data_a14150_0m _audit_creation_date 2015-05-05 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2013-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H79 N2 Ni2 P4, C F3 O3 S, C6 H6' _chemical_formula_sum 'C65 H85 F3 N2 Ni2 O3 P4 S' _chemical_formula_weight 1272.71 _chemical_melting_point ? 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' 'F' 'F' 0.0171 0.0103 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.003(3) _cell_length_b 13.924(2) _cell_length_c 22.832(4) _cell_angle_alpha 90 _cell_angle_beta 99.777(4) _cell_angle_gamma 90 _cell_volume 6267.1(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9992 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.24 _cell_measurement_theta_min 2.33 _shelx_estimated_absorpt_T_max 0.961 _shelx_estimated_absorpt_T_min 0.657 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0616 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.8992. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2688 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_unetI/netI 0.0705 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 84832 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.677 _diffrn_reflns_theta_min 1.720 _diffrn_ambient_temperature 100.01 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 10238 _reflns_number_total 14952 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 0.688 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.083 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 737 _refine_ls_number_reflns 14952 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0437 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+3.4813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0970 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C50(H50), C30(H30), C56(H56), C53(H53), C47(H47), C1(H1), C18(H18), C21(H21), C24(H24), C27(H27) 2.b Aromatic/amide H refined with riding coordinates: C4(H4), N2(H2), C33(H33), C32(H32), C46(H46), C45(H45), C44(H44), C43(H43), C40(H40), C39(H39), C38(H38), C37(H37), C3(H3), C11(H11), C10(H10), C9(H9), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C63(H63), C62(H62), C61(H61), C60(H60), C64(H64), C65(H65) 2.c Idealised Me refined as rotating group: C58(H58A,H58B,H58C), C55(H55A,H55B,H55C), C49(H49A,H49B,H49C), C52(H52A,H52B, H52C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C54(H54A,H54B,H54C), C48(H48A, H48B,H48C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C28(H28A,H28B, H28C), C29(H29A,H29B,H29C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 Ni1 Ni 1.04813(2) 0.20479(2) -0.18470(2) 0.01322(8) Uani 1 1 d . . . . . Ni2 Ni 1.31242(2) 0.09668(2) -0.07411(2) 0.01123(8) Uani 1 1 d . . . . . N1 N 1.22506(10) 0.14675(14) -0.12606(8) 0.0125(4) Uani 1 1 d . . . . . S1 S 1.27343(4) 0.50374(5) 0.09164(3) 0.02397(16) Uani 1 1 d . . . . . P3 P 1.27708(3) -0.05182(5) -0.05137(3) 0.01387(14) Uani 1 1 d . . . . . P4 P 1.39150(3) 0.13506(5) -0.13170(3) 0.01159(13) Uani 1 1 d . . . . . P1 P 1.00440(3) 0.11341(5) -0.25854(3) 0.01385(14) Uani 1 1 d . . . . . P2 P 1.00703(3) 0.28873(5) -0.11871(3) 0.01675(14) Uani 1 1 d . . . . . C58 C 1.40757(13) 0.21475(19) -0.24628(11) 0.0200(6) Uani 1 1 d . . . . . H58A H 1.4459 0.2543 -0.2276 0.030 Uiso 1 1 calc GR . . . . H58B H 1.3839 0.2472 -0.2819 0.030 Uiso 1 1 calc GR . . . . H58C H 1.4244 0.1523 -0.2573 0.030 Uiso 1 1 calc GR . . . . C55 C 1.41917(14) -0.02599(19) -0.19794(11) 0.0205(6) Uani 1 1 d . . . . . H55A H 1.3895 -0.0667 -0.1785 0.031 Uiso 1 1 calc GR . . . . H55B H 1.4539 -0.0658 -0.2115 0.031 Uiso 1 1 calc GR . . . . H55C H 1.3922 0.0064 -0.2321 0.031 Uiso 1 1 calc GR . . . . C49 C 1.26775(14) -0.1640(2) -0.15374(11) 0.0226(6) Uani 1 1 d . . . . . H49A H 1.2183 -0.1577 -0.1594 0.034 Uiso 1 1 calc GR . . . . H49B H 1.2797 -0.2238 -0.1721 0.034 Uiso 1 1 calc GR . . . . H49C H 1.2869 -0.1093 -0.1723 0.034 Uiso 1 1 calc GR . . . . F2 F 1.15908(10) 0.55894(17) 0.02659(8) 0.0593(6) Uani 1 1 d . . . . . F1 F 1.21952(8) 0.46457(11) -0.01728(6) 0.0291(4) Uani 1 1 d . . . . . F3 F 1.24756(12) 0.61220(13) -0.00406(8) 0.0566(6) Uani 1 1 d . . . . . C4 C 1.19149(12) 0.22462(18) -0.11466(10) 0.0138(5) Uani 1 1 d . . . . . H4 H 1.2024 0.2510 -0.0758 0.017 Uiso 1 1 calc R . . . . N2 N 1.28699(11) 0.26154(16) 0.04146(9) 0.0188(5) Uani 1 1 d . . . . . H2 H 1.2612 0.3057 0.0539 0.023 Uiso 1 1 calc R . . . . C33 C 1.33104(13) 0.28645(19) 0.00545(10) 0.0182(5) Uani 1 1 d . . . . . H33 H 1.3327 0.3515 -0.0068 0.022 Uiso 1 1 calc R . . . . O2 O 1.33894(10) 0.48782(15) 0.07550(9) 0.0319(5) Uani 1 1 d . . . . . O1 O 1.23919(10) 0.41770(14) 0.10565(8) 0.0282(5) Uani 1 1 d . . . . . O3 O 1.26909(12) 0.58394(15) 0.13014(9) 0.0420(6) Uani 1 1 d . . . . . C5 C 1.14007(12) 0.27271(18) -0.15591(10) 0.0128(5) Uani 1 1 d . . . . . C50 C 1.18254(12) -0.05905(19) -0.06073(11) 0.0179(6) Uani 1 1 d . . . . . H50 H 1.1647 -0.0372 -0.1022 0.021 Uiso 1 1 calc R . . . . C52 C 1.15192(13) -0.1583(2) -0.05407(12) 0.0249(6) Uani 1 1 d . . . . . H52A H 1.1024 -0.1530 -0.0594 0.037 Uiso 1 1 calc GR . . . . H52B H 1.1693 -0.1837 -0.0144 0.037 Uiso 1 1 calc GR . . . . H52C H 1.1644 -0.2017 -0.0842 0.037 Uiso 1 1 calc GR . . . . C51 C 1.15601(13) 0.0119(2) -0.01922(12) 0.0240(6) Uani 1 1 d . . . . . H51A H 1.1704 -0.0085 0.0221 0.036 Uiso 1 1 calc GR . . . . H51B H 1.1064 0.0139 -0.0283 0.036 Uiso 1 1 calc GR . . . . H51C H 1.1743 0.0760 -0.0247 0.036 Uiso 1 1 calc GR . . . . C36 C 1.30219(12) -0.07815(18) 0.02823(10) 0.0152(5) Uani 1 1 d . . . . . C35 C 1.31861(12) 0.00067(19) 0.06543(11) 0.0165(5) Uani 1 1 d . . . . . C31 C 1.32131(12) 0.09861(19) 0.04041(10) 0.0165(5) Uani 1 1 d . . . . . C32 C 1.28204(13) 0.16912(19) 0.05866(11) 0.0189(6) Uani 1 1 d . . . . . H32 H 1.2506 0.1530 0.0839 0.023 Uiso 1 1 calc R . . . . C34 C 1.37371(12) 0.22066(18) -0.01410(10) 0.0146(5) Uani 1 1 d . . . . . C30 C 1.37103(12) 0.12085(17) 0.00278(10) 0.0129(5) Uani 1 1 d . . . . . H30 H 1.4151 0.0853 0.0109 0.015 Uiso 1 1 calc R . . . . C41 C 1.43331(12) 0.25761(17) -0.03814(10) 0.0137(5) Uani 1 1 d . . . . . C46 C 1.47493(13) 0.32669(18) -0.00600(11) 0.0189(6) Uani 1 1 d . . . . . H46 H 1.4637 0.3512 0.0299 0.023 Uiso 1 1 calc R . . . . C45 C 1.53241(13) 0.35996(19) -0.02585(11) 0.0199(6) Uani 1 1 d . . . . . H45 H 1.5597 0.4081 -0.0041 0.024 Uiso 1 1 calc R . . . . C44 C 1.55015(13) 0.32325(18) -0.07722(11) 0.0174(6) Uani 1 1 d . . . . . H44 H 1.5898 0.3455 -0.0907 0.021 Uiso 1 1 calc R . . . . C43 C 1.50979(12) 0.25371(18) -0.10911(10) 0.0155(5) Uani 1 1 d . . . . . H43 H 1.5227 0.2274 -0.1439 0.019 Uiso 1 1 calc R . . . . C42 C 1.45050(12) 0.22167(17) -0.09091(10) 0.0131(5) Uani 1 1 d . . . . . C56 C 1.35841(12) 0.19978(18) -0.20235(10) 0.0151(5) Uani 1 1 d . . . . . H56 H 1.3197 0.1609 -0.2235 0.018 Uiso 1 1 calc R . . . . C57 C 1.32910(13) 0.29666(18) -0.18777(11) 0.0207(6) Uani 1 1 d . . . . . H57A H 1.3662 0.3413 -0.1736 0.031 Uiso 1 1 calc GR . . . . H57B H 1.3012 0.2879 -0.1568 0.031 Uiso 1 1 calc GR . . . . H57C H 1.3011 0.3229 -0.2236 0.031 Uiso 1 1 calc GR . . . . C53 C 1.45325(12) 0.04900(18) -0.15388(10) 0.0149(5) Uani 1 1 d . . . . . H53 H 1.4851 0.0866 -0.1744 0.018 Uiso 1 1 calc R . . . . C54 C 1.49550(13) 0.00356(19) -0.09863(11) 0.0207(6) Uani 1 1 d . . . . . H54A H 1.4652 -0.0219 -0.0729 0.031 Uiso 1 1 calc GR . . . . H54B H 1.5253 0.0523 -0.0770 0.031 Uiso 1 1 calc GR . . . . H54C H 1.5230 -0.0488 -0.1107 0.031 Uiso 1 1 calc GR . . . . C40 C 1.33216(13) -0.0121(2) 0.12705(11) 0.0220(6) Uani 1 1 d . . . . . H40 H 1.3430 0.0418 0.1524 0.026 Uiso 1 1 calc R . . . . C39 C 1.32988(14) -0.1029(2) 0.15126(12) 0.0265(7) Uani 1 1 d . . . . . H39 H 1.3387 -0.1109 0.1932 0.032 Uiso 1 1 calc R . . . . C38 C 1.31483(14) -0.1818(2) 0.11484(12) 0.0252(6) Uani 1 1 d . . . . . H38 H 1.3138 -0.2442 0.1315 0.030 Uiso 1 1 calc R . . . . C37 C 1.30116(13) -0.1693(2) 0.05372(12) 0.0219(6) Uani 1 1 d . . . . . H37 H 1.2909 -0.2237 0.0287 0.026 Uiso 1 1 calc R . . . . C47 C 1.29669(13) -0.16572(18) -0.08697(11) 0.0182(6) Uani 1 1 d . . . . . H47 H 1.2729 -0.2183 -0.0689 0.022 Uiso 1 1 calc R . . . . C48 C 1.37218(13) -0.18999(19) -0.07560(12) 0.0226(6) Uani 1 1 d . . . . . H48A H 1.3889 -0.1909 -0.0327 0.034 Uiso 1 1 calc GR . . . . H48B H 1.3970 -0.1414 -0.0944 0.034 Uiso 1 1 calc GR . . . . H48C H 1.3791 -0.2533 -0.0924 0.034 Uiso 1 1 calc GR . . . . C3 C 1.20522(11) 0.10472(18) -0.18125(10) 0.0125(5) Uani 1 1 d . . . . . H3 H 1.2242 0.0443 -0.1887 0.015 Uiso 1 1 calc R . . . . C2 C 1.15968(11) 0.14603(17) -0.22541(10) 0.0117(5) Uani 1 1 d . . . . . C1 C 1.12917(12) 0.23597(18) -0.21608(10) 0.0125(5) Uani 1 1 d . . . . . H1 H 1.1248 0.2839 -0.2491 0.015 Uiso 1 1 calc R . . . . C6 C 1.13785(12) 0.09785(17) -0.28360(10) 0.0118(5) Uani 1 1 d . . . . . C11 C 1.18581(13) 0.07188(18) -0.31806(10) 0.0154(5) Uani 1 1 d . . . . . H11 H 1.2325 0.0835 -0.3036 0.018 Uiso 1 1 calc R . . . . C10 C 1.16661(13) 0.02917(18) -0.37345(11) 0.0175(5) Uani 1 1 d . . . . . H10 H 1.1998 0.0130 -0.3971 0.021 Uiso 1 1 calc R . . . . C9 C 1.09878(13) 0.01046(18) -0.39375(10) 0.0169(5) Uani 1 1 d . . . . . H9 H 1.0854 -0.0200 -0.4311 0.020 Uiso 1 1 calc R . . . . C8 C 1.05042(13) 0.03570(17) -0.36006(10) 0.0157(5) Uani 1 1 d . . . . . H8 H 1.0040 0.0226 -0.3748 0.019 Uiso 1 1 calc R . . . . C7 C 1.06835(12) 0.08024(17) -0.30464(10) 0.0133(5) Uani 1 1 d . . . . . C18 C 0.93245(12) 0.15336(19) -0.31513(11) 0.0172(5) Uani 1 1 d . . . . . H18 H 0.9252 0.1050 -0.3480 0.021 Uiso 1 1 calc R . . . . C20 C 0.86784(13) 0.1602(2) -0.28843(12) 0.0237(6) Uani 1 1 d . . . . . H20A H 0.8318 0.1896 -0.3173 0.036 Uiso 1 1 calc GR . . . . H20B H 0.8763 0.1996 -0.2524 0.036 Uiso 1 1 calc GR . . . . H20C H 0.8538 0.0956 -0.2784 0.036 Uiso 1 1 calc GR . . . . C19 C 0.95071(13) 0.2497(2) -0.34074(12) 0.0237(6) Uani 1 1 d . . . . . H19A H 0.9576 0.2980 -0.3091 0.035 Uiso 1 1 calc GR . . . . H19B H 0.9137 0.2701 -0.3721 0.035 Uiso 1 1 calc GR . . . . H19C H 0.9925 0.2425 -0.3574 0.035 Uiso 1 1 calc GR . . . . C21 C 0.97762(13) -0.00271(19) -0.23062(11) 0.0181(5) Uani 1 1 d . . . . . H21 H 0.9401 0.0121 -0.2082 0.022 Uiso 1 1 calc R . . . . C23 C 0.95002(14) -0.07767(19) -0.27717(12) 0.0232(6) Uani 1 1 d . . . . . H23A H 0.9347 -0.1341 -0.2575 0.035 Uiso 1 1 calc GR . . . . H23B H 0.9859 -0.0967 -0.2992 0.035 Uiso 1 1 calc GR . . . . H23C H 0.9118 -0.0505 -0.3047 0.035 Uiso 1 1 calc GR . . . . C22 C 1.03610(14) -0.0431(2) -0.18530(12) 0.0252(6) Uani 1 1 d . . . . . H22A H 1.0739 -0.0601 -0.2055 0.038 Uiso 1 1 calc GR . . . . H22B H 1.0207 -0.1004 -0.1665 0.038 Uiso 1 1 calc GR . . . . H22C H 1.0511 0.0055 -0.1548 0.038 Uiso 1 1 calc GR . . . . C12 C 1.12279(12) 0.37391(18) -0.14165(10) 0.0132(5) Uani 1 1 d . . . . . C13 C 1.06235(12) 0.39336(19) -0.12005(10) 0.0170(5) Uani 1 1 d . . . . . C24 C 0.92109(13) 0.3433(2) -0.12935(11) 0.0209(6) Uani 1 1 d . . . . . H24 H 0.9203 0.3918 -0.0972 0.025 Uiso 1 1 calc R . . . . C26 C 0.86671(13) 0.2675(2) -0.12445(13) 0.0266(6) Uani 1 1 d . . . . . H26A H 0.8727 0.2126 -0.1499 0.040 Uiso 1 1 calc GR . . . . H26B H 0.8216 0.2955 -0.1372 0.040 Uiso 1 1 calc GR . . . . H26C H 0.8710 0.2461 -0.0831 0.040 Uiso 1 1 calc GR . . . . C25 C 0.90600(14) 0.3952(2) -0.18907(12) 0.0274(6) Uani 1 1 d . . . . . H25A H 0.8620 0.4275 -0.1928 0.041 Uiso 1 1 calc GR . . . . H25B H 0.9049 0.3485 -0.2214 0.041 Uiso 1 1 calc GR . . . . H25C H 0.9415 0.4429 -0.1914 0.041 Uiso 1 1 calc GR . . . . C27 C 1.02482(14) 0.2470(2) -0.04028(11) 0.0249(6) Uani 1 1 d . . . . . H27 H 1.0752 0.2407 -0.0297 0.030 Uiso 1 1 calc R . . . . C28 C 0.99573(15) 0.1459(2) -0.03497(13) 0.0343(7) Uani 1 1 d . . . . . H28A H 0.9461 0.1494 -0.0403 0.051 Uiso 1 1 calc GR . . . . H28B H 1.0134 0.1195 0.0044 0.051 Uiso 1 1 calc GR . . . . H28C H 1.0090 0.1042 -0.0656 0.051 Uiso 1 1 calc GR . . . . C29 C 1.00326(16) 0.3172(2) 0.00465(12) 0.0383(8) Uani 1 1 d . . . . . H29A H 1.0163 0.2914 0.0449 0.057 Uiso 1 1 calc GR . . . . H29B H 0.9540 0.3261 -0.0040 0.057 Uiso 1 1 calc GR . . . . H29C H 1.0257 0.3792 0.0018 0.057 Uiso 1 1 calc GR . . . . C14 C 1.04719(13) 0.4878(2) -0.10606(11) 0.0219(6) Uani 1 1 d . . . . . H14 H 1.0069 0.5011 -0.0907 0.026 Uiso 1 1 calc R . . . . C15 C 1.09047(14) 0.5616(2) -0.11439(11) 0.0220(6) Uani 1 1 d . . . . . H15 H 1.0799 0.6256 -0.1048 0.026 Uiso 1 1 calc R . . . . C16 C 1.14940(13) 0.54284(19) -0.13673(11) 0.0182(6) Uani 1 1 d . . . . . H16 H 1.1787 0.5941 -0.1430 0.022 Uiso 1 1 calc R . . . . C17 C 1.16559(13) 0.44970(18) -0.14990(10) 0.0163(5) Uani 1 1 d . . . . . H17 H 1.2063 0.4373 -0.1647 0.020 Uiso 1 1 calc R . . . . C63 C 1.21538(16) 1.1804(3) 0.22741(14) 0.0456(9) Uani 1 1 d . . . . . H63 H 1.2444 1.1982 0.2631 0.055 Uiso 1 1 calc R . . . . C62 C 1.20637(18) 1.0858(3) 0.21357(17) 0.0518(10) Uani 1 1 d . . . . . H62 H 1.2289 1.0379 0.2393 0.062 Uiso 1 1 calc R . . . . C61 C 1.1642(2) 1.0604(3) 0.1618(2) 0.0650(13) Uani 1 1 d . . . . . H61 H 1.1580 0.9948 0.1508 0.078 Uiso 1 1 calc R . . . . C60 C 1.13063(19) 1.1324(5) 0.12579(17) 0.0721(16) Uani 1 1 d . . . . . H60 H 1.1001 1.1159 0.0907 0.086 Uiso 1 1 calc R . . . . C64 C 1.18360(18) 1.2502(3) 0.19115(16) 0.0478(9) Uani 1 1 d . . . . . H64 H 1.1911 1.3159 0.2014 0.057 Uiso 1 1 calc R . . . . C65 C 1.14153(19) 1.2262(4) 0.14083(17) 0.0646(13) Uani 1 1 d . . . . . H65 H 1.1194 1.2751 0.1157 0.078 Uiso 1 1 calc R . . . . C59 C 1.22246(15) 0.5366(2) 0.02157(12) 0.0274(7) 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 Ni1 0.01185(15) 0.01564(18) 0.01169(15) -0.00248(13) 0.00060(12) 0.00067(13) Ni2 0.01092(15) 0.01077(17) 0.01066(14) 0.00013(12) -0.00204(11) 0.00066(13) N1 0.0117(10) 0.0130(11) 0.0117(9) -0.0011(8) -0.0008(8) -0.0002(9) S1 0.0309(4) 0.0192(4) 0.0183(3) -0.0047(3) -0.0056(3) 0.0062(3) P3 0.0134(3) 0.0120(3) 0.0149(3) 0.0009(3) -0.0013(2) -0.0006(3) P4 0.0119(3) 0.0112(3) 0.0104(3) -0.0008(2) -0.0017(2) 0.0008(3) P1 0.0113(3) 0.0160(4) 0.0132(3) -0.0022(3) -0.0010(2) 0.0006(3) P2 0.0145(3) 0.0210(4) 0.0152(3) -0.0024(3) 0.0038(2) 0.0016(3) C58 0.0244(14) 0.0208(15) 0.0143(12) 0.0003(11) 0.0017(10) 0.0003(12) C55 0.0256(14) 0.0160(14) 0.0185(13) -0.0036(11) -0.0001(11) 0.0019(12) C49 0.0243(14) 0.0178(15) 0.0243(14) -0.0046(12) 0.0001(11) 0.0006(12) F2 0.0488(12) 0.0941(17) 0.0295(10) -0.0145(11) -0.0091(9) 0.0482(12) F1 0.0375(10) 0.0286(10) 0.0190(8) -0.0075(7) -0.0015(7) 0.0061(8) F3 0.1042(18) 0.0238(11) 0.0352(10) 0.0088(9) -0.0071(11) -0.0038(11) C4 0.0145(12) 0.0172(14) 0.0099(11) -0.0025(10) 0.0022(9) -0.0019(11) N2 0.0181(11) 0.0179(12) 0.0204(11) -0.0049(9) 0.0034(9) 0.0043(9) C33 0.0250(14) 0.0139(14) 0.0152(12) 0.0003(11) 0.0023(10) 0.0031(11) O2 0.0234(11) 0.0310(12) 0.0389(12) -0.0043(10) -0.0017(9) -0.0004(9) O1 0.0362(12) 0.0252(11) 0.0239(10) 0.0015(9) 0.0072(9) 0.0026(9) O3 0.0627(16) 0.0293(12) 0.0270(11) -0.0151(10) -0.0125(10) 0.0164(11) C5 0.0103(11) 0.0143(13) 0.0137(11) -0.0018(10) 0.0015(9) -0.0005(10) C50 0.0123(12) 0.0223(15) 0.0180(12) 0.0020(11) -0.0006(10) -0.0029(11) C52 0.0189(14) 0.0281(17) 0.0274(14) 0.0019(13) 0.0034(11) -0.0072(12) C51 0.0142(13) 0.0263(16) 0.0315(15) 0.0011(13) 0.0038(11) 0.0017(12) C36 0.0132(12) 0.0155(14) 0.0161(12) 0.0022(10) 0.0004(10) 0.0014(10) C35 0.0121(12) 0.0199(14) 0.0177(12) 0.0014(11) 0.0029(10) -0.0005(11) C31 0.0130(12) 0.0198(14) 0.0151(12) -0.0016(11) -0.0019(9) -0.0013(11) C32 0.0157(13) 0.0209(15) 0.0205(13) -0.0030(11) 0.0042(10) -0.0025(11) C34 0.0173(12) 0.0140(14) 0.0115(11) -0.0007(10) -0.0005(10) 0.0015(10) C30 0.0118(11) 0.0145(13) 0.0105(11) -0.0007(10) -0.0031(9) 0.0021(10) C41 0.0180(12) 0.0084(12) 0.0129(11) 0.0036(10) -0.0026(10) 0.0023(10) C46 0.0282(14) 0.0128(13) 0.0137(12) -0.0013(10) -0.0022(11) 0.0033(11) C45 0.0228(14) 0.0138(14) 0.0193(13) 0.0017(11) -0.0079(11) -0.0031(11) C44 0.0156(12) 0.0146(14) 0.0200(13) 0.0050(11) -0.0030(10) -0.0027(11) C43 0.0184(13) 0.0146(13) 0.0132(11) 0.0020(10) 0.0021(10) 0.0025(11) C42 0.0147(12) 0.0108(13) 0.0117(11) 0.0011(10) -0.0033(9) 0.0014(10) C56 0.0161(12) 0.0154(13) 0.0121(11) 0.0004(10) -0.0026(9) -0.0004(11) C57 0.0233(14) 0.0175(15) 0.0206(13) 0.0039(11) 0.0015(11) 0.0023(12) C53 0.0141(12) 0.0138(13) 0.0159(12) 0.0002(10) 0.0006(10) 0.0004(10) C54 0.0189(13) 0.0175(15) 0.0231(13) -0.0021(11) -0.0042(11) 0.0035(11) C40 0.0210(14) 0.0266(16) 0.0189(13) -0.0009(12) 0.0045(11) -0.0015(12) C39 0.0256(15) 0.0360(18) 0.0177(13) 0.0087(13) 0.0027(11) -0.0016(13) C38 0.0224(14) 0.0257(16) 0.0277(15) 0.0112(13) 0.0053(12) 0.0020(12) C37 0.0212(14) 0.0186(15) 0.0260(14) 0.0046(12) 0.0045(11) 0.0016(12) C47 0.0202(13) 0.0122(13) 0.0216(13) 0.0001(11) 0.0023(11) -0.0013(11) C48 0.0208(14) 0.0189(15) 0.0266(14) 0.0048(12) -0.0004(11) 0.0052(12) C3 0.0116(11) 0.0133(13) 0.0123(11) -0.0011(10) 0.0009(9) 0.0008(10) C2 0.0094(11) 0.0139(13) 0.0115(11) 0.0000(10) 0.0015(9) -0.0024(10) C1 0.0123(11) 0.0128(13) 0.0121(11) 0.0001(10) 0.0014(9) -0.0006(10) C6 0.0162(12) 0.0081(12) 0.0105(11) 0.0022(9) 0.0006(9) 0.0009(10) C11 0.0167(12) 0.0131(13) 0.0154(12) 0.0019(10) 0.0003(10) 0.0012(10) C10 0.0233(14) 0.0161(14) 0.0144(12) 0.0000(10) 0.0067(10) 0.0021(11) C9 0.0276(14) 0.0117(13) 0.0103(11) -0.0010(10) 0.0003(10) 0.0010(11) C8 0.0186(13) 0.0119(13) 0.0147(12) 0.0018(10) -0.0028(10) -0.0001(11) C7 0.0151(12) 0.0124(13) 0.0117(11) 0.0016(10) 0.0007(9) 0.0013(10) C18 0.0150(12) 0.0174(14) 0.0170(12) -0.0026(11) -0.0034(10) 0.0008(11) C20 0.0168(13) 0.0263(16) 0.0264(14) -0.0045(12) -0.0009(11) 0.0016(12) C19 0.0220(14) 0.0244(16) 