data_global _audit_creation_method 'APEX2 v2013.6-2' _publ_requested_journal ; Inorganic Chemistry ; _publ_contact_author_name 'Ryan J. Trovitch' _publ_contact_author_address ; Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; _publ_contact_author_email 'ryan.trovitch@asu.edu' _publ_contact_author_fax '(480) 965-2747' _publ_contact_author_phone '(480) 727-8930' loop_ _publ_author_name _publ_author_address 'Raja Pal' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'Thomas L. Groy' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'Ryan J. Trovitch' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; _publ_section_title ; Conversion of Carbon Dioxide to Methanol Using a C-H Activated Bis(imino)pyridine Molybdenum Hydroboration Catalyst ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_Ph2PPrPDIMoI2 _chemical_name_systematic Ph2PPrPDIMoI2 _chemical_name_common Ph2PPrPDIMoI2 _chemical_formula_moiety ? _chemical_formula_sum 'C39 H41 I2 Mo N3 P2' _chemical_formula_iupac ? _chemical_formula_weight 963.43 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 10.270(5) _cell_length_b 18.930(10) _cell_length_c 19.310(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3754.(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5245 _cell_measurement_theta_min 2.2461 _cell_measurement_theta_max 23.8834 _cell_measurement_temperature 123.(2) _exptl_crystal_description Needle _exptl_crystal_colour 'clear dark red-orange' _exptl_crystal_size_max 0.576 _exptl_crystal_size_mid 0.133 _exptl_crystal_size_min 0.119 _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 2.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.79 _exptl_special_details ; ; _diffrn_ambient_temperature 123.(2) _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3330 _diffrn_reflns_number 29746 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.44 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Attempts to refine an inversion twin resulted in a twin fraction of 0.00166 and was therefore removed from the final refinement. ; _reflns_number_total 6929 _reflns_number_gt 5607 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_gt 0.1166 _refine_ls_wR_factor_ref 0.1273 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_number_reflns 6929 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.748 _refine_diff_density_min -0.608 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.007(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' N N 0.0061 0.0033 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2010.9.0.0' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'XShell ver. 6.3.1 (Bruker AXS, 2004)' _computing_publication_material 'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo1 0.51323(10) 0.44972(5) 0.09375(5) 0.0212(2) Uani d . . . 1 . . I I1 0.31319(9) 0.35108(5) 0.08532(4) 0.0368(2) Uani d . . . 1 . . I I2 0.70828(10) 0.70495(5) 0.86208(4) 0.0368(2) Uani d . . . 1 . . P P1 0.6194(4) 0.38188(16) 0.00007(16) 0.0261(7) Uani d . . . 1 . . P P2 0.3825(3) 0.49734(17) 0.18928(16) 0.0231(7) Uani d . . . 1 . . N N1 0.6678(11) 0.4095(5) 0.1467(5) 0.026(2) Uani d . . . 1 . . N N2 0.6609(10) 0.5271(5) 0.1001(5) 0.025(2) Uani d . . . 1 . . N N3 0.4475(10) 0.5424(5) 0.0479(5) 0.023(2) Uani d . . . 1 . . C C1 0.8948(15) 0.4110(9) 0.1952(8) 0.045(4) Uani d . . . 1 . . H H1A 0.9587 0.3955 0.1607 0.067 Uiso calc U . R 1 . . H H1B 0.8665 0.3704 0.2229 0.067 Uiso calc U . R 1 . . H H1C 0.9344 0.4464 0.2256 0.067 Uiso calc U . R 1 . . C C2 0.7797(13) 0.4426(6) 0.1592(6) 0.026(3) Uani d . . . 1 . . C C3 0.7749(12) 0.5140(7) 0.1331(6) 0.028(3) Uani d . . . 1 . . C C4 0.8724(12) 0.5651(7) 0.1376(7) 0.031(3) Uani d . . . 1 . . H H4 0.9516 0.5544 0.1607 0.037 Uiso calc U . R 1 . . C C5 0.8547(13) 0.6302(7) 0.1089(7) 0.035(3) Uani d . . . 1 . . H H5 0.9207 0.6653 0.1112 0.042 Uiso calc U . R 1 . . C C6 0.7365(13) 0.6433(7) 0.0762(7) 0.035(3) Uani d . . . 1 . . H H6 0.7212 0.6882 0.0559 0.042 Uiso calc U . R 1 . . C C7 0.6429(13) 0.5931(6) 0.0729(6) 0.025(3) Uani d . . . 1 . . C C8 0.5183(13) 0.6007(6) 0.0443(6) 0.025(3) Uani d . . . 1 . . C C9 0.4654(14) 0.6699(6) 0.0176(7) 0.034(3) Uani d . . . 1 . . H H9A 0.4678 0.7052 0.0547 0.051 Uiso calc U . R 1 . . H H9B 0.3754 0.6633 0.0021 0.051 Uiso calc U . R 1 . . H H9C 0.5187 0.6861 -0.0214 0.051 Uiso calc U . R 1 . . C C10 0.6563(13) 0.3320(6) 0.1614(6) 0.028(3) Uani d . . . 1 . . H H10A 0.5632 0.3191 0.1652 0.034 Uiso calc U . R 1 . . H H10B 0.6987 0.3212 0.2062 0.034 Uiso calc U . R 1 . . C C11 0.7198(16) 0.2888(6) 0.1043(6) 0.038(3) Uani d . . . 1 . . H H11A 0.8109 0.3049 0.0988 0.045 Uiso calc U . R 1 . . H H11B 0.7224 0.2387 0.1191 0.045 Uiso calc U . R 1 . . C C12 0.6533(12) 0.2926(7) 0.0345(6) 0.029(3) Uani d . . . 1 . . H H12A 0.5698 0.2668 0.0378 0.035 Uiso calc U . R 1 . . H H12B 0.7083 0.2673 0.0005 0.035 Uiso calc U . R 1 . . C C13 0.5371(12) 0.3622(6) -0.0820(6) 0.026(3) Uani d . . . 1 . . C C14 0.5809(14) 0.3081(7) -0.1255(6) 0.034(3) Uani d . . . 1 . . H H14 0.6548 0.2809 -0.1127 0.04 Uiso calc U . R 1 . . C C15 0.5167(13) 0.2941(7) -0.1873(6) 0.031(3) Uani d . . . 1 . . H H15 0.5469 0.2574 -0.2168 0.037 Uiso calc U . R 1 . . C C16 0.4109(15) 0.3327(7) -0.2055(7) 0.034(3) Uani d . . . 1 . . H H16 0.3658 0.322 -0.2471 0.04 Uiso calc U . R 1 . . C C17 0.3689(17) 0.3861(7) -0.1652(7) 0.041(4) Uani d . . . 1 . . H H17 0.2961 0.4133 -0.1797 0.049 Uiso calc U . R 1 . . C C18 0.4313(14) 0.4024(7) -0.1017(7) 0.037(3) Uani d . . . 1 . . H H18 0.401 0.44 -0.0734 0.045 Uiso calc U . R 1 . . C C19 0.7751(13) 0.4175(7) -0.0260(5) 0.027(3) Uani d . . . 1 . . C C20 0.8939(14) 0.3803(7) -0.0239(7) 0.036(3) Uani d . . . 1 . . H H20 0.8953 0.3324 -0.0091 0.044 Uiso calc U . R 1 . . C C21 1.0061(15) 0.4125(8) -0.0429(7) 0.041(3) Uani d . . . 1 . . H H21 1.0855 0.387 -0.0403 0.05 Uiso calc U . R 1 . . C C22 1.0079(15) 0.4826(8) -0.0664(7) 0.041(4) Uani d . . . 1 . . H H22 1.0872 0.504 -0.0807 0.049 Uiso calc U . R 1 . . C C23 0.8926(14) 0.5201(7) -0.0683(6) 0.034(3) Uani d . . . 1 . . H H23 0.8931 0.5681 -0.0827 0.041 Uiso calc U . R 1 . . C C24 0.7770(14) 0.4887(7) -0.0496(6) 0.029(3) Uani d . . . 1 . . H H24 0.698 0.5146 -0.0526 0.035 Uiso calc U . R 1 . . C C25 0.3077(13) 0.5414(7) 0.0307(6) 0.029(3) Uani d . . . 1 . . H H25A 0.2801 0.492 0.0224 0.035 Uiso calc U . R 1 . . H H25B 0.2937 0.5683 -0.0127 0.035 Uiso calc U . R 1 . . C C26 0.2234(12) 0.5732(6) 0.0878(6) 0.028(3) Uani d . . . 1 . . H H26A 0.1325 0.5765 0.071 0.034 Uiso calc U . R 1 . . H H26B 0.2541 0.6217 0.0976 0.034 Uiso calc U . R 1 . . C C27 0.2252(12) 0.5296(6) 0.1568(6) 0.025(3) Uani d . . . 1 . . H H27A 0.1677 0.4882 0.1504 0.03 Uiso calc U . R 1 . . H H27B 0.1858 0.5593 0.1934 0.03 Uiso calc U . R 1 . . C C28 0.3369(12) 0.4388(6) 0.2611(5) 0.024(3) Uani d . . . 1 . . C C29 0.2090(14) 0.4314(7) 0.2844(6) 0.031(3) Uani d . . . 1 . . H H29 0.1419 0.4595 0.2646 0.038 Uiso calc U . R 1 . . C C30 0.1792(15) 0.3833(8) 0.3363(7) 0.040(4) Uani d . . . 1 . . H H30 0.0921 0.3787 0.3522 0.049 Uiso calc U . R 1 . . C C31 0.2737(16) 0.3434(7) 0.3641(7) 0.041(4) Uani d . . . 1 . . H H31 0.2518 0.3105 0.3994 0.049 Uiso calc U . R 1 . . C C32 0.4014(15) 0.3486(7) 0.3430(6) 0.035(3) Uani d . . . 1 . . H H32 0.4668 0.3202 0.3639 0.042 Uiso calc U . R 1 . . C C33 0.4334(14) 0.3957(6) 0.2910(6) 0.027(3) Uani d . . . 1 . . H H33 0.5209 0.399 0.2754 0.032 Uiso calc U . R 1 . . C C34 0.4658(12) 0.5729(6) 0.2294(6) 0.026(3) Uani d . . . 1 . . C C35 0.4242(13) 0.6411(6) 0.2197(6) 0.027(3) Uani d . . . 1 . . H H35 0.3446 0.6502 0.1964 0.033 Uiso calc U . R 1 . . C C36 0.4991(14) 0.6962(7) 0.2442(7) 0.034(3) Uani d . . . 1 . . H H36 0.4687 0.7432 0.2382 0.041 Uiso calc U . R 1 . . C C37 0.6161(15) 0.6853(7) 0.2769(7) 0.038(3) Uani d . . . 1 . . H H37 0.6685 0.7239 0.2917 0.046 Uiso calc U . R 1 . . C C38 0.6551(15) 0.6157(7) 0.2877(7) 0.036(4) Uani d . . . 1 . . H H38 0.7333 0.6069 0.3125 0.043 Uiso calc U . R 1 . . C C39 0.5836(13) 0.5593(7) 0.2634(6) 0.027(3) Uani d . . . 1 . . H H39 0.6135 0.5122 0.2696 0.032 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.0219(6) 0.0213(5) 0.0202(5) -0.0014(4) -0.0013(4) -0.0001(4) I1 0.0416(6) 0.0323(4) 0.0366(5) -0.0092(4) -0.0058(4) -0.0011(4) I2 0.0384(5) 0.0422(5) 0.0299(4) -0.0074(5) 0.0027(4) 0.0039(4) P1 0.032(2) 0.0236(16) 0.0222(16) 0.0014(15) -0.0013(14) 0.0004(13) P2 0.0208(17) 0.0260(16) 0.0224(15) -0.0010(14) -0.0001(13) 0.0004(13) N1 0.037(7) 0.014(5) 0.028(5) -0.002(5) 0.004(5) -0.002(4) N2 0.027(6) 0.027(5) 0.020(5) 0.002(4) -0.003(4) -0.003(4) N3 0.022(6) 0.026(5) 0.019(5) 0.003(5) 0.001(4) 0.001(4) C1 0.035(9) 0.055(10) 0.045(8) -0.003(8) -0.008(7) 0.003(7) C2 0.026(7) 0.028(6) 0.025(6) 0.002(6) 0.004(5) 0.007(5) C3 0.022(7) 0.041(7) 0.020(6) 0.004(6) -0.002(5) 0.002(5) C4 0.014(6) 0.041(8) 0.038(7) -0.001(6) -0.008(6) 0.007(6) C5 0.017(7) 0.036(8) 0.052(9) -0.011(6) 0.002(6) -0.002(6) C6 0.038(8) 0.031(7) 0.036(7) 0.001(6) 0.010(6) -0.002(6) C7 0.038(8) 0.019(6) 0.017(6) -0.005(5) 0.003(5) -0.001(5) C8 0.034(8) 0.022(6) 0.018(6) -0.005(6) 0.003(5) 0.000(5) C9 0.034(8) 0.027(7) 0.041(7) 0.004(6) 0.006(6) -0.003(6) C10 0.034(8) 0.024(6) 0.026(6) 0.001(6) -0.005(5) 0.002(5) C11 0.060(10) 0.021(6) 0.031(7) 0.015(7) -0.005(7) 0.006(5) C12 0.027(7) 0.032(7) 0.029(6) 0.005(6) 0.004(5) 0.002(6) C13 0.034(7) 0.022(6) 0.022(6) -0.005(5) 0.004(5) 0.005(5) C14 0.032(8) 0.040(8) 0.030(7) 0.005(6) -0.003(6) 0.003(6) C15 0.038(8) 0.026(6) 0.028(6) -0.009(7) 0.001(6) -0.008(5) C16 0.041(9) 0.032(7) 0.029(7) -0.006(7) 0.001(6) 0.007(6) C17 0.053(10) 0.036(8) 0.033(7) -0.003(7) -0.007(7) -0.001(6) C18 0.043(9) 0.039(8) 0.029(7) 0.018(7) -0.001(6) -0.002(6) C19 0.030(8) 0.037(7) 0.013(5) 0.005(6) -0.001(5) -0.004(5) C20 0.035(9) 0.040(8) 0.033(7) 0.006(7) 0.008(6) 0.007(6) C21 0.034(9) 0.057(9) 0.033(7) 0.011(8) 0.001(7) 0.000(7) C22 0.031(8) 0.063(10) 0.030(7) -0.006(8) 0.000(6) 0.011(7) C23 0.040(9) 0.036(7) 0.025(7) -0.005(7) 0.000(6) 0.002(5) C24 0.034(8) 0.031(7) 0.022(6) 0.003(6) 0.001(6) -0.004(5) C25 0.028(7) 0.030(7) 0.030(6) -0.008(6) -0.002(6) 0.003(5) C26 0.021(7) 0.032(6) 0.031(6) 0.003(5) 0.003(6) 0.006(6) C27 0.022(7) 0.029(6) 0.025(6) 0.003(5) 0.002(5) 0.006(5) C28 0.030(7) 0.029(7) 0.014(5) -0.006(6) -0.006(5) 0.002(5) C29 0.024(7) 0.042(8) 0.028(6) -0.003(7) 0.004(6) 0.004(6) C30 0.030(8) 0.049(9) 0.043(8) -0.020(7) 0.008(6) -0.005(7) C31 0.062(11) 0.028(7) 0.032(7) 0.000(7) 0.005(7) 0.004(6) C32 0.041(9) 0.030(7) 0.035(7) 0.005(7) 0.007(6) 0.003(6) C33 0.039(8) 0.017(6) 0.026(6) -0.002(6) 0.009(6) -0.010(5) C34 0.024(7) 0.022(6) 0.030(6) -0.005(5) 0.002(5) 0.000(5) C35 0.027(7) 0.029(7) 0.026(6) 0.003(6) 0.001(5) -0.006(5) C36 0.035(8) 0.026(6) 0.041(7) 0.003(6) 0.000(6) 0.000(6) C37 0.042(9) 0.034(8) 0.039(8) -0.002(7) 0.006(7) 0.003(6) C38 0.050(10) 0.026(7) 0.032(7) -0.013(7) -0.001(6) -0.004(6) C39 0.028(7) 0.025(6) 0.028(6) 0.001(6) -0.001(5) 0.004(5) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 N1 . 