# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_stahl108 _database_code_depnum_ccdc_archive 'CCDC 885442' #TrackingRef 'stahl108_MOD.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H31 Co2 N10 O2, 3(F6 P), 2(C H2 Cl2)' _chemical_formula_sum 'C45 H35 Cl4 Co2 F18 N10 O2 P3' _chemical_formula_weight 1442.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6543(6) _cell_length_b 24.2520(10) _cell_length_c 18.6535(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.437(2) _cell_angle_gamma 90.00 _cell_volume 6158.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.4506 _cell_measurement_theta_max 25.6907 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2007) ; _exptl_absorpt_correction_T_min 0.8017 _exptl_absorpt_correction_T_max 0.8856 _exptl_special_details ? _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source . _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.60\% \w and 0.6\% \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 83280 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10763 _reflns_number_gt 8592 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT Ver. 7.24A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT Ver. 7.24A' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL, OLEX2 (Dolomanov et al., 2009)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+11.5809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10763 _refine_ls_number_parameters 780 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1823 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.90106(4) 0.08456(2) 0.84405(3) 0.02015(16) Uani 1 1 d . . . Co2 Co 0.79912(4) -0.04507(2) 0.74736(3) 0.02506(17) Uani 1 1 d . . . O1 O 0.9510(2) 0.01362(13) 0.81973(16) 0.0273(7) Uani 1 1 d . . . O2 O 0.8893(2) -0.02972(13) 0.82797(16) 0.0304(7) Uani 1 1 d . . . N1 N 0.9818(3) 0.11420(16) 0.77099(18) 0.0257(8) Uani 1 1 d . . . N2 N 1.0168(2) 0.09384(14) 0.90210(18) 0.0220(7) Uani 1 1 d . . . N3 N 0.8521(3) 0.06280(15) 0.93443(18) 0.0235(7) Uani 1 1 d . . . N4 N 0.8384(2) 0.15947(14) 0.85102(18) 0.0221(7) Uani 1 1 d . . . N5 N 0.7849(2) 0.07250(14) 0.78564(18) 0.0219(7) Uani 1 1 d . . . N6 N 0.7532(2) 0.02888(15) 0.74830(17) 0.0224(7) Uani 1 1 d . . . N7 N 0.6823(3) -0.04914(16) 0.6723(2) 0.0313(9) Uani 1 1 d . . . N8 N 0.8954(3) -0.03467(17) 0.6772(2) 0.0317(9) Uani 1 1 d . . . N9 N 0.8508(3) -0.11724(15) 0.74820(19) 0.0282(8) Uani 1 1 d . . . N10 N 0.7125(3) -0.07884(16) 0.81550(19) 0.0294(8) Uani 1 1 d . . . C1 C 0.9522(3) 0.13021(19) 0.7039(2) 0.0287(10) Uani 1 1 d . . . H1 H 0.8841 0.1300 0.6892 0.034 Uiso 1 1 calc R . . C2 C 1.0186(4) 0.1472(2) 0.6552(2) 0.0328(10) Uani 1 1 d . . . H2 H 0.9962 0.1581 0.6078 0.039 Uiso 1 1 calc R . . C3 C 1.1172(3) 0.1478(2) 0.6772(3) 0.0324(10) Uani 1 1 d . . . H3 H 1.1640 0.1573 0.6441 0.039 Uiso 1 1 calc R . . C4 C 1.1481(3) 0.1346(2) 0.7476(2) 0.0307(10) Uani 1 1 d . . . H4 H 1.2158 0.1361 0.7637 0.037 Uiso 1 1 calc R . . C5 C 1.0785(3) 0.11924(18) 0.7940(2) 0.0256(9) Uani 1 1 d . . . C6 C 1.0989(3) 0.10699(18) 0.8703(2) 0.0251(9) Uani 1 1 d . . . C7 C 1.1884(3) 0.10823(19) 0.9102(2) 0.0287(10) Uani 1 1 d . . . H7 H 1.2466 0.1184 0.8887 0.034 Uiso 1 1 calc R . . C8 C 1.1911(3) 0.0943(2) 0.9823(3) 0.0322(10) Uani 1 1 d . . . H8 H 1.2522 0.0943 1.0103 0.039 Uiso 1 1 calc R . . C9 C 1.1058(3) 