0.0224(14) 0.0025(12) -0.0024(11) 0.0022(12) C21 0.0162(12) 0.0192(15) 0.0191(12) -0.0001(11) 0.0039(10) -0.0017(11) C23 0.0235(14) 0.0190(15) 0.0264(14) -0.0016(12) 0.0025(11) -0.0018(12) C22 0.0273(15) 0.0243(16) 0.0218(14) 0.0030(12) -0.0016(12) 0.0010(13) C12 0.0138(12) 0.0159(14) 0.0083(11) -0.0014(10) -0.0028(9) 0.0023(10) C13 0.0165(12) 0.0198(15) 0.0142(12) -0.0027(11) 0.0007(10) 0.0018(11) C24 0.0175(13) 0.0239(16) 0.0217(13) -0.0049(12) 0.0046(11) 0.0037(12) C26 0.0188(14) 0.0316(17) 0.0297(15) 0.0001(13) 0.0051(12) 0.0029(12) C25 0.0242(14) 0.0279(17) 0.0278(15) -0.0004(13) -0.0016(12) 0.0026(13) C27 0.0236(14) 0.0359(18) 0.0161(13) 0.0037(12) 0.0056(11) 0.0101(13) C28 0.0329(17) 0.042(2) 0.0309(16) 0.0135(15) 0.0147(13) 0.0129(15) C29 0.0397(18) 0.058(2) 0.0172(14) -0.0029(14) 0.0062(13) 0.0154(17) C14 0.0190(13) 0.0243(16) 0.0226(13) -0.0065(12) 0.0042(11) 0.0047(12) C15 0.0271(15) 0.0150(14) 0.0225(13) -0.0052(11) 0.0003(11) 0.0048(12) C16 0.0220(13) 0.0153(14) 0.0161(12) -0.0018(11) -0.0002(10) 0.0002(11) C17 0.0181(13) 0.0179(14) 0.0129(12) -0.0018(10) 0.0024(10) 0.0010(11) C63 0.0308(18) 0.076(3) 0.0288(17) 0.0044(18) 0.0019(14) -0.0151(18) C62 0.039(2) 0.065(3) 0.058(2) 0.016(2) 0.0265(19) -0.0030(19) C61 0.058(3) 0.078(3) 0.072(3) -0.028(3) 0.048(2) -0.035(2) C60 0.029(2) 0.154(5) 0.035(2) -0.028(3) 0.0105(16) -0.025(3) C64 0.040(2) 0.062(3) 0.045(2) -0.0006(19) 0.0177(17) -0.0025(18) C65 0.039(2) 0.119(4) 0.037(2) 0.013(2) 0.0116(18) 0.017(2) C59 0.0370(17) 0.0206(16) 0.0233(14) -0.0075(12) 0.0015(13) 0.0120(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 Ni1 P1 2.1739(7) . ? Ni1 P2 2.1755(7) . ? Ni1 C5 2.073(2) . ? Ni1 C1 1.930(2) . ? Ni2 N1 2.0597(19) . ? Ni2 P3 2.2737(8) . ? Ni2 P4 2.2854(7) . ? Ni2 C34 2.406(2) . ? Ni2 C30 1.968(2) . ? N1 C4 1.324(3) . ? N1 C3 1.385(3) . ? S1 O2 1.437(2) . ? S1 O1 1.443(2) . ? S1 O3 1.433(2) . ? S1 C59 1.804(3) . ? P3 C50 1.869(2) . ? P3 C36 1.838(2) . ? P3 C47 1.854(3) . ? P4 C42 1.828(2) . ? P4 C56 1.868(2) . ? P4 C53 1.852(2) . ? P1 C7 1.848(2) . ? P1 C18 1.849(2) . ? P1 C21 1.850(3) . ? P2 C13 1.833(3) . ? P2 C24 1.857(3) . ? P2 C27 1.859(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C58 C56 1.533(3) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C55 C53 1.528(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C49 C47 1.536(3) . ? F2 C59 1.329(3) . ? F1 C59 1.333(3) . ? F3 C59 1.343(3) . ? C4 H4 0.9500 . ? C4 C5 1.437(3) . ? N2 H2 0.8800 . ? N2 C33 1.349(3) . ? N2 C32 1.354(3) . ? C33 H33 0.9500 . ? C33 C34 1.377(3) . ? C5 C1 1.448(3) . ? C5 C12 1.500(3) . ? C50 H50 1.0000 . ? C50 C52 1.529(4) . ? C50 C51 1.526(4) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C36 C35 1.392(3) . ? C36 C37 1.398(4) . ? C35 C31 1.483(4) . ? C35 C40 1.398(3) . ? C31 C32 1.366(4) . ? C31 C30 1.454(3) . ? C32 H32 0.9500 . ? C34 C30 1.446(3) . ? C34 C41 1.487(3) . ? C30 H30 1.0000 . ? C41 C46 1.396(3) . ? C41 C42 1.400(3) . ? C46 H46 0.9500 . ? C46 C45 1.385(4) . ? C45 H45 0.9500 . ? C45 C44 1.380(4) . ? C44 H44 0.9500 . ? C44 C43 1.385(3) . ? C43 H43 0.9500 . ? C43 C42 1.395(3) . ? C56 H56 1.0000 . ? C56 C57 1.530(3) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C53 H53 1.0000 . ? C53 C54 1.531(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C40 H40 0.9500 . ? C40 C39 1.384(4) . ? C39 H39 0.9500 . ? C39 C38 1.380(4) . ? C38 H38 0.9500 . ? C38 C37 1.387(4) . ? C37 H37 0.9500 . ? C47 H47 1.0000 . ? C47 C48 1.526(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C3 H3 0.9500 . ? C3 C2 1.366(3) . ? C2 C1 1.425(3) . ? C2 C6 1.486(3) . ? C1 H1 1.0000 . ? C6 C11 1.388(3) . ? C6 C7 1.413(3) . ? C11 H11 0.9500 . ? C11 C10 1.391(3) . ? C10 H10 0.9500 . ? C10 C9 1.382(4) . ? C9 H9 0.9500 . ? C9 C8 1.380(3) . ? C8 H8 0.9500 . ? C8 C7 1.400(3) . ? C18 H18 1.0000 . ? C18 C20 1.523(4) . ? C18 C19 1.532(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21 1.0000 . ? C21 C23 1.525(4) . ? C21 C22 1.531(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C12 C13 1.407(3) . ? C12 C17 1.392(3) . ? C13 C14 1.398(4) . ? C24 H24 1.0000 . ? C24 C26 1.533(4) . ? C24 C25 1.528(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 H27 1.0000 . ? C27 C28 1.535(4) . ? C27 C29 1.532(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C14 H14 0.9500 . ? C14 C15 1.378(4) . ? C15 H15 0.9500 . ? C15 C16 1.386(4) . ? C16 H16 0.9500 . ? C16 C17 1.382(3) . ? C17 H17 0.9500 . ? C63 H63 0.9500 . ? C63 C62 1.360(5) . ? C63 C64 1.362(5) . ? C62 H62 0.9500 . ? C62 C61 1.377(6) . ? C61 H61 0.9500 . ? C61 C60 1.395(6) . ? C60 H60 0.9500 . ? C60 C65 1.358(6) . ? C64 H64 0.9500 . ? C64 C65 1.346(5) . ? C65 H65 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 P1 Ni1 P2 134.59(3) . . ? C5 Ni1 P1 137.00(7) . . ? C5 Ni1 P2 87.39(7) . . ? C1 Ni1 P1 95.53(7) . . ? C1 Ni1 P2 125.19(7) . . ? C1 Ni1 C5 42.21(9) . . ? N1 Ni2 P3 99.96(6) . . ? N1 Ni2 P4 101.07(6) . . ? N1 Ni2 C34 112.68(8) . . ? P3 Ni2 P4 128.06(3) . . ? P3 Ni2 C34 132.10(6) . . ? P4 Ni2 C34 79.88(6) . . ? C30 Ni2 N1 140.78(9) . . ? C30 Ni2 P3 96.49(7) . . ? C30 Ni2 P4 96.18(7) . . ? C30 Ni2 C34 36.91(9) . . ? C4 N1 Ni2 124.95(16) . . ? C4 N1 C3 116.6(2) . . ? C3 N1 Ni2 117.70(15) . . ? O2 S1 O1 114.63(12) . . ? O2 S1 C59 102.37(13) . . ? O1 S1 C59 100.89(13) . . ? O3 S1 O2 115.49(14) . . ? O3 S1 O1 115.51(13) . . ? O3 S1 C59 105.22(12) . . ? C50 P3 Ni2 111.75(9) . . ? C36 P3 Ni2 111.34(8) . . ? C36 P3 C50 101.74(11) . . ? C36 P3 C47 102.72(11) . . ? C47 P3 Ni2 125.49(9) . . ? C47 P3 C50 100.89(12) . . ? C42 P4 Ni2 108.14(8) . . ? C42 P4 C56 103.01(11) . . ? C42 P4 C53 99.39(11) . . ? C56 P4 Ni2 115.55(8) . . ? C53 P4 Ni2 124.40(8) . . ? C53 P4 C56 103.35(11) . . ? C7 P1 Ni1 111.21(8) . . ? C7 P1 C18 102.08(11) . . ? C7 P1 C21 104.29(11) . . ? C18 P1 Ni1 121.92(9) . . ? C21 P1 Ni1 110.25(8) . . ? C21 P1 C18 105.49(11) . . ? C13 P2 Ni1 96.62(8) . . ? C13 P2 C24 102.77(12) . . ? C13 P2 C27 104.33(12) . . ? C24 P2 Ni1 125.40(9) . . ? C24 P2 C27 105.99(12) . . ? C27 P2 Ni1 117.77(9) . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? N1 C4 H4 117.2 . . ? N1 C4 C5 125.7(2) . . ? C5 C4 H4 117.2 . . ? C33 N2 H2 119.7 . . ? C33 N2 C32 120.6(2) . . ? C32 N2 H2 119.7 . . ? N2 C33 H33 118.9 . . ? N2 C33 C34 122.1(2) . . ? C34 C33 H33 118.9 . . ? C4 C5 Ni1 119.54(17) . . ? C4 C5 C1 115.7(2) . . ? C4 C5 C12 117.5(2) . . ? C1 C5 Ni1 63.60(13) . . ? C1 C5 C12 122.3(2) . . ? C12 C5 Ni1 105.82(15) . . ? P3 C50 H50 106.5 . . ? C52 C50 P3 116.86(18) . . ? C52 C50 H50 106.5 . . ? C51 C50 P3 110.24(17) . . ? C51 C50 H50 106.5 . . ? C51 C50 C52 109.6(2) . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C35 C36 P3 116.25(18) . . ? C35 C36 C37 118.7(2) . . ? C37 C36 P3 124.87(19) . . ? C36 C35 C31 120.7(2) . . ? C36 C35 C40 119.9(2) . . ? C40 C35 C31 119.4(2) . . ? C32 C31 C35 118.9(2) . . ? C32 C31 C30 120.9(2) . . ? C30 C31 C35 119.8(2) . . ? N2 C32 C31 121.4(2) . . ? N2 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C33 C34 Ni2 112.20(17) . . ? C33 C34 C30 120.0(2) . . ? C33 C34 C41 118.0(2) . . ? C30 C34 Ni2 54.81(12) . . ? C30 C34 C41 120.0(2) . . ? C41 C34 Ni2 113.64(15) . . ? Ni2 C30 H30 117.0 . . ? C31 C30 Ni2 97.31(15) . . ? C31 C30 H30 117.0 . . ? C34 C30 Ni2 88.28(14) . . ? C34 C30 C31 115.0(2) . . ? C34 C30 H30 117.0 . . ? C46 C41 C34 119.2(2) . . ? C46 C41 C42 119.1(2) . . ? C42 C41 C34 121.6(2) . . ? C41 C46 H46 119.6 . . ? C45 C46 C41 120.8(2) . . ? C45 C46 H46 119.6 . . ? C46 C45 H45 119.9 . . ? C44 C45 C46 120.1(2) . . ? C44 C45 H45 119.9 . . ? C45 C44 H44 120.2 . . ? C45 C44 C43 119.6(2) . . ? C43 C44 H44 120.2 . . ? C44 C43 H43 119.5 . . ? C44 C43 C42 121.1(2) . . ? C42 C43 H43 119.5 . . ? C41 C42 P4 116.26(18) . . ? C43 C42 P4 124.57(18) . . ? C43 C42 C41 119.2(2) . . ? P4 C56 H56 106.7 . . ? C58 C56 P4 117.25(17) . . ? C58 C56 H56 106.7 . . ? C57 C56 P4 109.27(16) . . ? C57 C56 C58 109.5(2) . . ? C57 C56 H56 106.7 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? P4 C53 H53 107.3 . . ? C55 C53 P4 112.23(17) . . ? C55 C53 H53 107.3 . . ? C55 C53 C54 112.5(2) . . ? C54 C53 P4 110.03(17) . . ? C54 C53 H53 107.3 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C35 C40 H40 119.9 . . ? C39 C40 C35 120.3(3) . . ? C39 C40 H40 119.9 . . ? C40 C39 H39 119.8 . . ? C38 C39 C40 120.4(2) . . ? C38 C39 H39 119.8 . . ? C39 C38 H38 120.3 . . ? C39 C38 C37 119.4(3) . . ? C37 C38 H38 120.3 . . ? C36 C37 H37 119.4 . . ? C38 C37 C36 121.2(3) . . ? C38 C37 H37 119.4 . . ? P3 C47 H47 107.1 . . ? C49 C47 P3 110.45(18) . . ? C49 C47 H47 107.1 . . ? C48 C47 P3 113.06(18) . . ? C48 C47 C49 111.6(2) . . ? C48 C47 H47 107.