2.036(11) ? Mo1 N3 . 2.077(10) ? Mo1 N2 . 2.112(10) ? Mo1 P2 . 2.453(3) ? Mo1 P1 . 2.472(3) ? Mo1 I1 . 2.7810(17) ? P1 C19 . 1.807(13) ? P1 C13 . 1.834(13) ? P1 C12 . 1.849(13) ? P2 C28 . 1.835(12) ? P2 C27 . 1.838(13) ? P2 C34 . 1.839(12) ? N1 C2 . 1.332(16) ? N1 C10 . 1.498(15) ? N2 C3 . 1.356(16) ? N2 C7 . 1.368(15) ? N3 C8 . 1.324(15) ? N3 C25 . 1.474(16) ? C1 C2 . 1.496(19) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? C2 C3 . 1.442(17) ? C3 C4 . 1.395(17) ? C4 C5 . 1.363(18) ? C4 H4 . 0.95 ? C5 C6 . 1.391(19) ? C5 H5 . 0.95 ? C6 C7 . 1.353(18) ? C6 H6 . 0.95 ? C7 C8 . 1.401(18) ? C8 C9 . 1.508(17) ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 C11 . 1.521(17) ? C10 H10A . 0.99 ? C10 H10B . 0.99 ? C11 C12 . 1.512(17) ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C13 C18 . 1.380(18) ? C13 C14 . 1.398(17) ? C14 C15 . 1.390(17) ? C14 H14 . 0.95 ? C15 C16 . 1.356(19) ? C15 H15 . 0.95 ? C16 C17 . 1.346(19) ? C16 H16 . 0.95 ? C17 C18 . 1.419(19) ? C17 H17 . 0.95 ? C18 H18 . 0.95 ? C19 C20 . 1.410(18) ? C19 C24 . 1.423(17) ? C20 C21 . 1.35(2) ? C20 H20 . 0.95 ? C21 C22 . 1.40(2) ? C21 H21 . 0.95 ? C22 C23 . 1.38(2) ? C22 H22 . 0.95 ? C23 C24 . 1.376(19) ? C23 H23 . 0.95 ? C24 H24 . 0.95 ? C25 C26 . 1.525(17) ? C25 H25A . 0.99 ? C25 H25B . 0.99 ? C26 C27 . 1.567(16) ? C26 H26A . 0.99 ? C26 H26B . 0.99 ? C27 H27A . 0.99 ? C27 H27B . 0.99 ? C28 C29 . 1.396(18) ? C28 C33 . 1.408(18) ? C29 C30 . 1.388(18) ? C29 H29 . 0.95 ? C30 C31 . 1.34(2) ? C30 H30 . 0.95 ? C31 C32 . 1.38(2) ? C31 H31 . 0.95 ? C32 C33 . 1.382(17) ? C32 H32 . 0.95 ? C33 H33 . 0.95 ? C34 C35 . 1.372(17) ? C34 C39 . 1.400(17) ? C35 C36 . 1.379(18) ? C35 H35 . 0.95 ? C36 C37 . 1.37(2) ? C36 H36 . 0.95 ? C37 C38 . 1.392(19) ? C37 H37 . 0.95 ? C38 C39 . 1.380(17) ? C38 H38 . 0.95 ? C39 H39 . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Mo1 N3 . . 141.6(4) ? N1 Mo1 N2 . . 70.8(4) ? N3 Mo1 N2 . . 70.9(4) ? N1 Mo1 P2 . . 100.8(3) ? N3 Mo1 P2 . . 80.3(3) ? N2 Mo1 P2 . . 95.4(3) ? N1 Mo1 P1 . . 80.2(3) ? N3 Mo1 P1 . . 105.7(3) ? N2 Mo1 P1 . . 95.0(3) ? P2 Mo1 P1 . . 169.30(12) ? N1 Mo1 I1 . . 110.8(3) ? N3 Mo1 I1 . . 107.6(3) ? N2 Mo1 I1 . . 178.2(3) ? P2 Mo1 I1 . . 83.48(9) ? P1 Mo1 I1 . . 86.22(9) ? C19 P1 C13 . . 104.0(5) ? C19 P1 C12 . . 105.9(6) ? C13 P1 C12 . . 102.3(5) ? C19 P1 Mo1 . . 113.6(4) ? C13 P1 Mo1 . . 122.3(4) ? C12 P1 Mo1 . . 107.1(4) ? C28 P2 C27 . . 103.5(6) ? C28 P2 C34 . . 105.7(5) ? C27 P2 C34 . . 107.1(6) ? C28 P2 Mo1 . . 119.1(4) ? C27 P2 Mo1 . . 110.3(4) ? C34 P2 Mo1 . . 110.4(4) ? C2 N1 C10 . . 119.7(10) ? C2 N1 Mo1 . . 126.0(8) ? C10 N1 Mo1 . . 113.6(8) ? C3 N2 C7 . . 117.7(11) ? C3 N2 Mo1 . . 121.3(8) ? C7 N2 Mo1 . . 120.9(8) ? C8 N3 C25 . . 122.2(10) ? C8 N3 Mo1 . . 123.3(8) ? C25 N3 Mo1 . . 113.8(8) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? N1 C2 C3 . . 110.3(11) ? N1 C2 C1 . . 125.3(11) ? C3 C2 C1 . . 124.4(12) ? N2 C3 C4 . . 121.4(11) ? N2 C3 C2 . . 111.5(11) ? C4 C3 C2 . . 127.1(11) ? C5 C4 C3 . . 120.4(12) ? C5 C4 H4 . . 119.8 ? C3 C4 H4 . . 119.8 ? C4 C5 C6 . . 117.5(12) ? C4 C5 H5 . . 121.3 ? C6 C5 H5 . . 121.3 ? C7 C6 C5 . . 121.2(12) ? C7 C6 H6 . . 119.4 ? C5 C6 H6 . . 119.4 ? C6 C7 N2 . . 121.8(12) ? C6 C7 C8 . . 126.6(12) ? N2 C7 C8 . . 111.6(11) ? N3 C8 C7 . . 113.3(10) ? N3 C8 C9 . . 123.0(12) ? C7 C8 C9 . . 123.5(11) ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? N1 C10 C11 . . 110.8(10) ? N1 C10 H10A . . 109.5 ? C11 C10 H10A . . 109.5 ? N1 C10 H10B . . 109.5 ? C11 C10 H10B . . 109.5 ? H10A C10 H10B . . 108.1 ? C12 C11 C10 . . 115.3(11) ? C12 C11 H11A . . 108.5 ? C10 C11 H11A . . 108.5 ? C12 C11 H11B . . 108.5 ? C10 C11 H11B . . 108.5 ? H11A C11 H11B . . 107.5 ? C11 C12 P1 . . 116.7(9) ? C11 C12 H12A . . 108.1 ? P1 C12 H12A . . 108.1 ? C11 C12 H12B . . 108.1 ? P1 C12 H12B . . 108.1 ? H12A C12 H12B . . 107.3 ? C18 C13 C14 . . 119.5(12) ? C18 C13 P1 . . 119.3(9) ? C14 C13 P1 . . 121.2(10) ? C15 C14 C13 . . 120.2(13) ? C15 C14 H14 . . 119.9 ? C13 C14 H14 . . 119.9 ? C16 C15 C14 . . 120.0(12) ? C16 C15 H15 . . 120.0 ? C14 C15 H15 . . 120.0 ? C17 C16 C15 . . 120.8(13) ? C17 C16 H16 . . 119.6 ? C15 C16 H16 . . 119.6 ? C16 C17 C18 . . 121.2(15) ? C16 C17 H17 . . 119.4 ? C18 C17 H17 . . 119.4 ? C13 C18 C17 . . 118.3(12) ? C13 C18 H18 . . 120.9 ? C17 C18 H18 . . 120.9 ? C20 C19 C24 . . 118.1(12) ? C20 C19 P1 . . 124.9(10) ? C24 C19 P1 . . 117.1(10) ? C21 C20 C19 . . 120.2(13) ? C21 C20 H20 . . 119.9 ? C19 C20 H20 . . 119.9 ? C20 C21 C22 . . 121.7(14) ? C20 C21 H21 . . 119.1 ? C22 C21 H21 . . 119.1 ? C23 C22 C21 . . 118.9(14) ? C23 C22 H22 . . 120.5 ? C21 C22 H22 . . 120.5 ? C24 C23 C22 . . 120.7(13) ? C24 C23 H23 . . 119.7 ? C22 C23 H23 . . 119.7 ? C23 C24 C19 . . 120.4(13) ? C23 C24 H24 . . 119.8 ? C19 C24 H24 . . 119.8 ? N3 C25 C26 . . 112.6(10) ? N3 C25 H25A . . 109.1 ? C26 C25 H25A . . 109.1 ? N3 C25 H25B . . 109.1 ? C26 C25 H25B . . 109.1 ? H25A C25 H25B . . 107.8 ? C25 C26 C27 . . 113.6(10) ? C25 C26 H26A . . 108.8 ? C27 C26 H26A . . 108.8 ? C25 C26 H26B . . 108.8 ? C27 C26 H26B . . 108.8 ? H26A C26 H26B . . 107.7 ? C26 C27 P2 . . 118.4(8) ? C26 C27 H27A . . 107.7 ? P2 C27 H27A . . 107.7 ? C26 C27 H27B . . 107.7 ? P2 C27 H27B . . 107.7 ? H27A C27 H27B . . 107.1 ? C29 C28 C33 . . 118.2(11) ? C29 C28 P2 . . 123.0(9) ? C33 C28 P2 . . 118.6(9) ? C30 C29 C28 . . 120.4(13) ? C30 C29 H29 . . 119.8 ? C28 C29 H29 . . 119.8 ? C31 C30 C29 . . 119.9(14) ? C31 C30 H30 . . 120.0 ? C29 C30 H30 . . 120.0 ? C30 C31 C32 . . 122.0(13) ? C30 C31 H31 . . 119.0 ? C32 C31 H31 . . 119.0 ? C31 C32 C33 . . 119.2(14) ? C31 C32 H32 . . 120.4 ? C33 C32 H32 . . 120.4 ? C32 C33 C28 . . 120.3(13) ? C32 C33 H33 . . 119.9 ? C28 C33 H33 . . 119.9 ? C35 C34 C39 . . 120.5(12) ? C35 C34 P2 . . 122.0(10) ? C39 C34 P2 . . 117.1(9) ? C34 C35 C36 . . 119.4(13) ? C34 C35 H35 . . 120.3 ? C36 C35 H35 . . 120.3 ? C37 C36 C35 . . 122.2(13) ? C37 C36 H36 . . 118.9 ? C35 C36 H36 . . 118.9 ? C36 C37 C38 . . 117.5(14) ? C36 C37 H37 . . 121.3 ? C38 C37 H37 . . 121.3 ? C39 C38 C37 . . 122.0(14) ? C39 C38 H38 . . 119.0 ? C37 C38 H38 . . 119.0 ? C38 C39 C34 . . 118.4(12) ? C38 C39 H39 . . 120.8 ? C34 C39 H39 . . 120.8 ? _shelx_res_file ; TITL RP_1_246_0m_P212121 in P2(1)2(1)2(1) CELL 0.71073 10.2703 18.9300 19.3097 90.000 90.000 90.000 ZERR 4.00 0.0054 0.0099 0.0101 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N P Mo I UNIT 156 164 12 8 4 8 L.S. 20 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.119 0.133 0.576 FREE C33 C34 TEMP -150.000 WGHT 0.068900 FVAR 0.07352 MOLE 1 MO1 5 0.513232 0.449721 0.093753 11.00000 0.02193 0.02130 = 0.02024 -0.00010 -0.00127 -0.00138 I1 6 0.313193 0.351084 0.085323 11.00000 0.04159 0.03230 = 0.03662 -0.00109 -0.00578 -0.00918 I2 6 0.708278 0.704953 0.862081 11.00000 0.03836 0.04222 = 0.02989 0.00388 0.00273 -0.00743 P1 4 0.619363 0.381880 0.000070 11.00000 0.03242 0.02355 = 0.02219 0.00041 -0.00127 0.00140 P2 4 0.382544 0.497341 0.189281 11.00000 0.02084 0.02602 = 0.02243 0.00038 -0.00007 -0.00100 N1 3 0.667832 0.409485 0.146673 11.00000 0.03725 0.01446 = 0.02761 -0.00247 0.00356 -0.00165 N2 3 0.660879 0.527137 0.100142 11.00000 0.02676 0.02677 = 0.02035 -0.00300 -0.00308 0.00208 N3 3 0.447484 0.542354 0.047924 11.00000 0.02188 0.02645 = 0.01922 0.00095 0.00064 0.00263 C1 1 0.894750 0.410988 0.195216 11.00000 0.03480 0.05455 = 0.04501 0.00323 -0.00807 -0.00321 AFIX 137 H1A 2 0.958680 0.395479 0.160742 11.00000 -1.50000 H1B 2 0.866480 0.370367 0.222853 11.00000 -1.50000 H1C 2 0.934445 0.446387 0.225641 11.00000 -1.50000 AFIX 0 C2 1 0.779733 0.442629 0.159211 11.00000 0.02644 0.02766 = 0.02538 0.00729 0.00408 0.00236 C3 1 0.774880 0.513953 0.133076 11.00000 0.02196 0.04120 = 0.02043 0.00215 -0.00173 0.00351 C4 1 0.872393 0.565068 0.137572 11.00000 0.01381 0.04078 = 0.03776 0.00744 -0.00764 -0.00076 AFIX 43 H4 2 0.951597 0.554422 0.160742 11.00000 -1.20000 AFIX 0 C5 1 0.854741 0.630189 0.108929 11.00000 0.01702 0.03637 = 0.05249 -0.00155 0.00237 -0.01102 AFIX 43 H5 2 0.920687 0.665303 0.111208 11.00000 -1.20000 AFIX 0 C6 1 0.736475 0.643255 0.076236 11.00000 0.03840 0.03090 = 0.03555 -0.00188 0.01021 0.00114 AFIX 43 H6 2 0.721170 0.688194 0.055906 11.00000 -1.20000 AFIX 0 C7 1 0.642891 0.593100 0.072886 11.00000 0.03776 0.01944 = 0.01714 -0.00069 0.00310 -0.00545 C8 1 0.518275 0.600704 0.044286 11.00000 0.03415 0.02232 = 0.01809 -0.00022 0.00340 -0.00466 C9 1 0.465423 0.669883 0.017599 11.00000 0.03382 0.02735 = 0.04120 -0.00274 0.00630 0.00405 AFIX 137 H9A 2 0.467830 0.705190 0.054694 11.00000 -1.50000 H9B 2 0.375356 0.663296 0.002132 11.00000 -1.50000 H9C 2 0.518744 0.686109 -0.021368 11.00000 -1.50000 AFIX 0 C10 1 0.656281 0.332044 0.161407 11.00000 0.03435 0.02407 = 0.02570 0.00155 -0.00482 0.00097 AFIX 23 H10A 2 0.563175 0.319052 0.165156 11.00000 -1.20000 H10B 2 0.698723 0.321227 0.206202 11.00000 -1.20000 AFIX 0 C11 1 0.719792 0.288772 0.104279 11.00000 0.06004 0.02139 = 0.03110 0.00596 -0.00490 0.01477 AFIX 23 H11A 2 0.810909 0.304902 0.098809 11.00000 -1.20000 H11B 2 0.722389 0.238737 0.119135 11.00000 -1.20000 AFIX 0 C12 1 0.653338 0.292638 0.034500 11.00000 0.02704 0.03176 = 0.02901 0.00217 0.00398 0.00475 AFIX 23 H12A 2 0.569765 0.266788 0.037754 11.00000 -1.20000 H12B 2 0.708305 0.267341 0.000458 11.00000 -1.20000 AFIX 0 C13 1 0.537128 0.362231 -0.082027 11.00000 0.03399 0.02221 = 0.02210 0.00519 0.00415 -0.00534 C14 1 0.580936 0.308111 -0.125454 11.00000 0.03174 0.03957 = 0.02950 0.00304 -0.00256 0.00479 AFIX 43 H14 2 0.654810 0.280875 -0.112660 11.00000 -1.20000 AFIX 0 C15 1 0.516674 0.294051 -0.187305 11.00000 0.03768 0.02599 = 0.02795 -0.00762 0.00100 -0.00871 AFIX 43 H15 2 0.546856 0.257390 -0.216820 11.00000 -1.20000 AFIX 0 C16 1 0.410856 0.332709 -0.205483 11.00000 0.04061 0.03160 = 0.02876 0.00681 0.00138 -0.00618 AFIX 43 H16 2 0.365828 0.321966 -0.247148 11.00000 -1.20000 AFIX 0 C17 1 0.368851 0.386088 -0.165243 11.00000 0.05325 0.03634 = 0.03331 -0.00113 -0.00650 -0.00278 AFIX 43 H17 2 0.296068 0.413344 -0.179663 11.00000 -1.20000 AFIX 0 C18 1 0.431258 0.402405 -0.101686 11.00000 0.04311 0.03919 = 0.02897 -0.00230 -0.00063 0.01798 AFIX 43 H18 2 0.400955 0.440019 -0.073384 11.00000 -1.20000 AFIX 0 C19 1 0.775096 0.417500 -0.025989 11.00000 0.03030 0.03704 = 0.01275 -0.00361 -0.00130 0.00491 C20 1 