11 -4 -3 4.30 1.00 10 -4 -3 1.30 1.40 10 -4 -3 1.20 1.10 9 -4 -3 3.60 1.60 9 -4 -3 4.30 1.40 8 -4 -3 5.90 1.60 8 -4 -3 2.80 1.40 7 -4 -3 23.90 2.40 7 -4 -3 26.20 2.50 7 -4 -3 23.10 9.70 6 -4 -3 39.10 9.30 5 -4 -3 970.60 44.20 4 -4 -3 14.00 3.90 4 -4 -3 5.50 4.50 -4 4 3 14.50 4.40 3 -4 -3 178.88 9.90 3 -4 -3 185.48 13.10 -3 4 3 181.68 10.40 2 -4 -3 33.60 4.40 2 -4 -3 26.10 5.20 -2 4 3 37.60 4.40 1 -4 -3 4.90 2.30 1 -4 -3 8.90 3.00 -1 4 3 7.30 2.90 0 -4 -3 536.75 21.30 0 4 3 555.24 21.00 0 4 3 570.24 21.90 -1 -4 -3 47.00 5.00 1 4 3 50.99 5.50 -2 -4 -3 209.48 11.70 2 4 3 224.98 12.60 -3 -4 -3 35.30 6.20 3 4 3 35.20 6.40 -4 -4 -3 22.20 5.50 4 4 3 29.60 6.90 -5 -4 -3 698.23 31.90 5 4 3 792.72 35.90 -6 -4 -3 -0.40 5.00 6 4 3 14.10 7.40 7 4 3 -3.50 7.40 8 4 3 2.50 1.40 9 4 3 41.80 3.10 11 -5 -3 19.60 1.60 11 -5 -3 18.60 1.70 10 -5 -3 0.40 1.10 10 -5 -3 0.20 1.30 9 -5 -3 2.20 1.50 9 -5 -3 -1.60 1.10 8 -5 -3 160.88 6.50 8 -5 -3 141.29 6.50 7 -5 -3 2.90 1.50 7 -5 -3 2.60 1.40 6 -5 -3 47.10 10.30 5 -5 -3 12.60 6.60 4 -5 -3 116.89 12.10 -4 5 3 89.49 8.90 3 -5 -3 590.64 27.00 3 -5 -3 560.44 22.60 -3 5 3 533.75 23.60 2 -5 -3 688.63 28.10 2 -5 -3 647.24 25.10 -2 5 3 597.84 25.40 1 -5 -3 10.50 3.10 1 -5 -3 10.10 3.20 -1 5 3 10.20 3.30 0 -5 -3 5.60 2.70 0 5 3 5.40 2.90 -1 -5 -3 62.19 6.10 1 5 3 79.39 7.10 -2 -5 -3 187.98 11.00 2 5 3 150.98 10.70 -3 -5 -3 288.27 15.90 3 5 3 308.77 17.40 -4 -5 -3 340.07 18.40 4 5 3 317.37 19.80 -5 -5 -3 402.36 21.50 5 5 3 368.56 23.00 -6 -5 -3 73.29 10.90 6 5 3 75.29 12.80 7 5 3 269.17 23.70 8 5 3 15.60 2.10 8 5 3 13.80 2.20 9 5 3 1.10 1.50 11 -6 -3 0.80 0.90 11 -6 -3 0.50 0.90 10 -6 -3 21.00 2.30 10 -6 -3 21.80 2.10 9 -6 -3 27.90 2.70 9 -6 -3 31.80 2.60 8 -6 -3 108.49 5.30 8 -6 -3 108.99 5.10 7 -6 -3 187.48 7.70 7 -6 -3 189.88 7.70 6 -6 -3 9.50 6.50 5 -6 -3 21.00 7.20 4 -6 -3 92.79 11.20 -4 6 3 93.49 9.20 3 -6 -3 50.29 8.30 3 -6 -3 45.50 5.60 2 -6 -3 202.18 11.10 2 -6 -3 214.28 13.50 -2 6 3 193.48 12.20 1 -6 -3 1.40 2.80 1 -6 -3 5.10 3.00 -1 6 3 4.80 3.40 0 -6 -3 12.50 3.60 0 6 3 17.00 4.40 -1 -6 -3 342.07 16.50 1 6 3 333.17 17.40 -2 -6 -3 10.40 4.10 2 6 3 4.00 3.40 -3 -6 -3 111.39 10.00 3 6 3 111.09 10.90 -4 -6 -3 628.24 29.50 4 6 3 657.73 31.40 -5 -6 -3 154.58 13.60 5 6 3 182.98 16.30 -6 -6 -3 38.00 8.90 6 6 3 46.60 10.60 7 6 3 72.79 3.80 7 6 3 63.79 3.80 8 6 3 13.20 1.90 8 6 3 12.50 1.90 9 6 3 27.00 2.60 11 -7 -3 3.00 0.90 11 -7 -3 4.10 1.00 10 -7 -3 57.49 3.30 10 -7 -3 56.99 3.00 9 -7 -3 1.90 1.30 9 -7 -3 1.80 1.50 8 -7 -3 22.80 2.70 8 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12 -4 11.30 1.80 8 -12 4 11.50 1.70 -9 12 -4 -0.40 0.90 9 -12 4 0.00 0.80 8 11 -4 2.60 0.90 8 11 -4 2.20 0.80 7 11 -4 4.40 1.10 7 11 -4 3.70 1.10 6 11 -4 -0.20 1.10 6 11 -4 0.80 1.10 5 11 -4 0.00 1.20 5 11 -4 -0.40 1.20 4 11 -4 17.30 2.40 4 11 -4 25.40 2.40 3 11 -4 8.50 1.70 3 11 -4 9.20 1.80 2 11 -4 93.39 4.50 2 11 -4 85.09 4.40 1 11 -4 25.00 2.90 1 11 -4 25.10 2.70 1 11 -4 31.60 2.70 0 11 -4 28.10 2.80 -1 11 -4 10.30 2.00 1 -11 4 11.70 2.00 -2 11 -4 24.10 2.70 2 -11 4 24.80 3.00 -3 11 -4 8.10 1.70 3 -11 4 5.90 1.80 -4 11 -4 0.40 1.50 4 -11 4 4.80 1.70 -5 11 -4 137.89 6.20 5 -11 4 140.49 6.40 -6 11 -4 4.60 1.60 6 -11 4 3.60 1.60 -7 11 -4 29.70 2.70 7 -11 4 30.30 2.70 -8 11 -4 4.10 1.40 8 -11 4 1.30 1.20 -9 11 -4 6.80 1.30 9 -11 4 7.00 1.20 8 10 -4 0.90 1.00 8 10 -4 -0.10 0.90 7 10 -4 3.30 1.30 7 10 -4 4.50 1.20 6 10 -4 15.70 2.00 6 10 -4 7.00 1.60 5 10 -4 4.50 1.40 5 10 -4 5.60 1.60 4 10 -4 6.80 1.60 4 10 -4 6.50 1.50 3 10 -4 122.19 5.50 3 10 -4 117.99 5.30 2 10 -4 12.30 2.10 2 10 -4 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9 -9 4 5.60 1.40 9 -9 4 6.80 1.60 -10 9 -4 6.90 1.30 10 -9 4 4.50 1.10 10 -9 4 7.70 1.40 9 8 -4 3.30 0.90 9 8 -4 0.30 1.10 8 8 -4 3.60 1.30 8 8 -4 3.40 1.20 7 8 -4 0.00 1.10 7 8 -4 0.00 1.10 6 8 -4 2.70 1.40 6 8 -4 0.30 1.20 5 8 -4 3.00 1.30 5 8 -4 3.40 1.40 4 8 -4 99.59 4.50 4 8 -4 94.09 4.60 -3 -8 4 18.60 7.90 -2 -8 4 13.30 6.80 1 8 -4 1.00 5.40 -1 -8 4 -2.30 5.10 0 8 -4 18.90 6.60 0 -8 4 20.80 10.90 -1 8 -4 11.10 5.70 -2 8 -4 116.89 12.40 2 -8 4 133.99 13.90 -3 8 -4 49.00 9.10 3 -8 4 51.39 10.70 -4 8 -4 101.39 12.20 4 -8 4 120.49 15.10 -5 8 -4 0.50 6.20 5 -8 4 3.80 7.00 5 -8 4 1.30 1.40 5 -8 4 0.90 1.40 6 -8 4 68.79 4.10 6 -8 4 70.39 4.10 6 -8 4 72.49 4.30 7 -8 4 154.98 6.70 7 -8 4 154.98 6.70 7 -8 4 158.88 6.90 8 -8 4 61.49 3.70 8 -8 4 56.79 3.70 9 -8 4 6.40 1.50 9 -8 4 10.10 1.80 -10 8 -4 3.00 1.20 10 -8 4 2.50 1.30 10 -8 4 2.30 1.20 9 7 -4 14.00 1.50 8 7 -4 3.10 1.40 8 7 -4 5.90 1.30 7 7 -4 0.90 1.30 7 7 -4 -0.20 1.10 6 7 -4 2.10 1.20 6 7 -4 1.90 1.40 5 7 -4 34.50 2.80 5 7 -4 36.20 2.60 -4 -7 4 1.30 6.20 2 7 -4 11.80 5.60 1 7 -4 9.90 4.70 -1 -7 4 9.60 5.40 0 7 -4 621.14 28.90 0 -7 4 641.34 29.40 0 -7 4 592.64 28.00 -1 7 -4 34.70 7.10 1 -7 4 26.90 7.00 -2 7 -4 36.40 7.50 2 -7 4 46.20 9.20 -3 7 -4 4.30 4.60 3 -7 4 -5.50 4.70 -4 7 -4 70.99 10.30 4 -7 4 82.39 12.60 -5 7 -4 2.30 5.60 5 -7 4 0.80 6.40 6 -7 4 4.20 1.60 6 -7 4 5.00 1.60 6 -7 4 7.30 1.70 7 -7 4 32.60 3.00 7 -7 4 36.60 3.00 7 -7 4 36.00 3.00 8 -7 4 23.50 2.70 8 -7 4 27.10 2.80 8 -7 4 26.70 2.80 9 -7 4 5.00 1.50 9 -7 4 3.70 1.60 10 -7 4 40.40 2.70 10 -7 4 40.60 2.80 11 -7 4 8.60 1.40 11 -7 4 7.30 1.20 9 6 -4 0.50 1.00 8 6 -4 5.50 1.30 8 6 -4 7.60 1.60 7 6 -4 3.30 1.50 7 6 -4 4.20 1.40 6 6 -4 129.79 5.50 6 6 -4 126.89 5.60 4 6 -4 10.60 6.30 3 6 -4 8.90 5.20 2 6 -4 292.27 17.10 2 6 -4 306.57 17.80 1 6 -4 81.89 8.60 1 6 -4 70.09 8.30 -1 -6 4 88.59 9.60 0 6 -4 325.67 17.60 0 -6 4 319.17 18.30 -1 6 -4 2.00 3.40 1 -6 4 0.10 3.10 1 -6 4 9.20 4.80 -2 6 -4 29.10 6.30 2 -6 4 18.80 5.80 -3 6 -4 31.70 6.80 3 -6 4 23.40 6.60 -4 6 -4 7.90 5.20 4 -6 4 2.10 5.50 -5 6 -4 95.09 11.80 5 -6 4 113.79 13.60 -6 6 -4 142.59 14.70 6 -6 4 113.19 15.10 7 -6 4 158.88 6.90 7 -6 4 149.59 6.70 7 -6 4 167.68 6.90 8 -6 4 1.80 1.50 8 -6 4 1.40 1.50 8 -6 4 -0.40 1.40 9 -6 4 19.50 2.50 9 -6 4 17.20 2.40 9 -6 4 14.50 2.40 10 -6 4 -1.10 1.10 10 -6 4 1.20 1.30 11 -6 4 7.60 1.40 9 5 -4 1.10 1.10 8 5 -4 4.50 1.30 7 5 -4 16.70 2.20 7 5 -4 19.60 2.40 6 5 -4 35.60 2.80 6 5 -4 41.80 2.70 5 5 -4 33.10 8.20 4 5 -4 177.48 14.00 3 5 -4 142.09 11.70 -3 -5 4 131.29 18.20 2 5 -4 5.10 3.80 2 5 -4 6.60 4.00 -2 -5 4 7.40 5.00 1 5 -4 -1.40 2.80 1 5 -4 2.90 3.00 -1 -5 4 -4.50 3.40 0 5 -4 0.30 2.80 0 5 -4 6.80 3.10 0 -5 4 6.90 4.00 -1 5 -4 24.80 5.10 1 -5 4 17.00 5.30 -2 5 -4 7.60 3.80 2 -5 4 3.00 3.80 -3 5 -4 190.08 13.00 3 -5 4 184.18 14.60 -4 5 -4 67.29 8.70 4 -5 4 77.19 10.70 -5 5 -4 1.40 4.40 5 -5 4 -1.00 5.20 -6 5 -4 7.60 6.00 6 -5 4 7.70 6.80 7 -5 4 26.30 2.70 7 -5 4 28.20 2.80 7 -5 4 28.70 2.70 8 -5 4 -2.00 1.40 8 -5 4 -0.30 1.40 8 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10 -5 4.50 1.40 3 10 -5 -0.30 1.30 3 10 -5 -0.20 1.30 2 10 -5 9.60 1.70 2 10 -5 14.90 2.20 1 10 -5 23.80 2.50 1 10 -5 24.60 2.50 0 10 -5 18.90 9.70 0 10 -5 2.40 1.60 0 -10 5 4.90 1.70 -1 10 -5 29.80 13.50 -1 10 -5 17.60 2.50 1 -10 5 17.10 2.30 -2 10 -5 19.00 2.40 2 -10 5 22.70 2.70 -3 10 -5 11.30 1.90 3 -10 5 14.50 2.50 -4 10 -5 8.30 1.70 4 -10 5 8.60 1.80 -5 10 -5 3.10 1.50 5 -10 5 3.00 1.60 6 -10 5 1.40 1.50 -7 10 -5 -2.40 1.30 7 -10 5 1.80 1.50 -8 10 -5 5.80 1.60 8 -10 5 4.20 1.50 -9 10 -5 36.90 2.50 9 -10 5 37.60 2.50 8 9 -5 0.60 1.10 8 9 -5 1.90 1.00 7 9 -5 4.00 1.30 7 9 -5 4.10 1.20 6 9 -5 1.00 1.10 6 9 -5 3.20 1.40 5 9 -5 1.00 1.10 5 9 -5 0.30 1.30 4 9 -5 0.60 1.20 4 9 -5 -0.40 1.30 3 9 -5 76.09 4.00 3 9 -5 72.09 3.80 2 9 -5 41.50 2.90 2 9 -5 42.30 2.90 -2 -9 5 42.30 10.70 0 9 -5 4.90 6.90 -1 9 -5 27.40 9.00 -2 9 -5 0.20 6.40 -3 9 -5 75.29 11.70 -3 9 -5 73.19 3.90 3 -9 5 72.79 4.30 4 -9 5 4.70 1.60 5 -9 5 4.60 1.60 6 -9 5 14.30 2.50 7 -9 5 20.70 2.60 8 -9 5 11.20 1.80 8 -9 5 12.30 2.20 -9 9 -5 -2.40 1.20 9 -9 5 0.10 1.30 9 -9 5 0.30 1.20 -10 9 -5 11.80 1.60 10 -9 5 15.10 1.60 10 -9 5 15.70 1.60 9 8 -5 2.60 0.90 8 8 -5 4.20 1.20 8 8 -5 1.60 1.00 7 8 -5 13.80 1.90 7 8 -5 16.80 2.10 6 8 -5 21.50 2.20 6 8 -5 22.20 2.50 5 8 -5 0.70 1.10 5 8 -5 -0.30 1.30 4 8 -5 56.79 3.50 4 8 -5 62.59 3.40 3 8 -5 6.40 1.50 3 8 -5 6.80 1.60 -3 -8 5 11.90 8.10 -1 -8 5 24.80 8.00 0 8 -5 7.10 6.00 -1 8 -5 25.70 7.00 -2 8 -5 4.50 5.50 2 -8 5 3.50 6.10 -3 8 -5 26.20 7.60 3 -8 5 43.50 11.00 -4 8 -5 74.49 13.10 4 -8 5 78.89 14.30 5 -8 5 46.50 3.30 5 -8 5 48.10 3.40 6 -8 5 -0.20 1.40 6 -8 5 0.90 1.50 7 -8 5 13.40 2.40 7 -8 5 15.00 2.50 7 -8 5 10.50 2.00 8 -8 5 8.20 1.70 8 -8 5 8.80 1.80 9 -8 5 26.20 2.40 9 -8 5 30.80 2.60 -10 8 -5 3.50 1.30 10 -8 5 2.10 1.30 10 -8 5 1.80 1.10 9 7 -5 3.00 1.00 8 7 -5 9.70 1.60 8 7 -5 7.90 1.30 7 7 -5 3.30 1.30 7 7 -5 3.50 1.40 6 7 -5 15.30 2.30 6 7 -5 16.50 2.10 5 7 -5 0.20 1.30 5 7 -5 -0.10 1.10 4 7 -5 38.50 2.90 4 7 -5 41.80 2.70 1 7 -5 28.40 7.10 0 7 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21.30 2.40 -2 -8 6 27.50 9.30 -1 8 -6 12.60 7.30 -2 8 -6 24.80 8.30 2 -8 6 26.00 9.80 -3 8 -6 -2.00 5.40 3 -8 6 1.00 7.90 -4 8 -6 23.30 7.70 4 -8 6 20.90 10.10 4 -8 6 21.40 2.60 5 -8 6 62.89 3.80 6 -8 6 61.59 3.90 7 -8 6 -0.80 1.50 7 -8 6 -0.20 1.40 8 -8 6 61.99 3.70 8 -8 6 67.69 3.80 9 -8 6 4.20 1.40 9 -8 6 5.60 1.60 -10 8 -6 27.40 2.20 10 -8 6 34.30 2.30 10 -8 6 31.70 2.10 9 7 -6 -0.20 0.80 8 7 -6 2.30 1.20 8 7 -6 4.20 1.10 7 7 -6 6.40 1.50 7 7 -6 4.80 1.30 6 7 -6 198.78 7.60 6 7 -6 193.18 7.80 5 7 -6 56.99 3.40 5 7 -6 60.99 3.60 4 7 -6 85.59 4.10 4 7 -6 79.59 4.20 0 7 -6 -0.70 4.50 0 -7 6 7.60 7.00 -1 7 -6 5.20 5.30 1 -7 6 19.60 7.20 -2 7 -6 46.60 8.60 2 -7 6 49.60 10.50 -3 7 -6 29.20 7.40 3 -7 6 23.50 8.40 -4 7 -6 0.00 5.10 4 -7 6 -5.80 6.40 -5 7 -6 101.99 14.10 5 -7 6 93.19 4.80 5 -7 6 99.69 4.70 5 -7 6 79.69 15.80 6 -7 6 0.90 1.40 6 -7 6 4.30 1.60 7 -7 6 13.10 2.30 7 -7 6 11.10 2.00 7 -7 6 12.60 2.00 8 -7 6 0.00 1.30 8 -7 6 1.20 1.50 8 -7 6 4.50 1.60 9 -7 6 1.40 1.30 9 -7 6 2.70 1.40 10 -7 6 18.80 2.00 10 -7 6 20.20 2.00 -11 7 -6 1.60 0.90 11 -7 6 1.50 0.90 9 6 -6 6.60 1.10 8 6 -6 0.60 1.00 7 6 -6 21.40 2.20 7 6 -6 22.90 2.40 6 6 -6 33.80 2.60 6 6 -6 35.00 2.80 5 6 -6 1.50 1.30 5 6 -6 1.20 1.20 4 6 -6 17.00 7.70 4 6 -6 12.50 2.00 3 6 -6 85.09 11.60 2 6 -6 199.48 15.00 1 6 -6 55.79 8.50 -1 -6 6 71.79 11.50 0 6 -6 34.50 6.80 0 6 -6 35.30 6.90 0 -6 6 27.00 7.20 -1 6 -6 45.90 7.70 1 -6 6 42.80 9.00 -2 6 -6 28.90 6.50 2 -6 6 41.20 9.10 -3 6 -6 1.70 4.60 3 -6 6 0.80 5.30 -4 6 -6 3.80 4.90 4 -6 6 6.50 6.60 -5 6 -6 -2.30 4.70 5 -6 6 5.60 7.50 6 -6 6 41.70 3.10 6 -6 6 38.70 3.10 6 -6 6 36.80 3.00 7 -6 6 16.80 2.50 7 -6 6 19.80 2.60 7 -6 6 16.80 2.70 8 -6 6 31.50 2.90 8 -6 6 31.50 2.80 8 -6 6 31.30 3.10 9 -6 6 10.00 1.80 9 -6 6 9.20 1.80 9 -6 6 13.10 2.20 10 -6 6 1.80 1.20 10 -6 6 0.10 1.20 10 -6 6 0.30 1.20 11 -6 6 -1.00 1.00 9 5 -6 1.30 1.00 8 5 -6 0.40 1.10 7 5 -6 54.29 3.20 7 5 -6 49.80 3.20 6 5 -6 77.19 4.10 6 5 -6 81.49 4.00 5 5 -6 64.89 3.40 5 5 -6 65.29 3.60 5 5 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6.90 1.70 -2 -10 7 11.20 2.10 1 10 -7 -0.50 1.20 1 10 -7 1.00 2.30 -1 -10 7 0.40 1.60 0 10 -7 15.80 2.30 0 -10 7 19.20 2.80 1 -10 7 39.80 3.40 -2 10 -7 5.20 1.70 2 -10 7 5.50 1.70 -3 10 -7 25.80 2.60 3 -10 7 26.50 2.90 -4 10 -7 19.70 2.50 4 -10 7 21.10 2.60 -5 10 -7 27.20 2.60 5 -10 7 30.70 2.90 -6 10 -7 18.50 2.30 6 -10 7 17.30 2.50 -7 10 -7 6.40 1.50 7 -10 7 4.50 1.60 -8 10 -7 -1.00 1.10 8 -10 7 1.00 1.20 -9 10 -7 9.30 1.60 9 -10 7 11.60 1.60 8 9 -7 0.70 0.80 8 9 -7 1.60 0.80 7 9 -7 0.10 0.90 7 9 -7 0.70 1.00 6 9 -7 3.40 1.20 6 9 -7 0.70 1.00 5 9 -7 16.30 2.20 5 9 -7 14.90 2.00 4 9 -7 0.80 1.30 4 9 -7 0.90 1.20 3 9 -7 3.60 1.50 3 9 -7 5.40 1.50 -3 -9 7 5.30 2.40 2 9 -7 55.19 3.40 2 9 -7 59.99 3.40 -2 -9 7 56.29 3.90 1 9 -7 69.69 3.80 1 9 -7 66.99 4.20 -1 -9 7 74.59 4.40 0 9 -7 54.69 3.30 0 -9 7 50.29 3.60 1 -9 7 18.00 2.70 -2 9 -7 22.50 2.50 2 -9 7 31.30 3.00 -3 9 -7 28.00 2.50 3 -9 7 26.40 2.80 4 -9 7 75.19 4.30 5 -9 7 11.70 1.90 6 -9 7 5.30 1.70 7 -9 7 1.60 1.40 8 -9 7 2.90 1.40 -9 9 -7 -0.60 1.10 9 -9 7 0.80 1.10 -10 9 -7 15.70 1.50 10 -9 7 13.80 1.60 8 8 -7 0.90 1.00 8 8 -7 0.00 0.80 7 8 -7 -1.50 1.00 7 8 -7 0.20 1.00 6 8 -7 0.50 1.10 6 8 -7 1.90 1.30 5 8 -7 2.20 1.30 5 8 -7 2.60 1.20 4 8 -7 26.20 2.50 4 8 -7 23.70 2.30 3 8 -7 15.20 2.20 3 8 -7 14.50 2.10 3 8 -7 10.40 1.90 2 8 -7 248.48 9.30 2 8 -7 252.97 9.40 1 8 -7 6.70 1.60 -2 8 -7 111.19 14.00 2 -8 7 168.08 19.00 -3 8 -7 -1.90 6.60 3 -8 7 15.30 9.40 3 -8 7 1.70 1.50 4 -8 7 218.28 8.70 5 -8 7 2.70 1.50 6 -8 7 3.40 1.60 7 -8 7 4.40 1.60 8 -8 7 1.40 1.40 8 -8 7 0.80 1.30 9 -8 7 1.50 1.20 9 -8 7 -2.10 1.20 -10 8 -7 1.60 1.00 10 -8 7 1.70 1.00 10 -8 7 5.40 1.30 9 7 -7 1.80 0.80 8 7 -7 25.70 2.00 8 7 -7 22.30 1.80 7 7 -7 5.90 1.30 7 7 -7 9.40 1.60 6 7 -7 3.10 1.20 6 7 -7 4.00 1.40 5 7 -7 8.50 1.50 5 7 -7 11.20 1.70 4 7 -7 144.99 6.20 4 7 -7 149.19 6.10 4 7 -7 148.09 6.30 3 7 -7 49.80 3.30 3 7 -7 49.40 3.00 3 7 -7 49.60 3.00 2 7 -7 116.09 13.60 0 -7 7 2.70 7.10 -1 7 -7 26.30 7.40 1 -7 7 12.40 7.30 -2 7 -7 75.19 10.90 2 -7 7 98.99 14.00 -3 7 -7 87.39 11.50 3 -7 7 81.19 13.60 -4 7 -7 2.10 6.30 4 -7 7 5.50 7.90 4 -7 7 -1.50 2.10 5 -7 7 52.29 3.50 5 -7 7 54.59 3.50 6 -7 7 14.50 2.40 6 -7 7 9.70 1.90 7 -7 7 25.30 2.80 7 -7 7 34.00 2.80 7 -7 7 24.40 2.80 8 -7 7 1.80 1.40 8 -7 7 2.20 1.50 8 -7 7 5.10 1.60 9 -7 7 31.80 2.50 9 -7 7 29.20 2.60 10 -7 7 33.60 2.30 10 -7 7 32.80 2.20 9 6 -7 2.00 0.80 8 6 -7 -0.60 0.90 7 6 -7 27.10 2.20 7 6 -7 27.30 2.50 6 6 -7 2.80 1.30 6 6 -7 3.70 1.30 5 6 -7 24.50 2.40 5 6 -7 28.70 2.60 5 6 -7 32.40 2.60 4 6 -7 127.39 5.60 4 6 -7 133.89 5.60 4 6 -7 127.59 5.50 3 6 -7 235.28 18.30 2 6 -7 92.79 11.70 1 6 -7 5.40 5.00 -1 -6 7 -1.10 6.50 0 6 -7 9.60 5.70 0 -6 7 9.90 6.70 -1 6 -7 -2.40 3.90 1 -6 7 11.80 6.50 -2 6 -7 134.39 12.00 2 -6 7 106.19 13.60 -3 6 -7 57.39 9.70 3 -6 7 79.79 12.00 -4 6 -7 23.80 7.30 4 -6 7 30.00 8.30 -5 6 -7 65.29 11.40 5 -6 7 59.99 12.30 5 -6 7 56.89 4.90 6 -6 7 11.60 2.10 6 -6 7 8.40 1.90 6 -6 7 12.30 1.90 7 -6 7 116.79 5.40 7 -6 7 105.89 5.50 7 -6 7 114.09 5.50 8 -6 7 0.90 1.40 8 -6 7 0.10 1.40 8 -6 7 0.80 1.30 9 -6 7 19.80 2.30 9 -6 7 13.40 2.10 9 -6 7 15.90 2.30 10 -6 7 10.30 1.70 10 -6 7 10.60 2.40 11 -6 7 -1.50 0.90 9 5 -7 4.40 1.00 8 5 -7 2.10 1.10 7 5 -7 4.90 1.30 7 5 -7 6.60 1.60 6 5 -7 16.20 2.20 6 5 -7 19.40 2.30 6 5 -7 20.80 2.40 5 5 -7 -0.80 1.20 5 5 -7 0.20 1.10 5 5 -7 1.10 1.30 4 5 -7 20.90 7.20 3 5 -7 19.70 6.60 2 5 -7 27.90 6.70 -2 -5 7 29.80 9.50 1 5 -7 261.27 16.40 -1 -5 7 228.68 18.40 0 5 -7 10.40 4.50 0 -5 7 9.30 5.90 -1 5 -7 99.29 9.50 1 -5 7 108.29 12.30 -2 5 -7 30.20 6.70 2 -5 7 32.90 8.10 -3 5 -7 137.89 12.40 3 -5 7 160.38 14.80 -4 5 -7 53.59 8.90 4 -5 7 57.39 10.90 -5 5 -7 17.30 6.70 5 -5 7 15.60 7.80 6 -5 7 71.49 4.20 6 -5 7 74.49 4.00 6 -5 7 76.69 4.10 7 -5 7 86.89 4.70 7 -5 7 91.49 4.80 7 -5 7 88.89 4.70 8 -5 7 28.80 3.00 8 -5 7 32.70 2.90 8 -5 7 31.50 2.80 9 -5 7 0.00 1.30 9 -5 7 1.70 1.40 9 -5 7 1.90 1.50 10 -5 7 2.00 1.30 10 -5 7 0.30 1.10 11 -5 7 13.50 1.70 9 4 -7 0.10 0.90 8 4 -7 1.90 1.10 7 4 -7 86.59 4.20 7 4 -7 87.59 4.10 6 4 -7 51.59 3.30 6 4 -7 50.29 3.40 6 4 -7 51.59 3.10 5 4 -7 262.97 9.50 5 4 -7 250.47 9.70 5 4 -7 265.57 9.70 4 4 -7 -4.70 4.50 3 4 -7 1.80 4.30 -3 -4 7 -3.10 6.80 2 4 -7 5.70 4.00 -2 -4 7 -2.00 5.40 1 4 -7 105.69 9.80 -1 -4 7 105.19 12.50 0 4 -7 33.10 5.90 0 -4 7 33.20 7.50 -1 4 -7 4.00 3.00 -1 4 -7 2.00 3.10 1 -4 7 -1.10 3.80 -2 4 -7 199.78 12.90 2 -4 7 183.18 15.30 -3 4 -7 86.19 9.30 3 -4 7 87.79 11.10 -4 4 -7 58.99 8.80 4 -4 7 44.00 9.20 -5 4 -7 13.60 5.20 5 -4 7 22.20 7.60 -6 4 -7 83.19 11.60 6 -4 7 109.89 15.40 7 -4 7 183.48 7.90 7 -4 7 187.08 7.80 7 -4 7 200.88 7.90 8 -4 7 4.30 1.60 8 -4 7 3.20 1.70 8 -4 7 5.70 1.60 9 -4 7 22.30 2.60 9 -4 7 16.10 2.30 10 -4 7 4.00 1.40 10 -4 7 2.10 1.40 11 -4 7 0.00 1.00 11 -4 7 3.10 1.20 9 3 -7 8.60 1.30 8 3 -7 0.90 1.30 8 3 -7 0.00 1.10 7 3 -7 9.10 1.50 7 3 -7 10.30 1.70 6 3 -7 467.05 16.20 6 3 -7 476.55 16.50 5 3 -7 0.40 1.40 5 3 -7 1.10 5.40 4 3 -7 153.58 13.20 -4 -3 7 164.78 17.00 3 3 -7 40.70 7.60 -3 -3 7 34.60 8.80 2 3 -7 41.50 6.90 -2 -3 7 29.60 8.20 1 3 -7 124.59 10.40 -1 -3 7 121.89 12.40 0 3 -7 96.99 8.80 0 3 -7 104.39 8.90 0 -3 7 112.79 11.30 -1 3 -7 0.10 2.70 -1 3 -7 5.80 3.10 1 -3 7 -0.90 3.60 -2 3 -7 568.74 24.70 2 -3 7 542.45 27.60 -3 3 -7 416.76 20.70 3 -3 7 398.86 23.10 -4 3 -7 2.60 3.80 4 -3 7 -2.30 3.70 -5 3 -7 18.60 6.20 5 -3 7 20.30 6.90 -6 3 -7 4.20 5.30 6 -3 7 3.10 6.60 7 -3 7 23.70 2.70 7 -3 7 23.30 2.50 8 -3 7 45.50 3.40 8 -3 7 56.49 3.70 9 -3 7 3.80 1.50 9 -3 7 3.20 1.50 10 -3 7 4.40 1.50 10 -3 7 5.00 1.40 11 -3 7 9.60 1.60 11 -3 7 6.30 1.40 9 2 -7 10.20 1.70 9 2 -7 9.80 1.50 8 2 -7 0.30 1.20 8 2 -7 0.70 1.10 7 2 -7 0.20 1.10 7 2 -7 1.60 1.20 6 2 -7 0.90 1.30 6 2 -7 0.00 1.10 5 2 -7 82.89 11.10 -5 -2 7 69.39 14.00 4 2 -7 12.90 5.00 -4 -2 7 14.60 7.20 3 2 -7 1.10 4.20 -3 -2 7 1.60 5.10 2 2 -7 784.12 33.30 -2 -2 7 802.22 37.10 1 2 -7 230.18 13.20 -1 -2 7 220.18 16.10 0 2 -7 17.70 3.70 0 2 -7 25.30 4.60 0 -2 7 11.30 4.70 -1 2 -7 907.51 34.30 -1 2 -7 919.31 34.20 -2 2 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11 -5 8 -0.80 1.00 9 4 -8 5.80 1.00 8 4 -8 0.10 1.00 8 4 -8 0.30 1.70 7 4 -8 8.50 1.50 7 4 -8 8.60 1.50 6 4 -8 143.99 5.80 6 4 -8 129.19 5.80 6 4 -8 138.49 5.90 5 4 -8 0.70 1.20 5 4 -8 1.80 1.10 5 4 -8 -0.10 1.20 4 4 -8 79.39 12.30 4 4 -8 60.59 3.30 3 4 -8 23.70 7.40 -3 -4 8 7.00 9.00 2 4 -8 36.70 7.50 -2 -4 8 39.00 10.10 1 4 -8 16.40 5.30 -1 -4 8 17.60 7.70 0 4 -8 40.30 6.80 0 -4 8 34.90 9.00 1 -4 8 12.20 6.10 -2 4 -8 67.19 8.50 2 -4 8 78.59 11.00 -3 4 -8 49.40 7.90 3 -4 8 58.39 10.30 -4 4 -8 -0.50 4.10 4 -4 8 11.20 6.70 -5 4 -8 146.99 14.00 5 -4 8 118.79 15.30 -6 4 -8 5.60 7.70 6 -4 8 0.60 1.50 6 -4 8 2.70 1.50 6 -4 8 1.80 13.20 6 -4 8 3.30 1.40 7 -4 8 8.10 1.90 7 -4 8 10.10 1.90 7 -4 8 10.30 1.90 8 -4 8 13.80 2.40 8 -4 8 10.10 1.90 9 -4 8 21.80 2.50 9 -4 8 19.70 2.60 10 -4 8 10.90 1.80 10 -4 8 9.80 1.60 11 -4 8 11.20 1.60 11 -4 8 10.10 1.60 9 3 -8 3.60 1.00 8 3 -8 3.80 1.30 8 3 -8 4.50 1.20 7 3 -8 37.90 2.60 7 3 -8 38.00 2.90 6 3 -8 1.40 1.10 6 3 -8 -0.50 1.30 5 3 -8 16.30 2.00 5 3 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9.90 1.60 8 -10 9 10.70 1.70 7 9 -9 0.50 0.80 7 9 -9 0.50 0.80 6 9 -9 2.20 1.00 6 9 -9 -0.50 0.90 5 9 -9 1.90 1.10 5 9 -9 2.10 1.20 4 9 -9 16.50 2.20 4 9 -9 16.90 2.00 -4 -9 9 16.80 2.60 3 9 -9 19.40 2.20 3 9 -9 21.20 2.40 -3 -9 9 15.40 2.70 2 9 -9 65.59 3.60 2 9 -9 64.39 3.70 -2 -9 9 65.39 4.30 1 9 -9 23.60 2.40 -1 -9 9 26.90 3.20 0 9 -9 184.18 7.30 0 -9 9 185.18 7.90 -1 9 -9 83.79 4.20 1 -9 9 85.89 4.80 2 -9 9 65.29 4.20 -3 9 -9 14.80 2.30 3 -9 9 12.60 2.10 -4 9 -9 64.59 3.70 4 -9 9 68.19 4.10 -5 9 -9 7.90 1.60 5 -9 9 8.20 1.80 -6 9 -9 2.90 1.40 6 -9 9 -0.10 1.40 -7 9 -9 -0.30 1.20 7 -9 9 -0.10 1.30 -8 9 -9 0.20 1.10 8 -9 9 2.30 1.20 -9 9 -9 0.20 0.90 9 -9 9 -0.70 0.90 7 8 -9 1.00 0.90 7 8 -9 3.50 1.00 6 8 -9 2.00 1.20 6 8 -9 2.00 1.00 5 8 -9 2.50 1.30 5 8 -9 3.00 1.20 4 8 -9 16.30 2.00 4 8 -9 14.70 2.20 3 8 -9 3.00 1.30 3 8 -9 5.00 1.50 2 8 -9 88.19 4.30 2 8 -9 90.79 4.40 1 8 -9 100.99 4.70 -1 -8 9 93.99 5.20 0 8 -9 61.09 3.50 0 -8 9 58.69 4.10 -1 8 -9 2.70 1.30 1 -8 9 -1.40 1.60 2 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82.19 4.30 4 6 -9 86.89 4.20 3 6 -9 76.09 4.10 3 6 -9 74.29 3.90 3 6 -9 74.79 3.80 2 6 -9 145.19 6.00 2 6 -9 145.39 6.00 2 6 -9 148.99 6.30 2 6 -9 131.19 15.20 -1 -6 9 23.70 10.50 0 -6 9 1.20 8.00 1 -6 9 68.29 13.70 2 -6 9 102.99 14.60 -3 6 -9 2.10 6.30 3 -6 9 7.90 7.20 -4 6 -9 45.00 11.10 4 -6 9 55.99 3.50 4 -6 9 56.59 3.50 5 -6 9 1.20 1.50 5 -6 9 2.20 1.40 6 -6 9 51.09 3.40 6 -6 9 44.30 3.50 7 -6 9 7.70 1.80 7 -6 9 10.10 1.90 7 -6 9 7.10 1.80 8 -6 9 10.30 1.80 8 -6 9 13.80 2.00 8 -6 9 13.80 2.20 9 -6 9 1.40 1.40 9 -6 9 1.10 1.30 9 -6 9 1.90 1.30 10 -6 9 7.10 1.40 9 5 -9 1.70 0.70 8 5 -9 15.20 1.50 7 5 -9 -1.00 1.00 7 5 -9 1.30 1.20 6 5 -9 1.90 1.20 6 5 -9 0.50 1.30 6 5 -9 0.00 1.10 5 5 -9 0.20 1.10 5 5 -9 -0.40 1.20 5 5 -9 -0.60 1.20 4 5 -9 7.40 1.50 4 5 -9 7.90 1.60 4 5 -9 9.90 1.60 3 5 -9 36.30 2.60 3 5 -9 37.70 2.60 3 5 -9 42.30 2.90 2 5 -9 283.87 19.20 -2 -5 9 214.08 21.60 1 5 -9 56.29 10.00 -1 -5 9 55.49 12.20 0 -5 9 14.00 7.90 1 -5 9 68.39 11.90 2 -5 9 35.60 9.60 -3 5 -9 0.60 5.20 3 -5 9 1.70 5.80 -4 5 -9 11.60 6.60 4 -5 9 4.90 7.00 5 -5 9 84.59 4.60 5 -5 9 94.19 4.70 6 -5 9 25.10 2.90 6 -5 9 24.90 2.80 6 -5 9 31.90 3.00 7 -5 9 132.89 6.10 7 -5 9 129.29 6.10 7 -5 9 132.89 6.10 8 -5 9 -1.80 1.30 8 -5 9 0.60 1.40 8 -5 9 -0.40 1.40 9 -5 9 0.10 1.30 9 -5 9 0.40 1.20 10 -5 9 4.00 1.30 10 -5 9 3.90 1.30 11 -5 9 1.10 0.90 9 4 -9 22.20 1.50 8 4 -9 23.70 1.90 8 4 -9 26.30 2.00 7 4 -9 14.10 1.90 7 4 -9 7.30 1.40 6 4 -9 2.60 1.40 6 4 -9 4.30 1.30 6 4 -9 4.30 1.40 5 4 -9 307.17 11.00 5 4 -9 307.07 11.20 5 4 -9 301.87 11.10 4 4 -9 13.50 2.20 4 4 -9 13.30 1.90 4 4 -9 14.00 2.00 3 4 -9 40.90 9.20 -3 -4 9 35.40 12.20 2 4 -9 5.30 4.60 -2 -4 9 -1.70 7.40 1 4 -9 83.79 10.30 -1 -4 9 84.19 13.80 0 4 -9 340.57 19.10 0 -4 9 354.66 24.40 1 -4 9 -0.30 5.20 2 -4 9 160.38 16.00 -3 4 -9 25.60 6.50 3 -4 9 38.60 9.20 -4 4 -9 -0.40 4.80 4 -4 9 1.80 5.80 -5 4 -9 30.20 8.40 5 -4 9 40.60 9.80 6 -4 9 59.19 3.60 6 -4 9 49.90 3.40 6 -4 9 49.99 3.60 7 -4 9 2.60 1.60 7 -4 9 3.70 1.70 7 -4 9 4.50 1.60 8 -4 9 70.09 4.10 8 -4 9 72.69 4.20 9 -4 9 0.50 1.40 9 -4 9 -0.90 1.40 10 -4 9 53.29 3.10 10 -4 9 55.19 3.30 11 -4 9 4.70 1.10 11 -4 9 0.70 1.00 9 3 -9 0.50 0.80 8 3 -9 12.20 1.60 8 3 -9 14.00 1.80 7 3 -9 2.50 1.30 7 3 -9 -0.10 1.00 6 3 -9 44.10 2.90 6 3 -9 47.90 3.10 5 3 -9 27.60 2.60 5 3 -9 27.90 2.60 5 3 -9 22.10 2.30 4 3 -9 91.69 4.50 4 3 -9 92.49 4.30 4 3 -9 90.99 4.20 4 3 -9 89.59 12.40 -4 -3 9 89.59 17.30 3 3 -9 8.30 5.60 -3 -3 9 -8.90 6.80 2 3 -9 117.59 11.50 -2 -3 9 101.69 15.10 1 3 -9 15.10 5.10 -1 -3 9 29.70 9.30 0 3 -9 12.20 4.90 0 -3 9 16.00 7.20 1 -3 9 161.38 15.50 -2 3 -9 377.76 19.30 2 -3 9 348.67 22.70 -3 3 -9 0.60 4.20 3 -3 9 0.80 4.40 -4 3 -9 15.50 5.90 4 -3 9 18.60 6.60 -5 3 -9 10.50 5.90 5 -3 9 2.10 6.00 6 -3 9 1.80 1.50 6 -3 9 1.30 1.40 7 -3 9 205.58 8.30 7 -3 9 195.98 8.10 8 -3 9 30.20 2.80 8 -3 9 32.40 3.10 9 -3 9 16.50 2.30 9 -3 9 17.30 2.50 10 -3 9 4.30 1.40 10 -3 9 1.20 1.40 11 -3 9 2.40 1.10 11 -3 9 2.80 1.00 9 2 -9 11.70 1.40 9 2 -9 14.30 1.50 8 2 -9 21.30 1.90 8 2 -9 22.40 2.10 7 2 -9 1.50 1.30 7 2 -9 -0.90 1.00 6 2 -9 2.70 1.40 6 2 -9 3.10 1.20 5 2 -9 104.09 4.90 5 2 -9 102.49 4.60 4 2 -9 16.80 5.90 -4 -2 9 29.20 10.30 3 2 -9 4.00 5.00 -3 -2 9 -0.40 6.90 2 2 -9 37.30 7.40 -2 -2 9 61.69 12.10 1 2 -9 -0.40 3.10 -1 -2 9 0.20 5.10 0 2 -9 112.89 9.50 0 -2 9 106.49 12.70 -1 2 -9 123.39 9.50 1 -2 9 107.79 12.60 -2 2 -9 37.30 6.70 2 -2 9 31.90 7.70 -3 2 -9 86.69 9.00 3 -2 9 71.19 10.80 -4 2 -9 64.89 9.20 4 -2 9 84.59 11.40 -5 2 -9 -1.00 4.50 5 -2 9 3.70 6.20 -6 2 -9 21.00 8.10 6 -2 9 4.30 7.80 7 -2 9 121.29 5.60 7 -2 9 116.79 5.50 8 -2 9 10.60 2.10 8 -2 9 9.70 1.80 9 -2 9 42.90 3.30 9 -2 9 38.60 3.00 10 -2 9 4.00 1.50 10 -2 9 4.60 1.50 11 -2 9 32.50 2.20 11 -2 9 28.40 2.20 9 1 -9 0.90 1.00 9 1 -9 -0.20 0.90 8 1 -9 26.60 2.20 8 1 -9 30.60 2.40 7 1 -9 59.29 3.50 7 1 -9 52.69 3.10 6 1 -9 2.40 1.30 6 1 -9 2.10 1.20 5 1 -9 177.58 7.10 5 1 -9 178.98 6.90 4 1 -9 2.40 4.70 -4 -1 9 6.80 8.10 3 1 -9 206.38 15.20 -3 -1 9 191.88 18.00 2 1 -9 90.99 9.30 -2 -1 9 86.29 12.30 1 1 -9 -2.60 2.90 -1 -1 9 -2.30 4.60 0 1 -9 20.80 4.80 0 -1 9 16.00 6.10 -1 1 -9 313.87 16.00 1 -1 9 315.37 20.30 -2 1 -9 215.88 12.60 2 -1 9 198.28 15.70 -3 1 -9 5.60 3.70 3 -1 9 11.70 5.20 -4 1 -9 474.65 25.00 4 -1 9 541.25 28.90 -5 1 -9 35.90 8.50 5 -1 9 14.40 7.10 -6 1 -9 267.77 20.40 6 -1 9 257.77 22.20 7 -1 9 19.80 2.40 7 -1 9 21.00 2.50 8 -1 9 122.99 5.60 8 -1 9 120.39 5.80 9 -1 9 -2.90 1.30 9 -1 9 -0.70 1.20 10 -1 9 24.20 2.50 10 -1 9 20.00 2.20 11 -1 9 3.30 1.20 11 -1 9 1.50 1.10 10 0 -9 6.10 1.20 9 0 -9 -1.00 1.00 9 0 -9 -0.70 0.90 8 0 -9 43.60 2.60 8 0 -9 35.90 2.70 7 0 -9 7.90 1.50 7 0 -9 10.10 1.70 6 0 -9 267.87 10.00 6 0 -9 280.57 10.30 5 0 -9 1.80 1.40 5 0 -9 -3.80 6.70 5 0 -9 2.80 1.10 -5 0 9 -4.10 8.70 4 0 -9 37.40 7.90 -4 0 9 44.60 11.00 3 0 -9 5.40 3.60 -3 0 9 1.70 6.20 2 0 -9 431.66 22.10 -2 0 9 431.96 26.20 1 0 -9 31.30 6.20 -1 0 9 42.50 8.80 0 0 -9 1020.10 39.40 0 0 9 1009.50 44.50 -1 0 -9 26.10 5.00 1 0 9 24.70 6.70 -2 0 -9 161.18 9.70 -2 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19.20 2.20 10 2 9 19.00 2.30 11 2 9 4.40 1.20 11 2 9 4.40 1.30 10 -3 -9 1.30 0.90 9 -3 -9 5.40 1.20 9 -3 -9 5.60 1.30 8 -3 -9 -1.50 1.00 8 -3 -9 0.90 1.30 7 -3 -9 1.40 1.20 7 -3 -9 0.10 1.10 6 -3 -9 182.78 7.50 6 -3 -9 178.98 7.00 5 -3 -9 18.90 7.30 5 -3 -9 11.10 1.70 5 -3 -9 7.90 1.40 -5 3 9 14.30 9.90 4 -3 -9 -0.80 4.70 -4 3 9 6.60 6.80 3 -3 -9 19.50 5.40 -3 3 9 19.80 7.20 2 -3 -9 71.79 8.10 -2 3 9 75.69 10.40 1 -3 -9 93.39 8.70 -1 3 9 80.99 10.20 0 -3 -9 80.49 7.80 0 3 9 72.79 9.50 -1 -3 -9 135.69 10.00 1 3 9 129.79 11.00 1 3 9 148.69 12.60 -2 -3 -9 38.10 6.20 2 3 9 40.60 7.50 2 3 9 25.40 6.30 -3 -3 -9 196.88 12.10 3 3 9 185.48 13.90 3 3 9 176.88 14.80 4 3 9 0.60 5.10 4 3 9 0.00 4.40 -6 -3 -9 74.19 12.70 7 3 9 1.90 1.40 7 3 9 1.20 1.50 7 3 9 2.80 1.40 8 3 9 21.90 2.70 8 3 9 20.00 2.40 8 3 9 28.20 2.70 9 3 9 -0.70 1.30 9 3 9 2.40 1.50 10 3 9 5.20 1.50 10 3 9 3.00 1.30 11 3 9 2.20 1.10 11 3 9 1.20 1.10 10 -4 -9 5.80 1.10 9 -4 -9 6.20 1.20 9 -4 -9 4.00 1.20 8 -4 -9 1.70 1.20 8 -4 -9 1.10 1.40 8 -4 -9 -0.10 1.10 7 -4 -9 0.90 1.50 7 -4 -9 1.50 1.20 7 -4 -9 0.50 1.30 6 -4 -9 44.60 3.20 6 -4 -9 39.90 3.00 6 -4 -9 42.20 2.80 5 -4 -9 115.69 5.10 5 -4 -9 113.79 13.60 5 -4 -9 109.09 4.80 5 -4 -9 115.89 5.60 -5 4 9 95.69 15.90 4 -4 -9 -1.80 3.80 -4 4 9 5.20 6.30 3 -4 -9 239.48 15.70 -3 4 9 226.68 19.00 2 -4 -9 37.40 7.40 -2 4 9 41.50 8.70 1 -4 -9 -2.60 2.60 -1 4 9 0.20 4.40 0 -4 -9 61.49 7.20 0 4 9 47.20 7.90 -1 -4 -9 124.49 10.00 1 4 9 120.79 10.30 1 4 9 127.59 11.60 -2 -4 -9 69.19 7.70 2 4 9 50.89 8.40 2 4 9 45.00 8.10 -3 -4 -9 39.30 6.40 3 4 9 53.59 9.40 -4 -4 -9 249.97 15.10 4 4 9 253.67 19.60 5 4 9 92.99 14.60 7 4 9 88.19 4.50 7 4 9 82.19 4.30 7 4 9 86.89 4.50 8 4 9 13.40 2.30 8 4 9 14.80 2.10 8 4 9 10.30 1.90 9 4 9 5.20 1.50 9 4 9 7.00 1.70 10 4 9 4.20 1.50 10 4 9 5.20 1.40 11 4 9 24.90 2.00 10 -5 -9 11.00 1.30 9 -5 -9 11.30 1.70 9 -5 -9 11.50 1.70 8 -5 -9 2.20 1.20 8 -5 -9 3.10 1.20 8 -5 -9 1.00 1.30 7 -5 -9 55.59 3.50 7 -5 -9 52.49 3.40 7 -5 -9 51.39 3.10 6 -5 -9 14.40 2.40 6 -5 -9 19.20 2.40 6 -5 -9 16.40 2.00 5 -5 -9 200.58 7.70 5 -5 -9 223.28 17.60 5 -5 -9 203.08 8.20 5 -5 -9 210.88 8.10 4 -5 -9 13.90 6.50 -4 5 9 8.00 7.40 3 -5 -9 78.99 9.50 -3 5 9 94.29 13.70 2 -5 -9 14.40 5.10 -2 5 9 1.50 5.50 1 -5 -9 8.00 3.70 -1 5 9 3.30 4.90 0 -5 -9 -2.00 3.00 -1 -5 -9 4.50 4.10 1 5 9 10.80 5.10 1 5 9 7.90 5.00 -2 -5 -9 206.58 13.30 2 5 9 200.38 14.90 -3 -5 -9 97.39 9.30 3 5 9 98.89 11.50 -4 -5 -9 120.29 10.80 4 5 9 121.39 14.40 5 5 9 5.20 6.70 6 5 9 24.60 11.30 7 5 9 15.70 2.40 7 5 9 20.70 2.40 7 5 9 14.70 2.30 8 5 9 117.59 5.50 8 5 9 122.19 5.50 8 5 9 119.19 5.60 9 5 9 4.90 1.60 9 5 9 4.30 1.60 9 5 9 5.00 1.60 10 5 9 1.40 1.20 11 5 9 15.70 1.70 10 -6 -9 14.00 1.30 9 -6 -9 3.60 1.20 9 -6 -9 2.90 1.20 8 -6 -9 41.70 2.90 8 -6 -9 43.80 2.60 8 -6 -9 44.90 3.00 7 -6 -9 48.60 3.00 7 -6 -9 44.60 3.30 7 -6 -9 48.50 3.20 6 -6 -9 11.40 1.90 6 -6 -9 13.30 2.20 6 -6 -9 9.30 1.50 5 -6 -9 0.90 1.40 5 -6 -9 0.00 1.10 5 -6 -9 0.60 1.30 4 -6 -9 170.18 14.80 -4 6 9 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0.80 1.30 6 8 9 32.90 2.90 6 8 9 32.00 2.80 7 8 9 51.49 3.40 7 8 9 44.00 3.30 8 8 9 35.90 2.90 8 8 9 36.20 2.90 9 8 9 1.30 1.40 9 8 9 1.60 1.30 10 8 9 2.20 1.10 10 8 9 6.00 1.40 11 8 9 6.00 1.00 9 -9 -9 0.90 1.00 9 -9 -9 2.90 1.00 8 -9 -9 -0.50 1.20 8 -9 -9 1.20 1.20 7 -9 -9 5.70 1.40 7 -9 -9 7.50 1.40 7 -9 -9 7.50 1.70 6 -9 -9 0.90 1.50 6 -9 -9 -0.90 1.20 6 -9 -9 2.60 1.30 5 -9 -9 87.19 4.30 5 -9 -9 93.79 4.50 5 -9 -9 90.49 4.70 4 -9 -9 30.60 2.40 4 -9 -9 33.00 2.80 3 -9 -9 24.10 2.60 3 -9 -9 30.30 8.70 3 -9 -9 23.00 2.20 2 -9 -9 5.00 5.30 1 -9 -9 87.69 11.20 0 -9 -9 188.58 14.40 -1 -9 -9 -0.10 4.70 1 9 9 -1.20 5.40 -2 -9 -9 67.69 10.20 2 9 9 69.99 12.50 -3 -9 -9 1.70 5.70 3 9 9 4.20 7.30 -4 -9 -9 5.60 6.30 4 9 9 14.00 10.10 5 9 9 41.40 3.00 5 9 9 39.80 3.20 6 9 9 70.79 3.90 6 9 9 66.39 4.00 7 9 9 5.10 1.60 7 9 9 2.60 1.50 8 9 9 7.50 1.70 8 9 9 7.20 1.70 9 9 9 -0.40 1.20 9 9 9 2.00 1.20 10 9 9 -1.20 0.90 10 9 9 -0.20 1.00 9 -10 -9 0.70 0.90 9 -10 -9 0.00 0.80 8 -10 -9 4.80 1.20 8 -10 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2.20 -2 -9 10 14.10 2.30 1 9 -10 15.70 2.10 -1 -9 10 19.60 2.90 0 9 -10 -0.80 1.20 0 -9 10 -1.40 1.50 -1 9 -10 12.00 1.80 1 -9 10 18.00 2.80 2 -9 10 30.60 3.30 3 -9 10 42.00 3.40 -4 9 -10 2.20 1.50 4 -9 10 0.30 1.40 -5 9 -10 18.90 2.20 5 -9 10 15.90 2.50 -6 9 -10 29.30 2.40 6 -9 10 25.80 2.60 -7 9 -10 2.20 1.10 7 -9 10 2.00 1.30 -8 9 -10 10.90 1.60 8 -9 10 9.60 1.60 -9 9 -10 8.60 1.30 9 -9 10 6.60 1.60 7 8 -10 1.20 0.80 7 8 -10 1.20 0.80 6 8 -10 14.60 1.70 6 8 -10 16.10 1.60 5 8 -10 6.90 1.30 5 8 -10 8.10 1.40 -5 -8 10 7.80 1.70 4 8 -10 2.90 1.30 4 8 -10 5.70 1.30 3 8 -10 -0.10 1.20 3 8 -10 -1.30 1.10 2 8 -10 17.90 2.30 2 8 -10 18.30 2.30 -2 -8 10 17.50 2.80 1 8 -10 4.40 1.50 -1 -8 10 2.60 1.80 0 8 -10 0.30 1.20 0 -8 10 0.20 1.70 -1 8 -10 26.70 2.40 1 -8 10 16.40 2.80 -2 8 -10 75.59 5.30 2 -8 10 65.89 4.20 3 -8 10 28.70 3.00 -4 8 -10 38.90 3.00 4 -8 10 45.70 3.40 5 -8 10 19.00 2.60 6 -8 10 1.40 1.40 7 -8 10 1.90 1.40 8 -8 10 1.10 1.20 -9 8 -10 -1.00 0.90 9 -8 10 0.20 0.90 7 7 -10 4.70 1.00 7 7 -10 3.70 0.90 6 7 -10 0.20 0.90 6 7 -10 0.20 1.00 6 7 -10 -0.30 1.10 5 7 -10 11.80 1.70 5 7 -10 6.00 1.50 5 7 -10 8.10 1.50 4 7 -10 1.50 1.30 4 7 -10 2.30 1.10 4 7 -10 0.00 1.20 3 7 -10 11.80 1.90 3 7 -10 9.20 1.60 3 7 -10 10.70 1.80 2 7 -10 36.70 2.70 2 7 -10 36.60 3.00 2 7 -10 37.10 2.80 1 7 -10 16.90 2.20 0 7 -10 195.48 7.60 0 -7 10 193.58 8.30 -1 7 -10 151.68 6.10 1 -7 10 141.99 6.60 -2 7 -10 205.28 7.90 2 -7 10 207.88 8.50 3 -7 10 -0.30 1.50 4 -7 10 1.30 1.50 5 -7 10 4.90 1.70 6 -7 10 3.50 1.50 7 -7 10 -0.40 1.30 8 -7 10 -0.60 1.20 9 -7 10 0.90 1.10 -10 7 -10 14.90 1.40 8 6 -10 3.10 0.80 7 6 -10 2.30 1.00 7 6 -10 3.60 1.10 6 6 -10 3.70 1.30 6 6 -10 1.90 1.20 6 6 -10 3.80 1.20 5 6 -10 0.70 1.20 5 6 -10 0.50 1.20 5 6 -10 -0.80 1.00 4 6 -10 0.90 1.20 4 6 -10 1.20 1.10 4 6 -10 1.50 1.30 3 6 -10 2.30 1.40 3 6 -10 2.00 1.20 3 6 -10 0.30 1.10 2 6 -10 48.30 3.30 2 6 -10 42.80 2.90 2 6 -10 44.90 2.90 1 6 -10 7.20 1.40 1 6 -10 6.10 1.60 0 6 -10 83.09 4.00 0 -6 10 68.69 15.10 -1 6 -10 18.90 2.10 1 -6 10 16.00 2.60 1 -6 10 17.10 10.90 -2 6 -10 2.20 1.20 2 -6 10 5.50 7.40 2 -6 10 -0.10 1.40 3 -6 10 68.89 4.00 4 -6 10 63.69 3.90 5 -6 10 109.39 5.30 5 -6 10 107.09 5.20 6 -6 10 2.70 1.60 6 -6 10 1.80 1.40 7 -6 10 1.00 1.40 7 -6 10 0.30 1.50 8 -6 10 -1.30 1.30 8 -6 10 1.30 1.40 8 -6 10 -0.90 1.30 9 -6 10 12.60 1.90 10 -6 10 21.60 1.90 8 5 -10 -0.30 0.80 7 5 -10 9.40 1.50 7 5 -10 10.50 1.70 6 5 -10 9.20 1.50 6 5 -10 12.00 1.90 6 5 -10 10.80 1.90 5 5 -10 16.40 2.20 5 5 -10 14.60 2.00 5 5 -10 13.90 1.90 4 5 -10 50.79 3.20 4 5 -10 51.89 3.10 4 5 -10 51.29 3.30 3 5 -10 45.80 2.90 3 5 -10 42.30 3.10 3 5 -10 45.60 2.90 2 5 -10 187.28 7.60 2 5 -10 243.38 23.50 2 5 -10 186.18 7.30 2 5 -10 184.78 7.30 -2 -5 10 224.98 23.10 1 5 -10 14.10 7.90 1 5 -10 6.90 1.50 1 5 -10 3.20 1.60 -1 -5 10 5.70 8.10 0 -5 10 42.20 11.50 1 -5 10 14.60 8.80 2 -5 10 4.40 6.60 3 -5 10 87.89 14.90 -4 5 -10 23.20 9.20 4 -5 10 20.60 2.70 4 -5 10 20.30 2.70 5 -5 10 22.90 2.60 5 -5 10 18.10 2.70 6 -5 10 21.40 2.80 6 -5 10 23.10 2.70 7 -5 10 18.70 2.70 7 -5 10 16.80 2.50 7 -5 10 11.90 2.00 8 -5 10 6.30 1.60 8 -5 10 5.10 1.70 8 -5 10 7.70 1.70 9 -5 10 2.10 1.30 9 -5 10 1.60 1.30 10 -5 10 16.20 1.90 10 -5 10 18.30 1.90 8 4 -10 0.10 0.90 8 4 -10 -0.50 0.80 7 4 -10 6.50 1.30 7 4 -10 4.20 1.20 6 4 -10 4.40 1.30 6 4 -10 4.60 1.40 6 4 -10 4.60 1.50 5 4 -10 -0.10 1.20 5 4 -10 0.90 1.10 5 4 -10 -0.40 1.20 4 4 -10 5.30 1.60 4 4 -10 3.80 1.30 4 4 -10 2.70 1.20 3 4 -10 14.10 2.20 3 4 -10 12.60 2.00 3 4 -10 13.40 1.90 2 4 -10 119.19 13.10 -2 -4 10 135.49 18.20 1 4 -10 142.69 13.10 -1 -4 10 131.59 17.80 0 -4 10 3.70 6.90 1 -4 10 4.40 6.10 2 -4 10 62.89 12.40 3 -4 10 11.00 6.60 -4 4 -10 -4.10 5.50 4 -4 10 5.70 6.80 5 -4 10 31.10 2.90 5 -4 10 27.70 2.70 6 -4 10 66.99 4.00 6 -4 10 73.99 4.30 6 -4 10 75.39 4.10 7 -4 10 -0.70 1.50 7 -4 10 2.20 1.40 8 -4 10 1.60 1.50 8 -4 10 0.10 1.40 9 -4 10 18.50 2.50 9 -4 10 23.30 2.40 10 -4 10 -0.80 1.10 10 -4 10 -0.70 1.10 11 -4 10 15.10 1.50 9 3 -10 -0.60 0.70 8 3 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4 2 -10 2.10 1.20 3 2 -10 33.60 7.70 -3 -2 10 29.10 11.40 2 2 -10 130.49 12.60 -2 -2 10 177.98 18.80 1 2 -10 6.70 4.00 -1 -2 10 -4.90 5.60 0 2 -10 3.30 3.90 0 -2 10 9.20 6.60 -1 2 -10 9.00 4.60 1 -2 10 20.60 7.60 2 -2 10 85.99 11.40 -3 2 -10 -6.10 3.60 3 -2 10 4.30 5.90 -4 2 -10 21.70 6.00 4 -2 10 25.10 8.00 -5 2 -10 29.00 7.30 5 -2 10 9.00 8.00 6 -2 10 15.90 2.40 6 -2 10 17.50 2.50 7 -2 10 71.09 4.00 7 -2 10 71.59 4.20 8 -2 10 22.20 2.80 8 -2 10 23.20 2.60 9 -2 10 40.20 3.20 9 -2 10 44.90 3.10 10 -2 10 0.30 1.20 10 -2 10 1.50 1.30 11 -2 10 6.00 1.20 11 -2 10 6.10 1.30 9 1 -10 4.70 0.90 9 1 -10 3.60 1.00 8 1 -10 6.60 1.30 8 1 -10 5.10 1.20 7 1 -10 23.30 2.30 7 1 -10 18.10 2.00 6 1 -10 8.40 1.70 6 1 -10 8.50 1.40 5 1 -10 118.99 5.00 5 1 -10 111.39 5.20 4 1 -10 34.70 8.90 4 1 -10 16.50 1.80 4 1 -10 16.60 2.20 -4 -1 10 24.40 10.00 3 1 -10 4.90 5.40 -3 -1 10 -0.80 7.00 2 1 -10 55.49 8.50 -2 -1 10 42.00 10.70 1 1 -10 2.10 3.50 -1 -1 10 1.10 5.70 0 1 -10 22.50 5.60 0 -1 10 16.20 6.90 -1 1 -10 8.80 4.00 1 -1 10 14.60 6.40 2 -1 10 25.20 7.00 -3 1 -10 157.28 12.30 3 -1 10 181.98 15.70 -4 1 -10 12.80 5.60 4 -1 10 3.70 5.80 -5 1 -10 48.80 9.60 5 -1 10 26.60 9.30 -6 1 -10 130.69 15.10 6 -1 10 144.49 18.50 6 -1 10 114.29 5.30 6 -1 10 112.49 5.30 7 -1 10 91.69 4.60 7 -1 10 79.59 4.40 8 -1 10 39.90 3.20 8 -1 10 33.10 2.90 9 -1 10 29.70 2.90 9 -1 10 32.10 2.70 10 -1 10 2.30 1.30 10 -1 10 0.90 1.20 11 -1 10 9.40 1.50 11 -1 10 8.20 1.40 9 0 -10 0.10 0.80 9 0 -10 -0.20 0.90 8 0 -10 0.20 1.10 8 0 -10 0.30 1.00 7 0 -10 2.30 1.10 7 0 -10 0.00 1.30 6 0 -10 82.39 4.00 6 0 -10 90.49 4.40 5 0 -10 60.59 3.20 5 0 -10 60.99 3.60 4 0 -10 30.00 8.40 -4 0 10 33.40 11.10 3 0 -10 -0.10 4.20 -3 0 10 4.80 6.60 2 0 -10 215.98 15.20 -2 0 10 209.18 18.70 1 0 -10 82.09 9.10 -1 0 10 77.89 11.90 0 0 -10 3.40 3.80 0 0 10 4.20 4.50 -1 0 -10 23.70 5.00 1 0 10 10.10 5.80 -2 0 -10 621.94 25.90 2 0 10 570.64 30.80 -3 0 -10 2.10 3.90 3 0 10 1.90 4.40 -4 0 -10 57.29 8.90 4 0 10 41.60 9.40 -5 0 -10 6.90 5.10 5 0 10 13.00 7.50 -6 0 -10 27.80 8.80 6 0 10 19.40 2.60 6 0 10 11.50 8.90 7 0 10 1.50 1.40 7 0 10 1.90 1.40 8 0 10 25.30 2.60 8 0 10 29.50 2.80 9 0 10 1.10 1.40 9 0 10 -0.10 1.30 10 0 10 48.90 3.10 10 0 10 43.70 2.90 11 0 10 1.30 1.00 11 0 10 1.90 1.10 9 -1 -10 0.70 1.00 9 -1 -10 0.40 0.90 8 -1 -10 4.80 1.30 8 -1 -10 3.00 1.10 7 -1 -10 31.20 2.30 7 -1 -10 27.20 2.50 6 -1 -10 7.90 1.70 6 -1 -10 8.10 1.40 5 -1 -10 5.90 1.30 5 -1 -10 5.40 1.60 4 -1 -10 2.70 4.60 -4 1 10 13.20 8.70 3 -1 -10 -0.60 3.70 -3 1 10 0.60 6.00 2 -1 -10 247.48 16.20 -2 1 10 248.88 19.30 1 -1 -10 22.90 5.80 -1 1 10 12.70 6.30 0 -1 -10 212.48 13.30 0 1 10 183.28 16.00 -1 -1 -10 57.39 7.10 1 1 10 51.39 9.20 -2 -1 -10 355.76 17.60 2 1 10 346.37 22.00 -3 -1 -10 317.97 18.00 3 1 10 333.47 21.20 -4 -1 -10 229.78 16.20 4 1 10 217.98 18.00 -5 -1 -10 1.30 4.80 5 1 10 -4.30 5.50 -6 -1 -10 233.58 19.40 7 1 10 62.39 3.80 7 1 10 58.79 3.70 8 1 10 24.30 2.70 8 1 10 21.70 2.50 9 1 10 1.60 1.40 9 1 10 2.80 1.50 10 1 10 15.60 2.20 10 1 10 15.90 2.10 11 1 10 4.90 1.30 11 1 10 3.30 1.10 9 -2 -10 17.30 1.80 9 -2 -10 19.00 1.60 8 -2 -10 7.00 1.30 8 -2 -10 7.10 1.40 7 -2 -10 17.20 2.00 7 -2 -10 19.60 2.40 6 -2 -10 -0.40 1.10 6 -2 -10 3.40 1.50 5 -2 -10 132.29 5.50 5 -2 -10 135.69 5.90 4 -2 -10 3.30 4.60 -4 2 10 8.20 7.70 3 -2 -10 6.10 4.30 -3 2 10 -0.50 5.90 2 -2 -10 294.47 17.70 -2 2 10 278.37 20.70 1 -2 -10 0.30 3.20 -1 2 10 9.10 5.20 0 -2 -10 -3.90 3.00 0 2 10 1.90 4.50 -1 -2 -10 118.59 9.70 1 2 10 136.39 13.40 -2 -2 -10 299.77 15.80 2 2 10 294.17 19.70 -3 -2 -10 32.80 6.70 -3 -2 -10 33.50 6.00 3 2 10 34.30 7.70 -4 -2 -10 -6.50 3.80 4 2 10 2.70 5.50 -5 -2 -10 2.90 5.00 5 2 10 4.80 7.00 -6 -2 -10 4.60 6.00 7 2 10 222.38 8.70 7 2 10 222.68 8.80 7 2 10 222.98 8.80 8 2 10 52.79 3.40 8 2 10 49.10 3.40 9 2 10 61.09 3.60 9 2 10 61.39 3.70 10 2 10 -0.60 1.20 10 2 10 0.70 1.30 11 2 10 8.40 1.40 11 2 10 5.80 1.20 9 -3 -10 -0.70 0.90 9 -3 -10 0.00 1.00 8 -3 -10 0.70 1.00 8 -3 -10 1.50 1.20 7 -3 -10 44.00 3.20 7 -3 -10 48.60 2.80 6 -3 -10 40.10 3.10 6 -3 -10 41.10 2.70 5 -3 -10 39.40 2.70 5 -3 -10 49.40 3.10 4 -3 -10 48.00 9.60 -4 3 10 43.20 11.60 3 -3 -10 7.30 5.00 -3 3 10 7.70 6.00 2 -3 -10 261.97 16.50 -2 3 10 231.88 18.80 1 -3 -10 109.29 10.50 -1 3 10 130.19 13.30 0 -3 -10 203.78 13.10 0 3 10 203.68 16.30 -1 -3 -10 65.99 8.00 1 3 10 58.19 9.70 -2 -3 -10 9.70 4.30 2 3 10 8.10 5.30 -3 -3 -10 58.49 7.50 3 3 10 32.50 7.70 4 3 10 115.69 16.40 -5 -3 -10 14.40 6.80 -6 -3 -10 20.30 8.70 7 3 10 8.00 1.80 7 3 10 8.80 1.80 7 3 10 10.50 2.00 8 3 10 94.09 4.70 8 3 10 89.29 4.70 8 3 10 88.09 4.70 9 3 10 1.60 1.40 9 3 10 3.30 1.50 10 3 10 0.80 1.20 10 3 10 -1.20 1.20 11 3 10 -0.40 1.10 11 3 10 0.20 1.00 9 -4 -10 22.70 1.90 9 -4 -10 24.20 1.70 8 -4 -10 0.50 1.10 8 -4 -10 0.80 1.20 7 -4 -10 0.10 1.10 7 -4 -10 0.60 1.50 7 -4 -10 -1.20 1.20 6 -4 -10 160.18 7.00 6 -4 -10 169.88 6.50 6 -4 -10 157.38 6.80 5 -4 -10 203.48 8.30 5 -4 -10 196.58 8.10 5 -4 -10 216.58 7.80 4 -4 -10 11.10 5.80 -4 4 10 -4.60 7.00 3 -4 -10 38.30 8.00 -3 4 10 30.00 9.00 2 -4 -10 10.20 5.00 -2 4 10 4.30 6.20 1 -4 -10 4.90 4.30 -1 4 10 3.70 5.30 0 -4 -10 3.10 3.80 0 4 10 7.00 5.00 -1 -4 -10 245.88 14.40 1 4 10 199.88 16.20 -2 -4 -10 392.96 20.20 2 4 10 376.06 21.50 2 4 10 391.46 22.40 -3 -4 -10 271.07 16.20 3 4 10 259.57 18.90 4 4 10 14.60 7.60 5 4 10 1.20 7.10 6 4 10 0.20 1.30 6 4 10 0.00 1.40 6 4 10 -1.50 1.80 7 4 10 70.99 3.80 7 4 10 64.79 4.00 7 4 10 64.99 3.80 8 4 10 22.70 2.50 8 4 10 18.20 2.60 8 4 10 19.30 2.50 9 4 10 0.10 1.40 9 4 10 0.30 1.30 9 4 10 1.80 1.40 10 4 10 0.70 1.30 10 4 10 -1.70 1.00 11 4 10 11.10 1.60 9 -5 -10 1.80 1.10 9 -5 -10 1.60 1.00 8 -5 -10 12.40 2.00 8 -5 -10 9.10 1.60 8 -5 -10 11.70 1.60 7 -5 -10 21.70 2.50 7 -5 -10 24.00 2.20 7 -5 -10 20.40 2.30 6 -5 -10 13.80 2.50 6 -5 -10 14.40 2.00 6 -5 -10 17.80 2.40 5 -5 -10 2.80 1.60 5 -5 -10 3.30 1.20 5 -5 -10 5.00 1.40 4 -5 -10 5.00 1.80 4 -5 -10 7.80 6.60 -4 5 10 6.20 8.20 3 -5 -10 34.50 8.00 -3 5 10 45.60 11.30 2 -5 -10 12.70 6.00 -2 5 10 5.60 5.70 1 -5 -10 277.27 16.70 -1 5 10 264.57 19.10 0 -5 -10 41.80 7.40 0 5 10 26.60 7.80 -1 -5 -10 17.90 5.60 1 5 10 25.00 6.90 -2 -5 -10 35.10 6.60 2 5 10 39.60 8.80 -3 -5 -10 47.80 7.50 3 5 10 60.19 10.70 -4 -5 -10 69.69 9.50 4 5 10 65.19 12.30 5 5 10 3.60 7.50 6 5 10 3.00 1.40 6 5 10 -0.30 1.20 6 5 10 -1.10 1.30 6 5 10 11.80 9.50 7 5 10 128.59 5.70 7 5 10 111.29 5.50 7 5 10 126.99 5.60 8 5 10 134.09 6.10 8 5 10 133.99 6.00 8 5 10 139.59 6.00 9 5 10 0.60 1.40 9 5 10 1.30 1.40 9 5 10 1.20 1.40 10 5 10 4.00 1.30 10 5 10 5.40 1.50 11 5 10 0.80 1.00 9 -6 -10 9.20 1.50 9 -6 -10 8.80 1.40 8 -6 -10 6.00 1.20 8 -6 -10 6.50 1.50 8 -6 -10 4.20 1.30 7 -6 -10 1.60 1.50 7 -6 -10 3.60 1.30 7 -6 -10 3.30 1.30 6 -6 -10 5.40 1.60 6 -6 -10 4.80 1.40 6 -6 -10 0.90 1.20 5 -6 -10 4.40 1.30 5 -6 -10 7.50 1.80 5 -6 -10 2.40 1.40 4 -6 -10 79.49 4.40 4 -6 -10 93.49 13.20 4 -6 -10 80.39 3.80 -4 6 10 90.29 16.20 3 -6 -10 94.69 11.40 -3 6 10 89.09 14.20 2 -6 -10 172.28 13.80 -2 6 10 205.48 17.50 1 -6 -10 17.70 5.40 -1 6 10 9.90 6.50 0 -6 -10 136.29 11.80 0 6 10 150.78 13.90 -1 -6 -10 10.30 5.10 -2 -6 -10 5.70 4.20 2 6 10 5.70 5.30 -3 -6 -10 -5.20 3.70 3 6 10 7.30 6.60 -4 -6 -10 76.89 10.50 4 6 10 96.29 14.20 5 6 10 14.20 9.10 6 6 10 15.30 2.30 6 6 10 14.10 2.30 6 6 10 13.70 2.30 7 6 10 1.40 1.30 7 6 10 0.60 1.30 7 6 10 -2.50 1.20 8 6 10 10.80 1.90 8 6 10 12.80 2.20 8 6 10 7.70 1.70 9 6 10 20.00 2.30 9 6 10 19.10 2.30 10 6 10 -0.10 1.10 10 6 10 0.60 1.10 11 6 10 1.40 0.90 9 -7 -10 5.90 1.20 9 -7 -10 5.50 1.10 8 -7 -10 4.60 1.20 8 -7 -10 5.40 1.20 8 -7 -10 5.70 1.40 7 -7 -10 4.00 1.60 7 -7 -10 4.50 1.30 7 -7 -10 5.00 1.50 6 -7 -10 154.08 6.00 6 -7 -10 140.89 6.20 6 -7 -10 144.09 6.40 5 -7 -10 100.29 4.50 5 -7 -10 105.99 5.10 5 -7 -10 98.79 4.80 4 -7 -10 8.10 1.80 4 -7 -10 7.80 1.60 4 -7 -10 9.10 1.50 3 -7 -10 23.00 7.20 -3 7 10 23.10 9.50 2 -7 -10 24.20 7.00 -2 7 10 18.40 7.80 1 -7 -10 4.90 4.00 0 -7 -10 23.20 6.60 -1 -7 -10 38.60 8.20 -2 -7 -10 1.30 4.30 2 7 10 0.80 6.10 -3 -7 -10 -0.60 4.50 3 7 10 2.80 6.10 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1.40 8 8 10 18.70 2.30 8 8 10 16.60 2.30 9 8 10 15.80 2.10 9 8 10 14.00 2.10 10 8 10 -0.10 1.00 10 8 10 1.60 