#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705237.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705237 loop_ _publ_author_name 'Melle, Philipp' 'S\'egaud, Nathalie' 'Albrecht, Martin' _publ_section_title ; Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12662 _journal_page_last 12673 _journal_paper_doi 10.1039/d0dt02482a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C38 H34 Co N10 O4, 2(F6 P), 3(C2 H3 N)' _chemical_formula_sum 'C44 H43 Co F12 N13 O4 P2' _chemical_formula_weight 1166.78 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-01-25T16:48:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 67.212(3) _cell_angle_beta 82.957(2) _cell_angle_gamma 83.194(2) _cell_formula_units_Z 2 _cell_length_a 12.5415(4) _cell_length_b 13.9618(4) _cell_length_c 15.2652(4) _cell_measurement_reflns_used 14148 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 27.883 _cell_measurement_theta_min 1.695 _cell_volume 2438.35(13) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0965 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0248567 _diffrn_orient_matrix_UB_12 0.05147 _diffrn_orient_matrix_UB_13 -0.0146446 _diffrn_orient_matrix_UB_21 -0.0512511 _diffrn_orient_matrix_UB_22 -0.0201381 _diffrn_orient_matrix_UB_23 0.0160662 _diffrn_orient_matrix_UB_31 0.0047545 _diffrn_orient_matrix_UB_32 0.0004333 _diffrn_orient_matrix_UB_33 0.0456669 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_unetI/netI 0.0639 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.913 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 44161 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.913 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.22 _diffrn_reflns_theta_min 1.587 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.522 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.589 _exptl_crystal_description needle _exptl_crystal_F_000 1190 _exptl_crystal_size_max 0.332 _exptl_crystal_size_mid 0.082 _exptl_crystal_size_min 0.043 _refine_diff_density_max 2.21 _refine_diff_density_min -0.72 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 692 _refine_ls_number_reflns 11003 _refine_ls_number_restraints 63 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.067 _refine_ls_R_factor_gt 0.0497 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+3.3586P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1136 _refine_ls_wR_factor_ref 0.1237 _reflns_Friedel_coverage 0 _reflns_number_gt 8749 _reflns_number_total 11003 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 17ma005c2_pm107 _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_database_code 7705237 _shelx_res_file ; TITL 17MA005C2_PM107 in P-1 shelx.res created by SHELXL-2016/6 at 16:48:42 on 25-Jan-2017 CELL 0.71073 12.5415 13.9618 15.2652 67.212 82.957 83.194 ZERR 2.00 0.0004 0.0004 0.0004 0.003 0.002 0.002 LATT 1 SFAC C H CO F N O P UNIT 88 86 2 24 26 8 4 MERG 2 RIGU P2 > F12 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 TEMP -150.00 WGHT 0.049800 3.358600 FVAR 2.25714 C6 1 0.507550 0.823348 0.220147 11.00000 0.01180 0.01608 = 0.01809 -0.00697 -0.00087 -0.00200 C5 1 0.536606 0.774635 0.314141 11.00000 0.01828 0.01545 = 0.01779 -0.00410 -0.00186 -0.00348 AFIX 43 H5 2 0.537263 0.700969 0.344567 11.00000 -1.20000 AFIX 0 C4 1 0.564308 0.831544 0.363443 11.00000 0.02590 0.02114 = 0.01712 -0.00650 -0.00414 -0.00112 AFIX 43 H4 2 0.582426 0.797418 0.427491 11.00000 -1.20000 AFIX 0 C3 1 0.565400 0.937800 0.319020 11.00000 0.02741 0.02247 = 0.01959 -0.01028 -0.00459 -0.00437 AFIX 43 H3 2 0.583889 0.977733 0.352336 11.00000 -1.20000 AFIX 0 C2 1 0.542154 1.099820 0.183130 11.00000 0.03675 0.01507 = 0.02662 -0.00663 -0.00658 -0.00371 AFIX 137 H2A 2 0.483382 1.132382 0.213226 11.00000 -1.50000 H2B 2 0.533121 1.122977 0.114942 11.00000 -1.50000 H2C 2 0.611278 1.120056 0.191456 11.00000 -1.50000 AFIX 0 C1 1 0.512186 0.932011 0.177984 11.00000 0.01946 0.01778 = 0.01580 -0.00568 -0.00233 -0.00393 AFIX 43 H1 2 0.495510 0.968375 0.113749 11.00000 -1.20000 AFIX 0 C7 1 0.425751 0.802039 0.097144 11.00000 0.01628 0.01588 = 0.01590 -0.00448 -0.00241 -0.00198 C8 1 0.391172 0.719626 0.067580 11.00000 0.01848 0.01681 = 0.01352 -0.00317 -0.00113 -0.00429 C9 1 0.312727 0.739137 0.004935 11.00000 0.02003 0.02139 = 0.01597 -0.00508 -0.00515 -0.00032 AFIX 43 H9 2 0.279733 0.807393 -0.024697 11.00000 -1.20000 AFIX 0 C10 1 0.283729 0.656032 -0.013285 11.00000 0.01985 0.02988 = 0.01912 -0.00954 -0.00677 -0.00318 AFIX 43 H10 2 0.229487 0.666945 -0.055223 11.00000 -1.20000 AFIX 0 C11 1 0.333850 0.557109 0.029663 11.00000 0.02004 0.02655 = 0.02083 -0.01214 -0.00261 -0.00672 AFIX 43 H11 2 0.314149 0.499629 0.018175 11.00000 -1.20000 AFIX 0 C12 1 0.413372 0.544233 0.089740 11.00000 0.01659 0.01916 = 0.01406 -0.00720 0.00061 -0.00413 C13 1 0.474285 0.440372 