0.893916 0.380271 -0.023887 11.00000 0.03537 0.04040 = 0.03325 0.00743 0.00824 0.00591 AFIX 43 H20 2 0.895321 0.332422 -0.009072 11.00000 -1.20000 AFIX 0 C21 1 1.006055 0.412506 -0.042922 11.00000 0.03427 0.05663 = 0.03327 0.00039 0.00086 0.01065 AFIX 43 H21 2 1.085528 0.386964 -0.040332 11.00000 -1.20000 AFIX 0 C22 1 1.007899 0.482639 -0.066365 11.00000 0.03061 0.06285 = 0.03020 0.01138 0.00027 -0.00581 AFIX 43 H22 2 1.087162 0.503994 -0.080677 11.00000 -1.20000 AFIX 0 C23 1 0.892610 0.520129 -0.068297 11.00000 0.04019 0.03631 = 0.02549 0.00158 0.00024 -0.00496 AFIX 43 H23 2 0.893103 0.568127 -0.082658 11.00000 -1.20000 AFIX 0 C24 1 0.777007 0.488675 -0.049634 11.00000 0.03404 0.03098 = 0.02158 -0.00387 0.00117 0.00334 AFIX 43 H24 2 0.698036 0.514636 -0.052556 11.00000 -1.20000 AFIX 0 C25 1 0.307684 0.541429 0.030674 11.00000 0.02848 0.02961 = 0.03022 0.00251 -0.00205 -0.00836 AFIX 23 H25A 2 0.280081 0.492042 0.022371 11.00000 -1.20000 H25B 2 0.293662 0.568274 -0.012689 11.00000 -1.20000 AFIX 0 C26 1 0.223412 0.573182 0.087791 11.00000 0.02123 0.03244 = 0.03147 0.00626 0.00262 0.00294 AFIX 23 H26A 2 0.132537 0.576481 0.070999 11.00000 -1.20000 H26B 2 0.254106 0.621747 0.097555 11.00000 -1.20000 AFIX 0 C27 1 0.225239 0.529615 0.156798 11.00000 0.02208 0.02865 = 0.02479 0.00595 0.00248 0.00267 AFIX 23 H27A 2 0.167652 0.488181 0.150432 11.00000 -1.20000 H27B 2 0.185821 0.559289 0.193441 11.00000 -1.20000 AFIX 0 C28 1 0.336855 0.438828 0.261068 11.00000 0.02970 0.02920 = 0.01390 0.00153 -0.00646 -0.00590 C29 1 0.208959 0.431423 0.284387 11.00000 0.02419 0.04175 = 0.02820 0.00409 0.00366 -0.00318 AFIX 43 H29 2 0.141851 0.459459 0.264611 11.00000 -1.20000 AFIX 0 C30 1 0.179215 0.383331 0.336310 11.00000 0.02969 0.04908 = 0.04267 -0.00487 0.00786 -0.01960 AFIX 43 H30 2 0.092065 0.378701 0.352161 11.00000 -1.20000 AFIX 0 C31 1 0.273662 0.343402 0.364078 11.00000 0.06225 0.02753 = 0.03221 0.00416 0.00529 -0.00040 AFIX 43 H31 2 0.251779 0.310517 0.399371 11.00000 -1.20000 AFIX 0 C32 1 0.401445 0.348647 0.342957 11.00000 0.04111 0.02965 = 0.03468 0.00282 0.00656 0.00451 AFIX 43 H32 2 0.466776 0.320244 0.363880 11.00000 -1.20000 AFIX 0 C33 1 0.433417 0.395719 0.290977 11.00000 0.03880 0.01665 = 0.02554 -0.00954 0.00905 -0.00192 AFIX 43 H33 2 0.520916 0.399014 0.275351 11.00000 -1.20000 AFIX 0 C34 1 0.465813 0.572923 0.229450 11.00000 0.02412 0.02225 = 0.03021 -0.00010 0.00157 -0.00548 C35 1 0.424234 0.641059 0.219728 11.00000 0.02689 0.02928 = 0.02562 -0.00609 0.00073 0.00332 AFIX 43 H35 2 0.344600 0.650209 0.196361 11.00000 -1.20000 AFIX 0 C36 1 0.499056 0.696156 0.244175 11.00000 0.03459 0.02558 = 0.04143 -0.00048 0.00016 0.00314 AFIX 43 H36 2 0.468664 0.743156 0.238168 11.00000 -1.20000 AFIX 0 C37 1 0.616130 0.685322 0.276940 11.00000 0.04200 0.03375 = 0.03913 0.00343 0.00569 -0.00244 AFIX 43 H37 2 0.668490 0.723857 0.291698 11.00000 -1.20000 AFIX 0 C38 1 0.655128 0.615745 0.287697 11.00000 0.04989 0.02647 = 0.03156 -0.00446 -0.00150 -0.01278 AFIX 43 H38 2 0.733346 0.606905 0.312488 11.00000 -1.20000 AFIX 0 C39 1 0.583567 0.559252 0.263425 11.00000 0.02807 0.02493 = 0.02760 0.00408 -0.00055 0.00088 AFIX 43 H39 2 0.613490 0.512188 0.269621 11.00000 -1.20000 AFIX 0 HKLF 4 REM RP_1_246_0m_P212121 in P2(1)2(1)2(1) REM R1 = 0.0515 for 5607 Fo > 4sig(Fo) and 0.0708 for all 6929 data REM 426 parameters refined using 0 restraints END WGHT 0.0689 0.0000 REM Highest difference peak 1.748, deepest hole -0.608, 1-sigma level 0.200 Q1 1 0.6230 0.7094 0.8606 11.00000 0.05 1.75 Q2 1 0.4110 0.3953 0.0881 11.00000 0.05 1.69 Q3 1 0.7934 0.6959 0.8634 11.00000 0.05 1.47 Q4 1 0.7022 0.7337 0.8910 11.00000 0.05 1.39 Q5 1 0.4075 0.3379 0.0834 11.00000 0.05 1.35 ; _shelx_res_checksum 56716 _shelx_hkl_file ; 2 0 0 158.81 9.28 2 0 0 168.47 9.05 3 0 0 -0.15 1.00 3 0 0 -0.62 0.90 3 0 0 -0.78 1.64 4 0 0 66.48 4.52 4 0 0 64.41 4.60 5 0 0 -3.63 2.15 5 0 0 -0.46 1.26 5 0 0 -2.00 1.33 6 0 0 105.58 7.13 6 0 0 111.85 7.04 7 0 0 -3.44 2.81 7 0 0 2.27 1.77 7 0 0 2.73 1.83 8 0 0 3.14 2.27 8 0 0 -1.04 2.12 8 0 0 3.24 3.23 9 0 0 -3.71 3.20 9 0 0 0.77 2.39 9 0 0 -2.08 2.32 10 0 0 125.41 9.40 10 0 0 142.87 9.37 11 0 0 1.88 2.95 11 0 0 0.39 3.71 11 0 0 2.56 2.82 12 0 0 6.91 3.52 12 0 0 5.80 3.26 12 0 0 -0.12 3.99 1 1 0 4.66 0.62 1 1 0 4.41 0.65 -1 1 0 4.37 0.50 2 -1 0 140.63 8.35 2 1 0 146.84 8.38 2 1 0 145.23 8.14 2 -1 0 150.60 8.12 3 1 0 2.86 1.11 3 -1 0 -2.05 1.61 3 -1 0 2.86 1.15 3 -1 0 4.57 1.16 3 1 0 -0.94 1.54 3 1 0 2.71 1.14 4 1 0 352.98 20.64 4 -1 0 378.96 20.09 4 1 0 357.98 20.08 4 -1 0 381.75 20.71 5 -1 0 4.51 1.58 5 1 0 -0.59 1.43 5 -1 0 2.08 1.50 5 1 0 0.73 1.36 6 1 0 92.65 6.15 6 -1 0 94.81 6.14 6 -1 0 92.15 6.34 6 1 0 85.18 6.23 7 -1 0 3.82 1.93 7 1 0 3.41 1.89 7 1 0 -0.44 2.77 7 -1 0 3.59 2.97 7 -1 0 8.39 2.18 7 1 0 1.51 1.96 8 1 0 68.41 6.02 8 -1 0 80.11 6.06 8 -1 0 80.71 5.98 8 1 0 76.74 6.05 9 1 0 35.60 4.28 9 -1 0 33.88 4.23 9 1 0 43.29 4.48 9 -1 0 42.45 4.36 10 -1 0 5.34 3.98 10 1 0 2.57 2.91 10 1 0 7.32 3.02 10 -1 0 5.15 2.95 10 1 0 4.01 3.82 11 1 0 -4.01 3.68 11 -1 0 11.31 3.25 11 -1 0 0.81 3.81 11 1 0 11.56 3.36 11 -1 0 10.74 3.24 11 1 0 10.29 3.32 12 -1 0 -0.29 3.06 12 1 0 0.49 2.96 12 1 0 0.31 3.17 12 -1 0 1.08 3.04 12 -1 0 1.99 4.04 0 -2 0 116.78 6.30 -1 2 0 119.42 7.64 1 2 0 147.74 7.75 1 -2 0 145.71 7.43 -2 2 0 262.66 15.13 2 -2 0 294.11 14.82 2 2 0 277.85 15.31 2 2 0 259.96 14.84 3 2 0 33.74 2.82 3 2 0 30.84 2.86 3 -2 0 38.41 2.82 3 -2 0 36.78 2.75 4 2 0 -1.32 1.41 4 2 0 2.76 1.38 4 -2 0 -1.15 2.04 4 -2 0 4.86 1.64 4 2 0 5.07 2.19 5 2 0 -1.93 2.59 5 -2 0 -2.02 2.30 5 -2 0 1.25 1.46 5 2 0 -2.19 1.59 5 -2 0 6.36 1.67 5 2 0 3.54 1.58 6 -2 0 5.23 1.81 6 2 0 1.52 2.77 6 -2 0 -2.83 1.70 6 2 0 1.39 1.78 6 2 0 4.36 1.85 6 -2 0 -2.94 2.58 7 -2 0 25.28 3.14 7 2 0 26.86 3.26 7 2 0 24.31 3.20 7 -2 0 32.91 3.34 8 -2 0 94.29 7.13 8 2 0 88.99 7.10 8 2 0 100.95 7.04 8 -2 0 105.24 6.95 9 -2 0 11.42 2.77 9 2 0 -3.19 3.61 9 -2 0 7.25 2.65 9 2 0 11.49 2.98 9 2 0 17.92 3.04 9 -2 0 -0.76 3.56 10 2 0 5.67 2.94 10 -2 0 3.39 2.65 10 2 0 6.82 4.14 10 2 0 5.19 2.93 10 -2 0 2.82 3.82 10 -2 0 -4.32 2.53 11 2 0 16.63 3.72 11 2 0 1.56 4.26 11 -2 0 27.53 4.09 11 2 0 17.45 3.80 12 2 0 2.55 3.31 12 2 0 6.22 3.21 12 -2 0 0.56 4.14 0 -3 0 -0.83 0.48 0 -3 0 -0.25 0.65 0 3 0 -0.17 0.51 -1 -3 0 23.01 1.78 1 -3 0 20.48 1.62 -1 3 0 17.25 1.76 1 3 0 23.36 1.86 2 -3 0 0.27 0.87 2 3 0 0.50 1.07 -2 3 0 1.01 0.78 -2 -3 0 1.04 0.63 2 -3 0 -1.02 1.71 2 3 0 -0.21 1.02 3 3 0 -2.61 1.04 -3 3 0 2.62 0.89 3 3 0 -0.40 1.11 3 -3 0 0.92 1.06 4 3 0 0.16 1.28 4 3 0 -5.29 1.74 4 -3 0 -1.71 2.01 -4 3 0 0.44 0.83 4 -3 0 -0.58 1.21 4 3 0 -3.78 1.15 5 3 0 -1.78 1.37 5 3 0 0.30 2.29 5 -3 0 -7.10 2.31 5 -3 0 1.80 1.50 6 3 0 21.50 2.86 6 3 0 18.78 2.73 7 3 0 46.83 4.52 7 -3 0 59.01 4.62 7 -3 0 57.01 4.55 7 3 0 45.34 4.69 8 -3 0 1.45 2.34 8 3 0 1.91 2.33 8 -3 0 4.40 2.32 8 3 0 3.43 3.50 8 -3 0 1.14 3.31 8 3 0 10.56 2.64 -9 3 0 7.47 1.83 9 3 0 7.74 2.67 9 3 0 4.44 2.65 9 3 0 3.79 3.70 9 -3 0 1.76 3.61 10 -3 0 29.56 3.95 10 3 0 31.90 4.28 -10 3 0 25.12 3.04 10 3 0 30.12 4.23 11 3 0 3.56 3.07 11 -3 0 -1.14 3.66 11 3 0 0.99 3.01 -11 3 0 5.12 2.07 11 -3 0 1.15 3.08 12 -3 0 -2.19 3.92 12 3 0 14.40 4.05 0 4 0 203.47 11.42 0 -4 0 192.98 11.03 0 -4 0 214.60 14.66 -1 4 0 14.39 1.47 -1 -4 0 13.88 1.43 1 -4 0 14.93 1.39 1 4 0 15.16 1.60 2 4 0 2.87 1.16 -2 -4 0 0.09 1.01 2 -4 0 -2.03 1.82 -2 4 0 2.67 0.92 2 -4 0 3.28 0.91 3 4 0 45.31 3.35 3 -4 0 52.63 3.22 3 4 0 50.71 3.58 -3 -4 0 41.42 3.60 -3 4 0 42.69 3.11 4 4 0 86.05 5.56 -4 -4 0 74.55 6.15 -4 4 0 78.78 5.10 4 4 0 79.43 5.25 4 -4 0 87.46 5.27 5 4 0 53.59 4.36 5 -4 0 55.77 4.08 -5 4 0 54.85 3.82 5 4 0 47.12 4.05 6 4 0 -0.76 1.62 6 4 0 -2.93 2.45 6 -4 0 -2.73 2.62 6 4 0 6.21 2.00 7 4 0 0.58 2.00 7 4 0 -5.42 2.83 7 -4 0 -1.54 3.17 7 4 0 0.64 1.95 8 -4 0 21.89 3.08 8 4 0 16.50 3.28 8 4 0 20.00 3.19 -8 4 0 25.18 2.72 -9 4 0 60.98 4.81 9 -4 0 67.85 5.41 9 4 0 64.82 5.59 9 4 0 65.41 5.87 -9 -4 0 55.81 5.77 10 -4 0 7.28 2.69 10 -4 0 2.21 3.74 10 4 0 0.91 2.73 10 4 0 5.84 2.97 -10 4 0 2.18 1.83 11 -4 0 2.74 3.94 11 4 0 5.44 3.12 11 4 0 2.74 2.90 -11 4 0 0.87 1.98 12 4 0 -1.22 3.29 -12 -4 0 5.59 2.50 12 -4 0 2.78 4.38 0 -5 0 -0.89 0.70 0 5 0 -0.29 0.82 0 -5 0 -1.05 1.03 1 5 0 227.64 11.45 1 -5 0 181.80 10.94 -1 5 0 180.49 11.32 -1 -5 0 206.21 11.01 -1 -5 0 206.97 14.29 2 5 0 70.89 4.30 2 -5 0 61.95 3.83 -2 -5 0 61.79 4.00 -2 5 0 55.09 4.01 3 5 0 200.79 10.93 -3 -5 0 193.97 13.21 -3 -5 0 184.79 10.37 3 -5 0 162.18 10.27 -4 5 0 14.14 1.71 4 5 0 14.62 2.23 -4 -5 0 12.16 1.71 4 5 0 14.73 1.97 4 -5 0 15.22 1.87 5 -5 0 35.97 3.19 -5 -5 0 34.02 3.21 5 5 0 37.83 3.59 -5 5 0 32.58 2.85 5 5 0 35.63 3.12 -6 5 0 59.17 4.19 -6 -5 0 55.48 4.89 6 5 0 56.37 4.79 6 5 0 56.54 4.42 6 -5 0 58.33 4.50 -7 5 0 30.20 2.96 7 5 0 22.67 3.35 7 5 0 19.71 2.95 7 -5 0 27.04 3.09 -7 -5 0 22.88 3.04 -8 -5 0 10.02 2.48 8 5 0 10.71 2.73 8 -5 0 -0.10 3.56 8 5 0 13.12 3.03 -9 5 0 32.95 3.53 9 5 0 35.59 4.15 9 5 0 30.52 4.34 9 -5 0 32.34 3.84 -10 5 0 0.20 1.77 10 -5 0 -0.28 3.49 10 5 0 1.62 2.58 10 5 0 1.38 2.73 -11 -5 0 2.05 2.24 -11 5 0 -1.42 1.79 11 5 0 1.69 3.16 11 -5 0 3.82 4.04 12 5 0 42.04 5.59 -12 -5 0 35.41 4.36 0 6 0 80.94 5.05 0 -6 0 88.26 6.51 0 -6 0 76.02 4.80 -1 -6 0 0.06 0.81 1 6 0 -0.04 0.90 -1 -6 0 -0.97 0.77 1 -6 0 0.25 1.51 -1 6 0 -1.37 0.80 1 -6 0 0.17 0.81 -2 6 0 101.35 6.58 2 6 0 112.36 6.71 -2 -6 0 119.53 6.48 2 -6 0 104.57 6.36 3 6 0 488.31 25.91 -3 6 0 392.29 25.57 3 -6 0 418.15 24.79 -3 -6 0 529.97 32.51 -3 -6 0 476.26 24.98 4 6 0 8.89 1.93 -4 6 0 11.65 1.60 -4 -6 0 9.41 1.34 4 -6 0 10.08 1.58 -4 -6 0 11.04 1.69 5 6 0 34.78 3.54 -5 -6 0 36.12 3.10 5 -6 0 31.44 3.19 -5 6 0 32.38 2.85 6 6 0 -1.06 1.77 6 6 0 0.27 1.44 -6 6 0 -0.37 1.15 6 -6 0 0.01 1.57 6 -6 0 -2.71 2.81 -6 -6 0 -1.71 1.02 7 6 0 127.61 8.62 -7 6 0 135.90 8.46 -7 -6 0 133.49 10.36 7 -6 0 142.85 8.60 7 6 0 139.76 9.26 8 -6 0 1.09 3.70 8 -6 0 12.80 2.63 8 6 0 11.19 2.93 -8 6 0 14.55 2.22 8 6 0 9.77 2.55 9 6 0 -1.51 2.44 9 -6 0 -0.10 2.16 9 -6 0 -0.09 3.56 -9 -6 0 0.69 1.78 -9 6 0 0.54 1.58 10 -6 0 1.62 3.88 10 6 0 3.87 3.02 -10 -6 0 3.27 2.18 -10 6 0 4.57 1.91 11 6 0 2.65 3.25 11 -6 0 1.28 3.80 -11 -6 0 2.63 2.29 0 7 0 -0.93 0.86 0 -7 0 0.06 0.85 0 -7 0 -0.64 1.22 -1 7 0 544.45 31.66 -1 -7 0 587.72 30.74 1 -7 0 584.85 40.92 1 -7 0 541.25 30.65 -1 -7 0 574.55 40.46 1 7 0 606.65 31.76 2 -7 0 -1.42 2.11 -2 -7 0 7.20 1.34 -2 7 0 6.30 1.37 2 -7 0 6.49 1.28 -2 -7 0 7.59 1.08 2 7 0 7.12 1.48 -3 -7 0 19.98 2.08 3 7 0 16.77 2.28 3 -7 0 16.80 1.90 -3 7 0 18.90 2.07 -4 -7 0 135.21 8.72 4 -7 0 107.30 7.04 -4 -7 0 122.33 7.20 -4 7 0 104.52 7.22 5 -7 0 -1.82 2.45 5 7 0 0.56 1.57 5 -7 0 0.12 1.35 -5 7 0 0.81 1.13 -5 -7 0 0.04 0.85 -5 -7 0 -1.97 1.16 -6 -7 0 -0.65 1.04 6 -7 0 -1.12 2.99 6 7 0 0.53 1.92 -6 -7 0 -0.35 1.43 7 7 0 41.21 4.54 7 -7 0 45.83 4.15 -7 7 0 44.76 3.70 -7 -7 0 38.54 3.87 8 7 0 23.55 3.66 -8 7 0 24.23 2.84 8 -7 0 20.76 3.09 -8 -7 0 26.32 3.17 9 7 0 42.10 5.10 -9 -7 0 39.30 4.07 -9 7 0 37.18 3.72 10 7 0 -0.05 2.75 -10 7 0 3.57 1.86 10 -7 0 0.66 3.87 -10 -7 0 2.40 2.18 -11 -7 0 44.79 4.79 11 7 0 45.87 5.87 0 -8 0 74.76 5.03 0 8 0 88.46 5.40 0 -8 0 88.79 6.92 1 -8 0 107.93 8.35 -1 -8 0 96.03 5.96 1 8 0 108.59 6.33 -1 8 0 93.79 6.17 -1 -8 0 101.48 7.69 1 -8 0 93.00 5.91 -2 -8 0 18.56 1.96 -2 8 0 14.05 1.90 2 8 0 15.94 2.08 -2 -8 0 20.39 2.02 2 -8 0 13.93 1.80 3 8 0 77.45 5.31 -3 8 0 71.14 5.02 3 -8 0 70.25 4.85 -3 -8 0 82.00 5.03 -4 -8 0 210.77 11.45 -4 8 0 187.19 11.59 4 8 0 203.59 11.98 4 -8 0 192.63 11.24 5 -8 0 231.30 13.08 -5 8 0 211.80 13.40 -5 -8 0 227.63 13.16 -5 -8 0 247.22 16.56 5 8 0 232.48 13.92 6 -8 0 21.77 2.48 6 -8 0 -3.22 3.20 -6 -8 0 10.22 2.16 -6 8 0 15.34 2.10 6 8 0 9.50 2.57 -7 -8 0 4.44 2.02 7 -8 0 14.18 2.39 7 -8 0 2.67 3.74 -7 8 0 13.29 2.17 7 8 0 3.54 2.52 8 8 0 -1.37 2.30 8 -8 0 2.35 2.12 8 -8 0 2.50 3.75 -8 8 0 -1.38 1.49 -8 -8 0 -0.48 1.78 -9 8 0 17.95 2.56 9 8 0 17.17 3.65 9 -8 0 2.22 4.00 -9 -8 0 11.65 2.65 10 8 0 0.91 3.04 -10 8 0 6.28 2.07 -10 -8 0 4.06 2.34 10 -8 0 -2.81 3.77 11 -8 0 7.89 4.98 -11 -8 0 21.23 3.40 11 8 0 13.91 4.10 0 9 0 -1.31 1.18 0 -9 0 0.68 1.84 0 -9 0 1.06 1.13 1 -9 0 196.43 15.22 -1 -9 0 210.54 11.18 -1 9 0 195.62 11.57 -1 -9 0 202.42 14.59 1 9 0 201.24 11.67 1 -9 0 178.33 11.09 2 -9 0 -1.02 1.07 -2 -9 0 -1.27 0.99 2 -9 0 -3.09 2.26 -2 9 0 -1.27 1.10 2 9 0 -0.92 1.25 -2 -9 0 0.89 1.22 3 9 0 59.64 4.62 3 -9 0 57.15 4.28 -3 -9 0 64.21 4.27 -3 9 0 58.04 4.33 -4 9 0 14.06 2.02 -4 -9 0 16.76 2.21 4 9 0 19.61 2.58 4 -9 0 15.61 2.05 5 -9 0 0.15 3.14 -5 9 0 10.85 1.84 5 9 0 7.12 2.18 -5 -9 0 8.41 1.87 6 9 0 -0.82 2.06 6 -9 0 -0.03 3.18 -6 9 0 7.40 1.82 6 -9 0 6.87 1.96 7 -9 0 -0.20 3.67 7 -9 0 12.01 2.33 7 9 0 10.82 2.97 -7 9 0 11.58 2.07 -7 -9 0 7.77 2.25 8 9 0 7.51 2.99 8 -9 0 1.40 3.99 -8 -9 0 10.65 2.42 -8 9 0 13.15 2.20 9 9 0 29.86 4.37 -9 9 0 28.01 3.28 -9 -9 0 30.53 3.74 -10 9 0 22.30 2.98 10 9 0 24.19 4.42 -10 -9 0 21.96 3.50 10 -9 0 3.43 4.80 11 9 0 2.57 3.47 -11 -9 0 0.06 2.30 11 -9 0 3.99 4.60 0 -10 0 4.58 2.03 0 -10 0 2.66 1.20 0 10 0 2.06 1.30 1 -10 0 0.21 1.09 1 -10 0 -0.66 2.07 1 10 0 -0.60 1.23 -1 10 0 0.64 1.18 -1 -10 0 0.38 1.54 -1 -10 0 1.04 1.19 -2 10 0 34.13 3.16 2 10 0 33.72 3.27 -2 -10 0 33.04 3.08 2 -10 0 33.22 2.95 3 10 0 10.74 2.04 3 -10 0 8.47 1.69 3 -10 0 0.01 2.64 -3 10 0 7.97 1.66 -3 -10 0 11.89 1.81 4 10 0 23.28 3.05 -4 -10 0 24.98 2.80 -5 -10 0 7.50 2.09 5 10 0 7.40 2.39 5 -10 0 5.65 3.95 -6 10 0 58.47 4.76 6 -10 0 62.21 4.81 -6 -10 0 63.67 4.93 6 10 0 66.60 5.56 -7 -10 0 0.00 1.77 7 -10 0 -3.04 3.35 7 10 0 0.59 2.43 -7 10 0 3.57 1.73 -8 10 0 4.77 1.89 -8 -10 0 4.41 2.17 8 -10 0 -1.48 3.68 8 10 0 10.69 3.17 -9 10 0 9.96 2.15 9 10 0 5.49 3.14 9 -10 0 -0.58 4.15 -9 -10 0 7.96 2.52 -10 10 0 2.92 1.93 10 10 0 3.38 3.21 -10 -10 0 1.51 2.43 10 -10 0 3.68 4.50 11 -10 0 -2.33 4.27 11 10 0 3.69 3.56 -11 -10 0 4.06 2.58 0 -11 0 -4.11 2.08 0 11 0 -0.80 1.36 0 -11 0 -0.41 1.23 1 -11 0 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4 18.53 3.30 -5 10 -4 18.79 2.65 -6 10 4 36.01 3.27 6 10 -4 36.52 3.85 -6 -10 -4 33.81 3.54 6 10 -4 35.47 4.17 6 -10 -4 34.28 3.95 6 10 4 34.42 4.40 -6 10 -4 35.29 3.64 7 10 -4 3.91 2.30 -7 10 4 4.92 1.63 -7 -10 -4 6.75 2.15 7 10 -4 3.81 2.40 7 -10 4 -0.84 3.82 7 10 4 6.43 2.83 -7 10 -4 6.85 2.08 7 -10 -4 6.56 2.50 7 -10 -4 2.51 3.90 8 10 -4 12.00 2.99 -8 -10 -4 18.30 2.81 8 10 -4 13.76 3.19 8 -10 4 3.07 4.14 -8 10 -4 18.72 2.80 8 -10 -4 14.77 3.12 8 -10 -4 1.65 4.24 8 10 4 15.24 3.49 -9 -10 -4 19.58 3.04 9 10 -4 17.92 3.84 9 10 -4 12.57 3.28 9 10 4 17.53 4.09 -9 10 -4 20.05 3.05 9 -10 -4 9.93 3.21 9 -10 -4 2.88 4.88 -10 -10 -4 0.28 2.13 10 10 -4 -0.10 2.95 10 -10 4 0.04 4.28 -10 -10 4 2.29 2.54 10 -10 -4 -0.43 4.56 10 10 4 1.54 3.34 -10 10 -4 2.06 2.10 0 -11 -4 151.03 9.13 0 -11 -4 155.22 12.07 0 -11 4 145.21 8.73 0 11 4 153.26 9.42 0 -11 4 146.66 12.03 0 11 -4 160.69 9.46 -1 11 4 26.40 2.78 1 -11 4 24.93 2.43 1 -11 4 25.07 3.85 1 11 -4 24.00 2.88 -1 -11 -4 26.43 2.76 -1 -11 4 23.92 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25.35 4.29 -9 4 -9 31.71 3.76 10 4 -9 12.71 3.85 10 -4 9 2.28 4.17 -10 4 9 12.76 4.01 -10 4 -9 13.49 2.88 10 4 9 10.43 3.51 -10 -4 9 17.39 3.61 10 -4 -9 15.86 3.98 11 -4 9 1.10 4.24 11 4 -9 7.03 3.74 -11 4 9 8.14 3.83 11 4 9 6.74 3.67 -11 -4 9 3.87 2.87 -11 4 -9 8.52 2.67 11 -4 -9 7.53 3.76 0 5 9 0.71 1.46 0 -5 -9 1.05 1.32 0 5 -9 2.11 1.22 0 -5 9 1.78 1.69 0 5 9 1.48 1.21 0 5 -9 1.56 1.30 -1 5 9 59.86 4.00 -1 -5 -9 59.47 4.15 1 -5 9 55.39 5.87 1 5 -9 59.77 4.48 -1 5 9 62.82 5.55 1 5 -9 52.32 4.15 1 5 9 60.94 4.39 1 5 9 64.47 5.46 -1 5 -9 58.95 4.18 -1 -5 9 58.60 5.77 1 -5 -9 67.51 4.49 -1 5 -9 57.19 3.97 -2 5 9 59.90 5.28 -2 -5 -9 47.63 3.90 2 -5 9 60.67 5.77 -2 5 9 45.14 3.43 2 5 -9 54.81 3.90 2 5 -9 50.72 4.39 2 -5 -9 55.35 4.29 -2 5 -9 50.20 3.41 2 5 9 51.36 4.29 -2 -5 9 55.91 5.31 -2 5 -9 51.06 3.91 2 5 9 59.58 4.98 -3 -5 -9 1.76 1.26 -3 5 9 1.22 1.74 3 5 -9 2.57 1.23 3 5 -9 -0.85 1.72 3 -5 9 -0.78 1.80 3 -5 -9 -1.43 1.55 -3 5 -9 2.30 1.31 3 5 9 1.83 1.71 3 5 9 1.29 1.64 -3 -5 9 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2.33 1 3 22 2.94 3.16 -1 -3 22 -2.11 3.05 1 -3 -22 -1.59 2.37 -2 3 22 8.01 3.78 2 3 -22 6.94 2.90 2 -3 22 7.53 3.88 -2 -3 -22 6.91 2.70 -2 -3 22 8.25 3.68 2 -3 -22 9.08 3.16 2 3 22 6.59 3.74 -3 3 22 7.20 3.62 3 3 -22 2.84 2.69 3 -3 22 5.25 3.75 -3 -3 22 7.47 3.52 3 3 22 5.32 3.69 3 -3 -22 5.88 2.90 -3 3 -22 5.56 2.23 0 -4 22 -1.28 2.94 0 -4 -22 -0.16 2.31 0 4 22 -0.70 2.89 1 -4 22 17.17 4.66 -1 4 22 16.73 4.42 -1 -4 -22 14.94 3.21 1 -4 -22 14.55 3.33 1 4 22 15.12 4.19 -1 -4 22 12.49 4.21 -2 -4 -22 -1.86 2.02 -2 4 22 -0.78 2.91 2 4 -22 1.44 2.59 2 -4 22 -0.35 3.35 2 -4 -22 1.01 2.67 2 4 22 1.00 3.08 -2 -4 22 2.66 2.86 3 4 -22 -1.37 2.39 3 -4 22 0.63 3.53 -3 4 22 -1.55 3.12 3 -4 -22 -0.87 2.77 3 4 22 -0.45 3.13 -3 4 -22 -0.51 2.01 -3 -4 22 -0.60 2.70 0 -5 -22 -1.49 2.36 0 -5 22 -3.24 2.92 0 5 22 1.35 3.06 -1 5 22 11.63 4.04 1 -5 22 8.50 3.95 -1 -5 -22 9.77 2.89 1 -5 -22 11.65 3.22 1 5 22 12.74 3.92 -1 -5 22 7.27 3.49 2 -5 22 1.79 3.33 -2 5 22 1.74 3.30 -2 -5 -22 1.80 2.42 2 -5 -22 3.84 2.75 2 5 22 5.56 3.43 -2 -5 22 1.79 3.13 3 -5 22 15.52 4.98 -3 5 22 10.24 4.15 -3 -5 22 18.42 4.41 3 5 22 11.22 4.24 0 6 22 -0.89 2.91 0 -6 -22 -0.50 2.39 0 -6 22 0.58 3.14 -1 6 22 1.41 3.12 1 -6 22 0.88 3.23 -1 -6 -22 -0.34 2.40 1 -6 -22 0.85 2.50 1 6 22 0.72 3.16 -1 -6 22 0.98 2.96 -2 -6 -22 15.88 3.18 -2 6 22 11.67 4.14 2 -6 22 13.24 4.50 -2 -6 22 10.62 3.97 2 6 22 16.77 4.36 -2 6 -22 10.26 2.66 2 -6 -22 14.45 3.48 0 7 22 0.92 3.16 0 -7 22 1.37 3.06 0 -7 -22 1.00 2.61 -1 7 22 15.86 4.46 -1 -7 -22 17.36 3.40 1 -7 22 15.79 4.80 1 7 22 17.70 4.42 -1 -7 22 17.01 4.63 1 -7 -22 17.16 3.67 0 0 23 2.24 3.25 0 0 -23 -2.29 2.38 1 0 -23 4.99 2.84 1 0 23 4.37 3.64 -1 0 23 6.02 3.71 -2 0 23 1.88 3.26 2 0 23 -0.29 3.17 0 1 23 -0.82 3.22 0 -1 23 4.75 3.61 0 -1 -23 -1.50 2.51 1 1 -23 20.90 3.77 -1 1 23 14.95 4.58 1 -1 23 19.97 4.79 1 -1 -23 17.61 3.66 1 1 23 20.01 4.77 -1 -1 23 16.94 4.66 -2 1 23 -1.61 2.98 -2 -1 23 -1.30 3.01 0 2 23 5.52 3.61 0 -2 23 5.31 3.62 0 -2 -23 4.49 2.85 -1 2 23 16.52 4.75 -1 -2 -23 18.49 3.41 1 -2 23 18.68 4.71 1 -2 -23 15.58 3.56 -1 -2 23 19.65 4.82 1 2 23 15.02 4.41 0 3 23 8.19 3.87 0 -3 -23 8.78 3.01 0 -3 23 5.83 3.74 -1 3 23 1.33 3.25 1 -3 23 -1.24 3.09 -1 -3 23 1.52 3.27 1 3 23 2.38 3.15 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 54527 #===END data_K6Ph2PPrPDIMoH _chemical_name_systematic ? _chemical_name_common 'K6Ph2PPrPDIMoH' _chemical_formula_moiety '2(C39 H41 Mo N3 P2), C7 H7' _chemical_formula_sum 'C85 H89 Mo2 N6 P4' _chemical_formula_iupac ? _chemical_formula_weight 1510.38 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3197(12) _cell_length_b 13.0922(15) _cell_length_c 14.2479(17) _cell_angle_alpha 81.129(4) _cell_angle_beta 82.476(3) _cell_angle_gamma 76.341(3) _cell_volume 1839.2(4) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3985 _cell_measurement_theta_min 2.3061 _cell_measurement_theta_max 23.5586 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour 'clear dark brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 785 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.72 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'Bruker Kappa APEX II Duo' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II Duo' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 19605 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.26 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_max 0.930 _diffrn_measured_fraction_theta_full 0.930 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _refine_special_details ; ; _reflns_number_total 6213 _reflns_number_gt 4261 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_gt 0.1536 _refine_ls_wR_factor_ref 0.1734 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 11.227 _refine_ls_number_reflns 6213 _refine_ls_number_parameters 425 _refine_ls_number_restraints 13 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+20.1603P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.628 _refine_diff_density_min -1.324 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' N N 0.0061 0.0033 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-2013 (Sheldrick, 2013)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo1 0.32123(6) 0.66798(5) 0.69820(5) 0.0188(2) Uani d . . . 1.0 . . P P1 0.37785(18) 0.49357(15) 0.79263(15) 0.0186(5) Uani d . . . 1.0 . . P P2 0.37068(18) 0.83618(15) 0.62281(16) 0.0211(5) Uani d . . D 1.0 . . N N1 0.2032(6) 0.7123(5) 0.8091(5) 0.0216(15) Uani d . . . 1.0 . . N N2 0.1301(5) 0.6563(4) 0.6785(4) 0.0159(14) Uani d . . . 1.0 . . N N3 0.3274(6) 0.6355(5) 0.5562(4) 0.0186(14) Uani d . . . 1.0 . . C C1 0.0045(8) 0.7139(7) 0.9295(6) 0.034(2) Uani d . . . 1.0 . . H H1A 0.0074 0.644 0.9665 0.051 Uiso calc U . R 1.0 . . H H1B -0.0889 0.7504 0.9225 0.051 Uiso calc U . R 1.0 . . H H1C 0.0466 0.7558 0.9628 0.051 Uiso calc U . R 1.0 . . C C2 0.0784(8) 0.7012(6) 0.8331(6) 0.0223(18) Uani d . . . 1.0 . . C C3 0.0296(7) 0.6717(6) 0.7560(6) 0.0206(17) Uani d . . . 1.0 . . C C4 -0.0974(7) 0.6555(6) 0.7469(6) 0.027(2) Uani d . . . 1.0 . . H H4 -0.166 0.6648 0.7983 0.032 Uiso calc U . R 1.0 . . C C5 -0.1228(7) 0.6262(6) 0.6638(6) 0.0248(19) Uani d . . . 1.0 . . H H5 -0.2091 0.6148 0.6589 0.03 Uiso calc U . R 1.0 . . C C6 -0.0269(7) 0.6128(6) 0.5875(6) 0.0242(19) Uani d . . . 