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N1 C3 H3 118.5 . . ? C2 C3 N1 123.1(2) . . ? C2 C3 H3 118.5 . . ? C3 C2 C1 120.6(2) . . ? C3 C2 C6 121.8(2) . . ? C1 C2 C6 117.5(2) . . ? Ni1 C1 H1 117.3 . . ? C5 C1 Ni1 74.20(14) . . ? C5 C1 H1 117.3 . . ? C2 C1 Ni1 105.42(16) . . ? C2 C1 C5 117.0(2) . . ? C2 C1 H1 117.3 . . ? C11 C6 C2 119.9(2) . . ? C11 C6 C7 119.8(2) . . ? C7 C6 C2 120.3(2) . . ? C6 C11 H11 119.5 . . ? C6 C11 C10 121.1(2) . . ? C10 C11 H11 119.5 . . ? C11 C10 H10 120.4 . . ? C9 C10 C11 119.3(2) . . ? C9 C10 H10 120.4 . . ? C10 C9 H9 119.8 . . ? C8 C9 C10 120.4(2) . . ? C8 C9 H9 119.8 . . ? C9 C8 H8 119.3 . . ? C9 C8 C7 121.4(2) . . ? C7 C8 H8 119.3 . . ? C6 C7 P1 119.95(17) . . ? C8 C7 P1 121.98(18) . . ? C8 C7 C6 118.1(2) . . ? P1 C18 H18 108.5 . . ? C20 C18 P1 110.60(17) . . ? C20 C18 H18 108.5 . . ? C20 C18 C19 111.8(2) . . ? C19 C18 P1 108.81(17) . . ? C19 C18 H18 108.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P1 C21 H21 106.5 . . ? C23 C21 P1 116.73(18) . . ? C23 C21 H21 106.5 . . ? C23 C21 C22 111.4(2) . . ? C22 C21 P1 108.71(18) . . ? C22 C21 H21 106.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C12 C5 120.0(2) . . ? C17 C12 C5 120.9(2) . . ? C17 C12 C13 119.1(2) . . ? C12 C13 P2 114.20(19) . . ? C14 C13 P2 126.1(2) . . ? C14 C13 C12 119.6(2) . . ? P2 C24 H24 108.1 . . ? C26 C24 P2 111.22(19) . . ? C26 C24 H24 108.1 . . ? C25 C24 P2 110.40(18) . . ? C25 C24 H24 108.1 . . ? C25 C24 C26 110.8(2) . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P2 C27 H27 106.3 . . ? C28 C27 P2 110.48(19) . . ? C28 C27 H27 106.3 . . ? C29 C27 P2 114.6(2) . . ? C29 C27 H27 106.3 . . ? C29 C27 C28 112.3(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.3(2) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16 119.9 . . ? C12 C17 H17 119.7 . . ? C16 C17 C12 120.6(2) . . ? C16 C17 H17 119.7 . . ? C62 C63 H63 119.3 . . ? C62 C63 C64 121.3(3) . . ? C64 C63 H63 119.3 . . ? C63 C62 H62 120.4 . . ? C63 C62 C61 119.1(4) . . ? C61 C62 H62 120.4 . . ? C62 C61 H61 120.5 . . ? C62 C61 C60 119.0(4) . . ? C60 C61 H61 120.5 . . ? C61 C60 H60 119.9 . . ? C65 C60 C61 120.1(4) . . ? C65 C60 H60 119.9 . . ? C63 C64 H64 120.0 . . ? C65 C64 C63 120.1(4) . . ? C65 C64 H64 120.0 . . ? C60 C65 H65 119.8 . . ? C64 C65 C60 120.3(4) . . ? C64 C65 H65 119.8 . . ? F2 C59 S1 112.7(2) . . ? F2 C59 F1 107.4(2) . . ? F2 C59 F3 106.6(2) . . ? F1 C59 S1 110.74(19) . . ? F1 C59 F3 106.1(2) . . ? F3 C59 S1 112.9(2) . . ? 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 Ni1 P1 C7 C6 12.4(2) . . . . ? Ni1 P1 C7 C8 -168.97(18) . . . . ? Ni1 P1 C18 C20 -69.7(2) . . . . ? Ni1 P1 C18 C19 53.5(2) . . . . ? Ni1 P1 C21 C23 -176.14(17) . . . . ? Ni1 P1 C21 C22 -49.17(19) . . . . ? Ni1 P2 C13 C12 -21.77(18) . . . . ? Ni1 P2 C13 C14 153.3(2) . . . . ? Ni1 P2 C24 C26 76.9(2) . . . . ? Ni1 P2 C24 C25 -46.6(2) . . . . ? Ni1 P2 C27 C28 -60.5(2) . . . . ? Ni1 P2 C27 C29 171.50(19) . . . . ? Ni1 C5 C1 C2 -99.6(2) . . . . ? Ni1 C5 C12 C13 32.1(2) . . . . ? Ni1 C5 C12 C17 -147.45(18) . . . . ? Ni2 N1 C4 C5 165.29(18) . . . . ? Ni2 N1 C3 C2 -162.67(18) . . . . ? Ni2 P3 C50 C52 172.86(16) . . . . ? Ni2 P3 C50 C51 -61.11(19) . . . . ? Ni2 P3 C36 C35 19.2(2) . . . . ? Ni2 P3 C36 C37 -165.52(19) . . . . ? Ni2 P3 C47 C49 -61.5(2) . . . . ? Ni2 P3 C47 C48 64.4(2) . . . . ? Ni2 P4 C42 C41 -7.9(2) . . . . ? Ni2 P4 C42 C43 172.67(19) . . . . ? Ni2 P4 C56 C58 -171.87(16) . . . . ? Ni2 P4 C56 C57 62.77(18) . . . . ? Ni2 P4 C53 C55 69.32(19) . . . . ? Ni2 P4 C53 C54 -56.75(19) . . . . ? Ni2 C34 C30 C31 -97.26(19) . . . . ? Ni2 C34 C41 C46 -177.11(17) . . . . ? Ni2 C34 C41 C42 0.0(3) . . . . ? N1 C4 C5 Ni1 67.4(3) . . . . ? N1 C4 C5 C1 -5.4(4) . . . . ? N1 C4 C5 C12 -162.2(2) . . . . ? N1 C3 C2 C1 -0.8(4) . . . . ? N1 C3 C2 C6 -178.2(2) . . . . ? P3 C36 C35 C31 -5.3(3) . . . . ? P3 C36 C35 C40 174.11(19) . . . . ? P3 C36 C37 C38 -173.9(2) . . . . ? P2 C13 C14 C15 -173.6(2) . . . . ? C4 N1 C3 C2 8.2(3) . . . . ? C4 C5 C1 Ni1 111.8(2) . . . . ? C4 C5 C1 C2 12.3(3) . . . . ? C4 C5 C12 C13 -104.4(3) . . . . ? C4 C5 C12 C17 76.1(3) . . . . ? N2 C33 C34 Ni2 62.6(3) . . . . ? N2 C33 C34 C30 1.5(4) . . . . ? N2 C33 C34 C41 -162.3(2) . . . . ? C33 N2 C32 C31 0.2(4) . . . . ? C33 C34 C30 Ni2 97.3(2) . . . . ? C33 C34 C30 C31 0.0(3) . . . . ? C33 C34 C41 C46 48.5(3) . . . . ? C33 C34 C41 C42 -134.5(2) . . . . ? O2 S1 C59 F2 -177.3(2) . . . . ? O2 S1 C59 F1 62.4(2) . . . . ? O2 S1 C59 F3 -56.4(2) . . . . ? O1 S1 C59 F2 64.3(2) . . . . ? O1 S1 C59 F1 -56.1(2) . . . . ? O1 S1 C59 F3 -174.8(2) . . . . ? O3 S1 C59 F2 -56.2(3) . . . . ? O3 S1 C59 F1 -176.5(2) . . . . ? O3 S1 C59 F3 64.7(2) . . . . ? C5 C12 C13 P2 -5.5(3) . . . . ? C5 C12 C13 C14 179.1(2) . . . . ? C5 C12 C17 C16 180.0(2) . . . . ? C50 P3 C36 C35 -99.9(2) . . . . ? C50 P3 C36 C37 75.3(2) . . . . ? C50 P3 C47 C49 65.5(2) . . . . ? C50 P3 C47 C48 -168.72(18) . . . . ? C36 P3 C50 C52 -68.3(2) . . . . ? C36 P3 C50 C51 57.8(2) . . . . ? C36 P3 C47 C49 170.30(18) . . . . ? C36 P3 C47 C48 -63.9(2) . . . . ? C36 C35 C31 C32 123.7(3) . . . . ? C36 C35 C31 C30 -63.6(3) . . . . ? C36 C35 C40 C39 0.5(4) . . . . ? C35 C36 C37 C38 1.2(4) . . . . ? C35 C31 C32 N2 174.0(2) . . . . ? C35 C31 C30 Ni2 94.5(2) . . . . ? C35 C31 C30 C34 -174.0(2) . . . . ? C35 C40 C39 C38 0.6(4) . . . . ? C31 C35 C40 C39 180.0(2) . . . . ? C32 N2 C33 C34 -1.6(4) . . . . ? C32 C31 C30 Ni2 -92.9(2) . . . . ? C32 C31 C30 C34 -1.4(3) . . . . ? C34 C41 C46 C45 177.4(2) . . . . ? C34 C41 C42 P4 5.3(3) . . . . ? C34 C41 C42 C43 -175.2(2) . . . . ? C30 C31 C32 N2 1.4(4) . . . . ? C30 C34 C41 C46 -115.4(3) . . . . ? C30 C34 C41 C42 61.7(3) . . . . ? C41 C34 C30 Ni2 -99.2(2) . . . . ? C41 C34 C30 C31 163.5(2) . . . . ? C41 C46 C45 C44 -1.6(4) . . . . ? C46 C41 C42 P4 -177.65(18) . . . . ? C46 C41 C42 C43 1.9(3) . . . . ? C46 C45 C44 C43 0.7(4) . . . . ? C45 C44 C43 C42 1.5(4) . . . . ? C44 C43 C42 P4 176.68(19) . . . . ? C44 C43 C42 C41 -2.8(4) . . . . ? C42 P4 C56 C58 70.4(2) . . . . ? C42 P4 C56 C57 -54.91(19) . . . . ? C42 P4 C53 C55 -170.97(18) . . . . ? C42 P4 C53 C54 62.96(19) . . . . ? C42 C41 C46 C45 0.3(4) . . . . ? C56 P4 C42 C41 114.93(19) . . . . ? C56 P4 C42 C43 -64.5(2) . . . . ? C56 P4 C53 C55 -65.1(2) . . . . ? C56 P4 C53 C54 168.85(17) . . . . ? C53 P4 C42 C41 -138.91(19) . . . . ? C53 P4 C42 C43 41.6(2) . . . . ? C53 P4 C56 C58 -32.7(2) . . . . ? C53 P4 C56 C57 -158.03(17) . . . . ? C40 C35 C31 C32 -55.7(3) . . . . ? C40 C35 C31 C30 117.0(3) . . . . ? C40 C39 C38 C37 -0.8(4) . . . . ? C39 C38 C37 C36 -0.1(4) . . . . ? C37 C36 C35 C31 179.1(2) . . . . ? C37 C36 C35 C40 -1.4(4) . . . . ? C47 P3 C50 C52 37.4(2) . . . . ? C47 P3 C50 C51 163.38(18) . . . . ? C47 P3 C36 C35 155.90(19) . . . . ? C47 P3 C36 C37 -28.9(2) . . . . ? C3 N1 C4 C5 -4.8(4) . . . . ? C3 C2 C1 Ni1 -89.5(2) . . . . ? C3 C2 C1 C5 -9.7(3) . . . . ? C3 C2 C6 C11 -57.8(3) . . . . ? C3 C2 C6 C7 123.6(3) . . . . ? C2 C6 C11 C10 -178.2(2) . . . . ? C2 C6 C7 P1 -2.1(3) . . . . ? C2 C6 C7 C8 179.2(2) . . . . ? C1 C5 C12 C13 100.5(3) . . . . ? C1 C5 C12 C17 -79.0(3) . . . . ? C1 C2 C6 C11 124.8(2) . . . . ? C1 C2 C6 C7 -53.8(3) . . . . ? C6 C2 C1 Ni1 88.0(2) . . . . ? C6 C2 C1 C5 167.8(2) . . . . ? C6 C11 C10 C9 -1.5(4) . . . . ? C11 C6 C7 P1 179.30(18) . . . . ? C11 C6 C7 C8 0.6(3) . . . . ? C11 C10 C9 C8 1.4(4) . . . . ? C10 C9 C8 C7 -0.3(4) . . . . ? C9 C8 C7 P1 -179.35(19) . . . . ? C9 C8 C7 C6 -0.7(4) . . . . ? C7 P1 C18 C20 165.63(18) . . . . ? C7 P1 C18 C19 -71.15(19) . . . . ? C7 P1 C21 C23 -56.7(2) . . . . ? C7 P1 C21 C22 70.30(19) . . . . ? C7 C6 C11 C10 0.4(4) . . . . ? C18 P1 C7 C6 143.9(2) . . . . ? C18 P1 C7 C8 -37.4(2) . . . . ? C18 P1 C21 C23 50.5(2) . . . . ? C18 P1 C21 C22 177.43(18) . . . . ? C21 P1 C7 C6 -106.4(2) . . . . ? C21 P1 C7 C8 72.2(2) . . . . ? C21 P1 C18 C20 56.9(2) . . . . ? C21 P1 C18 C19 -179.89(17) . . . . ? C12 C5 C1 Ni1 -92.6(2) . . . . ? C12 C5 C1 C2 167.8(2) . . . . ? C12 C13 C14 C15 1.2(4) . . . . ? C13 P2 C24 C26 -175.29(18) . . . . ? C13 P2 C24 C25 61.2(2) . . . . ? C13 P2 C27 C28 -166.13(19) . . . . ? C13 P2 C27 C29 65.9(2) . . . . ? C13 C12 C17 C16 0.4(3) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C24 P2 C13 C12 -150.39(18) . . . . ? C24 P2 C13 C14 24.7(2) . . . . ? C24 P2 C27 C28 85.8(2) . . . . ? C24 P2 C27 C29 -42.2(3) . . . . ? C27 P2 C13 C12 99.15(19) . . . . ? C27 P2 C13 C14 -85.7(2) . . . . ? C27 P2 C24 C26 -66.1(2) . . . . ? C27 P2 C24 C25 170.44(19) . . . . ? C14 C15 C16 C17 -1.0(4) . . . . ? C15 C16 C17 C12 0.8(4) . . . . ? C17 C12 C13 P2 174.02(17) . . . . ? C17 C12 C13 C14 -1.4(3) . . . . ? C63 C62 C61 C60 -1.5(5) . . . . ? C63 C64 C65 C60 -0.2(5) . . . . ? C62 C63 C64 C65 0.9(5) . . . . ? C62 C61 C60 C65 2.2(5) . . . . ? C61 C60 C65 C64 -1.4(6) . . . . ? C64 C63 C62 C61 0.0(5) . . . . ? _shelx_res_file ; TITL a14150_0m in P2(1)/n CELL 0.71073 20.0035 13.924 22.8323 90 99.777 90 ZERR 