0.140425 11.00000 0.01794 0.01864 = 0.01597 -0.00777 -0.00013 -0.00394 C14 1 0.603339 0.356476 0.249403 11.00000 0.02794 0.01758 = 0.02068 -0.01122 -0.00564 0.00050 C15 1 0.550137 0.270922 0.314170 11.00000 0.03902 0.02175 = 0.02524 -0.01093 -0.00418 -0.00416 AFIX 43 H15 2 0.474293 0.270500 0.315247 11.00000 -1.20000 AFIX 0 C16 1 0.608191 0.187111 0.376512 11.00000 0.06719 0.01743 = 0.02579 -0.00691 -0.00905 -0.00694 AFIX 43 H16 2 0.572054 0.129592 0.421278 11.00000 -1.20000 AFIX 0 C17 1 0.718440 0.186921 0.373781 11.00000 0.06160 0.02110 = 0.03345 -0.01141 -0.02258 0.00950 AFIX 43 H17 2 0.758477 0.129244 0.416417 11.00000 -1.20000 AFIX 0 C18 1 0.887878 0.267420 0.308144 11.00000 0.03830 0.05218 = 0.05652 -0.03181 -0.02386 0.01908 AFIX 137 H18A 2 0.906200 0.283575 0.361247 11.00000 -1.50000 H18B 2 0.914771 0.319841 0.247670 11.00000 -1.50000 H18C 2 0.921101 0.198382 0.313651 11.00000 -1.50000 AFIX 0 C19 1 0.714857 0.351580 0.249860 11.00000 0.02880 0.02238 = 0.02216 -0.01193 -0.00628 0.00283 AFIX 43 H19 2 0.753458 0.408021 0.206362 11.00000 -1.20000 AFIX 0 C20 1 0.252974 0.626217 0.275869 11.00000 0.01538 0.01743 = 0.01852 -0.00467 -0.00076 -0.00273 AFIX 43 H20 2 0.287560 0.687924 0.262463 11.00000 -1.20000 AFIX 0 C21 1 0.098068 0.738486 0.202657 11.00000 0.02265 0.02092 = 0.03522 -0.00406 -0.00813 0.00308 AFIX 137 H21A 2 0.125436 0.765023 0.135316 11.00000 -1.50000 H21B 2 0.113480 0.785885 0.232148 11.00000 -1.50000 H21C 2 0.020047 0.733854 0.207619 11.00000 -1.50000 AFIX 0 C22 1 0.098256 0.549538 0.270467 11.00000 0.01669 0.02248 = 0.03353 -0.00321 -0.00480 -0.00444 AFIX 43 H22 2 0.026774 0.556890 0.252848 11.00000 -1.20000 AFIX 0 C23 1 0.148416 0.452330 0.314843 11.00000 0.02394 0.02269 = 0.04137 -0.00488 -0.00827 -0.00869 AFIX 43 H23 2 0.110825 0.392287 0.328528 11.00000 -1.20000 AFIX 0 C24 1 0.252845 0.440627 0.339878 11.00000 0.02259 0.01781 = 0.02942 -0.00501 -0.00654 -0.00326 AFIX 43 H24 2 0.286781 0.373039 0.370597 11.00000 -1.20000 AFIX 0 C25 1 0.308308 0.529397 0.319544 11.00000 0.01424 0.01686 = 0.01479 -0.00472 0.00009 -0.00150 C26 1 0.458035 0.453307 0.410057 11.00000 0.01730 0.01408 = 0.01588 -0.00697 -0.00209 -0.00104 C27 1 0.578083 0.457587 0.409052 11.00000 0.01716 0.01423 = 0.01500 -0.00713 -0.00187 -0.00196 C28 1 0.640580 0.391707 0.481404 11.00000 0.02167 0.01599 = 0.01331 -0.00407 -0.00259 0.00009 AFIX 43 H28 2 0.609479 0.338166 0.535347 11.00000 -1.20000 AFIX 0 C29 1 0.749949 0.406243 0.472747 11.00000 0.02179 0.01972 = 0.01640 -0.00632 -0.00709 0.00375 AFIX 43 H29 2 0.793993 0.363217 0.521883 11.00000 -1.20000 AFIX 0 C30 1 0.794753 0.483241 0.392717 11.00000 0.01637 0.02061 = 0.01954 -0.00847 -0.00533 -0.00007 AFIX 43 H30 2 0.868865 0.494847 0.386950 11.00000 -1.20000 AFIX 0 C31 1 0.728607 0.543029 0.321140 11.00000 0.01661 0.01325 = 0.01707 -0.00699 -0.00293 -0.00032 C32 1 0.765511 0.624718 0.226633 11.00000 0.01574 0.01507 = 0.01689 -0.00778 -0.00087 -0.00176 C33 1 0.711537 0.730419 0.074094 11.00000 0.01406 0.01795 = 0.01685 -0.00640 -0.00121 -0.00164 C34 1 0.679199 0.717689 -0.005183 11.00000 0.01924 0.02227 = 0.02098 -0.01025 -0.00091 -0.00393 AFIX 43 H34 2 0.641952 0.658770 0.003692 11.00000 -1.20000 AFIX 0 C35 1 0.700960 0.789895 -0.095893 11.00000 0.02953 0.02998 = 0.01678 -0.00911 -0.00057 -0.00728 AFIX 43 H35 2 0.681167 0.779443 -0.149465 11.00000 -1.20000 AFIX 0 C36 1 0.751584 0.877405 -0.108634 11.00000 0.02832 0.02598 = 0.01617 -0.00332 0.00001 -0.00292 AFIX 43 H36 2 0.766779 0.927536 -0.170950 11.00000 -1.20000 AFIX 0 C37 1 0.829793 0.986946 -0.045888 11.00000 0.02831 0.01905 = 0.03140 -0.00882 0.00223 -0.00888 AFIX 137 H37A 2 0.860166 1.018300 -0.112089 11.00000 -1.50000 H37B 2 0.887333 0.969463 -0.002944 11.00000 -1.50000 H37C 2 0.775397 1.036536 -0.031641 11.00000 -1.50000 AFIX 0 C38 1 0.760909 0.820504 0.057354 11.00000 0.01814 0.01878 = 0.01695 -0.00756 -0.00005 -0.00196 AFIX 43 H38 2 0.782117 0.832661 0.109575 11.00000 -1.20000 AFIX 0 C40 1 0.924177 0.576091 0.042509 11.00000 0.03692 0.04336 = 0.06238 -0.02967 0.01298 -0.00437 C39 1 0.976279 0.672459 -0.005631 11.00000 0.04079 0.04539 = 0.09387 -0.03351 0.02134 -0.00951 AFIX 137 H39A 2 0.940676 0.715143 -0.063484 11.00000 -1.50000 H39B 2 1.052309 0.656684 -0.022847 11.00000 -1.50000 H39C 2 0.971071 0.710689 0.036897 11.00000 -1.50000 AFIX 0 C42 1 1.073987 0.315842 0.572482 11.00000 0.02831 0.03687 = 0.04387 -0.01258 -0.00225 -0.00774 C41 1 1.178460 0.265927 0.600695 11.00000 0.02790 0.04030 = 0.03628 -0.01920 -0.00486 -0.00388 AFIX 137 H41A 2 1.181646 0.249628 0.668848 11.00000 -1.50000 H41B 2 1.234267 0.312796 0.563984 11.00000 -1.50000 H41C 2 1.190504 0.201420 0.588434 11.00000 -1.50000 AFIX 0 C44 1 0.843998 0.127616 0.636365 11.00000 0.05618 0.03133 = 0.06121 -0.01312 -0.02226 -0.00954 C43 1 0.936936 0.101256 0.582032 11.00000 