1.10 9 -9 -10 0.90 0.80 8 -9 -10 1.50 1.10 8 -9 -10 -0.20 1.00 7 -9 -10 1.40 1.30 7 -9 -10 0.90 1.20 7 -9 -10 0.40 1.20 6 -9 -10 5.70 1.50 6 -9 -10 5.10 1.70 6 -9 -10 4.30 1.30 5 -9 -10 9.00 1.50 5 -9 -10 9.50 1.90 5 -9 -10 6.60 1.50 4 -9 -10 4.30 1.60 4 -9 -10 3.30 1.30 3 -9 -10 6.00 1.60 3 -9 -10 2.30 1.20 2 -9 -10 44.30 3.20 2 -9 -10 42.20 2.70 2 -9 -10 27.50 8.60 1 -9 -10 -3.20 4.70 0 -9 -10 -1.10 5.10 -1 -9 -10 5.00 4.90 -2 -9 -10 -4.20 5.10 2 9 10 2.70 7.60 -3 -9 -10 8.60 6.10 3 9 10 7.40 8.50 -4 -9 -10 3.20 7.90 4 9 10 -1.00 1.40 4 9 10 -0.20 1.40 4 9 10 9.00 10.30 5 9 10 85.59 4.50 5 9 10 86.69 4.60 6 9 10 46.30 3.30 6 9 10 49.30 3.40 7 9 10 -1.90 1.30 7 9 10 -1.60 1.30 8 9 10 4.40 1.50 8 9 10 2.90 1.40 9 9 10 10.10 1.60 9 9 10 9.40 1.60 10 9 10 10.00 1.50 10 9 10 6.80 1.20 8 -10 -10 5.00 1.10 8 -10 -10 4.80 1.20 7 -10 -10 0.20 1.20 7 -10 -10 -0.30 1.00 7 -10 -10 0.00 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-10 11 4.00 1.60 0 10 -11 16.70 2.00 0 -10 11 22.80 2.80 -1 10 -11 1.20 1.20 1 -10 11 -0.80 1.60 2 -10 11 19.30 2.70 3 -10 11 7.60 1.90 4 -10 11 -0.10 1.40 -5 10 -11 2.00 1.30 5 -10 11 3.40 1.50 -6 10 -11 0.10 1.10 6 -10 11 -1.10 1.10 -7 10 -11 4.20 1.10 7 -10 11 5.10 1.20 6 9 -11 2.90 0.80 6 9 -11 3.00 0.80 5 9 -11 0.10 0.90 5 9 -11 -0.20 0.90 4 9 -11 11.50 1.70 4 9 -11 11.30 1.60 -4 -9 11 10.70 1.70 3 9 -11 1.70 1.20 3 9 -11 -1.20 1.10 -3 -9 11 0.80 1.50 2 9 -11 44.60 2.90 -2 -9 11 49.90 3.50 1 9 -11 20.30 2.20 -1 -9 11 22.20 2.80 0 9 -11 15.20 2.10 0 -9 11 10.60 2.10 -1 9 -11 17.80 2.10 1 -9 11 16.90 2.70 2 -9 11 0.20 1.60 3 -9 11 8.90 1.90 4 -9 11 -0.60 1.30 -5 9 -11 44.50 3.00 5 -9 11 46.50 3.30 -6 9 -11 6.40 1.40 6 -9 11 5.00 1.50 -7 9 -11 6.50 1.30 7 -9 11 7.10 1.40 -8 9 -11 5.80 1.20 8 -9 11 2.30 1.10 6 8 -11 1.00 0.90 6 8 -11 0.80 0.90 5 8 -11 4.50 1.20 5 8 -11 2.30 1.00 -5 -8 11 4.70 1.50 4 8 -11 0.60 1.10 4 8 -11 1.20 1.10 -4 -8 11 1.30 1.60 3 8 -11 4.30 1.30 3 8 -11 5.50 1.30 -3 -8 11 3.50 1.80 2 8 -11 50.89 3.10 -2 -8 11 40.20 3.50 1 8 -11 30.90 2.60 -1 -8 11 38.70 3.40 0 -8 11 6.70 1.90 -1 8 -11 3.90 1.40 1 -8 11 0.90 1.60 -2 8 -11 12.40 2.10 2 -8 11 11.10 2.00 3 -8 11 92.79 5.00 4 -8 11 -0.60 1.40 -5 8 -11 5.20 1.50 5 -8 11 6.80 1.70 -6 8 -11 73.99 3.90 6 -8 11 74.59 4.10 7 -8 11 16.70 2.20 -8 8 -11 27.70 2.10 8 -8 11 30.50 2.20 -9 8 -11 4.30 1.00 7 7 -11 2.70 0.80 6 7 -11 10.60 1.40 6 7 -11 13.10 1.60 5 7 -11 22.30 2.10 5 7 -11 27.50 2.20 5 7 -11 26.50 2.00 4 7 -11 20.00 2.20 4 7 -11 16.50 2.10 4 7 -11 20.90 2.00 3 7 -11 6.40 1.40 3 7 -11 6.80 1.50 3 7 -11 6.00 1.40 2 7 -11 47.10 3.10 2 7 -11 44.50 4.20 1 7 -11 49.40 3.10 -1 -7 11 48.90 3.80 0 7 -11 4.40 1.30 0 -7 11 0.70 1.70 -1 7 -11 42.20 2.90 1 -7 11 39.20 3.40 -2 7 -11 11.80 1.70 2 -7 11 8.40 1.90 3 -7 11 37.80 3.30 4 -7 11 0.70 1.40 5 -7 11 3.30 1.50 6 -7 11 2.80 1.50 7 -7 11 11.00 1.80 8 -7 11 9.10 1.50 7 6 -11 2.90 0.90 6 6 -11 11.00 1.80 6 6 -11 14.60 1.60 6 6 -11 16.40 1.80 5 6 -11 1.30 1.20 5 6 -11 0.40 1.10 5 6 -11 0.80 1.00 4 6 -11 1.20 1.20 4 6 -11 1.20 1.10 4 6 -11 1.80 1.30 3 6 -11 10.20 1.70 3 6 -11 11.90 1.80 3 6 -11 11.90 1.90 2 6 -11 80.49 4.00 2 6 -11 82.69 4.40 2 6 -11 82.09 4.10 1 6 -11 33.70 2.80 1 6 -11 31.80 2.60 0 6 -11 19.70 2.20 0 -6 11 19.00 2.90 -1 6 -11 243.48 9.00 1 -6 11 238.58 9.70 -2 6 -11 26.30 2.30 2 -6 11 20.00 2.70 -3 6 -11 30.10 2.40 3 -6 11 27.40 2.90 4 -6 11 40.80 3.30 5 -6 11 6.50 1.60 6 -6 11 2.60 1.50 6 -6 11 1.10 1.50 7 -6 11 -1.80 1.30 7 -6 11 0.20 1.40 8 -6 11 1.80 1.30 8 -6 11 2.20 1.50 9 -6 11 -0.80 1.20 8 5 -11 1.50 0.70 7 5 -11 2.00 1.00 7 5 -11 3.50 1.10 6 5 -11 6.60 1.30 6 5 -11 8.80 1.50 6 5 -11 8.00 1.40 5 5 -11 0.40 1.20 5 5 -11 -0.20 1.00 5 5 -11 -0.80 1.20 4 5 -11 0.90 1.30 4 5 -11 0.60 1.10 4 5 -11 1.30 1.20 3 5 -11 57.99 3.40 3 5 -11 54.89 3.30 3 5 -11 64.09 3.70 2 5 -11 48.60 3.10 2 5 -11 52.89 3.20 2 5 -11 51.79 3.40 1 5 -11 18.00 2.40 1 5 -11 16.30 2.10 0 5 -11 32.20 2.60 0 5 -11 32.00 2.50 0 -5 11 23.30 13.70 -1 5 -11 13.40 1.90 1 -5 11 7.70 1.90 1 -5 11 11.10 9.00 -2 5 -11 5.50 1.30 2 -5 11 5.50 1.70 -3 5 -11 59.39 3.20 3 -5 11 56.19 3.70 4 -5 11 27.80 2.90 5 -5 11 164.78 6.90 5 -5 11 162.08 7.10 6 -5 11 102.29 5.10 6 -5 11 94.49 4.90 7 -5 11 5.70 1.70 7 -5 11 5.80 1.70 7 -5 11 5.70 1.60 8 -5 11 10.20 1.80 8 -5 11 9.50 1.70 9 -5 11 8.10 1.50 9 -5 11 8.50 1.60 10 -5 11 0.90 1.10 8 4 -11 31.00 1.80 8 4 -11 27.90 1.80 7 4 -11 23.20 2.00 7 4 -11 23.80 1.90 6 4 -11 4.90 1.30 6 4 -11 2.10 1.10 6 4 -11 -0.10 1.20 5 4 -11 9.50 1.50 5 4 -11 13.10 2.10 5 4 -11 16.30 2.20 4 4 -11 100.89 4.60 4 4 -11 102.59 4.70 4 4 -11 101.19 4.90 3 4 -11 1.50 1.20 3 4 -11 3.20 1.20 3 4 -11 0.30 1.30 2 4 -11 6.00 1.50 2 4 -11 4.40 1.30 2 4 -11 2.20 1.20 1 4 -11 1.00 1.20 1 4 -11 2.70 1.10 1 4 -11 2.90 6.00 -1 -4 11 7.40 8.30 0 -4 11 -0.60 8.30 1 -4 11 11.00 8.20 2 -4 11 67.19 13.70 3 -4 11 97.09 14.80 -4 4 -11 21.70 2.40 4 -4 11 19.10 2.80 5 -4 11 25.80 2.90 5 -4 11 24.30 2.80 6 -4 11 7.10 1.80 6 -4 11 6.20 1.80 6 -4 11 5.60 1.70 7 -4 11 7.90 1.80 7 -4 11 4.80 1.70 8 -4 11 -1.60 1.40 8 -4 11 0.10 1.40 9 -4 11 2.00 1.40 9 -4 11 2.30 1.40 10 -4 11 6.40 1.30 10 -4 11 10.90 1.60 8 3 -11 5.00 1.00 8 3 -11 2.70 1.00 7 3 -11 -0.10 1.00 7 3 -11 0.00 1.10 6 3 -11 16.40 2.10 6 3 -11 12.20 1.80 5 3 -11 8.40 1.60 5 3 -11 6.70 1.30 5 3 -11 13.10 2.10 4 3 -11 7.80 1.30 4 3 -11 12.10 1.70 4 3 -11 6.20 1.60 3 3 -11 25.70 2.60 3 3 -11 26.30 2.20 3 3 -11 23.60 2.30 2 3 -11 98.89 12.10 2 3 -11 97.89 4.70 2 3 -11 96.49 4.40 -2 -3 11 95.99 17.30 1 3 -11 21.70 6.90 -1 -3 11 0.70 8.50 0 -3 11 35.10 10.30 1 -3 11 73.59 13.60 2 -3 11 173.48 17.50 3 -3 11 8.50 7.20 4 -3 11 15.40 7.20 5 -3 11 32.10 2.90 5 -3 11 39.00 3.20 6 -3 11 63.09 3.80 6 -3 11 59.69 3.70 7 -3 11 -0.10 1.40 7 -3 11 1.30 1.50 8 -3 11 4.40 1.60 8 -3 11 4.00 1.60 9 -3 11 2.10 1.40 9 -3 11 0.10 1.40 10 -3 11 42.70 2.60 10 -3 11 38.90 2.80 11 -3 11 9.30 1.30 11 -3 11 9.30 1.30 9 2 -11 19.10 1.30 8 2 -11 0.90 1.00 8 2 -11 0.70 0.90 7 2 -11 5.40 1.20 7 2 -11 6.70 1.30 6 2 -11 24.40 2.40 6 2 -11 26.60 2.20 5 2 -11 34.20 2.50 5 2 -11 35.70 2.80 4 2 -11 148.59 6.10 4 2 -11 138.39 5.70 4 2 -11 135.19 5.90 3 2 -11 2.60 1.10 3 2 -11 -0.40 1.10 3 2 -11 0.20 1.30 2 2 -11 -6.80 4.40 -2 -2 11 2.40 7.70 1 2 -11 14.90 5.80 -1 -2 11 4.40 7.00 0 2 -11 8.20 4.70 0 -2 11 3.00 6.50 1 -2 11 0.10 5.60 2 -2 11 5.90 6.00 3 -2 11 10.20 6.70 4 -2 11 -2.00 5.70 -5 2 -11 7.30 6.40 5 -2 11 -0.40 1.50 5 -2 11 -9.00 6.80 6 -2 11 128.79 5.90 6 -2 11 130.09 5.90 7 -2 11 15.10 2.50 7 -2 11 21.30 2.50 8 -2 11 16.80 2.30 8 -2 11 15.60 2.60 9 -2 11 43.20 3.20 9 -2 11 38.40 2.90 10 -2 11 5.80 1.60 10 -2 11 8.00 1.50 11 -2 11 1.20 1.00 11 -2 11 1.30 0.90 9 1 -11 2.10 0.80 9 1 -11 1.30 0.70 8 1 -11 6.30 1.30 8 1 -11 5.80 1.20 7 1 -11 24.90 2.10 7 1 -11 25.50 2.30 6 1 -11 8.10 1.70 6 1 -11 8.50 1.40 5 1 -11 74.89 3.80 5 1 -11 79.49 4.20 4 1 -11 9.20 1.70 4 1 -11 8.10 1.40 3 1 -11 30.40 8.60 3 1 -11 15.90 2.10 -3 -1 11 14.50 10.20 2 1 -11 7.10 4.90 -2 -1 11 -7.60 6.30 1 1 -11 -0.60 3.70 -1 -1 11 -5.80 5.60 0 1 -11 27.20 6.60 0 -1 11 21.20 8.80 -1 1 -11 3.30 4.00 1 -1 11 6.60 5.60 2 -1 11 62.49 10.70 3 -1 11 11.00 6.60 -4 1 -11 23.30 6.90 4 -1 11 28.10 9.30 -5 1 -11 24.30 8.30 5 -1 11 23.90 9.40 6 -1 11 0.80 1.40 6 -1 11 0.00 1.40 7 -1 11 0.80 1.40 7 -1 11 1.90 1.40 8 -1 11 3.70 1.60 8 -1 11 3.70 1.50 9 -1 11 1.30 1.40 9 -1 11 1.10 1.30 10 -1 11 30.40 2.40 10 -1 11 30.20 2.50 11 -1 11 31.90 2.00 11 -1 11 30.30 2.20 9 0 -11 6.90 1.10 9 0 -11 5.10 1.00 8 0 -11 2.70 1.00 8 0 -11 5.00 1.20 7 0 -11 0.90 1.00 7 0 -11 0.00 1.30 6 0 -11 14.70 1.90 6 0 -11 12.80 2.20 5 0 -11 11.00 1.80 5 0 -11 13.80 1.90 4 0 -11 34.40 2.40 4 0 -11 36.00 2.90 3 0 -11 26.60 7.30 -3 0 11 30.90 10.30 2 0 -11 63.19 8.90 -2 0 11 48.80 11.40 1 0 -11 7.40 4.70 -1 0 11 -0.70 5.60 0 0 -11 3.50 4.00 0 0 11 1.90 5.50 -1 0 -11 6.10 4.20 1 0 11 5.10 5.60 2 0 11 20.50 7.10 3 0 11 9.00 6.00 -4 0 -11 6.30 5.30 4 0 11 2.40 5.60 -5 0 -11 -6.80 5.10 5 0 11 3.00 6.80 6 0 11 11.90 1.90 6 0 11 10.70 1.80 7 0 11 5.40 1.70 7 0 11 7.40 1.80 8 0 11 -0.40 1.30 8 0 11 -0.40 1.30 9 0 11 7.20 1.70 9 0 11 8.60 1.90 10 0 11 59.29 3.30 10 0 11 55.39 3.40 11 0 11 2.90 1.00 11 0 11 0.70 1.00 9 -1 -11 14.70 1.40 9 -1 -11 13.00 1.50 8 -1 -11 13.50 1.80 8 -1 -11 14.30 1.60 7 -1 -11 15.70 2.20 7 -1 -11 17.50 1.90 6 -1 -11 6.40 1.50 6 -1 -11 10.10 1.50 5 -1 -11 49.40 3.30 5 -1 -11 45.90 2.90 4 -1 -11 51.79 2.90 4 -1 -11 51.79 3.30 3 -1 -11 64.29 10.80 -3 1 11 53.19 12.10 2 -1 -11 3.20 4.60 -2 1 11 -2.10 5.30 1 -1 -11 42.80 7.90 -1 1 11 24.80 8.10 0 -1 -11 254.67 15.50 0 1 11 210.68 18.40 -1 -1 -11 11.80 4.80 1 1 11 10.30 6.30 -2 -1 -11 67.69 8.10 2 1 11 53.59 10.10 3 1 11 97.99 12.80 -4 -1 -11 52.49 9.50 4 1 11 67.89 12.10 -5 -1 -11 0.40 5.40 5 1 11 8.00 7.60 6 1 11 10.50 1.80 6 1 11 12.40 1.90 6 1 11 11.30 1.90 7 1 11 57.99 3.60 7 1 11 55.09 3.60 7 1 11 58.19 3.80 8 1 11 6.80 1.70 8 1 11 7.60 1.70 9 1 11 44.00 3.10 9 1 11 41.70 3.00 10 1 11 1.40 1.40 10 1 11 4.20 1.40 11 1 11 55.39 2.90 11 1 11 60.79 3.00 9 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2.70 1.50 6 7 11 4.20 1.70 7 7 11 37.50 3.00 7 7 11 37.80 3.00 7 7 11 32.00 2.90 8 7 11 13.50 2.00 8 7 11 13.10 2.20 8 7 11 14.40 2.20 9 7 11 16.70 2.20 9 7 11 12.60 2.00 10 7 11 11.80 1.60 10 7 11 10.90 1.70 9 -8 -11 7.80 1.10 -9 8 11 7.40 1.70 8 -8 -11 24.70 1.70 8 -8 -11 23.70 2.00 8 -8 -11 21.00 2.00 7 -8 -11 1.80 1.10 7 -8 -11 0.60 1.10 7 -8 -11 0.00 1.20 6 -8 -11 18.10 2.20 6 -8 -11 15.90 2.30 6 -8 -11 13.10 1.90 5 -8 -11 0.30 1.10 5 -8 -11 0.70 1.30 5 -8 -11 0.80 1.40 4 -8 -11 25.30 2.70 4 -8 -11 22.90 2.30 3 -8 -11 0.30 1.30 3 -8 -11 1.80 1.30 2 -8 -11 -0.30 1.10 2 -8 -11 -4.50 5.20 2 -8 -11 0.90 1.30 1 -8 -11 8.10 5.40 0 -8 -11 98.39 11.20 -1 -8 -11 49.60 9.40 -2 -8 -11 3.30 5.30 -3 -8 -11 46.10 9.00 3 8 11 34.10 10.80 -4 -8 -11 -6.50 6.30 4 8 11 2.60 1.40 4 8 11 0.70 2.50 4 8 11 5.40 9.40 4 8 11 -0.60 1.50 5 8 11 17.10 2.40 5 8 11 23.20 2.60 5 8 11 19.80 2.60 6 8 11 110.89 5.40 6 8 11 114.29 5.30 6 8 11 116.09 5.30 7 8 11 -0.50 1.30 7 8 11 0.10 1.40 8 8 11 62.09 3.80 8 8 11 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5.90 1.30 6 -9 12 2.90 1.30 -7 9 -12 18.30 1.80 7 -9 12 21.10 1.90 -8 9 -12 35.80 2.10 8 -9 12 31.50 2.40 6 8 -12 0.70 0.70 6 8 -12 1.20 0.80 5 8 -12 0.60 0.90 5 8 -12 1.30 1.00 -5 -8 12 1.00 1.20 4 8 -12 0.60 1.10 4 8 -12 0.80 1.00 -4 -8 12 0.00 1.30 3 8 -12 -0.20 1.10 3 8 -12 -1.10 1.10 -3 -8 12 0.00 1.50 2 8 -12 6.30 1.40 -2 -8 12 2.20 1.70 1 8 -12 11.00 1.70 -1 -8 12 9.60 2.00 0 8 -12 4.70 1.30 0 -8 12 5.10 1.70 -1 8 -12 6.00 1.40 1 -8 12 2.40 1.70 -2 8 -12 -1.20 1.10 2 -8 12 0.30 1.60 3 -8 12 0.50 1.50 4 -8 12 67.29 4.00 5 -8 12 20.70 2.50 -6 8 -12 2.30 1.20 6 -8 12 0.70 1.30 -7 8 -12 16.10 1.80 7 -8 12 12.60 2.00 -8 8 -12 2.30 1.00 8 -8 12 1.20 1.00 6 7 -12 4.70 1.00 6 7 -12 4.30 0.90 -6 -7 12 5.30 1.20 5 7 -12 3.70 1.10 5 7 -12 1.00 1.00 -5 -7 12 1.10 1.30 4 7 -12 0.40 1.00 4 7 -12 1.30 1.10 3 7 -12 19.50 2.10 3 7 -12 21.20 2.00 2 7 -12 8.70 1.60 -2 -7 12 6.70 1.90 1 7 -12 4.30 1.30 -1 -7 12 6.90 2.00 0 7 -12 216.18 8.30 0 -7 12 219.28 9.10 -1 7 -12 9.50 1.60 1 -7 12 7.10 1.90 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51.39 3.50 1 5 -12 51.69 3.10 0 5 -12 26.30 2.30 -1 5 -12 1.40 1.10 1 -5 12 -0.60 1.50 -2 5 -12 0.90 1.10 2 -5 12 1.50 1.50 -3 5 -12 2.50 1.20 3 -5 12 1.10 1.40 -4 5 -12 65.59 4.50 4 -5 12 58.59 3.90 5 -5 12 62.59 3.90 5 -5 12 57.69 4.00 6 -5 12 -1.40 1.50 6 -5 12 1.30 1.30 7 -5 12 -0.10 1.40 7 -5 12 -1.80 1.20 8 -5 12 3.60 1.40 8 -5 12 2.20 1.50 9 -5 12 4.80 1.30 10 -5 12 7.30 1.30 7 4 -12 15.90 1.60 7 4 -12 19.10 1.70 6 4 -12 15.90 1.70 6 4 -12 14.10 1.80 5 4 -12 0.10 1.10 5 4 -12 1.00 1.20 5 4 -12 -0.80 1.00 4 4 -12 0.50 1.30 4 4 -12 1.40 1.20 4 4 -12 1.60 1.10 3 4 -12 23.10 2.60 3 4 -12 19.50 2.20 3 4 -12 19.70 2.20 2 4 -12 19.20 2.20 2 4 -12 18.50 2.40 2 4 -12 22.50 2.20 1 4 -12 27.70 2.30 1 4 -12 26.10 2.60 0 4 -12 82.19 4.30 0 4 -12 86.39 4.00 -1 4 -12 -0.90 1.00 -2 4 -12 12.50 1.90 2 -4 12 13.10 2.10 -3 4 -12 52.59 3.00 3 -4 12 44.00 3.40 -4 4 -12 69.89 3.60 4 -4 12 66.79 4.20 5 -4 12 5.90 1.80 5 -4 12 6.20 2.50 6 -4 12 4.30 1.60 6 -4 12 1.00 1.60 6 -4 12 6.30 2.10 7 -4 12 37.50 3.00 7 -4 12 39.20 3.00 8 -4 12 1.20 1.40 8 -4 12 4.60 1.60 9 -4 12 30.30 2.40 9 -4 12 27.00 2.30 10 -4 12 27.60 1.90 8 3 -12 29.30 1.80 8 3 -12 29.70 1.70 7 3 -12 21.40 1.90 7 3 -12 17.40 1.80 6 3 -12 10.10 1.50 6 3 -12 11.10 1.80 5 3 -12 -0.90 1.20 5 3 -12 0.70 1.00 5 3 -12 2.30 1.30 4 3 -12 3.90 1.40 4 3 -12 0.90 1.10 4 3 -12 0.10 1.30 3 3 -12 75.09 4.10 3 3 -12 72.69 3.80 3 3 -12 72.49 3.60 2 3 -12 25.30 2.20 2 3 -12 23.70 2.60 2 3 -12 19.60 2.10 1 3 -12 6.30 1.60 1 3 -12 12.30 6.80 1 3 -12 7.20 1.40 0 3 -12 5.40 1.40 0 3 -12 5.00 1.20 0 -3 12 -0.10 8.10 -1 3 -12 57.39 4.10 1 -3 12 49.90 12.40 -2 3 -12 41.00 3.40 2 -3 12 31.40 9.80 -3 3 -12 0.40 1.20 3 -3 12 -1.90 1.30 3 -3 12 -4.80 8.60 -4 3 -12 10.40 1.60 4 -3 12 5.00 1.70 -5 3 -12 65.39 3.80 5 -3 12 60.29 5.10 6 -3 12 69.19 4.10 6 -3 12 74.19 4.20 7 -3 12 4.40 1.60 7 -3 12 3.00 1.60 8 -3 12 35.10 3.00 8 -3 12 31.20 2.80 9 -3 12 16.30 2.30 9 -3 12 16.50 2.20 10 -3 12 4.40 1.20 10 -3 12 1.80 1.10 8 2 -12 22.90 1.70 8 2 -12 24.50 1.70 7 2 -12 34.00 2.40 7 2 -12 34.60 2.30 6 2 -12 16.10 2.10 6 2 -12 17.30 1.90 5 2 -12 13.40 2.20 5 2 -12 15.50 1.90 4 2 -12 7.20 1.50 4 2 -12 8.10 1.40 4 2 -12 10.00 1.70 3 2 -12 16.60 2.10 3 2 -12 18.50 2.10 3 2 -12 17.50 2.40 2 2 -12 39.50 2.60 2 2 -12 36.40 2.60 2 2 -12 43.70 2.90 1 2 -12 45.20 4.20 1 2 -12 37.80 2.80 1 2 -12 25.60 8.20 -1 -2 12 26.80 10.80 0 -2 12 17.80 9.10 1 -2 12 -0.20 7.50 2 -2 12 3.90 6.00 3 -2 12 140.29 17.70 -4 2 -12 10.80 1.80 4 -2 12 11.60 9.80 -5 2 -12 19.00 2.20 5 -2 12 16.10 2.60 6 -2 12 15.20 2.30 6 -2 12 11.30 2.00 7 -2 12 30.90 2.90 7 -2 12 27.90 2.70 8 -2 12 -0.40 1.40 8 -2 12 0.90 1.40 9 -2 12 14.50 2.30 9 -2 12 17.60 2.20 10 -2 12 13.30 2.00 10 -2 12 14.20 1.90 8 1 -12 7.80 1.30 8 1 -12 7.60 1.20 7 1 -12 2.70 1.20 7 1 -12 4.40 1.20 6 1 -12 2.60 1.30 6 1 -12 5.00 1.20 5 1 -12 37.40 2.80 5 1 -12 34.90 2.50 4 1 -12 4.50 1.50 4 1 -12 8.30 1.40 3 1 -12 -0.90 1.20 3 1 -12 -0.70 1.10 3 1 -12 1.10 1.10 2 1 -12 27.20 2.30 2 1 -12 30.00 8.40 2 1 -12 26.20 2.30 -2 -1 12 46.50 11.90 1 1 -12 2.30 4.70 -1 -1 12 6.90 7.50 0 1 -12 16.00 6.00 0 -1 12 21.70 9.50 1 -1 12 6.50 6.70 2 -1 12 152.68 16.20 3 -1 12 15.20 8.20 4 -1 12 29.60 10.60 -5 1 -12 -1.40 1.10 5 -1 12 -1.40 1.50 -6 1 -12 -0.80 1.30 6 -1 12 1.40 1.50 6 -1 12 0.80 1.50 7 -1 12 0.20 1.50 7 -1 12 3.10 1.50 8 -1 12 45.80 3.40 8 -1 12 46.50 3.20 9 -1 12 9.30 1.70 9 -1 12 6.70 1.70 10 -1 12 0.20 1.20 10 -1 12 2.00 1.20 11 -1 12 4.30 1.00 11 -1 12 5.20 1.10 8 0 -12 6.40 1.20 8 0 -12 9.80 1.40 7 0 -12 25.70 2.00 7 0 -12 22.70 2.10 6 0 -12 62.19 3.60 6 0 -12 60.49 3.30 5 0 -12 46.50 2.90 5 0 -12 51.29 3.40 4 0 -12 98.39 4.40 4 0 -12 101.39 4.90 3 0 -12 0.40 1.30 3 0 -12 2.50 1.10 2 0 -12 -3.60 4.30 -2 0 12 1.70 8.00 1 0 -12 7.00 4.90 -1 0 12 -1.80 6.40 0 0 -12 64.69 9.50 0 0 12 59.89 12.50 -1 0 -12 0.20 4.10 1 0 12 6.90 6.00 2 0 12 47.00 9.90 3 0 12 -0.40 5.60 4 0 12 0.20 6.10 -5 0 -12 9.40 1.50 5 0 12 8.60 1.70 5 0 12 -1.70 7.90 -6 0 -12 1.50 1.20 6 0 12 -1.90 1.20 6 0 12 -1.00 1.30 -7 0 -12 -1.60 1.90 7 0 12 -0.20 1.40 7 0 12 3.80 1.60 8 0 12 168.38 6.90 8 0 12 154.18 6.90 9 0 12 5.20 1.50 9 0 12 4.80 1.60 10 0 12 79.29 3.80 10 0 12 76.09 3.90 11 0 12 -1.50 0.90 11 0 12 -0.20 0.80 9 -1 -12 4.50 0.90 9 -1 -12 1.60 0.70 8 -1 -12 -0.90 0.90 8 -1 -12 1.30 0.90 7 -1 -12 4.70 1.20 7 -1 -12 4.70 1.40 6 -1 -12 6.90 1.30 6 -1 -12 6.00 1.60 5 -1 -12 8.10 1.40 5 -1 -12 8.80 1.80 4 -1 -12 2.90 1.10 4 -1 -12 2.40 1.50 3 -1 -12 9.80 1.70 3 -1 -12 13.00 1.80 2 -1 -12 24.00 7.30 -2 1 12 34.90 11.10 1 -1 -12 37.30 7.60 -1 1 12 16.30 8.70 0 -1 -12 44.60 8.50 0 1 12 37.80 10.00 -1 -1 -12 26.80 6.70 1 1 12 12.60 6.60 2 1 12 117.29 14.40 3 1 12 8.40 7.10 4 1 12 35.90 8.90 -5 -1 -12 -9.20 8.30 5 1 12 7.30 8.50 5 1 12 0.70 1.40 5 1 12 1.80 1.30 6 1 12 1.90 1.50 6 1 12 1.80 1.40 6 1 12 0.30 1.60 7 1 12 20.80 2.60 7 1 12 20.80 2.50 8 1 12 60.59 3.80 8 1 12 63.49 3.80 9 1 12 1.30 1.40 9 1 12 -0.40 1.30 10 1 12 15.60 1.90 10 1 12 14.20 2.00 11 1 12 0.10 0.90 11 1 12 1.00 0.90 9 -2 -12 0.10 0.70 9 -2 -12 -0.10 0.70 8 -2 -12 7.60 1.20 8 -2 -12 6.50 1.30 7 -2 -12 4.30 1.40 7 -2 -12 3.10 1.10 6 -2 -12 12.30 2.20 6 -2 -12 14.70 1.90 5 -2 -12 106.89 4.90 5 -2 -12 91.69 4.40 4 -2 -12 46.40 2.80 4 -2 -12 48.90 3.20 3 -2 -12 16.50 1.90 3 -2 -12 16.30 2.30 3 -2 -12 14.00 7.90 -3 2 12 25.80 11.60 2 -2 -12 3.70 5.00 -2 2 12 1.60 6.20 1 -2 -12 18.50 6.60 -1 2 12 10.50 7.40 0 -2 -12 2.70 4.20 0 2 12 2.60 6.10 -1 -2 -12 26.80 6.60 1 2 12 19.30 8.50 -2 -2 -12 29.60 6.70 2 2 12 26.10 8.60 3 2 12 9.70 6.60 4 2 12 -0.30 6.50 -5 -2 -12 7.50 7.30 5 2 12 9.80 1.80 5 2 12 13.70 2.20 6 2 12 109.09 5.20 6 2 12 101.99 5.00 6 2 12 111.09 5.20 7 2 12 8.50 1.80 7 2 12 8.90 1.80 7 2 12 9.00 1.90 8 2 12 14.30 2.40 8 2 12 18.00 2.40 8 2 12 19.70 2.60 9 2 12 33.50 2.70 9 2 12 36.20 2.80 10 2 12 10.70 1.70 10 2 12 7.60 1.50 11 2 12 2.00 1.00 11 2 12 0.50 0.90 9 -3 -12 14.10 1.20 9 -3 -12 12.30 1.30 8 -3 -12 5.40 1.10 8 -3 -12 8.20 1.40 7 -3 -12 0.80 1.20 7 -3 -12 2.90 1.10 6 -3 -12 0.90 1.10 6 -3 -12 2.60 1.30 5 -3 -12 119.69 5.60 5 -3 -12 125.59 5.30 4 -3 -12 2.90 1.20 4 -3 -12 4.10 1.50 3 -3 -12 0.70 1.30 3 -3 -12 0.10 1.00 3 -3 -12 3.90 5.60 -3 3 12 7.70 8.20 2 -3 -12 231.98 16.80 -2 3 12 186.98 19.10 1 -3 -12 3.40 5.00 -1 3 12 5.40 7.90 0 -3 -12 3.30 4.30 0 3 12 0.70 5.90 -1 -3 -12 -2.30 4.20 1 3 12 1.40 5.70 -2 -3 -12 64.89 8.80 2 3 12 30.20 9.20 3 3 12 20.30 8.00 -5 -3 -12 112.59 14.50 5 3 12 106.09 5.00 6 3 12 2.70 1.60 6 3 12 6.10 1.60 6 3 12 2.10 1.50 7 3 12 5.60 1.60 7 3 12 5.20 1.60 7 3 12 3.10 1.60 8 3 12 6.30 1.70 8 3 12 4.30 1.60 8 3 12 7.20 1.70 9 3 12 5.10 1.50 9 3 12 4.70 1.50 10 3 12 9.20 1.60 10 3 12 6.60 1.50 11 3 12 21.10 1.60 11 3 12 21.30 1.80 9 -4 -12 1.10 0.80 9 -4 -12 -0.80 0.70 8 -4 -12 -0.80 0.90 8 -4 -12 -2.20 1.00 7 -4 -12 1.30 1.00 7 -4 -12 4.00 1.30 6 -4 -12 3.70 1.40 6 -4 -12 2.90 1.20 5 -4 -12 48.50 3.50 5 -4 -12 52.89 3.10 5 -4 -12 51.19 3.40 4 -4 -12 4.70 1.60 4 -4 -12 4.80 1.80 4 -4 -12 4.00 1.20 3 -4 -12 29.60 2.60 3 -4 -12 26.00 2.10 3 -4 -12 41.00 11.80 -3 4 12 15.40 9.70 2 -4 -12 66.79 10.90 -2 4 12 62.99 12.60 1 -4 -12 116.89 12.00 -1 4 12 97.89 14.60 0 -4 -12 47.20 8.50 0 4 12 40.30 10.70 -1 -4 -12 28.40 6.50 1 4 12 14.20 6.80 -2 -4 -12 350.56 20.00 2 4 12 321.97 22.90 -3 -4 -12 180.18 14.20 -5 -4 -12 134.99 15.40 5 4 12 104.99 5.00 5 4 12 103.79 4.90 6 4 12 11.70 1.90 6 4 12 11.80 1.90 6 4 12 13.50 2.30 7 4 12 33.90 3.00 7 4 12 31.50 2.90 7 4 12 29.00 2.90 8 4 12 20.20 2.50 8 4 12 27.80 2.60 8 4 12 21.30 2.60 9 4 12 0.80 1.30 9 4 12 0.60 1.30 9 4 12 -0.30 1.30 10 4 12 24.00 2.20 10 4 12 22.20 2.00 11 4 12 11.70 1.50 11 4 12 13.10 1.40 9 -5 -12 7.10 1.20 8 -5 -12 4.70 1.20 8 -5 -12 7.40 1.10 7 -5 -12 1.50 1.00 7 -5 -12 -0.50 1.10 6 -5 -12 2.40 1.20 6 -5 -12 2.90 1.40 6 -5 -12 5.10 1.70 5 -5 -12 -1.80 1.30 5 -5 -12 0.00 1.50 5 -5 -12 -0.60 1.10 4 -5 -12 17.50 2.40 4 -5 -12 17.90 2.50 4 -5 -12 12.90 2.00 3 -5 -12 19.70 1.90 3 -5 -12 21.90 2.50 3 -5 -12 15.10 2.50 2 -5 -12 235.78 17.70 -2 5 12 221.88 21.00 1 -5 -12 20.10 7.30 -1 5 12 34.00 10.80 0 -5 -12 8.20 5.70 0 5 12 23.80 9.40 -1 -5 -12 55.09 9.20 1 5 12 55.79 17.20 -2 -5 -12 2.20 4.40 -3 -5 -12 92.09 11.10 5 5 12 79.69 4.20 5 5 12 80.89 4.20 5 5 12 78.59 4.20 6 5 12 38.50 3.10 6 5 12 41.60 3.10 6 5 12 41.10 3.00 7 5 12 100.79 5.00 7 5 12 94.09 4.90 7 5 12 102.89 5.00 8 5 12 11.50 1.90 8 5 12 12.50 2.00 8 5 12 11.40 1.90 9 5 12 1.00 1.20 9 5 12 0.00 1.20 9 5 12 0.90 1.30 10 5 12 2.70 1.20 10 5 12 2.20 1.10 11 5 12 3.10 1.00 8 -6 -12 20.00 1.70 8 -6 -12 19.50 1.90 -8 6 12 20.50 2.20 7 -6 -12 0.80 1.00 7 -6 -12 0.50 1.10 7 -6 -12 0.90 1.20 6 -6 -12 0.40 1.30 6 -6 -12 1.10 1.20 6 -6 -12 0.20 1.40 5 -6 -12 -0.20 1.30 5 -6 -12 1.70 1.20 5 -6 -12 0.50 1.50 4 -6 -12 150.18 6.40 4 -6 -12 140.19 6.50 4 -6 -12 151.48 6.00 3 -6 -12 36.40 3.00 3 -6 -12 35.40 2.50 2 -6 -12 171.28 15.50 -2 6 12 190.08 20.00 1 -6 -12 2.80 5.60 -1 6 12 4.50 7.80 0 -6 -12 19.50 6.40 -1 -6 -12 9.20 5.50 -2 -6 -12 9.80 5.80 -3 -6 -12 152.08 14.60 4 6 12 0.70 1.90 5 6 12 5.00 1.70 5 6 12 5.60 1.50 5 6 12 6.40 1.60 6 6 12 -1.30 1.30 6 6 12 -0.40 1.30 6 6 12 -0.10 1.40 7 6 12 0.00 1.40 7 6 12 -0.60 1.30 7 6 12 0.60 1.40 8 6 12 6.50 1.70 8 6 12 4.80 1.60 8 6 12 7.50 1.70 9 6 12 6.60 1.50 9 6 12 5.90 1.40 9 6 12 4.80 1.50 10 6 12 1.60 1.00 10 6 12 -0.20 1.10 8 -7 -12 2.90 1.00 8 -7 -12 2.60 1.00 -8 7 12 4.10 1.50 7 -7 -12 4.40 1.20 7 -7 -12 8.20 1.50 7 -7 -12 3.00 1.30 6 -7 -12 -0.30 1.20 6 -7 -12 2.40 1.50 6 -7 -12 0.90 1.10 5 -7 -12 10.20 1.70 5 -7 -12 6.20 1.40 5 -7 -12 4.60 1.70 4 -7 -12 4.00 1.70 4 -7 -12 4.00 1.30 4 -7 -12 3.90 1.50 3 -7 -12 144.59 6.00 3 -7 -12 148.29 6.40 2 -7 -12 48.60 2.90 2 -7 -12 40.90 13.90 1 -7 -12 84.49 11.00 0 -7 -12 11.40 5.70 -1 -7 -12 5.80 5.30 -2 -7 -12 25.00 7.90 -3 -7 -12 25.70 8.30 -4 -7 -12 3.80 7.40 4 7 12 1.80 1.60 4 7 12 1.80 1.20 5 7 12 34.20 2.90 5 7 12 37.30 3.10 5 7 12 39.10 3.10 6 7 12 10.00 1.90 6 7 12 8.20 1.70 6 7 12 8.10 1.80 7 7 12 -0.30 1.30 7 7 12 0.70 1.30 7 7 12 -0.10 1.30 8 7 12 -0.70 1.30 8 7 12 0.50 1.30 8 7 12 1.00 1.30 9 7 12 2.20 1.30 9 7 12 3.90 1.40 10 7 12 30.50 2.20 10 7 12 35.80 2.20 8 -8 -12 11.80 1.40 8 -8 -12 12.40 1.40 -8 8 12 9.60 1.70 7 -8 -12 0.00 1.10 7 -8 -12 1.50 1.00 7 -8 -12 1.10 1.20 6 -8 -12 0.50 1.40 6 -8 -12 -1.80 1.00 6 -8 -12 -1.60 1.20 5 -8 -12 6.10 1.40 5 -8 -12 7.20 1.80 5 -8 -12 4.90 1.50 4 -8 -12 4.80 1.30 4 -8 -12 3.70 1.70 3 -8 -12 25.50 2.90 3 -8 -12 30.90 2.40 2 -8 -12 103.69 4.60 1 -8 -12 1.80 1.20 1 -8 -12 7.40 6.00 -1 8 12 -0.10 1.60 0 -8 -12 7.30 5.50 -1 -8 -12 2.60 6.50 -2 -8 -12 119.49 14.00 -3 -8 -12 -5.30 6.60 3 8 12 2.10 1.40 3 8 12 2.10 1.60 4 8 12 138.29 5.90 4 8 12 122.29 6.00 4 8 12 140.89 6.00 5 8 12 9.80 1.90 5 8 12 7.20 1.60 5 8 12 6.10 1.80 6 8 12 4.90 1.80 6 8 12 8.50 1.70 6 8 12 8.10 1.80 7 8 12 0.80 1.40 7 8 12 -0.50 1.30 7 8 12 0.30 1.30 8 8 12 18.50 2.40 8 8 12 20.80 2.40 9 8 12 1.10 1.20 9 8 12 -1.20 1.10 10 8 12 5.90 1.10 10 8 12 6.70 1.20 8 -9 -12 4.60 1.00 8 -9 -12 3.40 0.80 -8 9 12 5.10 1.40 7 -9 -12 0.50 1.10 7 -9 -12 2.00 1.00 6 -9 -12 -1.40 1.20 6 -9 -12 0.80 1.10 6 -9 -12 0.50 1.20 5 -9 -12 7.20 1.70 5 -9 -12 5.60 1.40 5 -9 -12 7.20 1.70 4 -9 -12 56.09 3.20 4 -9 -12 54.89 3.60 3 -9 -12 7.70 1.50 3 -9 -12 8.30 1.90 2 -9 -12 42.10 2.80 1 -9 -12 61.39 3.30 -1 9 12 55.59 4.10 0 -9 -12 20.30 2.20 0 9 12 20.10 2.90 -1 -9 -12 15.50 2.10 1 9 12 11.40 2.20 2 9 12 38.70 3.20 3 9 12 31.20 3.10 3 9 12 29.90 2.80 4 9 12 2.90 1.60 4 9 12 1.10 1.40 4 9 12 -0.10 1.50 5 9 12 17.20 2.40 5 9 12 16.80 2.50 5 9 12 21.60 2.60 6 9 12 11.10 1.90 6 9 12 8.80 1.80 7 9 12 17.90 2.30 7 9 12 16.90 2.30 8 9 12 2.00 1.30 8 9 12 4.00 1.40 9 9 12 23.80 2.20 9 9 12 28.30 2.30 10 9 12 4.30 1.00 10 9 12 4.20 1.00 -8 10 12 0.60 1.10 7 -10 -12 0.60 0.90 7 -10 -12 1.80 1.00 6 -10 -12 6.70 1.50 6 -10 -12 7.30 1.30 6 -10 -12 9.50 1.60 5 -10 -12 -1.20 1.30 5 -10 -12 1.30 1.10 4 -10 -12 33.40 2.90 4 -10 -12 27.40 2.40 3 -10 -12 102.49 4.70 2 -10 -12 88.49 4.20 -2 10 12 87.09 5.00 1 -10 -12 18.50 2.10 -1 10 12 10.10 2.30 0 -10 -12 40.90 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7.30 1.70 2 3 -13 6.80 1.50 1 3 -13 23.90 2.30 1 3 -13 32.00 2.70 0 3 -13 204.58 8.20 0 3 -13 216.38 8.00 -1 3 -13 5.50 1.30 -2 3 -13 161.38 6.40 2 -3 13 157.48 7.00 -3 3 -13 4.70 1.40 3 -3 13 1.60 1.50 -4 3 -13 172.38 6.60 4 -3 13 156.88 7.10 -5 3 -13 13.80 2.20 6 -3 13 4.60 1.80 6 -3 13 -2.30 1.40 7 -3 13 20.20 2.50 7 -3 13 20.80 2.60 8 -3 13 7.10 1.70 8 -3 13 5.20 1.60 9 -3 13 1.10 1.20 9 -3 13 2.10 1.20 10 -3 13 6.70 1.20 10 -3 13 5.40 1.20 8 2 -13 0.30 0.60 8 2 -13 1.50 0.80 7 2 -13 0.50 1.00 7 2 -13 1.60 1.00 6 2 -13 5.30 1.20 6 2 -13 3.80 1.20 5 2 -13 0.50 1.30 5 2 -13 4.00 1.20 4 2 -13 1.60 1.20 4 2 -13 1.50 1.10 4 2 -13 3.90 1.50 3 2 -13 54.19 3.20 3 2 -13 47.90 3.30 3 2 -13 51.49 3.00 2 2 -13 31.90 2.50 2 2 -13 31.80 2.40 2 2 -13 32.50 2.70 1 2 -13 21.00 2.10 1 2 -13 22.50 2.40 0 2 -13 78.89 3.80 0 2 -13 76.99 4.00 -1 2 -13 30.60 2.40 -1 2 -13 28.90 2.40 -2 2 -13 96.89 4.40 2 -2 13 101.69 5.10 -3 2 -13 65.59 3.50 3 -2 13 64.89 3.90 -4 2 -13 7.50 1.50 -5 2 -13 41.60 2.90 5 -2 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6.20 1.30 8 0 -13 1.80 0.90 8 0 -13 2.70 0.90 7 0 -13 20.00 1.90 7 0 -13 20.70 1.80 6 0 -13 -0.70 0.90 6 0 -13 -0.10 1.20 5 0 -13 2.20 1.40 5 0 -13 0.20 1.00 4 0 -13 20.80 2.10 4 0 -13 20.10 2.40 3 0 -13 6.30 1.30 3 0 -13 2.60 1.30 3 0 -13 4.00 1.50 2 0 -13 180.08 7.10 2 0 -13 189.58 7.40 2 0 -13 180.68 7.00 1 0 -13 11.70 1.80 1 0 -13 28.30 7.90 1 0 -13 11.10 1.90 -1 0 13 5.70 8.40 0 0 -13 151.68 13.90 0 0 13 148.99 18.80 1 0 13 43.30 11.50 2 0 13 21.10 9.40 -3 0 -13 -0.40 1.70 3 0 13 -3.80 6.40 -4 0 -13 157.68 6.30 4 0 13 164.18 6.70 4 0 13 148.29 25.00 -5 0 -13 16.20 2.10 5 0 13 15.70 2.40 -6 0 -13 34.80 2.60 6 0 13 30.50 2.90 6 0 13 33.00 2.90 -7 0 -13 -1.10 1.20 7 0 13 1.70 1.50 7 0 13 -0.70 1.40 8 0 13 80.19 4.40 8 0 13 81.59 4.20 9 0 13 6.30 1.60 9 0 13 11.80 2.00 10 0 13 36.00 2.50 10 0 13 38.30 2.60 8 -1 -13 1.10 0.80 8 -1 -13 1.90 1.00 7 -1 -13 16.40 1.90 7 -1 -13 16.30 1.80 6 -1 -13 22.30 2.40 6 -1 -13 22.00 2.00 5 -1 -13 1.80 1.10 5 -1 -13 0.70 1.40 4 -1 -13 53.59 3.60 4 -1 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2 1 -15 9.10 1.70 1 1 -15 9.90 1.50 1 1 -15 6.80 1.60 0 1 -15 -1.10 1.00 0 1 -15 1.50 1.20 -1 1 -15 22.30 2.20 -2 1 -15 19.60 2.10 -3 1 -15 10.40 1.70 -4 1 -15 2.90 1.30 -5 1 -15 148.59 6.10 5 -1 15 147.69 6.50 -6 1 -15 119.69 5.30 6 -1 15 130.69 5.80 -7 1 -15 -2.00 1.30 7 -1 15 2.60 1.50 8 -1 15 9.80 1.70 8 -1 15 7.00 1.60 9 -1 15 -0.80 1.00 9 -1 15 -0.70 1.10 7 0 -15 16.50 1.50 7 0 -15 16.70 1.40 6 0 -15 1.30 1.10 6 0 -15 0.90 1.00 5 0 -15 5.30 1.20 5 0 -15 3.10 1.30 4 0 -15 28.70 2.60 4 0 -15 31.00 2.30 3 0 -15 -0.40 1.20 3 0 -15 -0.30 1.10 3 0 -15 -1.10 1.10 2 0 -15 82.09 4.30 2 0 -15 86.79 4.10 1 0 -15 -0.30 1.20 1 0 -15 0.00 1.00 0 0 -15 72.89 3.70 0 0 -15 70.49 3.80 -1 0 -15 0.50 1.10 -2 0 -15 21.70 2.30 -3 0 -15 33.00 2.60 3 0 15 33.50 3.30 -4 0 -15 284.37 10.30 4 0 15 278.07 10.70 -5 0 -15 3.90 1.40 5 0 15 5.40 1.80 -6 0 -15 -0.20 1.20 6 0 15 1.60 1.50 -7 0 -15 3.50 1.40 7 0 15 1.00 1.30 7 0 15 3.00 1.50 8 0 15 6.90 1.50 8 0 15 7.70 1.60 9 0 15 3.70 1.30 9 0 15 3.10 1.30 10 0 15 3.00 1.00 10 0 15 2.70 1.00 7 -1 -15 3.70 1.00 7 -1 -15 2.90 0.90 6 -1 -15 5.30 1.10 6 -1 -15 1.20 1.20 5 -1 -15 1.40 1.30 5 -1 -15 1.70 1.10 4 -1 -15 33.80 2.40 4 -1 -15 34.80 2.80 3 -1 -15 0.30 1.10 3 -1 -15 -0.10 1.30 2 -1 -15 11.90 1.90 2 -1 -15 12.60 1.90 2 -1 -15 12.10 2.20 1 -1 -15 5.50 1.30 1 -1 -15 5.70 1.50 0 -1 -15 6.90 1.50 0 -1 -15 5.40 1.30 -1 -1 -15 191.68 7.50 -2 -1 -15 6.50 1.40 2 1 15 5.20 1.80 -3 -1 -15 67.69 3.50 3 1 15 67.39 4.00 -4 -1 -15 21.90 2.20 4 1 15 23.50 2.70 -5 -1 -15 134.59 5.50 5 1 15 119.09 5.80 -6 -1 -15 0.60 1.20 6 1 15 1.30 1.50 -7 -1 -15 0.00 1.10 7 1 15 -1.30 1.30 7 1 15 0.70 1.40 -8 -1 -15 30.30 2.30 8 1 15 29.70 2.60 8 1 15 27.60 2.50 9 1 15 7.40 1.40 9 1 15 8.30 1.40 10 1 15 -0.30 0.90 10 1 15 2.40 1.00 7 -2 -15 29.50 1.80 7 -2 -15 29.20 2.00 6 -2 -15 4.50 1.30 6 -2 -15 2.70 1.10 5 -2 -15 14.40 1.80 5 -2 -15 17.80 2.10 4 -2 -15 26.30 2.20 4 -2 -15 25.90 2.50 3 -2 -15 0.20 1.30 3 -2 -15 2.00 1.10 2 -2 -15 3.10 1.40 2 -2 -15 0.10 1.10 1 -2 -15 24.30 2.40 1 -2 -15 24.00 2.20 0 -2 -15 0.60 1.10 -1 -2 -15 3.20 1.30 1 2 15 3.70 1.60 -2 -2 -15 93.39 4.40 2 2 15 97.49 4.90 -3 -2 -15 59.89 3.30 3 2 15 54.19 3.60 -4 -2 -15 68.29 3.60 4 2 15 67.19 3.90 -5 -2 -15 17.00 2.20 5 2 15 16.90 2.50 -6 -2 -15 15.10 2.10 6 2 15 15.00 2.40 -7 -2 -15 46.00 2.90 7 2 15 48.50 3.20 7 2 15 43.60 3.20 -8 -2 -15 -0.60 1.10 8 2 15 1.10 1.30 8 2 15 0.40 1.20 9 2 15 1.90 1.20 9 2 15 0.30 1.10 10 2 15 8.20 1.40 10 2 15 7.80 1.20 7 -3 -15 5.90 1.20 7 -3 -15 6.50 1.10 6 -3 -15 9.20 1.50 6 -3 -15 10.00 1.60 5 -3 -15 34.50 2.70 5 -3 -15 35.10 2.40 4 -3 -15 17.00 2.20 4 -3 -15 16.70 1.90 3 -3 -15 4.60 1.30 3 -3 -15 4.20 1.50 2 -3 -15 16.30 2.10 2 -3 -15 17.00 2.30 1 -3 -15 50.59 3.10 -1 3 15 62.09 3.80 0 -3 -15 14.80 2.00 0 3 15 20.90 2.70 -1 -3 -15 125.59 5.40 1 3 15 132.19 6.00 -2 -3 -15 116.49 5.10 2 3 15 124.59 5.70 -3 -3 -15 44.30 2.90 3 3 15 50.89 3.50 -4 -3 -15 44.60 2.90 4 3 15 45.70 3.30 -5 -3 -15 15.00 2.10 5 3 15 14.20 2.30 -6 -3 -15 -0.20 1.10 6 3 15 0.90 1.40 -7 -3 -15 2.80 1.30 7 3 15 2.30 1.40 7 3 15 5.20 1.60 -8 -3 -15 16.70 1.90 8 3 15 12.30 2.00 8 3 15 15.70 2.20 -9 -3 -15 3.40 1.00 9 3 15 2.20 1.20 9 3 15 2.00 1.20 10 3 15 1.70 1.00 10 3 15 1.10 1.00 7 -4 -15 7.00 1.20 7 -4 -15 8.90 1.20 6 -4 -15 1.60 1.20 6 -4 -15 0.10 0.90 5 -4 -15 8.10 1.30 5 -4 -15 10.30 1.70 4 -4 -15 -1.20 1.30 4 -4 -15 2.60 1.10 3 -4 -15 1.70 1.20 3 -4 -15 1.00 1.30 -3 4 15 0.70 1.80 2 -4 -15 43.40 2.80 -2 4 15 45.00 3.60 -1 4 15 4.30 1.80 0 -4 -15 8.70 1.50 0 4 15 7.10 1.90 -1 -4 -15 7.80 1.40 1 4 15 9.10 2.00 -2 -4 -15 135.29 5.50 2 4 15 124.99 6.00 -3 -4 -15 49.70 3.10 3 4 15 56.99 3.70 4 4 15 0.00 1.40 5 4 15 27.20 2.80 6 4 15 2.20 1.50 7 4 15 11.80 1.90 7 4 15 12.70 2.00 -8 -4 -15 34.10 2.30 8 4 15 33.10 2.60 8 4 15 29.50 2.60 -9 -4 -15 4.60 1.10 9 4 15 4.40 1.30 9 4 15 6.20 1.40 10 4 15 5.30 1.10 10 4 15 5.50 1.10 7 -5 -15 -1.10 0.80 7 -5 -15 1.20 1.00 6 -5 -15 5.60 1.30 6 -5 -15 6.80 1.20 5 -5 -15 3.70 1.20 5 -5 -15 5.70 1.50 4 -5 -15 48.10 3.20 4 -5 -15 48.80 2.90 -4 5 15 46.10 3.50 3 -5 -15 72.99 3.70 3 -5 -15 73.39 4.00 -3 5 15 69.39 4.40 2 -5 -15 118.49 5.00 -2 5 15 116.59 5.80 1 -5 -15 176.48 6.80 -1 5 15 174.88 7.60 0 5 15 14.30 2.30 -1 -5 -15 2.10 1.20 1 5 15 1.50 1.60 -2 -5 -15 -0.40 1.10 2 5 15 -0.80 1.60 3 5 15 18.00 2.60 4 5 15 38.10 3.10 5 5 15 18.70 2.50 5 5 15 27.40 2.90 6 5 15 4.00 1.60 6 5 15 7.40 1.70 7 5 15 1.00 1.50 7 5 15 -1.00 1.20 7 5 15 -1.20 1.40 8 5 15 -0.20 1.20 8 5 15 0.40 1.20 -9 -5 -15 2.90 1.00 9 5 15 2.50 1.20 9 5 15 2.10 1.20 10 5 15 1.40 0.90 10 5 15 -0.30 0.90 7 -6 -15 0.20 0.90 7 -6 -15 -1.10 0.70 6 -6 -15 5.30 1.40 6 -6 -15 4.40 1.10 -6 6 15 6.10 1.80 5 -6 -15 1.50 1.10 5 -6 -15 3.90 1.40 -5 6 15 1.70 1.50 4 -6 -15 2.40 1.40 4 -6 -15 0.80 1.20 -4 6 15 5.00 1.80 3 -6 -15 0.00 1.00 -3 6 15 1.90 1.80 2 -6 -15 78.29 3.90 -2 6 15 85.39 4.80 1 -6 -15 4.90 1.40 -1 6 15 5.30 2.00 0 6 15 270.27 10.50 -1 -6 -15 182.18 7.10 1 6 15 188.68 7.80 -2 -6 -15 2.70 1.20 2 6 15 2.40 1.70 3 6 15 2.80 1.60 4 6 15 -1.90 1.40 4 6 15 -0.40 1.20 5 6 15 27.10 2.80 5 6 15 25.30 2.70 6 6 15 3.20 1.50 6 6 15 9.00 1.80 7 6 15 7.60 1.70 7 6 15 8.20 1.60 7 6 15 7.30 1.70 8 6 15 -0.60 1.10 8 6 15 1.20 1.30 8 6 15 0.30 1.30 -9 -6 -15 1.70 0.90 9 6 15 1.80 1.10 9 6 15 1.50 1.10 10 6 15 -0.20 0.80 7 -7 -15 10.20 1.30 7 -7 -15 11.00 1.20 6 -7 -15 4.30 1.10 6 -7 -15 7.00 1.30 -6 7 15 6.20 1.50 5 -7 -15 28.20 2.20 5 -7 -15 30.70 2.40 -5 7 15 31.90 2.90 4 -7 -15 5.00 1.30 -4 7 15 6.30 1.90 3 -7 -15 0.70 1.10 -3 7 15 2.50 1.80 2 -7 -15 12.70 2.00 -2 7 15 15.30 2.70 1 -7 -15 114.39 4.90 -1 7 15 111.99 5.70 0 7 15 73.59 4.40 1 7 15 0.30 1.60 -2 -7 -15 0.30 1.00 2 7 15 -0.60 1.50 3 7 15 33.20 3.10 3 7 15 34.00 3.00 4 7 15 6.70 1.80 4 7 15 10.00 1.90 5 7 15 18.90 2.50 5 7 15 18.90 2.40 6 7 15 0.30 1.30 6 7 15 -0.30 1.30 7 7 15 -0.60 1.20 7 7 15 0.80 1.40 7 7 15 0.10 1.30 8 7 15 0.70 1.30 8 7 15 1.00 1.20 8 7 15 -0.70 1.20 9 7 15 9.00 1.50 9 7 15 9.00 1.50 7 -8 -15 4.10 0.90 6 -8 -15 10.50 1.60 6 -8 -15 17.60 1.50 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10.60 1.80 6 9 15 12.50 2.00 7 9 15 2.20 1.30 7 9 15 3.80 1.40 7 9 15 2.40 1.40 8 9 15 0.00 1.10 8 9 15 4.60 1.60 8 9 15 -0.30 1.10 9 9 15 6.70 1.10 6 -10 -15 1.80 0.90 -6 10 15 0.80 1.20 5 -10 -15 9.80 1.50 -5 10 15 10.10 1.80 4 -10 -15 0.50 1.00 -4 10 15 1.90 1.50 3 -10 -15 16.10 1.90 -3 10 15 17.50 2.70 2 -10 -15 13.60 1.90 -2 10 15 8.30 2.00 1 -10 -15 0.20 1.20 -1 10 15 2.10 1.80 0 -10 -15 -2.20 1.10 0 10 15 -0.50 1.50 -1 -10 -15 -0.10 1.60 1 10 15 0.10 1.50 2 10 15 0.40 1.60 3 10 15 1.30 1.50 3 10 15 0.00 1.40 4 10 15 -0.50 1.40 4 10 15 1.60 1.50 5 10 15 45.40 3.10 5 10 15 49.20 3.20 6 10 15 11.50 2.00 6 10 15 12.10 2.00 6 10 15 15.80 2.10 7 10 15 -0.30 1.20 7 10 15 2.10 1.20 8 10 15 0.10 1.10 8 10 15 -1.10 1.00 6 -11 -15 1.20 0.80 -6 11 15 1.60 1.10 5 -11 -15 8.30 1.30 -5 11 15 8.40 1.60 4 -11 -15 2.50 1.10 -4 11 15 1.30 1.30 3 -11 -15 1.20 1.10 -3 11 15 1.20 1.60 2 -11 -15 1.80 1.20 -2 11 15 0.50 1.60 1 -11 -15 37.90 2.60 -1 11 15 40.50 3.30 0 -11 -15 22.70 2.10 0 11 15 21.40 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1.30 -6 -8 -19 1.50 0.90 6 8 19 2.20 1.10 -7 -8 -19 8.90 1.20 7 8 19 7.20 1.30 3 -9 -19 6.10 1.00 -3 9 19 6.60 1.30 2 -9 -19 2.30 1.00 -2 9 19 1.50 1.20 -1 9 19 0.50 1.30 0 9 19 -0.50 1.20 1 9 19 1.50 1.30 2 9 19 2.00 1.40 -3 -9 -19 11.20 1.60 3 9 19 11.40 1.90 -4 -9 -19 1.10 0.90 4 9 19 1.00 1.20 -5 -9 -19 18.10 1.60 5 9 19 20.40 1.90 -6 -9 -19 9.10 1.20 6 9 19 13.80 1.50 -7 -9 -19 -0.20 0.70 7 9 19 0.40 0.80 3 -10 -19 0.40 0.70 -3 10 19 0.50 1.00 2 -10 -19 0.40 0.80 -2 10 19 0.70 1.10 -1 10 19 1.90 1.20 0 10 19 11.30 1.70 1 10 19 0.10 1.10 2 10 19 -1.00 1.10 3 10 19 -0.10 1.10 -4 -10 -19 -0.90 0.80 4 10 19 -1.10 1.00 -5 -10 -19 0.90 0.80 5 10 19 -2.00 0.90 -6 -10 -19 1.70 0.80 6 10 19 1.30 0.90 2 -11 -19 0.00 0.80 -2 11 19 0.00 1.00 -1 11 19 11.30 1.70 0 11 19 2.90 1.20 1 11 19 0.70 1.10 2 11 19 3.20 1.20 3 11 19 0.00 1.10 4 11 19 1.80 1.00 -5 -11 -19 2.00 0.80 5 11 19 2.50 1.00 -2 12 19 3.80 1.00 -1 12 19 -0.80 0.90 0 12 19 12.80 1.50 1 12 19 1.50 1.10 2 12 19 0.30 1.00 3 12 19 -0.50 0.90 4 12 19 0.50 0.90 0 13 19 5.00 1.00 1 13 19 3.40 1.00 2 13 19 4.10 1.00 3 13 19 1.40 0.80 0 3 -20 4.90 0.90 -1 3 -20 7.00 1.10 -2 3 -20 0.30 0.80 -3 3 -20 0.40 0.80 -4 3 -20 47.20 2.20 1 2 -20 4.80 0.90 0 2 -20 2.00 0.90 0 -2 20 4.70 1.70 -1 2 -20 1.40 0.90 -2 2 -20 1.10 0.90 -3 2 -20 37.80 2.10 -4 2 -20 0.00 0.80 -5 2 -20 12.20 1.20 1 1 -20 17.90 1.40 -1 -1 20 15.50 1.70 0 1 -20 -0.40 0.80 -1 1 -20 2.40 1.00 -2 1 -20 -1.30 0.80 -3 1 -20 -0.70 0.90 -4 1 -20 2.70 1.00 -5 1 -20 0.90 0.80 -2 0 20 11.60 2.10 1 0 -20 5.40 1.00 0 0 -20 1.40 0.90 -1 0 -20 7.40 1.20 -2 0 -20 15.40 1.70 -3 0 -20 0.60 0.90 -4 0 -20 41.00 2.30 -5 0 -20 5.50 1.10 -6 0 -20 -0.30 0.70 1 -1 -20 9.50 1.30 0 -1 -20 0.60 0.90 -1 -1 -20 4.50 1.10 -2 -1 -20 7.70 1.30 -3 -1 -20 2.20 1.00 -4 -1 -20 0.10 0.90 -5 -1 -20 1.30 0.90 -6 -1 -20 -0.80 0.80 1 -2 -20 2.30 1.10 0 -2 -20 5.10 1.10 -1 -2 -20 0.80 0.90 -2 -2 -20 0.50 1.00 -3 -2 -20 3.50 1.10 -4 -2 -20 4.20 1.10 4 2 20 3.60 1.30 -5 -2 -20 8.10 1.30 5 2 20 12.00 1.70 -6 -2 -20 5.10 1.00 6 2 20 5.50 1.10 0 -3 -20 8.50 1.40 -1 -3 -20 21.40 1.80 -2 -3 -20 2.80 1.10 -3 -3 -20 0.30 1.00 3 3 20 1.20 1.20 -4 -3 -20 11.60 1.70 4 3 20 10.80 1.80 -5 -3 -20 2.40 1.10 5 3 20 2.80 1.20 -6 -3 -20 -0.30 0.90 6 3 20 0.10 1.00 -7 -3 -20 7.30 1.10 7 3 20 8.30 1.20 0 -4 -20 16.70 1.80 -1 -4 -20 1.40 1.00 1 4 20 2.90 1.30 -2 -4 -20 18.60 1.80 2 4 20 15.10 2.00 -3 -4 -20 37.80 2.50 3 4 20 39.70 2.60 -4 -4 -20 0.50 1.00 4 4 20 -0.60 1.20 -5 -4 -20 6.40 1.20 5 4 20 8.40 1.50 -6 -4 -20 11.00 1.40 6 4 20 11.70 1.50 -7 -4 -20 -0.30 0.80 7 4 20 -1.20 0.80 0 5 20 4.70 1.40 -1 -5 -20 5.50 1.10 1 5 20 7.30 1.50 -2 -5 -20 17.80 1.70 2 5 20 18.50 2.10 -3 -5 -20 4.00 1.20 3 5 20 1.80 1.20 -4 -5 -20 8.20 1.30 4 5 20 4.30 1.40 -5 -5 -20 1.00 1.00 5 5 20 1.00 1.20 -6 -5 -20 2.50 1.00 6 5 20 0.30 1.00 -7 -5 -20 1.30 0.80 7 5 20 3.00 0.90 -1 6 20 0.30 1.20 0 6 20 2.20 1.30 1 6 20 4.60 1.40 -2 -6 -20 -0.10 0.90 2 6 20 0.20 1.20 -3 -6 -20 -1.00 1.00 3 6 20 0.80 1.20 -4 -6 -20 18.10 1.70 4 6 20 16.20 1.90 -5 -6 -20 3.90 1.10 5 6 20 2.40 1.20 -6 -6 -20 2.00 1.00 6 6 20 2.20 1.10 7 6 20 0.50 0.70 -2 7 20 1.00 1.10 -1 7 20 4.60 1.30 0 7 20 0.40 1.20 1 7 20 5.60 1.50 -2 -7 -20 14.70 1.60 2 7 20 14.90 1.90 -3 -7 -20 6.30 1.20 3 7 20 8.50 1.50 -4 -7 -20 12.30 1.60 4 7 20 9.80 1.70 -5 -7 -20 4.70 1.10 5 7 20 4.00 1.20 -6 -7 -20 -0.50 0.80 6 7 20 0.50 0.90 -2 8 20 0.40 1.10 -1 8 20 0.50 1.20 0 8 20 18.80 2.00 1 8 20 4.30 1.40 2 8 20 8.00 1.50 -3 -8 -20 3.30 1.00 3 8 20 5.60 1.40 -4 -8 -20 30.20 2.00 4 8 20 26.10 2.20 -5 -8 -20 29.30 1.90 5 8 20 27.90 2.10 -6 -8 -20 2.10 0.80 6 8 20 2.20 1.00 -2 9 20 5.60 1.20 -1 9 20 0.90 1.10 0 9 20 2.40 1.20 1 9 20 -0.30 1.10 2 9 20 18.80 2.00 3 9 20 0.50 1.10 -4 -9 -20 12.40 1.40 4 9 20 13.00 1.60 -5 -9 -20 3.10 0.90 5 9 20 3.70 1.10 -6 -9 -20 0.80 0.70 6 9 20 0.90 0.90 -2 10 20 1.10 1.00 -1 10 20 -0.90 0.90 0 10 20 3.40 1.20 1 10 20 3.60 1.30 2 10 20 -0.60 1.00 3 10 20 9.90 1.50 -4 -10 -20 0.30 0.90 4 10 20 0.00 0.90 -5 -10 -20 1.80 0.80 5 10 20 0.00 0.80 -1 11 20 -0.60 0.90 0 11 20 -0.10 0.90 1 11 20 -0.30 0.90 2 11 20 -1.00 0.80 3 11 20 -0.90 0.90 4 11 20 0.20 0.90 0 12 20 1.40 0.90 1 12 20 -0.80 0.70 2 12 20 -0.10 0.80 3 12 20 4.20 0.90 -1 1 -21 3.20 0.80 -2 1 -21 1.50 0.80 -3 1 -21 11.30 1.30 0 0 -21 4.40 0.90 -1 0 -21 4.00 0.90 -2 0 -21 10.60 1.30 -3 0 -21 -0.40 0.80 -4 0 -21 8.10 1.30 0 -1 -21 0.90 0.80 -1 -1 -21 9.10 1.30 -2 -1 -21 1.40 0.90 -3 -1 -21 8.50 1.30 -4 -1 -21 18.10 1.50 -5 -1 -21 0.20 0.80 0 -2 -21 13.80 1.30 -1 -2 -21 -0.30 0.80 -2 -2 -21 3.60 1.00 -3 -2 -21 19.20 1.60 -4 -2 -21 4.60 1.00 -5 -2 -21 1.30 0.90 0 -3 -21 0.60 0.80 -1 -3 -21 9.20 1.30 -2 -3 -21 1.80 0.90 -3 -3 -21 10.00 1.40 -4 -3 -21 11.60 1.40 4 3 21 10.20 1.50 -5 -3 -21 25.90 1.70 5 3 21 26.80 1.80 -1 -4 -21 18.80 1.60 -2 -4 -21 8.60 1.20 2 4 21 8.50 2.10 -3 -4 -21 7.10 1.10 3 4 21 6.30 1.30 -4 -4 -21 21.10 1.70 4 4 21 21.90 1.80 -5 -4 -21 9.70 1.30 5 4 21 8.10 1.40 -1 -5 -21 5.80 1.00 1 5 21 6.20 1.20 -2 -5 -21 -0.70 0.80 2 5 21 -0.60 1.00 -3 -5 -21 1.20 0.90 3 5 21 1.80 1.20 -4 -5 -21 12.90 1.50 4 5 21 17.80 1.70 -5 -5 -21 14.90 1.50 5 5 21 13.10 1.50 0 6 21 12.70 1.60 1 6 21 2.20 1.10 -2 -6 -21 20.60 1.60 2 6 21 22.80 1.90 -3 -6 -21 38.00 2.10 3 6 21 37.30 2.40 -4 -6 -21 -0.10 0.80 4 6 21 1.60 1.10 -5 -6 -21 12.60 1.40 5 6 21 12.70 1.50 -1 7 21 27.70 1.80 0 7 21 28.00 2.00 1 7 21 19.10 1.80 2 7 21 2.60 1.10 -3 -7 -21 -0.80 0.80 3 7 21 -1.80 0.90 -4 -7 -21 15.30 1.40 4 7 21 18.50 1.70 -5 -7 -21 2.00 0.80 5 7 21 2.60 1.00 -1 8 21 3.80 1.00 0 8 21 2.20 1.10 1 8 21 4.50 1.10 2 8 21 0.30 1.00 -3 -8 -21 -0.20 0.70 3 8 21 0.50 1.00 -4 -8 -21 4.00 0.90 4 8 21 4.10 1.10 -5 -8 -21 2.30 0.80 5 8 21 3.30 0.90 -1 9 21 2.60 1.00 0 9 21 7.90 1.40 1 9 21 0.50 1.00 2 9 21 2.80 1.10 3 9 21 3.80 1.10 4 9 21 1.00 0.90 0 10 21 -0.30 0.80 1 10 21 4.20 1.00 2 10 21 4.50 1.00 3 10 21 -0.20 0.80 -2 -2 -22 0.10 0.70 -2 -3 -22 0.00 0.70 -3 -3 -22 11.70 1.20 -2 -4 -22 5.60 0.90 -3 -4 -22 0.80 0.70 -2 -5 -22 -1.20 0.70 -3 -5 -22 0.50 0.70 2 6 22 1.80 0.90 -3 -6 -22 6.40 1.10 3 6 22 7.40 1.30 2 7 22 14.80 1.40 3 7 22 16.20 1.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' ; _shelx_hkl_checksum 30208 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Warren Piers' _publ_contact_author_address ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Morgan, Matthew' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; 'Piers, Warren' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_newMM_a _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 K N2 O6, C25 H19 B N' _chemical_formula_sum 'C57.33 H73.33 B1.33 K1.33 N4 O8' _chemical_formula_weight 1013.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.31(2) _cell_length_b 17.619(14) _cell_length_c 24.71(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8408(14) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 70.57 _exptl_crystal_description 'block' _exptl_crystal_colour 'Yellow' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.201 _exptl_crystal_F_000 3248 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_absorpt_coefficient_mu 1.493 _shelx_estimated_absorpt_T_min 0.755 _shelx_estimated_absorpt_T_max 0.