4 0.0034 0.0022 0.0038 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N Ni O P S UNIT 260 340 12 8 8 12 16 4 L.S. 20 PLAN -5 0 0 SIZE 0.05 0.1 0.58 TEMP -173.14 HTAB BOND $H CONF MORE -1 fmap 2 acta OMIT -1 0 1 OMIT 1 0 1 OMIT 1 1 0 REM REM REM WGHT 0.039700 3.481300 FVAR 0.07073 NI1 5 1.048127 0.204785 -0.184697 11.00000 0.01185 0.01564 = 0.01169 -0.00248 0.00060 0.00067 NI2 5 1.312417 0.096684 -0.074114 11.00000 0.01092 0.01077 = 0.01066 0.00013 -0.00204 0.00066 N1 4 1.225059 0.146747 -0.126060 11.00000 0.01170 0.01302 = 0.01174 -0.00114 -0.00079 -0.00022 S1 8 1.273433 0.503737 0.091643 11.00000 0.03094 0.01921 = 0.01832 -0.00468 -0.00565 0.00622 P3 7 1.277080 -0.051820 -0.051369 11.00000 0.01342 0.01200 = 0.01492 0.00088 -0.00128 -0.00059 P4 7 1.391496 0.135061 -0.131699 11.00000 0.01188 0.01123 = 0.01043 -0.00080 -0.00168 0.00076 P1 7 1.004404 0.113406 -0.258542 11.00000 0.01127 0.01597 = 0.01324 -0.00218 -0.00101 0.00058 P2 7 1.007031 0.288735 -0.118708 11.00000 0.01448 0.02102 = 0.01522 -0.00244 0.00385 0.00163 C58 1 1.407570 0.214750 -0.246275 11.00000 0.02443 0.02083 = 0.01432 0.00032 0.00165 0.00027 AFIX 137 H58A 2 1.445861 0.254311 -0.227645 11.00000 -1.50000 H58B 2 1.383908 0.247180 -0.281948 11.00000 -1.50000 H58C 2 1.424361 0.152328 -0.257304 11.00000 -1.50000 AFIX 0 C55 1 1.419169 -0.025986 -0.197944 11.00000 0.02559 0.01605 = 0.01850 -0.00363 -0.00011 0.00187 AFIX 137 H55A 2 1.389480 -0.066654 -0.178484 11.00000 -1.50000 H55B 2 1.453946 -0.065825 -0.211491 11.00000 -1.50000 H55C 2 1.392218 0.006424 -0.232123 11.00000 -1.50000 AFIX 0 C49 1 1.267750 -0.163972 -0.153744 11.00000 0.02434 0.01783 = 0.02434 -0.00460 0.00011 0.00060 AFIX 137 H49A 2 1.218276 -0.157692 -0.159366 11.00000 -1.50000 H49B 2 1.279664 -0.223786 -0.172118 11.00000 -1.50000 H49C 2 1.286852 -0.109324 -0.172341 11.00000 -1.50000 AFIX 0 F2 3 1.159085 0.558940 0.026595 11.00000 0.04876 0.09413 = 0.02948 -0.01452 -0.00906 0.04824 F1 3 1.219520 0.464566 -0.017278 11.00000 0.03747 0.02858 = 0.01905 -0.00750 -0.00145 0.00613 F3 3 1.247556 0.612200 -0.004062 11.00000 0.10425 0.02377 = 0.03523 0.00883 -0.00713 -0.00377 C4 1 1.191494 0.224618 -0.114659 11.00000 0.01447 0.01717 = 0.00990 -0.00252 0.00221 -0.00187 AFIX 43 H4 2 1.202358 0.250975 -0.075829 11.00000 -1.20000 AFIX 0 N2 4 1.286987 0.261541 0.041458 11.00000 0.01810 0.01793 = 0.02040 -0.00485 0.00335 0.00428 AFIX 43 H2 2 1.261230 0.305743 0.053884 11.00000 -1.20000 AFIX 0 C33 1 1.331038 0.286455 0.005452 11.00000 0.02496 0.01393 = 0.01523 0.00033 0.00227 0.00309 AFIX 43 H33 2 1.332683 0.351479 -0.006822 11.00000 -1.20000 AFIX 0 O2 6 1.338944 0.487823 0.075496 11.00000 0.02344 0.03097 = 0.03892 -0.00426 -0.00167 -0.00043 O1 6 1.239192 0.417701 0.105647 11.00000 0.03617 0.02516 = 0.02391 0.00146 0.00717 0.00264 O3 6 1.269087 0.583944 0.130144 11.00000 0.06266 0.02934 = 0.02697 -0.01506 -0.01250 0.01643 C5 1 1.140073 0.272713 -0.155907 11.00000 0.01031 0.01435 = 0.01370 -0.00176 0.00153 -0.00045 C50 1 1.182541 -0.059054 -0.060732 11.00000 0.01230 0.02226 = 0.01801 0.00205 -0.00059 -0.00292 AFIX 13 H50 2 1.164665 -0.037195 -0.102151 11.00000 -1.20000 AFIX 0 C52 1 1.151923 -0.158264 -0.054072 11.00000 0.01894 0.02809 = 0.02742 0.00190 0.00335 -0.00719 AFIX 137 H52A 2 1.102409 -0.152971 -0.059356 11.00000 -1.50000 H52B 2 1.169298 -0.183702 -0.014384 11.00000 -1.50000 H52C 2 1.164440 -0.201701 -0.084206 11.00000 -1.50000 AFIX 0 C51 1 1.156008 0.011937 -0.019216 11.00000 0.01422 0.02633 = 0.03154 0.00110 0.00384 0.00171 AFIX 137 H51A 2 1.170360 -0.008520 0.022074 11.00000 -1.50000 H51B 2 1.106355 0.013932 -0.028332 11.00000 -1.50000 H51C 2 1.174268 0.075995 -0.024725 11.00000 -1.50000 AFIX 0 C36 1 1.302187 -0.078152 0.028229 11.00000 0.01318 0.01552 = 0.01610 0.00215 0.00042 0.00135 C35 1 1.318607 0.000667 0.065430 11.00000 0.01212 0.01986 = 0.01770 0.00137 0.00294 -0.00050 C31 1 1.321309 0.098609 0.040414 11.00000 0.01300 0.01976 = 0.01513 -0.00161 -0.00186 -0.00127 C32 1 1.282039 0.169119 0.058661 11.00000 0.01565 0.02093 = 0.02050 -0.00305 0.00425 -0.00251 AFIX 43 H32 2 1.250603 0.152980 0.083945 11.00000 -1.20000 AFIX 0 C34 1 1.373712 0.220662 -0.014096 11.00000 0.01729 0.01397 = 0.01152 -0.00073 -0.00049 0.00150 C30 1 1.371028 0.120850 0.002784 11.00000 0.01181 0.01447 = 0.01055 -0.00073 -0.00313 0.00208 AFIX 13 H30 2 1.415068 0.085303 0.010935 11.00000 -1.20000 AFIX 0 C41 1 1.433311 0.257608 -0.038142 11.00000 0.01803 0.00838 = 0.01295 0.00365 -0.00261 0.00234 C46 1 1.474933 0.326691 -0.005995 11.00000 0.02825 0.01282 = 0.01366 -0.00134 -0.00217 0.00333 AFIX 43 H46 2 1.463695 0.351181 0.029936 11.00000 -1.20000 AFIX 0 C45 1 1.532413 0.359962 -0.025851 11.00000 0.02276 0.01377 = 0.01926 0.00169 -0.00789 -0.00306 AFIX 43 H45 2 1.559668 0.408134 -0.004064 11.00000 -1.20000 AFIX 0 C44 1 1.550146 0.323246 -0.077224 11.00000 0.01557 0.01462 = 0.01999 0.00500 -0.00300 -0.00271 AFIX 43 H44 2 1.589812 0.345529 -0.090654 11.00000 -1.20000 AFIX 0 C43 1 1.509789 0.253712 -0.109108 11.00000 0.01844 0.01459 = 0.01316 0.00204 0.00213 0.00249 AFIX 43 H43 2 1.522707 0.227431 -0.143928 11.00000 -1.20000 AFIX 0 C42 1 1.450500 0.221667 -0.090915 11.00000 0.01474 0.01077 = 0.01174 0.00108 -0.00329 0.00144 C56 1 1.358409 0.199778 -0.202353 11.00000 0.01615 0.01544 = 0.01207 0.00044 -0.00257 -0.00035 AFIX 13 H56 2 1.319660 0.160909 -0.223517 11.00000 -1.20000 AFIX 0 C57 1 1.329095 0.296664 -0.187768 11.00000 0.02334 0.01745 = 0.02060 0.00387 0.00154 0.00230 AFIX 137 H57A 2 1.366235 0.341262 -0.173620 11.00000 -1.50000 H57B 2 1.301224 0.287895 -0.156778 11.00000 -1.50000 H57C 2 1.301050 0.322893 -0.223566 11.00000 -1.50000 AFIX 0 C53 1 1.453253 0.048998 -0.153879 11.00000 0.01413 0.01380 = 0.01593 0.00022 0.00061 0.00042 AFIX 13 H53 2 1.485053 0.086572 -0.174434 11.00000 -1.20000 AFIX 0 C54 1 1.495502 0.003561 -0.098630 11.00000 0.01890 0.01747 = 0.02307 -0.00210 -0.00425 0.00353 AFIX 137 H54A 2 1.465213 -0.021923 -0.072857 11.00000 -1.50000 H54B 2 1.525338 0.052271 -0.076978 11.00000 -1.50000 H54C 2 1.523001 -0.048753 -0.110689 11.00000 -1.50000 AFIX 0 C40 1 1.332161 -0.012076 0.127050 11.00000 0.02101 0.02656 = 0.01892 -0.00092 0.00447 -0.00148 AFIX 43 H40 2 1.342977 0.041821 0.152400 11.00000 -1.20000 AFIX 0 C39 1 1.329882 -0.102879 0.151256 11.00000 0.02556 0.03598 = 0.01769 0.00874 0.00268 -0.00157 AFIX 43 H39 2 1.338728 -0.110932 0.193177 11.00000 -1.20000 AFIX 0 C38 1 1.314829 -0.181835 0.114838 11.00000 0.02243 0.02575 = 0.02769 0.01124 0.00531 0.00202 AFIX 43 H38 2 1.313841 -0.244226 0.131508 11.00000 -1.20000 AFIX 0 C37 1 1.301162 -0.169318 0.053717 11.00000 0.02120 0.01857 = 0.02603 0.00458 0.00454 0.00161 AFIX 43 H37 2 1.290908 -0.223720 0.028693 11.00000 -1.20000 AFIX 0 C47 1 1.296687 -0.165718 -0.086971 11.00000 0.02017 0.01222 = 0.02165 0.00013 0.00232 -0.00126 AFIX 13 H47 2 1.272862 -0.218322 -0.068928 11.00000 -1.20000 AFIX 0 C48 1 1.372180 -0.189989 -0.075602 11.00000 0.02080 0.01886 = 0.02660 0.00483 -0.00038 0.00520 AFIX 137 H48A 2 1.388931 -0.190884 -0.032702 11.00000 -1.50000 H48B 2 1.397019 -0.141418 -0.094379 11.00000 -1.50000 H48C 2 1.379069 -0.253250 -0.092425 11.00000 -1.50000 AFIX 0 C3 1 1.205221 0.104715 -0.181251 11.00000 0.01165 0.01331 = 0.01226 -0.00114 0.00091 0.00077 AFIX 43 H3 2 1.224179 0.044313 -0.188746 11.00000 -1.20000 AFIX 0 C2 1 1.159679 0.146033 -0.225410 11.00000 0.00944 0.01394 = 0.01151 0.00005 0.00150 -0.00238 C1 1 1.129175 0.235966 -0.216085 11.00000 0.01231 0.01282 = 0.01206 0.00008 0.00141 -0.00063 AFIX 13 H1 2 1.124826 0.283949 -0.249103 11.00000 -1.20000 AFIX 0 C6 1 1.137849 0.097848 -0.283600 11.00000 0.01617 0.00810 = 0.01053 0.00224 0.00063 0.00087 C11 1 1.185812 0.071881 -0.318056 11.00000 0.01669 0.01309 = 0.01541 0.00194 0.00026 0.00122 AFIX 43 H11 2 1.232498 0.083458 -0.303585 11.00000 -1.20000 AFIX 0 C10 1 1.166613 0.029166 -0.373452 11.00000 0.02331 0.01611 = 0.01435 0.00000 0.00667 0.00214 AFIX 43 H10 2 1.199769 0.013035 -0.397068 11.00000 -1.20000 AFIX 0 C9 1 1.098776 0.010463 -0.393746 11.00000 0.02761 0.01174 = 0.01028 -0.00102 0.00035 0.00102 AFIX 43 H9 2 1.085359 -0.019970 -0.431134 11.00000 -1.20000 AFIX 0 C8 1 1.050422 0.035702 -0.360061 11.00000 0.01861 0.01191 = 0.01469 0.00182 -0.00284 -0.00007 AFIX 43 H8 2 1.004001 0.022593 -0.374774 11.00000 -1.20000 AFIX 0 C7 1 1.068351 0.080237 -0.304636 11.00000 0.01507 0.01241 = 0.01173 0.00162 0.00070 0.00127 C18 1 0.932454 0.153357 -0.315129 11.00000 0.01495 0.01744 = 0.01700 -0.00261 -0.00345 0.00080 AFIX 13 H18 2 0.925221 0.104959 -0.347956 11.00000 -1.20000 AFIX 0 C20 1 0.867835 0.160161 -0.288427 11.00000 0.01684 0.02626 = 0.02637 -0.00448 -0.00090 0.00160 AFIX 137 H20A 2 0.831837 0.189629 -0.317306 11.00000 -1.50000 H20B 2 