0.06037 0.04975 = 0.04545 -0.00611 -0.01460 -0.01698 AFIX 137 H43A 2 0.962674 0.165023 0.532058 11.00000 -1.50000 H43B 2 0.917147 0.055296 0.552745 11.00000 -1.50000 H43C 2 0.994144 0.065535 0.624369 11.00000 -1.50000 AFIX 0 N1 5 0.540166 0.985218 0.228042 11.00000 0.02166 0.01408 = 0.01894 -0.00604 -0.00146 -0.00240 N2 5 0.477213 0.760068 0.177213 11.00000 0.01461 0.01415 = 0.01546 -0.00506 -0.00297 -0.00223 N3 5 0.439989 0.624278 0.107896 11.00000 0.01508 0.01658 = 0.01270 -0.00531 -0.00054 -0.00291 N4 5 0.551690 0.448853 0.190288 11.00000 0.01729 0.01512 = 0.01872 -0.00885 -0.00377 -0.00001 N5 5 0.768749 0.268121 0.310975 11.00000 0.03801 0.02947 = 0.03269 -0.01903 -0.01685 0.01178 N6 5 0.151323 0.633752 0.252360 11.00000 0.01570 0.02025 = 0.02241 -0.00392 -0.00222 -0.00027 N7 5 0.416598 0.528717 0.332767 11.00000 0.01431 0.01424 = 0.01419 -0.00334 -0.00153 -0.00133 N8 5 0.622965 0.529545 0.331069 11.00000 0.01463 0.01287 = 0.01470 -0.00615 -0.00283 -0.00120 N9 5 0.689789 0.654453 0.164657 11.00000 0.01565 0.01545 = 0.01466 -0.00480 -0.00132 -0.00462 N10 5 0.779241 0.891228 -0.032302 11.00000 0.02064 0.01752 = 0.01978 -0.00514 0.00041 -0.00271 N11 5 0.882831 0.500681 0.079566 11.00000 0.06098 0.04705 = 0.08046 -0.03299 0.03227 -0.01429 N12 5 0.991378 0.355210 0.551376 11.00000 0.03731 0.06194 = 0.08510 -0.01628 -0.01511 -0.00537 N13 5 0.771624 0.149627 0.679419 11.00000 0.06953 0.05377 = 0.11115 -0.04422 -0.01340 -0.00770 O1 6 0.402349 0.895510 0.048062 11.00000 0.03511 0.01578 = 0.02490 -0.00371 -0.01442 -0.00046 O2 6 0.450351 0.361764 0.130835 11.00000 0.03110 0.01889 = 0.02577 -0.01085 -0.00740 -0.00584 O3 6 0.410547 0.387121 0.478335 11.00000 0.01954 0.01773 = 0.01796 -0.00014 -0.00100 -0.00412 O4 6 0.858411 0.653720 0.214591 11.00000 0.01490 0.02687 = 0.02344 -0.00641 -0.00412 -0.00541 P1 7 0.885019 0.048421 0.183581 11.00000 0.02716 0.02530 = 0.02687 -0.00784 -0.00567 0.00358 F1 4 0.820894 0.156518 0.178222 11.00000 0.04728 0.03741 = 0.03916 -0.02109 -0.01695 0.01476 F2 4 0.991483 0.084943 0.205680 11.00000 0.03891 0.04913 = 0.04548 -0.01459 -0.01890 -0.00148 F3 4 0.920316 0.100327 0.071568 11.00000 0.03929 0.03434 = 0.02940 -0.01093 -0.00206 -0.00630 F4 4 0.948524 -0.059251 0.188013 11.00000 0.04029 0.02480 = 0.06674 -0.00913 0.00311 0.00679 F5 4 0.779123 0.012093 0.159701 11.00000 0.03132 0.04618 = 0.04714 -0.02234 0.00120 -0.00710 F6 4 0.848425 -0.001646 0.294547 11.00000 0.04940 0.05507 = 0.03001 -0.00335 -0.00345 0.00583 P2 7 0.744762 -0.123955 0.603765 11.00000 0.06134 0.04484 = 0.03311 -0.02417 0.00795 -0.02216 F7 4 0.656295 -0.051695 0.627565 11.00000 0.11727 0.22627 = 0.20255 -0.16366 -0.03863 0.08617 F8 4 0.819375 -0.106006 0.672047 11.00000 0.10326 0.07762 = 0.04455 -0.01918 -0.00833 -0.05049 F9 4 0.796384 -0.034542 0.515930 11.00000 0.13253 0.04336 = 0.04726 0.00556 -0.01803 -0.02962 F10 4 0.839467 -0.202717 0.582714 11.00000 0.10260 0.05828 = 0.06883 -0.02204 -0.00355 0.01228 F11 4 0.675198 -0.148146 0.537462 11.00000 0.08306 0.17828 = 0.07130 -0.06916 -0.00303 -0.05414 F12 4 0.700467 -0.221068 0.692491 11.00000 0.14336 0.12498 = 0.04727 -0.04261 0.03138 -0.10083 CO1 3 0.535286 0.594697 0.215475 11.00000 0.01320 0.01271 = 0.01188 -0.00370 -0.00303 -0.00270 HKLF 4 REM 17MA005C2_PM107 in P-1 REM R1 = 0.0497 for 8749 Fo > 4sig(Fo) and 0.0670 for all 11003 data REM 692 parameters refined using 63 restraints END WGHT 0.0498 3.3586 REM Highest difference peak 2.210, deepest hole -0.720, 1-sigma level 0.076 Q1 1 0.6752 -0.0947 0.5793 11.00000 0.05 2.21 Q2 1 0.6964 0.0249 0.5715 11.00000 0.05 0.83 Q3 1 0.6494 -0.1456 0.6717 11.00000 0.05 0.65 Q4 1 0.6027 -0.0799 0.5644 11.00000 0.05 0.63 Q5 1 0.8402 -0.1616 0.6304 11.00000 0.05 0.62 Q6 1 0.7509 -0.2162 0.6104 11.00000 0.05 0.62 Q7 1 0.7171 -0.0586 0.6711 11.00000 0.05 0.55 Q8 1 0.7588 -0.1916 0.5516 11.00000 0.05 0.43 Q9 1 0.4345 0.4911 0.3701 11.00000 0.05 0.38 Q10 1 1.0018 0.3324 0.4984 11.00000 0.05 0.38 Q11 1 0.4133 0.7672 0.0672 11.00000 0.05 0.36 Q12 1 0.5189 0.4500 0.4148 11.00000 0.05 0.36 Q13 1 0.2707 0.5777 0.3063 11.00000 0.05 0.36 Q14 1 0.6818 -0.0807 0.4889 11.00000 0.05 0.34 Q15 1 0.3682 0.5549 0.0723 11.00000 0.05 0.34 Q16 1 0.4614 0.4956 0.1037 11.00000 0.05 0.31 Q17 1 0.7488 0.5813 0.2806 11.00000 0.05 0.31 Q18 1 0.5738 0.4916 0.1995 11.00000 0.05 0.31 Q19 1 1.0617 0.3017 0.5284 11.00000 0.05 0.31 Q20 1 0.3584 0.7248 0.0374 11.00000 0.05 0.30 ; _shelx_res_checksum 68331 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C6 C 0.50755(19) 0.82335(19) 0.22015(17) 0.0151(5) Uani 1 1 d . . . . . C5 C 0.5366(2) 0.77463(19) 0.31414(17) 0.0176(5) Uani 1 1 d . . . . . H5 H 0.537263 0.700969 0.344567 0.021 Uiso 1 1 calc R U . . . C4 C 0.5643(2) 0.8315(2) 0.36344(18) 0.0215(5) Uani 1 1 d . . . . . H4 H 0.582426 0.797418 0.427491 0.026 Uiso 1 1 