1.0 . . H H6 -0.0467 0.5925 0.5307 0.029 Uiso calc U . R 1.0 . . C C7 0.1025(7) 0.6297(5) 0.5946(6) 0.0189(17) Uani d . . . 1.0 . . C C8 0.2132(7) 0.6216(6) 0.5247(6) 0.0211(18) Uani d . . . 1.0 . . C C9 0.2055(8) 0.6020(7) 0.4253(6) 0.029(2) Uani d . . . 1.0 . . H H9A 0.2357 0.6579 0.3798 0.044 Uiso calc U . R 1.0 . . H H9B 0.1128 0.6022 0.4168 0.044 Uiso calc U . R 1.0 . . H H9C 0.2632 0.5331 0.414 0.044 Uiso calc U . R 1.0 . . C C10 0.3234(7) 0.7081(6) 0.8465(6) 0.0249(19) Uani d . . . 1.0 . . H H10 0.3444 0.7782 0.8498 0.03 Uiso calc U . R 1.0 . . C C11 0.3644(8) 0.6212(7) 0.9299(6) 0.030(2) Uani d . . . 1.0 . . H H11A 0.4622 0.6084 0.9334 0.036 Uiso calc U . R 1.0 . . H H11B 0.3184 0.6452 0.9907 0.036 Uiso calc U . R 1.0 . . C C12 0.3278(7) 0.5181(6) 0.9167(6) 0.0240(18) Uani d . . . 1.0 . . H H12A 0.2301 0.5241 0.9316 0.029 Uiso calc U . R 1.0 . . H H12B 0.3747 0.4586 0.9604 0.029 Uiso calc U . R 1.0 . . C C13 0.5501(7) 0.4164(6) 0.8010(5) 0.0202(17) Uani d . . . 1.0 . . C C14 0.6530(7) 0.4688(6) 0.8032(6) 0.0229(18) Uani d . . . 1.0 . . H H14 0.6344 0.544 0.7943 0.027 Uiso calc U . R 1.0 . . C C15 0.7810(7) 0.4126(7) 0.8181(6) 0.027(2) Uani d . . . 1.0 . . H H15 0.8491 0.4499 0.8197 0.032 Uiso calc U . R 1.0 . . C C16 0.8119(7) 0.3037(7) 0.8308(6) 0.028(2) Uani d . . . 1.0 . . H H16 0.9001 0.2654 0.8418 0.034 Uiso calc U . R 1.0 . . C C17 0.7122(8) 0.2515(7) 0.8270(7) 0.038(2) Uani d . . . 1.0 . . H H17 0.7325 0.1762 0.8346 0.045 Uiso calc U . R 1.0 . . C C18 0.5815(7) 0.3067(6) 0.8123(7) 0.031(2) Uani d . . . 1.0 . . H H18 0.5141 0.269 0.81 0.037 Uiso calc U . R 1.0 . . C C19 0.2868(7) 0.3937(6) 0.7757(5) 0.0184(17) Uani d . . . 1.0 . . C C20 0.2412(7) 0.3258(6) 0.8510(6) 0.0252(19) Uani d . . . 1.0 . . H H20 0.2556 0.3299 0.9147 0.03 Uiso calc U . R 1.0 . . C C21 0.1738(7) 0.2514(7) 0.8320(6) 0.029(2) Uani d . . . 1.0 . . H H21 0.1403 0.2059 0.8831 0.035 Uiso calc U . R 1.0 . . C C22 0.1559(7) 0.2438(6) 0.7396(6) 0.028(2) Uani d . . . 1.0 . . H H22 0.1115 0.192 0.7276 0.033 Uiso calc U . R 1.0 . . C C23 0.2012(7) 0.3100(6) 0.6642(6) 0.0235(18) Uani d . . . 1.0 . . H H23 0.1886 0.3044 0.6005 0.028 Uiso calc U . R 1.0 . . C C24 0.2668(6) 0.3863(6) 0.6840(6) 0.0190(17) Uani d . . . 1.0 . . H H24 0.2977 0.4332 0.6329 0.023 Uiso calc U . R 1.0 . . C C25 0.4400(8) 0.6423(6) 0.4827(6) 0.027(2) Uani d . . . 1.0 . . H H25A 0.434 0.6022 0.4305 0.033 Uiso calc U . R 1.0 . . H H25B 0.5254 0.6098 0.5107 0.033 Uiso calc U . R 1.0 . . C C26 0.4386(7) 0.7591(6) 0.4419(6) 0.0250(19) Uani d . . . 1.0 . . H H26A 0.5006 0.7605 0.3827 0.03 Uiso calc U . R 1.0 . . H H26B 0.3474 0.7943 0.4245 0.03 Uiso calc U . R 1.0 . . C C27 0.4791(7) 0.8226(6) 0.5111(6) 0.0235(18) Uani d . . . 1.0 . . H H27A 0.4813 0.8944 0.4778 0.028 Uiso calc U . R 1.0 . . H H27B 0.5713 0.7881 0.5268 0.028 Uiso calc U . R 1.0 . . C C28 0.4606(5) 0.9057(4) 0.6861(4) 0.0247(19) Uani d . P DG 0.61(3) A -1 C C29 0.5903(5) 0.8553(4) 0.7074(4) 0.030(2) Uani d . P DG 0.61(3) A -1 H H29A 0.6271 0.7856 0.6919 0.036 Uiso calc U P R 0.61(3) A -1 C C30 0.6668(4) 0.9055(5) 0.7510(7) 0.0369(19) Uani d . P DG 0.61(3) A -1 H H30A 0.7551 0.8702 0.7646 0.044 Uiso calc U P R 0.61(3) A -1 C C31 0.6136(7) 1.0075(8) 0.7747(12) 0.045(4) Uani d . P DG 0.61(3) A -1 H H31A 0.6644 1.0414 0.806 0.054 Uiso calc U P R 0.61(3) A -1 C C32 0.4844(8) 1.0596(9) 0.7518(14) 0.0369(19) Uani d . P DG 0.61(3) A -1 H H32A 0.4479 1.1296 0.7664 0.044 Uiso calc U P R 0.61(3) A -1 C C33 0.4106(5) 1.0094(7) 0.7082(10) 0.0369(19) Uani d . P DG 0.61(3) A -1 H H33A 0.3235 1.0459 0.6926 0.044 Uiso calc U P R 0.61(3) A -1 C C28' 0.4646(5) 0.8960(5) 0.6920(4) 0.0247(19) Uani d . P DG 0.39(3) A -2 C C29' 0.5976(5) 0.8496(4) 0.7079(4) 0.030(2) Uani d . P DG 0.39(3) A -2 H H29B 0.6421 0.7881 0.6793 0.036 Uiso calc U P R 0.39(3) A -2 C C30' 0.6661(4) 0.8918(6) 0.7649(6) 0.0369(19) Uani d . P DG 0.39(3) A -2 H H30B 0.7567 0.8595 0.7746 0.044 Uiso calc U P R 0.39(3) A -2 C C31' 0.6016(6) 0.9816(10) 0.8077(10) 0.045(4) Uani d . P DG 0.39(3) A -2 H H31B 0.6471 1.0096 0.8481 0.054 Uiso calc U P R 0.39(3) A -2 C C32' 0.4690(7) 1.0300(12) 0.7906(12) 0.0369(19) Uani d . P DG 0.39(3) A -2 H H32B 0.4247 1.0921 0.8185 0.044 Uiso calc U P R 0.39(3) A -2 C C33' 0.4030(4) 0.9880(9) 0.7338(9) 0.0369(19) Uani d . P DG 0.39(3) A -2 H H33B 0.3134 1.022 0.7224 0.044 Uiso calc U P R 0.39(3) A -2 C C34 0.2279(7) 0.9430(6) 0.5920(6) 0.0245(19) Uani d . . . 1.0 . . C C35 0.2352(8) 1.0262(6) 0.5190(7) 0.030(2) Uani d . . . 1.0 . . H H35 0.3171 1.0261 0.4798 0.036 Uiso calc U . R 1.0 . . C C36 0.1256(8) 1.1090(7) 0.5021(7) 0.032(2) Uani d . . . 1.0 . . H H36 0.1322 1.1638 0.4508 0.039 Uiso calc U . R 1.0 . . C C37 0.0062(9) 1.1116(7) 0.5606(6) 0.033(2) Uani d . . . 1.0 . . H H37 -0.0682 1.1695 0.5511 0.04 Uiso calc U . R 1.0 . . C C38 -0.0035(8) 1.0282(7) 0.6335(6) 0.031(2) Uani d . . . 1.0 . . H H38 -0.0854 1.0286 0.6728 0.037 Uiso calc U . R 1.0 . . C C39 0.1060(7) 0.9449(6) 0.6486(6) 0.0264(19) Uani d . . . 1.0 . . H H39 0.0981 0.8883 0.6979 0.032 Uiso calc U . R 1.0 . . C C40 0.8603(11) 0.0124(8) 1.0063(8) 0.052(3) Uani d . . . 1.0 . . C C41 0.9423(12) -0.0083(8) 0.9218(8) 0.056(3) Uani d . . . 1.0 . . H H41 0.9016 -0.0147 0.8675 0.068 Uiso calc U . R 1.0 . . C C42 1.0810(9) -0.0199(8) 0.9139(8) 0.047(3) Uani d . . . 1.0 . . H H42 1.1337 -0.0327 0.8553 0.057 Uiso calc U . R 1.0 . . C C43 0.7005(19) 0.0253(19) 1.0208(15) 0.058(6) Uani d . P . 0.5 . . H H43A 0.6572 0.0955 0.991 0.086 Uiso calc U P R 0.5 . . H H43B 0.6705 0.0175 1.0892 0.086 Uiso calc U P R 0.5 . . H H43C 0.6762 -0.0294 0.9911 0.086 Uiso calc U P R 0.5 . . H H1M 0.495(8) 0.653(6) 0.693(6) 0.04 Uiso d U . . 1.0 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.0107(3) 0.0116(4) 0.0366(4) -0.0029(3) -0.0069(3) -0.0059(3) P1 0.0108(9) 0.0143(11) 0.0326(13) -0.0031(8) -0.0064(8) -0.0042(9) P2 0.0142(10) 0.0125(11) 0.0398(13) -0.0064(8) -0.0081(9) -0.0037(9) N1 0.012(3) 0.012(3) 0.041(4) 0.002(3) -0.008(3) -0.006(3) N2 0.013(3) 0.003(3) 0.028(4) 0.002(2) 0.000(3) 0.000(3) N3 0.012(3) 0.011(3) 0.029(4) -0.003(3) 0.005(3) 0.002(3) C1 0.032(5) 0.034(5) 0.038(6) -0.011(4) 0.000(4) -0.010(4) C2 0.027(4) 0.012(4) 0.028(5) -0.007(3) -0.001(3) 0.000(3) C3 0.015(4) 0.010(4) 0.037(5) -0.002(3) -0.002(3) -0.003(3) C4 0.015(4) 0.017(5) 0.048(6) -0.003(3) -0.002(4) -0.003(4) C5 0.014(4) 0.018(4) 0.044(5) -0.005(3) -0.004(4) -0.005(4) C6 0.020(4) 0.013(4) 0.040(5) -0.003(3) -0.007(4) -0.002(4) C7 0.015(4) 0.003(4) 0.039(5) 0.001(3) -0.007(3) -0.002(3) C8 0.022(4) 0.008(4) 0.032(5) -0.003(3) -0.009(3) 0.003(3) C9 0.027(4) 0.028(5) 0.037(5) -0.013(4) -0.005(4) -0.006(4) C10 0.015(4) 0.014(4) 0.041(5) 0.007(3) -0.009(4) -0.002(4) C11 0.033(5) 0.029(5) 0.030(5) -0.010(4) -0.004(4) -0.008(4) C12 0.019(4) 0.024(5) 0.031(5) -0.005(4) -0.005(3) -0.005(4) C13 0.017(4) 0.024(5) 0.021(4) -0.006(3) -0.003(3) -0.006(3) C14 0.021(4) 0.018(4) 0.031(5) -0.007(3) -0.007(3) 0.002(4) C15 0.014(4) 0.036(5) 0.032(5) -0.011(4) -0.004(3) 0.000(4) C16 0.009(4) 0.036(6) 0.038(5) 0.001(4) -0.004(3) -0.005(4) C17 0.029(5) 0.019(5) 0.065(7) -0.002(4) -0.011(4) -0.006(4) C18 0.013(4) 0.011(4) 0.070(7) -0.001(3) -0.012(4) -0.009(4) C19 0.012(4) 0.018(4) 0.025(5) -0.001(3) -0.005(3) 0.000(3) C20 0.014(4) 0.025(5) 0.036(5) -0.004(3) -0.001(3) -0.005(4) C21 0.018(4) 0.026(5) 0.044(6) -0.010(4) 0.002(4) -0.001(4) C22 0.006(4) 0.023(5) 0.053(6) -0.001(3) -0.002(4) -0.005(4) C23 0.015(4) 0.017(4) 0.041(5) -0.001(3) -0.007(3) -0.011(4) C24 0.008(3) 0.010(4) 0.037(5) 0.004(3) -0.003(3) -0.004(3) C25 0.026(4) 0.021(5) 0.039(5) -0.014(4) -0.001(4) -0.003(4) C26 0.014(4) 0.016(4) 0.046(5) -0.006(3) -0.002(4) -0.004(4) C27 0.021(4) 0.015(4) 0.036(5) -0.006(3) -0.009(4) 0.000(4) C28 0.018(4) 0.010(4) 0.048(6) -0.006(3) -0.009(4) -0.001(4) C29 0.016(4) 0.012(4) 0.061(6) 0.005(3) -0.014(4) -0.009(4) C30 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C31 0.035(6) 0.012(7) 0.098(13) -0.015(5) -0.032(7) -0.001(8) C32 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C33 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C28' 0.018(4) 0.010(4) 0.048(6) -0.006(3) -0.009(4) -0.001(4) C29' 0.016(4) 0.012(4) 0.061(6) 0.005(3) -0.014(4) -0.009(4) C30' 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C31' 0.035(6) 0.012(7) 0.098(13) -0.015(5) -0.032(7) -0.001(8) C32' 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C33' 0.021(3) 0.002(3) 0.090(6) 0.001(2) -0.024(3) -0.004(3) C34 0.018(4) 0.018(5) 0.042(5) -0.012(3) -0.007(4) -0.004(4) C35 0.017(4) 0.013(4) 0.064(6) -0.007(4) -0.012(4) -0.003(4) C36 0.025(5) 0.020(5) 0.052(6) -0.008(4) -0.011(4) 0.002(4) C37 0.035(5) 0.019(5) 0.051(6) -0.004(4) -0.020(4) -0.007(4) C38 0.016(4) 0.026(5) 0.052(6) -0.001(4) -0.009(4) -0.008(4) C39 0.017(4) 0.017(4) 0.048(6) -0.007(4) -0.009(4) -0.003(4) C40 0.066(7) 0.037(6) 0.059(8) -0.013(5) -0.030(6) -0.002(5) C41 0.076(8) 0.042(7) 0.059(8) -0.011(6) -0.041(7) -0.005(6) C42 0.035(6) 0.041(6) 0.060(7) 0.009(5) -0.014(5) -0.009(5) C43 0.046(12) 0.079(18) 0.051(14) -0.018(12) -0.011(10) -0.008(12) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 N1 . 1.940(7) ? Mo1 N2 . 2.072(5) ? Mo1 N3 . 2.121(6) ? Mo1 C10 . 2.259(8) ? Mo1 P2 . 2.433(2) ? Mo1 P1 . 2.448(2) ? Mo1 H1M . 1.75(8) ? P1 C12 . 1.831(8) ? P1 C13 . 1.834(8) ? P1 C19 . 1.840(7) ? P2 C34 . 1.824(8) ? P2 C27 . 1.829(8) ? P2 C28' . 1.837(4) ? P2 C28 . 1.837(4) ? N1 C2 . 1.324(9) ? N1 C10 . 1.399(9) ? N2 C7 . 1.377(9) ? N2 C3 . 1.417(9) ? N3 C8 . 1.374(9) ? N3 C25 . 1.469(9) ? C1 C2 . 1.495(11) ? C1 H1A . 0.98 ? C1 H1B . 0.98 ? C1 H1C . 0.98 ? C2 C3 . 1.406(10) ? C3 C4 . 1.401(10) ? C4 C5 . 1.374(11) ? C4 H4 . 0.95 ? C5 C6 . 1.373(11) ? C5 H5 . 0.95 ? C6 C7 . 1.423(9) ? C6 H6 . 0.95 ? C7 C8 . 1.408(11) ? C8 C9 . 1.493(11) ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 C11 . 1.541(11) ? C10 H10 . 1.0 ? C11 C12 . 1.529(10) ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C13 C18 . 1.384(11) ? C13 C14 . 1.399(10) ? C14 C15 . 1.377(11) ? C14 H14 . 0.95 ? C15 C16 . 1.374(11) ? C15 H15 . 0.95 ? C16 C17 . 1.374(11) ? C16 H16 . 0.95 ? C17 C18 . 1.398(11) ? C17 H17 . 0.95 ? C18 H18 . 0.95 ? C19 C24 . 1.370(10) ? C19 C20 . 1.391(10) ? C20 C21 . 1.399(10) ? C20 H20 . 0.95 ? C21 C22 . 1.374(11) ? C21 H21 . 0.95 ? C22 C23 . 1.377(11) ? C22 H22 . 0.95 ? C23 C24 . 1.412(10) ? C23 H23 . 0.95 ? C24 H24 . 0.95 ? C25 C26 . 1.547(10) ? C25 H25A . 0.99 ? C25 H25B . 0.99 ? C26 C27 . 1.538(10) ? C26 H26A . 0.99 ? C26 H26B . 0.99 ? C27 H27A . 0.99 ? C27 H27B . 0.99 ? C28 C29 . 1.3955 ? C28 C33 . 1.4026 ? C29 C30 . 1.3928 ? C29 H29A . 