0.876325 0.199590 -0.252374 11.00000 -1.50000 H20C 2 0.853760 0.095642 -0.278418 11.00000 -1.50000 AFIX 0 C19 1 0.950711 0.249671 -0.340742 11.00000 0.02196 0.02440 = 0.02244 0.00250 -0.00243 0.00222 AFIX 137 H19A 2 0.957645 0.298037 -0.309109 11.00000 -1.50000 H19B 2 0.913719 0.270098 -0.372072 11.00000 -1.50000 H19C 2 0.992452 0.242497 -0.357432 11.00000 -1.50000 AFIX 0 C21 1 0.977615 -0.002706 -0.230620 11.00000 0.01617 0.01924 = 0.01912 -0.00007 0.00391 -0.00170 AFIX 13 H21 2 0.940060 0.012070 -0.208177 11.00000 -1.20000 AFIX 0 C23 1 0.950022 -0.077673 -0.277165 11.00000 0.02353 0.01900 = 0.02644 -0.00159 0.00250 -0.00176 AFIX 137 H23A 2 0.934682 -0.134086 -0.257464 11.00000 -1.50000 H23B 2 0.985854 -0.096652 -0.299243 11.00000 -1.50000 H23C 2 0.911794 -0.050467 -0.304708 11.00000 -1.50000 AFIX 0 C22 1 1.036100 -0.043057 -0.185300 11.00000 0.02734 0.02432 = 0.02185 0.00303 -0.00165 0.00096 AFIX 137 H22A 2 1.073927 -0.060127 -0.205504 11.00000 -1.50000 H22B 2 1.020694 -0.100389 -0.166547 11.00000 -1.50000 H22C 2 1.051116 0.005516 -0.154840 11.00000 -1.50000 AFIX 0 C12 1 1.122787 0.373915 -0.141651 11.00000 0.01385 0.01586 = 0.00828 -0.00141 -0.00276 0.00229 C13 1 1.062349 0.393362 -0.120052 11.00000 0.01655 0.01976 = 0.01416 -0.00266 0.00070 0.00175 C24 1 0.921093 0.343258 -0.129351 11.00000 0.01749 0.02391 = 0.02170 -0.00488 0.00458 0.00371 AFIX 13 H24 2 0.920263 0.391762 -0.097182 11.00000 -1.20000 AFIX 0 C26 1 0.866710 0.267543 -0.124450 11.00000 0.01883 0.03156 = 0.02974 0.00005 0.00510 0.00287 AFIX 137 H26A 2 0.872722 0.212630 -0.149898 11.00000 -1.50000 H26B 2 0.821639 0.295532 -0.137211 11.00000 -1.50000 H26C 2 0.870994 0.246051 -0.083109 11.00000 -1.50000 AFIX 0 C25 1 0.906005 0.395203 -0.189072 11.00000 0.02419 0.02794 = 0.02783 -0.00038 -0.00158 0.00262 AFIX 137 H25A 2 0.861967 0.427530 -0.192796 11.00000 -1.50000 H25B 2 0.904853 0.348536 -0.221358 11.00000 -1.50000 H25C 2 0.941514 0.442864 -0.191374 11.00000 -1.50000 AFIX 0 C27 1 1.024823 0.246958 -0.040283 11.00000 0.02356 0.03587 = 0.01615 0.00372 0.00559 0.01008 AFIX 13 H27 2 1.075229 0.240676 -0.029681 11.00000 -1.20000 AFIX 0 C28 1 0.995730 0.145892 -0.034968 11.00000 0.03287 0.04225 = 0.03091 0.01345 0.01469 0.01288 AFIX 137 H28A 2 0.946136 0.149435 -0.040292 11.00000 -1.50000 H28B 2 1.013441 0.119498 0.004400 11.00000 -1.50000 H28C 2 1.009043 0.104239 -0.065620 11.00000 -1.50000 AFIX 0 C29 1 1.003256 0.317246 0.004653 11.00000 0.03975 0.05849 = 0.01724 -0.00286 0.00624 0.01536 AFIX 137 H29A 2 1.016290 0.291427 0.044902 11.00000 -1.50000 H29B 2 0.953959 0.326073 -0.003997 11.00000 -1.50000 H29C 2 1.025723 0.379203 0.001797 11.00000 -1.50000 AFIX 0 C14 1 1.047192 0.487794 -0.106057 11.00000 0.01904 0.02435 = 0.02262 -0.00647 0.00419 0.00466 AFIX 43 H14 2 1.006885 0.501099 -0.090741 11.00000 -1.20000 AFIX 0 C15 1 1.090470 0.561594 -0.114390 11.00000 0.02708 0.01495 = 0.02247 -0.00518 0.00029 0.00476 AFIX 43 H15 2 1.079896 0.625588 -0.104791 11.00000 -1.20000 AFIX 0 C16 1 1.149401 0.542841 -0.136732 11.00000 0.02198 0.01531 = 0.01610 -0.00180 -0.00020 0.00022 AFIX 43 H16 2 1.178711 0.594116 -0.143002 11.00000 -1.20000 AFIX 0 C17 1 1.165594 0.449697 -0.149902 11.00000 0.01814 0.01790 = 0.01291 -0.00178 0.00243 0.00102 AFIX 43 H17 2 1.206339 0.437286 -0.164730 11.00000 -1.20000 AFIX 0 C63 1 1.215377 1.180436 0.227410 11.00000 0.03078 0.07617 = 0.02882 0.00435 0.00187 -0.01512 AFIX 43 H63 2 1.244432 1.198238 0.263102 11.00000 -1.20000 AFIX 0 C62 1 1.206368 1.085801 0.213571 11.00000 0.03938 0.06475 = 0.05776 0.01631 0.02646 -0.00299 AFIX 43 H62 2 1.228886 1.037886 0.239269 11.00000 -1.20000 AFIX 0 C61 1 1.164175 1.060373 0.161819 11.00000 0.05807 0.07818 = 0.07188 -0.02758 0.04838 -0.03461 AFIX 43 H61 2 1.157999 0.994761 0.150813 11.00000 -1.20000 AFIX 0 C60 1 1.130634 1.132406 0.125788 11.00000 0.02875 0.15411 = 0.03514 -0.02760 0.01051 -0.02496 AFIX 43 H60 2 1.100117 1.115856 0.090668 11.00000 -1.20000 AFIX 0 C64 1 1.183596 1.250218 0.191145 11.00000 0.03963 0.06238 = 0.04520 -0.00056 0.01771 -0.00254 AFIX 43 H64 2 1.191130 1.315930 0.201377 11.00000 -1.20000 AFIX 0 C65 1 1.141533 1.226187 0.140834 11.00000 0.03927 0.11939 = 0.03696 0.01255 0.01156 0.01730 AFIX 43 H65 2 1.119350 1.275060 0.115714 11.00000 -1.20000 AFIX 0 C59 1 1.222465 0.536559 0.021571 11.00000 0.03701 0.02056 = 0.02332 -0.00755 0.00148 0.01197 HKLF 4 REM a14150_0m in P2(1)/n REM R1 = 0.0437 for 10238 Fo > 4sig(Fo) and 0.0856 for all 14952 data REM 737 parameters refined using 0 restraints END WGHT 0.0378 3.8172 REM Instructions for potential hydrogen bonds HTAB N2 S1 HTAB N2 O1 HTAB C33 O2 HTAB C57 N1 EQIV $1 x, y-1, z HTAB C37 F3_$1 EQIV $2 x-1/2, -y+1/2, z-1/2 HTAB C18 O2_$2 EQIV $3 -x+2, -y+1, -z HTAB C24 F2_$3 HTAB C26 O3_$3 REM Highest difference peak 0.688, deepest hole -0.452, 1-sigma level 0.083 Q1 1 1.2553 0.5251 0.0525 11.00000 0.05 0.69 Q2 1 1.0036 0.1779 -0.1683 11.00000 0.05 0.55 Q3 1 1.2981 0.0925 -0.0391 11.00000 0.05 0.52 Q4 1 1.3737 0.1021 -0.0957 11.00000 0.05 0.49 Q5 1 1.3238 0.0977 -0.1137 11.00000 0.05 0.49 ; _shelx_res_checksum 90342 _shelx_hkl_file ; -1 0 0 -0.19 0.07 1 0 0 -0.15 0.02 1 0 0 -0.26 0.07 1 0 0 -0.17 0.03 -1 0 0 -0.14 0.08 -1 0 0 -0.16 0.03 -2 0 0 89.31 2.76 -2 0 0 90.90 2.82 2 0 0 93.02 2.71 2 0 0 94.71 2.76 2 0 0 87.96 2.76 2 0 0 93.27 2.81 -2 0 0 92.52 3.15 -2 0 0 91.85 2.77 -2 0 0 91.87 2.71 3 0 0 -0.31 0.33 -3 0 0 0.24 0.40 -3 0 0 -0.57 0.27 -3 0 0 -0.49 0.36 -3 0 0 -0.18 0.37 -3 0 0 -0.75 0.33 3 0 0 -0.24 0.26 3 0 0 -0.11 0.34 3 0 0 0.17 0.36 4 0 0 69.81 2.40 4 0 0 68.52 2.37 4 0 0 68.68 2.36 -4 0 0 73.02 2.39 -4 0 0 70.25 2.45 4 0 0 69.70 2.21 -4 0 0 69.86 2.23 -4 0 0 74.07 2.61 5 0 0 -1.04 0.38 -5 0 0 -0.32 0.63 -5 0 0 -0.36 0.61 -5 0 0 -0.21 0.46 5 0 0 0.18 0.54 -5 0 0 -0.53 0.53 -6 0 0 311.12 10.71 -6 0 0 309.68 9.23 -6 0 0 329.71 9.41 -6 0 0 307.25 9.55 6 0 0 308.27 9.38 6 0 0 318.55 9.23 -7 0 0 -0.15 0.49 7 0 0 0.31 0.57 -7 0 0 0.32 0.69 7 0 0 0.08 0.41 -7 0 0 -0.22 0.64 -7 0 0 -0.85 0.56 -8 0 0 68.03 2.55 -8 0 0 64.17 2.60 -8 0 0 62.95 2.22 8 0 0 65.07 2.19 8 0 0 61.68 2.45 -8 0 0 60.41 2.55 -9 0 0 -0.06 0.56 -9 0 0 -0.59 0.78 -9 0 0 0.49 0.75 -9 0 0 0.38 0.62 9 0 0 -0.10 0.64 -10 0 0 1.33 0.88 -10 0 0 0.85 0.79 10 0 0 0.68 0.67 -10 0 0 0.87 0.66 -11 0 0 1.10 0.94 -11 0 0 -0.40 0.64 11 0 0 -0.81 0.66 12 0 0 9.82 1.16 -12 0 0 8.27 1.24 -12 0 0 11.31 1.07 -13 0 0 -0.29 0.73 13 0 0 0.00 0.73 -13 0 0 -0.33 0.93 -13 0 0 1.17 1.03 -14 0 0 4.47 1.24 14 0 0 4.49 0.98 -14 0 0 3.03 1.11 -14 0 0 3.54 0.83 15 0 0 -0.75 0.80 -15 0 0 -0.28 1.06 -15 0 0 0.69 1.22 -15 0 0 0.30 0.79 -16 0 0 20.60 2.07 -16 0 0 14.89 1.71 -16 0 0 20.67 1.72 16 0 0 19.32 1.68 -17 0 0 -0.88 1.20 -17 0 0 -1.96 1.36 17 0 0 0.68 0.95 -18 0 0 76.57 3.86 18 0 0 66.67 3.38 -18 0 0 72.03 3.74 -19 0 0 1.63 1.43 -19 0 0 2.64 1.64 19 0 0 0.44 1.07 20 0 0 3.27 1.19 -20 0 0 6.41 1.89 -20 0 0 3.97 1.64 -21 0 0 -0.59 1.55 21 0 0 0.17 1.18 -21 0 0 0.22 1.69 22 0 0 105.17 4.71 -22 0 0 94.80 4.95 -22 0 0 96.75 4.92 -23 0 0 1.76 1.77 23 0 0 0.99 1.40 -23 0 0 -0.59 1.91 -24 0 0 -1.93 1.74 24 0 0 -0.63 1.23 -24 0 0 1.42 2.10 -25 0 0 0.91 2.24 0 -1 0 0.02 0.08 0 -1 0 0.04 0.08 0 1 0 0.03 0.16 0 1 0 -0.02 0.16 -1 -1 0 -0.37 0.11 -1 -1 0 0.65 0.28 -1 -1 0 -0.40 0.11 1 -1 0 0.07 0.12 1 -1 0 -0.02 0.20 -1 -1 0 0.11 0.17 -1 -1 0 0.05 0.14 1 -1 0 -0.43 0.13 1 -1 0 -0.23 0.10 1 1 0 0.40 0.19 1 1 0 0.42 0.16 -1 1 0 0.10 0.25 -1 1 0 0.20 0.11 -1 1 0 -0.07 0.23 -1 1 0 0.43 0.15 1 1 0 0.27 0.15 1 1 0 0.06 0.17 -2 -1 0 0.77 0.27 2 -1 0 0.43 0.23 2 -1 0 0.74 0.25 -2 -1 0 0.43 0.24 -2 -1 0 0.36 0.29 2 -1 0 0.45 0.29 2 -1 0 0.68 0.29 -2 -1 0 1.28 0.39 -2 1 0 0.69 0.34 -2 1 0 0.44 0.29 -2 1 0 0.68 0.25 2 1 0 1.02 0.28 2 1 0 0.74 0.26 2 1 0 0.51 0.27 -2 1 0 0.33 0.34 3 -1 0 196.88 5.77 3 -1 0 193.50 5.66 -3 -1 0 179.19 5.64 -3 -1 0 190.17 6.57 -3 -1 0 192.56 5.74 3 -1 0 179.98 5.63 3 -1 0 196.99 5.64 3 1 0 191.89 5.74 3 1 0 184.14 5.64 -3 1 0 189.19 5.66 -3 1 0 185.31 5.77 3 1 0 190.61 5.65 -3 1 0 201.32 5.64 -4 -1 0 3.37 0.61 4 -1 0 3.13 0.54 4 -1 0 4.56 0.56 -4 -1 0 2.56 0.64 4 -1 0 2.29 0.56 -4 -1 0 2.68 0.60 4 -1 0 3.33 0.53 -4 -1 0 1.82 0.54 4 1 0 2.71 0.53 -4 1 0 3.00 0.65 -4 1 0 3.47 0.54 4 1 0 2.79 0.53 4 1 0 3.24 0.57 -4 1 0 2.85 0.59 -4 1 0 3.43 0.58 4 1 0 2.80 0.29 -5 -1 0 -0.14 0.65 -5 -1 0 1.30 0.66 5 -1 0 -0.21 0.51 -5 -1 0 0.33 0.62 5 -1 0 -0.02 0.49 5 1 0 0.49 0.29 -5 1 0 0.50 0.66 -5 1 0 0.87 0.61 -5 1 0 1.05 0.59 -5 1 0 -0.09 0.35 5 1 0 0.42 0.57 -6 -1 0 207.76 6.57 -6 -1 0 216.23 6.50 6 -1 0 213.30 6.46 -6 -1 0 212.51 7.43 6 -1 0 215.60 6.39 -6 1 0 207.55 6.60 6 1 0 208.45 6.45 -6 1 0 209.93 6.46 -6 1 0 212.97 7.19 6 1 0 213.58 6.20 -6 1 0 204.60 6.38 -7 -1 0 37.45 1.93 -7 -1 0 36.02 1.81 7 -1 0 37.19 1.70 -7 -1 0 38.50 1.80 