calc R U . . . C3 C 0.5654(2) 0.9378(2) 0.31902(18) 0.0220(5) Uani 1 1 d . . . . . H3 H 0.583889 0.977733 0.352336 0.026 Uiso 1 1 calc R U . . . C2 C 0.5422(2) 1.0998(2) 0.1831(2) 0.0260(6) Uani 1 1 d . . . . . H2A H 0.483382 1.132382 0.213226 0.039 Uiso 1 1 calc R U . . . H2B H 0.533121 1.122977 0.114942 0.039 Uiso 1 1 calc R U . . . H2C H 0.611278 1.120056 0.191456 0.039 Uiso 1 1 calc R U . . . C1 C 0.5122(2) 0.93201(19) 0.17798(17) 0.0176(5) Uani 1 1 d . . . . . H1 H 0.49551 0.968375 0.113749 0.021 Uiso 1 1 calc R U . . . C7 C 0.42575(19) 0.80204(19) 0.09714(17) 0.0163(5) Uani 1 1 d . . . . . C8 C 0.3912(2) 0.71963(19) 0.06758(16) 0.0168(5) Uani 1 1 d . . . . . C9 C 0.3127(2) 0.7391(2) 0.00493(17) 0.0195(5) Uani 1 1 d . . . . . H9 H 0.279733 0.807393 -0.024697 0.023 Uiso 1 1 calc R U . . . C10 C 0.2837(2) 0.6560(2) -0.01329(18) 0.0223(5) Uani 1 1 d . . . . . H10 H 0.229487 0.666945 -0.055223 0.027 Uiso 1 1 calc R U . . . C11 C 0.3339(2) 0.5571(2) 0.02966(18) 0.0210(5) Uani 1 1 d . . . . . H11 H 0.314149 0.499629 0.018175 0.025 Uiso 1 1 calc R U . . . C12 C 0.41337(19) 0.54423(19) 0.08974(16) 0.0163(5) Uani 1 1 d . . . . . C13 C 0.4743(2) 0.44037(19) 0.14043(17) 0.0170(5) Uani 1 1 d . . . . . C14 C 0.6033(2) 0.3565(2) 0.24940(18) 0.0207(5) Uani 1 1 d . . . . . C15 C 0.5501(3) 0.2709(2) 0.31417(19) 0.0278(6) Uani 1 1 d . . . . . H15 H 0.474293 0.2705 0.315247 0.033 Uiso 1 1 calc R U . . . C16 C 0.6082(3) 0.1871(2) 0.3765(2) 0.0364(8) Uani 1 1 d . . . . . H16 H 0.572054 0.129592 0.421278 0.044 Uiso 1 1 calc R U . . . C17 C 0.7184(3) 0.1869(2) 0.3738(2) 0.0378(8) Uani 1 1 d . . . . . H17 H 0.758477 0.129244 0.416417 0.045 Uiso 1 1 calc R U . . . C18 C 0.8879(3) 0.2674(3) 0.3081(3) 0.0457(9) Uani 1 1 d . . . . . H18A H 0.9062 0.283575 0.361247 0.069 Uiso 1 1 calc R U . . . H18B H 0.914771 0.319841 0.24767 0.069 Uiso 1 1 calc R U . . . H18C H 0.921101 0.198382 0.313651 0.069 Uiso 1 1 calc R U . . . C19 C 0.7149(2) 0.3516(2) 0.24986(19) 0.0234(6) Uani 1 1 d . . . . . H19 H 0.753458 0.408021 0.206362 0.028 Uiso 1 1 calc R U . . . C20 C 0.25297(19) 0.62622(19) 0.27587(17) 0.0177(5) Uani 1 1 d . . . . . H20 H 0.28756 0.687924 0.262463 0.021 Uiso 1 1 calc R U . . . C21 C 0.0981(2) 0.7385(2) 0.2027(2) 0.0282(6) Uani 1 1 d . . . . . H21A H 0.125436 0.765023 0.135316 0.042 Uiso 1 1 calc R U . . . H21B H 0.11348 0.785885 0.232148 0.042 Uiso 1 1 calc R U . . . H21C H 0.020047 0.733854 0.207619 0.042 Uiso 1 1 calc R U . . . C22 C 0.0983(2) 0.5495(2) 0.2705(2) 0.0260(6) Uani 1 1 d . . . . . H22 H 0.026774 0.55689 0.252848 0.031 Uiso 1 1 calc R U . . . C23 C 0.1484(2) 0.4523(2) 0.3148(2) 0.0305(6) Uani 1 1 d . . . . . H23 H 0.110825 0.392287 0.328528 0.037 Uiso 1 1 calc R U . . . C24 C 0.2528(2) 0.4406(2) 0.33988(19) 0.0239(6) Uani 1 1 d . . . . . H24 H 0.286781 0.373039 0.370597 0.029 Uiso 1 1 calc R U . . . C25 C 0.30831(19) 0.52940(19) 0.31954(16) 0.0158(5) Uani 1 1 d . . . . . C26 C 0.45804(19) 0.45331(18) 0.41006(16) 0.0153(5) Uani 1 1 d . . . . . C27 C 0.57808(19) 0.45759(18) 0.40905(16) 0.0149(5) Uani 1 1 d . . . . . C28 C 0.6406(2) 0.39171(19) 0.48140(17) 0.0175(5) Uani 1 1 d . . . . . H28 H 0.609479 0.338166 0.535347 0.021 Uiso 1 1 calc R U . . . C29 C 0.7499(2) 0.4062(2) 0.47275(17) 0.0194(5) Uani 1 1 d . . . . . H29 H 0.793993 0.363217 0.521883 0.023 Uiso 1 1 calc R U . . . C30 C 0.7948(2) 0.4832(2) 0.39272(17) 0.0183(5) Uani 1 1 d . . . . . H30 H 0.868865 0.494847 0.38695 0.022 Uiso 1 1 calc R U . . . C31 C 0.72861(19) 0.54303(18) 0.32114(17) 0.0152(5) Uani 1 1 d . . . . . C32 C 0.76551(19) 0.62472(19) 0.22663(17) 0.0154(5) Uani 1 1 d . . . . . C33 C 0.71154(19) 0.73042(19) 0.07409(17) 0.0163(5) Uani 1 1 d . . . . . C34 C 0.6792(2) 0.7177(2) -0.00518(17) 0.0201(5) Uani 1 1 d . . . . . H34 H 0.641952 0.65877 0.003692 0.024 Uiso 1 1 calc R U . . . C35 C 0.7010(2) 0.7899(2) -0.09589(18) 0.0250(6) Uani 1 1 d . . . . . H35 H 0.681167 0.779443 -0.149465 0.03 Uiso 1 1 calc R U . . . C36 C 0.7516(2) 0.8774(2) -0.10863(18) 0.0250(6) Uani 1 1 d . . . . . H36 H 0.766779 0.927536 -0.17095 0.03 Uiso 1 1 calc R U . . . C37 C 0.8298(2) 0.9869(2) -0.0459(2) 0.0263(6) Uani 1 1 d . . . . . H37A H 0.860166 1.0183 -0.112089 0.039 Uiso 1 1 calc R U . . . H37B H 0.887333 0.969463 -0.002944 0.039 Uiso 1 1 calc R U . . . H37C H 0.775397 1.036536 -0.031641 0.039 Uiso 1 1 calc R U . . . C38 C 0.7609(2) 0.82050(19) 0.05735(17) 0.0178(5) Uani 1 1 d . . . . . H38 H 0.782117 0.832661 0.109575 0.021 Uiso 1 1 calc R U . . . C40 C 0.9242(3) 0.5761(3) 0.0425(3) 0.0460(9) Uani 1 1 d . . . . . C39 C 0.9763(3) 0.6725(3) -0.0056(3) 0.0597(11) Uani 1 1 d . . . . . H39A H 0.940676 0.715143 -0.063484 0.09 Uiso 1 1 calc R U . . . H39B H 1.052309 0.656684 -0.022847 0.09 Uiso 1 1 calc R U . . . H39C H 0.971071 0.710689 0.036897 0.09 Uiso 1 1 calc R U . . . C42 C 