0.95 ? C30 C31 . 1.3935 ? C30 H30A . 0.95 ? C31 C32 . 1.4019 ? C31 H31A . 0.95 ? C32 C33 . 1.3715 ? C32 H32A . 0.95 ? C33 H33A . 0.95 ? C28' C29' . 1.3955 ? C28' C33' . 1.4025 ? C29' C30' . 1.3928 ? C29' H29B . 0.95 ? C30' C31' . 1.3933 ? C30' H30B . 0.95 ? C31' C32' . 1.4019 ? C31' H31B . 0.95 ? C32' C33' . 1.3715 ? C32' H32B . 0.95 ? C33' H33B . 0.95 ? C34 C35 . 1.394(11) ? C34 C39 . 1.400(11) ? C35 C36 . 1.387(11) ? C35 H35 . 0.95 ? C36 C37 . 1.391(12) ? C36 H36 . 0.95 ? C37 C38 . 1.398(12) ? C37 H37 . 0.95 ? C38 C39 . 1.386(11) ? C38 H38 . 0.95 ? C39 H39 . 0.95 ? C40 C42 2_757 1.382(13) ? C40 C41 . 1.402(15) ? C40 C43 . 1.61(2) ? C41 C42 . 1.395(14) ? C41 H41 . 0.95 ? C42 C40 2_757 1.382(13) ? C42 H42 . 0.95 ? C43 H43A . 0.98 ? C43 H43B . 0.98 ? C43 H43C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Mo1 N2 . . 72.4(2) ? N1 Mo1 N3 . . 144.3(2) ? N2 Mo1 N3 . . 72.9(2) ? N1 Mo1 C10 . . 38.0(2) ? N2 Mo1 C10 . . 109.8(3) ? N3 Mo1 C10 . . 176.8(3) ? N1 Mo1 P2 . . 100.84(19) ? N2 Mo1 P2 . . 112.10(16) ? N3 Mo1 P2 . . 84.56(16) ? C10 Mo1 P2 . . 92.7(2) ? N1 Mo1 P1 . . 86.41(19) ? N2 Mo1 P1 . . 94.98(16) ? N3 Mo1 P1 . . 104.79(17) ? C10 Mo1 P1 . . 77.0(2) ? P2 Mo1 P1 . . 152.91(7) ? N1 Mo1 H1M . . 122.(3) ? N2 Mo1 H1M . . 165.(3) ? N3 Mo1 H1M . . 94.(3) ? C10 Mo1 H1M . . 84.(3) ? P2 Mo1 H1M . . 73.(3) ? P1 Mo1 H1M . . 81.(3) ? C12 P1 C13 . . 101.0(3) ? C12 P1 C19 . . 104.5(3) ? C13 P1 C19 . . 103.0(3) ? C12 P1 Mo1 . . 104.9(3) ? C13 P1 Mo1 . . 123.5(3) ? C19 P1 Mo1 . . 117.3(2) ? C34 P2 C27 . . 104.9(4) ? C34 P2 C28' . . 103.9(3) ? C27 P2 C28' . . 102.6(3) ? C34 P2 C28 . . 100.2(3) ? C27 P2 C28 . . 101.5(3) ? C34 P2 Mo1 . . 116.8(2) ? C27 P2 Mo1 . . 112.1(3) ? C28' P2 Mo1 . . 115.1(2) ? C28 P2 Mo1 . . 119.3(2) ? C2 N1 C10 . . 143.2(7) ? C2 N1 Mo1 . . 127.5(5) ? C10 N1 Mo1 . . 83.5(4) ? C7 N2 C3 . . 120.8(6) ? C7 N2 Mo1 . . 121.4(5) ? C3 N2 Mo1 . . 117.8(5) ? C8 N3 C25 . . 115.7(6) ? C8 N3 Mo1 . . 119.2(5) ? C25 N3 Mo1 . . 124.5(5) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? N1 C2 C3 . . 109.9(7) ? N1 C2 C1 . . 124.3(7) ? C3 C2 C1 . . 125.8(7) ? C4 C3 C2 . . 130.2(7) ? C4 C3 N2 . . 118.7(7) ? C2 C3 N2 . . 111.2(6) ? C5 C4 C3 . . 120.1(8) ? C5 C4 H4 . . 120.0 ? C3 C4 H4 . . 120.0 ? C6 C5 C4 . . 121.9(7) ? C6 C5 H5 . . 119.1 ? C4 C5 H5 . . 119.1 ? C5 C6 C7 . . 119.2(7) ? C5 C6 H6 . . 120.4 ? C7 C6 H6 . . 120.4 ? N2 C7 C8 . . 112.6(6) ? N2 C7 C6 . . 119.4(7) ? C8 C7 C6 . . 127.9(7) ? N3 C8 C7 . . 113.7(7) ? N3 C8 C9 . . 123.4(7) ? C7 C8 C9 . . 122.9(6) ? C8 C9 H9A . . 109.5 ? C8 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C8 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? N1 C10 C11 . . 117.6(7) ? N1 C10 Mo1 . . 58.5(4) ? C11 C10 Mo1 . . 121.4(5) ? N1 C10 H10 . . 115.7 ? C11 C10 H10 . . 115.7 ? Mo1 C10 H10 . . 115.7 ? C12 C11 C10 . . 110.8(6) ? C12 C11 H11A . . 109.5 ? C10 C11 H11A . . 109.5 ? C12 C11 H11B . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 108.1 ? C11 C12 P1 . . 108.5(5) ? C11 C12 H12A . . 110.0 ? P1 C12 H12A . . 110.0 ? C11 C12 H12B . . 110.0 ? P1 C12 H12B . . 110.0 ? H12A C12 H12B . . 108.4 ? C18 C13 C14 . . 118.0(7) ? C18 C13 P1 . . 122.3(5) ? C14 C13 P1 . . 119.6(6) ? C15 C14 C13 . . 120.9(8) ? C15 C14 H14 . . 119.6 ? C13 C14 H14 . . 119.6 ? C16 C15 C14 . . 121.2(7) ? C16 C15 H15 . . 119.4 ? C14 C15 H15 . . 119.4 ? C17 C16 C15 . . 118.4(7) ? C17 C16 H16 . . 120.8 ? C15 C16 H16 . . 120.8 ? C16 C17 C18 . . 121.4(8) ? C16 C17 H17 . . 119.3 ? C18 C17 H17 . . 119.3 ? C13 C18 C17 . . 120.1(7) ? C13 C18 H18 . . 120.0 ? C17 C18 H18 . . 120.0 ? C24 C19 C20 . . 119.9(7) ? C24 C19 P1 . . 117.3(5) ? C20 C19 P1 . . 122.8(6) ? C19 C20 C21 . . 119.3(8) ? C19 C20 H20 . . 120.4 ? C21 C20 H20 . . 120.4 ? C22 C21 C20 . . 120.3(8) ? C22 C21 H21 . . 119.9 ? C20 C21 H21 . . 119.9 ? C21 C22 C23 . . 121.2(7) ? C21 C22 H22 . . 119.4 ? C23 C22 H22 . . 119.4 ? C22 C23 C24 . . 118.3(8) ? C22 C23 H23 . . 120.8 ? C24 C23 H23 . . 120.8 ? C19 C24 C23 . . 121.1(7) ? C19 C24 H24 . . 119.4 ? C23 C24 H24 . . 119.4 ? N3 C25 C26 . . 110.8(7) ? N3 C25 H25A . . 109.5 ? C26 C25 H25A . . 109.5 ? N3 C25 H25B . . 109.5 ? C26 C25 H25B . . 109.5 ? H25A C25 H25B . . 108.1 ? C27 C26 C25 . . 113.9(7) ? C27 C26 H26A . . 108.8 ? C25 C26 H26A . . 108.8 ? C27 C26 H26B . . 108.8 ? C25 C26 H26B . . 108.8 ? H26A C26 H26B . . 107.7 ? C26 C27 P2 . . 115.7(5) ? C26 C27 H27A . . 108.3 ? P2 C27 H27A . . 108.3 ? C26 C27 H27B . . 108.3 ? P2 C27 H27B . . 108.3 ? H27A C27 H27B . . 107.4 ? C29 C28 C33 . . 117.9 ? C29 C28 P2 . . 118.0(3) ? C33 C28 P2 . . 124.0(2) ? C30 C29 C28 . . 121.1 ? C30 C29 H29A . . 119.5 ? C28 C29 H29A . . 119.5 ? C29 C30 C31 . . 120.0 ? C29 C30 H30A . . 120.0 ? C31 C30 H30A . . 120.0 ? C30 C31 C32 . . 119.3 ? C30 C31 H31A . . 120.4 ? C32 C31 H31A . . 120.4 ? C33 C32 C31 . . 120.1 ? C33 C32 H32A . . 120.0 ? C31 C32 H32A . . 120.0 ? C32 C33 C28 . . 121.6 ? C32 C33 H33A . . 119.2 ? C28 C33 H33A . . 119.2 ? C29' C28' C33' . . 117.9 ? C29' C28' P2 . . 121.3(3) ? C33' C28' P2 . . 120.8(3) ? C30' C29' C28' . . 121.1 ? C30' C29' H29B . . 119.5 ? C28' C29' H29B . . 119.5 ? C29' C30' C31' . . 120.0 ? C29' C30' H30B . . 120.0 ? C31' C30' H30B . . 120.0 ? C30' C31' C32' . . 119.3 ? C30' C31' H31B . . 120.4 ? C32' C31' H31B . . 120.4 ? C33' C32' C31' . . 120.1 ? C33' C32' H32B . . 120.0 ? C31' C32' H32B . . 120.0 ? C32' C33' C28' . . 121.7 ? C32' C33' H33B . . 119.2 ? C28' C33' H33B . . 119.2 ? C35 C34 C39 . . 118.1(7) ? C35 C34 P2 . . 123.8(6) ? C39 C34 P2 . . 118.0(6) ? C36 C35 C34 . . 121.6(8) ? C36 C35 H35 . . 119.2 ? C34 C35 H35 . . 119.2 ? C35 C36 C37 . . 119.8(8) ? C35 C36 H36 . . 120.1 ? C37 C36 H36 . . 120.1 ? C36 C37 C38 . . 119.4(8) ? C36 C37 H37 . . 120.3 ? C38 C37 H37 . . 120.3 ? C39 C38 C37 . . 120.2(8) ? C39 C38 H38 . . 119.9 ? C37 C38 H38 . . 119.9 ? C38 C39 C34 . . 120.9(8) ? C38 C39 H39 . . 119.6 ? C34 C39 H39 . . 119.6 ? C42 C40 C41 2_757 . 118.9(10) ? C42 C40 C43 2_757 . 115.6(12) ? C41 C40 C43 . . 125.5(11) ? C42 C41 C40 . . 122.8(9) ? C42 C41 H41 . . 118.6 ? C40 C41 H41 . . 118.6 ? C40 C42 C41 2_757 . 118.3(10) ? C40 C42 H42 2_757 . 120.9 ? C41 C42 H42 . . 120.9 ? C40 C43 H43A . . 109.5 ? C40 C43 H43B . . 109.5 ? H43A C43 H43B . . 109.5 ? C40 C43 H43C . . 109.5 ? H43A C43 H43C . . 109.5 ? H43B C43 H43C . . 109.5 ? # start Validation Reply Form _vrf_PLAT029_K6Ph2PPrPDIMoH ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.930 Note RESPONSE: Data collection strategy failed to adequately cover reciprocal lattice. ; _vrf_PLAT213_K6Ph2PPrPDIMoH ; PROBLEM: Atom C30 has ADP max/min Ratio ..... 7.1 prolat RESPONSE: Atom is part of disordered phenyl ring. ; _vrf_PLAT250_K6Ph2PPrPDIMoH ; PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.4 Note RESPONSE: Data quality is marginal and weak. Possible whole molecule disorder. ; _vrf_PLAT342_K6Ph2PPrPDIMoH ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0120 Ang. RESPONSE: Data quality is marginal and weak. ; _vrf_PLAT906_K6Ph2PPrPDIMoH ; PROBLEM: Large K value in the Analysis of Variance ...... 2.073 Check RESPONSE: K value for the weakest reflections showed the largest effect of a fixed box size integration necessary for the poor spot shape correlation during integration. ; _vrf_PLAT911_K6Ph2PPrPDIMoH ; PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 455 Report RESPONSE: Data collection strategy failed to adequately cover reciprocal lattice. ; _vrf_PLAT971_K6Ph2PPrPDIMoH ; PROBLEM: Check Calcd Residual Density 1.19A From Mo1 2.77 eA-3 RESPONSE: Peaks are due to ellipsoidal modeling of Mo electron density, which would probably be more accurately modeled using a multipole strategy. ; # end Validation Reply Form _shelx_res_file ; TITL P-1 in P-1 CELL 0.71073 10.31970 13.09220 14.24790 81.1294 82.4759 76.3405 ZERR 1.00 0.00120 0.00150 0.00170 0.0035 0.0033 0.0034 LATT 1 SFAC C H N P Mo UNIT 85 89 6 4 2 L.S. 20 ACTA BOND $H FMAP 2 PLAN 10 SADI 0.0001 C33 C28 C33' C28' SADI 0.0001 C32 C33 C32' C33' SADI 0.0001 C31 C32 C31' C32' SADI 0.0001 C30 C31 C30' C31' SADI 0.0001 C29 C30 C29' C30' SADI 0.0001 C28 C29 C28' C29' SADI 0.0001 P2 C28 P2 C28' EADP C28 C28' EADP C29 C29' EADP C30 C30' C32 C32' C33 C33' EADP C31 C31' rem EADP C32 C32' rem EADP C33 C33' FLAT 0.0001 C28 C29 C30 C31 C32 C33 FLAT 0.0001 C28' C29' C30' C31' C32' C33' TEMP -173.150 WGHT 0.016400 20.160299 FVAR 0.13861 0.60757 MO1 5 0.321229 0.667982 0.698202 11.00000 0.01072 0.01158 = 0.03660 -0.00586 -0.00687 -0.00291 P1 4 0.377851 0.493572 0.792628 11.00000 0.01077 0.01433 = 0.03257 -0.00423 -0.00637 -0.00310 P2 4 0.370683 0.836178 0.622815 11.00000 0.01422 0.01255 = 0.03981 -0.00370 -0.00811 -0.00635 N1 3 0.203240 0.712280 0.809132 11.00000 0.01202 0.01168 = 0.04119 -0.00569 -0.00845 0.00180 N2 3 0.130132 0.656305 0.678491 11.00000 0.01269 0.00338 = 0.02850 -0.00032 -0.00035 0.00232 N3 3 0.327354 0.635482 0.556214 11.00000 0.01237 0.01064 = 0.02931 0.00236 0.00482 -0.00278 C1 1 0.004527 0.713950 0.929528 11.00000 0.03224 0.03441 = 0.03810 -0.00997 0.00037 -0.01121 AFIX 137 H1A 2 0.007379 0.643987 0.966548 11.00000 -1.50000 H1B 2 -0.088901 0.750370 0.922499 11.00000 -1.50000 H1C 2 0.046644 0.755820 0.962779 11.00000 -1.50000 AFIX 0 C2 1 0.078443 0.701247 0.833064 11.00000 0.02724 0.01177 = 0.02794 -0.00047 -0.00133 -0.00671 C3 1 0.029555 0.671653 0.756022 11.00000 0.01476 0.00967 = 0.03703 -0.00304 -0.00229 -0.00232 C4 1 -0.097418 0.655467 0.746918 11.00000 0.01499 0.01666 = 0.04760 -0.00269 -0.00153 -0.00309 AFIX 43 H4 2 -0.166026 0.664761 0.798269 11.00000 -1.20000 AFIX 0 C5 1 -0.122798 0.626156 0.663761 11.00000 0.01388 0.01812 = 0.04364 -0.00470 -0.00401 -0.00484 AFIX 43 H5 2 -0.209132 0.614813 0.658891 11.00000 -1.20000 AFIX 0 C6 1 -0.026896 0.612802 0.587509 11.00000 0.01962 0.01317 = 0.04011 -0.00177 -0.00700 -0.00334 AFIX 43 H6 2 -0.046705 0.592508 0.530714 11.00000 -1.20000 AFIX 0 C7 1 0.102530 0.629731 0.594599 11.00000 0.01455 0.00278 = 0.03876 -0.00217 -0.00697 0.00125 C8 1 0.213153 0.621644 0.524716 11.00000 0.02231 0.00832 = 0.03236 0.00258 -0.00873 -0.00268 C9 1 0.205535 0.602011 0.425280 11.00000 0.02664 0.02831 = 0.03746 -0.00636 -0.00520 -0.01296 AFIX 137 H9A 2 0.235670 0.657897 0.379801 11.00000 -1.50000 H9B 2 0.112772 0.602196 0.416757 11.00000 -1.50000 H9C 2 0.263163 0.533058 0.414033 11.00000 -1.50000 AFIX 0 C10 1 0.323435 0.708123 0.846515 11.00000 0.01536 0.01415 = 0.04119 -0.00204 -0.00929 0.00703 AFIX 13 H10 2 0.344393 0.778198 0.849759 11.00000 -1.20000 AFIX 0 C11 1 0.364423 0.621204 0.929929 11.00000 0.03310 0.02949 = 0.03041 -0.00817 -0.00412 -0.00974 AFIX 23 H11A 2 0.462227 0.608447 0.933434 11.00000 -1.20000 H11B 2 0.318359 0.645226 0.990697 