7 1 0 39.50 1.34 7 1 0 38.55 1.71 -7 1 0 38.48 1.58 -7 1 0 37.94 1.84 -7 1 0 38.69 1.77 -7 1 0 36.64 1.64 8 -1 0 13.53 1.03 -8 -1 0 12.97 1.09 -8 -1 0 12.09 1.12 -8 -1 0 10.86 1.05 -8 1 0 12.54 0.95 8 1 0 12.96 1.06 -8 1 0 12.90 0.98 -8 1 0 11.92 1.16 8 1 0 12.79 0.73 -9 -1 0 15.62 1.47 -9 -1 0 15.06 1.28 9 -1 0 16.33 1.29 -9 -1 0 16.55 1.23 -9 1 0 16.32 1.35 -9 1 0 14.56 1.09 9 1 0 15.94 0.83 -9 1 0 17.43 1.25 9 1 0 17.36 1.32 -10 -1 0 94.77 3.80 -10 -1 0 90.95 3.57 10 -1 0 88.64 3.39 -10 -1 0 94.61 3.48 -10 1 0 96.05 3.52 -10 1 0 92.70 3.62 10 1 0 89.87 3.39 -10 1 0 97.58 3.26 10 1 0 98.00 3.01 -11 -1 0 42.91 2.32 -11 -1 0 42.85 2.29 11 -1 0 41.21 2.10 -11 -1 0 42.02 2.24 -11 1 0 46.48 1.96 -11 1 0 43.82 2.24 11 1 0 46.42 1.63 11 1 0 42.99 2.10 -11 1 0 43.25 1.96 -11 1 0 42.97 2.37 12 -1 0 16.36 1.39 -12 -1 0 13.18 1.26 -12 -1 0 13.08 1.46 12 1 0 14.89 1.33 -12 1 0 15.18 1.18 -12 1 0 16.88 1.53 -12 1 0 14.15 1.36 -12 1 0 14.98 1.19 13 -1 0 19.25 1.59 -13 -1 0 18.73 1.68 -13 -1 0 18.26 1.68 -13 1 0 15.11 1.46 -13 1 0 19.37 1.72 -13 1 0 19.36 1.35 13 1 0 16.43 1.42 -14 -1 0 1.00 1.13 14 -1 0 1.96 0.84 -14 -1 0 1.48 0.93 -14 -1 0 2.21 1.10 -14 1 0 2.38 1.06 14 1 0 2.00 0.87 -14 1 0 2.52 0.71 -14 1 0 1.66 1.19 -15 -1 0 0.07 1.12 -15 -1 0 1.35 1.22 -15 -1 0 -0.43 0.93 15 -1 0 -0.59 0.80 15 1 0 0.25 0.86 -15 1 0 -0.74 1.04 -15 1 0 -0.39 1.18 -15 1 0 -0.60 0.68 -16 -1 0 -1.72 1.11 16 -1 0 0.49 0.90 -16 -1 0 -0.25 0.91 -16 -1 0 0.28 1.28 -16 1 0 -0.19 1.15 -16 1 0 1.07 1.31 16 1 0 -0.32 0.88 -17 -1 0 -0.52 1.43 -17 -1 0 2.95 1.06 -17 -1 0 1.31 1.35 17 -1 0 1.39 0.99 -17 1 0 -0.94 1.23 -17 1 0 3.65 1.47 17 1 0 1.09 1.02 18 -1 0 0.36 0.98 -18 -1 0 -0.37 1.48 -18 -1 0 -0.46 1.29 -18 1 0 -0.50 1.31 18 1 0 0.25 1.00 -18 1 0 2.94 1.52 -19 -1 0 10.87 2.01 19 -1 0 11.35 1.60 -19 -1 0 9.60 1.72 -19 1 0 7.71 1.73 -19 1 0 10.22 1.92 19 1 0 8.79 1.49 20 -1 0 1.77 1.18 -20 -1 0 -0.15 1.53 -20 -1 0 2.44 1.80 20 1 0 -0.62 1.11 -20 1 0 1.12 1.66 -20 1 0 2.61 1.54 -21 -1 0 0.78 1.75 -21 -1 0 1.53 1.65 21 -1 0 0.96 1.23 -21 1 0 2.43 1.61 -21 1 0 2.03 1.78 21 1 0 0.57 1.19 -22 -1 0 3.18 1.83 -22 -1 0 2.76 2.00 22 -1 0 4.55 1.43 -22 1 0 3.60 1.94 -22 1 0 6.54 1.85 22 1 0 4.36 1.49 -23 -1 0 -0.66 1.71 23 -1 0 0.56 1.26 -23 -1 0 -1.31 1.74 -23 1 0 0.00 1.62 23 1 0 -1.09 1.23 -23 1 0 -4.32 1.81 -24 -1 0 8.80 2.35 24 -1 0 6.38 1.63 -24 -1 0 9.47 2.17 24 1 0 8.37 1.77 -24 1 0 5.62 2.26 -24 1 0 9.57 2.09 -25 -1 0 5.81 2.34 -25 1 0 -1.00 1.81 0 -2 0 2.03 0.43 0 -2 0 1.80 0.37 0 -2 0 1.81 0.34 0 2 0 1.96 0.41 0 2 0 1.48 0.38 -1 -2 0 260.93 7.78 1 -2 0 269.31 7.78 -1 -2 0 264.86 7.57 1 -2 0 252.03 7.67 1 -2 0 267.68 8.91 -1 -2 0 263.01 9.00 -1 -2 0 265.34 7.70 -1 -2 0 258.57 7.69 -1 -2 0 267.18 7.57 1 2 0 267.48 7.78 -1 2 0 262.24 7.77 -1 2 0 256.68 7.68 1 2 0 262.59 7.70 1 2 0 264.49 7.70 2 -2 0 371.74 12.29 -2 -2 0 372.42 10.62 -2 -2 0 374.17 10.82 2 -2 0 343.81 10.85 2 -2 0 376.39 10.77 2 -2 0 364.38 10.67 2 -2 0 355.43 10.58 -2 -2 0 373.97 10.63 -2 -2 0 373.39 12.48 -2 -2 0 372.21 10.62 2 -2 0 370.95 10.58 2 2 0 376.11 10.60 -2 2 0 361.92 10.77 -2 2 0 364.05 10.55 2 2 0 364.55 10.63 2 2 0 376.66 10.60 2 2 0 364.88 10.81 -2 2 0 361.35 10.55 -2 2 0 347.42 10.66 -3 -2 0 86.15 3.27 3 -2 0 90.02 2.81 3 -2 0 78.34 2.81 -3 -2 0 83.64 2.70 3 -2 0 84.07 2.65 3 -2 0 85.00 2.65 -3 -2 0 87.67 2.76 -3 2 0 85.13 2.82 3 2 0 85.89 2.67 3 2 0 85.24 2.54 3 2 0 85.65 2.68 -3 2 0 86.25 2.64 -3 2 0 86.23 2.63 3 2 0 86.54 2.77 -3 2 0 85.06 2.78 -3 2 0 75.77 2.82 -4 -2 0 20.86 1.15 4 -2 0 19.04 1.01 -4 -2 0 20.20 1.15 4 -2 0 20.21 1.02 -4 -2 0 18.58 1.44 -4 2 0 18.97 1.01 -4 2 0 17.20 1.27 4 2 0 19.61 1.08 -4 2 0 18.85 1.05 -4 2 0 19.96 1.23 4 2 0 18.72 1.08 4 2 0 18.62 0.69 -4 2 0 19.68 1.22 4 2 0 19.63 1.07 -5 -2 0 12.85 0.94 -5 -2 0 14.22 0.96 -5 -2 0 13.28 1.10 5 -2 0 12.22 0.94 -5 2 0 13.26 1.00 -5 2 0 13.59 1.03 -5 2 0 14.82 0.98 -5 2 0 14.14 1.05 5 2 0 12.18 0.99 -6 -2 0 0.88 0.77 -6 -2 0 1.79 0.70 6 -2 0 1.94 0.57 -6 -2 0 1.32 0.67 6 2 0 1.63 0.58 -6 2 0 1.06 0.73 -6 2 0 1.21 0.69 -6 2 0 1.23 0.64 -7 -2 0 8.87 0.95 7 -2 0 9.70 0.87 -7 -2 0 9.85 0.98 -7 -2 0 8.34 1.03 -7 2 0 9.18 0.91 -7 2 0 9.33 0.96 -7 2 0 6.82 0.93 7 2 0 6.33 0.77 -8 -2 0 27.16 1.64 -8 -2 0 24.73 1.81 8 -2 0 26.15 1.45 -8 -2 0 28.43 1.65 8 2 0 25.50 1.48 -8 2 0 27.27 1.54 8 2 0 26.09 0.92 -8 2 0 24.60 1.68 -8 2 0 23.15 1.50 -9 -2 0 7.37 0.99 9 -2 0 6.46 0.89 -9 -2 0 8.67 1.07 -9 -2 0 9.41 1.11 9 2 0 8.47 0.52 -9 2 0 8.78 1.01 -9 2 0 6.94 0.98 -9 2 0 7.29 1.05 9 2 0 9.13 0.95 10 -2 0 0.29 0.63 -10 -2 0 0.71 0.85 -10 -2 0 1.73 0.84 -10 -2 0 -0.40 0.83 -10 2 0 0.51 0.79 -10 2 0 1.65 0.90 10 2 0 2.15 0.73 -10 2 0 1.33 0.84 10 2 0 1.47 0.31 -11 -2 0 4.25 0.96 -11 -2 0 3.25 0.95 11 -2 0 4.03 0.82 -11 -2 0 2.44 0.97 -11 2 0 1.13 0.84 -11 2 0 2.14 0.46 -11 2 0 3.87 0.93 11 2 0 3.33 0.81 11 2 0 3.14 0.38 -11 2 0 2.23 0.93 -12 -2 0 66.77 3.00 -12 -2 0 67.44 3.21 12 -2 0 68.38 2.85 -12 -2 0 74.41 3.04 -12 2 0 67.85 2.78 12 2 0 67.43 2.85 12 2 0 72.79 2.21 -12 2 0 66.25 2.58 -12 2 0 62.13 2.97 -12 2 0 68.56 2.93 13 -2 0 -0.03 0.71 -13 -2 0 1.38 0.95 -13 -2 0 -0.30 1.03 13 2 0 0.80 0.32 -13 2 0 -0.59 0.93 13 2 0 1.29 0.80 -13 2 0 -0.41 0.84 -13 2 0 -0.11 0.46 -13 2 0 -0.20 0.90 -14 -2 0 0.55 1.01 14 -2 0 4.24 0.96 -14 -2 0 2.61 1.18 -14 2 0 3.84 1.23 14 2 0 3.96 0.95 -14 2 0 3.16 1.01 -14 2 0 4.40 1.15 -15 -2 0 41.49 2.51 -15 -2 0 37.54 2.61 15 -2 0 36.55 2.22 -15 -2 0 35.52 2.58 -15 2 0 36.40 2.53 -15 2 0 33.71 2.38 15 2 0 36.24 2.17 -16 -2 0 39.07 2.74 -16 -2 0 43.47 2.72 -16 -2 0 39.97 2.86 16 -2 0 40.06 2.40 16 2 0 38.23 2.39 -16 2 0 41.82 2.69 -16 2 0 44.00 2.92 17 -2 0 0.28 0.96 -17 -2 0 0.50 1.32 -17 -2 0 0.58 1.14 -17 -2 0 1.26 1.46 17 2 0 1.01 1.04 -17 2 0 1.02 1.28 -17 2 0 0.14 1.45 -18 -2 0 0.80 1.40 18 -2 0 2.55 1.09 -18 -2 0 2.56 1.22 -18 -2 0 -0.29 1.56 18 2 0 1.79 1.16 -18 2 0 2.73 1.42 -18 2 0 2.32 1.53 -19 -2 0 10.28 1.82 19 -2 0 10.60 1.53 -19 -2 0 8.61 1.96 -19 2 0 9.70 1.79 -19 2 0 7.50 1.92 19 2 0 12.91 1.66 20 -2 0 16.52 1.88 -20 -2 0 15.64 2.22 -20 -2 0 13.18 2.00 20 2 0 16.69 1.92 -20 2 0 16.65 2.05 -20 2 0 17.74 2.35 -21 -2 0 -1.31 1.74 21 -2 0 -1.38 1.12 -21 -2 0 0.42 1.63 -21 2 0 -0.27 1.67 -21 2 0 -0.50 1.52 21 2 0 -0.71 1.19 -22 -2 0 -1.36 1.66 22 -2 0 1.03 1.28 -22 -2 0 0.46 1.81 -22 2 0 0.82 1.62 -22 2 0 1.01 1.95 22 2 0 1.19 1.34 23 -2 0 15.25 1.96 -23 -2 0 19.20 2.60 -23 -2 0 9.90 2.20 -23 2 0 14.65 2.63 -23 2 0 13.82 2.19 23 2 0 14.76 2.06 24 -2 0 6.88 1.70 -24 -2 0 9.58 2.27 -24 -2 0 10.01 2.32 24 2 0 14.46 2.03 -24 2 0 9.75 1.99 -24 2 0 11.62 2.52 -25 -2 0 -0.42 2.10 -25 2 0 -3.22 1.59 0 -3 0 -0.19 0.48 0 -3 0 0.39 0.48 0 -3 0 0.50 0.58 0 3 0 -0.38 0.55 0 3 0 0.16 0.52 -1 -3 0 12.17 0.88 -1 -3 0 10.21 0.93 1 -3 0 11.78 0.89 1 -3 0 12.48 0.92 -1 -3 0 10.90 0.81 1 -3 0 12.55 1.02 -1 -3 0 11.00 0.86 1 3 0 11.84 0.95 -1 3 0 11.07 0.84 1 3 0 14.22 0.83 -1 3 0 11.86 0.95 1 3 0 12.70 0.90 2 -3 0 0.45 0.45 2 -3 0 0.28 0.27 -2 -3 0 1.01 0.47 -2 -3 0 0.71 0.34 -2 -3 0 0.36 0.36 -2 -3 0 -0.10 0.50 -2 -3 0 0.72 0.71 -2 -3 0 1.67 0.46 2 -3 0 1.00 0.52 2 -3 0 0.59 0.29 2 3 0 0.69 0.44 -2 3 0 1.37 0.71 2 3 0 1.22 0.48 -2 3 0 0.85 0.58 2 3 0 0.48 0.24 -3 -3 0 86.14 2.71 -3 -3 0 87.60 3.46 3 -3 0 84.13 3.08 -3 -3 0 88.07 2.74 -3 -3 0 87.06 2.85 -3 -3 0 84.68 2.74 3 -3 0 82.99 2.67 3 3 0 87.11 2.85 -3 3 0 84.73 2.59 3 3 0 90.52 2.68 -3 3 0 85.71 2.94 -3 3 0 89.28 2.61 3 3 0 85.51 2.70 3 3 0 87.68 2.69 -3 3 0 84.24 2.89 4 -3 0 1.33 0.33 -4 -3 0 1.21 0.52 -4 -3 0 2.80 0.42 4 -3 0 1.71 0.47 -4 -3 0 2.12 0.78 4 -3 0 2.03 0.45 -4 -3 0 2.25 0.58 -4 3 0 2.93 0.49 -4 3 0 1.60 0.64 -4 3 0 1.55 0.39 4 3 0 1.56 0.50 4 3 0 1.50 0.34 -4 3 0 1.87 0.77 4 3 0 3.00 0.50 -5 -3 0 30.83 1.48 5 -3 0 28.55 1.34 -5 -3 0 33.55 1.92 -5 -3 0 32.87 1.49 5 3 0 31.11 1.41 -5 3 0 31.36 1.30 -5 3 0 30.96 1.57 -5 3 0 31.22 1.34 -5 3 0 30.30 1.65 5 3 0 30.22 1.06 6 -3 0 11.52 0.85 -6 -3 0 10.49 1.14 -6 -3 0 11.72 0.97 -6 -3 0 10.26 0.92 -6 3 0 11.26 0.99 -6 3 0 10.22 1.04 -6 3 0 11.97 0.87 6 3 0 11.22 0.87 -6 3 0 12.43 1.09 6 3 0 11.21 0.50 -7 -3 0 1.28 0.70 -7 -3 0 0.47 0.71 -7 -3 0 -0.76 0.82 7 -3 0 0.49 0.53 -7 3 0 -0.14 0.72 -7 3 0 0.20 0.62 -7 3 0 0.12 0.76 -7 3 0 0.04 0.76 7 3 0 -0.34 0.55 -8 -3 0 55.26 2.72 -8 -3 0 55.39 2.31 -8 -3 0 53.88 2.33 8 -3 0 54.20 2.16 -8 3 0 48.12 2.37 -8 3 0 55.44 2.36 8 3 0 51.84 2.17 -8 3 0 54.95 2.18 -9 -3 0 58.16 2.47 -9 -3 0 57.20 2.83 9 -3 0 57.03 2.32 -9 -3 0 55.37 2.51 -9 3 0 60.82 2.43 -9 3 0 56.07 2.58 9 3 0 55.56 2.34 -9 3 0 58.00 2.35 -10 -3 0 29.10 1.86 -10 -3 0 27.43 1.81 10 -3 0 28.24 1.60 -10 -3 0 27.85 2.07 -10 3 0 26.99 1.78 -10 3 0 28.45 1.95 10 3 0 27.24 1.64 -10 3 0 24.39 1.65 -11 -3 0 54.52 2.57 -11 -3 0 55.87 2.58 11 -3 0 56.19 2.39 -11 -3 0 54.74 2.88 11 3 0 52.71 2.37 -11 3 0 52.77 2.42 -11 3 0 