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.780 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57352 _diffrn_reflns_av_unetI/netI 0.0399 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.578 _diffrn_reflns_theta_max 69.730 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 7897 _reflns_number_gt 6036 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.8.3 (Spasyuk, 2009)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+0.0231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7897 _refine_ls_number_parameters 487 _refine_ls_number_restraints 555 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.50830(2) 0.19310(3) 0.34629(2) 0.03215(15) Uani 1 1 d . U . . . O4 O 0.36828(9) 0.15121(10) 0.32752(7) 0.0388(4) Uani 1 1 d . U . . . O2 O 0.51763(10) 0.14289(11) 0.45557(7) 0.0416(4) Uani 1 1 d . U . . . O1 O 0.60996(9) 0.08216(11) 0.37870(7) 0.0439(4) Uani 1 1 d . U . . . O6 O 0.48810(10) 0.35107(10) 0.36649(8) 0.0426(4) Uani 1 1 d . U . . . O3 O 0.46967(10) 0.12115(10) 0.24824(7) 0.0434(4) Uani 1 1 d . U . . . O5 O 0.60346(10) 0.30169(11) 0.30452(8) 0.0459(4) Uani 1 1 d . U . . . N3 N 0.39855(11) 0.24090(13) 0.42595(8) 0.0376(4) Uani 1 1 d . U . . . N1 N 0.51460(11) 0.64283(12) 0.42365(8) 0.0356(4) Uani 1 1 d . U . . . N2 N 0.61792(12) 0.14345(14) 0.26605(9) 0.0434(5) Uani 1 1 d . U . . . C3 C 0.56991(11) 0.67973(13) 0.39560(8) 0.0287(4) Uani 1 1 d . U . . . C1 C 0.47376(12) 0.76063(14) 0.39266(9) 0.0331(5) Uani 1 1 d . U . . . C14 C 0.43123(13) 0.82908(14) 0.38522(9) 0.0367(5) Uani 1 1 d . U . . . C8 C 0.38837(13) 0.66686(14) 0.45511(10) 0.0370(5) Uani 1 1 d . U . . . C20 C 0.59343(13) 0.79868(14) 0.33933(10) 0.0357(5) Uani 1 1 d . U . . . C7 C 0.52712(13) 0.57320(13) 0.44941(9) 0.0351(5) Uani 1 1 d . U . . . H7 H 0.4905 0.5490 0.4684 0.042 Uiso 1 1 calc R U . . . C6 C 0.59058(13) 0.53958(14) 0.44776(10) 0.0386(5) Uani 1 1 d . U . . . H6 H 0.5982 0.4931 0.4664 0.046 Uiso 1 1 calc R U . . . C15 C 0.45997(15) 0.90200(15) 0.37662(10) 0.0405(5) Uani 1 1 d . U . . . H15 H 0.5088 0.9072 0.3743 0.049 Uiso 1 1 calc R U . . . C4 C 0.63477(13) 0.64235(15) 0.39300(10) 0.0384(5) Uani 1 1 d . U . . . H4 H 0.6715 0.6653 0.3733 0.046 Uiso 1 1 calc R U . . . C21 C 0.57327(14) 0.81998(15) 0.28692(11) 0.0405(5) Uani 1 1 d . U . . . H21 H 0.5281 0.8070 0.2748 0.049 Uiso 1 1 calc R U . . . C13 C 0.35105(13) 0.60059(15) 0.44246(11) 0.0410(6) Uani 1 1 d . U . . . H13 H 0.3644 0.5713 0.4119 0.049 Uiso 1 1 calc R U . . . C2 C 0.54683(13) 0.75067(15) 0.37568(9) 0.0364(5) Uani 1 1 d . U . . . C5 C 0.64605(14) 0.57419(16) 0.41799(11) 0.0418(6) Uani 1 1 d . U . . . H5 H 0.6900 0.5501 0.4157 0.050 Uiso 1 1 calc R U . . . C35 C 0.35092(14) 0.13707(16) 0.27227(11) 0.0431(6) Uani 1 1 d . U . . . H35A H 0.3494 0.1856 0.2521 0.052 Uiso 1 1 calc R U . . . H35B H 0.3045 0.1133 0.2702 0.052 Uiso 1 1 calc R U . . . C34 C 0.40366(15) 0.08548(16) 0.24713(11) 0.0448(6) Uani 1 1 d . U . . . H34A H 0.4056 0.0370 0.2674 0.054 Uiso 1 1 calc R U . . . H34B H 0.3905 0.0741 0.2093 0.054 Uiso 1 1 calc R U . . . C37 C 0.33345(13) 0.20082(17) 0.41395(11) 0.0439(6) Uani 1 1 d . U . . . H37A H 0.2950 0.2272 0.4327 0.053 Uiso 1 1 calc R U . . . H37B H 0.3364 0.1488 0.4289 0.053 Uiso 1 1 calc R U . . . C30 C 0.45439(15) 0.14357(17) 0.48591(11) 0.0455(6) Uani 1 1 d . U . . . H30A H 0.4641 0.1317 0.5244 0.055 Uiso 1 1 calc R U . . . H30B H 0.4224 0.1045 0.4716 0.055 Uiso 1 1 calc R U . . . C19 C 0.35768(15) 0.82599(16) 0.38753(12) 0.0456(6) Uani 1 1 d . U . . . H19 H 0.3356 0.7783 0.3925 0.055 Uiso 1 1 calc R U . . . C36 C 0.31637(13) 0.19570(17) 0.35394(11) 0.0445(6) Uani 1 1 d . U . . . H36A H 0.2704 0.1719 0.3490 0.053 Uiso 1 1 calc R U . . . H36B H 0.3149 0.2472 0.3380 0.053 Uiso 1 1 calc R U . . . C31 C 0.42145(15) 0.22104(18) 0.48148(10) 0.0461(6) Uani 1 1 d . U . . . H31A H 0.3810 0.2231 0.5060 0.055 Uiso 1 1 calc R U . . . H31B H 0.4551 0.2596 0.4939 0.055 Uiso 1 1 calc R U . . . C40 C 0.58193(15) 0.37882(15) 0.30591(12) 0.0460(6) Uani 1 1 d . U . . . H40A H 0.5475 0.3884 0.2770 0.055 Uiso 1 1 calc R U . . . H40B H 0.6221 0.4126 0.2998 0.055 Uiso 1 1 calc R U . . . B1 B 0.45440(13) 0.69088(15) 0.42283(10) 0.0306(5) Uani 1 1 d . U . . . C29 C 0.55707(16) 0.07622(16) 0.46588(11) 0.0486(6) Uani 1 1 d . U . . . H29A H 0.5307 0.0309 0.4542 0.058 Uiso 1 1 calc R U . . . H29B H 0.5664 0.0717 0.5052 0.058 Uiso 1 1 calc R U . . . C25 C 0.66041(14) 0.82015(17) 0.35547(12) 0.0449(6) Uani 1 1 d . U . . . H25 H 0.6756 0.8078 0.3910 0.054 Uiso 1 1 calc R U . . . C28 C 0.62424(15) 0.08056(17) 0.43538(12) 0.0497(7) Uani 1 1 d . U . . . H28A H 0.6498 0.1269 0.4460 0.060 Uiso 1 1 calc R U . . . H28B H 0.6533 0.0360 0.4442 0.060 Uiso 1 1 calc R U . . . C12 C 0.29456(14) 0.57664(17) 0.47385(12) 0.0480(6) Uani 1 1 d . U . . . H12 H 0.2701 0.5318 0.4643 0.058 Uiso 1 1 calc R U . . . C16 C 0.41861(17) 0.96641(16) 0.37144(11) 0.0484(6) Uani 1 1 d . U . . . H16 H 0.4399 1.0144 0.3660 0.058 Uiso 1 1 calc R U . . . C41 C 0.55042(15) 0.39453(15) 0.36047(12) 0.0468(6) Uani 1 1 d . U . . . H41A H 0.5837 0.3807 0.3894 0.056 Uiso 1 1 calc R U . . . H41B H 0.5398 0.4493 0.3638 0.056 Uiso 1 1 calc R U . . . C26 C 0.65228(16) 0.07513(17) 0.28771(12) 0.0506(7) Uani 1 1 d . U . . . H26A H 0.6948 0.0656 0.2664 0.061 Uiso 1 1 calc R U . . . H26B H 0.6212 0.0311 0.2824 0.061 Uiso 1 1 calc R U . . . C9 C 0.36577(15) 0.70787(18) 0.50041(12) 0.0475(6) Uani 1 1 d . U . . . H9 H 0.3894 0.7532 0.5101 0.057 Uiso 1 1 calc R U . . . C22 C 0.61697(16) 0.85942(16) 0.25215(11) 0.0481(6) Uani 1 1 d . U . . . H22 H 0.6016 0.8732 0.2170 0.058 Uiso 1 1 calc R U . . . C11 C 0.27441(15) 0.61812(19) 0.51871(12) 0.0523(7) Uani 1 1 d . U . . . H11 H 0.2367 0.6014 0.5404 0.063 Uiso 1 1 calc R U . . . C27 C 0.67170(15) 0.07951(19) 0.34707(13) 0.0509(7) Uani 1 1 d . U . . . H27A H 0.6995 0.0346 0.3573 0.061 Uiso 1 1 calc R U . . . H27B H 0.6998 0.1255 0.3538 0.061 Uiso 1 1 calc R U . . . C39 C 0.63478(15) 0.28280(17) 0.25357(12) 0.0501(7) Uani 1 1 d . U . . . H39A H 0.6700 0.3213 0.2439 0.060 Uiso 1 1 calc R U . . . H39B H 0.5992 0.2818 0.2247 0.060 Uiso 1 1 calc R U . . . C23 C 0.68345(16) 0.87861(18) 0.26914(13) 0.0545(7) Uani 1 1 d . U . . . H23 H 0.7138 0.9050 0.2455 0.065 Uiso 1 1 calc R U . . . C43 C 0.38862(15) 0.32386(17) 0.42153(12) 0.0488(6) Uani 1 1 d . U . . . H43A H 0.3630 0.3418 0.4538 0.059 Uiso 1 1 calc R U . . . H43B H 0.3597 0.3346 0.3893 0.059 Uiso 1 1 calc R U . . . C24 C 0.70518(16) 0.85895(18) 0.32098(14) 0.0545(7) Uani 1 1 d . U . . . H24 H 0.7504 0.8720 0.3328 0.065 Uiso 1 1 calc R U . . . C32 C 0.58503(17) 0.12541(19) 0.21356(11) 0.0540(7) Uani 1 1 d . U . . . H32A H 0.6186 0.0971 0.1911 0.065 Uiso 1 1 calc R U . . . H32B H 0.5744 0.1735 0.1946 0.065 Uiso 1 1 calc R U . . . C33 C 0.51940(17) 0.07942(18) 0.21782(12) 0.0521(7) Uani 1 1 d . U . . . H33A H 0.5011 0.0686 0.1812 0.063 Uiso 1 1 calc R U . . . H33B H 0.5292 0.0304 0.2359 0.063 Uiso 1 1 calc R U . . . C42 C 0.45538(16) 0.36812(16) 0.41696(12) 0.0499(7) Uani 1 1 d . U . . . H42A H 0.4456 0.4232 0.4191 0.060 Uiso 1 1 calc R U . . . H42B H 0.4866 0.3545 0.4472 0.060 Uiso 1 1 calc R U . . . C10 C 0.30962(16) 0.6843(2) 0.53181(13) 0.0563(7) Uani 1 1 d . U . . . H10 H 0.2955 0.7135 0.5622 0.068 Uiso 1 1 calc R U . . . C38 C 0.66825(15) 0.20565(18) 0.25882(13) 0.0540(7) Uani 1 1 d . U . . . H38A H 0.6961 0.1956 0.2260 0.065 Uiso 1 1 calc R U . . . H38B H 0.7002 0.2063 0.2902 0.065 Uiso 1 1 calc R U . . . C17 C 0.34712(18) 0.96178(18) 0.37412(14) 0.0593(8) Uani 1 1 d . U . . . H17 H 0.3192 1.0058 0.3702 0.071 Uiso 1 1 calc R U . . . C18 C 0.31738(17) 0.8911(2) 0.38263(14) 0.0593(8) Uani 1 1 d . U . . . H18 H 0.2684 0.8871 0.3852 0.071 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0324(3) 0.0334(3) 0.0306(3) 0.00017(17) 0.00048(17) -0.00098(18) O4 0.0342(9) 0.0464(10) 0.0357(9) -0.0002(7) -0.0071(6) -0.0012(7) O2 0.0451(10) 0.0458(10) 0.0341(9) 0.0061(7) -0.0013(7) -0.0004(8) O1 0.0385(10) 0.0518(11) 0.0414(10) 0.0070(8) -0.0035(7) 0.0050(8) O6 0.0519(11) 0.0386(9) 0.0372(10) -0.0061(7) -0.0026(7) -0.0042(8) O3 0.0512(11) 0.0413(10) 0.0377(9) -0.0090(7) -0.0027(7) 0.0026(8) O5 0.0458(11) 0.0406(10) 0.0512(11) 0.0095(8) 0.0071(8) -0.0008(8) N3 0.0365(10) 0.0448(11) 0.0314(10) -0.0029(8) 0.0025(8) 0.0000(9) N1 0.0412(11) 0.0346(10) 0.0310(10) -0.0032(8) 0.0010(8) -0.0024(8) N2 0.0407(12) 0.0503(13) 0.0391(11) 0.0041(9) 0.0088(8) 0.0102(9) C3 0.0305(11) 0.0333(11) 0.0223(10) -0.0017(8) 0.0010(7) -0.0015(8) C1 0.0321(11) 0.0388(12) 0.0284(11) 0.0010(9) -0.0025(8) -0.0013(9) C14 0.0446(13) 0.0386(12) 0.0270(11) -0.0016(9) -0.0051(9) 0.0036(10) C8 0.0350(12) 0.0401(12) 0.0358(12) 0.0053(9) -0.0022(9) 0.0052(10) C20 0.0351(12) 0.0396(13) 0.0325(12) -0.0020(9) 0.0013(9) 0.0018(9) C7 0.0433(13) 0.0328(12) 0.0291(12) -0.0011(8) 0.0011(9) -0.0031(9) C6 0.0449(13) 0.0352(12) 0.0356(13) 0.0003(9) -0.0013(9) 0.0039(10) C15 0.0489(14) 0.0411(13) 0.0313(12) 0.0019(9) -0.0032(9) 0.0011(11) C4 0.0374(13) 0.0419(13) 0.0359(13) 0.0004(10) 0.0028(9) 0.0006(10) C21 0.0438(14) 0.0417(13) 0.0362(13) 0.0006(10) -0.0021(10) 0.0068(11) C13 0.0416(13) 0.0399(13) 0.0414(14) 0.0042(10) -0.0030(10) 0.0024(10) C2 0.0387(12) 0.0416(12) 0.0290(11) -0.0017(9) -0.0013(8) -0.0002(10) C5 0.0376(13) 0.0473(14) 0.0405(14) -0.0014(10) 0.0014(10) 0.0084(10) C35 0.0418(14) 0.0476(15) 0.0398(13) -0.0005(10) -0.0133(10) -0.0069(11) C34 0.0560(15) 0.0411(13) 0.0373(13) -0.0057(10) -0.0137(11) -0.0034(11) C37 0.0332(13) 0.0593(17) 0.0391(14) 0.0020(11) 0.0051(10) -0.0006(11) C30 0.0494(15) 0.0571(16) 0.0299(12) 0.0054(11) -0.0006(10) -0.0052(12) C19 0.0445(14) 0.0443(14) 0.0479(16) 0.0077(11) -0.0011(11) 0.0044(11) C36 0.0301(12) 0.0588(17) 0.0447(15) -0.0001(11) -0.0048(10) 0.0000(11) C31 0.0467(15) 0.0608(17) 0.0308(13) -0.0060(11) 0.0019(10) -0.0010(12) C40 0.0502(16) 0.0356(13) 0.0524(16) 0.0104(11) -0.0051(11) -0.0074(11) B1 0.0315(12) 0.0329(13) 0.0273(12) -0.0021(9) -0.0005(9) 0.0007(10) C29 0.0623(17) 0.0481(15) 0.0353(14) 0.0093(11) -0.0061(11) 0.0060(12) C25 0.0404(14) 0.0512(15) 0.0433(14) 0.0057(11) -0.0049(10) -0.0019(11) C28 0.0508(16) 0.0527(16) 0.0456(15) 0.0061(12) -0.0132(11) 0.0112(13) C12 0.0391(14) 0.0495(15) 0.0555(16) 0.0127(12) -0.0043(11) -0.0026(11) C16 0.0695(18) 0.0368(13) 0.0390(14) 0.0063(10) 0.0012(11) 0.0058(12) C41 0.0569(16) 0.0353(13) 0.0482(15) -0.0016(11) -0.0109(11) -0.0078(11) C26 0.0492(16) 0.0503(16) 0.0522(16) 0.0021(12) 0.0114(12) 0.0149(12) C9 0.0429(14) 0.0554(16) 0.0443(15) -0.0071(12) 0.0028(11) 0.0010(12) C22 0.0598(17) 0.0470(15) 0.0375(14) 0.0050(11) 0.0042(11) 0.0112(12) C11 0.0369(14) 0.0704(19) 0.0494(15) 0.0178(13) 0.0063(11) 0.0030(13) C27 0.0380(14) 0.0564(17) 0.0584(17) 0.0081(13) -0.0006(11) 0.0101(12) C39 0.0438(15) 0.0542(16) 0.0524(16) 0.0151(12) 0.0150(12) -0.0023(12) C23 0.0562(17) 0.0507(16) 0.0566(17) 0.0128(13) 0.0163(13) 0.0052(13) C43 0.0522(16) 0.0505(15) 0.0436(15) -0.0074(11) 0.0060(11) 0.0118(12) C24 0.0415(15) 0.0555(17) 0.0663(19) 0.0110(14) 0.0046(12) -0.0041(12) C32 0.0632(18) 0.0627(18) 0.0363(14) 0.0000(12) 0.0096(12) 0.0155(14) C33 0.0675(18) 0.0515(16) 0.0373(14) -0.0101(11) -0.0017(12) 0.0134(13) C42 0.0652(18) 0.0407(14) 0.0438(15) -0.0102(11) 0.0002(12) 0.0014(12) C10 0.0469(16) 0.075(2) 0.0469(16) -0.0051(14) 0.0099(12) 0.0065(14) C38 0.0411(15) 0.0613(17) 0.0595(18) 0.0107(13) 0.0186(12) 0.0078(12) C17 0.0681(19) 0.0492(16) 0.0606(19) 0.0132(14) 0.0071(14) 0.0217(14) C18 0.0511(17) 0.0629(18) 0.064(2) 0.0154(14) 0.0089(13) 0.0180(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O3 2.834(3) . ? K1 O4 2.841(3) . ? K1 O2 2.847(3) . ? K1 O5 2.847(3) . ? K1 O6 2.855(3) . ? K1 O1 2.884(3) . ? K1 N3 3.013(3) . ? K1 N2 3.029(3) . ? O4 C35 1.428(3) . ? O4 C36 1.430(3) . ? O2 C29 1.423(3) . ? O2 C30 1.433(3) . ? O1 C27 1.426(4) . ? O1 C28 1.427(4) . ? O6 C42 1.430(4) . ? O6 C41 1.434(4) . ? O3 C34 1.422(4) . ? O3 C33 1.424(3) . ? O5 C40 1.422(4) . ? O5 C39 1.436(4) . ? N3 C37 1.472(4) . ? N3 C43 1.478(4) . ? N3 C31 1.483(4) . ? N1 C7 1.403(3) . ? N1 C3 1.430(3) . ? N1 B1 1.438(4) . ? N2 C26 1.475(4) . ? N2 C38 1.476(4) . ? N2 C32 1.479(4) . ? C3 C2 1.415(4) . ? C3 C4 1.417(4) . ? C1 C14 1.471(4) . ? C1 C2 1.483(4) . ? C1 B1 1.485(4) . ? C14 C15 1.416(4) . ? C14 C19 1.423(4) . ? C8 C9 1.402(4) . ? C8 C13 1.407(4) . ? C8 B1 1.562(4) . ? C20 C21 1.403(4) . ? C20 C25 1.406(4) . ? C20 C2 1.527(4) . ? C7 C6 1.362(4) . ? C7 H7 0.9500 . ? C6 C5 1.436(4) . ? C6 H6 0.9500 . ? C15 C16 1.394(4) . ? C15 H15 0.9500 . ? C4 C5 1.368(4) . ? C4 H4 0.9500 . ? C21 C22 1.390(4) . ? C21 H21 0.9500 . ? C13 C12 1.404(4) . ? C13 H13 0.9500 . ? C5 H5 0.9500 . ? C35 C34 1.500(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C37 C36 1.522(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C30 C31 1.510(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C19 C18 1.392(4) . ? C19 H19 0.9500 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C40 C41 1.505(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C29 C28 1.502(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C25 C24 1.393(4) . ? C25 H25 0.9500 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C12 C11 1.383(5) . ? C12 H12 0.9500 . ? C16 C17 1.385(5) . ? C16 H16 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C26 C27 1.516(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C9 C10 1.397(4) . ? C9 H9 0.9500 . ? C22 C23 1.393(5) . ? C22 H22 0.9500 . ? C11 C10 1.388(5) . ? C11 H11 0.9500 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C39 C38 1.511(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C43 C42 1.511(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C24 H24 0.9500 . ? C32 C33 1.508(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C10 H10 0.9500 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C17 C18 1.387(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 K1 O4 59.58(6) . . ? O3 K1 O2 133.50(7) . . ? O4 K1 O2 97.72(6) . . ? O3 K1 O5 99.25(8) . . ? O4 K1 O5 136.88(7) . . ? O2 K1 O5 120.78(6) . . ? O3 K1 O6 123.34(6) . . ? O4 K1 O6 98.72(6) . . ? O2 K1 O6 98.39(7) . . ? O5 K1 O6 59.75(7) . . ? O3 K1 O1 96.51(7) . . ? O4 K1 O1 121.15(8) . . ? O2 K1 O1 58.87(6) . . ? O5 K1 O1 96.70(9) . . ? O6 K1 O1 134.86(6) . . ? O3 K1 N3 119.88(8) . . ? O4 K1 N3 60.63(8) . . ? O2 K1 N3 60.78(7) . . ? O5 K1 N3 120.21(8) . . ? O6 K1 N3 61.12(6) . . ? O1 K1 N3 119.16(8) . . ? O3 K1 N2 59.70(9) . . ? O4 K1 N2 118.91(8) . . ? O2 K1 N2 119.12(8) . . ? O5 K1 N2 60.37(8) . . ? O6 K1 N2 119.44(6) . . ? O1 K1 N2 60.67(8) . . ? N3 K1 N2 179.41(7) . . ? C35 O4 C36 111.6(2) . . ? C35 O4 K1 115.15(15) . . ? C36 O4 K1 116.77(16) . . ? C29 O2 C30 111.7(2) . . ? C29 O2 K1 117.40(15) . . ? C30 O2 K1 116.08(15) . . ? C27 O1 C28 112.0(2) . . ? C27 O1 K1 116.05(16) . . ? C28 O1 K1 114.66(16) . . ? C42 O6 C41 110.4(2) . . ? C42 O6 K1 114.69(16) . . ? C41 O6 K1 112.81(16) . . ? C34 O3 C33 111.5(2) . . ? C34 O3 K1 116.76(15) . . ? C33 O3 K1 120.29(17) . . ? C40 O5 C39 111.5(2) . . ? C40 O5 K1 116.41(16) . . ? C39 O5 K1 115.72(16) . . ? C37 N3 C43 110.4(2) . . ? C37 N3 C31 109.1(2) . . ? C43 N3 C31 109.9(2) . . ? C37 N3 K1 109.59(16) . . ? C43 N3 K1 108.63(15) . . ? C31 N3 K1 109.17(16) . . ? C7 N1 C3 119.3(2) . . ? C7 N1 B1 131.3(2) . . ? C3 N1 B1 109.2(2) . . ? C26 N2 C38 110.7(2) . . ? C26 N2 C32 109.6(2) . . ? C38 N2 C32 109.7(2) . . ? C26 N2 K1 108.22(16) . . ? C38 N2 K1 108.97(17) . . ? C32 N2 K1 109.62(17) . . ? C2 C3 C4 132.3(2) . . ? C2 C3 N1 109.6(2) . . ? C4 C3 N1 118.1(2) . . ? C14 C1 C2 126.4(2) . . ? C14 C1 B1 126.9(2) . . ? C2 C1 B1 106.5(2) . . ? C15 C14 C19 115.6(2) . . ? C15 C14 C1 123.0(2) . . ? C19 C14 C1 121.4(2) . . ? C9 C8 C13 116.4(3) . . ? C9 C8 B1 121.5(2) . . ? C13 C8 B1 122.0(2) . . ? C21 C20 C25 116.4(2) . . ? C21 C20 C2 121.8(2) . . ? C25 C20 C2 121.6(2) . . ? C6 C7 N1 121.4(2) . . ? C6 C7 H7 119.3 . . ? N1 C7 H7 119.3 . . ? C7 C6 C5 120.2(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C16 C15 C14 121.9(3) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C5 C4 C3 121.9(2) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C22 C21 C20 122.4(3) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C12 C13 C8 121.7(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C3 C2 C1 107.8(2) . . ? C3 C2 C20 120.5(2) . . ? C1 C2 C20 131.4(2) . . ? C4 C5 C6 119.0(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? O4 C35 C34 110.0(2) . . ? O4 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? O4 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? O3 C34 C35 109.5(2) . . ? O3 C34 H34A 109.8 . . ? C35 C34 H34A 109.8 . . ? O3 C34 H34B 109.8 . . ? C35 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? N3 C37 C36 114.2(2) . . ? N3 C37 H37A 108.7 . . ? C36 C37 H37A 108.7 . . ? N3 C37 H37B 108.7 . . ? C36 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? O2 C30 C31 109.2(2) . . ? O2 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? O2 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.3 . . ? C18 C19 C14 121.5(3) . . ? C18 C19 H19 119.2 . . ? C14 C19 H19 119.2 . . ? O4 C36 C37 109.0(2) . . ? O4 C36 H36A 109.9 . . ? C37 C36 H36A 109.9 . . ? O4 C36 H36B 109.9 . . ? C37 C36 H36B 109.9 . . ? H36A C36 H36B 108.3 . . ? N3 C31 C30 114.0(2) . . ? N3 C31 H31A 108.8 . . ? C30 C31 H31A 108.8 . . ? N3 C31 H31B 108.8 . . ? C30 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? O5 C40 C41 108.4(2) . . ? O5 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? O5 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? N1 B1 C1 106.9(2) . . ? N1 B1 C8 119.6(2) . . ? C1 B1 C8 133.3(2) . . ? O2 C29 C28 109.3(2) . . ? O2 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O2 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? C24 C25 C20 122.0(3) . . ? C24 C25 H25 119.0 . . ? C20 C25 H25 119.0 . . ? O1 C28 C29 109.0(2) . . ? O1 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O1 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? O6 C41 C40 109.5(2) . . ? O6 C41 H41A 109.8 . . ? C40 C41 H41A 109.8 . . ? O6 C41 H41B 109.8 . . ? C40 C41 H41B 109.8 . . ? H41A C41 H41B 108.2 . . ? N2 C26 C27 114.9(2) . . ? N2 C26 H26A 108.5 . . ? C27 C26 H26A 108.5 . . ? N2 C26 H26B 108.5 . . ? C27 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C10 C9 C8 122.1(3) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? O1 C27 C26 109.0(2) . . ? O1 C27 H27A 109.9 . . ? C26 C27 H27A 109.9 . . ? O1 C27 H27B 109.9 . . ? C26 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O5 C39 C38 108.3(2) . . ? O5 C39 H39A 110.0 . . ? C38 C39 H39A 110.0 . . ? O5 C39 H39B 110.0 . . ? C38 C39 H39B 110.0 . . ? H39A C39 H39B 108.4 . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? N3 C43 C42 113.9(2) . . ? N3 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? N3 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N2 C32 C33 114.5(2) . . ? N2 C32 H32A 108.6 . . ? C33 C32 H32A 108.6 . . ? N2 C32 H32B 108.6 . . ? C33 C32 H32B 108.6 . . ? H32A C32 H32B 107.6 . . ? O3 C33 C32 109.0(2) . . ? O3 C33 H33A 109.9 . . ? C32 C33 H33A 109.9 . . ? O3 C33 H33B 109.9 . . ? C32 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O6 C42 C43 109.5(2) . . ? O6 C42 H42A 109.8 . . ? C43 C42 H42A 109.8 . . ? O6 C42 H42B 109.8 . . ? C43 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? N2 C38 C39 113.4(2) . . ? N2 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? N2 C38 H38B 108.9 . . ? C39 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? C16 C17 C18 118.2(3) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C17 C18 C19 121.4(3) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 C3 C2 -176.5(2) . . . . ? B1 N1 C3 C2 -0.9(3) . . . . ? C7 N1 C3 C4 2.8(3) . . . . ? B1 N1 C3 C4 178.4(2) . . . . ? C2 C1 C14 C15 -20.9(4) . . . . ? B1 C1 C14 C15 153.1(2) . . . . ? C2 C1 C14 C19 160.6(2) . . . . ? B1 C1 C14 C19 -25.4(4) . . . . ? C3 N1 C7 C6 -0.8(3) . . . . ? B1 N1 C7 C6 -175.3(2) . . . . ? N1 C7 C6 C5 -1.7(4) . . . . ? C19 C14 C15 C16 0.7(4) . . . . ? C1 C14 C15 C16 -177.9(2) . . . . ? C2 C3 C4 C5 176.7(3) . . . . ? N1 C3 C4 C5 -2.4(3) . . . . ? C25 C20 C21 C22 0.7(4) . . . . ? C2 C20 C21 C22 -175.7(2) . . . . ? C9 C8 C13 C12 -0.5(4) . . . . ? B1 C8 C13 C12 175.7(2) . . . . ? C4 C3 C2 C1 -177.9(2) . . . . ? N1 C3 C2 C1 1.2(3) . . . . ? C4 C3 C2 C20 6.9(4) . . . . ? N1 C3 C2 C20 -174.0(2) . . . . ? C14 C1 C2 C3 173.9(2) . . . . ? B1 C1 C2 C3 -1.1(3) . . . . ? C14 C1 C2 C20 -11.6(4) . . . . ? B1 C1 C2 C20 173.4(2) . . . . ? C21 C20 C2 C3 121.0(3) . . . . ? C25 C20 C2 C3 -55.3(3) . . . . ? C21 C20 C2 C1 -53.0(4) . . . . ? C25 C20 C2 C1 130.8(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C7 C6 C5 C4 2.2(4) . . . . ? C36 O4 C35 C34 -175.7(2) . . . . ? K1 O4 C35 C34 48.2(3) . . . . ? C33 O3 C34 C35 -171.4(2) . . . . ? K1 O3 C34 C35 44.9(2) . . . . ? O4 C35 C34 O3 -61.7(3) . . . . ? C43 N3 C37 C36 77.5(3) . . . . ? C31 N3 C37 C36 -161.6(2) . . . . ? K1 N3 C37 C36 -42.1(3) . . . . ? C29 O2 C30 C31 169.6(2) . . . . ? K1 O2 C30 C31 -52.1(2) . . . . ? C15 C14 C19 C18 -1.2(4) . . . . ? C1 C14 C19 C18 177.4(3) . . . . ? C35 O4 C36 C37 173.3(2) . . . . ? K1 O4 C36 C37 -51.4(3) . . . . ? N3 C37 C36 O4 64.1(3) . . . . ? C37 N3 C31 C30 77.1(3) . . . . ? C43 N3 C31 C30 -161.7(2) . . . . ? K1 N3 C31 C30 -42.6(3) . . . . ? O2 C30 C31 N3 65.3(3) . . . . ? C39 O5 C40 C41 -179.4(2) . . . . ? K1 O5 C40 C41 44.8(3) . . . . ? C7 N1 B1 C1 175.1(2) . . . . ? C3 N1 B1 C1 0.1(2) . . . . ? C7 N1 B1 C8 0.2(4) . . . . ? C3 N1 B1 C8 -174.7(2) . . . . ? C14 C1 B1 N1 -174.4(2) . . . . ? C2 C1 B1 N1 0.6(2) . . . . ? C14 C1 B1 C8 -0.5(4) . . . . ? C2 C1 B1 C8 174.4(3) . . . . ? C9 C8 B1 N1 112.7(3) . . . . ? C13 C8 B1 N1 -63.2(3) . . . . ? C9 C8 B1 C1 -60.5(4) . . . . ? C13 C8 B1 C1 123.5(3) . . . . ? C30 O2 C29 C28 -177.0(2) . . . . ? K1 O2 C29 C28 45.4(3) . . . . ? C21 C20 C25 C24 -1.5(4) . . . . ? C2 C20 C25 C24 175.0(3) . . . . ? C27 O1 C28 C29 -174.8(2) . . . . ? K1 O1 C28 C29 50.2(3) . . . . ? O2 C29 C28 O1 -63.1(3) . . . . ? C8 C13 C12 C11 -0.4(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C42 O6 C41 C40 -177.0(2) . . . . ? K1 O6 C41 C40 53.2(2) . . . . ? O5 C40 C41 O6 -65.7(3) . . . . ? C38 N2 C26 C27 74.1(3) . . . . ? C32 N2 C26 C27 -164.8(2) . . . . ? K1 N2 C26 C27 -45.3(3) . . . . ? C13 C8 C9 C10 0.5(4) . . . . ? B1 C8 C9 C10 -175.6(3) . . . . ? C20 C21 C22 C23 0.4(4) . . . . ? C13 C12 C11 C10 1.2(4) . . . . ? C28 O1 C27 C26 175.6(2) . . . . ? K1 O1 C27 C26 -50.1(3) . . . . ? N2 C26 C27 O1 66.6(3) . . . . ? C40 O5 C39 C38 169.3(2) . . . . ? K1 O5 C39 C38 -54.6(3) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C37 N3 C43 C42 -163.1(2) . . . . ? C31 N3 C43 C42 76.5(3) . . . . ? K1 N3 C43 C42 -42.9(3) . . . . ? C22 C23 C24 C25 0.1(5) . . . . ? C20 C25 C24 C23 1.1(5) . . . . ? C26 N2 C32 C33 74.8(3) . . . . ? C38 N2 C32 C33 -163.5(2) . . . . ? K1 N2 C32 C33 -43.9(3) . . . . ? C34 O3 C33 C32 171.7(2) . . . . ? K1 O3 C33 C32 -46.0(3) . . . . ? N2 C32 C33 O3 60.8(3) . . . . ? C41 O6 C42 C43 178.0(2) . . . . ? K1 O6 C42 C43 -53.2(3) . . . . ? N3 C43 C42 O6 67.1(3) . . . . ? C12 C11 C10 C9 -1.2(5) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C26 N2 C38 C39 -162.2(3) . . . . ? C32 N2 C38 C39 76.7(3) . . . . ? K1 N2 C38 C39 -43.3(3) . . . . ? O5 C39 C38 N2 67.3(3) . . . . ? C15 C16 C17 C18 0.6(5) . . . . ? C16 C17 C18 C19 -1.1(5) . . . . ? C14 C19 C18 C17 1.4(5) . . . . ? _refine_diff_density_max 0.404 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.063 _shelxl_version_number 2014/6 _shelx_res_file ; TITL newMM_a.res in Pbca CELL 1.54178 19.3147 17.6193 24.7059 90.000 90.000 90.000 ZERR 6.000 0.0214 0.0140 0.0234 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H B N O K UNIT 344 440 8 24 48 8 L.S. 20 HTAB CONF ACTA PLAN 0 BOND $H RIGU WPDB -1 FMAP 2 LIST 6 SIZE 0.20 0.20 0.20 TEMP -99.950 WGHT 0.122400 0.023100 FVAR 0.14967 K1 6 0.508299 0.193095 0.346293 11.00000 0.03241 0.03341 = 0.03062 0.00017 0.00048 -0.00098 O4 5 0.368277 0.151210 0.327519 11.00000 0.03421 0.04635 = 0.03569 -0.00021 -0.00707 -0.00124 O2 5 0.517630 0.142894 0.455568 11.00000 0.04509 0.04579 = 0.03407 0.00609 -0.00131 -0.00039 O1 5 0.609964 0.082158 0.378704 11.00000 0.03851 0.05175 = 0.04138 0.00698 -0.00353 0.00499 O6 5 0.488099 0.351067 0.366488 11.00000 0.05187 0.03862 = 0.03719 -0.00614 -0.00265 -0.00419 O3 5 0.469665 0.121145 0.248235 11.00000 0.05116 0.04135 = 0.03773 -0.00896 -0.00266 0.00256 O5 5 0.603459 0.301694 0.304516 11.00000 0.04583 0.04059 = 0.05115 0.00950 0.00708 -0.00084 N3 4 0.398552 0.240900 0.425951 11.00000 0.03646 0.04485 = 0.03141 -0.00291 0.00245 -0.00002 N1 4 0.514600 0.642828 0.423647 11.00000 0.04119 0.03462 = 0.03095 -0.00324 0.00100 -0.00239 N2 4 0.617918 0.143450 0.266053 11.00000 0.04073 0.05035 = 0.03912 0.00408 0.00881 0.01024 C3 1 0.569915 0.679728 0.395596 11.00000 0.03047 0.03327 = 0.02234 -0.00169 0.00096 -0.00145 C1 1 0.473759 0.760631 0.392664 11.00000 0.03207 0.03884 = 0.02841 0.00104 -0.00245 -0.00131 C14 1 0.431226 0.829082 0.385220 11.00000 0.04461 0.03857 = 0.02695 -0.00163 -0.00511 0.00363 C8 1 0.388375 0.666863 0.455107 11.00000 0.03502 0.04012 = 0.03580 0.00532 -0.00218 0.00518 C20 1 0.593426 0.798678 0.339325 11.00000 0.03515 0.03959 = 0.03246 -0.00205 0.00129 0.00178 C7 1 0.527116 0.573202 0.449415 11.00000 0.04331 0.03281 = 0.02910 -0.00107 0.00109 -0.00306 AFIX 43 H7 2 0.490522 0.548978 0.468432 11.00000 -1.20000 AFIX 0 C6 1 0.590583 0.539580 0.447761 11.00000 0.04488 0.03516 = 0.03565 0.00026 -0.00129 0.00395 AFIX 43 H6 2 0.598157 0.493120 0.466354 11.00000 -1.20000 AFIX 0 C15 1 0.459970 0.902001 0.376620 11.00000 0.04895 0.04106 = 0.03135 0.00188 -0.00317 0.00106 AFIX 43 H15 2 0.508839 0.907178 0.374315 11.00000 -1.20000 AFIX 0 C4 1 0.634775 0.642352 0.392995 11.00000 0.03745 0.04188 = 0.03585 0.00037 0.00283 0.00063 AFIX 43 H4 2 0.671494 0.665292 0.373326 11.00000 -1.20000 AFIX 0 C21 1 0.573271 0.819977 0.286920 11.00000 0.04377 0.04166 = 0.03620 0.00058 -0.00211 0.00685 AFIX 43 H21 2 0.528144 0.806978 0.274755 11.00000 -1.20000 AFIX 0 C13 1 0.351048 0.600593 0.442459 11.00000 0.04163 0.03989 = 0.04141 0.00418 -0.00296 0.00245 AFIX 43 H13 2 0.364427 0.571330 0.411904 11.00000 -1.20000 AFIX 0 C2 1 0.546832 0.750670 0.375681 11.00000 0.03867 0.04165 = 0.02902 -0.00167 -0.00132 -0.00018 C5 1 0.646053 0.574186 0.417989 11.00000 0.03757 0.04725 = 0.04054 -0.00143 0.00144 0.00835 AFIX 43 H5 2 0.689958 0.550098 0.415676 11.00000 -1.20000 AFIX 0 C35 1 0.350917 0.137071 0.272268 11.00000 0.04184 0.04761 = 0.03977 -0.00054 -0.01330 -0.00687 AFIX 23 H35A 2 0.349365 0.185632 0.252146 11.00000 -1.20000 H35B 2 0.304547 0.113309 0.270166 11.00000 -1.20000 AFIX 0 C34 1 0.403665 0.085475 0.247131 11.00000 0.05597 0.04110 = 0.03730 -0.00575 -0.01373 -0.00336 AFIX 23 H34A 2 0.405555 0.037029 0.267375 11.00000 -1.20000 H34B 2 0.390455 0.074140 0.209267 11.00000 -1.20000 AFIX 0 C37 1 0.333451 0.200816 0.413954 11.00000 0.03323 0.05931 = 0.03914 0.00203 0.00507 -0.00057 AFIX 23 H37A 2 0.295045 0.227180 0.432681 11.00000 -1.20000 H37B 2 0.336358 0.148777 0.428896 11.00000 -1.20000 AFIX 0 C30 1 0.454393 0.143568 0.485914 11.00000 0.04940 0.05715 = 0.02986 0.00542 -0.00062 -0.00517 AFIX 23 H30A 2 0.464053 0.131735 0.524352 11.00000 -1.20000 H30B 2 0.422403 0.104513 0.471615 11.00000 -1.20000 AFIX 0 C19 1 0.357680 0.825988 0.387531 11.00000 0.04455 0.04432 = 0.04792 0.00775 -0.00109 0.00436 AFIX 43 H19 2 0.335550 0.778349 0.392533 11.00000 -1.20000 AFIX 0 C36 1 0.316372 0.195698 0.353936 11.00000 0.03007 0.05877 = 0.04470 -0.00007 -0.00478 0.00001 AFIX 23 H36A 2 0.270382 0.171882 0.348978 11.00000 -1.20000 H36B 2 0.314932 0.247205 0.337962 11.00000 -1.20000 AFIX 0 C31 1 0.421453 0.221038 0.481476 11.00000 0.04667 0.06085 = 0.03081 -0.00598 0.00186 -0.00100 AFIX 23 H31A 2 0.380955 0.223098 0.505994 11.00000 -1.20000 H31B 2 0.455114 0.259634 0.493948 11.00000 -1.20000 AFIX 0 C40 1 0.581926 0.378817 0.305914 11.00000 0.05017 0.03557 = 0.05239 0.01037 -0.00514 -0.00743 AFIX 23 H40A 2 0.547471 0.388400 0.277045 11.00000 -1.20000 H40B 2 0.622117 0.412632 0.299839 11.00000 -1.20000 AFIX 0 B1 3 0.454403 0.690879 0.422830 11.00000 0.03147 0.03289 = 0.02732 -0.00208 -0.00045 0.00075 C29 1 0.557072 0.076215 0.465879 11.00000 0.06231 0.04808 = 0.03528 0.00930 -0.00613 0.00597 AFIX 23 H29A 2 0.530731 0.030870 0.454223 11.00000 -1.20000 H29B 2 0.566369 0.071689 0.505154 11.00000 -1.20000 AFIX 0 C25 1 0.660415 0.820154 0.355470 11.00000 0.04035 0.05118 = 0.04330 0.00568 -0.00495 -0.00195 AFIX 43 H25 2 0.675617 0.807842 0.390970 11.00000 -1.20000 AFIX 0 C28 1 0.624245 0.080558 0.435382 11.00000 0.05085 0.05269 = 0.04558 0.00615 -0.01323 0.01120 AFIX 23 H28A 2 0.649815 0.126924 0.445999 11.00000 -1.20000 H28B 2 0.653335 0.035959 0.444150 11.00000 -1.20000 AFIX 0 C12 1 0.294557 0.576645 0.473847 11.00000 0.03909 0.04954 = 0.05551 0.01273 -0.00425 -0.00263 AFIX 43 H12 2 0.270095 0.531840 0.464263 11.00000 -1.20000 AFIX 0 C16 1 0.418611 0.966413 0.371439 11.00000 0.06952 0.03678 = 0.03904 0.00630 0.00120 0.00579 AFIX 43 H16 2 0.439874 1.014422 0.365966 11.00000 -1.20000 AFIX 0 C41 1 0.550423 0.394529 0.360472 11.00000 0.05687 0.03530 = 0.04818 -0.00160 -0.01094 -0.00778 AFIX 23 H41A 2 0.583652 0.380727 0.389351 11.00000 -1.20000 H41B 2 0.539830 0.449301 0.363841 11.00000 -1.20000 AFIX 0 C26 1 0.652285 0.075128 0.287715 11.00000 0.04922 0.05034 = 0.05216 0.00214 0.01140 0.01495 AFIX 23 H26A 2 0.694816 0.065646 0.266398 11.00000 -1.20000 H26B 2 0.621160 0.031108 0.282416 11.00000 -1.20000 AFIX 0 C9 1 0.365769 0.707866 0.500408 11.00000 0.04290 0.05544 = 0.04428 -0.00710 0.00284 0.00099 AFIX 43 H9 2 0.389407 0.753169 0.510064 11.00000 -1.20000 AFIX 0 C22 1 0.616971 0.859424 0.252152 11.00000 0.05977 0.04701 = 0.03747 0.00505 0.00422 0.01121 AFIX 43 H22 2 0.601552 0.873219 0.216988 11.00000 -1.20000 AFIX 0 C11 1 0.274409 0.618122 0.518707 11.00000 0.03691 0.07042 = 0.04945 0.01778 0.00632 0.00299 AFIX 43 H11 2 0.236744 0.601442 0.540386 11.00000 -1.20000 AFIX 0 C27 1 0.671695 0.079515 0.347074 11.00000 0.03805 0.05635 = 0.05842 0.00805 -0.00055 0.01011 AFIX 23 H27A 2 0.699522 0.034555 0.357293 11.00000 -1.20000 H27B 2 0.699843 0.125512 0.353810 11.00000 -1.20000 AFIX 0 C39 1 0.634775 0.282797 0.253573 11.00000 0.04384 0.05416 = 0.05241 0.01511 0.01496 -0.00232 AFIX 23 H39A 2 0.670013 0.321276 0.243890 11.00000 -1.20000 H39B 2 0.599200 0.281789 0.224733 11.00000 -1.20000 AFIX 0 C23 1 0.683454 0.878608 0.269136 11.00000 0.05619 0.05066 = 0.05662 0.01282 0.01635 0.00515 AFIX 43 H23 2 0.713825 0.904984 0.245451 11.00000 -1.20000 AFIX 0 C43 1 0.388624 0.323863 0.421532 11.00000 0.05221 0.05048 = 0.04361 -0.00735 0.00602 0.01178 AFIX 23 H43A 2 0.362986 0.341843 0.453774 11.00000 -1.20000 H43B 2 0.359739 0.334626 0.389331 11.00000 -1.20000 AFIX 0 C24 1 0.705178 0.858948 0.320976 11.00000 0.04152 0.05552 = 0.06632 0.01098 0.00457 -0.00410 AFIX 43 H24 2 0.750442 0.871954 0.332822 11.00000 -1.20000 AFIX 0 C32 1 0.585027 0.125407 0.213562 11.00000 0.06319 0.06268 = 0.03627 0.00002 0.00957 0.01554 AFIX 23 H32A 2 0.618640 0.097071 0.191051 11.00000 -1.20000 H32B 2 0.574424 0.173535 0.194617 11.00000 -1.20000 AFIX 0 C33 1 0.519404 0.079416 0.217820 11.00000 0.06755 0.05150 = 0.03727 -0.01006 -0.00173 0.01342 AFIX 23 H33A 2 0.501070 0.068641 0.181198 11.00000 -1.20000 H33B 2 0.529157 0.030443 0.235925 11.00000 -1.20000 AFIX 0 C42 1 0.455381 0.368123 0.416955 11.00000 0.06522 0.04071 = 0.04381 -0.01018 0.00023 0.00138 AFIX 23 H42A 2 0.445568 0.423186 0.419146 11.00000 -1.20000 H42B 2 0.486607 0.354506 0.447212 11.00000 -1.20000 AFIX 0 C10 1 0.309621 0.684271 0.531806 11.00000 0.04691 0.07499 = 0.04688 -0.00508 0.00990 0.00653 AFIX 43 H10 2 0.295521 0.713537 0.562162 11.00000 -1.20000 AFIX 0 C38 1 0.668250 0.205649 0.258824 11.00000 0.04115 0.06131 = 0.05953 0.01066 0.01864 0.00779 AFIX 23 H38A 2 0.696115 0.195553 0.225971 11.00000 -1.20000 H38B 2 0.700183 0.206266 0.290166 11.00000 -1.20000 AFIX 0 C17 1 0.347122 0.961781 0.374116 11.00000 0.06807 0.04921 = 0.06063 0.01316 0.00714 0.02166 AFIX 43 H17 2 0.319191 1.005824 0.370221 11.00000 -1.20000 AFIX 0 C18 1 0.317385 0.891144 0.382633 11.00000 0.05110 0.06295 = 0.06383 0.01540 0.00888 0.01804 AFIX 43 H18 2 0.268445 0.887126 0.385182 11.00000 -1.20000 AFIX 0 HKLF 4 REM newMM_a.res in Pbca REM R1 = 0.0612 for 6036 Fo > 4sig(Fo) and 0.0786 for all 7897 data REM 487 parameters refined using 555 restraints END WGHT 0.1219 0.0985 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.404, deepest hole -0.361, 1-sigma level 0.063 Q1 1 0.4225 0.6830 0.4346 11.00000 0.05 0.40 Q2 1 0.4561 0.7217 0.4120 11.00000 0.05 0.36 Q3 1 0.5899 0.6662 0.3855 11.00000 0.05 0.35 Q4 1 0.4743 0.6794 0.4300 11.00000 0.05 0.30 Q5 1 0.6221 0.8206 0.3497 11.00000 0.05 0.28 Q6 1 0.3274 0.5828 0.4604 11.00000 0.05 0.25 Q7 1 0.3952 0.8276 0.3867 11.00000 0.05 0.24 Q8 1 0.3353 0.1576 0.3410 11.00000 0.05 0.24 Q9 1 0.3178 0.5908 0.4511 11.00000 0.05 0.24 Q10 1 0.5076 0.1983 0.3780 11.00000 0.05 0.23 Q11 1 0.3015 0.6459 0.5208 11.00000 0.05 0.23 Q12 1 0.3816 0.9602 0.3787 11.00000 0.05 0.23 Q13 1 0.5746 0.8222 0.3159 11.00000 0.05 0.23 Q14 1 0.3669 0.1077 0.2602 11.00000 0.05 0.23 Q15 1 0.5231 0.1604 0.4269 11.00000 0.05 0.21 Q16 1 0.3332 0.8582 0.4018 11.00000 0.05 0.21 Q17 1 0.3542 0.6468 0.4414 11.00000 0.05 0.21 Q18 1 0.4022 0.2768 0.4151 11.00000 0.05 0.21 Q19 1 0.6535 0.6192 0.4181 11.00000 0.05 0.21 Q20 1 0.6956 0.8784 0.2938 11.00000 0.05 0.21 ; _shelx_res_checksum 97201 _shelx_hkl_file ; 0 1 0 -5.70 0.50 0 1 0 -5.00 0.50 0 -1 0 -4.70 0.50 0 1 0 -3.10 0.70 0 2 0 4609.34 225.58 0 2 0 4634.34 225.68 0 2 0 4958.70 225.58 0 -2 0 4884.81 225.68 0 -3 0 -0.10 1.30 0 3 0 -0.10 1.10 0 3 0 1.00 1.10 0 3 0 -0.30 1.30 0 -4 0 9876.61 453.25 0 4 0 9215.18 453.05 0 4 0 9999.00 453.05 0 4 0 9363.26 453.25 0 -5 0 -1.90 1.70 0 5 0 -1.80 1.90 0 5 0 -0.70 1.60 0 -6 0 92.59 5.80 0 6 0 81.69 6.20 0 -6 0 93.89 6.60 0 6 0 88.59 6.80 0 -7 0 1.20 1.40 0 7 0 2.00 1.70 0 -7 0 0.20 2.00 0 7 0 1.10 2.00 0 8 0 479.95 25.50 0 8 0 482.35 26.10 0 -8 0 507.45 26.00 0 -8 0 491.65 25.00 0 9 0 -0.90 2.50 0 9 0 0.80 2.00 0 -9 0 -0.60 2.20 0 -9 0 -1.60 1.50 0 10 0 56.99 6.80 0 10 0 57.89 6.00 0 -10 0 60.59 5.40 0 11 0 3.10 3.10 0 11 0 -1.60 2.10 0 12 0 13.30 4.50 0 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284.47 14.10 6 5 0 7.60 2.00 6 5 0 5.00 2.00 6 5 0 5.60 2.20 -6 -5 0 4.50 3.10 -6 5 0 9.40 2.80 6 -5 0 5.60 2.00 6 6 0 67.59 5.70 -6 -6 0 66.19 7.40 -6 6 0 58.29 6.20 6 6 0 68.69 5.20 6 -6 0 62.19 5.60 6 6 0 67.19 6.10 -6 -7 0 5.60 3.60 -6 7 0 7.30 2.90 6 -7 0 4.10 2.20 6 7 0 2.40 2.10 6 7 0 2.40 2.30 -6 8 0 111.39 9.30 6 -8 0 99.79 8.10 6 8 0 102.79 8.60 6 8 0 118.49 8.40 -6 -8 0 135.69 10.60 -6 -9 0 28.70 7.00 6 -9 0 28.40 4.60 -6 9 0 34.10 5.70 6 9 0 19.50 4.20 -6 10 0 29.90 5.90 6 10 0 13.70 3.90 -6 -10 0 24.30 5.80 6 -10 0 16.50 3.80 -6 -11 0 5.90 4.30 6 11 0 1.30 2.90 6 -11 0 1.80 2.80 -6 11 0 -0.40 3.40 6 12 0 4.20 3.70 -6 -12 0 15.10 6.50 -6 12 0 7.20 4.40 -6 13 0 29.50 3.60 6 -13 0 23.30 3.20 6 13 0 17.90 3.30 6 13 0 23.40 2.80 6 14 0 71.39 5.00 -6 14 0 74.29 5.40 6 -14 0 66.79 5.20 6 15 0 10.70 2.50 -6 -15 0 6.80 2.00 -6 15 0 3.80 1.80 6 -15 0 4.60 1.70 6 -16 0 11.30 2.50 -6 -16 0 11.60 2.50 6 16 0 14.20 2.60 6 -17 0 -0.40 1.20 -6 -17 0 -1.90 1.50 6 17 0 0.60 1.30 6 18 0 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5.40 8 -2 0 64.39 5.70 8 2 0 73.49 5.80 -8 -3 0 251.37 15.60 -8 3 0 232.78 13.90 -8 3 0 245.68 14.00 8 -3 0 248.58 14.20 8 3 0 245.98 14.00 8 3 0 249.38 14.10 8 -3 0 263.37 13.60 8 4 0 107.79 7.40 8 -4 0 95.49 6.70 -8 -4 0 103.69 9.20 8 -4 0 110.89 7.60 -8 4 0 103.99 7.70 8 4 0 98.09 7.50 8 -5 0 786.32 38.40 -8 5 0 772.62 39.50 -8 -5 0 765.72 41.00 8 -5 0 746.13 39.20 8 5 0 766.82 39.00 8 5 0 806.82 39.40 -8 -6 0 145.89 11.50 -8 6 0 129.09 10.00 8 -6 0 132.69 9.40 8 6 0 131.29 9.70 8 6 0 142.49 9.40 8 -7 0 24.60 4.20 8 7 0 21.40 4.40 8 7 0 16.50 3.80 -8 7 0 29.90 5.20 -8 -7 0 20.00 5.10 -8 8 0 8.60 3.60 8 8 0 16.00 3.70 8 8 0 12.10 3.60 8 -8 0 15.50 3.60 -8 -8 0 12.70 4.70 -8 -9 0 232.18 17.00 8 -9 0 229.18 14.20 -8 9 0 205.18 15.00 8 9 0 207.78 14.50 8 10 0 87.39 9.00 -8 -10 0 82.49 10.70 -8 10 0 97.09 9.70 8 -10 0 85.89 8.20 -8 -11 0 5.70 5.70 8 -11 0 7.70 3.70 8 11 0 7.00 4.00 -8 11 0 3.20 4.20 8 12 0 0.80 1.20 -8 12 0 3.90 1.50 -8 12 0 3.50 1.70 8 12 0 2.50 1.80 -8 13 0 67.39 5.20 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173.98 12.20 10 1 0 174.68 11.00 10 -2 0 128.19 8.20 10 2 0 133.39 9.00 -10 -2 0 110.19 10.20 -10 2 0 118.99 8.20 10 2 0 119.99 8.60 10 -2 0 114.09 8.60 10 3 0 344.47 19.10 -10 -3 0 352.06 21.20 10 -3 0 347.97 19.40 -10 3 0 342.47 18.90 10 3 0 325.97 19.10 10 -3 0 351.66 18.60 10 -4 0 15.30 3.50 10 4 0 26.70 4.70 10 4 0 21.40 4.20 -10 -4 0 20.40 5.10 -10 4 0 26.30 4.30 10 5 0 129.49 9.80 -10 -5 0 144.29 12.10 10 -5 0 136.69 9.90 10 5 0 138.39 9.90 -10 5 0 145.69 10.20 10 6 0 74.69 7.30 10 6 0 73.99 7.10 -10 6 0 79.39 7.70 -10 -6 0 66.79 9.30 10 -6 0 79.19 7.20 10 7 0 84.29 8.40 -10 7 0 86.49 8.50 -10 -7 0 98.19 10.60 10 -7 0 92.59 8.10 10 7 0 81.79 8.00 -10 -8 0 61.29 9.70 10 8 0 64.69 7.30 10 -8 0 65.89 7.30 -10 8 0 43.40 7.40 10 -9 0 309.97 19.10 -10 -9 0 351.46 22.60 10 9 0 285.27 19.20 -10 9 0 299.47 19.90 10 10 0 9.70 2.10 -10 10 0 3.00 1.70 -10 10 0 6.70 2.10 -10 11 0 33.30 3.70 -10 11 0 28.00 3.20 10 11 0 35.60 3.20 -10 12 0 14.20 2.60 10 12 0 20.10 3.30 10 12 0 15.00 2.50 -10 12 0 14.50 2.80 10 13 0 15.90 2.60 -10 13 0 17.60 2.70 -10 13 0 14.40 2.90 10 13 0 18.50 3.20 10 14 0 4.00 1.60 -10 14 0 3.90 1.80 10 15 0 5.00 1.60 -10 -15 0 7.10 2.00 -10 15 0 6.00 1.90 -10 16 0 9.00 2.00 10 16 0 6.60 1.70 -10 -16 0 5.80 1.80 -10 -17 0 -0.70 1.30 -10 17 0 1.70 1.20 10 17 0 1.90 1.30 -10 -18 0 25.00 2.50 -10 18 0 22.90 2.30 10 18 0 25.40 2.40 10 19 0 5.50 1.20 11 0 0 1.90 2.20 -11 0 0 3.40 3.10 11 0 0 -0.60 1.80 -11 1 0 2.10 4.10 11 -1 0 0.00 1.90 11 1 0 0.50 2.10 -11 -1 0 6.90 3.60 11 -1 0 0.50 2.10 11 1 0 -1.50 1.70 11 2 0 0.00 2.00 11 2 0 0.60 2.00 -11 -2 0 5.50 3.80 11 -2 0 1.80 2.10 11 -3 0 -1.80 1.80 -11 -3 0 -0.30 3.40 11 3 0 0.40 2.20 11 3 0 1.70 2.20 11 4 0 0.00 2.20 11 4 0 1.10 2.40 -11 4 0 -0.20 2.30 -11 -4 0 2.10 3.60 11 -4 0 0.90 2.30 11 5 0 -0.70 2.20 -11 -5 0 0.90 3.50 11 5 0 -4.20 2.30 -11 5 0 1.00 2.40 11 -5 0 -2.40 2.00 11 -6 0 4.80 2.60 -11 6 0 -2.50 2.20 -11 -6 0 7.50 4.40 11 6 0 -3.00 2.40 11 6 0 -2.50 2.60 11 -7 0 3.40 2.80 -11 -7 0 -3.10 3.90 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12 -5 0 15.50 4.10 12 6 0 75.69 8.20 -12 -6 0 75.19 10.20 12 -6 0 63.29 7.70 12 6 0 66.39 7.70 12 7 0 52.79 7.50 -12 -7 0 49.80 9.80 12 -7 0 55.59 7.40 -12 8 0 240.88 15.60 -12 -8 0 168.78 10.40 -12 8 0 165.98 10.10 -12 9 0 29.50 3.60 -12 -9 0 29.70 4.00 12 9 0 23.90 2.90 -12 10 0 88.49 6.10 -12 -10 0 87.89 6.30 12 10 0 80.09 5.50 12 11 0 10.60 2.20 -12 11 0 6.90 2.00 12 -12 0 43.30 3.80 12 12 0 46.30 3.80 -12 12 0 43.90 4.30 12 13 0 1.90 1.30 12 -13 0 0.50 1.20 -12 13 0 1.80 1.50 -12 14 0 28.10 3.30 12 14 0 30.40 3.10 12 -14 0 28.60 3.00 -12 15 0 -1.60 1.30 12 15 0 0.70 1.30 12 16 0 5.70 1.40 -12 16 0 6.10 1.50 12 17 0 18.60 2.20 -12 17 0 25.30 2.40 -12 18 0 5.60 1.30 12 18 0 3.60 1.00 13 0 0 -1.20 2.20 -13 -1 0 4.00 4.60 13 -1 0 1.80 2.60 13 1 0 -2.70 2.40 -13 -2 0 -4.40 3.60 13 2 0 3.40 2.90 13 2 0 2.30 2.90 13 -2 0 2.90 3.10 13 3 0 -0.40 2.70 -13 -3 0 6.70 4.50 13 3 0 0.00 2.90 13 -3 0 0.80 2.80 13 4 0 -2.70 2.70 -13 -4 0 -0.20 4.40 13 4 0 2.40 3.00 13 -4 0 1.50 2.80 13 5 0 2.00 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41.90 7.50 0 12 -1 45.40 6.20 0 13 -1 0.50 3.90 0 13 1 -0.60 3.10 0 13 1 3.30 3.80 0 13 -1 3.20 3.30 0 -14 -1 2.70 1.60 0 14 -1 3.40 1.40 0 14 1 1.40 1.20 0 -14 1 2.40 1.70 0 15 -1 -1.40 1.00 0 15 1 -1.40 1.10 0 -15 -1 1.80 1.60 0 -15 1 0.10 1.60 0 16 1 168.08 9.40 0 -16 1 163.08 9.90 0 -16 -1 178.18 10.10 0 16 -1 160.48 9.30 0 17 1 -1.30 1.30 0 17 -1 -2.40 1.20 0 -17 -1 0.50 1.50 0 -17 1 0.10 1.40 0 -18 -1 2.40 1.60 0 -18 1 3.00 1.70 0 18 1 4.50 1.40 0 18 -1 7.00 1.60 0 -19 -1 0.90 1.40 0 -19 1 1.30 1.40 0 19 1 1.40 1.10 0 19 -1 -2.20 1.00 0 -20 1 22.30 2.60 0 -20 -1 20.20 2.50 0 20 1 23.40 2.30 0 20 -1 21.40 2.10 0 -21 -1 0.60 1.00 0 -21 1 -2.10 0.90 1 0 1 0.00 0.40 1 0 1 0.00 0.30 1 0 1 0.60 0.60 -1 0 1 -0.50 0.40 -1 0 -1 -0.30 0.30 1 0 -1 0.10 0.30 1 0 -1 0.40 0.50 -1 0 1 0.30 0.50 1 -1 -1 5.60 0.90 1 1 1 4.80 1.00 1 1 1 6.00 0.80 -1 -1 1 4.70 1.10 -1 1 -1 5.00 1.10 -1 1 -1 5.40 0.60 1 1 1 5.10 1.10 -1 1 1 5.60 1.20 1 1 -1 6.10 0.70 1 -1 1 5.60 0.90 -1 -1 -1 4.00 1.00 1 -1 1 5.60 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4 6 -4 34.00 4.70 4 -6 4 39.50 5.00 4 -7 -4 97.29 7.20 4 7 4 94.29 7.40 4 7 4 90.09 7.50 -4 7 -4 93.89 7.90 -4 -7 4 84.49 8.90 4 7 -4 98.19 7.30 4 7 -4 93.79 7.60 4 -7 4 94.09 7.50 -4 -7 -4 84.69 8.10 4 -7 4 101.79 6.50 -4 7 4 82.29 7.70 4 8 4 11.20 3.30 -4 8 -4 13.80 3.80 4 -8 -4 14.50 3.60 -4 -8 4 13.30 4.30 4 8 4 8.70 3.00 4 -8 4 14.60 3.40 -4 8 4 14.50 3.60 -4 -8 -4 10.00 3.70 4 8 -4 19.40 4.50 4 8 -4 17.30 3.50 4 -8 4 15.70 3.20 4 9 4 208.98 13.40 4 9 4 216.98 13.40 4 -9 -4 202.68 12.80 -4 -9 4 199.48 14.80 -4 9 -4 202.68 14.00 4 9 -4 207.08 13.50 4 9 -4 