1.0740(3) 0.3158(3) 0.5725(2) 0.0368(7) Uani 1 1 d . . . . . C41 C 1.1785(2) 0.2659(3) 0.6007(2) 0.0331(7) Uani 1 1 d . . . . . H41A H 1.181646 0.249628 0.668848 0.05 Uiso 1 1 calc R U . . . H41B H 1.234267 0.312796 0.563984 0.05 Uiso 1 1 calc R U . . . H41C H 1.190504 0.20142 0.588434 0.05 Uiso 1 1 calc R U . . . C44 C 0.8440(4) 0.1276(3) 0.6364(3) 0.0488(9) Uani 1 1 d . . . . . C43 C 0.9369(3) 0.1013(3) 0.5820(3) 0.0535(10) Uani 1 1 d . . . . . H43A H 0.962674 0.165023 0.532058 0.08 Uiso 1 1 calc R U . . . H43B H 0.917147 0.055296 0.552745 0.08 Uiso 1 1 calc R U . . . H43C H 0.994144 0.065535 0.624369 0.08 Uiso 1 1 calc R U . . . N1 N 0.54017(17) 0.98522(16) 0.22804(14) 0.0182(4) Uani 1 1 d . . . . . N2 N 0.47721(16) 0.76007(15) 0.17721(14) 0.0147(4) Uani 1 1 d . . . . . N3 N 0.43999(16) 0.62428(16) 0.10790(13) 0.0148(4) Uani 1 1 d . . . . . N4 N 0.55169(16) 0.44885(16) 0.19029(14) 0.0162(4) Uani 1 1 d . . . . . N5 N 0.7687(2) 0.26812(19) 0.31098(17) 0.0312(6) Uani 1 1 d . . . . . N6 N 0.15132(17) 0.63375(17) 0.25236(15) 0.0208(5) Uani 1 1 d . . . . . N7 N 0.41660(16) 0.52872(15) 0.33277(14) 0.0148(4) Uani 1 1 d . . . . . N8 N 0.62297(16) 0.52955(15) 0.33107(13) 0.0136(4) Uani 1 1 d . . . . . N9 N 0.68979(16) 0.65445(16) 0.16466(14) 0.0152(4) Uani 1 1 d . . . . . N10 N 0.77924(17) 0.89123(16) -0.03230(15) 0.0200(4) Uani 1 1 d . . . . . N11 N 0.8828(3) 0.5007(3) 0.0796(3) 0.0627(10) Uani 1 1 d . . . . . N12 N 0.9914(3) 0.3552(3) 0.5514(3) 0.0639(10) Uani 1 1 d . . . . . N13 N 0.7716(3) 0.1496(3) 0.6794(3) 0.0734(11) Uani 1 1 d . . . . . O1 O 0.40235(16) 0.89551(14) 0.04806(13) 0.0255(4) Uani 1 1 d . . . . . O2 O 0.45035(15) 0.36176(14) 0.13083(13) 0.0237(4) Uani 1 1 d . . . . . O3 O 0.41055(14) 0.38712(13) 0.47833(12) 0.0203(4) Uani 1 1 d . . . . . O4 O 0.85841(14) 0.65372(14) 0.21459(13) 0.0221(4) Uani 1 1 d . . . . . P1 P 0.88502(6) 0.04842(6) 0.18358(5) 0.02725(17) Uani 1 1 d . . . . . F1 F 0.82089(15) 0.15652(14) 0.17822(13) 0.0396(4) Uani 1 1 d . . . . . F2 F 0.99148(15) 0.08494(16) 0.20568(14) 0.0443(5) Uani 1 1 d . . . . . F3 F 0.92032(14) 0.10033(14) 0.07157(12) 0.0345(4) Uani 1 1 d . . . . . F4 F 0.94852(16) -0.05925(14) 0.18801(15) 0.0479(5) Uani 1 1 d . . . . . F5 F 0.77912(14) 0.01209(15) 0.15970(13) 0.0402(4) Uani 1 1 d . . . . . F6 F 0.84842(17) -0.00165(17) 0.29455(13) 0.0496(5) Uani 1 1 d . . . . . P2 P 0.74476(8) -0.12396(7) 0.60376(6) 0.0431(2) Uani 1 1 d . . . . . F7 F 0.6563(3) -0.0517(4) 0.6276(4) 0.163(2) Uani 1 1 d . . . . . F8 F 0.8194(2) -0.1060(2) 0.67205(16) 0.0724(8) Uani 1 1 d . . . . . F9 F 0.7964(3) -0.03454(18) 0.51593(17) 0.0784(8) Uani 1 1 d . . . . . F10 F 0.8395(2) -0.2027(2) 0.58271(19) 0.0791(8) Uani 1 1 d . . . . . F11 F 0.6752(2) -0.1481(3) 0.5375(2) 0.1007(11) Uani 1 1 d . . . . . F12 F 0.7005(3) -0.2211(3) 0.69249(17) 0.0978(11) Uani 1 1 d . . . . . Co1 Co 0.53529(3) 0.59470(2) 0.21547(2) 0.01256(9) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C6 0.0118(11) 0.0161(12) 0.0181(11) -0.0070(10) -0.0009(9) -0.0020(9) C5 0.0183(12) 0.0155(12) 0.0178(12) -0.0041(10) -0.0019(9) -0.0035(10) C4 0.0259(14) 0.0211(13) 0.0171(12) -0.0065(10) -0.0041(10) -0.0011(11) C3 0.0274(14) 0.0225(13) 0.0196(12) -0.0103(11) -0.0046(10) -0.0044(11) C2 0.0367(16) 0.0151(13) 0.0266(14) -0.0066(11) -0.0066(12) -0.0037(12) C1 0.0195(12) 0.0178(12) 0.0158(11) -0.0057(10) -0.0023(9) -0.0039(10) C7 0.0163(12) 0.0159(12) 0.0159(11) -0.0045(10) -0.0024(9) -0.0020(10) C8 0.0185(12) 0.0168(12) 0.0135(11) -0.0032(9) -0.0011(9) -0.0043(10) C9 0.0200(13) 0.0214(13) 0.0160(11) -0.0051(10) -0.0051(10) -0.0003(10) C10 0.0198(13) 0.0299(14) 0.0191(12) -0.0095(11) -0.0068(10) -0.0032(11) C11 0.0200(13) 0.0265(14) 0.0208(12) -0.0121(11) -0.0026(10) -0.0067(11) C12 0.0166(12) 0.0192(12) 0.0141(11) -0.0072(10) 0.0006(9) -0.0041(10) C13 0.0179(12) 0.0186(12) 0.0160(11) -0.0078(10) -0.0001(9) -0.0039(10) C14 0.0279(14) 0.0176(12) 0.0207(12) -0.0112(10) -0.0056(10) 0.0005(11) C15 0.0390(17) 0.0217(14) 0.0252(14) -0.0109(12) -0.0042(12) -0.0042(12) C16 0.067(2) 0.0174(14) 0.0258(15) -0.0069(12) -0.0090(15) -0.0069(14) C17 0.062(2) 0.0211(15) 0.0334(16) -0.0114(13) -0.0226(16) 0.0095(15) C18 0.0383(19) 0.052(2) 0.057(2) -0.0318(19) -0.0239(17) 0.0191(17) C19 0.0288(14) 0.0224(13) 0.0222(13) -0.0119(11) -0.0063(11) 0.0028(11) C20 0.0154(12) 0.0174(12) 0.0185(12) -0.0047(10) -0.0008(9) -0.0027(10) C21 0.0227(14) 0.0209(14) 0.0352(15) -0.0041(12) -0.0081(12) 0.0031(11) C22 0.0167(13) 0.0225(14) 0.0335(15) -0.0032(12) -0.0048(11) -0.0044(11) C23 0.0239(14) 0.0227(14) 0.0414(17) -0.0049(13) -0.0083(12) -0.0087(12) C24 0.0226(13) 0.0178(13) 0.0294(14) -0.0050(11) -0.0065(11) -0.0033(11) C25 0.0142(11) 0.0169(12) 0.0148(11) -0.0047(9) 0.0001(9) -0.0015(9) C26 0.0173(12) 0.0141(11) 0.0159(11) -0.0070(9) -0.0021(9) -0.0010(9) C27 