11.00000 -1.20000 AFIX 0 C12 1 0.327801 0.518090 0.916695 11.00000 0.01860 0.02370 = 0.03110 -0.00457 -0.00486 -0.00531 AFIX 23 H12A 2 0.230075 0.524066 0.931618 11.00000 -1.20000 H12B 2 0.374688 0.458551 0.960371 11.00000 -1.20000 AFIX 0 C13 1 0.550105 0.416440 0.800972 11.00000 0.01729 0.02416 = 0.02113 -0.00600 -0.00298 -0.00609 C14 1 0.653049 0.468756 0.803202 11.00000 0.02075 0.01777 = 0.03079 0.00232 -0.00731 -0.00655 AFIX 43 H14 2 0.634405 0.544026 0.794295 11.00000 -1.20000 AFIX 0 C15 1 0.780998 0.412629 0.818131 11.00000 0.01381 0.03646 = 0.03185 -0.00033 -0.00383 -0.01060 AFIX 43 H15 2 0.849150 0.449873 0.819727 11.00000 -1.20000 AFIX 0 C16 1 0.811916 0.303697 0.830766 11.00000 0.00911 0.03596 = 0.03759 -0.00508 -0.00370 0.00102 AFIX 43 H16 2 0.900138 0.265421 0.841812 11.00000 -1.20000 AFIX 0 C17 1 0.712158 0.251504 0.827035 11.00000 0.02910 0.01890 = 0.06479 -0.00643 -0.01053 -0.00163 AFIX 43 H17 2 0.732469 0.176223 0.834648 11.00000 -1.20000 AFIX 0 C18 1 0.581451 0.306732 0.812285 11.00000 0.01319 0.01064 = 0.07034 -0.00883 -0.01155 -0.00074 AFIX 43 H18 2 0.514059 0.268959 0.810021 11.00000 -1.20000 AFIX 0 C19 1 0.286788 0.393731 0.775662 11.00000 0.01158 0.01750 = 0.02495 -0.00044 -0.00491 -0.00092 C20 1 0.241191 0.325814 0.851008 11.00000 0.01413 0.02500 = 0.03634 -0.00517 -0.00067 -0.00410 AFIX 43 H20 2 0.255635 0.329930 0.914684 11.00000 -1.20000 AFIX 0 C21 1 0.173828 0.251385 0.831959 11.00000 0.01812 0.02563 = 0.04358 -0.00122 0.00238 -0.01040 AFIX 43 H21 2 0.140338 0.205885 0.883092 11.00000 -1.20000 AFIX 0 C22 1 0.155900 0.243816 0.739600 11.00000 0.00586 0.02257 = 0.05343 -0.00525 -0.00225 -0.00086 AFIX 43 H22 2 0.111487 0.192023 0.727565 11.00000 -1.20000 AFIX 0 C23 1 0.201181 0.309986 0.664199 11.00000 0.01482 0.01707 = 0.04109 -0.01134 -0.00676 -0.00109 AFIX 43 H23 2 0.188573 0.304443 0.600466 11.00000 -1.20000 AFIX 0 C24 1 0.266815 0.386270 0.684012 11.00000 0.00753 0.01017 = 0.03671 -0.00390 -0.00263 0.00383 AFIX 43 H24 2 0.297651 0.433222 0.632935 11.00000 -1.20000 AFIX 0 C25 1 0.439991 0.642283 0.482676 11.00000 0.02642 0.02081 = 0.03867 -0.00336 -0.00065 -0.01442 AFIX 23 H25A 2 0.433956 0.602250 0.430450 11.00000 -1.20000 H25B 2 0.525443 0.609779 0.510650 11.00000 -1.20000 AFIX 0 C26 1 0.438593 0.759094 0.441870 11.00000 0.01408 0.01609 = 0.04585 -0.00361 -0.00246 -0.00571 AFIX 23 H26A 2 0.500583 0.760525 0.382689 11.00000 -1.20000 H26B 2 0.347386 0.794296 0.424548 11.00000 -1.20000 AFIX 0 C27 1 0.479136 0.822607 0.511110 11.00000 0.02121 0.01511 = 0.03600 0.00000 -0.00926 -0.00622 AFIX 23 H27A 2 0.481334 0.894439 0.477767 11.00000 -1.20000 H27B 2 0.571306 0.788092 0.526760 11.00000 -1.20000 AFIX 6 PART -1 C28 1 0.460567 0.905734 0.686132 21.00000 0.01791 0.01000 = 0.04816 -0.00060 -0.00888 -0.00573 C29 1 0.590302 0.855313 0.707431 21.00000 0.01605 0.01158 = 0.06121 -0.00889 -0.01351 0.00517 AFIX 43 H29A 2 0.627071 0.785593 0.691938 21.00000 -1.20000 AFIX 5 C30 1 0.666764 0.905524 0.751028 21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H30A 2 0.755140 0.870241 0.764642 21.00000 -1.20000 AFIX 5 C31 1 0.613624 1.007521 0.774678 21.00000 0.03508 0.01158 = 0.09814 -0.00134 -0.03224 -0.01465 AFIX 43 H31A 2 0.664407 1.041411 0.805981 21.00000 -1.20000 AFIX 5 C32 1 0.484408 1.059569 0.751770 21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H32A 2 0.447916 1.129646 0.766431 21.00000 -1.20000 AFIX 5 C33 1 0.410611 1.009448 0.708221 21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H33A 2 0.323480 1.045888 0.692626 21.00000 -1.20000 AFIX 5 PART -2 C28' 1 0.464628 0.896044 0.692045 -21.00000 0.01791 0.01000 = 0.04816 -0.00060 -0.00888 -0.00573 C29' 1 0.597567 0.849573 0.707865 -21.00000 0.01605 0.01158 = 0.06121 -0.00889 -0.01351 0.00517 AFIX 43 H29B 2 0.642077 0.788088 0.679267 -21.00000 -1.20000 AFIX 5 C30' 1 0.666070 0.891839 0.764884 -21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H30B 2 0.756735 0.859479 0.774567 -21.00000 -1.20000 AFIX 5 C31' 1 0.601620 0.981587 0.807725 -21.00000 0.03508 0.01158 = 0.09814 -0.00134 -0.03224 -0.01465 AFIX 43 H31B 2 0.647073 1.009633 0.848079 -21.00000 -1.20000 AFIX 5 C32' 1 0.468971 1.030048 0.790632 -21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H32B 2 0.424689 1.092095 0.818463 -21.00000 -1.20000 AFIX 5 C33' 1 0.403047 0.987993 0.733779 -21.00000 0.02111 0.00197 = 0.09021 -0.00402 -0.02401 0.00095 AFIX 43 H33B 2 0.313426 1.021995 0.722381 -21.00000 -1.20000 AFIX 0 PART 0 C34 1 0.227922 0.942973 0.591995 11.00000 0.01810 0.01797 = 0.04244 -0.00382 -0.00742 -0.01174 C35 1 0.235166 1.026177 0.518953 11.00000 0.01653 0.01306 = 0.06357 -0.00278 -0.01204 -0.00659 AFIX 43 H35 2 0.317090 1.026132 0.479784 11.00000 -1.20000 AFIX 0 C36 1 0.125643 1.108991 0.502122 11.00000 0.02530 0.02032 = 0.05203 0.00236 -0.01129 -0.00806 AFIX 43 H36 2 0.132175 1.163826 0.450810 11.00000 -1.20000 AFIX 0 C37 1 0.006154 1.111559 0.560589 11.00000 0.03453 0.01890 = 0.05094 -0.00650 -0.02028 -0.00420 AFIX 43 H37 2 -0.068203 1.169452 0.551084 11.00000 -1.20000 AFIX 0 C38 1 -0.003492 1.028162 0.633458 11.00000 0.01595 0.02619 = 0.05169 -0.00838 -0.00888 -0.00099 AFIX 43 H38 2 -0.085372 1.028585 0.672767 11.00000 -1.20000 AFIX 0 C39 1 0.105966 0.944875 0.648554 11.00000 0.01737 0.01710 = 0.04761 -0.00313 -0.00946 -0.00683 AFIX 43 H39 2 0.098130 0.888325 0.697939 11.00000 -1.20000 AFIX 0 C40 1 0.860293 0.012419 1.006322 11.00000 0.06573 0.03674 = 0.05914 -0.00180 -0.03046 -0.01341 C41 1 0.942271 -0.008299 0.921750 11.00000 0.07620 0.04205 = 0.05914 -0.00534 -0.04142 -0.01069 AFIX 43 H41 2 0.901596 -0.014679 0.867481 11.00000 -1.20000 AFIX 0 C42 1 1.080964 -0.019933 0.913937 11.00000 0.03541 0.04087 = 0.06007 -0.00851 -0.01382 0.00937 AFIX 43 H42 2 1.133713 -0.032693 0.855331 11.00000 -1.20000 AFIX 0 C43 1 0.700455 0.025271 1.020815 10.50000 0.04550 0.07932 = 0.05149 -0.00793 -0.01092 -0.01804 AFIX 137 H43A 2 0.657224 0.095508 0.991008 10.50000 -1.50000 H43B 2 0.670470 0.017547 1.089187 10.50000 -1.50000 H43C 2 0.676191 -0.029405 0.991090 10.50000 -1.50000 AFIX 0 H1M 2 0.495373 0.653382 0.692750 11.00000 10.04000 HKLF 4 REM P-1 in P-1 REM R1 = 0.0776 for 4261 Fo > 4sig(Fo) and 0.1221 for all 6213 data REM 425 parameters refined using 13 restraints END WGHT 0.0164 20.1654 REM Highest difference peak 2.628, deepest hole -1.324, 1-sigma level 0.134 Q1 1 0.3361 0.6755 0.6199 11.00000 0.05 2.63 Q2 1 0.3045 0.6630 0.7767 11.00000 0.05 2.62 Q3 1 0.3737 0.5949 0.7032 11.00000 0.05 0.91 Q4 1 0.3628 0.4905 0.8626 11.00000 0.05 0.85 Q5 1 0.3872 0.8393 0.5474 11.00000 0.05 0.81 Q6 1 0.3523 0.8236 0.7004 11.00000 0.05 0.77 Q7 1 0.4034 0.4960 0.7175 11.00000 0.05 0.73 Q8 1 0.4149 0.5993 0.6382 11.00000 0.05 0.71 Q9 1 0.1998 0.7240 0.7431 11.00000 0.05 0.70 Q10 1 0.2683 0.8430 0.6043 11.00000 0.05 0.68 ; _shelx_res_checksum 21561 _shelx_hkl_file ; -1 0 0 30.50 1.60 -1 0 0 32.32 1.58 -1 0 0 38.70 1.61 -1 0 0 37.12 1.67 1 0 0 37.54 1.62 1 0 0 36.93 1.71 1 0 0 31.02 1.58 1 0 0 32.31 1.58 -2 0 0 69.93 3.37 -2 0 0 66.13 3.11 -2 0 0 64.44 3.17 -2 0 0 74.05 3.22 2 0 0 70.29 3.14 2 0 0 66.87 3.25 2 0 0 62.53 3.36 2 0 0 67.26 3.23 -3 0 0 130.83 6.08 -3 0 0 127.20 5.71 -3 0 0 139.58 5.85 -3 0 0 130.24 5.68 3 0 0 132.32 6.11 3 0 0 128.25 5.84 3 0 0 132.96 5.74 3 0 0 127.31 5.68 -4 0 0 54.61 2.86 -4 0 0 55.15 3.13 -4 0 0 51.27 2.90 4 0 0 46.47 3.14 4 0 0 51.08 2.98 4 0 0 53.52 2.93 4 0 0 58.89 2.98 -5 0 0 4.05 1.30 -5 0 0 3.18 1.36 -5 0 0 3.66 1.16 -5 0 0 3.98 1.20 5 0 0 6.46 1.34 5 0 0 3.87 1.31 5 0 0 5.21 1.28 5 0 0 3.93 1.50 -6 0 0 53.51 3.18 -6 0 0 51.64 3.01 -6 0 0 56.55 3.36 -6 0 0 56.73 3.18 6 0 0 54.87 3.18 6 0 0 51.28 3.13 6 0 0 51.04 3.41 6 0 0 48.37 3.24 -7 0 0 10.35 1.77 7 0 0 9.46 1.71 7 0 0 8.59 1.98 7 0 0 9.96 1.67 -8 0 0 2.93 1.54 -8 0 0 2.72 1.82 8 0 0 1.09 1.68 8 0 0 0.45 2.06 8 0 0 1.54 1.80 -9 0 0 48.05 3.91 9 0 0 41.52 4.03 9 0 0 48.13 3.68 9 0 0 44.74 4.42 -10 0 0 6.79 2.36 10 0 0 7.11 2.87 10 0 0 2.98 2.41 -11 0 0 4.22 2.54 -11 1 0 4.63 2.34 10 -1 0 17.79 3.31 -10 1 0 11.04 2.47 9 -1 0 5.77 2.08 9 -1 0 3.92 1.90 9 -1 0 8.48 2.74 -9 1 0 6.73 2.13 8 -1 0 74.63 4.78 8 -1 0 78.96 5.03 8 -1 0 81.81 4.43 -8 1 0 79.09 4.42 7 -1 0 38.13 2.76 7 -1 0 27.09 2.97 7 -1 0 37.28 3.30 -7 1 0 37.96 2.80 -7 1 0 36.21 2.53 6 -1 0 7.94 1.48 6 -1 0 8.16 1.85 6 -1 0 11.06 1.54 6 -1 0 9.79 1.46 -6 1 0 9.80 1.38 -6 1 0 9.01 1.39 -6 1 0 11.57 1.54 5 -1 0 21.90 2.15 5 -1 0 22.80 1.85 5 -1 0 20.41 1.97 5 -1 0 22.42 2.07 -5 1 0 18.33 1.85 -5 1 0 20.48 1.88 -5 1 0 21.21 2.00 -5 1 0 19.38 1.75 4 -1 0 25.53 1.96 4 -1 0 22.77 2.16 4 -1 0 31.45 2.02 4 -1 0 22.00 2.05 -4 1 0 20.58 1.96 -4 1 0 22.80 1.89 -4 1 0 24.99 1.82 3 -1 0 77.97 3.65 3 -1 0 74.44 4.06 3 -1 0 83.72 3.72 3 -1 0 73.35 3.69 3 -1 0 84.58 3.75 -3 1 0 87.53 3.72 -3 1 0 82.81 3.65 -3 1 0 74.15 3.63 2 -1 0 608.17 25.68 2 -1 0 640.86 26.55 2 -1 0 638.22 27.52 2 -1 0 629.91 25.70 -2 1 0 661.51 26.55 -2 1 0 663.43 25.70 -2 1 0 596.15 25.68 1 -1 0 139.57 6.41 1 -1 0 146.69 6.14 -1 1 0 147.74 6.41 0 -1 0 56.00 2.56 0 -1 0 66.71 2.57 0 1 0 64.02 2.57 -1 -1 0 488.91 20.35 -1 -1 0 504.56 20.34 -1 -1 0 469.44 20.99 1 1 0 518.54 20.36 1 1 0 507.39 20.99 1 1 0 502.20 20.34 1 1 0 520.70 21.10 -2 -1 0 10.56 1.20 -2 -1 0 10.52 1.13 -2 -1 0 10.14 1.10 2 1 0 9.19 1.08 2 1 0 9.16 1.08 2 1 0 12.21 1.14 -3 -1 0 10.56 1.23 -3 -1 0 7.76 1.27 -3 -1 0 12.78 1.20 -3 -1 0 9.76 1.26 3 1 0 9.05 1.21 3 1 0 10.79 1.28 3 1 0 12.18 1.24 -4 -1 0 87.04 3.95 -4 -1 0 81.35 4.02 -4 -1 0 81.46 4.11 4 1 0 79.51 3.95 4 1 0 81.64 4.03 4 1 0 78.49 4.12 4 1 0 79.10 3.90 -5 -1 0 0.89 1.12 -5 -1 0 0.74 1.30 -5 -1 0 1.74 1.17 -5 -1 0 1.88 1.32 5 1 0 0.55 1.27 5 1 0 -0.11 1.36 5 1 0 1.76 1.22 5 1 0 2.58 1.29 -6 -1 0 27.36 2.47 -6 -1 0 23.00 2.35 -6 -1 0 25.94 2.34 6 1 0 24.28 2.51 6 1 0 24.79 2.39 6 1 0 28.58 2.38 6 1 0 28.27 2.44 -7 -1 0 78.94 4.09 -7 -1 0 88.67 4.36 7 1 0 68.32 4.32 7 1 0 76.44 4.19 7 1 0 75.33 4.55 -8 -1 0 3.67 1.96 -8 -1 0 5.62 1.61 8 1 0 6.40 2.16 8 1 0 3.83 1.94 8 1 0 5.32 1.78 -9 -1 0 32.07 3.00 -9 -1 0 34.82 3.07 9 1 0 28.17 3.07 9 1 0 35.24 3.78 9 1 0 30.23 2.91 -10 -1 0 15.60 2.68 10 1 0 17.91 2.76 10 1 0 17.13 3.08 10 1 0 13.26 2.65 -11 -1 0 5.79 2.53 -11 2 0 13.25 2.41 10 -2 0 50.98 4.45 -10 2 0 45.63 3.79 9 -2 0 51.16 4.10 9 -2 0 53.35 4.89 -9 2 0 40.54 3.56 8 -2 0 12.46 2.63 8 -2 0 11.69 1.81 8 -2 0 10.07 2.13 -8 2 0 8.31 1.87 7 -2 0 44.16 3.61 7 -2 0 42.47 3.20 7 -2 0 38.32 2.84 -7 2 0 40.49 2.75 -7 2 0 42.02 2.84 6 -2 0 55.29 3.67 6 -2 0 50.84 3.23 6 -2 0 53.71 2.98 -6 2 0 54.73 3.04 -6 2 0 47.16 3.09 -6 2 0 56.74 2.99 5 -2 0 6.32 1.36 5 -2 0 10.92 1.27 5 -2 0 5.54 1.77 -5 2 0 8.83 1.19 -5 2 0 8.88 1.24 -5 2 0 8.24 1.16 4 -2 0 4.11 1.48 4 -2 0 6.98 1.06 4 -2 0 5.65 1.02 -4 2 0 0.90 0.70 -4 2 0 3.45 0.95 -4 2 0 4.23 1.03 -4 2 0 2.32 1.31 3 -2 0 5.61 1.36 3 -2 0 6.72 0.96 -3 2 0 8.23 0.97 -3 2 0 6.69 0.88 2 -2 0 4.65 1.18 2 -2 0 5.14 0.89 -2 2 0 5.31 1.15 -2 2 0 8.84 0.99 1 -2 0 120.03 5.56 -1 2 0 124.22 5.57 0 -2 0 4.67 0.60 0 2 0 5.21 0.61 -1 -2 0 255.47 10.42 -1 -2 0 256.96 10.71 -1 -2 0 249.95 10.78 1 2 0 267.01 10.42 1 2 0 238.25 10.38 1 2 0 252.50 10.78 1 2 0 251.76 10.71 -2 -2 0 140.28 6.52 -2 -2 0 158.36 6.71 -2 -2 0 155.53 6.49 -2 -2 0 155.69 6.61 2 2 0 150.42 6.64 2 2 0 156.63 6.59 2 2 0 135.23 6.44 2 2 0 154.86 6.53 -3 -2 0 -0.05 0.94 -3 -2 0 1.62 1.09 -3 -2 0 0.48 0.97 3 2 0 0.90 0.92 3 2 0 2.29 1.04 3 2 0 2.19 0.90 3 2 0 2.83 1.04 -4 -2 0 26.25 2.00 -4 -2 0 24.55 2.24 -4 -2 0 25.16 1.95 4 2 0 28.27 2.27 4 2 0 26.19 1.97 4 2 0 26.61 2.13 -5 -2 0 68.11 3.85 -5 -2 0 68.97 3.84 -5 -2 0 75.09 3.81 5 2 0 67.03 3.80 5 2 0 74.38 3.84 5 2 0 68.74 3.86 -6 -2 0 9.55 1.56 -6 -2 0 7.19 1.42 -6 -2 0 8.50 1.62 -6 -2 0 6.63 1.38 6 2 0 5.67 1.57 6 2 0 9.87 1.57 6 2 0 7.44 1.58 -7 -2 0 118.39 5.86 -7 -2 0 118.36 5.73 7 2 0 117.79 6.07 7 2 0 120.91 5.82 7 2 0 115.97 5.93 -8 -2 0 86.21 4.93 -8 -2 0 91.99 4.83 8 2 0 88.70 4.87 8 2 0 78.99 4.99 8 2 0 90.72 5.13 -9 -2 0 15.22 2.20 -9 -2 0 14.76 2.54 9 2 0 16.01 2.46 9 2 0 17.92 2.37 9 2 0 12.90 2.65 -10 -2 0 69.50 4.92 10 2 0 67.52 5.09 10 2 0 79.01 5.45 10 2 0 64.05 4.68 -11 -2 0 13.60 2.98 11 2 0 13.81 3.30 -11 3 0 24.47 2.73 10 -3 0 17.08 3.56 -10 3 0 14.72 2.32 9 -3 0 52.81 4.26 -9 3 0 49.15 3.51 8 -3 0 33.64 3.55 8 -3 0 29.11 2.81 8 -3 0 28.88 2.61 7 -3 0 11.41 2.42 7 -3 0 6.56 1.50 7 -3 0 13.32 1.57 7 -3 0 12.24 1.88 -7 3 0 10.33 1.63 -7 3 0 9.49 1.47 6 -3 0 7.43 1.43 6 -3 0 4.77 1.92 6 -3 0 2.57 1.20 -6 3 0 6.81 1.25 5 -3 0 25.93 2.13 5 -3 0 25.98 2.67 -5 3 0 25.89 2.04 4 -3 0 63.46 3.33 4 -3 0 66.77 3.82 -4 3 0 70.13 3.78 3 -3 0 1.94 1.40 -3 3 0 6.62 0.99 -3 3 0 2.69 1.25 2 -3 0 108.43 5.10 -2 3 0 103.78 5.05 1 -3 0 61.47 3.13 -1 3 0 61.98 3.10 0 -3 0 900.70 36.05 0 -3 0 873.22 36.07 0 3 0 840.36 36.05 0 3 0 951.48 36.07 -1 -3 0 160.38 6.78 -1 -3 0 160.94 6.95 -1 -3 0 161.86 7.05 -1 -3 0 164.84 6.75 1 3 0 167.06 6.78 1 3 0 146.41 6.71 1 3 0 155.80 6.95 -2 -3 0 15.38 1.47 -2 -3 0 15.89 1.35 -2 -3 0 14.63 1.27 -2 -3 0 16.81 1.37 2 3 0 16.20 1.46 2 3 0 15.81 1.29 2 3 0 14.21 1.33 2 3 0 14.65 1.34 -3 -3 0 7.66 1.17 -3 -3 0 11.24 1.33 -3 -3 0 8.80 1.32 -3 -3 0 11.46 1.21 3 3 0 9.10 1.20 3 3 0 9.31 1.27 3 3 0 7.08 1.20 -4 -3 0 4.49 1.08 -4 -3 0 2.52 1.36 4 3 0 3.86 1.11 4 3 0 3.77 1.26 4 3 0 5.31 1.30 -5 -3 0 105.90 4.75 -5 -3 0 91.21 4.73 -5 -3 0 88.10 4.79 5 3 0 88.96 4.73 5 3 0 98.71 4.78 5 3 0 92.81 4.70 5 3 0 105.25 4.83 -6 -3 0 23.37 2.28 -6 -3 0 23.84 2.23 6 3 0 21.19 2.06 6 3 0 23.36 2.22 6 3 0 23.01 2.08 -7 -3 0 13.67 1.81 -7 -3 0 12.80 1.96 7 3 0 9.42 1.81 7 3 0 12.22 1.91 7 3 0 13.26 1.97 -8 -3 0 149.49 7.01 -8 -3 0 143.91 7.13 8 3 0 151.69 7.40 8 3 0 142.37 7.24 8 3 0 142.54 7.05 -9 -3 0 78.57 4.94 9 3 0 73.83 4.95 9 3 0 76.59 4.79 9 3 0 74.57 4.95 -10 -3 0 13.18 2.67 10 3 0 14.54 2.45 10 3 0 16.25 2.68 10 3 0 15.12 2.89 -11 -3 0 51.06 4.30 11 3 0 47.00 4.18 11 3 0 43.56 4.43 9 -4 0 6.27 2.14 8 -4 0 3.58 1.87 8 -4 0 2.18 2.74 7 -4 0 35.53 3.20 7 -4 0 36.21 3.85 6 -4 0 12.03 1.60 6 -4 0 12.85 2.21 -6 4 0 7.57 1.43 5 -4 0 61.93 3.76 5 -4 0 49.66 3.13 -5 4 0 58.27 3.16 4 -4 0 66.44 3.55 4 -4 0 69.88 4.06 -4 4 0 74.65 3.99 3 -4 0 8.34 1.61 -3 4 0 6.53 1.47 2 -4 0 11.35 1.37 -2 4 0 9.29 1.22 -1 4 0 38.18 2.19 0 -4 0 37.67 1.93 0 -4 0 35.97 2.03 0 4 0 31.75 1.92 0 4 0 43.15 1.99 -1 -4 0 72.08 3.56 -1 -4 0 71.99 3.41 -1 -4 0 72.37 3.40 -1 -4 0 70.51 3.30 1 4 0 67.61 3.30 1 4 0 74.19 3.34 -2 -4 0 2.05 1.02 -2 -4 0 -1.28 1.04 -2 -4 0 1.46 0.98 2 4 0 -0.14 0.91 2 4 0 0.53 0.94 2 4 0 1.51 1.02 2 4 0 2.69 0.97 -3 -4 0 1.58 1.19 -3 -4 0 0.04 0.84 -3 -4 0 1.04 1.07 -3 -4 0 1.09 1.08 3 4 0 0.77 0.92 3 4 0 0.99 1.07 3 4 0 0.11 1.08 3 4 0 0.92 1.02 -4 -4 0 44.49 2.96 -4 -4 0 50.58 2.75 -4 -4 0 44.37 2.93 -4 -4 0 44.08 2.82 4 4 0 48.41 2.91 4 4 0 42.96 2.86 4 4 0 44.38 2.94 -5 -4 0 12.34 1.62 -5 -4 0 16.73 1.69 -5 -4 0 12.45 1.79 5 4 0 11.68 1.61 5 4 0 11.17 1.65 5 4 0 12.23 1.68 -6 -4 0 50.95 3.39 -6 -4 0 49.58 3.15 6 4 0 46.49 3.24 6 4 0 48.84 3.20 6 4 0 46.49 3.05 -7 -4 0 31.19 2.80 -7 -4 0 29.40 2.72 7 4 0 30.80 2.71 7 4 0 30.88 2.99 7 4 0 28.17 2.86 -8 -4 0 7.51 2.18 8 4 0 3.96 2.00 8 4 0 5.72 1.96 8 4 0 6.06 1.91 -9 -4 0 120.76 6.44 9 4 0 113.68 6.45 9 4 0 109.58 6.47 9 4 0 120.82 6.35 -10 -4 0 30.07 3.37 10 4 0 29.22 3.16 10 4 0 31.09 3.37 10 4 0 29.35 3.30 -11 -4 0 5.12 2.82 11 4 0 4.00 2.43 11 4 0 6.19 2.64 8 -5 0 6.24 2.96 8 -5 0 5.60 1.90 7 -5 0 45.63 4.18 6 -5 0 37.60 3.62 5 -5 0 33.59 3.10 4 -5 0 40.14 3.08 -4 5 0 40.33 2.84 3 -5 0 19.30 1.97 -3 5 0 17.96 1.88 -2 5 0 8.75 1.22 0 -5 0 11.50 1.03 0 -5 0 11.53 1.17 0 5 0 10.57 1.03 -1 -5 0 19.50 1.90 -1 -5 0 15.27 1.62 -1 -5 0 19.14 1.56 -1 -5 0 18.69 1.79 1 5 0 19.02 1.57 1 5 0 21.97 1.60 -2 -5 0 145.79 6.45 -2 -5 0 140.44 6.32 -2 -5 0 135.17 6.48 -2 -5 0 142.32 6.25 2 5 0 146.14 6.47 2 5 0 145.23 6.28 2 5 0 146.46 6.29 -3 -5 0 40.48 2.66 -3 -5 0 52.53 2.99 -3 -5 0 51.35 3.08 -3 -5 0 56.04 3.01 3 5 0 50.82 2.92 3 5 0 44.94 2.84 3 5 0 58.40 3.01 3 5 0 52.57 2.85 -4 -5 0 9.07 1.45 -4 -5 0 12.01 1.59 -4 -5 0 10.04 1.51 -4 -5 0 8.21 1.63 4 5 0 9.32 1.52 4 5 0 10.41 1.53 4 5 0 9.75 1.57 4 5 0 10.67 1.34 -5 -5 0 82.91 4.29 -5 -5 0 88.06 4.38 -5 -5 0 87.12 4.48 -5 -5 0 74.48 4.45 5 5 0 88.62 4.52 5 5 0 81.77 4.37 5 5 0 88.28 4.48 -6 -5 0 43.65 3.33 -6 -5 0 41.71 3.00 6 5 0 41.00 3.12 6 5 0 41.42 3.16 -7 -5 0 31.43 2.84 7 5 0 32.78 2.80 7 5 0 28.89 2.76 -8 -5 0 19.95 2.71 8 5 0 22.53 2.38 8 5 0 19.64 2.51 8 5 0 22.55 2.65 -9 -5 0 8.58 2.50 9 5 0 6.39 2.25 9 5 0 8.39 2.40 9 5 0 7.95 2.18 -10 -5 0 8.11 2.81 10 5 0 5.07 2.40 10 5 0 1.82 2.43 10 5 0 9.79 2.44 -11 -5 0 5.81 2.81 11 5 0 8.53 2.71 11 5 0 6.80 2.65 11 5 0 8.71 2.76 9 -6 0 0.34 3.08 7 -6 0 5.66 2.55 6 -6 0 10.18 2.55 5 -6 0 6.91 2.07 4 -6 0 41.27 3.19 3 -6 0 84.08 4.63 -3 6 0 90.94 4.54 2 -6 0 10.33 1.69 0 -6 0 235.29 9.61 0 6 0 222.23 9.54 -1 -6 0 25.42 2.31 -1 -6 0 25.91 2.13 -1 -6 0 24.20 1.94 1 6 0 28.78 2.02 1 6 0 23.89 1.92 -2 -6 0 11.24 1.56 -2 -6 0 8.34 1.43 -2 -6 0 7.05 1.26 -2 -6 0 9.06 1.30 2 6 0 9.38 1.31 2 6 0 12.05 1.36 -3 -6 0 234.21 9.79 -3 -6 0 219.81 9.85 -3 -6 0 226.79 9.61 3 6 0 212.64 9.73 3 6 0 212.67 9.50 -4 -6 0 139.76 6.65 -4 -6 0 148.73 6.74 -4 -6 0 153.72 6.76 -4 -6 0 140.75 6.53 4 6 0 133.38 6.55 4 6 0 146.28 6.65 4 6 0 141.35 6.72 4 6 0 144.91 6.61 -5 -6 0 17.54 2.00 -5 -6 0 14.41 1.92 -5 -6 0 18.20 1.90 5 6 0 17.36 2.02 5 6 0 17.45 1.96 5 6 0 15.62 1.61 5 6 0 16.62 1.94 -6 -6 0 20.75 2.39 6 6 0 25.67 2.38 6 6 0 23.47 2.34 -7 -6 0 36.00 3.57 7 6 0 31.95 3.33 7 6 0 36.77 3.30 -8 -6 0 2.91 2.25 8 6 0 5.58 2.10 8 6 0 4.40 2.18 -9 -6 0 2.74 2.39 9 6 0 3.87 2.27 9 6 0 2.67 2.17 -10 -6 0 8.38 2.80 10 6 0 8.08 2.59 10 6 0 4.10 2.24 10 6 0 6.95 2.51 -11 -6 0 6.48 2.99 11 6 0 9.93 2.85 11 6 0 8.14 2.75 12 6 0 2.01 2.59 7 -7 0 30.38 3.80 6 -7 0 4.14 2.46 5 -7 0 122.82 6.70 4 -7 0 42.62 3.43 3 -7 0 17.30 2.10 2 -7 0 24.08 2.30 0 -7 0 13.37 1.41 0 -7 0 10.54 1.68 -1 -7 0 120.69 5.91 -1 -7 0 125.13 5.57 -1 -7 0 117.31 5.43 1 7 0 118.03 5.46 1 7 0 129.24 5.49 -2 -7 0 7.74 1.50 -2 -7 0 5.03 1.20 -2 -7 0 3.23 1.14 -2 -7 0 3.51 1.33 2 7 0 3.85 1.21 2 7 0 4.99 1.17 -3 -7 0 7.24 1.49 -3 -7 0 5.42 1.31 -3 -7 0 2.30 1.14 -3 -7 0 9.19 1.55 3 7 0 3.92 1.34 3 7 0 3.43 1.25 3 7 0 0.24 0.80 -4 -7 0 179.68 8.25 -4 -7 0 178.16 8.32 -4 -7 0 182.19 8.14 4 7 0 179.03 8.08 4 7 0 188.44 8.11 4 7 0 176.39 8.26 -5 -7 0 3.92 1.65 -5 -7 0 4.99 1.60 5 7 0 5.27 1.59 5 7 0 2.61 1.53 5 7 0 2.89 1.24 5 7 0 2.76 1.44 -6 -7 0 41.73 3.39 -6 -7 0 32.69 2.99 6 7 0 37.28 3.34 6 7 0 36.85 3.20 6 7 0 37.81 2.69 -7 -7 0 39.65 3.42 7 7 0 38.92 3.54 7 7 0 36.11 3.21 -8 -7 0 1.62 2.23 8 7 0 0.39 2.18 8 7 0 3.11 2.16 -9 -7 0 13.02 2.81 9 7 0 10.82 2.55 9 7 0 13.11 2.64 -10 -7 0 14.47 3.12 10 7 0 20.12 3.03 10 7 0 17.83 2.92 -11 -7 0 -0.63 2.87 11 7 0 -2.12 2.54 11 7 0 -2.49 2.60 6 -8 0 59.56 4.72 5 -8 0 17.76 2.72 4 -8 0 12.60 2.21 3 -8 0 11.67 2.02 0 -8 0 13.41 1.52 0 -8 0 12.83 1.87 -1 -8 0 2.34 1.54 -1 -8 0 1.79 1.22 -1 -8 0 3.48 1.00 1 8 0 1.61 1.15 1 8 0 0.59 1.10 -2 -8 0 58.83 3.63 -2 -8 0 56.95 3.36 -2 -8 0 60.19 3.29 2 8 0 59.01 3.20 2 8 0 58.17 3.30 -3 -8 0 5.19 1.51 -3 -8 0 4.39 1.66 -3 -8 0 6.65 1.39 3 8 0 4.59 1.19 3 8 0 5.96 1.46 -4 -8 0 91.25 4.73 -4 -8 0 87.63 4.84 4 8 0 87.87 4.55 4 8 0 85.99 4.73 4 8 0 89.77 4.67 -5 -8 0 21.89 2.24 -5 -8 0 15.01 2.17 5 8 0 14.47 2.01 5 8 0 19.33 2.18 5 8 0 16.42 2.01 -6 -8 0 15.81 2.18 -6 -8 0 11.09 2.22 6 8 0 16.21 2.33 6 8 0 15.19 2.22 -7 -8 0 20.73 2.85 7 8 0 21.76 2.67 7 8 0 21.16 2.72 -8 -8 0 13.46 2.71 8 8 0 13.08 2.67 8 8 0 11.46 2.63 -9 -8 0 4.68 2.57 9 8 0 4.11 2.31 9 8 0 2.65 2.41 -10 -8 0 41.38 4.07 10 8 0 33.32 3.79 10 8 0 46.93 4.40 -11 -8 0 21.28 3.76 11 8 0 25.08 3.56 5 -9 0 24.74 3.27 4 -9 0 12.36 2.38 3 -9 0 17.53 2.35 1 -9 0 0.67 1.77 0 -9 0 3.43 1.78 -1 -9 0 2.74 1.71 -1 -9 0 0.42 1.22 1 9 0 -0.52 1.22 1 9 0 -0.30 1.21 -2 -9 0 7.00 1.87 -2 -9 0 4.45 1.39 -2 -9 0 6.92 1.51 2 9 0 7.20 1.35 2 9 0 7.79 1.53 -3 -9 0 6.89 1.68 -3 -9 0 8.10 1.56 -3 -9 0 10.54 1.99 3 9 0 5.31 1.41 3 9 0 6.35 1.66 -4 -9 0 12.47 1.97 -4 -9 0 10.86 2.07 4 9 0 9.17 1.73 4 9 0 9.82 1.82 -5 -9 0 69.91 4.38 -5 -9 0 67.62 4.45 5 9 0 70.10 4.18 5 9 0 66.38 4.26 5 9 0 68.76 4.40 -6 -9 0 10.44 2.21 -6 -9 0 15.33 2.33 6 9 0 13.33 2.27 6 9 0 8.83 2.21 -7 -9 0 24.46 3.06 -7 -9 0 19.13 2.60 7 9 0 23.77 2.88 7 9 0 27.37 2.93 -8 -9 0 54.91 4.73 8 9 0 56.17 4.56 8 9 0 52.81 4.63 -9 -9 0 26.97 3.54 9 9 0 31.88 3.48 9 9 0 23.30 3.24 -10 -9 0 2.88 2.69 10 9 0 2.23 2.68 10 9 0 -1.78 2.52 11 9 0 43.77 4.43 6 -10 0 6.99 2.97 5 -10 0 29.16 3.56 4 -10 0 11.53 2.66 1 -10 0 0.07 2.09 0 -10 0 0.63 1.98 -1 -10 0 4.13 2.05 -1 -10 0 3.66 1.41 1 10 0 4.76 1.57 1 10 0 4.20 1.51 -2 -10 0 -0.84 1.42 -2 -10 0 -0.45 1.93 -2 -10 0 2.12 1.51 2 10 0 -0.02 1.50 2 10 0 0.45 1.34 -3 -10 0 0.92 1.99 -3 -10 0 2.53 1.68 3 10 0 1.12 1.44 3 10 0 -0.35 1.61 -4 -10 0 43.46 3.77 -4 -10 0 43.51 3.59 4 10 0 43.61 3.44 4 10 0 44.93 3.27 -5 -10 0 10.07 2.22 -5 -10 0 9.72 2.45 5 10 0 7.40 2.11 5 10 0 11.71 2.20 -6 -10 0 34.58 3.32 -6 -10 0 37.62 3.37 6 10 0 42.97 3.72 6 10 0 35.03 3.34 -7 -10 0 16.32 2.53 -7 -10 0 10.82 2.74 7 10 0 15.13 2.60 7 10 0 11.42 2.60 -8 -10 0 7.08 2.72 -8 -10 0 7.96 2.35 8 10 0 12.71 2.80 8 10 0 10.52 2.68 -9 -10 0 20.30 3.30 9 10 0 26.30 3.46 9 10 0 15.50 3.20 -10 -10 0 29.40 3.72 10 10 0 16.64 3.40 10 10 0 25.67 3.56 4 -11 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