190.88 12.90 -4 9 4 195.38 13.80 -4 -9 -4 228.18 14.60 4 10 4 30.10 5.40 4 10 4 30.70 5.30 -4 10 -4 25.60 5.90 4 -10 -4 19.90 4.50 -4 -10 4 17.60 4.90 4 10 -4 26.10 5.00 -4 -10 -4 29.20 6.50 4 10 -4 27.10 5.80 -4 10 4 15.80 4.40 4 11 4 38.70 6.20 4 -11 -4 28.80 5.20 -4 -11 4 40.50 8.00 -4 11 -4 37.40 7.20 4 11 4 37.20 6.10 -4 11 4 23.40 5.50 4 11 -4 28.10 5.60 4 11 -4 37.10 6.80 -4 12 -4 41.70 8.20 -4 -12 4 53.29 9.30 4 -12 -4 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4 33.80 3.20 -10 12 -4 20.80 3.50 -10 12 4 25.50 3.50 10 12 -4 30.70 3.10 -10 12 4 32.20 3.40 -10 13 -4 5.80 1.90 10 13 4 5.40 2.10 10 13 4 4.90 1.50 -10 13 4 3.30 1.60 10 13 -4 5.20 1.60 -10 13 4 3.80 1.70 10 14 4 19.40 3.20 -10 14 -4 20.20 3.20 10 14 4 13.40 2.60 -10 14 4 21.70 2.90 10 14 -4 21.90 2.60 -10 14 4 17.60 2.80 10 15 4 30.10 3.50 10 15 4 31.40 3.10 -10 15 -4 24.90 3.30 -10 15 4 28.50 3.10 10 15 -4 26.20 3.00 -10 15 4 32.90 3.20 10 16 4 2.60 1.40 -10 16 -4 2.30 1.50 -10 16 4 3.40 1.50 -10 16 4 3.50 1.40 10 16 -4 3.70 1.40 -10 17 -4 24.40 2.70 10 17 4 23.40 2.50 -10 -17 -4 24.30 2.90 10 17 -4 23.30 2.50 -10 17 4 23.70 3.30 10 18 4 6.00 1.30 -10 18 -4 8.00 1.80 -10 -18 -4 6.20 1.60 10 18 -4 7.90 1.70 10 19 4 1.00 0.90 10 19 -4 0.30 0.90 -10 -19 -4 0.20 1.10 11 0 4 7.30 3.00 11 0 -4 7.20 2.50 11 0 -4 2.10 2.30 -11 0 4 5.00 2.20 -11 0 -4 2.10 3.50 11 -1 -4 15.20 3.40 -11 1 -4 14.20 4.60 11 -1 -4 10.80 3.10 11 1 4 14.50 3.50 -11 -1 4 4.50 3.70 11 -1 4 8.20 3.00 11 1 -4 13.20 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6.20 11 7 4 17.20 4.40 11 7 -4 14.50 4.00 -11 -7 -4 19.60 6.40 -11 7 4 23.80 5.20 11 -7 4 24.10 5.50 11 8 4 0.30 3.40 11 8 4 0.00 3.90 -11 -8 4 4.60 4.70 11 -8 -4 2.80 3.50 -11 -8 -4 7.50 5.10 11 -8 4 5.20 3.40 11 8 -4 4.70 3.70 -11 8 4 2.90 3.40 -11 9 -4 4.50 2.00 -11 -9 4 13.10 3.20 11 9 4 5.30 2.10 11 9 4 5.50 1.80 11 -9 4 5.50 1.60 -11 9 4 7.80 1.70 11 9 -4 5.80 1.50 -11 9 4 3.60 1.50 -11 -10 4 -1.20 1.70 11 10 4 -0.10 1.40 11 10 4 2.30 1.60 -11 10 -4 0.00 1.60 11 10 -4 -0.10 1.10 -11 10 4 1.50 1.40 -11 10 4 -1.40 1.20 11 11 4 25.80 3.60 -11 11 -4 26.40 3.60 11 11 4 28.50 3.10 -11 -11 4 24.80 4.00 -11 11 4 29.50 3.30 11 11 -4 29.00 3.00 -11 11 4 20.80 3.20 11 12 4 3.50 1.90 11 12 4 0.10 1.30 -11 12 -4 3.10 1.70 -11 12 4 0.50 1.40 -11 12 4 0.60 1.40 11 12 -4 1.20 1.30 -11 13 -4 5.20 1.90 11 13 4 3.00 1.80 11 13 4 3.40 1.40 11 13 -4 2.30 1.40 -11 13 4 4.80 1.60 -11 13 4 0.50 1.40 -11 14 -4 11.50 2.80 11 14 4 11.40 2.40 11 14 4 7.90 2.10 11 14 -4 13.10 2.30 -11 14 4 12.60 2.50 -11 14 4 16.50 2.60 -11 15 -4 1.90 1.50 11 15 4 4.50 1.50 11 15 4 3.90 1.80 -11 15 4 4.90 1.60 -11 15 4 6.10 1.60 11 15 -4 5.80 1.60 -11 16 -4 7.20 1.80 11 16 4 7.50 1.60 11 16 -4 6.40 1.50 -11 16 4 8.50 2.00 -11 -16 -4 7.70 1.90 -11 17 -4 5.00 1.40 11 17 4 5.40 1.30 11 -17 -4 1.70 1.40 11 17 -4 2.60 1.20 -11 17 4 0.40 1.10 -11 -17 -4 5.30 1.50 -11 18 -4 -0.50 0.90 11 18 4 -0.50 0.90 -11 -18 -4 0.20 1.00 11 18 -4 -0.50 0.90 12 0 -4 186.28 12.30 12 0 4 195.18 12.80 12 0 -4 174.88 12.40 -12 0 -4 173.88 14.20 12 -1 -4 9.80 3.10 -12 1 -4 21.80 5.40 12 -1 -4 20.20 4.70 12 1 4 20.50 4.90 12 -1 4 19.40 4.60 12 1 -4 14.80 3.70 -12 -1 -4 14.60 4.90 12 1 -4 19.40 4.50 12 -2 -4 31.70 5.00 12 2 4 32.00 5.50 12 -2 -4 29.10 5.00 -12 -2 4 17.80 5.30 -12 2 4 33.00 5.20 12 -2 4 38.00 5.70 -12 -2 -4 28.20 6.30 12 2 -4 27.70 5.20 12 2 -4 22.30 4.70 -12 -3 4 44.50 8.30 12 3 4 54.19 6.80 12 -3 -4 55.99 6.30 12 -3 -4 49.70 6.30 -12 -3 -4 52.39 8.70 12 3 -4 41.80 5.90 12 -3 4 51.19 6.30 12 3 -4 45.70 6.30 -12 3 4 50.99 6.30 12 4 4 2.40 3.20 -12 -4 4 3.10 4.40 12 -4 -4 -3.10 2.50 12 -4 -4 4.30 3.00 12 4 -4 4.20 3.00 -12 4 4 1.80 3.00 -12 -4 -4 2.40 4.10 12 -4 4 6.50 3.10 12 5 4 51.19 7.30 12 -5 -4 43.60 6.50 -12 -5 4 59.49 10.00 -12 5 4 56.69 7.40 -12 -5 -4 61.19 9.50 12 5 -4 55.69 7.00 12 -5 4 57.19 7.20 -12 -6 4 90.39 12.00 12 -6 -4 91.39 9.20 12 6 4 122.49 10.20 12 6 4 99.39 9.20 -12 6 4 95.19 9.50 12 6 -4 100.69 9.60 12 -6 4 97.69 9.20 -12 -6 -4 107.79 12.20 12 7 4 109.99 10.20 12 7 4 111.59 10.20 12 -7 -4 104.69 13.90 -12 -7 4 98.39 14.40 -12 7 4 92.29 6.90 12 7 -4 148.59 14.50 12 -7 4 91.99 9.40 -12 7 4 100.29 10.20 -12 7 4 86.59 7.00 -12 -8 4 62.79 5.30 12 8 4 64.49 4.60 -12 8 -4 64.99 5.10 -12 8 4 67.59 4.70 -12 -8 -4 58.39 5.30 12 -8 4 52.19 4.30 -12 8 4 62.69 4.90 12 8 -4 55.69 4.20 12 9 4 36.20 3.40 -12 9 -4 27.30 3.60 -12 -9 4 29.40 3.90 -12 -9 -4 35.80 4.10 -12 9 4 25.60 3.10 12 -9 4 29.30 3.00 -12 9 4 21.80 3.30 12 9 -4 28.10 3.00 -12 10 -4 6.00 1.90 -12 -10 4 7.60 2.30 -12 10 4 5.20 1.90 12 10 -4 2.50 1.40 12 -10 4 6.50 1.60 -12 10 4 4.50 1.60 -12 -11 4 4.00 2.10 -12 11 -4 5.10 1.90 12 11 4 8.90 2.20 12 11 4 4.40 1.50 -12 11 4 3.40 1.50 12 11 -4 6.20 1.60 -12 11 4 6.90 1.80 -12 -12 4 12.70 2.60 12 12 4 12.50 2.40 12 12 4 14.90 3.10 -12 12 -4 14.70 3.10 -12 12 4 7.40 1.90 -12 12 4 16.80 2.60 12 12 -4 11.40 2.40 12 13 4 -1.00 1.10 12 13 4 3.00 1.70 -12 13 -4 -1.10 1.50 -12 13 4 -1.90 1.10 -12 13 4 1.30 1.40 12 13 -4 1.10 1.20 12 14 4 0.80 1.70 12 14 4 2.80 1.40 -12 14 -4 -1.40 1.40 -12 14 4 1.10 1.40 12 14 -4 0.90 1.20 -12 15 -4 2.60 1.70 12 15 4 2.50 1.30 -12 15 4 1.90 1.30 12 15 -4 4.80 1.30 12 16 4 1.80 1.10 -12 16 -4 3.50 1.50 12 -16 -4 1.80 1.10 12 16 -4 2.40 1.20 -12 -16 -4 1.30 1.40 -12 16 4 0.10 1.00 -12 17 -4 9.70 2.00 12 17 4 8.20 1.70 12 17 -4 12.40 1.80 -12 17 4 11.40 1.80 -12 -17 -4 7.80 1.60 -12 18 -4 6.60 1.40 12 18 -4 2.80 0.90 13 0 4 24.60 5.60 -13 0 -4 22.60 6.50 13 0 -4 35.50 5.60 13 0 -4 25.40 5.40 13 -1 -4 10.90 4.00 13 -1 -4 26.20 5.20 13 1 4 23.30 4.90 -13 -1 -4 19.50 6.10 13 1 -4 20.30 5.00 13 -1 4 13.40 3.80 13 1 -4 17.20 4.20 13 -2 -4 109.49 9.20 13 2 4 102.19 9.50 13 -2 -4 111.19 9.40 -13 -2 -4 109.59 11.80 13 -2 4 104.79 9.50 13 2 -4 103.19 9.30 13 2 -4 103.99 9.00 13 3 4 32.30 6.20 13 -3 -4 29.70 5.50 13 -3 -4 29.20 5.80 -13 -3 4 32.20 7.40 13 -3 4 26.30 5.60 13 3 -4 30.70 6.30 -13 -3 -4 35.20 7.30 13 4 4 38.90 7.00 -13 -4 4 41.00 8.30 13 -4 -4 38.30 6.50 13 -4 4 46.20 6.70 -13 -4 -4 44.10 9.40 13 4 -4 35.30 6.50 13 5 4 -1.60 3.30 13 -5 -4 -0.80 2.90 -13 -5 4 -0.70 5.30 -13 -5 -4 1.60 4.90 13 5 -4 -2.80 3.00 13 -5 4 2.70 3.20 13 6 4 2.40 1.30 -13 -6 4 -0.60 1.60 -13 6 4 7.30 4.40 -13 -6 -4 -1.40 1.60 13 -6 4 1.00 1.20 -13 6 4 -0.60 1.20 13 7 4 0.90 1.30 -13 -7 4 2.80 1.80 -13 7 -4 3.50 1.70 13 -7 4 4.40 1.50 -13 7 4 1.20 1.20 13 7 -4 0.00 1.10 -13 -7 -4 -0.60 1.80 -13 7 4 2.80 1.50 -13 8 -4 27.80 3.50 13 8 4 22.20 2.90 -13 -8 4 23.10 3.70 -13 8 4 23.00 2.90 -13 8 4 22.00 3.20 -13 -8 -4 21.00 3.70 13 -8 4 16.10 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12.10 4.20 14 -1 -4 16.00 4.20 14 -1 -4 17.60 4.40 14 1 4 6.30 3.90 -14 -1 -4 11.70 6.00 14 -1 4 15.50 4.50 14 1 -4 24.10 5.00 14 1 -4 11.10 4.00 14 -2 -4 9.70 3.60 14 2 4 9.50 4.20 -14 -2 -4 13.80 5.80 14 -2 4 6.40 3.80 14 2 -4 0.70 3.70 14 3 4 26.90 3.20 -14 -3 4 20.90 3.60 14 -3 -4 28.00 4.20 14 -3 4 16.30 2.70 -14 -3 -4 46.10 11.40 14 3 -4 33.60 6.70 -14 -4 4 23.60 3.60 14 -4 -4 22.20 2.90 14 4 4 24.40 2.90 14 -4 4 21.10 2.70 -14 4 4 23.90 2.80 -14 -4 -4 19.20 3.90 14 5 4 38.60 3.60 -14 -5 4 46.70 3.40 14 -5 -4 43.30 3.70 -14 -5 4 43.70 4.50 -14 5 4 45.50 3.90 14 -5 4 43.90 3.60 -14 -5 -4 41.60 4.70 -14 -6 4 201.08 11.90 14 6 4 196.48 11.10 -14 6 -4 203.28 11.50 14 -6 -4 220.98 11.30 -14 -6 -4 204.38 12.10 14 -6 4 207.28 11.10 14 6 -4 203.48 10.90 -14 6 4 201.08 11.30 -14 7 -4 13.40 3.00 14 7 4 14.70 2.70 14 -7 -4 10.00 2.00 -14 -7 4 13.70 2.80 -14 -7 -4 13.10 2.80 14 7 -4 12.00 2.20 14 -7 4 11.10 2.30 -14 7 4 13.50 2.90 -14 8 -4 5.70 1.90 -14 -8 4 7.80 2.20 14 8 4 12.30 2.60 14 -8 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15.50 4.00 -10 -4 -9 12.20 5.40 10 4 -9 16.60 4.10 10 -4 9 17.80 4.10 10 -5 -9 60.79 6.90 10 5 9 50.09 6.80 10 -5 -9 47.80 6.30 -10 -5 9 68.39 9.80 -10 5 9 55.29 6.90 10 5 -9 42.60 7.50 -10 -5 -9 52.89 9.20 10 -5 9 52.29 6.60 10 5 -9 44.80 6.70 10 6 9 141.09 12.30 10 -6 -9 151.08 11.90 10 -6 -9 153.88 11.80 -10 -6 9 175.18 15.00 -10 -6 -9 171.58 14.70 10 6 -9 168.78 13.00 10 6 -9 172.18 12.20 10 7 9 36.70 6.90 -10 -7 9 28.40 7.10 10 -7 -9 32.50 6.40 10 -7 -9 28.20 5.50 -10 -7 -9 21.70 6.60 10 7 -9 17.70 4.40 -10 7 9 29.80 6.80 -10 8 -9 47.60 4.70 -10 -8 9 41.10 4.60 -10 -8 9 53.79 3.60 10 8 9 47.80 4.00 10 8 9 45.80 4.40 -10 8 9 41.10 3.90 -10 8 9 53.99 4.10 -10 8 9 49.10 3.70 10 -8 9 46.30 4.30 -10 -9 9 36.60 4.20 10 9 9 30.40 3.70 10 9 9 33.10 3.40 -10 9 -9 39.00 4.30 -10 9 9 37.00 3.50 -10 9 9 33.70 3.40 10 -9 9 35.30 3.70 -10 9 9 41.20 3.20 10 9 -9 33.50 3.10 10 10 9 66.09 5.00 10 10 9 67.19 5.30 -10 -10 9 64.69 5.50 -10 10 -9 77.69 5.70 -10 10 9 68.19 5.00 -10 10 9 71.59 5.00 10 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23.50 6 2 10 461.55 23.90 6 -2 -10 433.16 22.80 -6 -2 10 428.26 24.40 6 2 -10 411.46 23.20 6 2 -10 424.86 23.90 -6 2 10 464.45 23.60 -6 -2 -10 434.36 25.30 6 -2 10 400.96 24.70 6 -2 10 435.36 23.10 -6 -3 10 11.80 4.00 6 -3 -10 13.40 3.10 6 -3 -10 9.00 2.50 6 3 10 21.20 4.30 -6 -3 -10 18.50 4.70 6 3 -10 12.40 2.90 6 -3 10 9.80 2.70 6 -3 10 10.80 3.80 6 3 -10 17.70 3.90 -6 3 10 15.00 3.40 6 4 10 123.09 8.90 -6 4 -10 137.79 9.40 6 4 10 125.29 9.80 6 -4 -10 114.39 9.20 -6 -4 10 149.49 11.50 6 -4 -10 128.79 9.00 6 4 -10 135.49 9.20 -6 4 10 124.49 9.30 -6 -4 -10 133.69 11.20 6 4 -10 129.19 10.00 6 -4 10 137.39 11.00 6 5 10 10.40 2.90 6 5 10 13.00 3.60 -6 5 -10 10.20 3.20 6 -5 -10 16.10 3.80 -6 -5 10 9.70 4.20 6 5 -10 10.10 3.00 -6 -5 -10 6.30 3.60 6 5 -10 4.00 3.20 -6 5 10 7.40 3.10 6 -5 10 5.00 3.60 -6 6 -10 216.18 14.50 6 6 10 196.18 14.50 -6 -6 10 237.68 16.50 6 -6 -10 218.98 14.00 6 6 10 230.08 14.10 6 6 -10 220.88 14.80 6 6 -10 219.78 14.00 6 -6 10 238.38 16.10 -6 6 10 233.58 14.70 -6 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85.89 9.80 8 -4 -10 85.39 7.60 -8 -4 10 91.29 9.70 8 -4 -10 76.39 7.10 8 4 10 96.19 8.20 -8 -4 -10 93.29 9.90 8 4 -10 72.49 7.80 8 -4 10 67.69 7.00 8 4 -10 81.59 7.40 -8 4 10 74.09 7.50 8 5 10 -2.20 2.60 8 -5 -10 1.60 2.50 -8 -5 10 1.20 4.00 8 -5 -10 0.00 2.00 8 5 -10 0.10 2.50 8 5 -10 -2.00 2.60 -8 -5 -10 -1.20 3.30 -8 5 10 0.10 2.30 8 6 10 173.28 12.70 -8 -6 10 166.08 14.30 8 -6 -10 166.78 12.10 8 -6 -10 172.18 11.90 8 6 -10 175.88 12.20 -8 6 10 174.18 12.60 8 6 -10 159.68 12.50 -8 -6 -10 153.68 13.70 8 -7 -10 3.50 2.60 -8 -7 10 2.30 4.40 8 -7 -10 -0.70 3.10 8 7 10 0.70 3.10 8 7 -10 1.20 2.70 8 7 -10 3.10 3.50 -8 7 10 1.00 3.10 -8 -7 -10 0.50 4.00 8 8 10 2.30 3.70 8 -8 -10 3.30 3.40 8 -8 -10 7.70 3.40 8 8 10 6.80 4.00 -8 -8 10 -2.80 4.40 -8 8 10 0.50 3.50 8 8 -10 5.30 4.20 8 8 -10 1.20 3.30 -8 -8 -10 4.40 5.00 8 9 10 12.80 2.60 8 9 10 13.80 5.40 8 9 10 12.70 2.90 -8 -9 10 12.90 2.50 -8 9 10 10.10 2.10 8 -9 10 15.50 2.90 8 9 -10 10.70 2.20 -8 9 10 11.40 2.40 -8 9 10 10.30 2.50 -8 -10 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-3 27 3.50 1.40 -4 -4 27 29.30 2.90 -4 -4 27 25.80 2.30 4 -4 27 32.30 2.90 -4 -5 27 0.60 0.80 -4 -5 27 0.10 1.20 4 -5 27 0.20 1.10 -4 -6 27 7.00 1.60 -4 -6 27 11.30 1.50 4 -6 27 6.00 1.50 -4 -7 27 2.40 0.80 -4 -7 27 1.90 1.20 4 -7 27 1.30 1.10 -4 -8 27 -0.50 0.90 -4 -8 27 0.00 0.70 4 -8 27 2.20 1.10 -5 0 27 0.20 0.90 5 0 27 -0.60 1.20 -5 -1 27 6.20 1.20 -5 1 27 5.30 1.20 5 -1 27 2.80 1.40 -5 -2 27 1.10 0.90 5 -2 27 -0.40 1.20 -5 -3 27 23.40 2.60 -5 -3 27 21.20 2.10 5 -3 27 20.20 2.50 -5 -4 27 9.10 1.60 -5 -4 27 11.60 2.30 5 -4 27 16.90 2.30 -5 -5 27 7.00 1.40 -5 -5 27 8.20 1.60 5 -5 27 7.60 1.60 -5 -6 27 1.10 0.80 -5 -6 27 4.30 1.30 5 -6 27 3.70 1.30 -5 -7 27 1.10 1.10 -5 -7 27 0.50 0.70 5 -7 27 1.00 1.00 -5 -8 27 0.60 0.60 -5 -8 27 0.10 1.00 5 -8 27 -0.30 0.90 6 0 27 -0.70 1.10 -6 0 27 -1.10 0.80 -6 -1 27 -0.10 0.90 -6 1 27 -0.10 0.90 6 -1 27 -0.10 1.00 -6 -2 27 23.10 2.20 6 -2 27 27.50 2.70 -6 2 27 29.30 2.40 6 -2 27 29.20 3.60 -6 -3 27 -1.60 1.10 -6 -3 27 -1.80 0.80 6 -3 27 0.50 1.20 6 -3 27 0.10 1.10 -6 -4 27 37.00 2.70 -6 -4 27 38.20 3.10 6 -4 27 38.10 3.20 6 -4 27 37.90 3.00 -6 -5 27 2.60 0.90 -6 -5 27 4.40 1.30 6 -5 27 4.00 1.30 6 -5 27 2.30 1.30 -6 -6 27 9.90 1.30 -6 -6 27 7.80 1.80 6 -6 27 8.70 1.70 -6 -7 27 0.40 0.70 -6 -7 27 0.60 1.00 6 -7 27 0.30 1.00 7 0 27 0.80 1.20 7 0 27 -0.90 1.10 -7 0 27 -0.90 0.80 7 1 27 0.20 1.10 7 1 27 0.90 1.20 -7 -1 27 -0.20 0.80 7 -1 27 -1.40 1.00 -7 1 27 -0.20 0.90 7 -1 27 0.70 1.20 -7 -2 27 0.20 0.80 7 2 27 -0.20 1.20 7 -2 27 -1.10 1.10 -7 2 27 -0.20 0.80 7 -2 27 1.20 1.10 -7 -3 27 7.80 1.40 7 3 27 5.80 1.50 7 -3 27 4.80 1.40 7 -3 27 4.70 1.30 -7 -4 27 3.80 1.00 -7 -4 27 1.00 1.10 7 -4 27 5.50 1.40 7 -4 27 3.60 1.30 -7 -5 27 13.70 2.00 -7 -5 27 12.70 1.60 7 -5 27 16.60 2.00 7 -5 27 14.70 1.90 -7 -6 27 -0.40 1.00 -7 -6 27 0.30 0.60 7 -6 27 -0.20 0.80 -8 0 27 0.70 0.80 8 0 27 1.40 1.10 8 0 27 -0.10 1.10 8 1 27 0.30 1.00 -8 -1 27 0.60 0.80 8 1 27 1.80 1.10 8 -1 27 -0.20 1.10 8 -1 27 -2.00 1.00 -8 1 27 1.50 0.90 8 2 27 18.00 2.30 -8 -2 27 19.70 1.90 8 -2 27 22.00 2.40 -8 2 27 23.70 1.90 8 -2 27 23.10 2.40 8 3 27 1.10 1.10 -8 -3 27 2.00 0.80 8 -3 27 2.40 1.10 8 -3 27 3.50 1.20 -8 3 27 1.60 0.80 -8 -4 27 5.70 1.20 8 4 27 7.30 1.60 8 -4 27 7.80 1.50 8 -4 27 8.20 1.70 -8 -5 27 0.80 0.80 8 -5 27 0.70 1.10 8 -5 27 2.00 1.40 9 0 27 -0.90 1.00 9 0 27 -0.50 0.90 -9 0 27 -0.20 0.70 9 1 27 1.90 1.10 -9 -1 27 -0.60 0.70 9 1 27 0.80 1.50 9 -1 27 -0.50 0.90 -9 1 27 0.10 0.70 9 -1 27 0.00 1.00 -9 -2 27 3.10 0.90 9 2 27 4.70 1.30 -9 2 27 4.10 0.90 9 -2 27 2.50 1.20 9 -2 27 7.50 1.70 9 3 27 1.50 1.30 -9 -3 27 2.00 0.80 9 -3 27 0.50 1.00 9 -3 27 0.70 1.00 -9 -4 27 0.70 0.70 9 -4 27 0.90 1.10 9 -4 27 1.90 1.70 -10 0 27 0.00 0.70 10 0 27 -0.90 1.00 10 1 27 0.30 1.20 -10 -1 27 1.60 0.70 -10 1 27 2.10 0.90 10 -1 27 2.40 1.20 10 -1 27 2.40 1.40 10 -2 27 7.30 1.70 0 -2 28 5.10 1.40 0 -3 28 1.50 1.20 0 -4 28 4.90 1.40 0 -4 28 6.20 1.50 0 -5 28 0.10 1.10 0 -5 28 0.90 0.70 0 -6 28 3.00 0.80 0 -6 28 3.60 1.20 0 -7 28 -0.60 0.90 0 -7 28 -0.50 0.50 1 -1 28 4.80 1.40 -1 -2 28 13.00 2.10 1 -2 28 12.60 2.10 -1 -3 28 4.50 1.20 -1 -3 28 3.60 1.40 1 -3 28 5.50 1.40 -1 -4 28 0.10 1.10 -1 -4 28 0.20 0.70 1 -4 28 -0.10 1.10 -1 -5 28 1.70 1.10 -1 -5 28 0.60 0.80 1 -5 28 -0.30 1.00 -1 -6 28 6.40 1.20 -1 -6 28 4.50 1.30 1 -6 28 5.80 1.10 1 -6 28 7.80 1.80 -1 -7 28 3.20 0.70 -1 -7 28 1.00 1.00 1 -7 28 1.00 1.00 2 -1 28 -0.50 1.10 -2 -2 28 4.10 1.20 2 -2 28 0.00 1.10 -2 -3 28 8.00 1.80 -2 -3 28 3.70 1.00 2 -3 28 5.50 1.40 -2 -4 28 6.50 1.30 -2 -4 28 4.80 1.30 2 -4 28 3.60 1.30 -2 -5 28 14.90 1.60 -2 -5 28 18.30 2.10 2 -5 28 15.30 2.10 -2 -6 28 2.10 1.10 -2 -6 28 0.70 0.70 2 -6 28 1.60 1.00 -2 -7 28 0.10 0.90 -2 -7 28 1.10 0.70 2 -7 28 1.50 1.00 3 -1 28 13.90 2.10 -3 -2 28 0.20 0.80 3 -2 28 2.40 1.20 -3 -3 28 8.50 1.40 -3 -3 28 8.00 1.80 3 -3 28 8.80 1.90 -3 -4 28 2.40 0.90 -3 -4 28 1.60 1.10 3 -4 28 4.00 1.20 -3 -5 28 4.30 0.90 -3 -5 28 9.90 1.70 3 -5 28 6.00 1.30 -3 -6 28 0.60 1.00 -3 -6 28 0.60 0.70 3 -6 28 0.10 1.00 -3 -7 28 12.60 1.30 -3 -7 28 14.50 1.80 3 -7 28 15.50 1.80 -4 -1 28 -1.20 0.80 4 -1 28 1.60 1.20 -4 -2 28 5.00 1.10 4 -2 28 5.20 1.40 -4 -3 28 1.50 1.10 -4 -3 28 1.20 0.80 4 -3 28 1.50 1.10 -4 -4 28 1.00 1.00 -4 -4 28 -0.70 0.70 4 -4 28 0.80 1.10 -4 -5 28 5.10 1.00 -4 -5 28 8.10 1.70 4 -5 28 5.10 1.30 -4 -6 28 0.60 0.60 -4 -6 28 0.60 0.90 4 -6 28 1.40 1.10 5 0 28 1.20 1.10 -5 0 28 0.10 0.80 -5 -1 28 9.80 1.50 5 -1 28 8.90 1.90 -5 -2 28 1.90 0.90 5 -2 28 2.30 1.20 -5 -3 28 3.80 1.00 5 -3 28 3.30 1.20 -5 -4 28 4.90 1.20 -5 -4 28 2.70 1.10 5 -4 28 5.50 1.30 -5 -5 28 -0.10 1.00 -5 -5 28 1.80 0.70 5 -5 28 0.90 1.10 -5 -6 28 0.90 0.70 -5 -6 28 0.80 1.30 5 -6 28 0.60 1.00 6 0 28 -1.30 1.00 -6 0 28 1.00 0.80 -6 -1 28 7.70 1.40 6 -1 28 9.50 1.80 -6 1 28 11.50 1.60 -6 -2 28 0.00 0.80 6 -2 28 0.60 1.10 -6 -3 28 1.80 0.80 6 -3 28 1.10 1.10 -6 -4 28 2.40 0.80 6 -4 28 1.60 1.10 -6 -5 28 0.30 0.70 6 -5 28 2.50 1.00 7 0 28 2.10 1.40 -7 0 28 1.10 0.80 -7 -1 28 5.70 1.30 -7 1 28 4.50 1.10 7 -1 28 5.40 1.30 -7 -2 28 0.90 0.80 7 -2 28 -2.00 1.00 -7 -3 28 7.00 1.20 7 -3 28 7.50 1.70 -7 -4 28 0.30 0.60 7 -4 28 -0.20 1.00 -8 0 28 0.00 0.90 -8 -1 28 13.20 1.60 -8 -2 28 -0.40 0.70 8 -2 28 -0.20 1.40 0 -2 29 19.70 2.60 0 -3 29 -1.70 0.80 0 -4 29 0.50 1.00 0 -5 29 2.10 1.00 1 -2 29 1.50 1.10 -1 -3 29 45.40 3.30 1 -3 29 54.09 3.40 -1 -4 29 2.20 1.10 1 -4 29 1.80 1.10 -1 -5 29 20.60 2.20 1 -5 29 25.50 2.20 2 -2 29 26.20 2.40 -2 -3 29 2.80 1.60 2 -3 29 0.80 1.00 -2 -4 29 -0.10 1.20 2 -4 29 0.80 1.00 2 -5 29 4.20 1.10 3 -2 29 1.40 1.10 3 -3 29 23.90 2.30 3 -4 29 2.90 1.10 4 -2 29 23.30 2.50 4 -3 29 -1.00 0.90 4 -4 29 12.10 2.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2946 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Warren Piers' _publ_contact_author_address ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Morgan, Matthew' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; 'Piers, Warren' ; University of Calgary Department of Chemistry 2500 University Drive Calgary, Alberta Canada, T2N 1N4 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_MM1510_0m _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C106 H54 B2 Cl8 F40 N2 Zr2' _chemical_formula_sum 'C106 H54 B2 Cl8 F40 N2 Zr2' _chemical_formula_weight 2603.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6013(2) _cell_length_b 14.2473(2) _cell_length_c 15.7688(2) _cell_angle_alpha 63.9930(10) _cell_angle_beta 86.3180(10) _cell_angle_gamma 80.9800(10) _cell_volume 2512.88(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2183 _cell_measurement_theta_min 31.76 _cell_measurement_theta_max 68.23 _exptl_crystal_description 'plate' _exptl_crystal_colour 'Yellow' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.720 _exptl_crystal_F_000 1290 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_absorpt_coefficient_mu 4.793 _shelx_estimated_absorpt_T_min 0.597 _shelx_estimated_absorpt_T_max 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23808 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.118 _diffrn_reflns_theta_max 67.489 _diffrn_reflns_theta_full 67.500 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 8791 _reflns_number_gt 7160 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.1.7' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0711P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8791 _refine_ls_number_parameters 750 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.8125(3) 0.0290(3) 0.7319(2) 0.0324(7) Uani 1 1 d . . . . . C1 C 0.8017(3) 0.5359(2) 0.6680(2) 0.0325(6) Uani 1 1 d . . . . . C2 C 0.9011(2) 0.4798(2) 0.6745(2) 0.0304(6) Uani 1 1 d . . . . . C3 C 0.9553(2) 0.4855(2) 0.5870(2) 0.0285(6) Uani 1 1 d . . . . . C4 C 0.9465(2) 0.5736(2) 0.4202(2) 0.0294(6) Uani 1 1 d . . . . . C5 C 0.8814(3) 0.6568(3) 0.3377(2) 0.0378(7) Uani 1 1 d . . . . . H5A H 0.8211 0.6920 0.3605 0.057 Uiso 1 1 calc R U . . . H5B H 0.8537 0.6239 0.3022 0.057 Uiso 1 1 calc R U . . . H5C H 0.9267 0.7088 0.2965 0.057 Uiso 1 1 calc R U . . . C6 C 0.9573(3) 0.4177(3) 0.7680(2) 0.0359(7) Uani 1 1 d . . . . . C7 C 0.9331(3) 0.3185(3) 0.8287(3) 0.0533(10) Uani 1 1 d . . . . . H7 H 0.8825 0.2877 0.8106 0.064 Uiso 1 1 calc R U . . . C8 C 0.9830(4) 0.2646(4) 0.9160(3) 0.0733(15) Uani 1 1 d . . . . . H8 H 0.9676 0.1959 0.9572 0.088 Uiso 1 1 calc R U . . . C9 C 1.0544(4) 0.3093(5) 0.9437(3) 0.0770(17) Uani 1 1 d . . . . . H9 H 1.0877 0.2717 1.0041 0.092 Uiso 1 1 calc R U . . . C10 C 1.0784(4) 0.4090(4) 0.8840(3) 0.0625(11) Uani 1 1 d . . . . . H10 H 1.1274 0.4402 0.9033 0.075 Uiso 1 1 calc R U . . . C11 C 1.0302(3) 0.4623(3) 0.7962(3) 0.0473(8) Uani 1 1 d . . . . . H11 H 1.0470 0.5303 0.7547 0.057 Uiso 1 1 calc R U . . . C12 C 0.7495(3) 0.5357(2) 0.7556(2) 0.0360(7) Uani 1 1 d . . . . . C13 C 0.7883(3) 0.5866(3) 0.8032(3) 0.0437(8) Uani 1 1 d . . . . . H13 H 0.8493 0.6217 0.7792 0.052 Uiso 1 1 calc R U . . . C14 C 0.7399(4) 0.5869(3) 0.8841(3) 0.0540(10) Uani 1 1 d . . . . . H14 H 0.7677 0.6222 0.9149 0.065 Uiso 1 1 calc R U . . . C15 C 0.6516(4) 0.5362(3) 0.9203(3) 0.0586(11) Uani 1 1 d . . . . . H15 H 0.6182 0.5366 0.9760 0.070 Uiso 1 1 calc R U . . . C16 C 0.6124(3) 0.4854(3) 0.8758(3) 0.0558(10) Uani 1 1 d . . . . . H16 H 0.5521 0.4495 0.9014 0.067 Uiso 1 1 calc R U . . . C17 C 0.6595(3) 0.4855(3) 0.7935(3) 0.0452(8) Uani 1 1 d . . . . . H17 H 0.6300 0.4511 0.7627 0.054 Uiso 1 1 calc R U . . . C18 C 0.8212(3) 0.8056(3) 0.4664(3) 0.0482(9) Uani 1 1 d . . . . . H18 H 0.8869 0.8100 0.4327 0.058 Uiso 1 1 calc R U . . . C19 C 0.7186(3) 0.8368(3) 0.4264(3) 0.0511(9) Uani 1 1 d . . . . . H19 H 0.7023 0.8651 0.3611 0.061 Uiso 1 1 calc R U . . . C20 C 0.6434(3) 0.8191(3) 0.5001(3) 0.0520(10) Uani 1 1 d . . . . . H20 H 0.5675 0.8346 0.4933 0.062 Uiso 1 1 calc R U . . . C21 C 0.7007(4) 0.7747(3) 0.5848(3) 0.0503(9) Uani 1 1 d . . . . . H21 H 0.6701 0.7535 0.6459 0.060 Uiso 1 1 calc R U . . . C22 C 0.8112(3) 0.7665(3) 0.5649(3) 0.0494(9) Uani 1 1 d . . . . . H22 H 0.8683 0.7396 0.6095 0.059 Uiso 1 1 calc R U . . . C23 C 0.6795(3) 0.5148(3) 0.4689(3) 0.0519(9) Uani 1 1 d . . . . . H23 H 0.7325 0.4772 0.4452 0.062 Uiso 1 1 calc R U . . . C24 C 0.6183(3) 0.6137(4) 0.4147(3) 0.0554(10) Uani 1 1 d . . . . . H24 H 0.6230 0.6546 0.3485 0.066 Uiso 1 1 calc R U . . . C25 C 0.5495(3) 0.6402(3) 0.4765(3) 0.0536(10) Uani 1 1 d . . . . . H25 H 0.4983 0.7022 0.4594 0.064 Uiso 1 1 calc R U . . . C26 C 0.5689(3) 0.5599(3) 0.5677(3) 0.0475(8) Uani 1 1 d . . . . . H26 H 0.5340 0.5584 0.6234 0.057 Uiso 1 1 calc R U . . . C27 C 0.6488(3) 0.4817(3) 0.5630(3) 0.0466(8) Uani 1 1 d . . . . . H27 H 0.6769 0.4178 0.6146 0.056 Uiso 1 1 calc R U . . . C28 C 0.8365(2) 0.1026(2) 0.6195(2) 0.0303(6) Uani 1 1 d . . . . . C29 C 0.8526(3) 0.2074(2) 0.5785(2) 0.0325(6) Uani 1 1 d . . . . . C30 C 0.8841(3) 0.2597(2) 0.4856(2) 0.0343(7) Uani 1 1 d . . . . . C31 C 0.9017(3) 0.2083(3) 0.4289(2) 0.0370(7) Uani 1 1 d . . . . . C32 C 0.8872(3) 0.1035(3) 0.4661(2) 0.0366(7) Uani 1 1 d . . . . . C33 C 0.8574(3) 0.0543(2) 0.5594(2) 0.0332(6) Uani 1 1 d . . . . . C34 C 0.9297(3) -0.0454(2) 0.7688(2) 0.0310(6) Uani 1 1 d . . . . . C35 C 1.0178(3) 0.0030(3) 0.7672(2) 0.0369(7) Uani 1 1 d . . . . . C36 C 1.1211(3) -0.0481(3) 0.7912(2) 0.0407(7) Uani 1 1 d . . . . . C37 C 1.1414(3) -0.1555(3) 0.8213(2) 0.0417(8) Uani 1 1 d . . . . . C38 C 1.0575(3) -0.2083(3) 0.8242(2) 0.0391(7) Uani 1 1 d . . . . . C39 C 0.9555(3) -0.1527(2) 0.7959(2) 0.0335(6) Uani 1 1 d . . . . . C40 C 0.7703(3) 0.0963(2) 0.7929(2) 0.0327(6) Uani 1 1 d . . . . . C41 C 0.6793(3) 0.1723(2) 0.7628(2) 0.0374(7) Uani 1 1 d . . . . . C42 C 0.6271(3) 0.2221(3) 0.8144(3) 0.0423(8) Uani 1 1 d . . . . . C43 C 0.6650(3) 0.1976(3) 0.9026(3) 0.0468(9) Uani 1 1 d . . . . . C44 C 0.7560(3) 0.1243(3) 0.9359(2) 0.0444(8) Uani 1 1 d . . . . . C45 C 0.8059(3) 0.0758(2) 0.8818(2) 0.0367(7) Uani 1 1 d . . . . . C46 C 0.7112(3) -0.0388(2) 0.7466(2) 0.0344(7) Uani 1 1 d . . . . . C47 C 0.6341(3) -0.0229(3) 0.6803(3) 0.0394(7) Uani 1 1 d . . . . . C48 C 0.5491(3) -0.0798(3) 0.6999(3) 0.0459(8) Uani 1 1 d . . . . . C49 C 0.5365(3) -0.1563(3) 0.7901(3) 0.0482(9) Uani 1 1 d . . . . . C50 C 0.6079(3) -0.1727(3) 0.8594(3) 0.0428(8) Uani 1 1 d . . . . . C51 C 0.6913(3) -0.1141(2) 0.8365(2) 0.0367(7) Uani 1 1 d . . . . . C70 C 0.6542(6) 0.3726(5) 0.2393(5) 0.098(2) Uani 1 1 d . . . . . H70A H 0.7213 0.3496 0.2131 0.118 Uiso 1 1 calc R U . . . H70B H 0.5936 0.3755 0.2009 0.118 Uiso 1 1 calc R U . . . Cl4 Cl 0.63949(14) 0.27871(16) 0.35569(15) 0.1057(5) Uani 1 1 d . . . . . Cl3 Cl 0.65817(15) 0.49802(17) 0.22911(17) 0.1139(7) Uani 1 1 d . . . . . F1 F 0.83911(16) 0.26596(14) 0.62733(13) 0.0391(4) Uani 1 1 d . . . . . F2 F 0.89857(18) 0.36193(14) 0.44959(14) 0.0446(5) Uani 1 1 d . . . . . F3 F 0.9312(2) 0.25955(16) 0.33922(14) 0.0495(5) Uani 1 1 d . . . . . F4 F 0.90289(19) 0.05183(16) 0.41221(14) 0.0467(5) Uani 1 1 d . . . . . F5 F 0.84986(17) -0.04963(14) 0.59244(13) 0.0405(4) Uani 1 1 d . . . . . F6 F 1.00397(17) 0.10876(15) 0.74034(14) 0.0432(4) Uani 1 1 d . . . . . F7 F 1.20167(17) 0.00569(19) 0.78568(15) 0.0525(5) Uani 1 1 d . . . . . F8 F 1.23999(18) -0.2082(2) 0.84692(18) 0.0577(6) Uani 1 1 d . . . . . F9 F 1.07613(18) -0.31309(16) 0.85172(15) 0.0488(5) Uani 1 1 d . . . . . F10 F 0.88113(16) -0.21125(14) 0.79616(14) 0.0403(4) Uani 1 1 d . . . . . F11 F 0.63438(17) 0.19798(16) 0.67832(15) 0.0446(5) Uani 1 1 d . . . . . F12 F 0.53882(18) 0.29337(18) 0.78052(19) 0.0576(6) Uani 1 1 d . . . . . F13 F 0.6145(2) 0.2421(2) 0.95564(19) 0.0639(7) Uani 1 1 d . . . . . F14 F 0.7945(2) 0.09837(19) 1.02171(15) 0.0592(6) Uani 1 1 d . . . . . F15 F 0.89311(18) 0.00355(16) 0.92205(14) 0.0464(5) Uani 1 1 d . . . . . F16 F 0.63764(18) 0.05202(16) 0.59070(15) 0.0471(5) Uani 1 1 d . . . . . F17 F 0.47953(19) -0.0612(2) 0.6316(2) 0.0628(6) Uani 1 1 d . . . . . F18 F 0.4550(2) -0.2128(2) 0.8103(2) 0.0693(7) Uani 1 1 d . . . . . F19 F 0.59526(19) -0.24422(18) 0.94847(17) 0.0559(6) Uani 1 1 d . . . . . F20 F 0.75704(16) -0.13373(15) 0.90834(13) 0.0417(4) Uani 1 1 d . . . . . N1 N 0.9052(2) 0.55711(18) 0.50520(17) 0.0283(5) Uani 1 1 d . . . . . Zr1 Zr 0.73659(2) 0.64232(2) 0.51889(2) 0.03097(9) Uani 1 1 d . . . . . C52A C 0.6240(7) 0.8908(5) 0.0768(5) 0.0567(18) Uani 0.730(11) 1 d . U P A 1 H52A H 0.5742 0.8564 0.0573 0.068 Uiso 0.730(11) 1 calc R U P A 1 H52B H 0.6610 0.9364 0.0196 0.068 Uiso 0.730(11) 1 calc R U P A 1 Cl1A Cl 0.7181(4) 0.7950(5) 0.1547(3) 0.1068(13) Uani 0.730(11) 1 d . U P A 1 Cl2A Cl 0.5507(2) 0.9682(2) 0.1263(3) 0.0753(9) Uani 0.730(11) 1 d . U P A 1 Cl1B Cl 0.6917(8) 0.7603(7) 0.1450(5) 0.076(2) Uani 0.270(11) 1 d . U P A 2 C52B C 0.6654(19) 0.901(2) 0.0970(16) 0.064(5) Uani 0.270(11) 1 d D U P A 2 H52C H 0.6324 0.9318 0.0335 0.077 Uiso 0.270(11) 1 calc R U P A 2 H52D H 0.7322 0.9313 0.0928 0.077 Uiso 0.270(11) 1 calc R U P A 2 Cl2B Cl 0.5733(10) 0.9250(15) 0.1800(15) 0.121(4) Uani 0.270(11) 1 d D U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0360(19) 0.0294(15) 0.0293(16) -0.0102(13) 0.0009(14) -0.0058(14) C1 0.0315(16) 0.0320(14) 0.0375(15) -0.0169(12) 0.0046(13) -0.0103(12) C2 0.0306(16) 0.0278(13) 0.0321(14) -0.0114(11) 0.0021(13) -0.0073(11) C3 0.0271(15) 0.0257(12) 0.0320(14) -0.0105(11) 0.0002(12) -0.0075(11) C4 0.0287(15) 0.0281(13) 0.0312(14) -0.0115(11) 0.0002(12) -0.0072(11) C5 0.0318(17) 0.0394(16) 0.0357(16) -0.0131(13) -0.0009(14) 0.0043(13) C6 0.0328(17) 0.0404(16) 0.0305(15) -0.0135(13) 0.0029(13) -0.0009(13) C7 0.041(2) 0.053(2) 0.046(2) -0.0046(17) 0.0060(17) -0.0077(16) C8 0.055(3) 0.074(3) 0.048(2) 0.012(2) 0.007(2) -0.007(2) C9 0.045(3) 0.119(4) 0.0322(19) -0.007(2) -0.0051(19) 0.008(3) C10 0.052(2) 0.094(3) 0.047(2) -0.038(2) -0.0087(19) 0.001(2) C11 0.046(2) 0.053(2) 0.0438(19) -0.0228(16) 0.0000(16) -0.0059(16) C12 0.0355(17) 0.0346(14) 0.0375(16) -0.0161(13) 0.0030(14) -0.0034(13) C13 0.044(2) 0.0464(18) 0.0439(18) -0.0226(15) 0.0059(16) -0.0080(15) C14 0.065(3) 0.055(2) 0.047(2) -0.0288(17) 0.0070(19) -0.0042(19) C15 0.072(3) 0.055(2) 0.046(2) -0.0243(18) 0.021(2) -0.003(2) C16 0.049(2) 0.054(2) 0.058(2) -0.0200(18) 0.0185(19) -0.0094(17) C17 0.0409(19) 0.0412(17) 0.052(2) -0.0193(15) 0.0082(17) -0.0076(14) C18 0.050(2) 0.0328(16) 0.061(2) -0.0206(16) 0.0088(19) -0.0088(15) C19 0.057(2) 0.0338(16) 0.053(2) -0.0122(15) -0.0001(19) -0.0010(15) C20 0.047(2) 0.0328(16) 0.070(3) -0.0210(16) 0.004(2) 0.0047(15) C21 0.066(3) 0.0321(16) 0.054(2) -0.0233(15) 0.0099(19) -0.0013(15) C22 0.055(2) 0.0354(16) 0.065(2) -0.0274(16) -0.0035(19) -0.0073(15) C23 0.043(2) 0.063(2) 0.069(2) -0.044(2) 0.0030(19) -0.0148(17) C24 0.046(2) 0.074(3) 0.051(2) -0.0261(19) -0.0065(18) -0.0210(19) C25 0.0332(19) 0.058(2) 0.067(2) -0.0245(19) -0.0101(18) -0.0034(16) C26 0.0303(18) 0.060(2) 0.057(2) -0.0274(18) 0.0024(16) -0.0135(15) C27 0.0350(18) 0.0440(18) 0.063(2) -0.0229(16) -0.0047(17) -0.0121(15) C28 0.0280(15) 0.0316(14) 0.0305(14) -0.0122(12) -0.0008(12) -0.0053(11) C29 0.0312(16) 0.0343(14) 0.0359(15) -0.0187(12) -0.0032(13) -0.0034(12) C30 0.0353(17) 0.0295(14) 0.0352(15) -0.0103(12) -0.0013(13) -0.0069(12) C31 0.0397(18) 0.0402(16) 0.0288(14) -0.0120(13) 0.0022(13) -0.0099(13) C32 0.0406(18) 0.0388(16) 0.0343(15) -0.0202(13) -0.0029(14) -0.0021(13) C33 0.0345(16) 0.0287(13) 0.0358(15) -0.0134(12) -0.0024(13) -0.0033(12) C34 0.0309(16) 0.0363(14) 0.0268(13) -0.0148(12) 0.0005(12) -0.0042(12) C35 0.0395(18) 0.0422(16) 0.0275(14) -0.0131(12) 0.0028(13) -0.0088(14) C36 0.0329(18) 0.058(2) 0.0319(15) -0.0185(14) 0.0014(14) -0.0128(15) C37 0.0324(17) 0.061(2) 0.0313(15) -0.0223(15) 0.0014(14) 0.0012(15) C38 0.0413(19) 0.0414(17) 0.0322(15) -0.0167(13) 0.0016(14) 0.0027(14) C39 0.0347(17) 0.0383(15) 0.0276(14) -0.0142(12) 0.0018(13) -0.0066(13) C40 0.0346(16) 0.0319(14) 0.0329(15) -0.0144(12) 0.0049(13) -0.0090(12) C41 0.0385(18) 0.0366(15) 0.0393(16) -0.0176(13) 0.0027(14) -0.0095(13) C42 0.0364(18) 0.0392(16) 0.054(2) -0.0235(15) 0.0072(16) -0.0069(14) C43 0.052(2) 0.0462(18) 0.052(2) -0.0299(16) 0.0217(18) -0.0158(16) C44 0.057(2) 0.0490(18) 0.0346(16) -0.0221(14) 0.0086(16) -0.0187(16) C45 0.0414(18) 0.0337(15) 0.0351(15) -0.0146(12) 0.0043(14) -0.0083(13) C46 0.0310(16) 0.0323(14) 0.0415(17) -0.0182(13) 0.0025(14) -0.0035(12) C47 0.0359(18) 0.0376(16) 0.0463(18) -0.0204(14) -0.0022(15) -0.0021(13) C48 0.0291(17) 0.0512(19) 0.066(2) -0.0341(18) -0.0047(17) -0.0017(15) C49 0.0325(18) 0.0502(19) 0.072(3) -0.0351(18) 0.0139(18) -0.0144(15) C50 0.0379(18) 0.0375(16) 0.052(2) -0.0185(15) 0.0144(16) -0.0095(14) C51 0.0341(17) 0.0366(15) 0.0400(17) -0.0185(13) 0.0027(14) -0.0021(13) C70 0.099(5) 0.108(5) 0.118(5) -0.084(4) -0.008(4) 0.011(4) Cl4 0.0758(9) 0.1196(12) 0.1315(14) -0.0708(11) -0.0237(10) 0.0183(9) Cl3 0.0911(11) 0.1344(14) 0.1731(19) -0.1137(15) 0.0382(12) -0.0467(10) F1 0.0512(11) 0.0338(8) 0.0380(9) -0.0201(7) 0.0037(8) -0.0093(8) F2 0.0579(13) 0.0329(9) 0.0422(10) -0.0130(8) 0.0041(9) -0.0159(8) F3 0.0680(14) 0.0471(10) 0.0326(9) -0.0153(8) 0.0105(10) -0.0167(10) F4 0.0636(13) 0.0468(10) 0.0373(10) -0.0256(8) 0.0058(9) -0.0095(9) F5 0.0555(12) 0.0300(8) 0.0387(9) -0.0166(7) 0.0050(9) -0.0101(8) F6 0.0459(11) 0.0390(9) 0.0443(10) -0.0148(8) -0.0025(9) -0.0146(8) F7 0.0402(11) 0.0726(14) 0.0448(11) -0.0213(10) 0.0016(9) -0.0219(10) F8 0.0339(11) 0.0790(15) 0.0625(14) -0.0370(12) -0.0067(10) 0.0078(10) F9 0.0535(13) 0.0414(10) 0.0456(11) -0.0184(8) -0.0055(10) 0.0104(9) F10 0.0412(11) 0.0326(8) 0.0475(10) -0.0176(8) 0.0006(9) -0.0063(8) F11 0.0400(11) 0.0471(10) 0.0464(11) -0.0216(9) -0.0085(9) 0.0019(8) F12 0.0432(12) 0.0555(12) 0.0812(16) -0.0395(12) 0.0033(12) 0.0024(10) F13 0.0740(17) 0.0668(14) 0.0670(15) -0.0463(12) 0.0257(13) -0.0128(12) F14 0.0824(17) 0.0672(14) 0.0377(11) -0.0303(10) 0.0044(11) -0.0165(12) F15 0.0518(12) 0.0503(11) 0.0355(9) -0.0182(8) -0.0065(9) -0.0017(9) F16 0.0468(12) 0.0482(10) 0.0443(11) -0.0162(9) -0.0103(9) -0.0093(9) F17 0.0427(12) 0.0709(15) 0.0852(17) -0.0404(13) -0.0154(13) -0.0108(11) F18 0.0440(13) 0.0779(16) 0.102(2) -0.0484(15) 0.0189(14) -0.0315(12) F19 0.0575(14) 0.0526(12) 0.0568(13) -0.0219(10) 0.0252(11) -0.0216(10) F20 0.0438(11) 0.0426(10) 0.0349(9) -0.0127(8) 0.0033(8) -0.0097(8) N1 0.0270(12) 0.0273(11) 0.0311(12) -0.0129(10) 0.0006(10) -0.0051(9) Zr1 0.02600(14) 0.02902(13) 0.03685(14) -0.01405(10) 0.00013(10) -0.00186(9) C52A 0.064(5) 0.048(3) 0.055(4) -0.022(3) 0.003(3) -0.002(3) Cl1A 0.097(2) 0.110(3) 0.0957(18) -0.0422(17) -0.0364(16) 0.0415(19) Cl2A 0.0643(13) 0.0754(14) 0.104(2) -0.0593(14) 0.0195(13) -0.0059(10) Cl1B 0.088(5) 0.073(4) 0.049(3) -0.018(2) 0.013(3) 0.009(3) C52B 0.076(12) 0.078(9) 0.059(9) -0.044(7) 0.007(9) -0.023(9) Cl2B 0.097(6) 0.142(9) 0.178(11) -0.115(8) 0.026(7) -0.042(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C40 1.647(5) . ? B1 C34 1.650(5) . ? B1 C28 1.652(4) . ? B1 C46 1.664(5) . ? C1 C2 1.360(5) . ? C1 C12 1.490(5) . ? C1 Zr1 2.288(3) . ? C2 C3 1.474(4) . ? C2 C6 1.500(4) . ? C3 N1 1.361(4) . ? C3 C4 1.411(4) 2_766 ? C4 N1 1.340(4) . ? C4 C3 1.411(4) 2_766 ? C4 C5 1.500(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.385(5) . ? C6 C11 1.390(5) . ? C7 C8 1.383(6) . ? C7 H7 0.9500 . ? C8 C9 1.371(8) . ? C8 H8 0.9500 . ? C9 C10 1.386(8) . ? C9 H9 0.9500 . ? C10 C11 1.379(6) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.395(5) . ? C12 C13 1.401(5) . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.376(7) . ? C14 H14 0.9500 . ? C15 C16 1.365(7) . ? C15 H15 0.9500 . ? C16 C17 1.392(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.395(6) . ? C18 C22 1.406(6) . ? C18 Zr1 2.492(4) . ? C18 H18 0.9500 . ? C19 C20 1.410(6) . ? C19 Zr1 2.482(3) . ? C19 H19 0.9500 . ? C20 C21 1.395(6) . ? C20 Zr1 2.505(3) . ? C20 H20 0.9500 . ? C21 C22 1.405(6) . ? C21 Zr1 2.497(4) . ? C21 H21 0.9500 . ? C22 Zr1 2.505(4) . ? C22 H22 0.9500 . ? C23 C27 1.393(6) . ? C23 C24 1.414(6) . ? C23 Zr1 2.486(4) . ? C23 H23 0.9500 . ? C24 C25 1.398(6) . ? C24 Zr1 2.486(4) . ? C24 H24 0.9500 . ? C25 C26 1.397(6) . ? C25 Zr1 2.500(4) . ? C25 H25 0.9500 . ? C26 C27 1.404(6) . ? C26 Zr1 2.492(4) . ? C26 H26 0.9500 . ? C27 Zr1 2.499(3) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 C33 1.388(5) . ? C29 F1 1.349(4) . ? C29 C30 1.385(5) . ? C30 F2 1.350(4) . ? C30 C31 1.372(5) . ? C31 F3 1.336(4) . ? C31 C32 1.382(5) . ? C32 F4 1.336(4) . ? C32 C33 1.379(5) . ? C33 F5 1.354(4) . ? C34 C39 1.383(4) . ? C34 C35 1.389(5) . ? C35 F6 1.359(4) . ? C35 C36 1.376(5) . ? C36 F7 1.341(4) . ? C36 C37 1.375(6) . ? C37 F8 1.333(4) . ? C37 C38 1.377(6) . ? C38 F9 1.344(4) . ? C38 C39 1.387(5) . ? C39 F10 1.348(4) . ? C40 C45 1.391(5) . ? C40 C41 1.393(5) . ? C41 F11 1.353(4) . ? C41 C42 1.375(5) . ? C42 F12 1.342(4) . ? C42 C43 1.376(6) . ? C43 F13 1.333(4) . ? C43 C44 1.379(6) . ? C44 F14 1.339(4) . ? C44 C45 1.382(5) . ? C45 F15 1.353(4) . ? C46 C51 1.388(5) . ? C46 C47 1.393(5) . ? C47 F16 1.349(4) . ? C47 C48 1.382(5) . ? C48 F17 1.340(5) . ? C48 C49 1.379(6) . ? C49 F18 1.341(4) . ? C49 C50 1.377(6) . ? C50 F19 1.342(4) . ? C50 C51 1.376(5) . ? C51 F20 1.348(4) . ? C70 Cl3 1.731(6) . ? C70 Cl4 1.753(8) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? N1 Zr1 2.323(2) . ? C52A Cl1A 1.728(8) . ? C52A Cl2A 1.739(7) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? Cl1B C52B 1.79(3) . ? C52B Cl2B 1.801(16) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 B1 C34 113.0(3) . . ? C40 B1 C28 114.4(2) . . ? C34 B1 C28 102.0(2) . . ? C40 B1 C46 101.2(2) . . ? C34 B1 C46 114.0(2) . . ? C28 B1 C46 112.7(3) . . ? C2 C1 C12 118.8(3) . . ? C2 C1 Zr1 116.3(2) . . ? C12 C1 Zr1 124.3(2) . . ? C1 C2 C3 118.7(3) . . ? C1 C2 C6 120.9(3) . . ? C3 C2 C6 120.3(3) . . ? N1 C3 C4 117.4(3) . 2_766 ? N1 C3 C2 115.6(3) . . ? C4 C3 C2 126.9(3) 2_766 . ? N1 C4 C3 120.1(3) . 2_766 ? N1 C4 C5 115.2(3) . . ? C3 C4 C5 124.7(3) 2_766 . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.5(4) . . ? C7 C6 C2 120.8(3) . . ? C11 C6 C2 119.7(3) . . ? C8 C7 C6 119.6(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.2(5) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C6 120.7(4) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C17 C12 C13 117.1(3) . . ? C17 C12 C1 121.6(3) . . ? C13 C12 C1 121.3(3) . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.7(4) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C19 C18 C22 108.6(4) . . ? C19 C18 Zr1 73.3(2) . . ? C22 C18 Zr1 74.2(2) . . ? C19 C18 H18 125.7 . . ? C22 C18 H18 125.7 . . ? Zr1 C18 H18 118.7 . . ? C18 C19 C20 107.9(4) . . ? C18 C19 Zr1 74.1(2) . . ? C20 C19 Zr1 74.5(2) . . ? C18 C19 H19 126.1 . . ? C20 C19 H19 126.1 . . ? Zr1 C19 H19 117.4 . . ? C21 C20 C19 107.6(4) . . ? C21 C20 Zr1 73.49(19) . . ? C19 C20 Zr1 72.7(2) . . ? C21 C20 H20 126.2 . . ? C19 C20 H20 126.2 . . ? Zr1 C20 H20 119.5 . . ? C20 C21 C22 108.8(4) . . ? C20 C21 Zr1 74.1(2) . . ? C22 C21 Zr1 74.0(2) . . ? C20 C21 H21 125.6 . . ? C22 C21 H21 125.6 . . ? Zr1 C21 H21 118.1 . . ? C21 C22 C18 107.1(4) . . ? C21 C22 Zr1 73.4(2) . . ? C18 C22 Zr1 73.2(2) . . ? C21 C22 H22 126.5 . . ? C18 C22 H22 126.5 . . ? Zr1 C22 H22 119.0 . . ? C27 C23 C24 108.4(4) . . ? C27 C23 Zr1 74.3(2) . . ? C24 C23 Zr1 73.5(2) . . ? C27 C23 H23 125.8 . . ? C24 C23 H23 125.8 . . ? Zr1 C23 H23 118.3 . . ? C25 C24 C23 107.4(4) . . ? C25 C24 Zr1 74.3(2) . . ? C23 C24 Zr1 73.5(2) . . ? C25 C24 H24 126.3 . . ? C23 C24 H24 126.3 . . ? Zr1 C24 H24 118.0 . . ? C26 C25 C24 108.2(4) . . ? C26 C25 Zr1 73.5(2) . . ? C24 C25 Zr1 73.2(2) . . ? C26 C25 H25 125.9 . . ? C24 C25 H25 125.9 . . ? Zr1 C25 H25 119.3 . . ? C25 C26 C27 108.4(4) . . ? C25 C26 Zr1 74.0(2) . . ? C27 C26 Zr1 73.9(2) . . ? C25 C26 H26 125.8 . . ? C27 C26 H26 125.8 . . ? Zr1 C26 H26 118.1 . . ? C23 C27 C26 107.6(4) . . ? C23 C27 Zr1 73.3(2) . . ? C26 C27 Zr1 73.4(2) . . ? C23 C27 H27 126.2 . . ? C26 C27 H27 126.2 . . ? Zr1 C27 H27 119.1 . . ? C29 C28 C33 113.6(3) . . ? C29 C28 B1 127.2(3) . . ? C33 C28 B1 118.6(3) . . ? F1 C29 C30 115.0(3) . . ? F1 C29 C28 121.7(3) . . ? C30 C29 C28 123.2(3) . . ? F2 C30 C31 118.9(3) . . ? F2 C30 C29 120.5(3) . . ? C31 C30 C29 120.6(3) . . ? F3 C31 C30 120.2(3) . . ? F3 C31 C32 121.1(3) . . ? C30 C31 C32 118.8(3) . . ? F4 C32 C33 121.5(3) . . ? F4 C32 C31 120.0(3) . . ? C33 C32 C31 118.5(3) . . ? F5 C33 C32 115.4(3) . . ? F5 C33 C28 119.4(3) . . ? C32 C33 C28 125.2(3) . . ? C39 C34 C35 113.2(3) . . ? C39 C34 B1 128.0(3) . . ? C35 C34 B1 118.6(3) . . ? F6 C35 C36 115.7(3) . . ? F6 C35 C34 119.3(3) . . ? C36 C35 C34 125.0(3) . . ? F7 C36 C37 120.0(3) . . ? F7 C36 C35 120.8(3) . . ? C37 C36 C35 119.3(3) . . ? F8 C37 C36 121.1(4) . . ? F8 C37 C38 120.2(3) . . ? C36 C37 C38 118.7(3) . . ? F9 C38 C37 119.5(3) . . ? F9 C38 C39 120.6(3) . . ? C37 C38 C39 119.9(3) . . ? F10 C39 C34 121.3(3) . . ? F10 C39 C38 114.8(3) . . ? C34 C39 C38 123.9(3) . . ? C45 C40 C41 113.1(3) . . ? C45 C40 B1 126.7(3) . . ? C41 C40 B1 119.5(3) . . ? F11 C41 C42 115.8(3) . . ? F11 C41 C40 119.3(3) . . ? C42 C41 C40 124.8(3) . . ? F12 C42 C41 121.0(4) . . ? F12 C42 C43 119.4(3) . . ? C41 C42 C43 119.7(3) . . ? F13 C43 C42 121.2(4) . . ? F13 C43 C44 120.5(4) . . ? C42 C43 C44 118.3(3) . . ? F14 C44 C43 119.8(3) . . ? F14 C44 C45 120.0(4) . . ? C43 C44 C45 120.2(3) . . ? F15 C45 C44 115.3(3) . . ? F15 C45 C40 120.8(3) . . ? C44 C45 C40 123.9(3) . . ? C51 C46 C47 113.3(3) . . ? C51 C46 B1 118.7(3) . . ? C47 C46 B1 127.6(3) . . ? F16 C47 C48 115.0(3) . . ? F16 C47 C46 121.1(3) . . ? C48 C47 C46 123.9(3) . . ? F17 C48 C49 120.1(3) . . ? F17 C48 C47 120.3(4) . . ? C49 C48 C47 119.6(4) . . ? F18 C49 C50 120.4(4) . . ? F18 C49 C48 120.5(4) . . ? C50 C49 C48 119.1(3) . . ? F19 C50 C51 120.6(4) . . ? F19 C50 C49 120.2(3) . . ? C51 C50 C49 119.2(3) . . ? F20 C51 C50 115.7(3) . . ? F20 C51 C46 119.4(3) . . ? C50 C51 C46 124.8(4) . . ? Cl3 C70 Cl4 113.7(4) . . ? Cl3 C70 H70A 108.8 . . ? Cl4 C70 H70A 108.8 . . ? Cl3 C70 H70B 108.8 . . ? Cl4 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C4 N1 C3 122.5(3) . . ? C4 N1 Zr1 120.75(19) . . ? C3 N1 Zr1 116.7(2) . . ? C1 Zr1 N1 72.30(10) . . ? C1 Zr1 C19 130.52(13) . . ? N1 Zr1 C19 112.93(11) . . ? C1 Zr1 C24 132.03(13) . . ? N1 Zr1 C24 104.65(13) . . ? C19 Zr1 C24 95.61(15) . . ? C1 Zr1 C23 102.74(13) . . ? N1 Zr1 C23 81.31(11) . . ? C19 Zr1 C23 126.72(15) . . ? C24 Zr1 C23 33.04(15) . . ? C1 Zr1 C18 105.09(12) . . ? N1 Zr1 C18 87.18(11) . . ? C19 Zr1 C18 32.57(14) . . ? C24 Zr1 C18 122.76(14) . . ? C23 Zr1 C18 144.91(14) . . ? C1 Zr1 C26 87.94(12) . . ? N1 Zr1 C26 125.74(11) . . ? C19 Zr1 C26 117.99(14) . . ? C24 Zr1 C26 54.11(14) . . ? C23 Zr1 C26 53.94(13) . . ? C18 Zr1 C26 147.07(13) . . ? C1 Zr1 C21 81.88(12) . . ? N1 Zr1 C21 125.20(12) . . ? C19 Zr1 C21 54.09(13) . . ? C24 Zr1 C21 127.88(15) . . ? C23 Zr1 C21 152.60(14) . . ? C18 Zr1 C21 53.89(13) . . ? C26 Zr1 C21 99.85(14) . . ? C1 Zr1 C27 77.77(12) . . ? N1 Zr1 C27 93.12(11) . . ? C19 Zr1 C27 145.38(14) . . ? C24 Zr1 C27 54.35(14) . . ? C23 Zr1 C27 32.47(14) . . ? C18 Zr1 C27 177.07(14) . . ? C26 Zr1 C27 32.68(13) . . ? C21 Zr1 C27 127.77(14) . . ? C1 Zr1 C25 120.28(13) . . ? N1 Zr1 C25 134.77(12) . . ? C19 Zr1 C25 91.48(14) . . ? C24 Zr1 C25 32.57(15) . . ? C23 Zr1 C25 54.08(14) . . ? C18 Zr1 C25 124.04(13) . . ? C26 Zr1 C25 32.50(14) . . ? C21 Zr1 C25 100.01(15) . . ? C27 Zr1 C25 54.06(13) . . ? C1 Zr1 C20 113.37(13) . . ? N1 Zr1 C20 141.13(11) . . ? C19 Zr1 C20 32.85(14) . . ? C24 Zr1 C20 98.44(16) . . ? C23 Zr1 C20 130.09(15) . . ? C18 Zr1 C20 53.97(13) . . ? C26 Zr1 C20 93.12(13) . . ? C21 Zr1 C20 32.38(14) . . ? C27 Zr1 C20 125.72(13) . . ? C25 Zr1 C20 77.78(14) . . ? C1 Zr1 C22 76.65(12) . . ? N1 Zr1 C22 93.59(11) . . ? C19 Zr1 C22 54.27(14) . . ? C24 Zr1 C22 149.42(14) . . ? C23 Zr1 C22 174.76(14) . . ? C18 Zr1 C22 32.67(14) . . ? C26 Zr1 C22 130.97(14) . . ? C21 Zr1 C22 32.63(14) . . ? C27 Zr1 C22 150.12(14) . . ? C25 Zr1 C22 130.79(14) . . ? C20 Zr1 C22 54.06(14) . . ? Cl1A C52A Cl2A 112.0(5) . . ? Cl1A C52A H52A 109.2 . . ? Cl2A C52A H52A 109.2 . . ? Cl1A C52A H52B 109.2 . . ? Cl2A C52A H52B 109.2 . . ? H52A C52A H52B 107.9 . . ? Cl1B C52B Cl2B 103.7(13) . . ? Cl1B C52B H52C 111.0 . . ? Cl2B C52B H52C 111.0 . . ? Cl1B C52B H52D 111.0 . . ? Cl2B C52B H52D 111.0 . . ? H52C C52B H52D 109.0 . . ? _refine_diff_density_max 0.782 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.070 _shelxl_version_number 2013-4 _shelx_res_file ; TITL MM1510_0m in P-1 CELL 1.54178 12.6013 14.2473 15.7688 63.993 86.318 80.980 ZERR 1.00 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N B F Cl Zr UNIT 106 54 2 2 40 8 2 L.S. 4 ACTA 135 BOND $H OMIT -4 135 FMAP 2 PLAN -5 SIMU 0.01 CL1A CL1B CL2A CL2B SIMU 0.02 C52A C52B DELU 0.02 C52A C52B ISOR 0.02 C52A C52B DFIX 1.76 C52B CL2B SIZE 0.070 0.080 0.120 TEMP -99.950 WGHT 0.071100 FVAR 0.11623 0.72981 B1 4 0.812468 0.029029 0.731852 11.00000 0.03597 0.02936 = 0.02930 -0.01023 0.00086 -0.00582 C1 1 0.801737 0.535942 0.668044 11.00000 0.03154 0.03196 = 0.03752 -0.01691 0.00464 -0.01031 C2 1 0.901113 0.479839 0.674474 11.00000 0.03055 0.02776 = 0.03208 -0.01141 0.00214 -0.00732 C3 1 0.955326 0.485536 0.587025 11.00000 0.02714 0.02566 = 0.03195 -0.01052 0.00015 -0.00746 C4 1 0.946546 0.573617 0.420171 11.00000 0.02868 0.02809 = 0.03117 -0.01148 0.00021 -0.00724 C5 1 0.881357 0.656786 0.337678 11.00000 0.03178 0.03936 = 0.03567 -0.01307 -0.00093 0.00427 AFIX 137 H5A 2 0.821086 0.691958 0.360454 11.00000 -1.50000 H5B 2 0.853696 0.623917 0.302173 11.00000 -1.50000 H5C 2 0.926711 0.708803 0.296526 11.00000 -1.50000 AFIX 0 C6 1 0.957273 0.417695 0.767967 11.00000 0.03284 0.04036 = 0.03050 -0.01350 0.00292 -0.00094 C7 1 0.933080 0.318495 0.828746 11.00000 0.04091 0.05328 = 0.04639 -0.00456 0.00603 -0.00775 AFIX 43 H7 2 0.882503 0.287676 0.810583 11.00000 -1.20000 AFIX 0 C8 1 0.982999 0.264587 0.916033 11.00000 0.05477 0.07362 = 0.04752 0.01207 0.00730 -0.00702 AFIX 43 H8 2 0.967638 0.195919 0.957233 11.00000 -1.20000 AFIX 0 C9 1 1.054417 0.309272 0.943672 11.00000 0.04519 0.11931 = 0.03224 -0.00748 -0.00509 0.00811 AFIX 43 H9 2 1.087659 0.271709 1.004052 11.00000 -1.20000 AFIX 0 C10 1 1.078375 0.408974 0.883975 11.00000 0.05218 0.09376 = 0.04703 -0.03806 -0.00865 0.00054 AFIX 43 H10 2 1.127438 0.440227 0.903278 11.00000 -1.20000 AFIX 0 C11 1 1.030191 0.462306 0.796237 11.00000 0.04591 0.05346 = 0.04381 -0.02281 0.00000 -0.00590 AFIX 43 H11 2 1.047026 0.530283 0.754666 11.00000 -1.20000 AFIX 0 C12 1 0.749478 0.535696 0.755639 11.00000 0.03550 0.03460 = 0.03746 -0.01607 0.00303 -0.00345 C13 1 0.788282 0.586585 0.803180 11.00000 0.04373 0.04644 = 0.04392 -0.02258 0.00590 -0.00803 AFIX 43 H13 2 0.849322 0.621701 0.779155 11.00000 -1.20000 AFIX 0 C14 1 0.739932 0.586904 0.884075 11.00000 0.06532 0.05507 = 0.04654 -0.02884 0.00698 -0.00420 AFIX 43 H14 2 0.767677 0.622229 0.914863 11.00000 -1.20000 AFIX 0 C15 1 0.651643 0.536231 0.920341 11.00000 0.07174 0.05535 = 0.04620 -0.02428 0.02084 -0.00333 AFIX 43 H15 2 0.618241 0.536613 0.975962 11.00000 -1.20000 AFIX 0 C16 1 0.612386 0.485402 0.875827 11.00000 0.04851 0.05432 = 0.05791 -0.02003 0.01847 -0.00941 AFIX 43 H16 2 0.552137 0.449477 0.901401 11.00000 -1.20000 AFIX 0 C17 1 0.659465 0.485522 0.793482 11.00000 0.04088 0.04115 = 0.05190 -0.01926 0.00817 -0.00763 AFIX 43 H17 2 0.630007 0.451088 0.762729 11.00000 -1.20000 AFIX 0 C18 1 0.821228 0.805609 0.466392 11.00000 0.05035 0.03278 = 0.06135 -0.02058 0.00885 -0.00877 AFIX 43 H18 2 0.886940 0.810027 0.432694 11.00000 -1.20000 AFIX 0 C19 1 0.718634 0.836842 0.426399 11.00000 0.05709 0.03382 = 0.05318 -0.01225 -0.00007 -0.00096 AFIX 43 H19 2 0.702311 0.865053 0.361098 11.00000 -1.20000 AFIX 0 C20 1 0.643435 0.819113 0.500103 11.00000 0.04692 0.03283 = 0.07045 -0.02104 0.00382 0.00471 AFIX 43 H20 2 0.567481 0.834619 0.493293 11.00000 -1.20000 AFIX 0 C21 1 0.700739 0.774698 0.584796 11.00000 0.06576 0.03207 = 0.05442 -0.02329 0.00986 -0.00127 AFIX 43 H21 2 0.670129 0.753469 0.645922 11.00000 -1.20000 AFIX 0 C22 1 0.811192 0.766503 0.564870 11.00000 0.05501 0.03536 = 0.06476 -0.02736 -0.00351 -0.00725 AFIX 43 H22 2 0.868300 0.739611 0.609523 11.00000 -1.20000 AFIX 0 C23 1 0.679472 0.514771 0.468914 11.00000 0.04273 0.06337 = 0.06904 -0.04442 0.00299 -0.01483 AFIX 43 H23 2 0.732473 0.477249 0.445225 11.00000 -1.20000 AFIX 0 C24 1 0.618272 0.613673 0.414745 11.00000 0.04594 0.07363 = 0.05093 -0.02610 -0.00651 -0.02099 AFIX 43 H24 2 0.623024 0.654589 0.348540 11.00000 -1.20000 AFIX 0 C25 1 0.549463 0.640218 0.476502 11.00000 0.03324 0.05779 = 0.06714 -0.02451 -0.01011 -0.00343 AFIX 43 H25 2 0.498316 0.702174 0.459408 11.00000 -1.20000 AFIX 0 C26 1 0.568922 0.559882 0.567691 11.00000 0.03033 0.05970 = 0.05687 -0.02736 0.00243 -0.01355 AFIX 43 H26 2 0.534040 0.558408 0.623401 11.00000 -1.20000 AFIX 0 C27 1 0.648822 0.481687 0.562974 11.00000 0.03501 0.04404 = 0.06327 -0.02293 -0.00473 -0.01213 AFIX 43 H27 2 0.676904 0.417786 0.614577 11.00000 -1.20000 AFIX 0 C28 1 0.836527 0.102629 0.619535 11.00000 0.02804 0.03155 = 0.03045 -0.01222 -0.00081 -0.00525 C29 1 0.852566 0.207422 0.578472 11.00000 0.03121 0.03426 = 0.03591 -0.01872 -0.00321 -0.00340 C30 1 0.884135 0.259665 0.485640 11.00000 0.03530 0.02947 = 0.03517 -0.01031 -0.00128 -0.00693 C31 1 0.901676 0.208264 0.428919 11.00000 0.03972 0.04022 = 0.02880 -0.01196 0.00217 -0.00994 C32 1 0.887210 0.103464 0.466143 11.00000 0.04056 0.03881 = 0.03434 -0.02023 -0.00295 -0.00215 C33 1 0.857397 0.054305 0.559387 11.00000 0.03446 0.02874 = 0.03576 -0.01340 -0.00236 -0.00332 C34 1 0.929699 -0.045404 0.768816 11.00000 0.03094 0.03632 = 0.02678 -0.01482 0.00046 -0.00417 C35 1 1.017807 0.003013 0.767200 11.00000 0.03952 0.04218 = 0.02747 -0.01310 0.00275 -0.00880 C36 1 1.121139 -0.048093 0.791246 11.00000 0.03289 0.05808 = 0.03193 -0.01853 0.00136 -0.01276 C37 1 1.141384 -0.155527 0.821274 11.00000 0.03241 0.06083 = 0.03126 -0.02227 0.00136 0.00122 C38 1 1.057509 -0.208335 0.824241 11.00000 0.04128 0.04136 = 0.03216 -0.01673 0.00158 0.00270 C39 1 0.955519 -0.152679 0.795881 11.00000 0.03474 0.03825 = 0.02760 -0.01417 0.00184 -0.00658 C40 1 0.770274 0.096332 0.792876 11.00000 0.03463 0.03195 = 0.03285 -0.01445 0.00487 -0.00902 C41 1 0.679273 0.172264 0.762764 11.00000 0.03848 0.03656 = 0.03934 -0.01760 0.00267 -0.00953 C42 1 0.627147 0.222069 0.814391 11.00000 0.03641 0.03916 = 0.05423 -0.02350 0.00724 -0.00691 C43 1 0.665029 0.197649 0.902618 11.00000 0.05215 0.04621 = 0.05150 -0.02992 0.02174 -0.01578 C44 1 0.755985 0.124280 0.935882 11.00000 0.05668 0.04901 = 0.03457 -0.02207 0.00863 -0.01866 C45 1 0.805923 0.075828 0.881827 11.00000 0.04144 0.03371 = 0.03513 -0.01465 0.00434 -0.00829 C46 1 0.711195 -0.038830 0.746609 11.00000 0.03100 0.03232 = 0.04154 -0.01817 0.00246 -0.00350 C47 1 0.634121 -0.022863 0.680285 11.00000 0.03592 0.03762 = 0.04626 -0.02037 -0.00224 -0.00214 C48 1 0.549109 -0.079759 0.699854 11.00000 0.02906 0.05121 = 0.06611 -0.03414 -0.00475 -0.00170 C49 1 0.536522 -0.156276 0.790057 11.00000 0.03254 0.05020 = 0.07213 -0.03507 0.01389 -0.01438 C50 1 0.607924 -0.172745 0.859431 11.00000 0.03790 0.03751 = 0.05152 -0.01846 0.01444 -0.00952 C51 1 0.691301 -0.114127 0.836489 11.00000 0.03409 0.03659 = 0.04004 -0.01852 0.00274 -0.00206 C70 1 0.654190 0.372640 0.239302 11.00000 0.09869 0.10808 = 0.11795 -0.08430 -0.00761 0.01104 AFIX 23 H70A 2 0.721311 0.349621 0.213134 11.00000 -1.20000 H70B 2 0.593566 0.375509 0.200890 11.00000 -1.20000 AFIX 0 CL4 6 0.639489 0.278710 0.355691 11.00000 0.07576 0.11958 = 0.13150 -0.07077 -0.02367 0.01830 CL3 6 0.658169 0.498020 0.229114 11.00000 0.09115 0.13443 = 0.17312 -0.11368 0.03823 -0.04673 F1 5 0.839106 0.265957 0.627330 11.00000 0.05125 0.03377 = 0.03797 -0.02014 0.00369 -0.00927 F2 5 0.898569 0.361930 0.449589 11.00000 0.05789 0.03295 = 0.04217 -0.01303 0.00414 -0.01590 F3 5 0.931166 0.259553 0.339225 11.00000 0.06800 0.04705 = 0.03263 -0.01528 0.01046 -0.01667 F4 5 0.902887 0.051828 0.412210 11.00000 0.06360 0.04683 = 0.03730 -0.02556 0.00580 -0.00948 F5 5 0.849859 -0.049634 0.592435 11.00000 0.05549 0.02998 = 0.03869 -0.01660 0.00503 -0.01010 F6 5 1.003974 0.108760 0.740342 11.00000 0.04591 0.03904 = 0.04429 -0.01478 -0.00247 -0.01457 F7 5 1.201665 0.005692 0.785679 11.00000 0.04016 0.07259 = 0.04477 -0.02129 0.00160 -0.02186 F8 5 1.239994 -0.208242 0.846923 11.00000 0.03389 0.07897 = 0.06254 -0.03701 -0.00667 0.00779 F9 5 1.076129 -0.313095 0.851724 11.00000 0.05353 0.04144 = 0.04556 -0.01845 -0.00552 0.01045 F10 5 0.881125 -0.211253 0.796156 11.00000 0.04124 0.03260 = 0.04746 -0.01758 0.00064 -0.00627 F11 5 0.634381 0.197983 0.678324 11.00000 0.03997 0.04715 = 0.04637 -0.02165 -0.00852 0.00189 F12 5 0.538819 0.293368 0.780517 11.00000 0.04317 0.05548 = 0.08116 -0.03946 0.00325 0.00236 F13 5 0.614475 0.242116 0.955640 11.00000 0.07403 0.06677 = 0.06700 -0.04632 0.02574 -0.01282 F14 5 0.794512 0.098368 1.021711 11.00000 0.08236 0.06724 = 0.03768 -0.03032 0.00436 -0.01654 F15 5 0.893110 0.003545 0.922045 11.00000 0.05181 0.05027 = 0.03546 -0.01815 -0.00653 -0.00166 F16 5 0.637641 0.052023 0.590696 11.00000 0.04676 0.04825 = 0.04427 -0.01619 -0.01029 -0.00926 F17 5 0.479527 -0.061187 0.631587 11.00000 0.04271 0.07089 = 0.08516 -0.04037 -0.01542 -0.01083 F18 5 0.454999 -0.212805 0.810334 11.00000 0.04397 0.07787 = 0.10178 -0.04843 0.01887 -0.03151 F19 5 0.595260 -0.244220 0.948473 11.00000 0.05750 0.05260 = 0.05685 -0.02187 0.02516 -0.02161 F20 5 0.757043 -0.133734 0.908339 11.00000 0.04379 0.04264 = 0.03490 -0.01268 0.00334 -0.00974 N1 3 0.905176 0.557108 0.505196 11.00000 0.02698 0.02729 = 0.03113 -0.01288 0.00057 -0.00507 ZR1 7 0.736585 0.642317 0.518886 11.00000 0.02600 0.02902 = 0.03685 -0.01405 0.00013 -0.00186 PART 1 21 C52A 1 0.623991 0.890775 0.076792 21.00000 0.06430 0.04807 = 0.05471 -0.02190 0.00271 -0.00221 AFIX 23 H52A 2 0.574156 0.856448 0.057348 21.00000 -1.20000 H52B 2 0.660994 0.936435 0.019624 21.00000 -1.20000 AFIX 0 CL1A 6 0.718061 0.795007 0.154658 21.00000 0.09694 0.11004 = 0.09567 -0.04215 -0.03638 0.04155 CL2A 6 0.550729 0.968249 0.126308 21.00000 0.06434 0.07544 = 0.10420 -0.05930 0.01953 -0.00588 PART 2 -21 CL1B 6 0.691722 0.760251 0.145013 -21.00000 0.08759 0.07286 = 0.04916 -0.01760 0.01307 0.00868 C52B 1 0.665383 0.901082 0.097043 -21.00000 0.07562 0.07813 = 0.05873 -0.04427 0.00680 -0.02251 AFIX 23 H52C 2 0.632393 0.931802 0.033506 -21.00000 -1.20000 H52D 2 0.732235 0.931262 0.092793 -21.00000 -1.20000 AFIX 0 CL2B 6 0.573298 0.924968 0.179998 -21.00000 0.09699 0.14154 = 0.17810 -0.11468 0.02646 -0.04186 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM MM1510_0m in P-1 REM R1 = 0.0416 for 7160 Fo > 4sig(Fo) and 0.0548 for all 8791 data REM 750 parameters refined using 31 restraints END WGHT 0.0643 0.4463 REM Highest difference peak 0.782, deepest hole -0.448, 1-sigma level 0.070 Q1 1 0.5625 0.9607 0.0217 11.00000 0.05 0.78 Q2 1 0.7120 0.4499 0.2475 11.00000 0.05 0.60 Q3 1 0.6794 0.3345 0.3327 11.00000 0.05 0.58 Q4 1 0.7230 0.5841 0.5714 11.00000 0.05 0.55 Q5 1 0.6262 0.8497 0.2224 11.00000 0.05 0.53 ; _shelx_res_checksum 28955 _shelx_hkl_file ; -1 0 0 22.53 0.73 1 0 0 22.20 0.73 1 0 0 22.59 0.78 -2 0 0 98.11 3.00 2 0 0 104.38 3.07 2 0 0 101.66 2.92 -3 0 0 79.21 2.54 3 0 0 80.53 2.51 3 0 0 83.31 2.72 -4 0 0 102.60 3.26 4 0 0 104.72 3.27 4 0 0 106.02 3.51 -5 0 0 38.25 1.53 5 0 0 41.69 1.72 -6 0 0 44.05 2.51 6 0 0 42.27 1.88 -7 0 0 12.22 1.60 7 0 0 14.87 1.15 -8 0 0 26.96 2.37 8 0 0 25.63 1.67 -9 0 0 -0.15 0.96 9 0 0 0.28 0.62 9 0 0 0.43 0.27 9 0 0 0.00 0.32 10 0 0 27.53 1.21 10 0 0 29.98 1.15 11 0 0 35.28 1.36 11 0 0 36.05 1.45 12 0 0 0.90 0.36 12 0 0 0.36 0.39 13 0 0 3.46 0.48 13 0 0 2.93 0.49 14 0 0 2.23 0.39 15 0 0 3.19 0.40 14 -1 0 1.86 0.36 13 -1 0 13.47 0.78 13 -1 0 13.27 0.81 12 -1 0 -0.06 0.35 12 -1 0 -0.28 0.30 11 -1 0 0.52 0.33 11 -1 0 0.18 0.33 10 -1 0 3.70 0.53 10 -1 0 3.72 0.47 9 -1 0 2.26 0.35 9 -1 0 2.01 0.43 -9 1 0 1.57 1.12 8 -1 0 56.86 2.60 -8 1 0 52.59 3.40 7 -1 0 0.53 0.47 -7 1 0 -0.55 0.69 6 -1 0 1.77 0.52 6 -1 0 1.07 0.58 5 -1 0 175.71 5.26 5 -1 0 174.49 5.71 -5 1 0 179.52 5.60 4 -1 0 0.91 0.47 4 -1 0 1.16 0.38 -4 1 0 1.01 0.40 3 -1 0 975.01 25.62 3 -1 0 1000.00 26.57 -3 1 0 928.47 27.28 2 -1 0 21.89 0.82 2 -1 0 22.70 1.02 -2 1 0 21.00 1.02 1 -1 0 12.91 0.46 1 -1 0 14.09 0.65 0 -1 0 49.24 1.43 0 -1 0 45.48 1.44 0 1 0 45.28 1.27 -1 -1 0 2.78 0.35 1 1 0 3.14 0.29 1 1 0 2.85 0.23 -2 -1 0 80.27 2.61 2 1 0 79.96 2.41 -3 -1 0 0.39 0.42 3 1 0 0.13 0.28 -4 -1 0 2.58 0.65 4 1 0 2.03 0.45 -5 -1 0 26.58 1.72 5 1 0 29.60 1.42 -6 -1 0 143.74 5.36 6 1 0 149.42 4.73 -7 -1 0 45.58 2.80 7 1 0 47.69 2.17 -8 -1 0 60.43 3.43 8 1 0 66.25 2.80 -9 -1 0 19.18 2.22 9 1 0 15.95 1.51 9 1 0 14.24 0.81 9 1 0 14.37 0.74 10 1 0 13.72 0.79 10 1 0 13.78 0.85 10 1 0 14.62 0.88 11 1 0 -0.29 0.31 11 1 0 0.10 0.34 11 1 0 0.09 0.37 12 1 0 26.03 1.12 12 1 0 23.25 1.12 12 1 0 21.85 1.15 13 1 0 5.08 0.60 13 1 0 5.92 0.64 14 1 0 15.24 0.81 15 1 0 0.28 0.28 14 -2 0 7.95 0.57 14 -2 0 7.11 0.54 13 -2 0 5.88 0.54 13 -2 0 6.49 0.61 12 -2 0 4.41 0.57 12 -2 0 5.29 0.58 11 -2 0 2.56 0.50 11 -2 0 1.59 0.38 10 -2 0 7.46 0.70 10 -2 0 7.79 0.60 10 -2 0 6.30 0.68 9 -2 0 -0.04 0.34 9 -2 0 0.58 0.27 9 -2 0 0.12 0.32 -9 2 0 0.17 1.11 -8 2 0 7.20 1.54 7 -2 0 14.63 1.47 6 -2 0 15.94 1.11 6 -2 0 16.20 1.40 -6 2 0 17.13 1.34 5 -2 0 3.91 0.59 5 -2 0 3.63 0.78 -5 2 0 4.64 0.75 4 -2 0 19.18 1.28 4 -2 0 20.04 0.96 -4 2 0 18.71 1.24 3 -2 0 50.55 1.69 3 -2 0 52.47 2.09 -3 2 0 51.90 2.12 2 -2 0 43.77 1.68 2 -2 0 38.92 1.28 -2 2 0 40.55 1.75 1 -2 0 106.64 3.13 -1 2 0 95.61 2.73 -1 2 0 99.60 3.27 0 -2 0 1.11 0.32 0 2 0 0.57 0.30 0 2 0 0.73 0.15 -1 -2 0 229.36 6.31 1 2 0 211.78 6.39 1 2 0 219.04 5.98 -2 -2 0 80.06 2.61 2 2 0 79.15 2.40 2 2 0 73.10 2.34 -3 -2 0 131.58 4.21 3 2 0 128.85 3.89 -4 -2 0 8.58 0.99 4 2 0 7.86 0.72 -5 -2 0 28.16 1.76 5 2 0 29.61 1.45 -6 -2 0 16.82 1.56 6 2 0 15.66 1.14 -7 -2 0 93.49 4.12 7 2 0 95.78 3.53 -8 -2 0 3.58 1.12 8 2 0 2.32 0.65 -9 -2 0 64.23 3.72 9 2 0 66.53 2.08 9 2 0 71.07 3.09 9 2 0 64.71 2.00 10 2 0 0.73 0.37 10 2 0 0.29 0.31 10 2 0 1.22 0.37 11 2 0 4.96 0.59 11 2 0 4.35 0.61 11 2 0 3.48 0.51 12 2 0 5.10 0.63 12 2 0 4.66 0.63 12 2 0 5.46 0.69 13 2 0 0.47 0.34 13 2 0 -0.20 0.33 14 2 0 4.40 0.51 14 2 0 3.26 0.46 15 2 0 0.81 0.32 14 -3 0 0.39 0.28 14 -3 0 0.85 0.31 13 -3 0 4.30 0.50 13 -3 0 5.94 0.56 12 -3 0 2.54 0.48 12 -3 0 2.06 0.39 11 -3 0 0.65 0.37 11 -3 0 0.87 0.43 11 -3 0 1.10 0.37 10 -3 0 11.43 0.71 10 -3 0 10.42 0.79 10 -3 0 9.12 0.78 9 -3 0 2.28 0.44 9 -3 0 1.54 0.41 9 -3 0 1.88 0.37 8 -3 0 1.74 0.79 8 -3 0 2.50 0.37 8 -3 0 2.27 0.42 8 -3 0 2.36 0.46 7 -3 0 1.37 0.76 6 -3 0 30.64 1.99 -6 3 0 37.02 2.08 5 -3 0 10.55 1.18 -5 3 0 10.18 1.14 4 -3 0 26.01 1.59 4 -3 0 26.66 1.16 -4 3 0 28.63 1.69 3 -3 0 18.34 0.82 3 -3 0 17.78 1.21 -3 3 0 18.57 1.29 2 -3 0 4.26 0.68 -2 3 0 4.39 0.38 -2 3 0 3.52 0.69 1 -3 0 241.82 7.06 -1 3 0 239.88 7.38 0 -3 0 22.82 1.12 0 3 0 20.02 0.73 0 3 0 21.38 1.18 -1 -3 0 10.91 0.80 1 3 0 8.33 0.54 1 3 0 9.28 0.76 -2 -3 0 155.99 4.69 2 3 0 149.32 4.59 2 3 0 148.50 4.35 -3 -3 0 314.20 9.05 3 3 0 292.25 8.78 3 3 0 318.99 8.60 -4 -3 0 5.17 0.83 4 3 0 5.49 0.68 -5 -3 0 167.91 5.67 5 3 0 168.31 5.19 -6 -3 0 62.34 2.95 6 3 0 63.46 2.52 -7 -3 0 10.32 1.41 7 3 0 12.31 1.13 -8 -3 0 0.09 0.79 8 3 0 0.73 0.50 -9 -3 0 48.82 3.13 9 3 0 49.24 1.64 9 3 0 55.44 2.60 9 3 0 47.35 1.67 10 3 0 7.60 0.64 10 3 0 8.12 0.73 10 3 0 7.60 0.66 11 3 0 66.03 2.15 11 3 0 60.19 2.05 12 3 0 -0.02 0.36 12 3 0 1.24 0.38 13 3 0 0.93 0.40 13 3 0 1.51 0.35 14 3 0 -0.27 0.32 14 3 0 0.36 0.30 -15 -3 0 6.91 0.49 15 3 0 7.46 0.57 15 3 0 6.23 0.48 13 -4 0 -0.28 0.28 13 -4 0 0.31 0.31 12 -4 0 3.64 0.49 12 -4 0 3.66 0.49 11 -4 0 6.70 0.70 11 -4 0 9.43 0.67 11 -4 0 8.06 0.71 10 -4 0 5.02 0.68 10 -4 0 5.91 0.58 10 -4 0 6.22 0.68 9 -4 0 19.19 0.89 9 -4 0 16.93 0.97 9 -4 0 18.16 0.98 8 -4 0 0.13 0.33 8 -4 0 0.38 0.29 8 -4 0 0.18 0.31 8 -4 0 -0.13 0.73 7 -4 0 19.74 1.77 6 -4 0 24.23 1.83 -6 4 0 27.49 1.97 5 -4 0 5.87 0.98 -5 4 0 10.09 1.24 4 -4 0 179.22 5.89 -4 4 0 172.92 6.13 3 -4 0 0.70 0.52 -3 4 0 -0.11 0.52 2 -4 0 1.27 0.51 -2 4 0 0.91 0.57 1 -4 0 83.51 2.96 -1 4 0 79.91 3.15 0 -4 0 132.93 4.21 0 4 0 131.56 4.41 0 4 0 128.29 3.61 -1 -4 0 26.75 1.35 1 4 0 23.26 0.98 1 4 0 26.54 1.38 -2 -4 0 264.05 7.59 2 4 0 251.81 7.62 2 4 0 244.97 7.06 -3 -4 0 42.07 1.94 3 4 0 40.83 1.64 3 4 0 45.94 1.71 -4 -4 0 290.52 8.95 4 4 0 299.37 8.45 -5 -4 0 0.00 0.52 5 4 0 0.58 0.44 -6 -4 0 100.49 4.04 6 4 0 98.38 3.55 -7 -4 0 33.65 2.21 7 4 0 31.89 1.80 -8 -4 0 59.85 3.29 8 4 0 62.10 2.78 -9 -4 0 -0.61 0.68 9 4 0 0.26 0.49 9 4 0 0.20 0.34 10 4 0 1.23 0.36 10 4 0 1.56 0.42 11 4 0 4.08 0.56 11 4 0 3.19 0.50 12 4 0 5.96 0.62 12 4 0 5.61 0.65 13 4 0 1.50 0.43 13 4 0 0.89 0.34 -14 -4 0 0.60 0.35 14 4 0 0.66 0.37 14 4 0 1.45 0.34 -15 -4 0 1.17 0.32 15 4 0 0.99 0.25 13 -5 0 4.36 0.46 12 -5 0 9.93 0.64 12 -5 0 8.64 0.68 12 -5 0 10.16 0.67 11 -5 0 1.83 0.44 11 -5 0 2.61 0.43 11 -5 0 2.52 0.45 10 -5 0 12.42 0.75 10 -5 0 12.90 0.87 10 -5 0 12.09 0.83 9 -5 0 50.49 1.61 9 -5 0 47.48 1.75 9 -5 0 46.64 1.69 8 -5 0 0.02 0.28 8 -5 0 0.00 0.33 8 -5 0 0.29 0.33 8 -5 0 0.26 0.33 7 -5 0 44.50 2.77 7 -5 0 44.59 1.58 7 -5 0 45.54 1.46 7 -5 0 43.67 1.57 6 -5 0 13.84 1.50 -6 5 0 13.31 1.66 5 -5 0 16.94 1.56 -5 5 0 18.86 1.75 4 -5 0 2.98 0.82 -4 5 0 2.34 0.82 3 -5 0 3.76 0.80 -3 5 0 2.65 0.85 2 -5 0 2.10 0.65 -2 5 0 1.78 0.73 1 -5 0 70.03 2.77 -1 5 0 67.59 2.96 0 -5 0 10.27 1.05 0 5 0 10.87 0.52 0 5 0 12.53 1.20 -1 -5 0 59.05 2.37 1 5 0 54.74 1.84 1 5 0 57.75 2.44 -2 -5 0 24.10 1.47 2 5 0 25.23 1.43 2 5 0 25.29 1.13 -3 -5 0 21.35 1.39 3 5 0 20.19 1.21 3 5 0 20.93 1.12 -4 -5 0 1.49 0.59 4 5 0 1.18 0.50 -5 -5 0 0.96 0.58 5 5 0 2.67 0.59 -6 -5 0 19.59 1.59 6 5 0 17.99 1.29 -7 -5 0 4.08 0.92 7 5 0 4.00 0.77 -8 -5 0 7.17 1.31 8 5 0 7.61 1.16 -9 -5 0 32.31 2.56 9 5 0 29.88 1.23 9 5 0 28.33 1.20 9 5 0 29.72 2.00 10 5 0 14.81 0.85 10 5 0 14.17 0.91 11 5 0 0.95 0.41 11 5 0 1.21 0.38 12 5 0 0.40 0.32 12 5 0 0.24 0.38 -13 -5 0 0.60 0.38 13 5 0 -0.18 0.25 13 5 0 0.19 0.41 -14 -5 0 6.12 0.59 14 5 0 6.43 0.64 14 5 0 8.08 0.57 15 5 0 0.80 0.24 12 -6 0 5.96 0.57 12 -6 0 6.98 0.56 11 -6 0 0.02 0.33 11 -6 0 0.18 0.34 10 -6 0 20.79 1.07 10 -6 0 24.48 1.10 9 -6 0 0.63 0.39 9 -6 0 0.24 0.36 9 -6 0 0.35 0.33 8 -6 0 24.13 1.12 8 -6 0 26.85 1.17 8 -6 0 25.55 1.19 8 -6 0 23.47 1.28 7 -6 0 0.59 0.38 7 -6 0 1.06 0.37 7 -6 0 0.37 0.41 7 -6 0 0.94 0.34 6 -6 0 34.95 1.36 6 -6 0 36.36 1.38 6 -6 0 39.35 2.50 -6 6 0 34.84 2.73 5 -6 0 -0.32 0.61 -5 6 0 0.37 0.77 4 -6 0 0.58 0.66 -4 6 0 4.18 1.03 3 -6 0 0.19 0.53 -3 6 0 1.44 0.74 2 -6 0 17.72 1.46 -2 6 0 15.97 1.57 1 -6 0 14.30 1.28 -1 6 0 15.15 1.48 0 -6 0 2.80 0.79 0 6 0 3.39 0.87 -1 -6 0 46.77 2.24 1 6 0 49.41 2.40 -2 -6 0 19.92 1.39 2 6 0 17.86 0.98 2 6 0 18.64 1.34 -3 -6 0 104.73 3.91 3 6 0 102.22 3.75 3 6 0 106.49 3.42 -4 -6 0 10.08 1.13 4 6 0 11.41 0.93 -5 -6 0 62.78 2.97 5 6 0 63.86 2.57 -6 -6 0 8.45 1.19 6 6 0 8.76 1.02 -7 -6 0 0.58 0.61 7 6 0 0.52 0.57 -8 -6 0 6.32 1.22 8 6 0 6.99 0.81 8 6 0 7.68 1.16 9 6 0 0.99 0.44 9 6 0 0.46 0.29 10 6 0 0.58 0.44 10 6 0 -0.33 0.28 11 6 0 13.39 0.95 11 6 0 13.03 0.82 -12 -6 0 1.01 0.43 12 6 0 0.25 0.44 12 6 0 0.60 0.35 -13 -6 0 4.57 0.61 13 6 0 4.66 0.51 13 6 0 5.96 0.69 -14 -6 0 -0.03 0.30 14 6 0 -0.02 0.25 14 6 0 0.06 0.42 15 6 0 3.00 0.33 12 -7 0 -0.14 0.27 11 -7 0 4.44 0.53 11 -7 0 3.47 0.46 10 -7 0 1.92 0.43 10 -7 0 2.29 0.46 9 -7 0 6.44 0.67 9 -7 0 6.94 0.66 9 -7 0 6.75 0.69 8 -7 0 5.77 0.65 8 -7 0 4.97 0.64 8 -7 0 5.50 0.74 8 -7 0 4.90 0.67 7 -7 0 3.33 0.51 7 -7 0 3.59 0.54 7 -7 0 3.38 0.48 7 -7 0 3.86 0.63 6 -7 0 7.77 0.79 6 -7 0 6.31 0.68 6 -7 0 5.71 0.60 6 -7 0 6.13 0.65 6 -7 0 6.31 0.77 -6 7 0 6.55 1.51 5 -7 0 17.51 0.90 5 -7 0 18.08 1.00 5 -7 0 15.04 1.75 5 -7 0 15.96 0.93 -5 7 0 16.01 2.06 4 -7 0 8.24 1.30 -4 7 0 6.73 1.37 3 -7 0 2.75 0.83 -3 7 0 2.37 0.94 2 -7 0 85.14 3.70 -2 7 0 90.30 4.03 1 -7 0 27.79 1.87 -1 7 0 30.74 2.12 0 -7 0 133.97 4.86 0 7 0 129.35 5.05 -1 -7 0 3.74 0.82 1 7 0 3.41 0.85 -2 -7 0 19.32 1.49 2 7 0 16.44 1.45 -3 -7 0 0.46 0.53 -4 -7 0 24.69 1.78 4 7 0 28.14 1.51 -5 -7 0 15.57 1.46 5 7 0 13.56 1.17 -6 -7 0 2.72 0.91 6 7 0 2.99 0.81 -7 -7 0 9.74 1.46 7 7 0 6.31 1.08 -8 -7 0 25.55 1.25 8 7 0 25.58 1.11 8 7 0 26.24 2.09 -9 -7 0 -0.09 0.36 9 7 0 0.15 0.28 -10 -7 0 6.81 0.78 10 7 0 6.85 0.63 -11 -7 0 10.47 0.86 11 7 0 10.56 0.75 -12 -7 0 3.03 0.53 12 7 0 3.47 0.47 -13 -7 0 8.37 0.68 13 7 0 8.97 0.63 -14 -7 0 0.65 0.28 -14 -7 0 0.40 0.27 14 7 0 0.38 0.25 11 -8 0 0.65 0.32 11 -8 0 0.54 0.29 10 -8 0 1.22 0.34 10 -8 0 1.20 0.37 10 -8 0 0.66 0.34 9 -8 0 2.52 0.42 9 -8 0 2.03 0.44 9 -8 0 2.90 0.47 8 -8 0 0.33 0.45 8 -8 0 0.35 0.33 8 -8 0 0.13 0.36 8 -8 0 -0.14 0.35 7 -8 0 10.33 0.93 7 -8 0 10.49 0.74 7 -8 0 9.49 0.86 7 -8 0 11.12 0.85 7 -8 0 9.49 0.79 6 -8 0 4.69 0.59 6 -8 0 4.86 0.62 6 -8 0 4.18 0.55 6 -8 0 3.38 0.60 6 -8 0 4.98 0.65 5 -8 0 1.55 0.48 5 -8 0 1.07 0.43 5 -8 0 0.67 0.40 5 -8 0 0.74 0.35 5 -8 0 0.84 0.33 4 -8 0 1.54 0.43 4 -8 0 1.59 0.49 4 -8 0 1.71 0.39 4 -8 0 -0.70 0.75 -4 8 0 -0.17 0.99 3 -8 0 37.11 1.49 3 -8 0 38.39 1.39 3 -8 0 38.34 1.46 3 -8 0 38.30 2.54 -3 8 0 37.65 2.73 2 -8 0 18.43 1.71 -2 8 0 17.39 1.94 1 -8 0 3.36 0.89 -1 8 0 3.85 1.06 0 -8 0 8.03 1.19 0 8 0 5.62 1.19 -1 -8 0 3.62 0.90 1 8 0 1.80 0.80 -2 -8 0 26.45 1.87 2 8 0 28.94 1.97 -3 -8 0 -0.72 0.50 -4 -8 0 23.02 1.78 -5 -8 0 1.86 0.74 -6 -8 0 27.31 1.13 -6 -8 0 25.85 2.10 -7 -8 0 0.23 0.36 7 8 0 1.09 0.77 -8 -8 0 42.60 1.71 8 8 0 41.16 1.52 -9 -8 0 0.95 0.44 9 8 0 1.22 0.37 -10 -8 0 -0.30 0.38 10 8 0 0.71 0.34 -11 -8 0 0.48 0.39 11 8 0 0.40 0.31 -12 -8 0 13.93 0.81 -12 -8 0 14.86 0.87 12 8 0 12.82 0.77 -13 -8 0 -0.46 0.27 -13 -8 0 0.09 0.28 13 8 0 -0.03 0.26 14 8 0 12.60 0.63 10 -9 0 0.13 0.28 10 -9 0 0.36 0.31 10 -9 0 0.07 0.24 9 -9 0 8.16 0.66 9 -9 0 8.93 0.65 9 -9 0 8.51 0.66 8 -9 0 1.92 0.43 8 -9 0 1.89 0.41 8 -9 0 2.73 0.48 7 -9 0 -0.28 0.31 7 -9 0 -0.03 0.40 7 -9 0 -0.18 0.29 7 -9 0 -0.43 0.41 7 -9 0 0.13 0.38 6 -9 0 14.74 0.96 6 -9 0 12.61 0.83 6 -9 0 12.77 0.91 6 -9 0 12.80 0.99 6 -9 0 13.40 0.86 5 -9 0 28.33 1.31 5 -9 0 27.02 1.20 5 -9 0 25.80 1.36 5 -9 0 29.02 1.26 5 -9 0 28.35 1.23 4 -9 0 8.75 0.82 4 -9 0 7.86 0.80 4 -9 0 8.93 0.67 4 -9 0 8.20 0.79 4 -9 0 9.12 0.72 3 -9 0 21.76 1.14 3 -9 0 22.74 1.02 3 -9 0 22.27 1.13 3 -9 0 21.10 1.20 3 -9 0 22.42 2.49 3 -9 0 20.33 1.01 2 -9 0 17.33 0.91 2 -9 0 19.91 1.96 2 -9 0 20.44 1.07 2 -9 0 18.58 1.05 -2 9 0 18.20 2.15 1 -9 0 75.92 2.32 1 -9 0 71.30 3.66 1 -9 0 79.71 2.43 1 -9 0 78.71 2.50 -1 9 0 79.99 4.08 0 -9 0 0.99 0.46 0 -9 0 1.43 0.35 0 -9 0 0.93 0.40 0 -9 0 1.08 0.76 0 9 0 2.11 0.98 -1 -9 0 6.44 1.14 -1 -9 0 8.00 0.72 1 9 0 7.07 1.36 -2 -9 0 2.11 0.50 -2 -9 0 2.88 0.95 -3 -9 0 21.51 1.02 -3 -9 0 23.22 1.89 -4 -9 0 16.67 1.71 -4 -9 0 16.50 0.88 -5 -9 0 23.05 1.99 -5 -9 0 21.18 1.11 -5 -9 0 18.91 0.96 -6 -9 0 2.43 0.45 -6 -9 0 1.94 0.43 6 9 0 2.74 0.52 -7 -9 0 3.15 0.53 -7 -9 0 3.05 0.48 -8 -9 0 1.26 0.41 -8 -9 0 0.48 0.37 8 9 0 0.74 0.37 -9 -9 0 2.66 0.51 -9 -9 0 2.35 0.46 9 9 0 2.28 0.43 -10 -9 0 15.48 0.95 -10 -9 0 13.72 0.85 10 9 0 13.79 0.83 -11 -9 0 6.12 0.60 -11 -9 0 5.49 0.64 11 9 0 6.80 0.60 -12 -9 0 0.50 0.33 -12 -9 0 0.57 0.31 12 9 0 0.78 0.30 -13 -9 0 0.77 0.28 -13 -9 0 0.32 0.27 13 9 0 1.26 0.30 10 -10 0 5.20 0.39 9 -10 0 1.06 0.33 9 -10 0 1.12 0.29 8 -10 0 7.63 0.60 8 -10 0 8.99 0.66 8 -10 0 8.95 0.66 7 -10 0 1.55 0.42 7 -10 0 1.48 0.35 7 -10 0 2.02 0.47 7 -10 0 2.12 0.47 7 -10 0 0.91 0.38 6 -10 0 5.92 0.61 6 -10 0 7.25 0.79 6 -10 0 7.05 0.75 6 -10 0 7.27 0.66 6 -10 0 6.76 0.72 5 -10 0 -0.17 0.36 5 -10 0 0.10 0.42 5 -10 0 -0.31 0.26 5 -10 0 -0.12 0.36 5 -10 0 0.12 0.35 4 -10 0 1.77 0.49 4 -10 0 1.91 0.48 4 -10 0 0.77 0.47 4 -10 0 2.19 0.43 4 -10 0 2.52 0.45 3 -10 0 8.60 0.83 3 -10 0 8.00 0.73 3 -10 0 7.94 0.67 3 -10 0 8.33 0.84 3 -10 0 8.65 0.80 3 -10 0 9.71 0.72 2 -10 0 8.06 0.80 2 -10 0 6.49 0.69 2 -10 0 7.57 0.79 2 -10 0 7.90 0.65 2 -10 0 7.35 0.67 2 -10 0 7.74 0.76 1 -10 0 2.82 0.43 1 -10 0 2.59 0.49 1 -10 0 2.14 0.52 1 -10 0 1.53 0.42 1 -10 0 2.62 0.49 1 -10 0 3.49 0.60 0 -10 0 8.93 0.76 0 -10 0 7.66 0.74 0 -10 0 8.20 0.73 0 -10 0 8.25 0.69 0 -10 0 9.23 0.86 0 -10 0 6.65 0.64 -1 -10 0 0.25 0.41 -1 -10 0 1.04 0.38 -1 -10 0 0.68 0.34 -1 -10 0 0.55 0.38 -1 -10 0 0.97 0.38 1 10 0 1.35 1.06 -2 -10 0 1.20 0.40 -2 -10 0 1.59 0.45 -2 -10 0 0.78 0.39 -2 -10 0 1.50 0.49 -3 -10 0 1.82 0.43 -3 -10 0 1.91 0.45 -4 -10 0 4.50 0.58 -4 -10 0 4.91 0.61 4 10 0 4.76 0.65 -5 -10 0 25.01 1.20 -5 -10 0 25.06 1.13 5 10 0 26.46 1.27 -6 -10 0 21.27 1.02 -6 -10 0 19.73 1.07 6 10 0 19.06 1.11 -7 -10 0 24.07 1.09 -7 -10 0 21.91 1.13 7 10 0 22.62 1.31 -8 -10 0 0.53 0.33 -8 -10 0 -0.12 0.32 -9 -10 0 21.58 1.02 -9 -10 0 20.60 1.08 -10 -10 0 0.83 0.35 -10 -10 0 -0.41 0.31 10 10 0 -0.25 0.30 -11 -10 0 5.85 0.57 -11 -10 0 5.89 0.59 11 10 0 6.04 0.53 -12 -10 0 -0.37 0.25 -12 -10 0 0.18 0.28 12 10 0 0.44 0.27 9 -11 0 0.87 0.23 8 -11 0 6.93 0.53 8 -11 0 6.38 0.53 7 -11 0 5.93 0.55 7 -11 0 5.48 0.63 7 -11 0 5.24 0.54 6 -11 0 1.48 0.44 6 -11 0 1.79 0.43 6 -11 0 1.54 0.34 6 -11 0 1.16 0.37 6 -11 0 1.35 0.44 5 -11 0 3.80 0.55 5 -11 0 2.42 0.50 5 -11 0 2.14 0.40 5 -11 0 2.43 0.51 5 -11 0 3.37 0.47 4 -11 0 4.03 0.63 4 -11 0 3.23 0.51 4 -11 0 2.64 0.44 4 -11 0 2.82 0.53 4 -11 0 2.70 0.53 3 -11 0 -0.59 0.34 3 -11 0 -0.13 0.38 3 -11 0 -0.61 0.39 3 -11 0 0.29 0.31 3 -11 0 0.22 0.32 2 -11 0 7.25 0.76 2 -11 0 6.51 0.79 2 -11 0 6.97 0.71 2 -11 0 7.85 0.67 2 -11 0 8.04 0.68 2 -11 0 8.06 0.81 1 -11 0 5.82 0.70 1 -11 0 4.55 0.58 1 -11 0 4.84 0.67 1 -11 0 4.90 0.60 1 -11 0 3.09 0.53 1 -11 0 4.76 0.63 0 -11 0 6.43 0.71 0 -11 0 5.62 0.75 0 -11 0 5.70 0.76 0 -11 0 4.35 0.59 0 -11 0 5.78 0.67 -1 -11 0 3.80 0.56 -1 -11 0 4.22 0.54 -1 -11 0 5.73 0.73 -1 -11 0 4.40 0.62 -1 -11 0 4.19 0.60 -2 -11 0 13.92 0.94 -2 -11 0 11.50 0.86 -2 -11 0 12.07 0.91 -3 -11 0 -0.02 0.35 -3 -11 0 -0.17 0.41 3 11 0 -0.23 0.38 -4 -11 0 8.35 0.75 -4 -11 0 8.44 0.77 4 11 0 6.96 0.78 -5 -11 0 8.12 0.73 -5 -11 0 8.05 0.76 5 11 0 7.84 0.82 -6 -11 0 2.95 0.53 -6 -11 0 4.10 0.57 6 11 0 3.58 0.57 -7 -11 0 0.78 0.37 -7 -11 0 0.51 0.38 7 11 0 0.58 0.42 -8 -11 0 4.66 0.60 -8 -11 0 5.28 0.62 -9 -11 0 0.37 0.30 -9 -11 0 0.31 0.34 -10 -11 0 0.21 0.30 -10 -11 0 0.03 0.32 -11 -11 0 1.05 0.33 -11 -11 0 1.56 0.37 -12 -11 0 4.39 0.42 8 -12 0 0.15 0.18 7 -12 0 6.83 0.50 7 -12 0 6.84 0.51 -7 12 0 5.83 0.80 6 -12 0 0.56 0.31 6 -12 0 0.03 0.26 6 -12 0 0.21 0.33 5 -12 0 13.81 0.89 5 -12 0 13.48 0.76 5 -12 0 13.94 0.85 5 -12 0 12.77 0.75 4 -12 0 1.26 0.44 4 -12 0 1.02 0.33 4 -12 0 1.47 0.44 4 -12 0 1.26 0.36 3 -12 0 -0.30 0.35 3 -12 0 -0.47 0.38 3 -12 0 0.40 0.28 3 -12 0 -0.23 0.34 3 -12 0 -0.15 0.33 -3 12 0 0.49 0.39 2 -12 0 0.15 0.29 2 -12 0 -0.24 0.28 2 -12 0 -0.40 0.32 2 -12 0 -0.54 0.33 2 -12 0 0.33 0.46 -2 12 0 0.42 0.41 1 -12 0 6.23 0.73 1 -12 0 5.76 0.72 1 -12 0 5.99 0.61 1 -12 0 5.20 0.66 1 -12 0 6.94 0.62 0 -12 0 5.13 0.61 0 -12 0 4.03 0.59 0 -12 0 5.11 0.71 0 -12 0 4.71 0.65 -1 -12 0 4.25 0.58 -1 -12 0 3.99 0.58 -1 -12 0 4.51 0.65 -1 -12 0 2.73 0.58 1 12 0 2.61 0.57 -2 -12 0 10.99 0.88 -2 -12 0 9.46 0.84 -2 -12 0 11.20 0.88 2 12 0 11.72 0.91 -3 -12 0 1.96 0.48 -3 -12 0 2.49 0.53 3 12 0 2.42 0.53 -4 -12 0 4.74 0.63 -4 -12 0 3.41 0.56 4 12 0 4.45 0.65 -5 -12 0 0.94 0.39 -5 -12 0 0.72 0.43 5 12 0 1.24 0.47 -6 -12 0 2.97 0.50 -6 -12 0 4.01 0.56 6 12 0 3.02 0.55 -7 -12 0 1.48 0.40 -7 -12 0 1.51 0.44 7 12 0 1.58 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0.09 0.35 4 7 17 -0.51 0.29 5 7 17 4.30 0.60 5 7 17 3.33 0.57 5 7 17 4.51 0.56 6 7 17 -0.06 0.31 6 7 17 0.10 0.36 6 7 17 0.06 0.31 7 7 17 1.87 0.42 7 7 17 1.89 0.35 8 7 17 3.94 0.38 8 7 17 4.16 0.47 -6 8 17 4.26 0.38 -5 8 17 0.52 0.26 -4 8 17 4.72 0.49 -3 8 17 2.23 0.38 -2 8 17 0.09 0.28 -2 8 17 0.01 0.41 -1 8 17 0.78 0.45 -1 8 17 0.84 0.33 0 8 17 3.23 0.46 0 8 17 5.19 0.71 1 8 17 0.83 0.46 1 8 17 0.70 0.45 2 8 17 13.03 0.92 2 8 17 14.42 0.94 3 8 17 0.30 0.35 3 8 17 0.52 0.44 3 8 17 0.19 0.39 4 8 17 1.00 0.48 4 8 17 1.33 0.38 4 8 17 1.87 0.46 5 8 17 4.37 0.60 5 8 17 4.48 0.64 5 8 17 4.44 0.56 6 8 17 3.53 0.46 6 8 17 3.79 0.51 6 8 17 3.82 0.52 7 8 17 0.97 0.32 7 8 17 0.89 0.36 8 8 17 0.59 0.25 8 8 17 0.71 0.30 -6 9 17 1.08 0.23 -5 9 17 1.15 0.27 -4 9 17 0.16 0.26 -3 9 17 1.79 0.35 -2 9 17 10.71 0.68 -2 9 17 9.88 0.81 -1 9 17 0.60 0.31 -1 9 17 0.39 0.44 0 9 17 6.03 0.55 0 9 17 5.38 0.74 1 9 17 1.83 0.57 2 9 17 2.59 0.56 3 9 17 0.50 0.42 3 9 17 0.50 0.42 3 9 17 0.04 0.32 4 9 17 0.01 0.40 4 9 17 0.20 0.39 4 9 17 -0.18 0.31 5 9 17 -0.60 0.34 5 9 17 0.11 0.38 5 9 17 0.10 0.31 6 9 17 10.32 0.72 6 9 17 8.23 0.66 6 9 17 10.04 0.66 7 9 17 1.14 0.32 7 9 17 1.85 0.39 8 9 17 3.08 0.41 8 9 17 2.86 0.36 -5 10 17 3.12 0.35 -4 10 17 -0.15 0.22 -3 10 17 8.18 0.56 -2 10 17 0.74 0.30 -2 10 17 0.38 0.42 -1 10 17 4.77 0.50 -1 10 17 5.44 0.70 0 10 17 0.39 0.43 1 10 17 2.52 0.59 2 10 17 1.12 0.48 3 10 17 1.60 0.39 3 10 17 1.52 0.48 4 10 17 2.67 0.43 4 10 17 2.01 0.48 5 10 17 2.12 0.40 5 10 17 1.72 0.42 5 10 17 2.19 0.45 6 10 17 3.23 0.46 6 10 17 1.31 0.39 6 10 17 2.78 0.41 7 10 17 2.12 0.38 7 10 17 1.67 0.32 8 10 17 0.19 0.21 -4 11 17 1.94 0.28 -3 11 17 -0.09 0.23 -2 11 17 0.70 0.27 -2 11 17 0.57 0.40 -1 11 17 2.01 0.37 -1 11 17 2.78 0.51 0 11 17 -0.09 0.42 1 11 17 8.36 0.79 2 11 17 1.33 0.47 3 11 17 -0.33 0.36 4 11 17 1.38 0.34 4 11 17 1.25 0.42 5 11 17 1.47 0.35 5 11 17 0.98 0.37 6 11 17 0.02 0.26 7 11 17 5.38 0.45 -2 12 17 7.41 0.47 -1 12 17 1.08 0.44 0 12 17 0.35 0.40 1 12 17 -0.08 0.38 2 12 17 3.37 0.54 3 12 17 -0.35 0.35 4 12 17 0.10 0.28 4 12 17 -0.16 0.33 5 12 17 0.27 0.28 5 12 17 -0.20 0.34 6 12 17 0.65 0.27 7 12 17 1.27 0.27 0 13 17 0.03 0.35 1 13 17 0.06 0.36 2 13 17 1.19 0.41 3 13 17 1.34 0.40 5 13 17 0.23 0.25 3 -2 -18 0.79 0.21 2 -2 -18 -0.20 0.17 -2 2 18 0.19 0.18 1 -2 -18 -0.02 0.19 -1 2 18 0.48 0.21 0 -2 -18 3.04 0.35 0 2 18 3.61 0.35 -1 -2 -18 3.66 0.38 1 2 18 2.94 0.34 -2 -2 -18 0.07 0.22 3 -3 -18 8.39 0.47 -3 3 18 9.22 0.50 2 -3 -18 2.45 0.33 -2 3 18 2.56 0.33 1 -3 -18 2.58 0.35 -1 3 18 2.20 0.31 0 -3 -18 0.29 0.24 0 3 18 -0.29 0.21 -1 -3 -18 0.70 0.27 1 3 18 1.13 0.32 1 3 18 1.46 0.27 -2 -3 -18 0.47 0.25 2 3 18 0.40 0.30 2 3 18 0.45 0.21 -3 -3 -18 2.44 0.34 3 3 18 2.60 0.38 3 3 18 2.85 0.38 -4 -3 -18 -0.19 0.20 -4 4 18 4.73 0.37 3 -4 -18 -0.24 0.19 -3 4 18 0.10 0.20 2 -4 -18 -0.01 0.22 -2 4 18 0.13 0.22 1 -4 -18 0.14 0.24 -1 4 18 0.31 0.24 0 -4 -18 0.76 0.28 0 4 18 0.59 0.36 0 4 18 0.27 0.24 -1 -4 -18 6.73 0.51 1 4 18 6.01 0.46 1 4 18 5.83 0.59 2 4 18 2.72 0.43 2 4 18 3.35 0.37 3 4 18 2.47 0.37 3 4 18 2.30 0.34 4 4 18 0.15 0.25 4 4 18 -0.09 0.28 4 4 18 0.44 0.28 5 4 18 1.19 0.28 5 4 18 1.03 0.31 -4 5 18 1.47 0.26 3 -5 -18 0.99 0.26 -3 5 18 0.95 0.28 2 -5 -18 5.68 0.47 -2 5 18 6.01 0.49 1 -5 -18 1.39 0.33 -1 5 18 0.59 0.28 -1 5 18 0.70 0.39 0 -5 -18 5.23 0.51 0 5 18 5.63 0.60 0 5 18 7.20 0.51 -1 -5 -18 2.12 0.38 1 5 18 2.11 0.32 1 5 18 1.90 0.42 2 5 18 3.27 0.39 2 5 18 2.79 0.44 3 5 18 0.47 0.32 3 5 18 0.81 0.30 3 5 18 0.24 0.34 4 5 18 1.93 0.32 4 5 18 1.62 0.38 4 5 18 1.31 0.39 5 5 18 0.45 0.30 5 5 18 -0.47 0.21 6 5 18 2.15 0.30 6 5 18 2.70 0.37 -5 6 18 0.62 0.21 -4 6 18 0.36 0.21 3 -6 -18 1.04 0.28 -3 6 18 0.59 0.27 2 -6 -18 0.33 0.24 -2 6 18 -0.06 0.24 1 -6 -18 4.05 0.45 -1 6 18 3.22 0.43 -1 6 18 3.39 0.46 0 -6 -18 1.01 0.31 0 6 18 0.69 0.28 0 6 18 1.22 0.38 1 6 18 2.99 0.41 1 6 18 1.49 0.41 2 6 18 1.25 0.42 2 6 18 1.43 0.38 3 6 18 2.71 0.38 3 6 18 3.13 0.45 3 6 18 3.48 0.52 4 6 18 1.11 0.29 4 6 18 0.96 0.35 4 6 18 0.84 0.38 5 6 18 1.75 0.38 5 6 18 1.97 0.32 5 6 18 1.82 0.36 6 6 18 0.43 0.30 6 6 18 0.27 0.24 -5 7 18 -0.10 0.20 -4 7 18 6.43 0.46 -3 7 18 0.25 0.25 -2 7 18 -0.34 0.24 1 -7 -18 0.19 0.26 -1 7 18 0.47 0.26 -1 7 18 0.20 0.38 0 -7 -18 4.67 0.50 0 7 18 5.05 0.47 0 7 18 5.20 0.61 1 7 18 2.71 0.36 1 7 18 4.16 0.58 2 7 18 0.94 0.40 2 7 18 0.99 0.40 3 7 18 1.31 0.31 3 7 18 0.80 0.39 3 7 18 0.81 0.38 4 7 18 -0.40 0.26 4 7 18 -0.13 0.32 4 7 18 -0.27 0.28 5 7 18 3.27 0.39 5 7 18 2.35 0.38 5 7 18 2.83 0.44 6 7 18 0.13 0.22 6 7 18 -0.19 0.27 -4 8 18 0.36 0.21 -3 8 18 0.57 0.24 -2 8 18 1.78 0.30 -1 8 18 3.11 0.47 -1 8 18 2.54 0.37 0 8 18 0.32 0.25 0 8 18 0.13 0.36 -1 -8 -18 0.95 0.31 1 8 18 1.93 0.44 2 8 18 7.93 0.70 3 8 18 0.39 0.34 3 8 18 -0.14 0.34 4 8 18 1.49 0.34 4 8 18 2.11 0.43 4 8 18 1.30 0.38 5 8 18 0.91 0.32 5 8 18 0.48 0.28 5 8 18 1.25 0.36 6 8 18 3.88 0.47 6 8 18 3.78 0.41 -4 9 18 0.73 0.23 -3 9 18 4.17 0.39 -2 9 18 1.57 0.31 -1 9 18 9.25 0.69 -1 9 18 8.62 0.54 0 9 18 1.61 0.41 1 9 18 0.97 0.38 2 9 18 2.91 0.50 3 9 18 0.37 0.45 3 9 18 0.36 0.34 4 9 18 4.31 0.54 4 9 18 4.62 0.54 4 9 18 4.48 0.46 5 9 18 1.50 0.35 5 9 18 1.34 0.31 5 9 18 1.12 0.34 6 9 18 4.77 0.47 6 9 18 5.10 0.44 -3 10 18 0.25 0.20 -2 10 18 -0.51 0.20 -1 10 18 0.75 0.25 -1 10 18 0.61 0.38 0 10 18 0.59 0.37 1 10 18 3.89 0.51 2 10 18 -0.32 0.33 3 10 18 2.91 0.46 4 10 18 -0.23 0.27 4 10 18 0.02 0.25 5 10 18 6.38 0.47 6 10 18 0.46 0.24 0 11 18 2.61 0.43 1 11 18 2.35 0.43 2 11 18 0.80 0.36 3 11 18 1.12 0.35 4 11 18 0.99 0.33 1 12 18 0.69 0.34 2 12 18 1.47 0.32 -1 -4 -19 0.97 0.21 0 -5 -19 0.49 0.21 -1 -5 -19 0.81 0.22 -2 -5 -19 2.18 0.31 -3 -5 -19 0.50 0.21 -2 6 19 0.07 0.20 -1 6 19 2.42 0.30 0 -6 -19 0.60 0.21 0 6 19 0.01 0.20 -1 -6 -19 0.81 0.24 -2 -6 -19 0.72 0.23 -3 -6 -19 0.60 0.22 -1 7 19 4.80 0.36 -1 -7 -19 2.41 0.34 -2 -7 -19 1.39 0.26 -3 -7 -19 1.24 0.24 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 21281 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Linxtl User' _publ_contact_author_address ; Universit\'e de Montr\'eal D\'epartement de Chimie C.P. 6128, Succ. Centre-ville Montr\'eal, Qu\'ebec Canada, H3C 3J7 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_mm1522_a _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C46 H36 B2 Cl2 N2 ' _chemical_formula_sum 'C23 H18 B Cl N' _chemical_formula_weight 354.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.4818(3) _cell_length_b 14.8376(3) _cell_length_c 15.0664(5) _cell_angle_alpha 112.9650(10) _cell_angle_beta 113.3580(10) _cell_angle_gamma 100.9890(10) _cell_volume 2497.76(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5826 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 72.54 _exptl_crystal_description 'block' _exptl_crystal_colour 'Orange' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 0.943 _exptl_crystal_F_000 740 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 1.367 _shelx_estimated_absorpt_T_min 0.772 _shelx_estimated_absorpt_T_max 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details '?' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean '?' _diffrn_reflns_number 26411 _diffrn_reflns_av_unetI/netI 0.0174 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.544 _diffrn_reflns_theta_max 72.829 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.946 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.946 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_point_group_measured_fraction_full 0.970 _reflns_number_total 9422 _reflns_number_gt 8400 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection '?' _computing_cell_refinement '?' _computing_data_reduction '?' _computing_structure_solution '?' _computing_structure_refinement '?' _computing_molecular_graphics '?' _computing_publication_material 'LinXTL v. 5.3.1' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.1358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9422 _refine_ls_number_parameters 471 _refine_ls_number_restraints 450 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl2 Cl 0.91205(2) 0.33657(2) 0.35622(2) 0.03588(8) Uani 1 1 d . U . . . Cl1 Cl 0.48486(2) 0.58706(2) 0.42244(2) 0.03718(8) Uani 1 1 d . U . . . N2 N 0.72226(7) 0.38469(7) 0.29352(7) 0.02573(18) Uani 1 1 d . U . . . N1 N 0.59639(7) 0.49273(7) 0.31961(7) 0.02665(18) Uani 1 1 d . U . . . C1 C 0.51856(9) 0.15775(8) 0.25940(9) 0.0278(2) Uani 1 1 d . U . . . C2 C 0.62679(8) 0.33541(8) 0.28483(9) 0.0261(2) Uani 1 1 d . U . . . C3 C 0.60871(9) 0.22510(8) 0.25945(9) 0.0269(2) Uani 1 1 d . U . . . C4 C 0.69735(8) 0.54529(8) 0.34003(9) 0.0265(2) Uani 1 1 d . U . . . C5 C 0.82623(9) 0.73607(8) 0.40907(9) 0.0282(2) Uani 1 1 d . U . . . C6 C 0.76003(8) 0.48712(8) 0.31992(9) 0.0271(2) Uani 1 1 d . U . . . C7 C 0.69464(9) 0.09425(8) 0.21231(9) 0.0283(2) Uani 1 1 d . U . . . C8 C 0.55791(9) 0.38976(8) 0.29160(9) 0.0277(2) Uani 1 1 d . U . . . C9 C 0.62850(9) 0.67654(8) 0.36444(9) 0.0272(2) Uani 1 1 d . U . . . C10 C 0.42933(9) 0.51412(8) 0.19012(10) 0.0312(2) Uani 1 1 d . U . . . C11 C 0.43697(10) 0.06238(9) 0.16014(10) 0.0345(2) Uani 1 1 d . U . . . H11 H 0.4394 0.0409 0.0932 0.041 Uiso 1 1 calc R U . . . C12 C 0.71871(9) 0.65770(8) 0.37257(9) 0.0271(2) Uani 1 1 d . U . . . C13 C 0.92075(10) 0.77036(9) 0.51017(11) 0.0356(2) Uani 1 1 d . U . . . H13 H 0.9172 0.7431 0.5568 0.043 Uiso 1 1 calc R U . . . C14 C 0.68512(9) 0.19765(8) 0.23830(9) 0.0267(2) Uani 1 1 d . U . . . C15 C 0.83259(10) 0.77833(9) 0.34275(11) 0.0355(2) Uani 1 1 d . U . . . H15 H 0.7682 0.7568 0.2742 0.043 Uiso 1 1 calc R U . . . C16 C 0.67182(10) 0.03685(9) 0.26184(11) 0.0340(2) Uani 1 1 d . U . . . H16 H 0.6489 0.0645 0.3140 0.041 Uiso 1 1 calc R U . . . C17 C 0.51479(10) 0.18720(9) 0.35694(10) 0.0332(2) Uani 1 1 d . U . . . H17 H 0.5705 0.2517 0.4250 0.040 Uiso 1 1 calc R U . . . C18 C 0.71222(9) 0.87818(9) 0.48631(10) 0.0333(2) Uani 1 1 d . U . . . H18 H 0.7810 0.8771 0.5275 0.040 Uiso 1 1 calc R U . . . C19 C 0.62206(9) 0.78175(8) 0.39641(9) 0.0280(2) Uani 1 1 d . U . . . C20 C 0.75068(9) 0.28202(8) 0.12968(10) 0.0298(2) Uani 1 1 d . U . . . C21 C 0.70230(11) 0.97560(9) 0.51603(11) 0.0385(3) Uani 1 1 d . U . . . H21 H 0.7641 1.0403 0.5775 0.046 Uiso 1 1 calc R U . . . C22 C 0.83559(10) 0.29372(10) 0.10792(11) 0.0383(3) Uani 1 1 d . U . . . H22 H 0.9054 0.3027 0.1608 0.046 Uiso 1 1 calc R U . . . C23 C 0.52179(10) 0.78660(9) 0.33890(10) 0.0348(2) Uani 1 1 d . U . . . H23 H 0.4588 0.7222 0.2790 0.042 Uiso 1 1 calc R U . . . C24 C 0.68247(11) -0.05962(10) 0.23532(12) 0.0402(3) Uani 1 1 d . U . . . H24 H 0.6680 -0.0970 0.2704 0.048 Uiso 1 1 calc R U . . . C25 C 0.86337(9) 0.53190(9) 0.32249(11) 0.0340(2) Uani 1 1 d . U . . . H25A H 0.9266 0.5680 0.3997 0.051 Uiso 1 1 calc R U . . . H25B H 0.8584 0.5835 0.2974 0.051 Uiso 1 1 calc R U . . . H25C H 0.8729 0.4735 0.2721 0.051 Uiso 1 1 calc R U . . . C26 C 0.44340(9) 0.33793(9) 0.26459(12) 0.0360(3) Uani 1 1 d . U . . . H26A H 0.4459 0.3440 0.3328 0.054 Uiso 1 1 calc R U . . . H26B H 0.4105 0.2620 0.2060 0.054 Uiso 1 1 calc R U . . . H26C H 0.3988 0.3738 0.2373 0.054 Uiso 1 1 calc R U . . . C27 C 0.43045(11) 0.12334(10) 0.35594(12) 0.0398(3) Uani 1 1 d . U . . . H27 H 0.4284 0.1441 0.4230 0.048 Uiso 1 1 calc R U . . . C28 C 0.60282(11) 0.97870(9) 0.45650(11) 0.0397(3) Uani 1 1 d . U . . . H28 H 0.5964 1.0454 0.4764 0.048 Uiso 1 1 calc R U . . . C29 C 0.73023(11) 0.05250(10) 0.13841(11) 0.0388(3) Uani 1 1 d . U . . . H29 H 0.7494 0.0917 0.1068 0.047 Uiso 1 1 calc R U . . . C30 C 0.44811(11) 0.47515(11) 0.10119(11) 0.0431(3) Uani 1 1 d . U . . . H30 H 0.5203 0.4815 0.1174 0.052 Uiso 1 1 calc R U . . . C31 C 0.35234(11) -0.00113(10) 0.15898(12) 0.0424(3) Uani 1 1 d . U . . . H31 H 0.2963 -0.0656 0.0910 0.051 Uiso 1 1 calc R U . . . C32 C 0.32246(11) 0.50342(11) 0.16212(12) 0.0461(3) Uani 1 1 d . U . . . H32 H 0.3066 0.5290 0.2205 0.055 Uiso 1 1 calc R U . . . C33 C 0.64827(11) 0.26466(11) 0.04710(11) 0.0425(3) Uani 1 1 d . U . . . H33 H 0.5877 0.2529 0.0578 0.051 Uiso 1 1 calc R U . . . C34 C 0.82043(13) 0.29258(11) 0.00995(12) 0.0499(3) Uani 1 1 d . U . . . H34 H 0.8796 0.3008 -0.0033 0.060 Uiso 1 1 calc R U . . . C35 C 0.51312(11) 0.88447(10) 0.36819(11) 0.0410(3) Uani 1 1 d . U . . . H35 H 0.4448 0.8864 0.3270 0.049 Uiso 1 1 calc R U . . . C36 C 0.93246(12) 0.85167(11) 0.37628(13) 0.0478(3) Uani 1 1 d . U . . . H36 H 0.9365 0.8797 0.3303 0.057 Uiso 1 1 calc R U . . . C37 C 0.71389(12) -0.10189(10) 0.15824(12) 0.0464(3) Uani 1 1 d . U . . . H37 H 0.7187 -0.1692 0.1385 0.056 Uiso 1 1 calc R U . . . C38 C 0.34930(11) 0.02920(10) 0.25690(13) 0.0435(3) Uani 1 1 d . U . . . H38 H 0.2914 -0.0147 0.2560 0.052 Uiso 1 1 calc R U . . . C39 C 1.02038(10) 0.84412(10) 0.54361(13) 0.0454(3) Uani 1 1 d . U . . . H39 H 1.0847 0.8671 0.6129 0.054 Uiso 1 1 calc R U . . . C40 C 0.71950(14) 0.27952(12) -0.06755(12) 0.0542(4) Uani 1 1 d . U . . . H40 H 0.7097 0.2811 -0.1330 0.065 Uiso 1 1 calc R U . . . C41 C 0.73838(14) -0.04542(11) 0.10984(13) 0.0498(3) Uani 1 1 d . U . . . H41 H 0.7607 -0.0737 0.0573 0.060 Uiso 1 1 calc R U . . . B2 B 0.76680(10) 0.29418(9) 0.24682(10) 0.0270(2) Uani 1 1 d . U . . . C42 C 0.25893(14) 0.41840(13) -0.03549(13) 0.0611(4) Uani 1 1 d . U . . . H42 H 0.2013 0.3864 -0.1116 0.073 Uiso 1 1 calc R U . . . C43 C 0.63299(14) 0.26412(13) -0.04999(12) 0.0548(4) Uani 1 1 d . U . . . H43 H 0.5628 0.2531 -0.1044 0.066 Uiso 1 1 calc R U . . . C44 C 1.02617(11) 0.88413(11) 0.47638(14) 0.0504(3) Uani 1 1 d . U . . . H44 H 1.0946 0.9340 0.4989 0.060 Uiso 1 1 calc R U . . . B1 B 0.52922(10) 0.56883(9) 0.31856(11) 0.0278(2) Uani 1 1 d . U . . . C45 C 0.36397(13) 0.42727(13) -0.01057(12) 0.0560(4) Uani 1 1 d . U . . . H45 H 0.3788 0.4007 -0.0696 0.067 Uiso 1 1 calc R U . . . C46 C 0.23841(12) 0.45609(14) 0.05050(14) 0.0613(4) Uani 1 1 d . U . . . H46 H 0.1661 0.4498 0.0336 0.074 Uiso 1 1 calc R U . . . loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.013 0.000 826 192 ' ' _platon_squeeze_details ; ; loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.02884(14) 0.03598(14) 0.03872(15) 0.02148(12) 0.01158(12) 0.01425(11) Cl1 0.04429(16) 0.03609(15) 0.03984(15) 0.02023(12) 0.02771(13) 0.01821(12) N2 0.0257(4) 0.0224(4) 0.0279(4) 0.0137(3) 0.0122(4) 0.0099(3) N1 0.0271(4) 0.0236(4) 0.0302(4) 0.0151(4) 0.0142(4) 0.0110(3) C1 0.0312(5) 0.0217(5) 0.0329(5) 0.0160(4) 0.0161(5) 0.0123(4) C2 0.0270(5) 0.0228(5) 0.0268(5) 0.0135(4) 0.0125(4) 0.0088(4) C3 0.0306(5) 0.0218(5) 0.0275(5) 0.0138(4) 0.0138(4) 0.0101(4) C4 0.0268(5) 0.0237(5) 0.0281(5) 0.0147(4) 0.0127(4) 0.0095(4) C5 0.0297(5) 0.0202(4) 0.0345(5) 0.0140(4) 0.0158(5) 0.0119(4) C6 0.0272(5) 0.0226(5) 0.0297(5) 0.0143(4) 0.0127(4) 0.0097(4) C7 0.0284(5) 0.0232(5) 0.0291(5) 0.0140(4) 0.0110(4) 0.0104(4) C8 0.0287(5) 0.0240(5) 0.0311(5) 0.0156(4) 0.0150(4) 0.0103(4) C9 0.0304(5) 0.0247(5) 0.0259(5) 0.0143(4) 0.0128(4) 0.0116(4) C10 0.0326(5) 0.0240(5) 0.0337(5) 0.0156(4) 0.0143(5) 0.0105(4) C11 0.0369(6) 0.0274(5) 0.0328(6) 0.0131(5) 0.0169(5) 0.0091(5) C12 0.0297(5) 0.0215(5) 0.0282(5) 0.0137(4) 0.0127(4) 0.0104(4) C13 0.0330(6) 0.0299(5) 0.0409(6) 0.0202(5) 0.0147(5) 0.0132(5) C14 0.0304(5) 0.0239(5) 0.0248(5) 0.0140(4) 0.0123(4) 0.0109(4) C15 0.0388(6) 0.0299(5) 0.0390(6) 0.0201(5) 0.0192(5) 0.0136(5) C16 0.0368(6) 0.0320(5) 0.0410(6) 0.0235(5) 0.0212(5) 0.0167(5) C17 0.0382(6) 0.0284(5) 0.0343(6) 0.0167(5) 0.0196(5) 0.0135(5) C18 0.0347(6) 0.0272(5) 0.0381(6) 0.0161(5) 0.0193(5) 0.0133(5) C19 0.0339(5) 0.0263(5) 0.0304(5) 0.0170(4) 0.0189(5) 0.0148(4) C20 0.0352(5) 0.0220(5) 0.0330(5) 0.0148(4) 0.0180(5) 0.0111(4) C21 0.0478(7) 0.0238(5) 0.0453(7) 0.0150(5) 0.0286(6) 0.0136(5) C22 0.0394(6) 0.0334(6) 0.0392(6) 0.0174(5) 0.0216(5) 0.0099(5) C23 0.0379(6) 0.0303(5) 0.0355(6) 0.0178(5) 0.0166(5) 0.0168(5) C24 0.0454(7) 0.0326(6) 0.0515(7) 0.0290(6) 0.0242(6) 0.0185(5) C25 0.0306(5) 0.0248(5) 0.0482(7) 0.0184(5) 0.0222(5) 0.0116(4) C26 0.0311(5) 0.0296(5) 0.0540(7) 0.0251(5) 0.0234(5) 0.0139(4) C27 0.0491(7) 0.0405(6) 0.0463(7) 0.0283(6) 0.0314(6) 0.0214(5) C28 0.0586(7) 0.0305(6) 0.0508(7) 0.0260(5) 0.0370(7) 0.0267(6) C29 0.0546(7) 0.0347(6) 0.0401(6) 0.0237(5) 0.0284(6) 0.0245(5) C30 0.0396(6) 0.0440(7) 0.0374(6) 0.0194(6) 0.0182(6) 0.0093(5) C31 0.0380(6) 0.0281(6) 0.0473(7) 0.0156(5) 0.0184(6) 0.0048(5) C32 0.0359(6) 0.0459(7) 0.0438(7) 0.0168(6) 0.0152(6) 0.0197(6) C33 0.0423(7) 0.0481(7) 0.0373(6) 0.0233(6) 0.0193(6) 0.0196(6) C34 0.0596(8) 0.0414(7) 0.0483(7) 0.0204(6) 0.0358(7) 0.0090(6) C35 0.0485(7) 0.0399(6) 0.0460(7) 0.0268(6) 0.0249(6) 0.0286(6) C36 0.0534(8) 0.0384(7) 0.0632(8) 0.0322(6) 0.0358(7) 0.0154(6) C37 0.0610(8) 0.0304(6) 0.0536(8) 0.0244(6) 0.0284(7) 0.0266(6) C38 0.0423(6) 0.0384(6) 0.0614(8) 0.0317(6) 0.0321(6) 0.0139(5) C39 0.0303(6) 0.0322(6) 0.0551(8) 0.0193(6) 0.0117(6) 0.0089(5) C40 0.0723(10) 0.0486(8) 0.0365(7) 0.0248(6) 0.0257(7) 0.0145(7) C41 0.0764(10) 0.0430(7) 0.0506(8) 0.0270(6) 0.0411(8) 0.0379(7) B2 0.0265(5) 0.0233(5) 0.0304(6) 0.0146(4) 0.0129(5) 0.0116(4) C42 0.0525(8) 0.0561(9) 0.0380(7) 0.0202(7) 0.0028(6) 0.0101(7) C43 0.0597(9) 0.0640(9) 0.0377(7) 0.0299(7) 0.0189(7) 0.0261(7) C44 0.0366(6) 0.0340(6) 0.0739(10) 0.0261(7) 0.0282(7) 0.0072(5) B1 0.0310(6) 0.0245(5) 0.0318(6) 0.0158(5) 0.0171(5) 0.0143(5) C45 0.0571(8) 0.0569(9) 0.0348(7) 0.0196(6) 0.0185(7) 0.0089(7) C46 0.0375(7) 0.0622(9) 0.0525(9) 0.0193(7) 0.0073(7) 0.0204(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 B2 1.8640(12) . ? Cl1 B1 1.8625(13) . ? N2 C6 1.3439(13) . ? N2 C2 1.3637(13) . ? N2 B2 1.6332(14) . ? N1 C8 1.3448(13) . ? N1 C4 1.3646(13) . ? N1 B1 1.6255(14) . ? C1 C17 1.3875(16) . ? C1 C11 1.3947(15) . ? C1 C3 1.4848(14) . ? C2 C8 1.4068(14) . ? C2 C3 1.4705(13) . ? C3 C14 1.3572(16) . ? C4 C6 1.4048(14) . ? C4 C12 1.4706(13) . ? C5 C13 1.3890(16) . ? C5 C15 1.3928(16) . ? C5 C12 1.4869(14) . ? C6 C25 1.4959(15) . ? C7 C29 1.3884(17) . ? C7 C16 1.4056(15) . ? C7 C14 1.4767(14) . ? C8 C26 1.4971(14) . ? C9 C12 1.3560(15) . ? C9 C19 1.4772(14) . ? C9 B1 1.6040(15) . ? C10 C32 1.3909(17) . ? C10 C30 1.3957(18) . ? C10 B1 1.6134(16) . ? C11 C31 1.3857(17) . ? C11 H11 0.9500 . ? C13 C39 1.3873(17) . ? C13 H13 0.9500 . ? C14 B2 1.5992(15) . ? C15 C36 1.3866(18) . ? C15 H15 0.9500 . ? C16 C24 1.3853(16) . ? C16 H16 0.9500 . ? C17 C27 1.3867(16) . ? C17 H17 0.9500 . ? C18 C21 1.3912(15) . ? C18 C19 1.3999(16) . ? C18 H18 0.9500 . ? C19 C23 1.3983(16) . ? C20 C22 1.3900(17) . ? C20 C33 1.3981(17) . ? C20 B2 1.6157(16) . ? C21 C28 1.3838(19) . ? C21 H21 0.9500 . ? C22 C34 1.3963(19) . ? C22 H22 0.9500 . ? C23 C35 1.3902(16) . ? C23 H23 0.9500 . ? C24 C37 1.382(2) . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C38 1.384(2) . ? C27 H27 0.9500 . ? C28 C35 1.3776(19) . ? C28 H28 0.9500 . ? C29 C41 1.3884(17) . ? C29 H29 0.9500 . ? C30 C45 1.3908(19) . ? C30 H30 0.9500 . ? C31 C38 1.386(2) . ? C31 H31 0.9500 . ? C32 C46 1.390(2) . ? C32 H32 0.9500 . ? C33 C43 1.3864(19) . ? C33 H33 0.9500 . ? C34 C40 1.378(2) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C44 1.382(2) . ? C36 H36 0.9500 . ? C37 C41 1.389(2) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C44 1.379(2) . ? C39 H39 0.9500 . ? C40 C43 1.376(2) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C46 1.372(3) . ? C42 C45 1.380(2) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 N2 C2 123.27(9) . . ? C6 N2 B2 127.57(9) . . ? C2 N2 B2 108.41(8) . . ? C8 N1 C4 123.13(9) . . ? C8 N1 B1 127.46(9) . . ? C4 N1 B1 108.92(8) . . ? C17 C1 C11 119.25(10) . . ? C17 C1 C3 121.15(10) . . ? C11 C1 C3 119.59(10) . . ? N2 C2 C8 118.79(9) . . ? N2 C2 C3 111.20(9) . . ? C8 C2 C3 129.79(9) . . ? C14 C3 C2 110.36(9) . . ? C14 C3 C1 127.15(9) . . ? C2 C3 C1 122.50(9) . . ? N1 C4 C6 118.92(9) . . ? N1 C4 C12 111.08(9) . . ? C6 C4 C12 129.78(10) . . ? C13 C5 C15 118.97(10) . . ? C13 C5 C12 121.11(10) . . ? C15 C5 C12 119.89(10) . . ? N2 C6 C4 117.53(9) . . ? N2 C6 C25 118.87(9) . . ? C4 C6 C25 123.57(9) . . ? C29 C7 C16 118.03(10) . . ? C29 C7 C14 119.33(10) . . ? C16 C7 C14 122.62(10) . . ? N1 C8 C2 117.55(9) . . ? N1 C8 C26 118.79(9) . . ? C2 C8 C26 123.61(9) . . ? C12 C9 C19 125.38(10) . . ? C12 C9 B1 110.63(9) . . ? C19 C9 B1 123.96(9) . . ? C32 C10 C30 117.00(11) . . ? C32 C10 B1 122.87(11) . . ? C30 C10 B1 120.14(10) . . ? C31 C11 C1 120.14(11) . . ? C31 C11 H11 119.9 . . ? C1 C11 H11 119.9 . . ? C9 C12 C4 110.43(9) . . ? C9 C12 C5 127.01(9) . . ? C4 C12 C5 122.56(9) . . ? C39 C13 C5 120.52(12) . . ? C39 C13 H13 119.7 . . ? C5 C13 H13 119.7 . . ? C3 C14 C7 125.82(10) . . ? C3 C14 B2 110.66(9) . . ? C7 C14 B2 123.52(9) . . ? C36 C15 C5 120.28(12) . . ? C36 C15 H15 119.9 . . ? C5 C15 H15 119.9 . . ? C24 C16 C7 120.59(12) . . ? C24 C16 H16 119.7 . . ? C7 C16 H16 119.7 . . ? C27 C17 C1 120.60(11) . . ? C27 C17 H17 119.7 . . ? C1 C17 H17 119.7 . . ? C21 C18 C19 120.83(11) . . ? C21 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C23 C19 C18 117.84(10) . . ? C23 C19 C9 119.70(10) . . ? C18 C19 C9 122.40(10) . . ? C22 C20 C33 117.12(11) . . ? C22 C20 B2 123.41(10) . . ? C33 C20 B2 119.38(10) . . ? C28 C21 C18 120.34(12) . . ? C28 C21 H21 119.8 . . ? C18 C21 H21 119.8 . . ? C20 C22 C34 121.40(13) . . ? C20 C22 H22 119.3 . . ? C34 C22 H22 119.3 . . ? C35 C23 C19 120.88(11) . . ? C35 C23 H23 119.6 . . ? C19 C23 H23 119.6 . . ? C37 C24 C16 120.49(11) . . ? C37 C24 H24 119.8 . . ? C16 C24 H24 119.8 . . ? C6 C25 H25A 109.5 . . ? C6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C26 H26A 109.5 . . ? C8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C38 C27 C17 119.82(12) . . ? C38 C27 H27 120.1 . . ? C17 C27 H27 120.1 . . ? C35 C28 C21 119.56(10) . . ? C35 C28 H28 120.2 . . ? C21 C28 H28 120.2 . . ? C7 C29 C41 121.31(12) . . ? C7 C29 H29 119.3 . . ? C41 C29 H29 119.3 . . ? C45 C30 C10 121.73(13) . . ? C45 C30 H30 119.1 . . ? C10 C30 H30 119.1 . . ? C11 C31 C38 120.10(12) . . ? C11 C31 H31 120.0 . . ? C38 C31 H31 120.0 . . ? C46 C32 C10 121.33(14) . . ? C46 C32 H32 119.3 . . ? C10 C32 H32 119.3 . . ? C43 C33 C20 121.65(13) . . ? C43 C33 H33 119.2 . . ? C20 C33 H33 119.2 . . ? C40 C34 C22 119.88(14) . . ? C40 C34 H34 120.1 . . ? C22 C34 H34 120.1 . . ? C28 C35 C23 120.52(12) . . ? C28 C35 H35 119.7 . . ? C23 C35 H35 119.7 . . ? C44 C36 C15 120.16(12) . . ? C44 C36 H36 119.9 . . ? C15 C36 H36 119.9 . . ? C24 C37 C41 119.64(11) . . ? C24 C37 H37 120.2 . . ? C41 C37 H37 120.2 . . ? C27 C38 C31 120.07(11) . . ? C27 C38 H38 120.0 . . ? C31 C38 H38 120.0 . . ? C44 C39 C13 120.04(12) . . ? C44 C39 H39 120.0 . . ? C13 C39 H39 120.0 . . ? C43 C40 C34 119.92(13) . . ? C43 C40 H40 120.0 . . ? C34 C40 H40 120.0 . . ? C29 C41 C37 119.87(13) . . ? C29 C41 H41 120.1 . . ? C37 C41 H41 120.1 . . ? C14 B2 C20 117.13(9) . . ? C14 B2 N2 98.07(8) . . ? C20 B2 N2 105.56(8) . . ? C14 B2 Cl2 110.66(7) . . ? C20 B2 Cl2 114.31(8) . . ? N2 B2 Cl2 109.48(7) . . ? C46 C42 C45 119.49(14) . . ? C46 C42 H42 120.3 . . ? C45 C42 H42 120.3 . . ? C40 C43 C33 119.95(14) . . ? C40 C43 H43 120.0 . . ? C33 C43 H43 120.0 . . ? C39 C44 C36 120.01(12) . . ? C39 C44 H44 120.0 . . ? C36 C44 H44 120.0 . . ? C9 B1 C10 115.81(9) . . ? C9 B1 N1 98.00(8) . . ? C10 B1 N1 107.17(8) . . ? C9 B1 Cl1 110.64(8) . . ? C10 B1 Cl1 114.36(8) . . ? N1 B1 Cl1 109.40(7) . . ? C42 C45 C30 119.85(15) . . ? C42 C45 H45 120.1 . . ? C30 C45 H45 120.1 . . ? C42 C46 C32 120.60(14) . . ? C42 C46 H46 119.7 . . ? C32 C46 H46 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N2 C2 C8 7.13(15) . . . . ? B2 N2 C2 C8 -163.61(9) . . . . ? C6 N2 C2 C3 -177.72(9) . . . . ? B2 N2 C2 C3 11.54(11) . . . . ? N2 C2 C3 C14 -7.20(12) . . . . ? C8 C2 C3 C14 167.27(11) . . . . ? N2 C2 C3 C1 172.29(9) . . . . ? C8 C2 C3 C1 -13.25(17) . . . . ? C17 C1 C3 C14 116.77(13) . . . . ? C11 C1 C3 C14 -62.30(15) . . . . ? C17 C1 C3 C2 -62.62(14) . . . . ? C11 C1 C3 C2 118.31(12) . . . . ? C8 N1 C4 C6 6.76(15) . . . . ? B1 N1 C4 C6 -165.83(9) . . . . ? C8 N1 C4 C12 -178.00(9) . . . . ? B1 N1 C4 C12 9.40(12) . . . . ? C2 N2 C6 C4 0.44(15) . . . . ? B2 N2 C6 C4 169.33(9) . . . . ? C2 N2 C6 C25 -177.48(10) . . . . ? B2 N2 C6 C25 -8.59(16) . . . . ? N1 C4 C6 N2 -7.31(15) . . . . ? C12 C4 C6 N2 178.47(10) . . . . ? N1 C4 C6 C25 170.50(10) . . . . ? C12 C4 C6 C25 -3.71(18) . . . . ? C4 N1 C8 C2 0.81(15) . . . . ? B1 N1 C8 C2 171.98(10) . . . . ? C4 N1 C8 C26 -176.58(10) . . . . ? B1 N1 C8 C26 -5.41(16) . . . . ? N2 C2 C8 N1 -7.65(15) . . . . ? C3 C2 C8 N1 178.24(10) . . . . ? N2 C2 C8 C26 169.60(10) . . . . ? C3 C2 C8 C26 -4.51(18) . . . . ? C17 C1 C11 C31 0.98(17) . . . . ? C3 C1 C11 C31 -179.94(11) . . . . ? C19 C9 C12 C4 176.42(10) . . . . ? B1 C9 C12 C4 -1.77(13) . . . . ? C19 C9 C12 C5 -3.31(18) . . . . ? B1 C9 C12 C5 178.50(10) . . . . ? N1 C4 C12 C9 -5.06(13) . . . . ? C6 C4 C12 C9 169.51(11) . . . . ? N1 C4 C12 C5 174.68(10) . . . . ? C6 C4 C12 C5 -10.74(18) . . . . ? C13 C5 C12 C9 111.85(13) . . . . ? C15 C5 C12 C9 -66.52(16) . . . . ? C13 C5 C12 C4 -67.84(15) . . . . ? C15 C5 C12 C4 113.79(12) . . . . ? C15 C5 C13 C39 -1.14(17) . . . . ? C12 C5 C13 C39 -179.53(11) . . . . ? C2 C3 C14 C7 178.49(10) . . . . ? C1 C3 C14 C7 -0.97(18) . . . . ? C2 C3 C14 B2 -0.74(12) . . . . ? C1 C3 C14 B2 179.81(10) . . . . ? C29 C7 C14 C3 146.25(12) . . . . ? C16 C7 C14 C3 -35.49(16) . . . . ? C29 C7 C14 B2 -34.62(15) . . . . ? C16 C7 C14 B2 143.64(11) . . . . ? C13 C5 C15 C36 1.43(17) . . . . ? C12 C5 C15 C36 179.84(11) . . . . ? C29 C7 C16 C24 -1.37(17) . . . . ? C14 C7 C16 C24 -179.65(11) . . . . ? C11 C1 C17 C27 -0.61(17) . . . . ? C3 C1 C17 C27 -179.68(10) . . . . ? C21 C18 C19 C23 -0.93(17) . . . . ? C21 C18 C19 C9 -178.19(11) . . . . ? C12 C9 C19 C23 149.17(12) . . . . ? B1 C9 C19 C23 -32.87(16) . . . . ? C12 C9 C19 C18 -33.62(17) . . . . ? B1 C9 C19 C18 144.35(11) . . . . ? C19 C18 C21 C28 -0.33(19) . . . . ? C33 C20 C22 C34 2.57(18) . . . . ? B2 C20 C22 C34 -173.85(11) . . . . ? C18 C19 C23 C35 1.86(18) . . . . ? C9 C19 C23 C35 179.20(11) . . . . ? C7 C16 C24 C37 -1.11(19) . . . . ? C1 C17 C27 C38 0.13(18) . . . . ? C18 C21 C28 C35 0.7(2) . . . . ? C16 C7 C29 C41 2.92(19) . . . . ? C14 C7 C29 C41 -178.74(12) . . . . ? C32 C10 C30 C45 -0.28(19) . . . . ? B1 C10 C30 C45 179.83(12) . . . . ? C1 C11 C31 C38 -0.86(19) . . . . ? C30 C10 C32 C46 -0.1(2) . . . . ? B1 C10 C32 C46 179.82(13) . . . . ? C22 C20 C33 C43 -2.97(19) . . . . ? B2 C20 C33 C43 173.60(12) . . . . ? C20 C22 C34 C40 -0.1(2) . . . . ? C21 C28 C35 C23 0.3(2) . . . . ? C19 C23 C35 C28 -1.6(2) . . . . ? C5 C15 C36 C44 -0.6(2) . . . . ? C16 C24 C37 C41 2.1(2) . . . . ? C17 C27 C38 C31 0.00(19) . . . . ? C11 C31 C38 C27 0.4(2) . . . . ? C5 C13 C39 C44 0.1(2) . . . . ? C22 C34 C40 C43 -2.1(2) . . . . ? C7 C29 C41 C37 -2.0(2) . . . . ? C24 C37 C41 C29 -0.6(2) . . . . ? C3 C14 B2 C20 -105.45(11) . . . . ? C7 C14 B2 C20 75.30(13) . . . . ? C3 C14 B2 N2 6.70(11) . . . . ? C7 C14 B2 N2 -172.55(9) . . . . ? C3 C14 B2 Cl2 121.12(9) . . . . ? C7 C14 B2 Cl2 -58.13(12) . . . . ? C22 C20 B2 C14 -126.99(11) . . . . ? C33 C20 B2 C14 56.67(14) . . . . ? C22 C20 B2 N2 125.17(11) . . . . ? C33 C20 B2 N2 -51.17(13) . . . . ? C22 C20 B2 Cl2 4.80(14) . . . . ? C33 C20 B2 Cl2 -171.54(9) . . . . ? C6 N2 B2 C14 178.95(9) . . . . ? C2 N2 B2 C14 -10.83(10) . . . . ? C6 N2 B2 C20 -59.89(13) . . . . ? C2 N2 B2 C20 110.34(9) . . . . ? C6 N2 B2 Cl2 63.60(12) . . . . ? C2 N2 B2 Cl2 -126.18(8) . . . . ? C34 C40 C43 C33 1.7(2) . . . . ? C20 C33 C43 C40 0.9(2) . . . . ? C13 C39 C44 C36 0.7(2) . . . . ? C15 C36 C44 C39 -0.4(2) . . . . ? C12 C9 B1 C10 -107.00(11) . . . . ? C19 C9 B1 C10 74.77(13) . . . . ? C12 C9 B1 N1 6.52(11) . . . . ? C19 C9 B1 N1 -171.70(9) . . . . ? C12 C9 B1 Cl1 120.81(9) . . . . ? C19 C9 B1 Cl1 -57.42(12) . . . . ? C32 C10 B1 C9 -116.71(12) . . . . ? C30 C10 B1 C9 63.18(14) . . . . ? C32 C10 B1 N1 135.16(11) . . . . ? C30 C10 B1 N1 -44.95(13) . . . . ? C32 C10 B1 Cl1 13.73(14) . . . . ? C30 C10 B1 Cl1 -166.38(9) . . . . ? C8 N1 B1 C9 178.39(10) . . . . ? C4 N1 B1 C9 -9.43(10) . . . . ? C8 N1 B1 C10 -61.38(13) . . . . ? C4 N1 B1 C10 110.81(10) . . . . ? C8 N1 B1 Cl1 63.12(12) . . . . ? C4 N1 B1 Cl1 -124.69(8) . . . . ? C46 C42 C45 C30 -0.6(3) . . . . ? C10 C30 C45 C42 0.6(2) . . . . ? C45 C42 C46 C32 0.3(3) . . . . ? C10 C32 C46 C42 0.0(3) . . . . ? _refine_diff_density_max 0.285 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.033 _shelxl_version_number 2014/6 _shelx_res_file ; TITL mm1522_a.res in P-1 CELL 1.54178 14.4818 14.8376 15.0664 112.965 113.358 100.989 ZERR 4.000 0.0003 0.0003 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H B N CL UNIT 92 72 4 4 4 L.S. 20 HTAB CONF ACTA PLAN 0 BOND $H RIGU WPDB -1 FMAP 2 LIST 6 SIZE 0.20 0.20 0.20 TEMP -99.950 WGHT 0.068100 0.135800 FVAR 4.16793 CL2 5 0.912047 0.336569 0.356217 11.00000 0.02884 0.03598 = 0.03872 0.02148 0.01158 0.01425 CL1 5 0.484862 0.587061 0.422443 11.00000 0.04429 0.03609 = 0.03984 0.02023 0.02771 0.01821 N2 4 0.722258 0.384687 0.293517 11.00000 0.02569 0.02238 = 0.02793 0.01371 0.01224 0.00991 N1 4 0.596385 0.492725 0.319610 11.00000 0.02713 0.02355 = 0.03016 0.01506 0.01422 0.01095 C1 1 0.518559 0.157745 0.259401 11.00000 0.03119 0.02168 = 0.03292 0.01595 0.01610 0.01230 C2 1 0.626788 0.335405 0.284829 11.00000 0.02703 0.02283 = 0.02681 0.01354 0.01246 0.00882 C3 1 0.608711 0.225101 0.259447 11.00000 0.03059 0.02181 = 0.02751 0.01383 0.01379 0.01011 C4 1 0.697348 0.545290 0.340028 11.00000 0.02683 0.02368 = 0.02810 0.01470 0.01269 0.00948 C5 1 0.826230 0.736073 0.409069 11.00000 0.02966 0.02022 = 0.03446 0.01403 0.01583 0.01189 C6 1 0.760029 0.487115 0.319921 11.00000 0.02716 0.02258 = 0.02969 0.01429 0.01269 0.00975 C7 1 0.694638 0.094247 0.212308 11.00000 0.02839 0.02325 = 0.02905 0.01401 0.01105 0.01038 C8 1 0.557909 0.389761 0.291603 11.00000 0.02869 0.02404 = 0.03108 0.01560 0.01499 0.01029 C9 1 0.628504 0.676535 0.364443 11.00000 0.03038 0.02471 = 0.02593 0.01429 0.01279 0.01157 C10 1 0.429326 0.514124 0.190115 11.00000 0.03256 0.02403 = 0.03368 0.01561 0.01433 0.01053 C11 1 0.436967 0.062379 0.160136 11.00000 0.03690 0.02735 = 0.03280 0.01313 0.01687 0.00908 AFIX 43 H11 2 0.439413 0.040913 0.093171 11.00000 -1.20000 AFIX 0 C12 1 0.718712 0.657696 0.372568 11.00000 0.02973 0.02148 = 0.02820 0.01368 0.01266 0.01039 C13 1 0.920753 0.770363 0.510174 11.00000 0.03301 0.02994 = 0.04093 0.02022 0.01469 0.01324 AFIX 43 H13 2 0.917150 0.743094 0.556792 11.00000 -1.20000 AFIX 0 C14 1 0.685115 0.197646 0.238297 11.00000 0.03040 0.02394 = 0.02482 0.01399 0.01226 0.01091 C15 1 0.832591 0.778330 0.342748 11.00000 0.03884 0.02991 = 0.03896 0.02007 0.01918 0.01364 AFIX 43 H15 2 0.768232 0.756813 0.274244 11.00000 -1.20000 AFIX 0 C16 1 0.671820 0.036849 0.261841 11.00000 0.03683 0.03204 = 0.04104 0.02353 0.02120 0.01671 AFIX 43 H16 2 0.648892 0.064460 0.313970 11.00000 -1.20000 AFIX 0 C17 1 0.514793 0.187197 0.356941 11.00000 0.03818 0.02841 = 0.03426 0.01666 0.01962 0.01345 AFIX 43 H17 2 0.570503 0.251702 0.425033 11.00000 -1.20000 AFIX 0 C18 1 0.712216 0.878184 0.486307 11.00000 0.03471 0.02718 = 0.03806 0.01613 0.01934 0.01328 AFIX 43 H18 2 0.781033 0.877090 0.527540 11.00000 -1.20000 AFIX 0 C19 1 0.622063 0.781750 0.396408 11.00000 0.03391 0.02628 = 0.03039 0.01699 0.01891 0.01478 C20 1 0.750678 0.282019 0.129678 11.00000 0.03516 0.02196 = 0.03300 0.01481 0.01800 0.01108 C21 1 0.702300 0.975599 0.516027 11.00000 0.04784 0.02378 = 0.04526 0.01502 0.02856 0.01360 AFIX 43 H21 2 0.764144 1.040325 0.577502 11.00000 -1.20000 AFIX 0 C22 1 0.835586 0.293716 0.107920 11.00000 0.03943 0.03341 = 0.03922 0.01744 0.02164 0.00986 AFIX 43 H22 2 0.905408 0.302671 0.160830 11.00000 -1.20000 AFIX 0 C23 1 0.521795 0.786603 0.338899 11.00000 0.03792 0.03030 = 0.03553 0.01778 0.01664 0.01684 AFIX 43 H23 2 0.458762 0.722163 0.279015 11.00000 -1.20000 AFIX 0 C24 1 0.682466 -0.059621 0.235324 11.00000 0.04537 0.03261 = 0.05148 0.02898 0.02418 0.01851 AFIX 43 H24 2 0.668050 -0.096994 0.270405 11.00000 -1.20000 AFIX 0 C25 1 0.863373 0.531899 0.322491 11.00000 0.03057 0.02482 = 0.04822 0.01837 0.02220 0.01165 AFIX 137 H25A 2 0.926597 0.568001 0.399687 11.00000 -1.50000 H25B 2 0.858371 0.583510 0.297375 11.00000 -1.50000 H25C 2 0.872856 0.473524 0.272096 11.00000 -1.50000 AFIX 0 C26 1 0.443402 0.337928 0.264591 11.00000 0.03109 0.02956 = 0.05395 0.02513 0.02338 0.01391 AFIX 137 H26A 2 0.445944 0.344030 0.332754 11.00000 -1.50000 H26B 2 0.410493 0.262030 0.206031 11.00000 -1.50000 H26C 2 0.398813 0.373796 0.237308 11.00000 -1.50000 AFIX 0 C27 1 0.430454 0.123338 0.355941 11.00000 0.04911 0.04053 = 0.04625 0.02826 0.03137 0.02145 AFIX 43 H27 2 0.428382 0.144140 0.423048 11.00000 -1.20000 AFIX 0 C28 1 0.602816 0.978700 0.456501 11.00000 0.05856 0.03055 = 0.05077 0.02599 0.03695 0.02671 AFIX 43 H28 2 0.596415 1.045366 0.476402 11.00000 -1.20000 AFIX 0 C29 1 0.730231 0.052500 0.138410 11.00000 0.05456 0.03473 = 0.04013 0.02369 0.02837 0.02454 AFIX 43 H29 2 0.749386 0.091710 0.106767 11.00000 -1.20000 AFIX 0 C30 1 0.448112 0.475155 0.101187 11.00000 0.03961 0.04404 = 0.03738 0.01945 0.01823 0.00930 AFIX 43 H30 2 0.520271 0.481503 0.117423 11.00000 -1.20000 AFIX 0 C31 1 0.352342 -0.001131 0.158976 11.00000 0.03803 0.02810 = 0.04725 0.01559 0.01842 0.00479 AFIX 43 H31 2 0.296328 -0.065553 0.090981 11.00000 -1.20000 AFIX 0 C32 1 0.322462 0.503419 0.162123 11.00000 0.03595 0.04588 = 0.04377 0.01680 0.01521 0.01967 AFIX 43 H32 2 0.306592 0.528969 0.220463 11.00000 -1.20000 AFIX 0 C33 1 0.648273 0.264657 0.047096 11.00000 0.04234 0.04808 = 0.03734 0.02332 0.01926 0.01961 AFIX 43 H33 2 0.587653 0.252937 0.057778 11.00000 -1.20000 AFIX 0 C34 1 0.820426 0.292583 0.009949 11.00000 0.05962 0.04135 = 0.04826 0.02037 0.03575 0.00904 AFIX 43 H34 2 0.879574 0.300803 -0.003262 11.00000 -1.20000 AFIX 0 C35 1 0.513122 0.884471 0.368192 11.00000 0.04850 0.03993 = 0.04601 0.02675 0.02493 0.02859 AFIX 43 H35 2 0.444805 0.886387 0.326987 11.00000 -1.20000 AFIX 0 C36 1 0.932455 0.851668 0.376280 11.00000 0.05345 0.03844 = 0.06322 0.03222 0.03580 0.01545 AFIX 43 H36 2 0.936457 0.879668 0.330323 11.00000 -1.20000 AFIX 0 C37 1 0.713892 -0.101887 0.158243 11.00000 0.06097 0.03043 = 0.05362 0.02441 0.02837 0.02662 AFIX 43 H37 2 0.718719 -0.169216 0.138462 11.00000 -1.20000 AFIX 0 C38 1 0.349295 0.029203 0.256903 11.00000 0.04225 0.03843 = 0.06136 0.03166 0.03207 0.01391 AFIX 43 H38 2 0.291441 -0.014670 0.256028 11.00000 -1.20000 AFIX 0 C39 1 1.020384 0.844123 0.543611 11.00000 0.03027 0.03223 = 0.05506 0.01930 0.01174 0.00895 AFIX 43 H39 2 1.084662 0.867095 0.612851 11.00000 -1.20000 AFIX 0 C40 1 0.719499 0.279516 -0.067554 11.00000 0.07226 0.04860 = 0.03654 0.02484 0.02574 0.01454 AFIX 43 H40 2 0.709679 0.281140 -0.133027 11.00000 -1.20000 AFIX 0 C41 1 0.738384 -0.045417 0.109840 11.00000 0.07638 0.04295 = 0.05058 0.02705 0.04114 0.03786 AFIX 43 H41 2 0.760674 -0.073726 0.057282 11.00000 -1.20000 AFIX 0 B2 3 0.766798 0.294182 0.246817 11.00000 0.02649 0.02334 = 0.03038 0.01458 0.01294 0.01164 C42 1 0.258931 0.418397 -0.035494 11.00000 0.05251 0.05613 = 0.03803 0.02016 0.00278 0.01006 AFIX 43 H42 2 0.201267 0.386437 -0.111602 11.00000 -1.20000 AFIX 0 C43 1 0.632986 0.264117 -0.049994 11.00000 0.05967 0.06397 = 0.03768 0.02989 0.01887 0.02615 AFIX 43 H43 2 0.562822 0.253121 -0.104356 11.00000 -1.20000 AFIX 0 C44 1 1.026172 0.884127 0.476382 11.00000 0.03663 0.03400 = 0.07389 0.02613 0.02820 0.00719 AFIX 43 H44 2 1.094597 0.933999 0.498904 11.00000 -1.20000 AFIX 0 B1 3 0.529218 0.568834 0.318557 11.00000 0.03097 0.02451 = 0.03183 0.01583 0.01714 0.01430 C45 1 0.363973 0.427274 -0.010574 11.00000 0.05712 0.05691 = 0.03481 0.01963 0.01848 0.00888 AFIX 43 H45 2 0.378776 0.400740 -0.069622 11.00000 -1.20000 AFIX 0 C46 1 0.238414 0.456087 0.050500 11.00000 0.03754 0.06215 = 0.05251 0.01928 0.00726 0.02040 AFIX 43 H46 2 0.166113 0.449775 0.033599 11.00000 -1.20000 AFIX 0 HKLF 4 REM mm1522_a.res in P-1 REM R1 = 0.0345 for 8400 Fo > 4sig(Fo) and 0.0373 for all 9422 data REM 471 parameters refined using 450 restraints END WGHT 0.0652 0.1575 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+1, -z+1 HTAB C25 Cl2_$1 HTAB C25 Cl2 REM Highest difference peak 0.285, deepest hole -0.210, 1-sigma level 0.033 Q1 1 0.4768 0.5408 0.2517 11.00000 0.05 0.29 Q2 1 0.5793 0.6320 0.3515 11.00000 0.05 0.27 Q3 1 0.7660 0.2875 0.1861 11.00000 0.05 0.26 Q4 1 0.7258 0.2355 0.2257 11.00000 0.05 0.25 Q5 1 0.5601 0.1914 0.2574 11.00000 0.05 0.23 Q6 1 0.7192 0.6073 0.3636 11.00000 0.05 0.23 Q7 1 0.6167 0.2797 0.2805 11.00000 0.05 0.23 Q8 1 0.4760 0.1226 0.2114 11.00000 0.05 0.22 Q9 1 0.5592 0.5265 0.3233 11.00000 0.05 0.22 Q10 1 0.7546 0.3501 0.2834 11.00000 0.05 0.22 Q11 1 0.7369 0.5224 0.3395 11.00000 0.05 0.21 Q12 1 0.5808 0.7913 0.3624 11.00000 0.05 0.21 Q13 1 0.8208 0.5204 0.3356 11.00000 0.05 0.21 Q14 1 0.7705 0.6984 0.3936 11.00000 0.05 0.21 Q15 1 0.6008 0.3646 0.3103 11.00000 0.05 0.21 Q16 1 0.5025 0.3617 0.2796 11.00000 0.05 0.21 Q17 1 0.4965 0.5709 0.3605 11.00000 0.05 0.20 Q18 1 0.6661 0.6638 0.3390 11.00000 0.05 0.20 Q19 1 0.6278 0.7227 0.3808 11.00000 0.05 0.20 Q20 1 0.4425 0.5170 0.1395 11.00000 0.05 0.19 ; _shelx_res_checksum 41284 _shelx_hkl_file ; 1 0 -1 556332 980 80912 114.40 -1.61 1.0000 1 0 -1 552493 980 79452 114.40 -1.61 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-4 2699 80 2720 0.05 0.04 1.0000 7 7 4 2689 80 2710 0.05 -0.04 1.0000 7 7 4 2849 90 2870 0.05 -0.04 1.0000 6 7 5 1720 80 1820 -0.29 -0.01 1.0000 5 7 6 2584 80 2290 -0.73 -0.19 1.0000 4 7 7 596 50 500 -0.52 -0.34 1.0000 3 7 8 53 20 40 0.19 -0.17 1.0000 -10 -6 -2 1198 60 1190 -0.04 -0.16 1.0000 10 6 2 987 60 980 -0.04 0.16 1.0000 -9 -6 -3 430 50 420 0.06 -0.07 1.0000 9 6 3 410 40 400 0.06 0.07 1.0000 -8 -6 -4 344 40 340 -0.03 -0.08 1.0000 8 6 4 454 50 450 -0.03 0.08 1.0000 8 6 4 364 40 360 -0.03 0.08 1.0000 -7 -6 -5 1614 70 1700 0.25 -0.17 1.0000 7 6 5 1721 70 1810 0.25 0.17 1.0000 -6 -6 -6 1014 50 820 0.80 -0.15 1.0000 6 6 6 980 60 790 0.80 0.15 1.0000 5 6 7 1840 80 2050 0.57 0.25 1.0000 4 6 8 53 30 40 -0.21 0.17 1.0000 -10 -5 -3 3799 100 3940 0.27 -0.17 1.0000 -9 -5 -4 303 40 250 0.40 -0.06 1.0000 9 5 4 247 40 200 0.40 0.06 1.0000 -8 -5 -5 5130 120 4990 -0.25 -0.07 1.0000 8 5 5 5019 120 4880 -0.25 0.07 1.0000 -7 -5 -6 388 50 560 -0.97 -0.18 1.0000 7 5 6 447 50 630 -0.97 0.18 1.0000 -6 -5 -7 592 50 740 -0.71 -0.03 1.0000 6 5 7 486 50 620 -0.71 0.03 1.0000 5 5 8 1654 70 1700 0.14 -0.08 1.0000 4 5 9 933 50 810 0.52 0.01 1.0000 -10 -4 -4 4073 100 4090 0.03 -0.02 1.0000 -9 -4 -5 219 30 160 0.54 0.16 1.0000 9 4 5 311 30 240 0.54 -0.16 1.0000 -8 -4 -6 22 30 60 0.75 0.08 1.0000 8 4 6 2 30 20 0.75 -0.08 1.0000 -7 -4 -7 1247 60 1140 0.38 -0.27 1.0000 7 4 7 1132 60 1030 0.38 0.27 1.0000 6 4 8 329 40 330 0.03 0.34 1.0000 -9 -3 -6 202 30 230 -0.23 0.06 1.0000 -8 -3 -7 693 50 720 -0.13 -0.11 1.0000 8 3 7 605 50 630 -0.13 0.11 1.0000 7 3 8 1 30 0 -0.04 0.25 1.0000 ; _shelx_hkl_checksum 44573 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Linxtl User' _publ_contact_author_address ; Universit\'e de Montr\'eal D\'epartement de Chimie C.P. 6128, Succ. Centre-ville Montr\'eal, Qu\'ebec Canada, H3C 3J7 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C46 H36 B2 Cl2 N2' _chemical_formula_sum 'C46 H36 B2 Cl2 N2' _chemical_formula_weight 709.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.2200(2) _cell_length_b 18.2840(4) _cell_length_c 16.2870(5) _cell_angle_alpha 90.0000(15) _cell_angle_beta 96.7120(13) _cell_angle_gamma 90.0000(15) _cell_volume 1839.57(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Purple' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.281 _exptl_crystal_F_000 740 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_absorpt_coefficient_mu 0.213 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.954 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14788 _diffrn_reflns_av_unetI/netI 0.0318 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.518 _diffrn_reflns_theta_max 27.507 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 4199 _reflns_number_gt 3545 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.2.4' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.8618P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4199 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.01775(9) 0.96851(4) 0.10876(3) 0.0411(2) Uani 1 1 d . . . . . N1 N 0.6012(3) 1.01629(10) -0.06641(10) 0.0287(4) Uani 1 1 d . . . . . C4 C 0.5905(3) 0.94565(12) -0.04501(12) 0.0301(4) Uani 1 1 d . . . . . C7 C 0.5843(4) 0.96943(13) 0.26026(14) 0.0358(5) Uani 1 1 d . . . . . H7 H 0.6745 0.9450 0.2277 0.043 Uiso 1 1 calc R U . . . C3 C 0.4846(3) 0.92838(12) 0.02460(12) 0.0291(4) Uani 1 1 d . . . . . C2 C 0.4499(3) 0.85719(12) 0.06211(12) 0.0307(4) Uani 1 1 d . . . . . C18 C 0.2685(4) 0.80559(13) 0.18184(13) 0.0335(5) Uani 1 1 d . . . . . C13 C 0.7530(4) 0.76944(13) 0.05399(14) 0.0374(5) Uani 1 1 d . . . . . H13 H 0.8378 0.7984 0.0920 0.045 Uiso 1 1 calc R U . . . C1 C 0.3327(3) 0.86459(12) 0.12771(12) 0.0307(5) Uani 1 1 d . . . . . C6 C 0.3675(4) 0.98030(11) 0.23027(13) 0.0318(5) Uani 1 1 d . . . . . C12 C 0.5397(3) 0.78885(12) 0.02957(12) 0.0306(5) Uani 1 1 d . . . . . C11 C 0.2382(5) 1.01619(14) 0.28172(15) 0.0437(6) Uani 1 1 d . . . . . H11 H 0.0930 1.0243 0.2633 0.052 Uiso 1 1 calc R U . . . B1 B 0.2779(4) 0.94911(14) 0.14064(14) 0.0310(5) Uani 1 1 d . . . . . C5 C 0.6957(4) 0.88972(13) -0.09411(14) 0.0397(5) Uani 1 1 d . . . . . H5A H 0.7329 0.9116 -0.1441 0.060 Uiso 1 1 calc R U . . . H5B H 0.5972 0.8499 -0.1075 0.060 Uiso 1 1 calc R U . . . H5C H 0.8244 0.8718 -0.0622 0.060 Uiso 1 1 calc R U . . . C23 C 0.1053(4) 0.81987(15) 0.23237(14) 0.0407(5) Uani 1 1 d . . . . . H23 H 0.0468 0.8666 0.2332 0.049 Uiso 1 1 calc R U . . . C16 C 0.5041(5) 0.68304(15) -0.05873(16) 0.0497(7) Uani 1 1 d . . . . . H16 H 0.4206 0.6540 -0.0970 0.060 Uiso 1 1 calc R U . . . C17 C 0.4131(4) 0.74491(14) -0.02628(14) 0.0402(5) Uani 1 1 d . . . . . H17 H 0.2686 0.7566 -0.0420 0.048 Uiso 1 1 calc R U . . . C8 C 0.6677(5) 0.99463(16) 0.33828(15) 0.0457(6) Uani 1 1 d . . . . . H8 H 0.8134 0.9878 0.3570 0.055 Uiso 1 1 calc R U . . . C15 C 0.7159(5) 0.66487(15) -0.03440(17) 0.0513(7) Uani 1 1 d . . . . . H15 H 0.7752 0.6236 -0.0564 0.062 Uiso 1 1 calc R U . . . C14 C 0.8415(5) 0.70727(14) 0.02240(17) 0.0461(6) Uani 1 1 d . . . . . H14 H 0.9844 0.6943 0.0394 0.055 Uiso 1 1 calc R U . . . C22 C 0.0296(5) 0.76558(17) 0.28103(16) 0.0520(7) Uani 1 1 d . . . . . H22 H -0.0818 0.7758 0.3127 0.062 Uiso 1 1 calc R U . . . C21 C 0.1187(6) 0.69635(17) 0.28267(17) 0.0562(8) Uani 1 1 d . . . . . H21 H 0.0664 0.6598 0.3147 0.067 Uiso 1 1 calc R U . . . C19 C 0.3592(5) 0.73543(14) 0.18677(15) 0.0465(6) Uani 1 1 d . . . . . H19 H 0.4716 0.7246 0.1558 0.056 Uiso 1 1 calc R U . . . C20 C 0.2856(6) 0.68187(15) 0.23655(16) 0.0557(8) Uani 1 1 d . . . . . H20 H 0.3493 0.6358 0.2389 0.067 Uiso 1 1 calc R U . . . C10 C 0.3213(5) 1.04016(16) 0.35999(16) 0.0535(7) Uani 1 1 d . . . . . H10 H 0.2311 1.0634 0.3935 0.064 Uiso 1 1 calc R U . . . C9 C 0.5343(5) 1.02981(16) 0.38798(15) 0.0519(7) Uani 1 1 d . . . . . H9 H 0.5897 1.0463 0.4402 0.062 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0322(3) 0.0562(4) 0.0362(3) 0.0086(2) 0.0097(2) 0.0034(2) N1 0.0302(9) 0.0312(9) 0.0259(8) 0.0007(7) 0.0091(7) 0.0000(7) C4 0.0304(10) 0.0328(11) 0.0280(10) 0.0006(8) 0.0080(8) 0.0016(8) C7 0.0401(12) 0.0390(12) 0.0295(10) 0.0031(9) 0.0089(9) -0.0026(9) C3 0.0299(10) 0.0310(11) 0.0271(10) -0.0015(8) 0.0070(8) -0.0002(8) C2 0.0330(11) 0.0322(11) 0.0277(10) 0.0002(8) 0.0063(8) -0.0022(8) C18 0.0382(12) 0.0364(12) 0.0261(10) 0.0000(8) 0.0049(8) -0.0085(9) C13 0.0414(12) 0.0337(12) 0.0373(11) 0.0010(9) 0.0061(9) -0.0029(9) C1 0.0306(10) 0.0349(11) 0.0268(9) 0.0000(8) 0.0048(8) -0.0036(8) C6 0.0419(12) 0.0274(11) 0.0282(10) 0.0032(8) 0.0128(9) -0.0012(8) C12 0.0382(11) 0.0295(11) 0.0253(9) 0.0012(8) 0.0091(8) -0.0033(8) C11 0.0504(14) 0.0475(15) 0.0360(12) -0.0035(10) 0.0172(10) 0.0055(11) B1 0.0297(12) 0.0371(13) 0.0279(11) 0.0029(9) 0.0110(9) 0.0008(9) C5 0.0529(14) 0.0340(12) 0.0362(11) 0.0024(9) 0.0214(10) 0.0062(10) C23 0.0402(13) 0.0502(15) 0.0329(11) 0.0025(10) 0.0092(9) -0.0059(10) C16 0.0727(19) 0.0390(14) 0.0382(13) -0.0111(11) 0.0098(12) -0.0118(13) C17 0.0475(13) 0.0409(13) 0.0323(11) -0.0020(9) 0.0051(10) -0.0079(10) C8 0.0507(15) 0.0507(15) 0.0353(12) 0.0065(11) 0.0022(10) -0.0109(12) C15 0.075(2) 0.0328(13) 0.0495(15) -0.0008(11) 0.0227(14) 0.0049(12) C14 0.0493(15) 0.0376(13) 0.0539(15) 0.0080(11) 0.0164(12) 0.0059(11) C22 0.0538(16) 0.0671(19) 0.0377(13) 0.0051(12) 0.0164(11) -0.0165(14) C21 0.082(2) 0.0503(17) 0.0389(13) 0.0030(12) 0.0180(13) -0.0290(15) C19 0.0728(18) 0.0359(13) 0.0341(12) 0.0009(10) 0.0200(12) -0.0057(12) C20 0.096(2) 0.0357(14) 0.0386(13) 0.0008(11) 0.0221(14) -0.0094(14) C10 0.075(2) 0.0527(17) 0.0364(13) -0.0108(11) 0.0218(13) -0.0007(14) C9 0.080(2) 0.0482(16) 0.0283(12) -0.0044(10) 0.0087(12) -0.0175(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 B1 1.885(3) . ? N1 C4 1.341(3) . ? N1 C3 1.363(3) 3_675 ? N1 B1 1.625(3) 3_675 ? C4 C3 1.412(3) . ? C4 C5 1.495(3) . ? C7 C6 1.394(3) . ? C7 C8 1.394(3) . ? C7 H7 0.9300 . ? C3 N1 1.363(3) 3_675 ? C3 C2 1.465(3) . ? C2 C1 1.369(3) . ? C2 C12 1.491(3) . ? C18 C19 1.400(4) . ? C18 C23 1.404(3) . ? C18 C1 1.478(3) . ? C13 C12 1.386(3) . ? C13 C14 1.388(3) . ? C13 H13 0.9300 . ? C1 B1 1.602(3) . ? C6 C11 1.392(3) . ? C6 B1 1.605(3) . ? C12 C17 1.388(3) . ? C11 C10 1.389(4) . ? C11 H11 0.9300 . ? B1 N1 1.625(3) 3_675 ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C23 C22 1.386(3) . ? C23 H23 0.9300 . ? C16 C15 1.372(4) . ? C16 C17 1.396(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C8 C9 1.384(4) . ? C8 H8 0.9300 . ? C15 C14 1.378(4) . ? C15 H15 0.9300 . ? C14 H14 0.9300 . ? C22 C21 1.381(5) . ? C22 H22 0.9300 . ? C21 C20 1.376(4) . ? C21 H21 0.9300 . ? C19 C20 1.383(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C10 C9 1.363(4) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 N1 C3 123.40(17) . 3_675 ? C4 N1 B1 127.56(17) . 3_675 ? C3 N1 B1 108.99(17) 3_675 3_675 ? N1 C4 C3 117.77(19) . . ? N1 C4 C5 118.79(18) . . ? C3 C4 C5 123.4(2) . . ? C6 C7 C8 121.0(2) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? N1 C3 C4 118.82(19) 3_675 . ? N1 C3 C2 111.45(17) 3_675 . ? C4 C3 C2 129.73(19) . . ? C1 C2 C3 110.84(19) . . ? C1 C2 C12 128.03(19) . . ? C3 C2 C12 121.12(18) . . ? C19 C18 C23 116.8(2) . . ? C19 C18 C1 124.6(2) . . ? C23 C18 C1 118.6(2) . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C2 C1 C18 126.8(2) . . ? C2 C1 B1 109.82(18) . . ? C18 C1 B1 123.33(18) . . ? C11 C6 C7 117.4(2) . . ? C11 C6 B1 123.5(2) . . ? C7 C6 B1 119.15(19) . . ? C13 C12 C17 119.4(2) . . ? C13 C12 C2 119.89(19) . . ? C17 C12 C2 120.7(2) . . ? C10 C11 C6 121.5(3) . . ? C10 C11 H11 119.3 . . ? C6 C11 H11 119.3 . . ? C1 B1 C6 113.93(18) . . ? C1 B1 N1 98.84(16) . 3_675 ? C6 B1 N1 113.37(18) . 3_675 ? C1 B1 Cl1 111.17(16) . . ? C6 B1 Cl1 114.05(15) . . ? N1 B1 Cl1 104.07(14) 3_675 . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C22 C23 C18 121.3(3) . . ? C22 C23 H23 119.4 . . ? C18 C23 H23 119.4 . . ? C15 C16 C17 120.3(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C12 C17 C16 119.5(2) . . ? C12 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C20 C21 C22 119.5(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C20 C19 C18 121.6(3) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C21 C20 C19 120.4(3) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C9 C10 C11 120.4(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? _refine_diff_density_max 0.772 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.216 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Compound X CELL 0.71073 6.2200 18.2840 16.2870 90.0000 96.7120 90.0000 ZERR 2 0.0002 0.0004 0.0005 0.0015 0.0013 0.0015 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H B N CL UNIT 92 72 4 4 4 OMIT -3.00 180.00 L.S. 8 ACTA BOND $H FMAP 2 PLAN -20 WGHT 0.088100 0.861800 FVAR 0.30751 CL1 5 -0.017749 0.968507 0.108759 11.00000 0.03225 0.05618 = 0.03624 0.00856 0.00969 0.00339 N1 4 0.601246 1.016291 -0.066412 11.00000 0.03021 0.03121 = 0.02595 0.00068 0.00911 0.00000 C4 1 0.590537 0.945651 -0.045013 11.00000 0.03043 0.03282 = 0.02801 0.00057 0.00804 0.00160 C7 1 0.584253 0.969433 0.260260 11.00000 0.04007 0.03902 = 0.02953 0.00309 0.00888 -0.00263 AFIX 43 H7 2 0.674530 0.945005 0.227737 11.00000 -1.20000 AFIX 0 C3 1 0.484624 0.928380 0.024600 11.00000 0.02995 0.03095 = 0.02711 -0.00153 0.00696 -0.00017 C2 1 0.449874 0.857189 0.062115 11.00000 0.03299 0.03223 = 0.02766 0.00019 0.00630 -0.00220 C18 1 0.268467 0.805585 0.181843 11.00000 0.03820 0.03644 = 0.02610 0.00004 0.00486 -0.00851 C13 1 0.753019 0.769437 0.053986 11.00000 0.04143 0.03374 = 0.03733 0.00105 0.00607 -0.00294 AFIX 43 H13 2 0.837793 0.798405 0.091963 11.00000 -1.20000 AFIX 0 C1 1 0.332708 0.864591 0.127712 11.00000 0.03058 0.03493 = 0.02677 0.00001 0.00475 -0.00359 C6 1 0.367495 0.980301 0.230267 11.00000 0.04190 0.02739 = 0.02818 0.00324 0.01279 -0.00125 C12 1 0.539679 0.788847 0.029574 11.00000 0.03822 0.02954 = 0.02530 0.00120 0.00908 -0.00332 C11 1 0.238203 1.016191 0.281721 11.00000 0.05043 0.04754 = 0.03602 -0.00349 0.01723 0.00550 AFIX 43 H11 2 0.092951 1.024307 0.263303 11.00000 -1.20000 AFIX 0 B1 3 0.277878 0.949112 0.140638 11.00000 0.02967 0.03710 = 0.02794 0.00293 0.01098 0.00078 C5 1 0.695660 0.889715 -0.094111 11.00000 0.05287 0.03396 = 0.03622 0.00235 0.02142 0.00621 AFIX 137 H5A 2 0.732895 0.911569 -0.144149 11.00000 -1.50000 H5B 2 0.597213 0.849891 -0.107520 11.00000 -1.50000 H5C 2 0.824372 0.871769 -0.062191 11.00000 -1.50000 AFIX 0 C23 1 0.105262 0.819865 0.232366 11.00000 0.04024 0.05019 = 0.03286 0.00254 0.00924 -0.00590 AFIX 43 H23 2 0.046798 0.866637 0.233204 11.00000 -1.20000 AFIX 0 C16 1 0.504063 0.683041 -0.058729 11.00000 0.07273 0.03897 = 0.03819 -0.01113 0.00980 -0.01181 AFIX 43 H16 2 0.420623 0.654001 -0.097038 11.00000 -1.20000 AFIX 0 C17 1 0.413073 0.744907 -0.026277 11.00000 0.04746 0.04086 = 0.03229 -0.00197 0.00512 -0.00790 AFIX 43 H17 2 0.268596 0.756590 -0.041984 11.00000 -1.20000 AFIX 0 C8 1 0.667742 0.994634 0.338283 11.00000 0.05065 0.05066 = 0.03525 0.00651 0.00215 -0.01085 AFIX 43 H8 2 0.813417 0.987793 0.356981 11.00000 -1.20000 AFIX 0 C15 1 0.715929 0.664869 -0.034395 11.00000 0.07536 0.03278 = 0.04948 -0.00085 0.02268 0.00490 AFIX 43 H15 2 0.775238 0.623602 -0.056411 11.00000 -1.20000 AFIX 0 C14 1 0.841542 0.707272 0.022402 11.00000 0.04934 0.03756 = 0.05387 0.00804 0.01640 0.00591 AFIX 43 H14 2 0.984418 0.694347 0.039427 11.00000 -1.20000 AFIX 0 C22 1 0.029565 0.765581 0.281035 11.00000 0.05379 0.06709 = 0.03767 0.00508 0.01636 -0.01654 AFIX 43 H22 2 -0.081789 0.775838 0.312727 11.00000 -1.20000 AFIX 0 C21 1 0.118747 0.696351 0.282671 11.00000 0.08186 0.05027 = 0.03895 0.00296 0.01797 -0.02899 AFIX 43 H21 2 0.066421 0.659785 0.314709 11.00000 -1.20000 AFIX 0 C19 1 0.359185 0.735428 0.186772 11.00000 0.07284 0.03585 = 0.03410 0.00092 0.01997 -0.00567 AFIX 43 H19 2 0.471632 0.724578 0.155830 11.00000 -1.20000 AFIX 0 C20 1 0.285600 0.681866 0.236550 11.00000 0.09605 0.03573 = 0.03865 0.00080 0.02214 -0.00937 AFIX 43 H20 2 0.349267 0.635776 0.238870 11.00000 -1.20000 AFIX 0 C10 1 0.321331 1.040162 0.359994 11.00000 0.07487 0.05271 = 0.03644 -0.01082 0.02176 -0.00074 AFIX 43 H10 2 0.231093 1.063409 0.393490 11.00000 -1.20000 AFIX 0 C9 1 0.534311 1.029812 0.387977 11.00000 0.07989 0.04820 = 0.02830 -0.00443 0.00869 -0.01747 AFIX 43 H9 2 0.589690 1.046311 0.440211 11.00000 -1.20000 AFIX 0 HKLF 4 REM Compound X REM R1 = 0.0571 for 3545 Fo > 4sig(Fo) and 0.0747 for all 4199 data REM 236 parameters refined using 0 restraints END WGHT 0.0874 0.8602 REM Highest difference peak 0.772, deepest hole -0.537, 1-sigma level 0.216 Q1 1 -0.0055 1.0122 0.1206 11.00000 0.05 0.77 Q2 1 0.0037 0.7174 0.2606 11.00000 0.05 0.61 Q3 1 -0.0035 0.6660 0.3337 11.00000 0.05 0.53 Q4 1 0.9987 0.8969 -0.1089 11.00000 0.05 0.49 Q5 1 0.1077 0.6377 0.3254 11.00000 0.05 0.47 Q6 1 0.0089 0.7081 0.3881 11.00000 0.05 0.44 Q7 1 -0.0265 0.5991 0.3204 11.00000 0.05 0.43 Q8 1 0.9076 0.8974 -0.0608 11.00000 0.05 0.42 Q9 1 0.9732 0.8431 -0.1271 11.00000 0.05 0.42 Q10 1 0.0083 0.6424 0.2350 11.00000 0.05 0.42 Q11 1 -0.0038 0.9708 0.0420 11.00000 0.05 0.42 Q12 1 -0.0292 0.8132 0.3760 11.00000 0.05 0.41 Q13 1 0.0829 1.0507 0.2569 11.00000 0.05 0.41 Q14 1 -0.0162 0.6242 0.2614 11.00000 0.05 0.41 Q15 1 -0.0611 0.7137 0.3130 11.00000 0.05 0.41 Q16 1 -0.0053 1.0096 0.2405 11.00000 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3.73 0.13 0 3 13 19.24 0.36 0 3 14 0.40 0.12 0 3 15 2.02 0.14 0 3 16 4.32 0.34 0 3 17 1.29 0.23 0 4 -19 0.93 0.26 0 4 -18 11.36 0.70 0 4 -17 -0.58 0.17 0 4 -16 4.75 0.28 0 4 -15 6.04 0.30 0 4 -14 11.45 0.32 0 4 -13 31.93 0.72 0 4 -12 12.50 0.34 0 4 -11 16.28 0.38 0 4 -10 1.15 0.12 0 4 -9 3.01 0.18 0 4 -8 3.83 0.16 0 4 -7 239.32 4.40 0 4 -6 0.21 0.11 0 4 -5 26.50 0.68 0 4 -4 50.09 1.21 0 4 -3 300.30 6.69 0 4 -2 198.92 4.37 0 4 -1 9.58 0.29 0 4 2 164.76 3.65 0 4 3 275.52 4.93 0 4 4 45.16 0.85 0 4 5 26.08 0.52 0 4 6 0.21 0.08 0 4 7 230.40 4.22 0 4 8 3.47 0.12 0 4 9 2.79 0.09 0 4 10 