56.40 2.48 -11 3 0 50.31 2.58 12 -3 0 128.82 4.58 -12 -3 0 134.64 5.34 -12 -3 0 127.07 4.71 -12 -3 0 136.88 4.83 -12 3 0 130.27 4.58 -12 3 0 132.02 4.60 12 3 0 127.89 4.59 -12 3 0 132.80 4.89 13 -3 0 4.38 0.93 -13 -3 0 4.14 1.18 -13 -3 0 3.08 1.09 -13 -3 0 5.52 1.23 13 3 0 4.87 1.00 -13 3 0 5.19 1.26 -13 3 0 2.65 1.09 -13 3 0 4.21 1.10 -14 -3 0 25.59 2.10 -14 -3 0 20.85 1.86 14 -3 0 25.46 1.85 -14 3 0 21.30 1.73 14 3 0 20.86 1.76 -14 3 0 24.96 1.96 -14 3 0 22.11 1.94 -15 -3 0 -2.51 1.07 15 -3 0 -0.18 0.82 -15 -3 0 0.03 1.27 -15 3 0 -0.57 1.07 -15 3 0 -0.30 1.24 -15 3 0 -0.03 1.07 15 3 0 -0.23 0.86 -16 -3 0 -0.24 1.19 -16 -3 0 -0.89 1.35 -16 -3 0 -0.98 1.24 16 -3 0 -1.44 0.79 -16 3 0 -0.19 1.35 -16 3 0 -0.33 1.13 -16 3 0 -1.02 1.13 16 3 0 -0.27 0.91 -17 -3 0 1.58 1.38 -17 -3 0 -2.14 1.13 17 -3 0 -0.18 0.88 -17 -3 0 0.33 1.39 -17 3 0 -1.11 1.20 -17 3 0 -1.95 1.37 17 3 0 -0.39 0.99 18 -3 0 0.34 0.97 -18 -3 0 0.31 1.30 -18 -3 0 1.04 1.55 -18 -3 0 0.25 1.41 -18 3 0 0.83 1.33 18 3 0 0.22 1.08 -18 3 0 2.38 1.68 -19 -3 0 9.96 1.68 19 -3 0 11.39 1.60 -19 -3 0 9.25 1.95 -19 -3 0 10.86 1.83 -19 3 0 12.61 1.77 19 3 0 13.12 1.74 -19 3 0 11.22 2.03 -20 -3 0 27.94 2.63 -20 -3 0 20.78 2.41 20 -3 0 25.13 2.22 -20 3 0 25.87 2.62 20 3 0 23.22 2.19 -20 3 0 24.39 2.22 -21 -3 0 0.98 1.67 21 -3 0 1.70 1.26 -21 -3 0 0.93 1.81 21 3 0 0.61 1.25 -21 3 0 5.98 2.03 -21 3 0 0.70 1.53 22 -3 0 15.51 2.01 -22 -3 0 17.18 2.34 -22 -3 0 21.31 2.64 -22 3 0 23.96 2.37 22 3 0 21.35 2.21 -22 3 0 22.26 2.67 -23 -3 0 11.01 2.26 23 -3 0 11.68 1.84 -23 -3 0 12.16 2.37 -23 3 0 13.74 2.56 23 3 0 11.51 1.90 -23 3 0 15.59 2.17 -24 -3 0 2.58 2.01 -24 -3 0 -1.81 1.81 24 -3 0 -0.11 1.25 -24 3 0 -0.11 1.66 24 3 0 1.68 1.45 -24 3 0 -2.31 2.14 -25 -3 0 0.16 2.12 -25 3 0 -1.01 1.65 0 -4 0 23.92 1.44 0 4 0 25.08 1.30 0 4 0 22.86 1.27 -1 -4 0 71.01 2.41 -1 -4 0 69.22 2.90 1 -4 0 71.69 2.79 1 4 0 71.13 2.48 -1 4 0 69.18 2.57 1 4 0 68.47 2.45 -1 4 0 69.57 2.47 -2 -4 0 41.01 1.36 -2 -4 0 39.06 1.60 -2 -4 0 41.14 1.35 -2 -4 0 43.01 2.11 -2 -4 0 38.95 1.60 2 -4 0 40.75 1.83 -2 4 0 38.22 1.69 2 4 0 42.07 1.61 -2 4 0 41.83 1.85 2 4 0 37.79 1.58 -3 -4 0 10.93 0.76 -3 -4 0 9.63 1.07 3 -4 0 9.50 0.92 -3 -4 0 9.52 0.76 -3 -4 0 9.59 0.77 -3 -4 0 11.56 0.88 3 -4 0 11.20 0.67 3 -4 0 10.38 0.63 3 4 0 9.75 0.52 -3 4 0 9.95 0.87 3 4 0 9.77 0.56 3 4 0 9.31 0.69 -3 4 0 9.20 0.93 -4 -4 0 2.03 0.56 4 -4 0 2.98 0.49 -4 -4 0 3.62 0.91 -4 -4 0 2.46 0.57 -4 -4 0 2.46 0.51 4 -4 0 3.33 0.46 4 -4 0 2.93 0.46 -4 4 0 2.98 0.31 4 4 0 3.42 0.48 4 4 0 2.38 0.46 -4 4 0 2.23 0.83 -4 4 0 4.22 0.73 -4 4 0 3.15 0.35 4 4 0 3.40 0.44 -5 -4 0 151.61 4.85 -5 -4 0 154.90 5.77 -5 -4 0 150.46 4.58 5 -4 0 154.71 5.24 5 -4 0 146.15 4.66 -5 -4 0 153.88 4.77 5 4 0 152.83 4.58 -5 4 0 149.52 4.97 -5 4 0 149.89 4.57 5 4 0 160.13 4.67 -5 4 0 146.66 4.85 5 4 0 148.39 4.67 -5 4 0 156.41 4.59 -6 -4 0 10.98 0.92 -6 -4 0 10.23 0.92 -6 -4 0 10.06 1.21 6 -4 0 10.46 0.81 -6 4 0 7.95 0.65 -6 4 0 11.30 0.78 6 4 0 9.66 0.61 -6 4 0 12.22 1.15 6 4 0 9.61 0.81 -6 4 0 9.30 0.97 -7 -4 0 24.69 1.86 -7 -4 0 25.22 1.47 -7 -4 0 22.80 1.49 7 -4 0 20.07 1.22 -7 4 0 22.20 1.52 -7 4 0 20.38 1.67 7 4 0 23.06 0.85 -7 4 0 20.79 1.24 7 4 0 24.00 1.33 8 -4 0 2.23 0.62 -8 -4 0 2.96 0.83 -8 -4 0 2.61 1.02 -8 -4 0 2.27 0.83 -8 4 0 2.94 0.69 -8 4 0 1.68 0.82 8 4 0 3.85 0.72 -8 4 0 1.97 0.88 -8 4 0 4.05 1.01 -9 -4 0 16.90 1.54 -9 -4 0 14.50 1.25 -9 -4 0 15.32 1.28 9 -4 0 16.37 1.24 -9 4 0 18.43 1.45 -9 4 0 14.44 1.11 -9 4 0 15.88 1.33 9 4 0 14.96 1.25 -9 4 0 14.69 1.38 -10 -4 0 76.77 3.12 10 -4 0 73.89 2.92 -10 -4 0 77.12 3.09 -10 -4 0 77.63 3.62 -10 4 0 77.28 2.90 10 4 0 79.60 2.96 -10 4 0 78.86 3.16 -10 4 0 78.89 3.15 -10 4 0 72.94 3.19 -11 -4 0 0.95 0.91 -11 -4 0 1.72 0.97 -11 -4 0 1.46 1.04 11 -4 0 0.11 0.64 -11 4 0 -1.16 0.93 -11 4 0 0.30 0.84 11 4 0 -0.62 0.68 -11 4 0 0.82 1.03 -11 4 0 0.02 0.77 12 -4 0 3.75 0.88 -12 -4 0 4.84 1.11 -12 -4 0 4.47 1.17 -12 -4 0 3.70 1.21 -12 4 0 3.85 1.06 -12 4 0 2.75 0.95 -12 4 0 3.86 1.13 -12 4 0 1.28 1.11 12 4 0 3.80 0.91 -13 -4 0 44.26 2.52 13 -4 0 40.74 2.22 -13 -4 0 42.21 2.47 -13 -4 0 41.83 2.78 13 4 0 42.02 2.23 -13 4 0 40.72 2.27 -13 4 0 40.26 2.40 -13 4 0 42.73 2.48 14 -4 0 6.81 1.14 -14 -4 0 9.61 1.53 -14 -4 0 7.94 1.43 14 4 0 7.19 1.15 -14 4 0 8.15 1.42 -14 4 0 9.07 1.40 -14 4 0 6.59 1.18 15 -4 0 0.47 0.85 -15 -4 0 1.58 1.32 -15 -4 0 0.73 1.27 15 4 0 1.16 0.94 -15 4 0 -0.65 1.02 -15 4 0 1.22 1.21 -15 4 0 1.00 1.25 -16 -4 0 35.27 2.77 16 -4 0 35.55 2.28 -16 -4 0 33.40 2.72 -16 -4 0 36.57 2.73 -16 4 0 34.10 2.37 -16 4 0 39.08 2.83 16 4 0 31.89 2.23 -16 4 0 34.53 2.42 17 -4 0 62.89 3.19 -17 -4 0 67.09 3.85 -17 -4 0 71.17 3.70 -17 -4 0 66.70 3.63 17 4 0 68.01 3.30 -17 4 0 71.42 3.40 -17 4 0 67.16 3.62 -17 4 0 68.59 3.35 18 -4 0 10.65 1.51 -18 -4 0 10.12 1.83 -18 -4 0 9.51 1.72 -18 -4 0 11.48 1.95 -18 4 0 9.85 1.58 18 4 0 9.23 1.47 -18 4 0 9.07 1.84 -19 -4 0 0.77 1.50 -19 -4 0 0.77 1.50 19 -4 0 -1.42 0.93 -19 -4 0 -0.29 1.54 19 4 0 0.61 1.12 -19 4 0 -1.77 1.24 -19 4 0 -2.91 1.52 -20 -4 0 -1.18 1.46 20 -4 0 0.74 1.10 -20 -4 0 1.33 1.76 -20 -4 0 -1.20 1.54 -20 4 0 -4.22 1.53 20 4 0 0.02 1.11 -20 4 0 1.05 1.34 -21 -4 0 4.99 1.86 -21 -4 0 4.49 1.92 21 -4 0 4.89 1.39 -21 4 0 1.35 1.46 -21 4 0 6.90 2.04 21 4 0 4.80 1.42 -21 4 0 4.54 1.82 -22 -4 0 6.60 1.94 -22 -4 0 5.64 2.01 22 -4 0 4.18 1.38 -22 4 0 3.22 1.59 -22 4 0 4.21 1.87 -22 4 0 8.55 2.26 22 4 0 5.47 1.55 -23 -4 0 -3.33 1.73 23 -4 0 1.12 1.27 -23 -4 0 2.49 1.95 -23 4 0 -0.05 2.04 23 4 0 1.97 1.50 -23 4 0 -3.44 1.43 -23 4 0 -1.14 1.65 24 -4 0 2.62 1.49 -24 -4 0 5.04 2.17 -24 -4 0 2.68 2.18 24 4 0 4.28 1.65 -24 4 0 0.84 1.85 -24 4 0 2.64 2.54 -24 4 0 4.80 1.83 -25 -4 0 4.64 2.32 -25 4 0 4.11 1.85 0 -5 0 -0.13 0.61 0 -5 0 -0.18 0.53 0 5 0 -0.29 0.66 0 5 0 -0.50 0.59 1 -5 0 11.47 1.02 -1 -5 0 12.00 0.88 -1 -5 0 10.51 1.06 1 5 0 14.16 1.13 -1 5 0 13.27 0.98 1 5 0 13.83 1.02 -1 5 0 12.37 1.08 -2 -5 0 22.62 0.87 2 -5 0 20.87 1.43 -2 -5 0 20.93 0.85 -2 -5 0 23.45 1.69 -2 -5 0 19.71 1.19 -2 5 0 22.07 1.48 2 5 0 22.22 1.24 -2 5 0 22.84 1.35 3 -5 0 135.94 3.97 3 -5 0 135.82 3.97 3 -5 0 134.02 4.85 -3 -5 0 135.39 4.06 -3 -5 0 130.44 5.13 -3 -5 0 134.70 4.28 -3 -5 0 132.38 4.06 3 5 0 131.74 4.22 -3 5 0 130.99 4.47 -3 5 0 130.94 4.33 -4 -5 0 -0.23 0.80 4 -5 0 0.20 0.36 -4 -5 0 0.31 0.48 4 -5 0 0.25 0.48 -4 -5 0 -0.05 0.53 4 5 0 0.21 0.46 4 5 0 0.49 0.30 4 5 0 0.04 0.26 -4 5 0 -0.09 0.64 -4 5 0 -0.62 0.78 -5 -5 0 0.15 0.50 -5 -5 0 -0.52 0.55 5 -5 0 -0.04 0.46 -5 -5 0 0.88 0.57 5 -5 0 0.07 0.40 -5 -5 0 -0.71 0.87 5 5 0 -0.30 0.43 -5 5 0 1.40 0.85 -5 5 0 1.31 0.72 5 5 0 0.38 0.37 5 5 0 -0.07 0.41 -6 -5 0 0.32 0.92 6 -5 0 0.86 0.47 -6 -5 0 0.34 0.63 6 -5 0 0.24 0.41 -6 -5 0 0.61 0.61 6 5 0 -0.23 0.37 -6 5 0 -0.18 0.87 -6 5 0 1.07 0.43 -6 5 0 0.61 0.75 -6 5 0 0.28 0.32 6 5 0 0.36 0.52 -7 -5 0 92.89 3.19 -7 -5 0 85.62 3.90 -7 -5 0 90.87 3.23 7 -5 0 91.79 3.05 -7 5 0 92.44 3.30 7 5 0 89.08 3.02 -7 5 0 89.66 2.91 -7 5 0 83.43 2.86 7 5 0 90.18 2.80 -7 5 0 81.84 3.41 8 -5 0 14.01 1.09 -8 -5 0 16.56 1.23 -8 -5 0 14.34 1.52 -8 -5 0 13.19 1.17 8 5 0 14.42 1.14 8 5 0 13.93 0.70 -8 5 0 14.77 1.08 -8 5 0 13.90 1.25 -8 5 0 16.44 1.46 -9 -5 0 132.57 5.47 -9 -5 0 135.36 4.63 9 -5 0 132.82 4.43 -9 -5 0 128.99 4.54 -9 5 0 130.09 4.64 -9 5 0 135.24 4.32 -9 5 0 131.77 4.74 9 5 0 137.52 4.43 -10 -5 0 8.98 1.13 -10 -5 0 7.10 1.07 10 -5 0 8.14 0.94 -10 -5 0 7.45 1.37 -10 5 0 9.05 0.94 -10 5 0 8.42 1.14 10 5 0 6.89 0.94 -10 5 0 7.64 1.27 -11 -5 0 5.48 1.09 -11 -5 0 5.52 1.10 -11 -5 0 6.81 1.34 11 -5 0 5.64 0.92 -11 5 0 4.41 1.14 11 5 0 6.44 0.98 -11 5 0 6.60 1.32 -11 5 0 5.76 0.92 -11 5 0 5.89 1.14 -12 -5 0 1.58 1.19 12 -5 0 -0.51 0.65 -12 -5 0 -0.11 0.94 -12 -5 0 0.13 0.97 12 5 0 -0.21 0.78 -12 5 0 -2.53 1.03 -12 5 0 0.01 1.12 -12 5 0 -0.43 0.78 -12 5 0 -1.26 0.93 -13 -5 0 76.63 3.40 -13 -5 0 82.41 3.47 -13 -5 0 80.89 4.02 13 -5 0 70.35 3.16 -13 5 0 79.76 3.50 -13 5 0 78.25 3.12 13 5 0 78.84 3.20 -13 5 0 78.01 3.64 -13 5 0 75.51 3.43 -14 -5 0 4.27 1.38 -14 -5 0 4.14 1.28 -14 -5 0 5.83 1.49 14 -5 0 4.91 1.04 -14 5 0 4.16 1.44 -14 5 0 4.60 1.24 14 5 0 4.36 1.03 -14 5 0 4.80 1.07 -14 5 0 0.57 1.26 -15 -5 0 63.31 3.29 15 -5 0 65.01 2.98 -15 -5 0 63.71 3.72 -15 5 0 64.52 3.25 -15 5 0 63.16 3.23 -15 5 0 57.71 3.32 15 5 0 62.63 2.99 -15 5 0 68.36 2.98 -16 -5 0 -0.24 1.40 16 -5 0 0.71 0.92 -16 -5 0 -1.59 1.34 16 5 0 1.76 1.06 -16 5 0 -0.65 1.18 -16 5 0 3.56 1.45 -16 5 0 -0.48 1.39 -16 5 0 -0.05 1.06 -17 -5 0 2.72 1.56 -17 -5 0 4.26 1.53 -17 -5 0 3.92 1.57 17 -5 0 6.53 1.24 17 5 0 6.12 1.27 -17 5 0 6.68 1.56 -17 5 0 4.06 1.47 -17 5 0 1.15 1.58 -17 5 0 4.04 1.27 18 -5 0 3.15 1.12 -18 -5 0 1.73 1.61 -18 -5 0 -1.12 1.45 -18 -5 0 0.34 1.48 -18 5 0 2.87 1.51 18 5 0 0.46 1.14 -18 5 0 6.23 1.64 -18 5 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