0.0172(12) 0.0142(11) 0.0150(11) -0.0071(9) -0.0019(9) -0.0020(9) C28 0.0217(13) 0.0160(12) 0.0133(11) -0.0041(10) -0.0026(9) 0.0001(10) C29 0.0218(13) 0.0197(13) 0.0164(11) -0.0063(10) -0.0071(10) 0.0037(10) C30 0.0164(12) 0.0206(13) 0.0195(12) -0.0085(10) -0.0053(10) -0.0001(10) C31 0.0166(12) 0.0132(11) 0.0171(11) -0.0070(9) -0.0029(9) -0.0003(9) C32 0.0157(12) 0.0151(12) 0.0169(11) -0.0078(10) -0.0009(9) -0.0018(9) C33 0.0141(11) 0.0179(12) 0.0169(11) -0.0064(10) -0.0012(9) -0.0016(10) C34 0.0192(12) 0.0223(13) 0.0210(12) -0.0102(11) -0.0009(10) -0.0039(10) C35 0.0295(15) 0.0300(15) 0.0168(12) -0.0091(11) -0.0006(11) -0.0073(12) C36 0.0283(14) 0.0260(14) 0.0162(12) -0.0033(11) 0.0000(10) -0.0029(12) C37 0.0283(15) 0.0190(13) 0.0314(15) -0.0088(12) 0.0022(12) -0.0089(11) C38 0.0181(12) 0.0188(12) 0.0169(12) -0.0076(10) -0.0001(9) -0.0020(10) C40 0.0369(19) 0.043(2) 0.062(2) -0.0297(19) 0.0130(17) -0.0044(16) C39 0.041(2) 0.045(2) 0.094(3) -0.034(2) 0.021(2) -0.0095(18) C42 0.0283(17) 0.0369(18) 0.0439(18) -0.0126(15) -0.0022(14) -0.0077(14) C41 0.0279(15) 0.0403(18) 0.0363(16) -0.0192(14) -0.0049(13) -0.0039(13) C44 0.056(2) 0.0313(19) 0.061(2) -0.0131(18) -0.022(2) -0.0095(18) C43 0.060(3) 0.050(2) 0.045(2) -0.0061(18) -0.0146(19) -0.0170(19) N1 0.0217(11) 0.0141(10) 0.0189(10) -0.0060(8) -0.0015(8) -0.0024(9) N2 0.0146(10) 0.0141(10) 0.0155(9) -0.0051(8) -0.0030(8) -0.0022(8) N3 0.0151(10) 0.0166(10) 0.0127(9) -0.0053(8) -0.0005(8) -0.0029(8) N4 0.0173(10) 0.0151(10) 0.0187(10) -0.0089(8) -0.0038(8) 0.0000(8) N5 0.0380(14) 0.0295(13) 0.0327(13) -0.0190(11) -0.0168(11) 0.0118(11) N6 0.0157(10) 0.0203(11) 0.0224(11) -0.0039(9) -0.0022(8) -0.0003(9) N7 0.0143(10) 0.0142(10) 0.0142(9) -0.0033(8) -0.0015(8) -0.0013(8) N8 0.0146(10) 0.0129(10) 0.0147(9) -0.0061(8) -0.0028(8) -0.0012(8) N9 0.0157(10) 0.0154(10) 0.0147(9) -0.0048(8) -0.0013(8) -0.0046(8) N10 0.0206(11) 0.0175(11) 0.0198(10) -0.0051(9) 0.0004(8) -0.0027(9) N11 0.061(2) 0.047(2) 0.080(3) -0.0330(19) 0.0323(19) -0.0143(17) N12 0.0373(18) 0.062(2) 0.085(3) -0.016(2) -0.0151(18) -0.0054(16) N13 0.070(3) 0.054(2) 0.111(3) -0.044(2) -0.013(2) -0.008(2) O1 0.0351(11) 0.0158(9) 0.0249(10) -0.0037(8) -0.0144(8) -0.0005(8) O2 0.0311(10) 0.0189(9) 0.0258(9) -0.0109(8) -0.0074(8) -0.0058(8) O3 0.0195(9) 0.0177(9) 0.0180(9) -0.0001(7) -0.0010(7) -0.0041(7) O4 0.0149(9) 0.0269(10) 0.0234(9) -0.0064(8) -0.0041(7) -0.0054(8) P1 0.0272(4) 0.0253(4) 0.0269(4) -0.0078(3) -0.0057(3) 0.0036(3) F1 0.0473(11) 0.0374(10) 0.0392(10) -0.0211(9) -0.0170(8) 0.0148(9) F2 0.0389(11) 0.0491(12) 0.0455(11) -0.0146(9) -0.0189(9) -0.0015(9) F3 0.0393(10) 0.0343(10) 0.0294(9) -0.0109(8) -0.0021(7) -0.0063(8) F4 0.0403(11) 0.0248(9) 0.0667(13) -0.0091(9) 0.0031(10) 0.0068(8) F5 0.0313(10) 0.0462(11) 0.0471(11) -0.0223(9) 0.0012(8) -0.0071(8) F6 0.0494(12) 0.0551(13) 0.0300(10) -0.0034(9) -0.0034(9) 0.0058(10) P2 0.0613(6) 0.0448(5) 0.0331(4) -0.0242(4) 0.0080(4) -0.0222(5) F7 0.117(3) 0.226(5) 0.203(4) -0.164(4) -0.039(3) 0.086(3) F8 0.103(2) 0.0776(17) 0.0446(13) -0.0192(12) -0.0083(13) -0.0505(15) F9 0.133(2) 0.0434(13) 0.0473(13) 0.0056(11) -0.0180(14) -0.0296(15) F10 0.103(2) 0.0583(15) 0.0688(17) -0.0220(13) -0.0036(15) 0.0123(15) F11 0.083(2) 0.178(3) 0.0713(18) -0.069(2) -0.0030(15) -0.054(2) F12 0.143(3) 0.125(2) 0.0473(14) -0.0426(15) 0.0314(15) -0.101(2) Co1 0.01320(16) 0.01271(16) 0.01188(15) -0.00370(12) -0.00303(11) -0.00270(12) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.0214 1 0 0 0.0214 0 -1 0 0.041 0 1 0 0.041 -1 -1 -5 0.1488 -3 5 4 0.072 1 3 5 0.1498 0 5 3 0.0793 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C6 C5 117.4(2) . . ? N2 C6 C1 126.1(2) . . ? C5 C6 C1 116.5(2) . . ? C4 C5 C6 121.4(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C3 C4 119.8(2) . . ? N1 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C1 C6 120.6(2) . . ? N1 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? O1 C7 N2 129.5(2) . . ? O1 C7 C8 118.6(2) . . ? N2 C7 C8 111.9(2) . . ? N3 C8 C9 121.4(2) . . ? N3 C8 C7 115.3(2) . . ? C9 C8 C7 123.2(2) . . ? C8 C9 C10 118.1(2) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 118.4(2) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? N3 C12 C11 121.2(2) . . ? N3 C12 C13 115.4(2) . . ? C11 C12 C13 123.4(2) . . ? O2 C13 N4 128.6(2) . . ? O2 C13 C12 119.1(2) . . ? N4 C13 C12 112.3(2) . . ? C19 C14 N4 117.9(2) . . ? C19 C14 C15 117.4(2) . . ? N4 C14 C15 124.5(3) . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? N5 C17 C16 119.7(3) . . ? N5 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C14 121.0(3) . . ? N5 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? N6 C20 C25 121.2(2) . . ? N6 C20 H20 119.4 . . ? C25 C20 H20 119.4 . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C23 119.2(2) . . ? N6 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 120.9(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C25 119.5(2) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C20 C25 N7 117.3(2) . . ? C20 C25 C24 117.2(2) . . ? N7 C25 C24 125.3(2) . . ? O3 C26 N7 128.6(2) . . ? O3 C26 C27 119.3(2) . . ? N7 C26 C27 112.1(2) . . ? N8 C27 C28 120.7(2) . . ? N8 C27 C26 115.0(2) . . ? C28 C27 C26 124.2(2) . . ? C27 C28 C29 118.3(2) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 118.4(2) . . ? C29 C30 H30 120.8 . . ? C31 C30 H30 120.8 . . ? N8 C31 C30 120.8(2) . . ? N8 C31 C32 113.9(2) . . ? C30 C31 C32 125.3(2) . . ? O4 C32 N9 128.7(2) . . ? O4 C32 C31 119.3(2) . . ? N9 C32 C31 112.0(2) . . ? C38 C33 N9 123.9(2) . . ? C38 C33 C34 117.2(2) . . ? N9 C33 C34 118.8(2) . . ? C35 C34 C33 120.6(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.8(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? N10 C36 C35 119.5(2) . . ? N10 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? N10 C37 H37A 109.5 . . ? N10 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N10 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N10 C38 C33 120.9(2) . . ? N10 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? N11 C40 C39 179.4(5) . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N12 C42 C41 179.1(4) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N13 C44 C43 178.8(4) . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C3 N1 C1 122.4(2) . . ? C3 N1 C2 117.9(2) . . ? C1 N1 C2 119.7(2) . . ? C7 N2 C6 120.4(2) . . ? C7 N2 Co1 114.75(15) . . ? C6 N2 Co1 123.75(15) . . ? C12 N3 C8 120.8(2) . . ? C12 N3 Co1 118.77(16) . . ? C8 N3 Co1 119.55(16) . . ? C13 N4 C14 117.0(2) . . ? C13 N4 Co1 114.14(16) . . ? C14 N4 Co1 123.69(15) . . ? C17 N5 C19 121.9(3) . . ? C17 N5 C18 119.5(3) . . ? C19 N5 C18 118.5(3) . . ? C22 N6 C20 122.0(2) . . ? C22 N6 C21 119.2(2) . . ? C20 N6 C21 118.8(2) . . ? C26 N7 C25 118.7(2) . . ? C26 N7 Co1 113.95(16) . . ? C25 N7 Co1 122.40(15) . . ? C27 N8 C31 121.4(2) . . ? C27 N8 Co1 117.53(15) . . ? C31 N8 Co1 119.56(16) . . ? C32 N9 C33 118.8(2) . . ? C32 N9 Co1 117.56(16) . . ? C33 N9 Co1 123.25(15) . . ? C36 N10 C38 121.9(2) . . ? C36 N10 C37 119.4(2) . . ? C38 N10 C37 118.7(2) . . ? F6 P1 F4 90.62(11) . . ? F6 P1 F2 90.78(11) . . ? F4 P1 F2 90.20(11) . . ? F6 P1 F1 89.78(11) . . ? F4 P1 F1 179.46(12) . . ? F2 P1 F1 90.16(11) . . ? F6 P1 F3 179.07(11) . . ? F4 P1 F3 90.26(11) . . ? F2 P1 F3 89.54(10) . . ? F1 P1 F3 89.34(10) . . ? F6 P1 F5 90.12(11) . . ? F4 P1 F5 89.53(11) . . ? F2 P1 F5 179.07(11) . . ? F1 P1 F5 90.10(10) . . ? F3 P1 F5 89.57(10) . . ? F7 P2 F11 93.5(2) . . ? F7 P2 F9 94.1(3) . . ? F11 P2 F9 90.82(16) . . ? F7 P2 F8 89.7(2) . . ? F11 P2 F8 176.53(19) . . ? F9 P2 F8 90.43(13) . . ? F7 P2 F12 90.4(3) . . ? F11 P2 F12 89.71(16) . . ? F9 P2 F12 175.4(2) . . ? F8 P2 F12 88.79(13) . . ? F7 P2 F10 177.8(2) . . ? F11 P2 F10 88.03(17) . . ? F9 P2 F10 87.43(16) . . ? F8 P2 F10 88.79(16) . . ? F12 P2 F10 88.03(17) . . ? N3 Co1 N8 166.40(8) . . ? N3 Co1 N9 112.35(8) . . ? N8 Co1 N9 75.88(8) . . ? N3 Co1 N7 97.52(8) . . ? N8 Co1 N7 76.05(8) . . ? N9 Co1 N7 149.55(7) . . ? N3 Co1 N4 75.85(8) . . ? N8 Co1 N4 91.94(7) . . ? N9 Co1 N4 103.21(8) . . ? N7 Co1 N4 89.30(8) . . ? N3 Co1 N2 75.92(8) . . ? N8 Co1 N2 116.52(7) . . ? N9 Co1 N2 84.22(8) . . ? N7 Co1 N2 97.97(8) . . ? N4 Co1 N2 151.53(7) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C6 N2 1.394(3) . ? C6 C5 1.403(3) . ? C6 C1 1.405(3) . ? C5 C4 1.382(3) . ? C5 H5 0.95 . ? C4 C3 1.373(4) . ? C4 H4 0.95 . ? C3 N1 1.347(3) . ? C3 H3 0.95 . ? C2 N1 1.479(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C1 N1 1.351(3) . ? C1 H1 0.95 . ? C7 O1 1.248(3) . ? C7 N2 1.343(3) . ? C7 C8 1.511(3) . ? C8 N3 1.338(3) . ? C8 C9 1.386(3) . ? C9 C10 1.390(4) . ? C9 H9 0.95 . ? C10 C11 1.388(4) . ? C10 H10 0.95 . ? C11 C12 1.386(3) . ? C11 H11 0.95 . ? C12 N3 1.337(3) . ? C12 C13 1.516(3) . ? C13 O2 1.237(3) . ? C13 N4 1.347(3) . ? C14 C19 1.393(4) . ? C14 N4 1.393(3) . ? C14 C15 1.401(4) . ? C15 C16 1.382(4) . ? C15 H15 0.95 . ? C16 C17 1.378(5) . ? C16 H16 0.95 . ? C17 N5 1.335(4) . ? C17 H17 0.95 . ? C18 N5 1.488(4) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 N5 1.346(3) . ? C19 H19 0.95 . ? C20 N6 1.348(3) . ? C20 C25 1.395(3) . ? C20 H20 0.95 . ? C21 N6 1.481(3) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 N6 1.338(3) . ? C22 C23 1.374(4) . ? C22 H22 0.95 . ? C23 C24 1.383(4) . ? C23 H23 0.95 . ? C24 C25 1.403(3) . ? C24 H24 0.95 . ? C25 N7 1.396(3) . ? C26 O3 1.236(3) . ? C26 N7 1.352(3) . ? C26 C27 1.512(3) . ? C27 N8 1.337(3) . ? C27 C28 1.391(3) . ? C28 C29 1.393(4) . ? C28 H28 0.95 . ? C29 C30 1.386(4) . ? C29 H29 0.95 . ? C30 C31 1.389(3) . ? C30 H30 0.95 . ? C31 N8 1.342(3) . ? C31 C32 1.511(3) . ? C32 O4 1.248(3) . ? C32 N9 1.339(3) . ? C33 C38 1.388(3) . ? C33 N9 1.397(3) . ? C33 C34 1.402(3) . ? C34 C35 1.378(4) . ? C34 H34 0.95 . ? C35 C36 1.380(4) . ? C35 H35 0.95 . ? C36 N10 1.343(3) . ? C36 H36 0.95 . ? C37 N10 1.478(3) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 N10 1.353(3) . ? C38 H38 0.95 . ? C40 N11 1.137(5) . ? C40 C39 1.450(5) . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C42 N12 1.135(4) . ? C42 C41 1.441(4) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C44 N13 1.138(6) . ? C44 C43 1.442(6) . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? N2 Co1 2.205(2) . ? N3 Co1 2.0334(19) . ? N4 Co1 2.196(2) . ? N7 Co1 2.160(2) . ? N8 Co1 2.0361(19) . ? N9 Co1 2.137(2) . ? P1 F6 1.593(2) . ? P1 F4 1.5967(19) . ? P1 F2 1.601(2) . ? P1 F1 1.6013(18) . ? P1 F3 1.6048(18) . ? P1 F5 1.6049(19) . ? P2 F7 1.517(3) . ? P2 F11 1.566(3) . ? P2 F9 1.568(2) . ? P2 F8 1.588(2) . ? P2 F12 1.598(3) . ? P2 F10 1.611(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C6 C5 C4 -177.8(2) . . . . ? C1 C6 C5 C4 2.4(4) . . . . ? C6 C5 C4 C3 -1.2(4) . . . . ? C5 C4 C3 N1 -0.4(4) . . . . ? N2 C6 C1 N1 178.2(2) . . . . ? C5 C6 C1 N1 -2.0(4) . . . . ? O1 C7 C8 N3 164.5(2) . . . . ? N2 C7 C8 N3 -16.9(3) . . . . ? O1 C7 C8 C9 -17.0(4) . . . . ? N2 C7 C8 C9 161.6(2) . . . . ? N3 C8 C9 C10 1.6(4) . . . . ? C7 C8 C9 C10 -176.8(2) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C9 C10 C11 C12 -0.6(4) . . . . ? C10 C11 C12 N3 1.4(4) . . . . ? C10 C11 C12 C13 -179.7(2) . . . . ? N3 C12 C13 O2 176.5(2) . . . . ? C11 C12 C13 O2 -2.4(4) . . . . ? N3 C12 C13 N4 -4.7(3) . . . . ? C11 C12 C13 N4 176.4(2) . . . . ? C19 C14 C15 C16 1.3(4) . . . . ? N4 C14 C15 C16 -173.3(2) . . . . ? C14 C15 C16 C17 -1.2(4) . . . . ? C15 C16 C17 N5 0.3(4) . . . . ? N4 C14 C19 N5 174.4(2) . . . . ? C15 C14 C19 N5 -0.6(4) . . . . ? N6 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? N6 C20 C25 N7 173.8(2) . . . . ? N6 C20 C25 C24 -1.5(4) . . . . ? C23 C24 C25 C20 1.1(4) . . . . ? C23 C24 C25 N7 -173.7(3) . . . . ? O3 C26 C27 N8 178.1(2) . . . . ? N7 C26 C27 N8 -3.7(3) . . . . ? O3 C26 C27 C28 -0.7(4) . . . . ? N7 C26 C27 C28 177.6(2) . . . . ? N8 C27 C28 C29 3.3(3) . . . . ? C26 C27 C28 C29 -178.1(2) . . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C28 C29 C30 C31 -1.6(4) . . . . ? C29 C30 C31 N8 2.8(4) . . . . ? C29 C30 C31 C32 -175.5(2) . . . . ? N8 C31 C32 O4 170.4(2) . . . . ? C30 C31 C32 O4 -11.2(4) . . . . ? N8 C31 C32 N9 -11.2(3) . . . . ? C30 C31 C32 N9 167.3(2) . . . . ? C38 C33 C34 C35 3.1(4) . . . . ? N9 C33 C34 C35 -178.8(2) . . . . ? C33 C34 C35 C36 -2.3(4) . . . . ? C34 C35 C36 N10 0.1(4) . . . . ? N9 C33 C38 N10 -179.7(2) . . . . ? C34 C33 C38 N10 -1.7(4) . . . . ? C4 C3 N1 C1 0.7(4) . . . . ? C4 C3 N1 C2 179.9(2) . . . . ? C6 C1 N1 C3 0.5(4) . . . . ? C6 C1 N1 C2 -178.6(2) . . . . ? O1 C7 N2 C6 3.7(4) . . . . ? C8 C7 N2 C6 -174.7(2) . . . . ? O1 C7 N2 Co1 -164.9(2) . . . . ? C8 C7 N2 Co1 16.7(3) . . . . ? C5 C6 N2 C7 164.8(2) . . . . ? C1 C6 N2 C7 -15.4(4) . . . . ? C5 C6 N2 Co1 -27.6(3) . . . . ? C1 C6 N2 Co1 152.2(2) . . . . ? C11 C12 N3 C8 -0.7(4) . . . . ? C13 C12 N3 C8 -179.7(2) . . . . ? C11 C12 N3 Co1 168.23(18) . . . . ? C13 C12 N3 Co1 -10.7(3) . . . . ? C9 C8 N3 C12 -0.9(4) . . . . ? C7 C8 N3 C12 177.7(2) . . . . ? C9 C8 N3 Co1 -169.73(18) . . . . ? C7 C8 N3 Co1 8.8(3) . . . . ? O2 C13 N4 C14 -9.4(4) . . . . ? C12 C13 N4 C14 172.0(2) . . . . ? O2 C13 N4 Co1 -165.0(2) . . . . ? C12 C13 N4 Co1 16.3(2) . . . . ? C19 C14 N4 C13 136.9(2) . . . . ? C15 C14 N4 C13 -48.4(3) . . . . ? C19 C14 N4 Co1 -69.9(3) . . . . ? C15 C14 N4 Co1 104.7(3) . . . . ? C16 C17 N5 C19 0.5(4) . . . . ? C16 C17 N5 C18 -179.8(3) . . . . ? C14 C19 N5 C17 -0.3(4) . . . . ? C14 C19 N5 C18 -180.0(2) . . . . ? C23 C22 N6 C20 0.4(4) . . . . ? C23 C22 N6 C21 178.7(3) . . . . ? C25 C20 N6 C22 0.7(4) . . . . ? C25 C20 N6 C21 -177.6(2) . . . . ? O3 C26 N7 C25 -7.3(4) . . . . ? C27 C26 N7 C25 174.69(19) . . . . ? O3 C26 N7 Co1 -163.0(2) . . . . ? C27 C26 N7 Co1 18.9(2) . . . . ? C20 C25 N7 C26 147.4(2) . . . . ? C24 C25 N7 C26 -37.8(3) . . . . ? C20 C25 N7 Co1 -59.0(3) . . . . ? C24 C25 N7 Co1 115.8(2) . . . . ? C28 C27 N8 C31 -2.2(3) . . . . ? C26 C27 N8 C31 179.1(2) . . . . ? C28 C27 N8 Co1 163.98(18) . . . . ? C26 C27 N8 Co1 -14.8(3) . . . . ? C30 C31 N8 C27 -1.0(3) . . . . ? C32 C31 N8 C27 177.5(2) . . . . ? C30 C31 N8 Co1 -166.83(18) . . . . ? C32 C31 N8 Co1 11.7(3) . . . . ? O4 C32 N9 C33 -2.3(4) . . . . ? C31 C32 N9 C33 179.5(2) . . . . ? O4 C32 N9 Co1 -175.7(2) . . . . ? C31 C32 N9 Co1 6.1(3) . . . . ? C38 C33 N9 C32 -43.5(3) . . . . ? C34 C33 N9 C32 138.5(2) . . . . ? C38 C33 N9 Co1 129.5(2) . . . . ? C34 C33 N9 Co1 -48.5(3) . . . . ? C35 C36 N10 C38 1.4(4) . . . . ? C35 C36 N10 C37 -177.7(3) . . . . ? C33 C38 N10 C36 -0.5(4) . . . . ? C33 C38 N10 C37 178.6(2) . . . . ?