1.98 0.11 0 4 11 14.02 0.28 0 4 12 11.64 0.26 0 4 13 32.54 0.83 0 4 14 12.06 0.42 0 4 15 5.10 0.21 0 4 16 4.58 0.33 0 4 17 0.58 0.18 0 5 -20 2.85 0.28 0 5 -19 0.11 0.18 0 5 -18 6.34 0.61 0 5 -17 11.53 0.71 0 5 -16 0.71 0.20 0 5 -15 0.54 0.24 0 5 -14 1.91 0.14 0 5 -13 5.51 0.21 0 5 -12 65.95 1.34 0 5 -11 2.32 0.15 0 5 -10 3.27 0.16 0 5 -9 1.98 0.14 0 5 -8 2.90 0.17 0 5 -7 53.27 1.06 0 5 -6 106.08 2.48 0 5 -5 19.85 0.51 0 5 -4 94.86 2.16 0 5 -3 0.35 0.16 0 5 -2 952.38 20.69 0 5 -1 115.06 2.65 0 5 1 111.49 3.54 0 5 2 880.97 19.15 0 5 3 -0.19 0.08 0 5 4 86.08 1.64 0 5 5 19.24 0.39 0 5 6 99.16 1.89 0 5 7 48.58 0.97 0 5 8 3.33 0.13 0 5 9 1.82 0.09 0 5 10 2.59 0.11 0 5 11 2.44 0.11 0 5 12 62.50 1.15 0 5 13 5.45 0.24 0 5 14 1.93 0.15 0 5 15 0.01 0.11 0 5 16 0.79 0.21 0 6 -20 1.64 0.30 0 6 -19 0.49 0.22 0 6 -18 33.23 1.20 0 6 -17 5.31 0.53 0 6 -16 8.37 0.57 0 6 -15 2.44 0.24 0 6 -14 1.18 0.22 0 6 -13 57.50 1.15 0 6 -12 2.56 0.16 0 6 -11 0.67 0.13 0 6 -10 13.43 0.35 0 6 -9 12.10 0.37 0 6 -8 15.90 0.38 0 6 -7 47.92 1.18 0 6 -6 238.34 5.37 0 6 -5 30.35 0.77 0 6 -4 3.99 0.20 0 6 -3 48.14 1.14 0 6 -1 135.65 3.09 0 6 0 854.52 26.25 0 6 1 116.01 3.75 0 6 2 256.34 8.00 0 6 3 44.52 1.06 0 6 4 3.10 0.16 0 6 5 26.57 0.55 0 6 6 225.53 4.18 0 6 7 44.82 0.89 0 6 8 15.43 0.35 0 6 9 11.26 0.28 0 6 10 13.09 0.30 0 6 11 0.58 0.09 0 6 12 2.78 0.17 0 6 13 55.79 1.37 0 6 14 0.28 0.12 0 6 15 2.90 0.25 0 6 16 7.01 0.40 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4.28 0 8 2 2.38 0.23 0 8 3 81.74 1.89 0 8 4 105.30 2.40 0 8 5 5.42 0.24 0 8 6 8.28 0.29 0 8 7 105.62 2.47 0 8 8 8.24 0.24 0 8 9 3.53 0.15 0 8 10 8.23 0.27 0 8 11 0.28 0.13 0 8 12 0.80 0.14 0 8 13 8.35 0.29 0 8 14 5.05 0.24 0 8 15 8.87 0.43 0 9 -19 0.43 0.23 0 9 -18 0.18 0.26 0 9 -17 1.51 0.25 0 9 -16 6.72 0.57 0 9 -15 2.46 0.26 0 9 -14 76.62 2.99 0 9 -13 0.12 0.32 0 9 -12 11.95 0.59 0 9 -11 1.28 0.17 0 9 -10 0.51 0.13 0 9 -9 4.84 0.26 0 9 -8 161.28 3.78 0 9 -7 12.93 0.41 0 9 -6 155.39 3.63 0 9 -5 90.72 2.17 0 9 -4 38.45 0.67 0 9 -3 67.96 2.29 0 9 -2 480.39 10.67 0 9 -1 6.59 0.34 0 9 1 7.36 0.40 0 9 2 429.16 13.63 0 9 3 72.15 1.77 0 9 4 38.49 0.98 0 9 5 73.60 1.79 0 9 6 153.98 3.61 0 9 7 13.13 0.41 0 9 8 155.16 5.04 0 9 9 5.16 0.36 0 9 10 0.38 0.23 0 9 11 1.51 0.16 0 9 12 13.48 0.42 0 9 13 0.01 0.20 0 9 14 68.64 1.78 0 10 -19 6.05 0.37 0 10 -18 0.55 0.24 0 10 -17 3.56 0.30 0 10 -16 2.58 0.45 0 10 -15 7.96 0.39 0 10 -14 2.22 0.41 0 10 -13 2.33 0.23 0 10 -12 25.34 0.73 0 10 -10 5.10 0.21 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0.20 0 12 -16 1.52 0.27 0 12 -15 29.65 1.48 0 12 -14 5.34 0.35 0 12 -13 7.33 0.38 0 12 -12 7.94 0.61 0 12 -11 11.11 0.65 0 12 -10 9.96 0.62 0 12 -9 11.32 0.66 0 12 -7 -0.12 0.24 0 12 -6 11.93 0.42 0 12 -5 2.98 0.10 0 12 -4 81.97 1.55 0 12 -3 0.44 0.37 0 12 -1 8.03 0.56 0 12 0 84.97 2.91 0 12 1 6.18 0.49 0 12 2 2.99 0.50 0 12 3 0.03 0.32 0 12 4 85.15 2.92 0 12 5 3.58 0.41 0 12 6 13.39 0.69 0 12 7 -0.10 0.28 0 12 8 37.29 1.43 0 12 9 9.27 0.56 0 12 10 9.94 0.58 0 12 11 9.58 0.51 0 12 12 6.01 0.43 0 12 13 7.01 0.50 0 13 -17 2.05 0.30 0 13 -16 21.05 0.90 0 13 -15 17.48 0.79 0 13 -14 0.35 0.26 0 13 -13 7.94 0.44 0 13 -12 3.80 0.34 0 13 -11 26.83 1.28 0 13 -10 -0.27 0.40 0 13 -9 28.33 1.18 0 13 -8 140.78 4.80 0 13 -5 0.67 0.08 0 13 -4 17.61 0.40 0 13 -3 119.37 4.01 0 13 -1 2.47 0.41 0 13 1 3.65 0.44 0 13 2 1.53 0.41 0 13 3 96.35 3.23 0 13 4 16.82 0.83 0 13 5 1.49 0.35 0 13 6 0.91 0.34 0 13 7 1.64 0.29 0 13 8 137.05 4.74 0 13 9 25.34 1.11 0 13 10 0.49 0.29 0 13 11 23.78 1.11 0 13 12 3.94 0.38 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32.65 0.54 1 -9 -5 111.49 2.14 1 -9 -4 9.74 0.35 1 -9 -3 3.10 0.22 1 -9 -2 134.10 2.49 1 -9 -1 27.76 0.63 1 -9 0 2.64 0.19 1 -9 1 11.84 0.33 1 -9 2 117.10 2.26 1 -9 3 7.55 0.35 1 -9 4 10.55 0.29 1 -9 5 28.06 0.80 1 -9 6 8.87 0.53 1 -9 7 83.98 2.90 1 -9 8 -0.48 0.27 1 -9 9 6.26 0.44 1 -9 10 51.80 1.87 1 -9 11 1.81 0.38 1 -9 12 70.97 2.61 1 -9 13 15.88 0.91 1 -9 14 19.02 0.72 1 -9 15 0.07 0.21 1 -9 16 1.86 0.36 1 -9 17 -0.20 0.32 1 -9 18 12.19 0.84 1 -8 -18 0.25 0.28 1 -8 -15 5.58 0.30 1 -8 -14 0.44 0.14 1 -8 -13 7.90 0.36 1 -8 -12 5.27 0.26 1 -8 -11 354.02 6.54 1 -8 -10 26.34 0.62 1 -8 -9 35.76 0.61 1 -8 -8 7.21 0.19 1 -8 -7 3.34 0.12 1 -8 -6 24.49 0.41 1 -8 -5 36.10 0.65 1 -8 -4 10.08 0.26 1 -8 -3 358.56 6.59 1 -8 -2 105.95 2.02 1 -8 -1 138.46 2.61 1 -8 0 24.49 0.56 1 -8 1 134.40 2.57 1 -8 2 0.82 0.15 1 -8 3 79.41 1.58 1 -8 4 3.30 0.21 1 -8 5 22.74 0.66 1 -8 6 84.74 2.10 1 -8 7 68.43 2.41 1 -8 8 2.43 0.12 1 -8 9 6.29 0.19 1 -8 10 0.37 0.08 1 -8 11 46.35 1.16 1 -8 12 11.79 0.37 1 -8 13 60.47 1.33 1 -8 14 1.43 0.33 1 -8 15 0.92 0.21 1 -8 16 3.22 0.39 1 -8 17 8.48 0.66 1 -8 19 3.59 0.47 1 -7 -20 0.16 0.32 1 -7 -17 10.20 0.67 1 -7 -16 41.74 1.43 1 -7 -15 42.73 1.12 1 -7 -14 8.48 0.39 1 -7 -13 97.53 2.31 1 -7 -12 1.44 0.16 1 -7 -11 1.34 0.17 1 -7 -10 6.22 0.17 1 -7 -9 2.07 0.12 1 -7 -8 14.19 0.29 1 -7 -7 1.71 0.11 1 -7 -6 74.15 1.09 1 -7 -5 219.59 4.03 1 -7 -4 6.22 0.25 1 -7 -3 22.17 0.60 1 -7 -2 249.40 5.59 1 -7 -1 110.96 2.07 1 -7 0 9.31 0.27 1 -7 1 3.45 0.15 1 -7 2 7.01 0.22 1 -7 3 58.47 1.45 1 -7 4 1.67 0.24 1 -7 5 0.94 0.09 1 -7 6 81.28 1.60 1 -7 7 175.31 3.27 1 -7 8 56.64 1.19 1 -7 9 45.24 0.94 1 -7 10 3.64 0.15 1 -7 11 0.34 0.10 1 -7 12 29.55 0.69 1 -7 13 0.39 0.22 1 -7 14 0.03 0.11 1 -7 15 21.99 0.98 1 -7 16 18.47 0.65 1 -7 17 9.64 0.65 1 -7 18 -0.47 0.34 1 -7 19 1.84 0.39 1 -6 -19 9.92 0.82 1 -6 -17 5.10 0.56 1 -6 -16 33.49 1.14 1 -6 -15 29.14 1.02 1 -6 -14 12.03 0.31 1 -6 -13 45.75 1.54 1 -6 -12 37.17 0.96 1 -6 -11 30.62 0.81 1 -6 -10 56.41 1.19 1 -6 -9 69.54 1.16 1 -6 -8 118.61 2.00 1 -6 -7 125.32 1.84 1 -6 -6 262.86 3.69 1 -6 -5 449.70 6.30 1 -6 -4 75.40 1.43 1 -6 -3 719.61 22.23 1 -6 -2 134.40 4.33 1 -6 -1 9.18 0.27 1 -6 0 0.82 0.13 1 -6 1 102.40 1.92 1 -6 2 12.54 0.27 1 -6 3 31.01 0.63 1 -6 4 12.88 0.30 1 -6 5 58.61 1.16 1 -6 6 0.82 0.09 1 -6 7 127.09 2.42 1 -6 8 0.70 0.08 1 -6 9 3.09 0.16 1 -6 10 11.34 0.32 1 -6 11 33.05 0.73 1 -6 12 1.72 0.14 1 -6 13 11.22 0.34 1 -6 14 44.52 0.97 1 -6 15 41.86 1.19 1 -6 16 -0.25 0.22 1 -6 17 25.54 1.18 1 -6 18 20.94 1.19 1 -6 19 -1.32 0.33 1 -5 -19 18.25 1.16 1 -5 -18 2.47 0.40 1 -5 -17 21.73 1.12 1 -5 -15 1.85 0.14 1 -5 -14 1.63 0.09 1 -5 -13 17.08 0.39 1 -5 -12 7.90 0.32 1 -5 -11 0.25 0.12 1 -5 -10 11.19 0.36 1 -5 -9 23.50 0.52 1 -5 -8 10.77 0.27 1 -5 -7 20.65 0.46 1 -5 -6 179.86 2.55 1 -5 -5 47.96 0.75 1 -5 -4 108.77 2.05 1 -5 -3 490.28 10.78 1 -5 -2 27.89 0.70 1 -5 -1 46.27 0.90 1 -5 0 86.50 1.65 1 -5 1 251.70 4.01 1 -5 2 140.70 2.25 1 -5 3 6.01 0.17 1 -5 4 103.04 1.93 1 -5 5 123.48 2.32 1 -5 6 3.05 0.13 1 -5 7 4.56 0.14 1 -5 8 21.52 0.41 1 -5 9 59.58 1.22 1 -5 10 18.17 0.38 1 -5 11 0.26 0.11 1 -5 12 22.53 0.54 1 -5 13 3.00 0.17 1 -5 14 3.39 0.17 1 -5 15 8.59 0.30 1 -5 16 30.21 0.94 1 -5 17 1.05 0.38 1 -5 18 8.37 0.77 1 -5 19 1.21 0.30 1 -5 20 1.43 0.43 1 -4 -19 1.76 0.43 1 -4 -17 15.03 0.91 1 -4 -16 1.70 0.46 1 -4 -15 44.10 1.13 1 -4 -14 0.27 0.08 1 -4 -13 41.09 0.81 1 -4 -12 24.21 0.53 1 -4 -11 147.76 2.69 1 -4 -10 2.37 0.13 1 -4 -9 2.19 0.29 1 -4 -8 31.40 0.78 1 -4 -7 1.07 0.11 1 -4 -6 109.76 2.05 1 -4 -5 26.41 0.46 1 -4 -4 808.92 14.57 1 -4 -2 53.22 1.01 1 -4 -1 106.80 2.03 1 -4 0 0.53 0.10 1 -4 1 1.18 0.10 1 -4 2 132.28 2.11 1 -4 3 579.27 12.79 1 -4 4 7.41 0.21 1 -4 5 28.43 0.51 1 -4 6 13.04 0.25 1 -4 7 8.21 0.20 1 -4 8 11.26 0.23 1 -4 9 0.14 0.08 1 -4 10 219.31 3.56 1 -4 11 8.15 0.23 1 -4 12 7.53 0.30 1 -4 13 12.10 0.35 1 -4 14 1.55 0.22 1 -4 15 3.80 0.20 1 -4 16 1.03 0.25 1 -4 18 4.46 0.44 1 -4 19 1.92 0.42 1 -4 20 0.44 0.38 1 -3 -17 0.81 0.43 1 -3 -16 51.80 2.28 1 -3 -15 0.13 0.05 1 -3 -14 11.49 0.28 1 -3 -13 222.69 4.06 1 -3 -12 22.86 0.48 1 -3 -11 23.07 0.46 1 -3 -10 21.87 0.44 1 -3 -9 165.81 3.01 1 -3 -8 163.05 2.99 1 -3 -7 240.49 5.39 1 -3 -6 2.90 0.23 1 -3 -5 0.99 0.15 1 -3 -4 102.53 1.99 1 -3 -3 314.95 4.94 1 -3 -2 65.64 0.87 1 -3 -1 387.63 8.59 1 -3 0 191.84 3.50 1 -3 1 52.03 0.87 1 -3 2 360.72 5.65 1 -3 3 4.32 0.17 1 -3 4 138.76 2.24 1 -3 6 -0.18 0.07 1 -3 7 120.55 1.74 1 -3 8 66.87 0.98 1 -3 9 32.62 0.54 1 -3 10 15.65 0.35 1 -3 11 23.93 0.49 1 -3 12 0.18 0.10 1 -3 13 3.31 0.16 1 -3 14 4.02 0.25 1 -3 15 27.23 0.69 1 -3 16 6.72 0.26 1 -3 19 8.45 0.75 1 -3 20 0.32 0.38 1 -2 -16 1.05 0.34 1 -2 -15 19.35 0.42 1 -2 -14 39.44 0.79 1 -2 -13 8.67 0.20 1 -2 -12 38.06 0.78 1 -2 -11 65.79 1.54 1 -2 -10 102.59 1.92 1 -2 -9 11.09 0.23 1 -2 -8 73.01 1.35 1 -2 -7 387.51 6.85 1 -2 -6 121.52 2.23 1 -2 -5 431.39 9.46 1 -2 -4 0.60 0.19 1 -2 -3 1.64 0.10 1 -2 -2 738.23 16.15 1 -2 -1 67.18 2.28 1 -2 2 151.87 2.81 1 -2 3 131.41 1.89 1 -2 5 7.94 0.18 1 -2 6 1.30 0.08 1 -2 7 57.94 0.87 1 -2 8 36.21 0.57 1 -2 9 13.36 0.25 1 -2 10 40.84 0.65 1 -2 11 5.67 0.20 1 -2 12 2.95 0.16 1 -2 13 5.81 0.21 1 -2 14 75.90 1.60 1 -2 15 0.03 0.12 1 -2 16 0.85 0.14 1 -2 17 8.87 0.60 1 -2 18 1.36 0.33 1 -2 19 10.65 0.74 1 -1 -16 27.13 0.63 1 -1 -15 5.48 0.16 1 -1 -14 0.42 0.07 1 -1 -13 122.64 2.31 1 -1 -12 0.22 0.08 1 -1 -11 22.50 0.48 1 -1 -10 5.37 0.13 1 -1 -9 230.59 3.65 1 -1 -8 0.11 0.04 1 -1 -7 9.70 0.32 1 -1 -6 58.27 1.45 1 -1 -5 277.94 6.22 1 -1 -4 177.58 2.78 1 -1 -3 231.84 4.14 1 -1 -2 897.95 27.48 1 -1 -1 270.61 4.89 1 -1 0 84.39 1.98 1 -1 1 218.46 6.82 1 -1 4 251.00 5.61 1 -1 5 269.98 3.85 1 -1 6 9.60 0.20 1 -1 7 58.66 0.87 1 -1 8 7.29 0.15 1 -1 9 160.96 2.33 1 -1 10 1.68 0.11 1 -1 11 11.82 0.28 1 -1 12 5.14 0.20 1 -1 13 0.47 0.14 1 -1 14 2.90 0.18 1 -1 15 43.22 0.96 1 -1 16 0.43 0.18 1 -1 17 1.31 0.40 1 0 -16 61.26 1.98 1 0 -14 0.69 0.07 1 0 -12 12.46 0.29 1 0 -10 155.95 2.53 1 0 -8 145.92 2.37 1 0 -6 30.31 0.52 1 0 -4 289.12 6.35 1 0 -2 33.01 1.05 1 0 0 -0.09 0.04 1 0 4 10.24 0.16 1 0 6 12.34 0.20 1 0 8 103.75 1.42 1 0 10 440.36 8.10 1 0 12 3.39 0.15 1 0 14 1.85 0.14 1 0 16 1.01 0.20 1 1 -17 31.47 1.06 1 1 -16 27.56 0.96 1 1 -15 5.16 0.16 1 1 -14 0.57 0.10 1 1 -13 120.55 2.29 1 1 -12 0.14 0.12 1 1 -11 24.02 0.62 1 1 -10 5.37 0.22 1 1 -9 240.00 5.39 1 1 -8 -0.04 0.10 1 1 -7 9.82 0.30 1 1 -6 56.50 1.33 1 1 -5 271.44 6.04 1 1 -4 185.42 4.13 1 1 -3 243.94 4.45 1 1 0 83.98 1.56 1 1 1 226.29 7.04 1 1 3 1103.34 34.03 1 1 4 257.96 3.66 1 1 5 269.36 3.74 1 1 6 9.78 0.20 1 1 7 60.32 0.88 1 1 8 7.67 0.16 1 1 9 157.53 2.14 1 1 10 3.99 0.14 1 1 11 12.63 0.29 1 1 12 4.97 0.17 1 1 13 1.14 0.13 1 1 14 3.16 0.21 1 1 15 38.42 1.10 1 1 16 0.72 0.25 1 2 -17 17.66 0.56 1 2 -16 2.06 0.19 1 2 -15 18.85 0.44 1 2 -14 40.84 1.05 1 2 -13 9.51 0.33 1 2 -12 38.57 0.98 1 2 -11 67.96 1.62 1 2 -10 107.85 2.56 1 2 -9 11.51 0.37 1 2 -8 76.40 1.77 1 2 -7 389.50 8.61 1 2 -6 124.82 2.83 1 2 -5 491.40 10.80 1 2 -4 0.65 0.09 1 2 -3 1.69 0.09 1 2 -2 812.34 14.42 1 2 -1 75.08 2.47 1 2 1 120.13 3.81 1 2 2 149.54 2.71 1 2 3 136.46 3.10 1 2 4 1268.33 38.97 1 2 5 8.26 0.18 1 2 6 1.47 0.11 1 2 7 56.17 0.95 1 2 8 34.78 0.56 1 2 9 12.75 0.25 1 2 10 39.05 0.63 1 2 11 5.16 0.19 1 2 12 2.89 0.19 1 2 13 5.16 0.22 1 2 14 71.99 1.99 1 2 15 0.36 0.12 1 3 -18 12.14 0.42 1 3 -17 0.02 0.13 1 3 -16 48.75 1.28 1 3 -14 11.49 0.41 1 3 -13 228.10 5.25 1 3 -12 24.49 0.66 1 3 -11 25.09 0.67 1 3 -10 23.59 0.98 1 3 -9 169.91 3.13 1 3 -8 168.43 3.86 1 3 -7 242.06 5.41 1 3 -6 1.44 0.13 1 3 -5 1.14 0.09 1 3 -4 99.04 1.57 1 3 -3 319.56 7.12 1 3 -2 72.04 1.34 1 3 -1 402.46 7.23 1 3 0 211.23 3.86 1 3 1 52.67 1.01 1 3 2 369.42 6.69 1 3 3 5.21 0.17 1 3 4 141.90 3.24 1 3 5 974.37 17.37 1 3 6 0.20 0.11 1 3 7 116.62 1.71 1 3 8 63.81 0.96 1 3 9 32.87 0.51 1 3 10 12.79 0.25 1 3 11 21.64 0.41 1 3 12 0.77 0.10 1 3 13 3.09 0.15 1 3 14 4.50 0.19 1 3 15 23.72 0.58 1 4 -19 -0.15 0.40 1 4 -18 31.01 0.92 1 4 -17 15.45 0.55 1 4 -16 2.49 0.21 1 4 -15 48.01 1.27 1 4 -14 0.94 0.16 1 4 -13 42.03 0.86 1 4 -12 24.52 0.53 1 4 -11 152.18 3.51 1 4 -10 2.77 0.17 1 4 -9 3.17 0.14 1 4 -8 33.01 0.84 1 4 -7 0.82 0.10 1 4 -6 111.42 2.54 1 4 -5 24.59 0.50 1 4 -4 764.40 23.61 1 4 -2 53.22 1.01 1 4 -1 112.22 2.08 1 4 0 0.18 0.11 1 4 1 0.85 0.11 1 4 2 134.32 2.49 1 4 3 545.53 9.75 1 4 4 7.14 0.22 1 4 5 28.22 0.71 1 4 6 13.23 0.32 1 4 7 8.30 0.24 1 4 8 10.65 0.29 1 4 9 0.17 0.05 1 4 10 222.41 3.58 1 4 11 8.41 0.20 1 4 12 7.43 0.19 1 4 13 10.42 0.29 1 4 14 1.57 0.11 1 4 15 2.80 0.29 1 5 -20 4.19 0.58 1 5 -19 18.69 1.20 1 5 -18 0.19 0.19 1 5 -17 26.44 0.81 1 5 -16 5.28 0.28 1 5 -15 1.97 0.20 1 5 -14 2.13 0.20 1 5 -13 17.19 0.42 1 5 -12 7.28 0.24 1 5 -11 0.54 0.12 1 5 -10 12.06 0.31 1 5 -9 22.95 0.52 1 5 -8 9.80 0.32 1 5 -7 21.17 0.47 1 5 -6 185.07 4.22 1 5 -5 47.96 1.14 1 5 -4 114.18 2.57 1 5 -2 26.90 0.66 1 5 -1 48.66 0.93 1 5 0 98.85 1.89 1 5 1 273.74 5.02 1 5 2 147.76 2.77 1 5 3 6.04 0.23 1 5 4 99.04 1.89 1 5 5 125.17 2.34 1 5 6 3.30 0.15 1 5 7 4.13 0.18 1 5 8 22.80 0.63 1 5 9 61.85 1.24 1 5 10 18.04 0.43 1 5 11 0.53 0.18 1 5 12 19.32 0.42 1 5 13 2.61 0.11 1 5 14 4.41 0.16 1 5 15 7.66 0.44 1 6 -20 1.14 0.53 1 6 -18 0.21 0.20 1 6 -17 3.12 0.27 1 6 -16 40.20 1.08 1 6 -15 33.31 0.91 1 6 -14 10.86 0.38 1 6 -13 44.52 0.93 1 6 -12 37.40 0.77 1 6 -11 29.38 0.79 1 6 -10 60.27 1.18 1 6 -9 68.17 1.62 1 6 -8 120.89 2.85 1 6 -7 133.88 3.07 1 6 -6 263.79 8.22 1 6 -5 463.90 10.08 1 6 -4 75.57 1.70 1 6 -3 781.28 13.97 1 6 -2 149.38 2.71 1 6 -1 9.01 0.23 1 6 0 0.16 0.09 1 6 1 109.83 2.06 1 6 2 13.00 0.32 1 6 3 30.76 0.63 1 6 4 11.60 0.30 1 6 5 53.87 1.07 1 6 6 0.12 0.14 1 6 7 126.03 2.98 1 6 8 0.53 0.14 1 6 9 1.66 0.17 1 6 10 10.80 0.40 1 6 11 31.01 0.92 1 6 12 1.17 0.18 1 6 13 11.56 0.43 1 6 14 43.93 1.59 1 6 15 38.81 1.50 1 7 -20 -0.12 0.41 1 7 -19 1.52 0.21 1 7 -18 4.50 0.30 1 7 -17 9.41 0.43 1 7 -16 48.97 1.28 1 7 -15 46.23 1.25 1 7 -14 9.62 0.39 1 7 -13 97.91 1.94 1 7 -12 1.35 0.16 1 7 -11 0.76 0.14 1 7 -10 5.85 0.34 1 7 -9 2.16 0.14 1 7 -8 13.64 0.35 1 7 -7 1.76 0.15 1 7 -6 78.01 2.57 1 7 -5 243.35 5.33 1 7 -4 7.52 0.23 1 7 -3 23.84 0.49 1 7 -2 275.73 5.04 1 7 -1 123.41 2.32 1 7 0 8.08 0.23 1 7 1 2.17 0.14 1 7 2 6.87 0.22 1 7 3 56.79 1.10 1 7 4 1.77 0.13 1 7 5 0.86 0.15 1 7 6 68.64 2.41 1 7 7 171.48 4.06 1 7 8 60.12 2.26 1 7 9 45.54 1.79 1 7 10 3.80 0.23 1 7 11 0.19 0.16 1 7 12 28.70 0.85 1 7 14 1.29 0.26 1 7 15 18.52 0.87 1 8 -19 1.09 0.22 1 8 -18 2.48 0.48 1 8 -17 12.25 0.51 1 8 -16 1.19 0.23 1 8 -15 6.12 0.34 1 8 -14 0.13 0.21 1 8 -13 8.05 0.29 1 8 -12 5.07 0.26 1 8 -11 377.86 8.48 1 8 -10 28.02 0.77 1 8 -9 39.64 0.84 1 8 -8 7.52 0.31 1 8 -7 4.52 0.23 1 8 -6 25.12 0.60 1 8 -5 36.48 0.88 1 8 -4 10.92 0.27 1 8 -3 420.55 7.52 1 8 -2 124.12 2.33 1 8 -1 151.32 2.80 1 8 0 23.87 0.53 1 8 1 134.10 3.08 1 8 2 0.59 0.16 1 8 3 81.05 1.54 1 8 4 3.09 0.20 1 8 5 23.87 0.65 1 8 6 80.54 1.99 1 8 7 65.90 2.26 1 8 8 2.60 0.35 1 8 9 7.07 0.45 1 8 10 0.06 0.29 1 8 11 47.00 1.78 1 8 12 10.96 0.61 1 8 13 65.13 2.40 1 8 14 3.01 0.34 1 9 -19 0.72 0.25 1 9 -18 2.14 0.26 1 9 -17 1.57 0.24 1 9 -16 10.98 0.44 1 9 -15 10.16 0.44 1 9 -14 11.69 0.48 1 9 -13 0.33 0.25 1 9 -12 115.87 2.25 1 9 -11 23.84 0.71 1 9 -10 52.81 1.98 1 9 -9 34.82 0.90 1 9 -8 -0.28 0.17 1 9 -6 34.34 0.81 1 9 -5 119.09 2.69 1 9 -4 10.55 0.29 1 9 -3 3.04 0.17 1 9 -2 157.13 2.93 1 9 -1 30.84 0.77 1 9 0 2.47 0.21 1 9 1 11.51 0.37 1 9 2 116.35 2.66 1 9 3 7.21 0.27 1 9 4 10.77 0.37 1 9 5 29.14 0.82 1 9 6 6.54 0.45 1 9 7 84.16 2.84 1 9 8 -0.46 0.26 1 9 9 5.67 0.36 1 9 10 48.80 1.81 1 9 11 3.48 0.41 1 9 12 65.33 2.50 1 9 13 16.36 0.79 1 9 14 18.09 0.86 1 10 -19 3.36 0.30 1 10 -18 0.51 0.23 1 10 -17 21.43 0.85 1 10 -16 -0.76 0.23 1 10 -15 13.41 0.56 1 10 -14 11.64 0.50 1 10 -13 7.87 0.41 1 10 -12 6.68 0.29 1 10 -11 179.86 3.48 1 10 -10 63.81 1.62 1 10 -9 39.01 0.83 1 10 -8 1.23 0.18 1 10 -6 0.32 0.06 1 10 -5 81.97 1.83 1 10 -4 8.35 0.26 1 10 -3 208.57 4.75 1 10 -2 16.87 0.42 1 10 -1 28.26 0.71 1 10 0 24.12 0.65 1 10 1 1.74 0.14 1 10 2 -0.04 0.14 1 10 3 37.17 0.77 1 10 4 46.48 1.77 1 10 5 54.15 1.91 1 10 6 19.63 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2 -15 9 9.51 0.74 2 -15 10 0.51 0.48 2 -15 11 7.69 0.68 2 -15 13 -0.82 0.29 2 -15 14 5.16 0.63 2 -14 -16 8.05 0.79 2 -14 -15 5.17 0.33 2 -14 -14 8.45 0.44 2 -14 -13 0.83 0.20 2 -14 -12 7.57 0.40 2 -14 -11 1.58 0.27 2 -14 -10 13.64 0.56 2 -14 -9 -0.15 0.18 2 -14 -8 48.89 1.33 2 -14 -7 50.09 1.34 2 -14 -6 4.37 0.24 2 -14 -5 0.87 0.13 2 -14 -4 27.23 0.69 2 -14 -3 1.51 0.27 2 -14 -1 51.17 1.90 2 -14 0 1.58 0.46 2 -14 1 1.30 0.28 2 -14 2 4.32 0.47 2 -14 3 20.54 0.89 2 -14 4 28.73 1.22 2 -14 5 15.70 0.88 2 -14 6 10.22 0.71 2 -14 7 6.77 0.59 2 -14 8 1.25 0.36 2 -14 9 0.10 0.31 2 -14 10 4.67 0.55 2 -14 11 20.14 1.02 2 -14 12 -0.77 0.28 2 -14 13 8.24 0.73 2 -14 15 1.57 0.45 2 -13 -17 11.09 0.91 2 -13 -16 2.61 0.56 2 -13 -15 3.03 0.25 2 -13 -14 6.64 0.34 2 -13 -13 0.32 0.16 2 -13 -12 1.44 0.25 2 -13 -11 9.94 0.46 2 -13 -10 0.09 0.21 2 -13 -9 43.10 1.16 2 -13 -8 6.46 0.27 2 -13 -7 2.80 0.20 2 -13 -6 83.46 1.50 2 -13 -5 0.78 0.15 2 -13 -4 6.26 0.25 2 -13 -3 2.56 0.22 2 -13 -2 37.79 1.01 2 -13 -1 16.23 0.79 2 -13 0 3.50 0.43 2 -13 1 5.75 0.50 2 -13 2 11.47 0.64 2 -13 3 -0.12 0.25 2 -13 4 3.19 0.50 2 -13 5 63.20 2.31 2 -13 6 32.47 1.30 2 -13 7 0.53 0.44 2 -13 9 4.57 0.54 2 -13 10 -0.36 0.30 2 -13 12 5.88 0.58 2 -13 13 0.72 0.45 2 -13 14 1.81 0.37 2 -13 15 -0.05 0.39 2 -12 -17 -0.04 0.34 2 -12 -16 0.19 0.47 2 -12 -15 6.43 0.31 2 -12 -14 24.34 0.78 2 -12 -13 10.06 0.40 2 -12 -12 7.16 0.35 2 -12 -11 0.26 0.22 2 -12 -10 1.44 0.23 2 -12 -9 4.48 0.21 2 -12 -8 10.26 0.30 2 -12 -7 72.90 1.30 2 -12 -6 17.53 0.40 2 -12 -5 17.16 0.47 2 -12 -4 8.23 0.27 2 -12 -3 24.46 0.59 2 -12 -2 0.47 0.26 2 -12 -1 45.67 1.03 2 -12 0 17.64 0.48 2 -12 1 9.53 0.59 2 -12 2 5.78 0.46 2 -12 3 10.80 0.58 2 -12 4 1.23 0.40 2 -12 6 15.55 0.80 2 -12 7 26.37 1.10 2 -12 8 -0.01 0.40 2 -12 9 17.69 0.90 2 -12 10 28.39 1.28 2 -12 11 -0.68 0.38 2 -12 12 1.00 0.44 2 -12 13 1.95 0.34 2 -12 14 15.40 1.02 2 -12 15 0.89 0.34 2 -11 -17 1.98 0.38 2 -11 -16 4.21 0.58 2 -11 -15 -0.11 0.14 2 -11 -14 0.75 0.16 2 -11 -13 0.44 0.16 2 -11 -12 8.86 0.43 2 -11 -11 33.23 0.95 2 -11 -10 -0.12 0.17 2 -11 -9 34.82 0.82 2 -11 -8 17.58 0.40 2 -11 -7 0.04 0.12 2 -11 -6 128.09 2.22 2 -11 -5 6.71 0.25 2 -11 -4 22.23 0.48 2 -11 -3 10.57 0.31 2 -11 -2 90.36 1.80 2 -11 -1 0.64 0.17 2 -11 0 4.87 0.28 2 -11 1 19.63 0.64 2 -11 2 22.29 0.90 2 -11 3 25.86 1.06 2 -11 4 21.00 0.90 2 -11 5 35.34 1.39 2 -11 6 21.52 1.00 2 -11 7 4.78 0.51 2 -11 8 6.76 0.56 2 -11 9 6.30 0.35 2 -11 10 2.19 0.48 2 -11 11 11.53 0.73 2 -11 12 12.14 0.53 2 -11 13 11.62 0.52 2 -11 14 2.42 0.46 2 -11 15 -0.22 0.39 2 -10 -18 7.52 0.75 2 -10 -17 3.41 0.47 2 -10 -16 0.86 0.44 2 -10 -15 0.29 0.41 2 -10 -14 1.10 0.16 2 -10 -13 49.37 1.29 2 -10 -12 4.69 0.30 2 -10 -11 0.08 0.14 2 -10 -10 27.52 0.73 2 -10 -9 0.54 0.13 2 -10 -8 0.46 0.12 2 -10 -7 79.19 1.41 2 -10 -6 8.80 0.24 2 -10 -5 10.04 0.26 2 -10 -4 3.30 0.13 2 -10 -3 2.53 0.15 2 -10 -2 3.75 0.14 2 -10 -1 52.12 1.10 2 -10 0 53.50 1.39 2 -10 1 12.10 0.40 2 -10 2 7.04 0.34 2 -10 3 39.92 1.52 2 -10 4 2.33 0.43 2 -10 5 0.05 0.22 2 -10 6 12.12 0.66 2 -10 7 0.22 0.12 2 -10 8 0.16 0.11 2 -10 9 18.06 0.46 2 -10 10 18.33 0.57 2 -10 11 81.22 1.71 2 -10 12 2.88 0.26 2 -10 13 4.50 0.30 2 -10 14 36.86 1.08 2 -10 15 1.46 0.44 2 -9 -19 6.12 0.61 2 -9 -17 1.28 0.36 2 -9 -16 29.51 1.44 2 -9 -14 3.49 0.17 2 -9 -13 1.46 0.19 2 -9 -12 1.47 0.16 2 -9 -11 2.67 0.21 2 -9 -10 9.66 0.32 2 -9 -9 -0.19 0.12 2 -9 -8 62.70 1.00 2 -9 -7 106.80 1.63 2 -9 -6 152.57 2.58 2 -9 -5 10.51 0.23 2 -9 -4 19.52 0.34 2 -9 -3 -0.09 0.09 2 -9 -2 94.68 1.60 2 -9 -1 24.62 0.47 2 -9 0 144.10 2.73 2 -9 1 34.30 0.81 2 -9 2 66.51 1.34 2 -9 3 30.84 0.70 2 -9 4 28.33 0.77 2 -9 5 35.23 0.90 2 -9 6 1.89 0.17 2 -9 7 9.43 0.33 2 -9 8 19.07 0.47 2 -9 9 6.77 0.23 2 -9 10 21.55 0.47 2 -9 11 2.89 0.16 2 -9 12 41.37 0.89 2 -9 13 2.49 0.24 2 -9 14 11.00 0.48 2 -9 15 4.21 0.29 2 -9 16 26.47 1.50 2 -8 -19 1.12 0.50 2 -8 -16 7.55 0.63 2 -8 -14 0.66 0.07 2 -8 -13 1.19 0.08 2 -8 -12 25.54 0.54 2 -8 -11 16.38 0.49 2 -8 -10 8.76 0.34 2 -8 -9 15.40 0.30 2 -8 -8 54.24 0.89 2 -8 -7 115.87 1.77 2 -8 -6 27.99 0.54 2 -8 -5 1.52 0.09 2 -8 -4 18.25 0.30 2 -8 -3 1.22 0.12 2 -8 -2 195.10 3.18 2 -8 -1 349.99 6.39 2 -8 0 7.80 0.39 2 -8 1 31.58 0.68 2 -8 2 1.97 0.13 2 -8 3 16.44 0.36 2 -8 4 22.77 0.45 2 -8 5 0.66 0.12 2 -8 6 3.80 0.17 2 -8 7 45.75 0.98 2 -8 8 3.54 0.16 2 -8 9 22.86 0.48 2 -8 10 3.24 0.16 2 -8 11 0.10 0.10 2 -8 12 4.33 0.20 2 -8 13 2.68 0.25 2 -8 14 0.57 0.19 2 -8 15 15.45 0.60 2 -8 16 1.54 0.25 2 -7 -19 1.58 0.36 2 -7 -16 19.77 1.04 2 -7 -14 -0.11 0.26 2 -7 -13 8.10 0.59 2 -7 -12 122.85 2.31 2 -7 -11 4.13 0.15 2 -7 -10 95.23 2.22 2 -7 -9 7.78 0.28 2 -7 -8 8.26 0.20 2 -7 -7 24.18 0.37 2 -7 -6 148.76 2.16 2 -7 -5 25.12 0.41 2 -7 -4 -0.17 0.10 2 -7 -3 210.50 3.03 2 -7 -2 74.26 1.09 2 -7 -1 2.19 0.12 2 -7 0 21.76 0.41 2 -7 1 27.29 0.50 2 -7 2 6.34 0.21 2 -7 3 11.19 0.28 2 -7 4 203.49 3.34 2 -7 5 2.82 0.16 2 -7 6 0.55 0.09 2 -7 7 51.08 0.90 2 -7 8 10.90 0.23 2 -7 9 11.86 0.26 2 -7 10 0.76 0.10 2 -7 11 0.83 0.11 2 -7 12 24.90 0.60 2 -7 13 0.40 0.11 2 -7 14 4.58 0.37 2 -7 15 2.83 0.27 2 -7 16 13.06 0.53 2 -7 17 26.37 1.40 2 -6 -18 2.13 0.39 2 -6 -17 1.14 0.33 2 -6 -16 34.97 1.61 2 -6 -14 2.98 0.44 2 -6 -13 52.53 2.11 2 -6 -12 11.30 0.64 2 -6 -11 127.09 2.35 2 -6 -10 2.86 0.11 2 -6 -9 39.64 0.96 2 -6 -8 8.26 0.27 2 -6 -7 59.49 0.98 2 -6 -6 159.84 2.96 2 -6 -5 16.18 0.31 2 -6 -4 353.79 5.00 2 -6 -3 27.32 0.46 2 -6 -2 -0.06 0.09 2 -6 -1 3.28 0.13 2 -6 0 1.43 0.09 2 -6 1 133.37 1.90 2 -6 2 169.09 2.71 2 -6 3 66.15 1.13 2 -6 4 72.52 1.24 2 -6 5 98.28 1.44 2 -6 6 35.12 0.56 2 -6 7 36.71 0.65 2 -6 8 0.11 0.08 2 -6 9 10.16 0.22 2 -6 10 1.70 0.10 2 -6 11 21.29 0.44 2 -6 12 3.47 0.17 2 -6 13 0.22 0.13 2 -6 14 2.15 0.24 2 -6 15 0.25 0.22 2 -6 16 11.69 0.45 2 -6 17 3.45 0.36 2 -5 -17 2.18 0.50 2 -5 -16 41.37 1.79 2 -5 -15 19.83 1.07 2 -5 -14 5.97 0.59 2 -5 -13 22.92 1.06 2 -5 -12 157.21 5.31 2 -5 -10 51.53 0.95 2 -5 -9 226.86 4.10 2 -5 -8 47.35 1.13 2 -5 -7 29.76 0.72 2 -5 -6 185.59 2.93 2 -5 -5 27.62 0.50 2 -5 -4 28.90 0.51 2 -5 -3 14.98 0.29 2 -5 -2 20.28 0.37 2 -5 -1 77.51 1.06 2 -5 0 33.31 0.55 2 -5 1 2.89 0.14 2 -5 2 6.05 0.19 2 -5 3 19.83 0.37 2 -5 4 0.33 0.06 2 -5 5 18.74 0.30 2 -5 6 184.64 2.41 2 -5 7 0.58 0.08 2 -5 8 11.69 0.24 2 -5 9 6.84 0.17 2 -5 10 10.80 0.25 2 -5 11 2.34 0.17 2 -5 12 65.69 1.38 2 -5 13 14.19 0.41 2 -5 14 3.77 0.18 2 -5 15 6.38 0.34 2 -5 16 1.53 0.25 2 -5 17 0.54 0.21 2 -4 -17 1.06 0.33 2 -4 -16 3.31 0.44 2 -4 -15 18.09 0.97 2 -4 -14 83.87 3.19 2 -4 -13 107.58 3.94 2 -4 -12 0.81 0.25 2 -4 -11 8.21 0.51 2 -4 -10 112.56 3.89 2 -4 -9 21.26 0.88 2 -4 -8 304.81 5.52 2 -4 -7 15.65 0.43 2 -4 -6 260.51 4.70 2 -4 -5 1.21 0.10 2 -4 -4 0.42 0.08 2 -4 -3 1.20 0.10 2 -4 -2 0.27 0.09 2 -4 -1 89.82 1.32 2 -4 0 128.95 2.08 2 -4 1 1.75 0.13 2 -4 2 65.13 1.12 2 -4 3 143.26 2.04 2 -4 4 205.84 3.27 2 -4 5 163.22 2.34 2 -4 6 1.02 0.07 2 -4 7 1.43 0.08 2 -4 8 16.18 0.28 2 -4 9 82.25 1.26 2 -4 10 22.47 0.42 2 -4 11 60.22 0.98 2 -4 12 22.50 0.57 2 -4 13 1.17 0.17 2 -4 14 12.84 0.50 2 -4 15 0.25 0.21 2 -4 16 18.12 0.97 2 -3 -15 0.10 0.30 2 -3 -14 25.79 1.29 2 -3 -13 14.09 0.74 2 -3 -12 19.77 0.93 2 -3 -11 20.71 0.92 2 -3 -10 1.16 0.32 2 -3 -9 6.08 0.41 2 -3 -8 14.16 0.62 2 -3 -7 17.45 0.34 2 -3 -6 2.27 0.13 2 -3 -5 465.67 10.24 2 -3 -4 34.45 0.59 2 -3 -3 254.62 3.63 2 -3 -2 113.50 1.62 2 -3 -1 109.63 1.59 2 -3 0 28.29 0.44 2 -3 1 153.82 2.51 2 -3 2 324.79 5.93 2 -3 3 133.15 2.12 2 -3 4 140.85 2.63 2 -3 5 3.62 0.12 2 -3 6 108.77 1.78 2 -3 7 0.19 0.06 2 -3 8 55.46 0.85 2 -3 9 28.90 0.54 2 -3 10 0.41 0.09 2 -3 11 11.09 0.25 2 -3 12 42.60 0.78 2 -3 13 9.84 0.32 2 -3 14 6.27 0.25 2 -3 15 0.17 0.15 2 -3 16 9.43 0.60 2 -2 -12 10.44 0.65 2 -2 -11 0.37 0.22 2 -2 -10 14.16 0.71 2 -2 -9 18.41 0.84 2 -2 -8 25.54 1.02 2 -2 -7 1.15 0.21 2 -2 -6 177.49 3.20 2 -2 -5 32.54 0.79 2 -2 -4 448.63 8.04 2 -2 -3 9.90 0.20 2 -2 -2 11.43 0.23 2 -2 -1 77.45 1.28 2 -2 0 122.99 2.03 2 -2 1 49.28 0.84 2 -2 2 374.42 6.73 2 -2 3 53.36 1.02 2 -2 4 3.39 0.12 2 -2 5 271.13 3.85 2 -2 6 18.20 0.32 2 -2 7 81.00 1.20 2 -2 8 8.86 0.23 2 -2 9 3.81 0.14 2 -2 10 65.43 1.13 2 -2 11 2.75 0.14 2 -2 12 8.39 0.28 2 -2 13 4.91 0.21 2 -2 14 35.57 0.79 2 -2 15 4.62 0.29 2 -2 16 -0.11 0.27 2 -1 -11 5.37 0.48 2 -1 -9 60.27 2.16 2 -1 -8 0.99 0.32 2 -1 -7 0.82 0.23 2 -1 -6 3.19 0.11 2 -1 -5 3.18 0.14 2 -1 -4 58.47 1.16 2 -1 -3 289.23 4.52 2 -1 -2 25.70 0.42 2 -1 -1 131.77 1.89 2 -1 0 53.68 0.88 2 -1 1 517.68 9.35 2 -1 2 185.07 4.13 2 -1 3 362.16 6.62 2 -1 4 197.49 3.20 2 -1 5 0.84 0.11 2 -1 6 121.10 1.81 2 -1 7 3.07 0.13 2 -1 8 6.21 0.16 2 -1 9 8.74 0.24 2 -1 10 0.43 0.11 2 -1 11 -0.01 0.09 2 -1 12 13.57 0.35 2 -1 13 60.86 1.28 2 -1 14 12.50 0.49 2 -1 15 16.05 0.79 2 -1 16 4.62 0.42 2 0 -14 42.93 1.70 2 0 -12 3.01 0.48 2 0 -10 36.67 1.38 2 0 -8 172.97 5.74 2 0 -6 590.13 12.91 2 0 -4 6.64 0.16 2 0 -2 174.64 2.76 2 0 0 109.89 1.59 2 0 4 7.29 0.19 2 0 6 18.58 0.41 2 0 8 0.55 0.09 2 0 10 39.52 0.72 2 0 12 33.89 0.74 2 0 14 50.53 1.80 2 0 16 14.69 0.85 2 1 -16 22.95 1.18 2 1 -15 20.74 1.09 2 1 -14 0.82 0.45 2 1 -13 2.87 0.36 2 1 -12 41.53 1.59 2 1 -11 3.56 0.42 2 1 -10 6.66 0.54 2 1 -9 57.94 2.07 2 1 -8 0.40 0.32 2 1 -7 0.86 0.08 2 1 -6 2.84 0.12 2 1 -5 3.42 0.13 2 1 -4 59.68 0.98 2 1 -3 288.48 4.51 2 1 -2 25.25 0.44 2 1 -1 137.86 2.23 2 1 0 55.27 0.94 2 1 1 539.49 9.69 2 1 2 193.60 6.16 2 1 3 358.92 8.03 2 1 4 197.23 2.75 2 1 5 0.42 0.08 2 1 6 122.29 1.75 2 1 7 3.43 0.10 2 1 8 6.53 0.15 2 1 9 9.55 0.22 2 1 10 0.40 0.08 2 1 11 0.31 0.07 2 1 12 13.20 0.34 2 1 13 62.30 1.55 2 1 14 14.21 0.74 2 1 15 17.03 0.78 2 1 16 7.11 0.49 2 2 -18 9.49 0.62 2 2 -17 0.56 0.44 2 2 -16 103.30 3.60 2 2 -15 30.62 1.37 2 2 -14 294.96 9.56 2 2 -13 2.73 0.50 2 2 -12 9.86 0.60 2 2 -11 0.23 0.06 2 2 -10 13.06 0.30 2 2 -9 18.01 0.38 2 2 -8 24.31 0.62 2 2 -7 1.39 0.12 2 2 -6 178.51 3.30 2 2 -5 33.89 0.59 2 2 -4 454.14 7.01 2 2 -3 10.02 0.24 2 2 -2 11.77 0.24 2 2 -1 81.68 1.31 2 2 0 126.03 2.06 2 2 1 49.60 0.85 2 2 2 390.62 7.12 2 2 3 56.83 1.14 2 2 4 3.91 0.17 2 2 5 274.05 4.40 2 2 6 17.80 0.29 2 2 7 77.90 1.17 2 2 8 8.95 0.19 2 2 9 4.40 0.13 2 2 10 65.38 1.12 2 2 11 2.31 0.14 2 2 12 7.17 0.19 2 2 13 5.05 0.17 2 2 14 34.08 0.89 2 2 15 6.30 0.52 2 2 16 0.60 0.36 2 3 -19 17.90 1.15 2 3 -18 11.43 0.83 2 3 -17 2.19 0.50 2 3 -16 17.69 0.96 2 3 -15 0.58 0.43 2 3 -14 24.84 0.54 2 3 -13 12.14 0.29 2 3 -12 19.71 0.42 2 3 -11 17.90 0.40 2 3 -10 0.44 0.11 2 3 -9 6.08 0.23 2 3 -8 15.10 0.42 2 3 -7 18.80 0.41 2 3 -6 2.56 0.11 2 3 -5 507.66 7.84 2 3 -4 37.40 0.74 2 3 -3 260.81 4.09 2 3 -2 120.76 1.95 2 3 -1 119.78 1.94 2 3 0 30.41 0.63 2 3 1 172.39 3.16 2 3 2 324.56 5.93 2 3 3 139.88 2.62 2 3 4 144.02 2.66 2 3 5 3.50 0.19 2 3 6 106.99 2.03 2 3 7 0.10 0.12 2 3 8 55.41 1.13 2 3 9 30.94 0.63 2 3 10 0.46 0.10 2 3 11 10.69 0.31 2 3 12 42.68 1.12 2 3 13 9.94 0.38 2 3 14 6.77 0.48 2 3 15 0.48 0.30 2 3 16 11.86 0.65 2 4 -20 1.42 0.49 2 4 -19 5.21 0.55 2 4 -17 0.57 0.46 2 4 -16 3.06 0.14 2 4 -15 17.29 0.39 2 4 -14 75.46 1.48 2 4 -13 109.69 2.12 2 4 -12 1.05 0.14 2 4 -11 9.04 0.30 2 4 -10 119.16 2.76 2 4 -9 20.88 0.58 2 4 -8 319.11 5.76 2 4 -7 16.46 0.33 2 4 -6 274.37 4.30 2 4 -5 0.82 0.12 2 4 -4 0.20 0.10 2 4 -3 0.93 0.10 2 4 -2 0.52 0.09 2 4 -1 91.02 1.75 2 4 0 142.96 2.65 2 4 1 0.83 0.13 2 4 2 65.59 1.28 2 4 3 145.16 2.67 2 4 4 206.84 3.82 2 4 5 170.82 3.31 2 4 6 0.58 0.12 2 4 7 1.88 0.13 2 4 8 17.34 0.53 2 4 9 76.90 1.55 2 4 10 21.17 0.52 2 4 11 57.07 1.43 2 4 12 21.52 0.62 2 4 13 0.38 0.17 2 4 14 11.86 0.63 2 4 15 0.06 0.38 2 5 -19 0.75 0.32 2 5 -18 1.29 0.50 2 5 -17 3.05 0.42 2 5 -16 36.48 1.03 2 5 -15 16.10 0.53 2 5 -14 5.97 0.29 2 5 -13 22.41 0.66 2 5 -12 157.29 3.57 2 5 -11 -0.45 0.38 2 5 -10 54.85 1.08 2 5 -9 232.42 4.24 2 5 -8 48.71 0.97 2 5 -7 28.83 0.51 2 5 -6 205.30 3.26 2 5 -5 29.00 0.55 2 5 -4 31.12 0.53 2 5 -3 15.33 0.35 2 5 -2 22.41 0.48 2 5 -1 80.94 1.54 2 5 0 32.98 0.65 2 5 1 2.82 0.14 2 5 2 6.19 0.20 2 5 3 19.99 0.45 2 5 4 0.11 0.12 2 5 5 19.91 0.48 2 5 6 186.02 3.54 2 5 7 0.67 0.19 2 5 8 10.73 0.37 2 5 9 7.02 0.32 2 5 10 11.05 0.34 2 5 11 1.88 0.20 2 5 12 61.45 1.54 2 5 13 13.46 0.49 2 5 15 6.34 0.49 2 6 -20 -0.15 0.31 2 6 -19 4.13 0.58 2 6 -17 1.15 0.15 2 6 -16 33.93 1.00 2 6 -15 0.22 0.15 2 6 -14 2.17 0.19 2 6 -13 48.53 1.01 2 6 -12 10.34 0.28 2 6 -11 127.24 2.92 2 6 -10 3.00 0.19 2 6 -9 44.86 0.93 2 6 -8 8.63 0.26 2 6 -7 64.77 1.07 2 6 -6 171.48 2.73 2 6 -5 15.80 0.33 2 6 -4 384.77 6.95 2 6 -3 23.84 0.62 2 6 -2 -0.53 0.19 2 6 -1 3.96 0.18 2 6 0 1.32 0.12 2 6 1 143.79 2.73 2 6 2 179.78 3.39 2 6 3 68.70 1.41 2 6 4 72.20 1.40 2 6 5 96.97 1.87 2 6 6 36.60 0.80 2 6 7 38.85 1.02 2 6 8 0.26 0.14 2 6 9 10.42 0.41 2 6 10 2.60 0.29 2 6 11 19.85 0.59 2 6 12 3.16 0.24 2 6 13 0.49 0.18 2 6 14 2.31 0.34 2 6 15 1.41 0.33 2 7 -19 0.49 0.46 2 7 -18 1.02 0.37 2 7 -17 -0.46 0.17 2 7 -16 19.94 0.68 2 7 -15 15.28 0.52 2 7 -14 1.00 0.19 2 7 -13 7.76 0.25 2 7 -12 130.10 2.45 2 7 -11 5.11 0.22 2 7 -10 103.04 1.99 2 7 -9 7.87 0.27 2 7 -8 9.60 0.25 2 7 -7 27.96 0.50 2 7 -6 165.24 2.68 2 7 -5 28.33 0.57 2 7 -4 0.25 0.12 2 7 -3 221.28 4.89 2 7 -2 80.32 1.87 2 7 -1 1.49 0.14 2 7 0 24.71 0.53 2 7 1 26.93 0.72 2 7 2 6.68 0.23 2 7 3 11.24 0.32 2 7 4 204.85 3.89 2 7 5 2.82 0.17 2 7 6 0.81 0.20 2 7 7 51.76 1.41 2 7 8 10.94 0.42 2 7 9 12.57 0.65 2 7 10 1.18 0.32 2 7 12 23.04 0.73 2 7 13 1.00 0.16 2 7 14 5.13 0.46 2 8 -19 0.03 0.49 2 8 -18 11.86 0.89 2 8 -17 1.65 0.20 2 8 -16 8.14 0.40 2 8 -15 28.56 1.12 2 8 -14 0.67 0.20 2 8 -13 1.52 0.27 2 8 -12 29.07 0.82 2 8 -11 19.24 0.47 2 8 -10 9.08 0.29 2 8 -9 18.17 0.46 2 8 -8 55.13 0.94 2 8 -7 125.74 2.06 2 8 -6 28.87 0.61 2 8 -5 1.70 0.11 2 8 -4 20.22 0.43 2 8 -3 2.26 0.16 2 8 -2 207.48 3.83 2 8 -1 355.93 7.88 2 8 0 3.50 0.17 2 8 1 33.97 0.74 2 8 2 2.75 0.16 2 8 3 18.20 0.54 2 8 4 22.23 0.54 2 8 5 0.61 0.18 2 8 6 4.29 0.25 2 8 7 48.62 1.32 2 8 8 5.27 0.45 2 8 9 22.77 0.94 2 8 10 4.10 0.45 2 8 11 0.21 0.32 2 8 12 2.84 0.42 2 8 13 5.33 0.48 2 8 14 0.08 0.30 2 8 15 12.03 0.75 2 9 -19 4.80 0.60 2 9 -18 10.20 0.51 2 9 -17 0.43 0.20 2 9 -16 28.73 0.88 2 9 -15 7.59 0.49 2 9 -14 3.81 0.37 2 9 -13 2.00 0.22 2 9 -12 1.77 0.15 2 9 -11 2.28 0.16 2 9 -10 10.92 0.35 2 9 -9 0.41 0.16 2 9 -8 69.91 1.22 2 9 -7 113.10 1.88 2 9 -6 158.56 2.95 2 9 -5 12.59 0.31 2 9 -4 22.08 0.51 2 9 -3 0.18 0.12 2 9 -2 103.81 2.00 2 9 -1 26.76 0.72 2 9 0 159.84 3.68 2 9 1 34.26 0.78 2 9 2 73.22 1.46 2 9 3 29.76 0.83 2 9 4 31.65 0.85 2 9 5 35.57 0.98 2 9 6 2.93 0.27 2 9 7 9.80 0.57 2 9 8 21.20 0.96 2 9 9 7.88 0.60 2 9 10 26.02 1.06 2 9 11 2.93 0.42 2 9 12 40.76 1.74 2 9 13 -0.35 0.32 2 9 14 10.59 0.70 2 10 -18 6.77 0.43 2 10 -17 3.92 0.33 2 10 -16 0.77 0.25 2 10 -15 -0.22 0.24 2 10 -14 1.11 0.31 2 10 -13 55.04 2.02 2 10 -12 4.32 0.38 2 10 -11 -0.21 0.19 2 10 -10 28.33 0.77 2 10 -9 0.44 0.14 2 10 -8 0.63 0.08 2 10 -7 82.89 1.61 2 10 -6 9.22 0.27 2 10 -5 9.08 0.25 2 10 -4 3.49 0.17 2 10 -3 3.45 0.16 2 10 -2 3.94 0.18 2 10 -1 56.55 1.38 2 10 0 58.13 1.45 2 10 1 12.17 0.35 2 10 2 7.01 0.42 2 10 3 44.48 1.14 2 10 4 5.42 0.47 2 10 5 1.00 0.21 2 10 6 10.90 0.46 2 10 7 0.71 0.38 2 10 8 -0.36 0.34 2 10 9 25.63 1.19 2 10 10 22.65 1.08 2 10 11 89.76 3.24 2 10 12 4.17 0.49 2 10 13 4.26 0.47 2 10 14 32.36 1.40 2 11 -18 0.43 0.26 2 11 -17 2.33 0.31 2 11 -16 4.68 0.36 2 11 -15 0.71 0.29 2 11 -13 1.72 0.25 2 11 -12 8.97 0.44 2 11 -11 37.67 1.05 2 11 -10 -0.08 0.12 2 11 -9 39.84 0.92 2 11 -8 19.10 0.44 2 11 -7 0.04 0.09 2 11 -6 135.13 2.57 2 11 -5 7.48 0.24 2 11 -4 26.28 0.58 2 11 -3 10.96 0.31 2 11 -2 111.22 3.73 2 11 -1 0.19 0.11 2 11 0 6.82 0.31 2 11 2 25.70 1.03 2 11 3 28.66 0.81 2 11 5 38.97 1.07 2 11 6 24.43 1.06 2 11 7 2.64 0.46 2 11 8 7.16 0.59 2 11 9 7.71 0.53 2 11 10 5.03 0.48 2 11 11 13.00 0.73 2 11 12 12.14 0.79 2 11 13 14.71 0.92 2 11 14 1.60 0.38 2 12 -16 0.64 0.28 2 12 -15 6.72 0.39 2 12 -14 24.06 0.84 2 12 -13 10.49 0.49 2 12 -12 8.12 0.54 2 12 -11 2.23 0.30 2 12 -10 2.28 0.20 2 12 -9 3.55 0.25 2 12 -8 11.99 0.31 2 12 -7 76.78 1.55 2 12 -6 19.26 0.44 2 12 -5 18.12 0.46 2 12 -4 11.28 0.38 2 12 -3 27.92 0.80 2 12 -2 0.61 0.29 2 12 -1 58.95 2.09 2 12 0 19.24 0.58 2 12 1 9.22 0.38 2 12 2 4.48 0.32 2 12 3 12.25 0.64 2 12 4 2.00 0.24 2 12 5 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0.48 4 6 11 20.85 1.04 4 6 12 0.27 0.31 4 6 13 1.14 0.41 4 6 14 12.95 0.91 4 6 15 2.63 0.53 4 7 -16 2.78 0.48 4 7 -14 0.08 0.16 4 7 -13 5.31 0.29 4 7 -12 11.00 0.46 4 7 -11 15.85 0.53 4 7 -10 30.76 0.60 4 7 -9 10.98 0.27 4 7 -8 34.93 0.67 4 7 -7 10.77 0.33 4 7 -6 35.87 0.68 4 7 -5 13.25 0.34 4 7 -4 121.10 2.02 4 7 -3 18.88 0.41 4 7 -2 85.32 1.69 4 7 -1 43.89 0.80 4 7 0 0.47 0.17 4 7 1 14.59 0.39 4 7 2 35.72 0.94 4 7 3 0.87 0.45 4 7 4 7.48 0.64 4 7 6 31.86 1.39 4 7 7 3.52 0.49 4 7 8 20.71 0.98 4 7 9 1.11 0.51 4 7 10 -0.78 0.27 4 7 11 2.90 0.57 4 7 12 38.97 1.78 4 7 13 -0.90 0.41 4 7 14 1.33 0.45 4 7 15 -0.02 0.37 4 8 -17 -0.37 0.36 4 8 -15 10.73 0.41 4 8 -14 5.76 0.32 4 8 -13 2.87 0.24 4 8 -12 1.07 0.20 4 8 -11 10.96 0.56 4 8 -10 2.17 0.18 4 8 -9 0.32 0.11 4 8 -8 6.46 0.23 4 8 -7 81.28 1.43 4 8 -6 31.44 0.60 4 8 -5 60.42 1.08 4 8 -4 5.21 0.26 4 8 -3 85.38 1.46 4 8 -2 1.68 0.19 4 8 -1 4.16 0.21 4 8 0 20.85 0.52 4 8 1 7.45 0.54 4 8 2 15.03 0.79 4 8 3 27.69 1.16 4 8 4 4.12 0.51 4 8 5 19.46 0.98 4 8 6 3.75 0.54 4 8 7 1.73 0.35 4 8 8 1.73 0.49 4 8 9 2.90 0.40 4 8 11 2.18 0.43 4 8 12 6.61 0.70 4 8 13 1.66 0.47 4 8 14 0.73 0.34 4 8 15 -0.11 0.39 4 9 -15 10.51 0.49 4 9 -14 7.71 0.46 4 9 -13 -0.71 0.34 4 9 -12 6.59 0.42 4 9 -11 6.43 0.43 4 9 -10 9.66 0.32 4 9 -9 14.11 0.64 4 9 -8 17.11 0.39 4 9 -7 0.68 0.14 4 9 -6 39.92 0.80 4 9 -5 32.83 0.91 4 9 -4 7.62 0.26 4 9 -3 28.19 0.60 4 9 -2 77.90 1.56 4 9 -1 4.28 0.22 4 9 0 35.31 1.43 4 9 1 2.21 0.47 4 9 2 0.04 0.45 4 9 4 38.18 1.60 4 9 5 2.42 0.50 4 9 6 17.11 0.94 4 9 7 -0.56 0.41 4 9 8 1.65 0.41 4 9 11 8.67 0.69 4 9 12 1.81 0.50 4 9 13 5.17 0.60 4 9 14 1.50 0.50 4 10 -17 -0.46 0.58 4 10 -16 0.68 0.41 4 10 -15 15.53 0.87 4 10 -14 0.58 0.19 4 10 -13 4.49 0.38 4 10 -12 -0.08 0.25 4 10 -11 17.24 0.63 4 10 -10 1.02 0.32 4 10 -9 0.72 0.14 4 10 -8 7.62 0.38 4 10 -7 69.27 1.47 4 10 -6 20.82 0.52 4 10 -5 22.05 0.56 4 10 -4 11.11 0.44 4 10 -3 4.84 0.31 4 10 -2 10.08 0.42 4 10 -1 7.74 0.67 4 10 0 5.84 0.56 4 10 1 -0.16 0.31 4 10 2 16.28 0.84 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0.35 0.17 5 -5 -9 17.40 0.71 5 -5 -8 117.92 3.98 5 -5 -7 3.84 0.34 5 -5 -6 84.91 2.10 5 -5 -5 144.32 3.42 5 -5 -4 1.24 0.24 5 -5 -3 16.36 0.54 5 -5 -2 4.71 0.43 5 -5 -1 32.26 1.26 5 -5 0 10.14 0.69 5 -5 1 20.88 0.95 5 -5 2 1.80 0.31 5 -5 4 1.40 0.45 5 -5 6 1.14 0.43 5 -5 7 3.12 0.54 5 -5 8 8.12 0.65 5 -5 9 7.82 0.73 5 -5 10 2.28 0.46 5 -5 11 4.48 0.52 5 -5 12 2.58 0.53 5 -5 13 0.24 0.44 5 -5 14 1.33 0.51 5 -4 -11 17.93 0.67 5 -4 -10 1.25 0.21 5 -4 -9 4.50 0.31 5 -4 -8 15.53 0.45 5 -4 -7 33.86 0.88 5 -4 -6 146.61 3.37 5 -4 -5 17.74 0.61 5 -4 -4 1.46 0.21 5 -4 -3 0.80 0.18 5 -4 -2 4.06 0.27 5 -4 -1 20.25 0.63 5 -4 0 115.60 3.94 5 -4 2 37.75 1.52 5 -4 3 35.80 1.48 5 -4 4 -0.15 0.40 5 -4 5 9.47 0.70 5 -4 6 -0.43 0.30 5 -4 7 12.61 0.81 5 -4 8 2.24 0.38 5 -4 9 3.45 0.53 5 -4 10 2.78 0.52 5 -4 12 2.48 0.51 5 -4 13 6.32 0.67 5 -4 14 0.81 0.50 5 -3 -11 0.79 0.12 5 -3 -10 3.47 0.24 5 -3 -9 65.90 2.21 5 -3 -8 3.03 0.17 5 -3 -7 11.75 0.39 5 -3 -6 12.77 0.43 5 -3 -5 17.06 0.55 5 -3 -4 0.33 0.20 5 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-5 -7 3.30 0.45 7 -5 -6 30.41 1.57 7 -5 -5 3.47 0.46 7 -5 -4 18.58 1.06 7 -5 -3 14.91 0.95 7 -5 -2 13.29 0.90 7 -5 -1 4.21 0.55 7 -5 0 6.84 0.64 7 -5 1 19.74 1.18 7 -5 2 -0.27 0.50 7 -5 3 -0.03 0.50 7 -5 4 7.88 0.80 7 -5 6 11.32 0.96 7 -5 7 -0.01 0.53 7 -4 -10 0.51 0.24 7 -4 -9 5.70 0.42 7 -4 -8 21.43 1.08 7 -4 -7 19.26 1.08 7 -4 -6 1.60 0.38 7 -4 -5 32.15 1.54 7 -4 -4 15.80 0.93 7 -4 -3 3.42 0.53 7 -4 -2 5.67 0.59 7 -4 -1 6.30 0.60 7 -4 0 4.37 0.54 7 -4 1 1.16 0.48 7 -4 2 24.34 1.34 7 -4 3 5.48 0.64 7 -4 4 0.48 0.51 7 -4 5 7.43 0.79 7 -4 6 2.59 0.48 7 -4 7 5.39 0.69 7 -3 -10 1.60 0.25 7 -3 -9 12.03 0.70 7 -3 -8 0.22 0.28 7 -3 -7 15.50 0.87 7 -3 -6 18.80 1.04 7 -3 -5 7.71 0.58 7 -3 -4 13.18 0.78 7 -3 -3 33.78 1.47 7 -3 -2 1.89 0.49 7 -3 -1 1.35 0.44 7 -3 0 0.63 0.44 7 -3 1 29.14 1.40 7 -3 2 8.54 0.78 7 -3 3 11.45 0.86 7 -3 4 8.78 0.82 7 -3 5 3.03 0.45 7 -3 6 -0.47 0.53 7 -2 -10 1.89 0.29 7 -2 -9 3.55 0.37 7 -2 -8 6.86 0.50 7 -2 -7 4.02 0.44 7 -2 -6 1.51 0.34 7 -2 -5 0.43 0.38 7 -2 -4 79.52 2.93 7 -2 -3 4.30 0.53 7 -2 -2 4.22 0.53 7 -2 -1 2.29 0.45 7 -2 0 3.92 0.54 7 -2 1 3.17 0.59 7 -2 2 13.46 0.95 7 -2 3 4.01 0.62 7 -2 4 0.46 0.53 7 -2 5 0.93 0.54 7 -2 6 13.46 0.91 7 -2 7 0.46 0.41 7 -2 8 0.99 0.62 7 -1 -10 1.43 0.28 7 -1 -9 1.98 0.28 7 -1 -8 1.38 0.28 7 -1 -6 0.24 0.31 7 -1 -5 16.87 0.88 7 -1 -4 1.52 0.43 7 -1 -3 23.23 1.13 7 -1 -2 0.61 0.39 7 -1 -1 0.19 0.39 7 -1 1 40.24 1.65 7 -1 2 3.41 0.65 7 -1 3 0.35 0.47 7 -1 4 0.15 0.34 7 -1 5 8.89 0.79 7 -1 6 2.61 0.62 7 -1 7 0.63 0.56 7 0 -10 1.64 0.30 7 0 -8 12.28 0.75 7 0 -4 10.47 0.68 7 0 -2 -0.49 0.36 7 0 0 30.62 1.37 7 0 2 16.05 0.94 7 0 4 2.38 0.57 7 0 6 0.25 0.39 7 0 8 -0.92 0.39 7 1 -11 0.36 0.26 7 1 -9 1.48 0.28 7 1 -8 1.25 0.37 7 1 -7 2.55 0.37 7 1 -5 19.54 1.01 7 1 -4 2.58 0.49 7 1 -3 22.86 1.12 7 1 -2 2.24 0.45 7 1 -1 -0.20 0.41 7 1 0 1.13 0.45 7 1 1 39.88 1.64 7 1 2 2.12 0.60 7 1 3 0.17 0.37 7 1 4 -0.61 0.49 7 1 5 9.90 0.82 7 1 6 2.00 0.59 7 1 7 2.29 0.51 7 1 8 2.50 0.57 7 2 -11 0.99 0.23 7 2 -10 1.25 0.26 7 2 -9 3.25 0.30 7 2 -8 6.86 0.40 7 2 -7 2.80 0.30 7 2 -6 0.14 0.24 7 2 -5 1.21 0.39 7 2 -4 66.87 2.59 7 2 -3 4.17 0.65 7 2 -2 7.64 0.68 7 2 -1 0.09 0.45 7 2 0 2.05 0.51 7 2 1 3.62 0.61 7 2 2 8.95 0.68 7 2 3 2.74 0.55 7 2 5 -0.61 0.39 7 2 7 0.87 0.55 7 2 8 -0.88 0.36 7 3 -12 0.46 0.56 7 3 -11 3.48 0.28 7 3 -10 0.99 0.24 7 3 -9 11.93 0.59 7 3 -8 1.49 0.31 7 3 -7 15.60 0.70 7 3 -6 18.41 0.76 7 3 -5 8.37 0.48 7 3 -4 10.75 0.56 7 3 -3 33.86 1.07 7 3 -2 1.94 0.30 7 3 -1 0.96 0.49 7 3 0 0.93 0.50 7 3 1 21.49 1.20 7 3 2 5.17 0.60 7 3 3 15.53 1.12 7 3 4 6.63 0.62 7 3 5 3.72 0.67 7 3 6 1.62 0.44 7 3 8 0.41 0.51 7 4 -11 2.67 0.31 7 4 -10 0.91 0.22 7 4 -9 3.59 0.34 7 4 -8 22.86 0.91 7 4 -7 20.11 0.85 7 4 -6 1.38 0.35 7 4 -5 32.01 1.18 7 4 -4 16.67 0.64 7 4 -3 0.67 0.32 7 4 -2 3.14 0.35 7 4 -1 6.99 0.65 7 4 0 3.66 0.32 7 4 1 0.29 0.37 7 4 2 22.80 1.30 7 4 3 5.37 0.60 7 4 4 2.52 0.63 7 4 5 5.26 0.59 7 4 6 0.48 0.54 7 5 -11 0.93 0.26 7 5 -10 3.32 0.42 7 5 -8 0.64 0.27 7 5 -7 2.00 0.34 7 5 -6 27.06 1.05 7 5 -5 1.35 0.32 7 5 -4 16.15 0.69 7 5 -3 15.73 0.70 7 5 -2 13.69 0.63 7 5 -1 4.28 0.48 7 5 0 2.95 0.32 7 5 1 20.22 1.22 7 5 4 8.59 0.82 7 5 5 0.85 0.67 7 5 6 16.28 1.02 7 6 -11 1.44 0.27 7 6 -10 -0.20 0.26 7 6 -9 9.01 0.47 7 6 -8 0.01 0.30 7 6 -7 22.68 0.90 7 6 -6 0.85 0.33 7 6 -5 22.29 1.22 7 6 -4 4.89 0.38 7 6 -3 1.90 0.34 7 6 -2 0.26 0.26 7 6 -1 30.41 1.12 7 6 0 1.42 0.30 7 6 5 1.45 0.46 7 7 -10 0.92 0.41 7 7 -9 1.66 0.36 7 7 -8 0.10 0.35 7 7 -7 -0.11 0.38 7 7 -6 19.77 0.87 7 7 -4 0.65 0.27 7 7 -3 4.36 0.61 7 7 -2 9.06 0.55 7 7 -1 -0.60 0.37 7 7 0 13.81 0.96 7 7 4 10.94 0.84 7 8 -9 8.71 0.58 7 8 -8 1.91 0.34 7 8 -7 12.08 0.81 7 8 -6 1.54 0.34 7 8 -5 2.85 0.41 7 8 -4 0.66 0.45 7 8 -3 4.78 0.62 7 8 -2 21.76 1.36 7 8 -1 8.76 0.51 7 8 1 0.11 0.37 7 8 3 12.06 0.92 7 8 4 1.18 0.61 7 9 -9 0.07 0.35 7 9 -7 2.43 0.45 7 9 -6 6.94 0.47 7 9 -5 1.19 0.28 7 9 -4 0.11 0.25 7 9 -3 -0.40 0.26 7 9 -2 6.05 0.69 7 9 -1 1.16 0.37 7 9 0 1.95 0.53 7 9 2 -0.81 0.37 7 9 3 -0.18 0.60 7 9 4 17.58 1.19 7 10 -7 3.30 0.41 7 10 -6 0.52 0.33 7 10 -5 -0.11 0.31 7 10 -4 1.19 0.36 7 10 -3 3.22 0.40 7 10 -2 0.73 0.29 7 10 -1 13.18 0.69 7 10 0 1.60 0.60 7 10 2 2.38 0.46 7 10 3 1.08 0.60 7 11 -6 0.59 0.34 7 11 -5 -0.07 0.32 7 11 -4 1.95 0.36 7 11 -3 0.46 0.43 7 11 -2 11.22 0.66 7 11 -1 4.86 0.75 7 11 0 15.35 1.14 7 11 1 1.69 0.58 8 -3 -3 2.08 0.56 8 -3 -2 5.18 0.61 8 -2 -4 2.36 0.45 8 -2 -3 1.42 0.46 8 -2 -2 0.66 0.44 8 -2 -1 4.73 0.62 8 -2 0 0.62 0.49 8 -1 -5 1.18 0.42 8 -1 -4 0.99 0.41 8 -1 -3 -0.03 0.42 8 -1 -2 2.35 0.48 8 -1 -1 -0.37 0.49 8 -1 0 -0.16 0.37 8 0 -4 0.03 0.42 8 0 -2 3.15 0.52 8 0 0 7.12 0.73 8 1 -5 1.74 0.47 8 1 -4 -0.38 0.39 8 1 -3 2.12 0.42 8 1 -2 1.28 0.53 8 1 -1 -0.01 0.46 8 1 0 0.23 0.47 8 2 -4 -0.31 0.40 8 2 -3 0.24 0.29 8 2 -1 2.45 0.59 8 2 0 0.95 0.56 8 3 -3 -0.07 0.45 8 3 -2 3.68 0.46 8 3 -1 2.56 0.47 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14704 #===END data_global #============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Linxtl User' _publ_contact_author_address ; Universit\'e de Montr\'eal D\'epartement de Chimie C.P. 6128, Succ. Centre-ville Montr\'eal, Qu\'ebec Canada, H3C 3J7 ; _publ_contact_author_phone '1-111-111-1111' _publ_contact_author_fax '1-111-111-1111' _publ_contact_author_email 'linxtl.user@user.com' #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Structure of Linxtl compound ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; 'linxtl, user' ; D\'epartement de Chimie Universit\'e de Montr\'eal C.P. 6128, Succ. Centre-ville, Montr\'eal, Qu\'ebec Canada H3C 3J7 ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; Here should be written a short abstract ; _publ_section_comment ; Here should be written the text of the article ; _publ_section_exptl_prep ; Small details about the preparation of the compound. ; _publ_section_exptl_refinement ; All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters. The H atoms were generated geometrically (C-H 0.93 to 0.98, N-H 0.86 and O-H 0.82\%A) and were included in the refinement in the riding model approximation; their temperature factors were set to 1.5 times those of the equivalent isotropic temperature factors of the parent site (methyl) and 1.2 times for others. A final verification of possible voids was performed using the VOID routine of the PLATON program (Spek, 2000). ; _publ_section_figure_captions ; Fig 1 Ortep view of the title compound. Thermal ellipsoids are shown at 30% probability levels. ; _publ_section_table_legends ; Table 1. Selected geometric parameters (\%A, \%) for the title compound. ; _publ_section_references ; Bruker (1997). SHELXTL (1997). Release 5.10; The Complete Software Package for Single Crystal Structure Determination. Bruker AXS Inc., Madison, USA. Bruker (1999a). SAINT Release 6.06. Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, USA. Bruker (1999b). SMART Release 5.059; Bruker Molecular Analysis Research Tool, Bruker AXS Inc., Madison, USA. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Sheldrick, G. M. (1986). SHELXS86. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections. Bruker AXS Inc., Madison, USA. Sheldrick, G. M. (1997a). SHELXS97. Program for Crystal Structure solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for crystal structure refinement. University of G\"ottingen, Germany. Spek, A. L. (2000). PLATON, 2000 version; Molecular Geometry Program, University of Utrecht, Utrecht, Holland. ; _publ_section_acknowledgements ; We are grateful to the Natural Sciences and Engineering Research Council of Canada and the Minist\`ere de l'Education du Qu\'ebec for financial support. ; data_shelxl_a _audit_creation_method SHELXL-2014/6 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C62 H68 B2 N2' _chemical_formula_sum 'C31 H34 B N' _chemical_formula_weight 431.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8060(4) _cell_length_b 12.3580(3) _cell_length_c 21.0340(7) _cell_angle_alpha 88.301(2) _cell_angle_beta 79.2670(10) _cell_angle_gamma 68.171(2) _cell_volume 2559.46(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 10126 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'plate' _exptl_crystal_colour 'Yellow' _exptl_crystal_density_meas '?' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.120 _exptl_crystal_F_000 928 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_absorpt_coefficient_mu 0.063 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.992 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16471 _diffrn_reflns_av_unetI/netI 0.0508 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.777 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.967 _reflns_number_total 8951 _reflns_number_gt 6611 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.8.3 (Spasyuk, 2009)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^+2.7885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8951 _refine_ls_number_parameters 609 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2449 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2258(3) 0.3092(2) 0.43120(12) 0.0228(6) Uani 1 1 d . . . . . N2 N 0.2254(3) 0.4854(2) 0.34467(12) 0.0244(6) Uani 1 1 d . . . . . C17 C 0.2153(3) 0.2783(3) 0.61272(15) 0.0252(7) Uani 1 1 d . . . . . C11 C 0.2363(3) 0.1059(3) 0.48883(15) 0.0258(7) Uani 1 1 d . . . . . C27 C 0.2393(3) 0.5056(3) 0.56114(15) 0.0250(7) Uani 1 1 d . . . . . C4 C 0.2190(3) 0.5055(3) 0.41062(15) 0.0248(7) Uani 1 1 d . . . . . C7 C 0.2210(3) 0.3773(2) 0.32387(14) 0.0233(6) Uani 1 1 d . . . . . C8 C 0.2244(3) 0.2918(3) 0.36579(15) 0.0245(7) Uani 1 1 d . . . . . C2 C 0.2185(3) 0.4167(3) 0.52213(14) 0.0239(7) Uani 1 1 d . . . . . C3 C 0.2208(3) 0.4206(2) 0.45260(15) 0.0236(6) Uani 1 1 d . . . . . C30 C 0.2863(3) 0.6654(3) 0.63827(15) 0.0271(7) Uani 1 1 d . . . . . C18 C 0.2968(3) 0.1662(3) 0.62696(16) 0.0300(7) Uani 1 1 d . . . . . H18 H 0.3490 0.1125 0.5931 0.036 Uiso 1 1 calc R U . . . C29 C 0.1569(3) 0.6811(3) 0.62950(15) 0.0295(7) Uani 1 1 d . . . . . H29 H 0.0838 0.7457 0.6495 0.035 Uiso 1 1 calc R U . . . C20 C 0.2246(3) 0.2084(3) 0.74263(15) 0.0282(7) Uani 1 1 d . . . . . C53 C 0.2266(3) 0.2859(3) 0.21182(15) 0.0258(7) Uani 1 1 d . . . . . C6 C 0.2213(3) 0.3826(3) 0.25442(15) 0.0251(7) Uani 1 1 d . . . . . C28 C 0.1336(3) 0.6032(3) 0.59173(15) 0.0270(7) Uani 1 1 d . . . . . H28 H 0.0453 0.6167 0.5868 0.032 Uiso 1 1 calc R U . . . C37 C 0.2550(4) 0.6752(3) 0.28811(15) 0.0301(7) Uani 1 1 d . . . . . C54 C 0.1151(3) 0.2564(3) 0.21047(15) 0.0295(7) Uani 1 1 d . . . . . H54 H 0.0325 0.2976 0.2372 0.035 Uiso 1 1 calc R U . . . C19 C 0.3016(3) 0.1330(3) 0.69025(16) 0.0302(7) Uani 1 1 d . . . . . H19 H 0.3581 0.0580 0.6978 0.036 Uiso 1 1 calc R U . . . C1 C 0.2162(3) 0.3123(3) 0.54482(15) 0.0257(7) Uani 1 1 d . . . . . C5 C 0.2262(3) 0.4863(3) 0.23207(15) 0.0277(7) Uani 1 1 d . . . . . C43 C 0.2275(3) 0.5203(3) 0.16409(15) 0.0292(7) Uani 1 1 d . . . . . C21 C 0.1395(3) 0.3188(3) 0.72870(16) 0.0322(8) Uani 1 1 d . . . . . H21 H 0.0840 0.3709 0.7627 0.039 Uiso 1 1 calc R U . . . C56 C 0.2461(3) 0.1030(3) 0.12815(15) 0.0286(7) Uani 1 1 d . . . . . C23 C 0.2275(4) 0.1729(3) 0.81300(16) 0.0339(8) Uani 1 1 d . . . . . C12 C 0.1315(4) 0.0775(3) 0.52522(18) 0.0371(8) Uani 1 1 d . . . . . H12 H 0.0527 0.1369 0.5456 0.044 Uiso 1 1 calc R U . . . C58 C 0.3461(3) 0.2253(3) 0.16937(17) 0.0329(8) Uani 1 1 d . . . . . H58 H 0.4215 0.2449 0.1685 0.039 Uiso 1 1 calc R U . . . C55 C 0.1254(4) 0.1665(3) 0.16989(16) 0.0320(8) Uani 1 1 d . . . . . H55 H 0.0495 0.1478 0.1704 0.038 Uiso 1 1 calc R U . . . C22 C 0.1353(3) 0.3533(3) 0.66552(15) 0.0310(7) Uani 1 1 d . . . . . H22 H 0.0778 0.4281 0.6582 0.037 Uiso 1 1 calc R U . . . C32 C 0.3682(3) 0.4899(3) 0.56925(17) 0.0336(8) Uani 1 1 d . . . . . H32 H 0.4410 0.4254 0.5490 0.040 Uiso 1 1 calc R U . . . C33 C 0.3159(4) 0.7471(3) 0.68198(17) 0.0357(8) Uani 1 1 d . . . . . C16 C 0.3534(4) 0.0127(3) 0.46107(17) 0.0368(8) Uani 1 1 d . . . . . H16 H 0.4262 0.0282 0.4374 0.044 Uiso 1 1 calc R U . . . C10 C 0.2297(4) 0.1742(3) 0.34742(16) 0.0339(8) Uani 1 1 d . . . . . H10A H 0.2200 0.1726 0.3031 0.051 Uiso 1 1 calc R U . . . H10B H 0.1573 0.1583 0.3748 0.051 Uiso 1 1 calc R U . . . H10C H 0.3153 0.1161 0.3526 0.051 Uiso 1 1 calc R U . . . C57 C 0.3553(3) 0.1365(3) 0.12844(17) 0.0326(8) Uani 1 1 d . . . . . H57 H 0.4368 0.0980 0.1002 0.039 Uiso 1 1 calc R U . . . C31 C 0.3929(3) 0.5672(3) 0.60670(17) 0.0350(8) Uani 1 1 d . . . . . H31 H 0.4814 0.5538 0.6110 0.042 Uiso 1 1 calc R U . . . C46 C 0.2353(4) 0.5869(3) 0.03264(17) 0.0387(9) Uani 1 1 d . . . . . C59 C 0.2608(4) 0.0030(3) 0.08250(16) 0.0339(8) Uani 1 1 d . . . . . C48 C 0.1457(4) 0.4988(3) 0.12589(17) 0.0360(8) Uani 1 1 d . . . . . H48 H 0.0873 0.4617 0.1437 0.043 Uiso 1 1 calc R U . . . C38 C 0.3825(4) 0.6778(3) 0.28851(19) 0.0416(9) Uani 1 1 d . . . . . H38 H 0.4543 0.6078 0.2909 0.050 Uiso 1 1 calc R U . . . C47 C 0.1494(4) 0.5311(3) 0.06236(17) 0.0420(9) Uani 1 1 d . . . . . H47 H 0.0932 0.5153 0.0386 0.050 Uiso 1 1 calc R U . . . C13 C 0.1428(5) -0.0377(4) 0.5315(2) 0.0478(10) Uani 1 1 d . . . . . H13 H 0.0714 -0.0548 0.5555 0.057 Uiso 1 1 calc R U . . . C25 C 0.3411(4) 0.0559(3) 0.81821(18) 0.0438(9) Uani 1 1 d . . . . . H25A H 0.3258 -0.0046 0.7972 0.066 Uiso 1 1 calc R U . . . H25B H 0.3424 0.0394 0.8630 0.066 Uiso 1 1 calc R U . . . H25C H 0.4267 0.0593 0.7977 0.066 Uiso 1 1 calc R U . . . C9 C 0.2064(4) 0.6254(3) 0.42982(17) 0.0404(9) Uani 1 1 d . . . . . H9A H 0.1844 0.6357 0.4762 0.061 Uiso 1 1 calc R U . . . H9B H 0.1359 0.6824 0.4114 0.061 Uiso 1 1 calc R U . . . H9C H 0.2909 0.6349 0.4142 0.061 Uiso 1 1 calc R U . . . C15 C 0.3642(5) -0.1015(3) 0.4677(2) 0.0485(10) Uani 1 1 d . . . . . H15 H 0.4434 -0.1617 0.4485 0.058 Uiso 1 1 calc R U . . . C14 C 0.2587(5) -0.1263(3) 0.5025(2) 0.0496(11) Uani 1 1 d . . . . . H14 H 0.2655 -0.2034 0.5065 0.059 Uiso 1 1 calc R U . . . C45 C 0.3152(4) 0.6096(3) 0.07099(17) 0.0426(9) Uani 1 1 d . . . . . H45 H 0.3732 0.6470 0.0533 0.051 Uiso 1 1 calc R U . . . C44 C 0.3111(4) 0.5779(3) 0.13506(16) 0.0379(8) Uani 1 1 d . . . . . H44 H 0.3655 0.5957 0.1592 0.045 Uiso 1 1 calc R U . . . C62 C 0.2797(5) 0.0413(4) 0.01276(18) 0.0497(10) Uani 1 1 d . . . . . H62A H 0.2007 0.1072 0.0071 0.075 Uiso 1 1 calc R U . . . H62B H 0.2926 -0.0218 -0.0165 0.075 Uiso 1 1 calc R U . . . H62C H 0.3579 0.0627 0.0039 0.075 Uiso 1 1 calc R U . . . C24 C 0.0910(4) 0.1638(4) 0.84258(19) 0.0478(10) Uani 1 1 d . . . . . H24A H 0.0191 0.2379 0.8413 0.072 Uiso 1 1 calc R U . . . H24B H 0.0913 0.1417 0.8867 0.072 Uiso 1 1 calc R U . . . H24C H 0.0772 0.1060 0.8183 0.072 Uiso 1 1 calc R U . . . C35 C 0.1899(4) 0.8564(4) 0.7049(2) 0.0516(11) Uani 1 1 d . . . . . H35A H 0.1201 0.8343 0.7302 0.077 Uiso 1 1 calc R U . . . H35B H 0.1580 0.8970 0.6680 0.077 Uiso 1 1 calc R U . . . H35C H 0.2124 0.9064 0.7308 0.077 Uiso 1 1 calc R U . . . C42 C 0.1513(4) 0.7820(3) 0.28318(18) 0.0432(9) Uani 1 1 d . . . . . H42 H 0.0647 0.7844 0.2820 0.052 Uiso 1 1 calc R U . . . C49 C 0.2381(5) 0.6204(3) -0.03780(18) 0.0500(11) Uani 1 1 d . . . . . C26 C 0.2492(5) 0.2652(3) 0.85202(19) 0.0476(10) Uani 1 1 d . . . . . H26A H 0.3345 0.2711 0.8336 0.071 Uiso 1 1 calc R U . . . H26B H 0.2494 0.2430 0.8961 0.071 Uiso 1 1 calc R U . . . H26C H 0.1771 0.3393 0.8507 0.071 Uiso 1 1 calc R U . . . B1 B 0.2253(3) 0.2356(3) 0.48652(18) 0.0252(8) Uani 1 1 d . . . . . C39 C 0.4064(5) 0.7799(4) 0.2855(2) 0.0537(11) Uani 1 1 d . . . . . H39 H 0.4928 0.7784 0.2864 0.064 Uiso 1 1 calc R U . . . C60 C 0.1376(4) -0.0318(4) 0.0954(2) 0.0485(10) Uani 1 1 d . . . . . H60A H 0.1220 -0.0524 0.1397 0.073 Uiso 1 1 calc R U . . . H60B H 0.1538 -0.0975 0.0674 0.073 Uiso 1 1 calc R U . . . H60C H 0.0594 0.0325 0.0873 0.073 Uiso 1 1 calc R U . . . C34 C 0.4249(4) 0.7883(4) 0.6448(2) 0.0503(10) Uani 1 1 d . . . . . H34A H 0.4505 0.8309 0.6739 0.075 Uiso 1 1 calc R U . . . H34B H 0.3896 0.8378 0.6111 0.075 Uiso 1 1 calc R U . . . H34C H 0.5029 0.7219 0.6259 0.075 Uiso 1 1 calc R U . . . C61 C 0.3855(4) -0.1052(3) 0.0906(2) 0.0495(10) Uani 1 1 d . . . . . H61A H 0.4644 -0.0851 0.0840 0.074 Uiso 1 1 calc R U . . . H61B H 0.3985 -0.1654 0.0593 0.074 Uiso 1 1 calc R U . . . H61C H 0.3713 -0.1328 0.1334 0.074 Uiso 1 1 calc R U . . . C40 C 0.3020(6) 0.8838(4) 0.2814(2) 0.0605(13) Uani 1 1 d . . . . . H40 H 0.3171 0.9533 0.2795 0.073 Uiso 1 1 calc R U . . . B2 B 0.2326(4) 0.5573(3) 0.28991(17) 0.0274(8) Uani 1 1 d . . . . . C41 C 0.1757(5) 0.8848(3) 0.2800(2) 0.0593(12) Uani 1 1 d . . . . . H41 H 0.1052 0.9553 0.2770 0.071 Uiso 1 1 calc R U . . . C50 C 0.3414(7) 0.6783(5) -0.0611(2) 0.0772(17) Uani 1 1 d . . . . . H50A H 0.3414 0.6962 -0.1058 0.116 Uiso 1 1 calc R U . . . H50B H 0.4303 0.6260 -0.0563 0.116 Uiso 1 1 calc R U . . . H50C H 0.3169 0.7490 -0.0356 0.116 Uiso 1 1 calc R U . . . C36 C 0.3637(7) 0.6809(4) 0.7409(2) 0.0845(19) Uani 1 1 d . . . . . H36A H 0.4462 0.6150 0.7269 0.127 Uiso 1 1 calc R U . . . H36B H 0.2952 0.6544 0.7635 0.127 Uiso 1 1 calc R U . . . H36C H 0.3798 0.7317 0.7692 0.127 Uiso 1 1 calc R U . . . C52 C 0.2801(7) 0.5114(5) -0.0808(2) 0.0822(18) Uani 1 1 d . . . . . H52A H 0.2159 0.4742 -0.0687 0.123 Uiso 1 1 calc R U . . . H52B H 0.3686 0.4587 -0.0756 0.123 Uiso 1 1 calc R U . . . H52C H 0.2823 0.5324 -0.1252 0.123 Uiso 1 1 calc R U . . . C51 C 0.1012(7) 0.7070(5) -0.0445(3) 0.094(2) Uani 1 1 d . . . . . H51A H 0.0344 0.6726 -0.0320 0.142 Uiso 1 1 calc R U . . . H51B H 0.1028 0.7289 -0.0888 0.142 Uiso 1 1 calc R U . . . H51C H 0.0787 0.7749 -0.0171 0.142 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0252(14) 0.0215(13) 0.0233(14) -0.0005(10) -0.0049(11) -0.0103(10) N2 0.0289(14) 0.0199(13) 0.0260(14) -0.0009(10) -0.0060(11) -0.0103(11) C17 0.0267(16) 0.0282(16) 0.0260(16) 0.0013(12) -0.0076(13) -0.0150(13) C11 0.0341(18) 0.0266(16) 0.0216(16) 0.0023(12) -0.0104(13) -0.0147(14) C27 0.0263(16) 0.0264(16) 0.0239(16) 0.0028(12) -0.0046(13) -0.0118(13) C4 0.0266(16) 0.0252(16) 0.0253(16) -0.0019(12) -0.0039(13) -0.0130(13) C7 0.0231(16) 0.0226(15) 0.0251(16) -0.0031(12) -0.0039(12) -0.0097(12) C8 0.0234(16) 0.0248(16) 0.0269(17) 0.0003(12) -0.0073(13) -0.0096(12) C2 0.0230(16) 0.0256(16) 0.0230(16) -0.0006(12) -0.0035(12) -0.0091(12) C3 0.0221(15) 0.0219(15) 0.0260(16) -0.0020(12) -0.0030(12) -0.0077(12) C30 0.0331(18) 0.0298(17) 0.0220(16) 0.0013(12) -0.0060(13) -0.0153(14) C18 0.0349(19) 0.0262(16) 0.0286(18) -0.0035(13) -0.0060(14) -0.0108(14) C29 0.0275(17) 0.0292(17) 0.0291(18) -0.0039(13) 0.0019(14) -0.0106(13) C20 0.0328(18) 0.0334(17) 0.0245(17) 0.0038(13) -0.0082(14) -0.0183(14) C53 0.0315(17) 0.0250(16) 0.0231(16) 0.0015(12) -0.0096(13) -0.0110(13) C6 0.0261(16) 0.0245(15) 0.0255(16) -0.0030(12) -0.0053(13) -0.0097(13) C28 0.0201(16) 0.0322(17) 0.0271(17) -0.0034(13) -0.0016(13) -0.0091(13) C37 0.043(2) 0.0276(17) 0.0227(16) 0.0026(12) -0.0088(14) -0.0153(15) C54 0.0310(18) 0.0349(18) 0.0237(16) -0.0035(13) -0.0027(13) -0.0143(14) C19 0.0358(19) 0.0251(16) 0.0317(18) 0.0038(13) -0.0122(15) -0.0109(14) C1 0.0247(16) 0.0265(16) 0.0257(17) 0.0010(12) -0.0051(13) -0.0092(13) C5 0.0299(17) 0.0281(16) 0.0260(17) 0.0011(12) -0.0062(13) -0.0116(13) C43 0.0378(19) 0.0213(16) 0.0265(17) -0.0023(12) -0.0068(14) -0.0081(14) C21 0.0333(19) 0.0332(18) 0.0278(18) -0.0025(13) -0.0021(14) -0.0110(15) C56 0.0352(18) 0.0306(17) 0.0250(17) 0.0015(13) -0.0060(14) -0.0178(14) C23 0.043(2) 0.0384(19) 0.0279(18) 0.0037(14) -0.0114(15) -0.0217(16) C12 0.036(2) 0.0351(19) 0.044(2) 0.0081(15) -0.0097(16) -0.0178(16) C58 0.0286(18) 0.0369(19) 0.038(2) -0.0048(14) -0.0046(15) -0.0176(15) C55 0.0362(19) 0.0404(19) 0.0274(18) 0.0007(14) -0.0056(14) -0.0233(16) C22 0.0350(19) 0.0282(17) 0.0280(18) 0.0020(13) -0.0041(14) -0.0107(14) C32 0.0279(18) 0.0269(17) 0.042(2) -0.0083(14) -0.0049(15) -0.0056(14) C33 0.045(2) 0.0360(19) 0.0330(19) -0.0012(14) -0.0121(16) -0.0199(16) C16 0.046(2) 0.0293(18) 0.035(2) 0.0038(14) -0.0056(16) -0.0145(16) C10 0.054(2) 0.0261(17) 0.0282(18) 0.0002(13) -0.0155(16) -0.0184(15) C57 0.0277(18) 0.0338(18) 0.0358(19) -0.0091(14) -0.0005(14) -0.0126(14) C31 0.0240(17) 0.0363(19) 0.046(2) -0.0082(15) -0.0125(15) -0.0091(14) C46 0.058(2) 0.0276(18) 0.0266(18) 0.0010(13) -0.0095(17) -0.0109(16) C59 0.041(2) 0.0385(19) 0.0285(18) -0.0060(14) -0.0035(15) -0.0228(16) C48 0.045(2) 0.0357(19) 0.0335(19) 0.0056(14) -0.0130(16) -0.0204(16) C38 0.044(2) 0.037(2) 0.047(2) 0.0007(16) -0.0061(18) -0.0203(17) C47 0.058(3) 0.038(2) 0.031(2) 0.0004(15) -0.0190(18) -0.0145(18) C13 0.057(3) 0.052(2) 0.054(2) 0.0182(19) -0.021(2) -0.039(2) C25 0.054(2) 0.046(2) 0.031(2) 0.0109(16) -0.0155(18) -0.0160(18) C9 0.068(3) 0.0280(18) 0.0261(18) -0.0024(13) -0.0073(17) -0.0200(17) C15 0.068(3) 0.0252(19) 0.046(2) 0.0016(16) -0.010(2) -0.0114(18) C14 0.079(3) 0.032(2) 0.051(2) 0.0069(17) -0.027(2) -0.030(2) C45 0.063(3) 0.037(2) 0.031(2) 0.0033(15) -0.0069(18) -0.0238(18) C44 0.057(2) 0.0366(19) 0.0268(18) 0.0014(14) -0.0103(16) -0.0240(17) C62 0.069(3) 0.053(2) 0.031(2) -0.0050(17) -0.0076(19) -0.029(2) C24 0.051(2) 0.066(3) 0.035(2) 0.0142(18) -0.0069(18) -0.032(2) C35 0.045(2) 0.052(2) 0.060(3) -0.029(2) 0.005(2) -0.025(2) C42 0.054(2) 0.0311(19) 0.045(2) 0.0044(15) -0.0157(18) -0.0131(17) C49 0.081(3) 0.044(2) 0.0254(19) 0.0055(16) -0.0138(19) -0.023(2) C26 0.068(3) 0.049(2) 0.034(2) 0.0014(16) -0.0183(19) -0.026(2) B1 0.0193(17) 0.0260(18) 0.0288(19) 0.0017(14) -0.0047(14) -0.0069(14) C39 0.064(3) 0.061(3) 0.051(3) -0.006(2) 0.000(2) -0.044(2) C60 0.057(3) 0.053(2) 0.049(2) -0.0128(18) -0.005(2) -0.036(2) C34 0.038(2) 0.048(2) 0.070(3) -0.0162(19) -0.008(2) -0.0223(18) C61 0.059(3) 0.039(2) 0.053(3) -0.0075(17) -0.011(2) -0.0206(19) C40 0.096(4) 0.038(2) 0.057(3) -0.0037(19) -0.003(3) -0.041(3) B2 0.031(2) 0.0258(18) 0.0244(19) 0.0020(14) -0.0065(15) -0.0085(15) C41 0.081(3) 0.025(2) 0.064(3) 0.0020(18) -0.008(2) -0.014(2) C50 0.131(5) 0.082(4) 0.034(2) 0.011(2) -0.012(3) -0.060(4) C36 0.161(6) 0.061(3) 0.060(3) 0.012(2) -0.069(4) -0.052(3) C52 0.144(6) 0.080(4) 0.029(2) -0.007(2) -0.010(3) -0.052(4) C51 0.112(5) 0.104(5) 0.057(3) 0.030(3) -0.040(3) -0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C8 1.402(4) . ? N1 C3 1.440(4) . ? N1 B1 1.456(4) . ? N2 C4 1.401(4) . ? N2 C7 1.437(4) . ? N2 B2 1.442(4) . ? C17 C22 1.396(4) . ? C17 C18 1.396(4) . ? C17 C1 1.476(4) . ? C11 C16 1.396(5) . ? C11 C12 1.396(5) . ? C11 B1 1.563(5) . ? C27 C32 1.376(5) . ? C27 C28 1.386(4) . ? C27 C2 1.496(4) . ? C4 C3 1.348(4) . ? C4 C9 1.497(4) . ? C7 C8 1.350(4) . ? C7 C6 1.460(4) . ? C8 C10 1.493(4) . ? C2 C1 1.369(4) . ? C2 C3 1.458(4) . ? C30 C29 1.385(5) . ? C30 C31 1.401(5) . ? C30 C33 1.540(4) . ? C18 C19 1.386(5) . ? C18 H18 0.9300 . ? C29 C28 1.387(4) . ? C29 H29 0.9300 . ? C20 C19 1.384(5) . ? C20 C21 1.392(5) . ? C20 C23 1.534(4) . ? C53 C58 1.384(5) . ? C53 C54 1.387(5) . ? C53 C6 1.493(4) . ? C6 C5 1.368(4) . ? C28 H28 0.9300 . ? C37 C38 1.391(5) . ? C37 C42 1.394(5) . ? C37 B2 1.563(5) . ? C54 C55 1.380(4) . ? C54 H54 0.9300 . ? C19 H19 0.9300 . ? C1 B1 1.538(5) . ? C5 C43 1.477(4) . ? C5 B2 1.547(5) . ? C43 C44 1.393(5) . ? C43 C48 1.397(5) . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C56 C57 1.389(5) . ? C56 C55 1.393(5) . ? C56 C59 1.530(4) . ? C23 C25 1.527(5) . ? C23 C24 1.533(5) . ? C23 C26 1.535(5) . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C58 C57 1.378(5) . ? C58 H58 0.9300 . ? C55 H55 0.9300 . ? C22 H22 0.9300 . ? C32 C31 1.384(5) . ? C32 H32 0.9300 . ? C33 C36 1.527(5) . ? C33 C34 1.529(5) . ? C33 C35 1.529(5) . ? C16 C15 1.377(5) . ? C16 H16 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C57 H57 0.9300 . ? C31 H31 0.9300 . ? C46 C45 1.388(5) . ? C46 C47 1.401(6) . ? C46 C49 1.525(5) . ? C59 C60 1.522(5) . ? C59 C62 1.529(5) . ? C59 C61 1.538(5) . ? C48 C47 1.381(5) . ? C48 H48 0.9300 . ? C38 C39 1.376(5) . ? C38 H38 0.9300 . ? C47 H47 0.9300 . ? C13 C14 1.369(6) . ? C13 H13 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C15 C14 1.367(6) . ? C15 H15 0.9300 . ? C14 H14 0.9300 . ? C45 C44 1.389(5) . ? C45 H45 0.9300 . ? C44 H44 0.9300 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C42 C41 1.387(6) . ? C42 H42 0.9300 . ? C49 C51 1.498(7) . ? C49 C52 1.518(6) . ? C49 C50 1.538(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C39 C40 1.372(7) . ? C39 H39 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C40 C41 1.366(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 N1 C3 118.5(2) . . ? C8 N1 B1 132.3(3) . . ? C3 N1 B1 109.2(2) . . ? C4 N2 C7 118.8(2) . . ? C4 N2 B2 131.4(3) . . ? C7 N2 B2 109.8(2) . . ? C22 C17 C18 116.4(3) . . ? C22 C17 C1 123.3(3) . . ? C18 C17 C1 120.3(3) . . ? C16 C11 C12 116.6(3) . . ? C16 C11 B1 123.0(3) . . ? C12 C11 B1 120.1(3) . . ? C32 C27 C28 117.3(3) . . ? C32 C27 C2 119.5(3) . . ? C28 C27 C2 123.1(3) . . ? C3 C4 N2 120.2(3) . . ? C3 C4 C9 124.1(3) . . ? N2 C4 C9 115.7(3) . . ? C8 C7 N2 120.8(3) . . ? C8 C7 C6 132.0(3) . . ? N2 C7 C6 107.2(2) . . ? C7 C8 N1 120.4(3) . . ? C7 C8 C10 124.3(3) . . ? N1 C8 C10 115.3(3) . . ? C1 C2 C3 110.8(3) . . ? C1 C2 C27 124.1(3) . . ? C3 C2 C27 124.3(3) . . ? C4 C3 N1 121.1(3) . . ? C4 C3 C2 131.7(3) . . ? N1 C3 C2 107.3(2) . . ? C29 C30 C31 116.8(3) . . ? C29 C30 C33 123.4(3) . . ? C31 C30 C33 119.8(3) . . ? C19 C18 C17 121.6(3) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C30 C29 C28 121.8(3) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C19 C20 C21 116.7(3) . . ? C19 C20 C23 122.7(3) . . ? C21 C20 C23 120.6(3) . . ? C58 C53 C54 117.7(3) . . ? C58 C53 C6 119.1(3) . . ? C54 C53 C6 123.1(3) . . ? C5 C6 C7 110.6(3) . . ? C5 C6 C53 123.8(3) . . ? C7 C6 C53 125.5(3) . . ? C27 C28 C29 121.2(3) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C38 C37 C42 116.6(3) . . ? C38 C37 B2 121.0(3) . . ? C42 C37 B2 122.3(3) . . ? C55 C54 C53 120.7(3) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C20 C19 C18 121.9(3) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C2 C1 C17 125.2(3) . . ? C2 C1 B1 107.8(3) . . ? C17 C1 B1 126.9(3) . . ? C6 C5 C43 124.8(3) . . ? C6 C5 B2 107.8(3) . . ? C43 C5 B2 127.5(3) . . ? C44 C43 C48 116.5(3) . . ? C44 C43 C5 120.7(3) . . ? C48 C43 C5 122.8(3) . . ? C22 C21 C20 121.8(3) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C57 C56 C55 116.5(3) . . ? C57 C56 C59 120.3(3) . . ? C55 C56 C59 123.3(3) . . ? C25 C23 C24 108.8(3) . . ? C25 C23 C20 112.4(3) . . ? C24 C23 C20 108.5(3) . . ? C25 C23 C26 107.8(3) . . ? C24 C23 C26 109.3(3) . . ? C20 C23 C26 110.0(3) . . ? C13 C12 C11 121.1(4) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C57 C58 C53 121.2(3) . . ? C57 C58 H58 119.4 . . ? C53 C58 H58 119.4 . . ? C54 C55 C56 122.0(3) . . ? C54 C55 H55 119.0 . . ? C56 C55 H55 119.0 . . ? C21 C22 C17 121.5(3) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C27 C32 C31 122.0(3) . . ? C27 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C36 C33 C34 110.2(4) . . ? C36 C33 C35 109.2(4) . . ? C34 C33 C35 106.9(3) . . ? C36 C33 C30 108.6(3) . . ? C34 C33 C30 110.4(3) . . ? C35 C33 C30 111.6(3) . . ? C15 C16 C11 122.0(4) . . ? C15 C16 H16 119.0 . . ? C11 C16 H16 119.0 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C58 C57 C56 121.8(3) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C32 C31 C30 121.0(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C45 C46 C47 116.2(3) . . ? C45 C46 C49 123.0(4) . . ? C47 C46 C49 120.8(4) . . ? C60 C59 C62 108.7(3) . . ? C60 C59 C56 112.6(3) . . ? C62 C59 C56 108.7(3) . . ? C60 C59 C61 107.7(3) . . ? C62 C59 C61 109.2(3) . . ? C56 C59 C61 109.9(3) . . ? C47 C48 C43 121.7(3) . . ? C47 C48 H48 119.2 . . ? C43 C48 H48 119.2 . . ? C39 C38 C37 122.5(4) . . ? C39 C38 H38 118.7 . . ? C37 C38 H38 118.7 . . ? C48 C47 C46 122.0(4) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C14 C13 C12 120.3(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C15 C16 120.0(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C46 C45 C44 121.9(4) . . ? C46 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? C45 C44 C43 121.7(3) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C42 C37 120.7(4) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C51 C49 C52 111.9(5) . . ? C51 C49 C46 109.2(4) . . ? C52 C49 C46 109.4(3) . . ? C51 C49 C50 107.1(4) . . ? C52 C49 C50 107.0(4) . . ? C46 C49 C50 112.2(4) . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 B1 C1 104.9(3) . . ? N1 B1 C11 129.4(3) . . ? C1 B1 C11 125.6(3) . . ? C40 C39 C38 119.6(4) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C41 C40 C39 119.7(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? N2 B2 C5 104.6(3) . . ? N2 B2 C37 127.7(3) . . ? C5 B2 C37 127.5(3) . . ? C40 C41 C42 120.9(4) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _refine_diff_density_max 0.758 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.103 _shelxl_version_number 2014/6 _shelx_res_file ; TITL shelxl_a.res in P-1 CELL 0.71073 10.8060 12.3580 21.0340 88.301 79.267 68.171 ZERR 4.000 0.0004 0.0003 0.0007 0.002 0.001 0.002 LATT 1 SFAC C H B N UNIT 124 136 4 4 OMIT -4.00 50.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 6 WGHT 0.109300 2.788500 FVAR 0.27921 N1 4 0.225811 0.309181 0.431198 11.00000 0.02518 0.02150 = 0.02333 -0.00051 -0.00487 -0.01027 N2 4 0.225361 0.485406 0.344667 11.00000 0.02888 0.01994 = 0.02601 -0.00087 -0.00600 -0.01034 C17 1 0.215343 0.278271 0.612724 11.00000 0.02667 0.02821 = 0.02596 0.00134 -0.00764 -0.01500 C11 1 0.236344 0.105924 0.488835 11.00000 0.03410 0.02664 = 0.02164 0.00235 -0.01040 -0.01473 C27 1 0.239310 0.505629 0.561144 11.00000 0.02633 0.02635 = 0.02392 0.00275 -0.00458 -0.01183 C4 1 0.219002 0.505500 0.410620 11.00000 0.02664 0.02522 = 0.02530 -0.00194 -0.00389 -0.01302 C7 1 0.221023 0.377331 0.323875 11.00000 0.02314 0.02258 = 0.02511 -0.00314 -0.00388 -0.00972 C8 1 0.224356 0.291841 0.365795 11.00000 0.02341 0.02483 = 0.02687 0.00032 -0.00734 -0.00965 C2 1 0.218463 0.416676 0.522134 11.00000 0.02304 0.02561 = 0.02296 -0.00063 -0.00353 -0.00909 C3 1 0.220805 0.420633 0.452601 11.00000 0.02212 0.02190 = 0.02595 -0.00199 -0.00304 -0.00766 C30 1 0.286280 0.665394 0.638272 11.00000 0.03311 0.02979 = 0.02199 0.00128 -0.00602 -0.01530 C18 1 0.296751 0.166229 0.626961 11.00000 0.03489 0.02616 = 0.02859 -0.00346 -0.00597 -0.01077 AFIX 43 H18 2 0.349041 0.112538 0.593146 11.00000 -1.20000 AFIX 0 C29 1 0.156945 0.681133 0.629503 11.00000 0.02753 0.02920 = 0.02911 -0.00393 0.00185 -0.01055 AFIX 43 H29 2 0.083790 0.745678 0.649477 11.00000 -1.20000 AFIX 0 C20 1 0.224602 0.208413 0.742633 11.00000 0.03278 0.03336 = 0.02453 0.00376 -0.00820 -0.01825 C53 1 0.226607 0.285852 0.211822 11.00000 0.03155 0.02501 = 0.02307 0.00152 -0.00963 -0.01104 C6 1 0.221327 0.382580 0.254425 11.00000 0.02609 0.02445 = 0.02549 -0.00303 -0.00533 -0.00970 C28 1 0.133580 0.603229 0.591735 11.00000 0.02009 0.03220 = 0.02714 -0.00337 -0.00156 -0.00914 AFIX 43 H28 2 0.045347 0.616704 0.586836 11.00000 -1.20000 AFIX 0 C37 1 0.255022 0.675246 0.288111 11.00000 0.04280 0.02758 = 0.02272 0.00258 -0.00884 -0.01527 C54 1 0.115130 0.256351 0.210470 11.00000 0.03099 0.03495 = 0.02370 -0.00353 -0.00271 -0.01425 AFIX 43 H54 2 0.032529 0.297617 0.237226 11.00000 -1.20000 AFIX 0 C19 1 0.301570 0.133031 0.690253 11.00000 0.03577 0.02512 = 0.03165 0.00379 -0.01217 -0.01095 AFIX 43 H19 2 0.358138 0.057951 0.697755 11.00000 -1.20000 AFIX 0 C1 1 0.216223 0.312272 0.544817 11.00000 0.02466 0.02651 = 0.02572 0.00105 -0.00509 -0.00921 C5 1 0.226190 0.486276 0.232068 11.00000 0.02991 0.02809 = 0.02604 0.00107 -0.00616 -0.01164 C43 1 0.227546 0.520333 0.164095 11.00000 0.03783 0.02132 = 0.02653 -0.00232 -0.00683 -0.00809 C21 1 0.139504 0.318843 0.728695 11.00000 0.03326 0.03320 = 0.02775 -0.00249 -0.00215 -0.01096 AFIX 43 H21 2 0.083992 0.370934 0.762652 11.00000 -1.20000 AFIX 0 C56 1 0.246140 0.102980 0.128152 11.00000 0.03515 0.03063 = 0.02498 0.00146 -0.00601 -0.01780 C23 1 0.227463 0.172860 0.812998 11.00000 0.04295 0.03838 = 0.02790 0.00370 -0.01138 -0.02171 C12 1 0.131504 0.077527 0.525223 11.00000 0.03628 0.03508 = 0.04424 0.00813 -0.00975 -0.01775 AFIX 43 H12 2 0.052713 0.136869 0.545608 11.00000 -1.20000 AFIX 0 C58 1 0.346089 0.225302 0.169370 11.00000 0.02860 0.03693 = 0.03758 -0.00478 -0.00465 -0.01760 AFIX 43 H58 2 0.421541 0.244924 0.168461 11.00000 -1.20000 AFIX 0 C55 1 0.125422 0.166497 0.169885 11.00000 0.03616 0.04038 = 0.02738 0.00069 -0.00557 -0.02327 AFIX 43 H55 2 0.049491 0.147754 0.170398 11.00000 -1.20000 AFIX 0 C22 1 0.135286 0.353267 0.665521 11.00000 0.03504 0.02817 = 0.02797 0.00196 -0.00406 -0.01074 AFIX 43 H22 2 0.077765 0.428074 0.658170 11.00000 -1.20000 AFIX 0 C32 1 0.368241 0.489887 0.569248 11.00000 0.02795 0.02693 = 0.04167 -0.00832 -0.00486 -0.00561 AFIX 43 H32 2 0.441012 0.425383 0.548962 11.00000 -1.20000 AFIX 0 C33 1 0.315922 0.747055 0.681984 11.00000 0.04452 0.03604 = 0.03301 -0.00116 -0.01207 -0.01994 C16 1 0.353378 0.012694 0.461068 11.00000 0.04589 0.02930 = 0.03458 0.00380 -0.00561 -0.01451 AFIX 43 H16 2 0.426215 0.028183 0.437367 11.00000 -1.20000 AFIX 0 C10 1 0.229721 0.174210 0.347423 11.00000 0.05374 0.02611 = 0.02817 0.00020 -0.01549 -0.01838 AFIX 137 H10A 2 0.220006 0.172603 0.303053 11.00000 -1.50000 H10B 2 0.157341 0.158253 0.374753 11.00000 -1.50000 H10C 2 0.315267 0.116121 0.352649 11.00000 -1.50000 AFIX 0 C57 1 0.355312 0.136520 0.128442 11.00000 0.02766 0.03378 = 0.03581 -0.00905 -0.00049 -0.01263 AFIX 43 H57 2 0.436837 0.097985 0.100239 11.00000 -1.20000 AFIX 0 C31 1 0.392864 0.567204 0.606699 11.00000 0.02399 0.03627 = 0.04609 -0.00824 -0.01254 -0.00908 AFIX 43 H31 2 0.481445 0.553786 0.610969 11.00000 -1.20000 AFIX 0 C46 1 0.235328 0.586883 0.032641 11.00000 0.05813 0.02764 = 0.02660 0.00098 -0.00950 -0.01095 C59 1 0.260809 0.002986 0.082496 11.00000 0.04109 0.03848 = 0.02848 -0.00597 -0.00349 -0.02278 C48 1 0.145750 0.498774 0.125893 11.00000 0.04547 0.03567 = 0.03346 0.00558 -0.01298 -0.02044 AFIX 43 H48 2 0.087324 0.461736 0.143685 11.00000 -1.20000 AFIX 0 C38 1 0.382509 0.677799 0.288507 11.00000 0.04425 0.03697 = 0.04706 0.00071 -0.00612 -0.02028 AFIX 43 H38 2 0.454323 0.607843 0.290861 11.00000 -1.20000 AFIX 0 C47 1 0.149444 0.531071 0.062364 11.00000 0.05816 0.03804 = 0.03115 0.00045 -0.01897 -0.01455 AFIX 43 H47 2 0.093193 0.515285 0.038585 11.00000 -1.20000 AFIX 0 C13 1 0.142820 -0.037682 0.531501 11.00000 0.05694 0.05182 = 0.05397 0.01821 -0.02069 -0.03854 AFIX 43 H13 2 0.071401 -0.054770 0.555507 11.00000 -1.20000 AFIX 0 C25 1 0.341141 0.055884 0.818209 11.00000 0.05450 0.04568 = 0.03130 0.01094 -0.01545 -0.01598 AFIX 137 H25A 2 0.325809 -0.004637 0.797177 11.00000 -1.50000 H25B 2 0.342413 0.039450 0.863029 11.00000 -1.50000 H25C 2 0.426681 0.059286 0.797698 11.00000 -1.50000 AFIX 0 C9 1 0.206436 0.625354 0.429815 11.00000 0.06826 0.02802 = 0.02615 -0.00243 -0.00733 -0.01998 AFIX 137 H9A 2 0.184434 0.635663 0.476162 11.00000 -1.50000 H9B 2 0.135893 0.682353 0.411408 11.00000 -1.50000 H9C 2 0.290922 0.634911 0.414186 11.00000 -1.50000 AFIX 0 C15 1 0.364229 -0.101481 0.467711 11.00000 0.06824 0.02519 = 0.04633 0.00159 -0.00991 -0.01140 AFIX 43 H15 2 0.443422 -0.161716 0.448511 11.00000 -1.20000 AFIX 0 C14 1 0.258656 -0.126319 0.502512 11.00000 0.07944 0.03196 = 0.05095 0.00694 -0.02669 -0.02983 AFIX 43 H14 2 0.265498 -0.203392 0.506500 11.00000 -1.20000 AFIX 0 C45 1 0.315221 0.609556 0.070987 11.00000 0.06291 0.03705 = 0.03146 0.00334 -0.00692 -0.02378 AFIX 43 H45 2 0.373228 0.647028 0.053265 11.00000 -1.20000 AFIX 0 C44 1 0.311087 0.577922 0.135063 11.00000 0.05688 0.03664 = 0.02682 0.00141 -0.01033 -0.02400 AFIX 43 H44 2 0.365495 0.595651 0.159197 11.00000 -1.20000 AFIX 0 C62 1 0.279739 0.041335 0.012762 11.00000 0.06939 0.05313 = 0.03122 -0.00503 -0.00758 -0.02860 AFIX 137 H62A 2 0.200666 0.107170 0.007080 11.00000 -1.50000 H62B 2 0.292567 -0.021783 -0.016455 11.00000 -1.50000 H62C 2 0.357872 0.062702 0.003870 11.00000 -1.50000 AFIX 0 C24 1 0.091000 0.163779 0.842576 11.00000 0.05095 0.06550 = 0.03507 0.01422 -0.00689 -0.03233 AFIX 137 H24A 2 0.019065 0.237941 0.841269 11.00000 -1.50000 H24B 2 0.091279 0.141670 0.886704 11.00000 -1.50000 H24C 2 0.077222 0.106041 0.818272 11.00000 -1.50000 AFIX 0 C35 1 0.189870 0.856354 0.704861 11.00000 0.04547 0.05188 = 0.05952 -0.02869 0.00456 -0.02494 AFIX 137 H35A 2 0.120071 0.834281 0.730174 11.00000 -1.50000 H35B 2 0.157964 0.897014 0.667958 11.00000 -1.50000 H35C 2 0.212426 0.906397 0.730817 11.00000 -1.50000 AFIX 0 C42 1 0.151258 0.782023 0.283177 11.00000 0.05389 0.03113 = 0.04475 0.00440 -0.01570 -0.01315 AFIX 43 H42 2 0.064696 0.784381 0.281978 11.00000 -1.20000 AFIX 0 C49 1 0.238108 0.620444 -0.037801 11.00000 0.08137 0.04429 = 0.02541 0.00549 -0.01384 -0.02330 C26 1 0.249151 0.265204 0.852025 11.00000 0.06765 0.04887 = 0.03364 0.00140 -0.01829 -0.02604 AFIX 137 H26A 2 0.334529 0.271071 0.833594 11.00000 -1.50000 H26B 2 0.249376 0.242969 0.896136 11.00000 -1.50000 H26C 2 0.177111 0.339311 0.850748 11.00000 -1.50000 AFIX 0 B1 3 0.225326 0.235645 0.486520 11.00000 0.01930 0.02597 = 0.02883 0.00167 -0.00469 -0.00688 C39 1 0.406408 0.779882 0.285547 11.00000 0.06397 0.06053 = 0.05088 -0.00553 0.00045 -0.04414 AFIX 43 H39 2 0.492758 0.778442 0.286366 11.00000 -1.20000 AFIX 0 C60 1 0.137628 -0.031836 0.095409 11.00000 0.05663 0.05293 = 0.04862 -0.01284 -0.00452 -0.03631 AFIX 137 H60A 2 0.122002 -0.052432 0.139729 11.00000 -1.50000 H60B 2 0.153757 -0.097511 0.067379 11.00000 -1.50000 H60C 2 0.059405 0.032465 0.087265 11.00000 -1.50000 AFIX 0 C34 1 0.424861 0.788265 0.644762 11.00000 0.03835 0.04839 = 0.06957 -0.01622 -0.00764 -0.02226 AFIX 137 H34A 2 0.450500 0.830942 0.673900 11.00000 -1.50000 H34B 2 0.389629 0.837843 0.611140 11.00000 -1.50000 H34C 2 0.502864 0.721889 0.625873 11.00000 -1.50000 AFIX 0 C61 1 0.385490 -0.105242 0.090567 11.00000 0.05899 0.03892 = 0.05342 -0.00747 -0.01098 -0.02061 AFIX 137 H61A 2 0.464443 -0.085052 0.084001 11.00000 -1.50000 H61B 2 0.398535 -0.165415 0.059311 11.00000 -1.50000 H61C 2 0.371331 -0.132826 0.133429 11.00000 -1.50000 AFIX 0 C40 1 0.301979 0.883819 0.281378 11.00000 0.09582 0.03786 = 0.05704 -0.00373 -0.00300 -0.04052 AFIX 43 H40 2 0.317125 0.953265 0.279477 11.00000 -1.20000 AFIX 0 B2 3 0.232609 0.557251 0.289911 11.00000 0.03066 0.02578 = 0.02437 0.00198 -0.00651 -0.00852 C41 1 0.175691 0.884784 0.280035 11.00000 0.08084 0.02540 = 0.06383 0.00203 -0.00823 -0.01354 AFIX 43 H41 2 0.105151 0.955256 0.276974 11.00000 -1.20000 AFIX 0 C50 1 0.341385 0.678346 -0.061080 11.00000 0.13084 0.08242 = 0.03366 0.01068 -0.01165 -0.05958 AFIX 137 H50A 2 0.341432 0.696216 -0.105811 11.00000 -1.50000 H50B 2 0.430313 0.625982 -0.056335 11.00000 -1.50000 H50C 2 0.316855 0.748971 -0.035620 11.00000 -1.50000 AFIX 0 C36 1 0.363697 0.680878 0.740856 11.00000 0.16108 0.06132 = 0.05986 0.01156 -0.06904 -0.05216 AFIX 137 H36A 2 0.446203 0.614955 0.726851 11.00000 -1.50000 H36B 2 0.295166 0.654423 0.763500 11.00000 -1.50000 H36C 2 0.379752 0.731661 0.769220 11.00000 -1.50000 AFIX 0 C52 1 0.280087 0.511420 -0.080781 11.00000 0.14433 0.07970 = 0.02920 -0.00712 -0.00982 -0.05184 AFIX 137 H52A 2 0.215905 0.474210 -0.068707 11.00000 -1.50000 H52B 2 0.368596 0.458732 -0.075643 11.00000 -1.50000 H52C 2 0.282312 0.532354 -0.125180 11.00000 -1.50000 AFIX 0 C51 1 0.101202 0.706969 -0.044542 11.00000 0.11225 0.10352 = 0.05685 0.03048 -0.04041 -0.01868 AFIX 137 H51A 2 0.034417 0.672565 -0.032043 11.00000 -1.50000 H51B 2 0.102752 0.728854 -0.088772 11.00000 -1.50000 H51C 2 0.078715 0.774929 -0.017130 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelxl_a.res in P-1 REM R1 = 0.0714 for 6611 Fo > 4sig(Fo) and 0.1066 for all 8951 data REM 609 parameters refined using 0 restraints END WGHT 0.1066 2.6991 REM Highest difference peak 0.758, deepest hole -0.393, 1-sigma level 0.103 Q1 1 0.1015 0.5990 -0.0679 11.00000 0.05 0.76 Q2 1 0.2062 0.7479 -0.0470 11.00000 0.05 0.56 Q3 1 0.3498 0.5606 -0.0757 11.00000 0.05 0.47 Q4 1 0.3821 0.6000 0.7580 11.00000 0.05 0.32 Q5 1 0.0964 -0.0385 0.5383 11.00000 0.05 0.32 Q6 1 0.2142 0.7547 -0.1128 11.00000 0.05 0.32 Q7 1 0.1989 0.8002 0.7396 11.00000 0.05 0.32 Q8 1 0.2181 -0.0977 0.5421 11.00000 0.05 0.31 Q9 1 0.2058 0.7219 0.8275 11.00000 0.05 0.30 Q10 1 0.2225 0.9024 0.3800 11.00000 0.05 0.30 Q11 1 0.2934 0.7016 0.6616 11.00000 0.05 0.30 Q12 1 0.3884 0.6832 0.7235 11.00000 0.05 0.29 Q13 1 0.2860 0.8240 0.7834 11.00000 0.05 0.29 Q14 1 -0.0229 -0.0254 0.5451 11.00000 0.05 0.29 Q15 1 0.1972 0.5341 -0.1223 11.00000 0.05 0.29 Q16 1 -0.0452 -0.0055 0.5612 11.00000 0.05 0.29 Q17 1 0.3402 0.5160 -0.1331 11.00000 0.05 0.29 Q18 1 0.1380 0.0049 0.5306 11.00000 0.05 0.28 Q19 1 0.2788 -0.0994 0.4651 11.00000 0.05 0.28 Q20 1 0.3129 0.6869 -0.1644 11.00000 0.05 0.27 ; 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1045.60 18.65 1 -2 0 291.99 6.46 1 -2 1 44.05 0.92 1 -2 2 36.61 0.84 1 -2 3 30.29 0.55 1 -2 4 899.34 12.52 1 -2 5 103.98 1.62 1 -2 6 24.03 0.44 1 -2 7 28.99 0.54 1 -2 8 6.08 0.22 1 -2 9 515.09 7.45 1 -2 10 31.56 0.62 1 -2 11 4.53 0.19 1 -2 12 4.92 0.22 1 -2 13 14.28 0.38 1 -2 14 0.22 0.17 1 -2 15 0.57 0.57 1 -2 16 0.69 0.15 1 -2 17 67.86 1.48 1 -2 18 46.05 1.69 1 -2 19 9.26 0.88 1 -2 20 13.61 1.06 1 -2 22 9.35 1.12 1 -2 23 0.71 0.59 1 -2 24 1.44 0.76 1 -2 26 0.42 0.91 1 -1 -25 1.68 0.75 1 -1 -24 0.94 0.96 1 -1 -23 38.19 2.34 1 -1 -22 18.45 1.28 1 -1 -21 2.94 0.87 1 -1 -20 0.96 0.66 1 -1 -19 26.32 1.63 1 -1 -18 0.15 0.54 1 -1 -16 61.16 2.41 1 -1 -15 11.80 0.96 1 -1 -14 19.71 1.10 1 -1 -13 51.54 2.00 1 -1 -12 92.83 3.45 1 -1 -11 2.92 0.56 1 -1 -10 81.96 2.97 1 -1 -9 119.41 3.04 1 -1 -8 0.22 0.22 1 -1 -7 131.44 2.51 1 -1 -6 40.69 0.83 1 -1 -5 206.16 3.86 1 -1 -4 5.21 0.25 1 -1 -3 192.40 3.45 1 -1 -2 25.77 0.56 1 -1 -1 335.46 5.28 1 -1 0 -0.27 0.10 1 -1 2 81.42 1.53 1 -1 3 2196.59 69.44 1 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6 379.24 7.17 1 0 7 0.62 0.17 1 0 8 1.19 0.23 1 0 9 8.06 0.28 1 0 10 108.38 1.97 1 0 11 8.72 0.38 1 0 12 7.72 0.30 1 0 13 8.49 0.32 1 0 14 0.71 0.13 1 0 15 150.19 2.92 1 0 16 1.48 0.15 1 0 17 4.09 0.54 1 0 18 29.42 1.24 1 0 19 4.79 0.87 1 0 20 4.66 0.92 1 0 21 -0.20 0.84 1 0 22 0.57 0.72 1 0 23 3.51 0.78 1 0 24 2.19 0.72 1 0 25 22.40 1.60 1 0 26 7.42 1.14 1 0 27 6.33 1.28 1 1 -26 2.42 0.79 1 1 -25 12.99 1.25 1 1 -23 3.01 0.76 1 1 -22 3.31 0.92 1 1 -21 1.21 0.57 1 1 -20 -1.53 0.79 1 1 -19 7.48 0.84 1 1 -18 7.81 1.00 1 1 -17 10.67 0.81 1 1 -16 4.72 0.82 1 1 -15 -0.05 0.50 1 1 -14 60.69 2.32 1 1 -13 2.27 0.65 1 1 -12 3.38 0.66 1 1 -11 54.51 1.98 1 1 -10 0.49 0.40 1 1 -9 339.48 10.99 1 1 -8 120.94 2.30 1 1 -7 0.25 0.10 1 1 -6 297.62 5.49 1 1 -5 24.77 0.64 1 1 -4 326.96 7.37 1 1 -1 0.02 0.05 1 1 2 -0.05 0.05 1 1 4 29.91 0.87 1 1 5 1078.97 16.66 1 1 6 276.56 4.46 1 1 7 148.73 2.55 1 1 8 0.57 0.17 1 1 9 137.67 2.33 1 1 10 148.73 3.03 1 1 11 63.67 1.43 1 1 12 57.26 1.35 1 1 13 1.41 0.20 1 1 14 5.32 0.30 1 1 15 79.37 1.42 1 1 16 36.61 1.02 1 1 17 9.35 0.97 1 1 18 4.98 0.80 1 1 19 4.72 0.80 1 1 20 7.81 0.81 1 1 21 10.03 0.88 1 1 22 1.16 0.74 1 1 23 10.09 1.08 1 1 24 2.84 0.97 1 1 25 -0.94 0.87 1 1 26 5.98 1.19 1 2 -26 4.89 0.84 1 2 -25 4.44 0.99 1 2 -24 1.13 0.69 1 2 -23 2.27 0.91 1 2 -22 2.25 0.76 1 2 -21 -0.07 0.77 1 2 -20 8.31 0.83 1 2 -19 3.76 0.89 1 2 -18 29.05 1.50 1 2 -17 14.09 1.12 1 2 -15 3.01 0.52 1 2 -14 1.41 0.64 1 2 -13 57.56 2.26 1 2 -12 -0.42 0.15 1 2 -11 -0.42 0.32 1 2 -10 10.70 0.36 1 2 -9 340.95 6.79 1 2 -8 0.05 0.15 1 2 -7 23.79 0.58 1 2 -6 1.44 0.10 1 2 -5 581.42 10.55 1 2 -4 1020.35 15.88 1 2 -3 64.79 1.52 1 2 2 135.34 4.74 1 2 3 37.94 1.90 1 2 4 12.32 0.35 1 2 5 506.78 8.06 1 2 6 47.55 0.89 1 2 7 6.86 0.23 1 2 8 0.42 0.15 1 2 9 0.47 0.20 1 2 10 1.39 0.25 1 2 11 69.10 1.98 1 2 12 32.92 0.91 1 2 13 16.62 0.61 1 2 14 8.69 0.23 1 2 15 61.24 1.48 1 2 16 82.68 1.99 1 2 17 3.46 0.68 1 2 18 0.62 0.64 1 2 19 15.66 1.38 1 2 20 0.87 0.56 1 2 21 5.89 0.80 1 2 22 6.33 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2 18.80 0.47 1 7 3 20.83 0.45 1 7 4 6.51 0.23 1 7 5 12.96 0.36 1 7 6 0.25 0.20 1 7 7 34.65 1.11 1 7 8 33.37 1.09 1 7 9 69.76 2.08 1 7 10 3.24 1.14 1 7 11 5.27 0.50 1 7 12 67.54 2.13 1 7 13 62.72 2.05 1 7 14 1.06 0.49 1 7 15 3.55 0.64 1 7 16 -0.47 0.64 1 7 17 1.80 0.64 1 7 18 0.02 0.47 1 7 19 10.38 1.06 1 7 20 14.09 1.12 1 8 -18 2.22 0.70 1 8 -17 2.01 0.62 1 8 -16 2.47 0.55 1 8 -15 1.53 0.54 1 8 -14 63.51 2.62 1 8 -13 3.44 0.39 1 8 -12 7.70 0.44 1 8 -11 111.72 3.05 1 8 -10 47.69 1.37 1 8 -9 55.32 1.63 1 8 -8 1.19 0.27 1 8 -7 3.01 0.33 1 8 -6 2.64 0.32 1 8 -4 1.51 0.12 1 8 -3 0.00 0.25 1 8 -2 5.62 0.23 1 8 -1 151.04 4.77 1 8 1 28.14 0.63 1 8 2 0.84 0.10 1 8 3 0.12 0.07 1 8 4 14.77 0.38 1 8 5 0.59 0.18 1 8 6 23.02 0.71 1 8 7 1.09 0.22 1 8 8 32.01 1.07 1 8 9 5.03 0.42 1 8 10 84.23 2.65 1 8 11 39.74 1.38 1 8 12 29.74 1.14 1 8 13 52.04 1.79 1 8 14 14.09 0.82 1 8 15 4.61 0.62 1 8 16 0.59 0.34 1 9 -13 8.52 0.78 1 9 -12 0.39 0.39 1 9 -11 118.76 3.36 1 9 -10 39.05 1.31 1 9 -9 6.11 0.39 1 9 -8 4.57 0.72 1 9 -7 4.76 0.35 1 9 -6 89.61 3.20 1 9 -5 13.98 0.63 1 9 -3 9.14 0.24 1 9 1 22.73 1.61 1 9 2 8.57 0.90 1 9 3 3.29 0.13 1 9 4 41.64 0.83 1 9 5 33.26 0.92 1 9 6 22.03 0.70 1 9 7 4.36 0.29 1 9 8 68.52 1.97 1 9 9 11.30 1.37 1 9 10 29.48 1.24 1 9 11 9.23 1.57 1 9 12 1.61 1.21 1 9 13 1.39 1.22 1 10 -14 4.61 0.75 1 10 -12 40.43 2.02 1 10 -11 0.87 0.72 1 10 -10 7.95 0.87 1 10 -9 12.74 0.96 1 10 -8 15.98 0.99 1 10 -7 -1.01 0.69 1 10 -6 2.67 0.80 1 10 0 42.94 2.21 1 10 1 23.16 1.58 1 10 2 64.87 2.96 1 10 3 29.91 2.01 1 10 4 35.42 2.19 1 10 5 12.64 0.88 1 10 6 14.62 0.91 1 10 7 9.69 0.81 1 10 8 54.66 3.09 1 10 9 16.62 1.54 1 10 10 1.31 0.99 1 10 11 2.42 1.08 1 10 12 -1.01 0.99 1 11 -14 0.42 0.49 1 11 -13 4.07 0.78 1 11 -12 -2.19 0.65 1 11 -11 -0.74 0.55 1 11 -10 1.41 0.59 1 11 -9 24.08 1.46 1 11 -8 79.46 3.37 1 11 -7 1.19 0.91 1 11 -6 3.51 0.89 1 11 -5 6.66 1.15 1 11 -1 15.04 1.35 1 11 0 3.22 0.98 1 11 1 7.45 1.19 1 11 2 29.58 1.73 1 11 3 29.10 1.88 1 11 4 0.62 0.87 1 11 5 5.46 1.11 1 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