0.08045(18) 1.0143(2) 0.0275(9) Uani 1 1 d . . . H9 H 1.1075 0.0716 1.0640 0.033 Uiso 1 1 calc R . . C10 C 1.0182(3) 0.07992(17) 0.9716(2) 0.0236(9) Uani 1 1 d . . . C11 C 0.9200(3) 0.06465(18) 0.9915(2) 0.0226(8) Uani 1 1 d . . . C12 C 0.8968(3) 0.05274(18) 1.0607(2) 0.0269(9) Uani 1 1 d . . . H12 H 0.9459 0.0535 1.0996 0.032 Uiso 1 1 calc R . . C13 C 0.8007(3) 0.0397(2) 1.0722(2) 0.0319(10) Uani 1 1 d . . . H13 H 0.7829 0.0314 1.1192 0.038 Uiso 1 1 calc R . . C14 C 0.7307(3) 0.0389(2) 1.0146(2) 0.0329(11) Uani 1 1 d . . . H14 H 0.6644 0.0300 1.0216 0.040 Uiso 1 1 calc R . . C15 C 0.7584(3) 0.05117(19) 0.9460(2) 0.0288(10) Uani 1 1 d . . . H15 H 0.7100 0.0513 0.9066 0.035 Uiso 1 1 calc R . . C16 C 0.8734(3) 0.20222(19) 0.8901(2) 0.0284(10) Uani 1 1 d . . . H16 H 0.9339 0.1984 0.9184 0.034 Uiso 1 1 calc R . . C17 C 0.8235(4) 0.2524(2) 0.8906(3) 0.0337(11) Uani 1 1 d . . . H17 H 0.8504 0.2825 0.9182 0.040 Uiso 1 1 calc R . . C18 C 0.7354(4) 0.2578(2) 0.8509(3) 0.0395(12) Uani 1 1 d . . . H18 H 0.6998 0.2914 0.8515 0.047 Uiso 1 1 calc R . . C19 C 0.6984(3) 0.2133(2) 0.8095(3) 0.0348(11) Uani 1 1 d . . . H19 H 0.6377 0.2164 0.7812 0.042 Uiso 1 1 calc R . . C20 C 0.7512(3) 0.16497(19) 0.8103(2) 0.0260(9) Uani 1 1 d . . . C21 C 0.7223(3) 0.11496(18) 0.7703(2) 0.0221(9) Uani 1 1 d . . . C22 C 0.6482(3) 0.09753(18) 0.7214(2) 0.0249(9) Uani 1 1 d . . . H22 H 0.5940 0.1184 0.7010 0.030 Uiso 1 1 calc R . . C23 C 0.6702(3) 0.04283(19) 0.7084(2) 0.0262(9) Uani 1 1 d . . . C24 C 0.6287(3) -0.0020(2) 0.6647(2) 0.0302(10) Uani 1 1 d . . . C25 C 0.5421(4) 0.0009(2) 0.6203(3) 0.0363(11) Uani 1 1 d . . . H25 H 0.5070 0.0346 0.6151 0.044 Uiso 1 1 calc R . . C26 C 0.5084(4) -0.0444(3) 0.5845(3) 0.0493(14) Uani 1 1 d . . . H26 H 0.4492 -0.0429 0.5543 0.059 Uiso 1 1 calc R . . C27 C 0.5609(4) -0.0931(2) 0.5922(3) 0.0474(14) Uani 1 1 d . . . H27 H 0.5374 -0.1255 0.5679 0.057 Uiso 1 1 calc R . . C28 C 0.6487(4) -0.0942(2) 0.6360(3) 0.0393(12) Uani 1 1 d . . . H28 H 0.6854 -0.1275 0.6402 0.047 Uiso 1 1 calc R . . C29 C 0.9086(4) 0.0101(2) 0.6385(3) 0.0383(11) Uani 1 1 d . . . H29 H 0.8651 0.0404 0.6418 0.046 Uiso 1 1 calc R . . C30 C 0.9847(4) 0.0140(2) 0.5931(3) 0.0454(13) Uani 1 1 d . . . H30 H 0.9936 0.0468 0.5666 0.054 Uiso 1 1 calc R . . C31 C 1.0465(4) -0.0299(2) 0.5871(3) 0.0449(13) Uani 1 1 d . . . H31 H 1.0991 -0.0276 0.5567 0.054 Uiso 1 1 calc R . . C32 C 1.0320(4) -0.0774(2) 0.6252(3) 0.0435(13) Uani 1 1 d . . . H32 H 1.0738 -0.1084 0.6209 0.052 Uiso 1 1 calc R . . C33 C 0.9555(4) -0.0794(2) 0.6701(3) 0.0348(11) Uani 1 1 d . . . C34 C 0.9295(4) -0.1266(2) 0.7130(3) 0.0333(10) Uani 1 1 d . . . C35 C 0.9776(4) -0.1763(2) 0.7198(3) 0.0452(13) Uani 1 1 d . . . H35 H 1.0338 -0.1835 0.6943 0.054 Uiso 1 1 calc R . . C36 C 0.9419(5) -0.2155(2) 0.7649(3) 0.0521(15) Uani 1 1 d . . . H36 H 0.9731 -0.2505 0.7694 0.063 Uiso 1 1 calc R . . C37 C 0.8623(5) -0.2050(2) 0.8032(3) 0.0470(13) Uani 1 1 d . . . H37 H 0.8399 -0.2315 0.8357 0.056 Uiso 1 1 calc R . . C38 C 0.8153(4) -0.15443(19) 0.7934(2) 0.0337(11) Uani 1 1 d . . . C39 C 0.7315(4) -0.1334(2) 0.8291(2) 0.0319(10) Uani 1 1 d . . . C40 C 0.6733(4) -0.1641(2) 0.8722(3) 0.0409(12) Uani 1 1 d . . . H40 H 0.6873 -0.2019 0.8814 0.049 Uiso 1 1 calc R . . C41 C 0.5957(4) -0.1392(2) 0.9013(3) 0.0442(13) Uani 1 1 d . . . H41 H 0.5559 -0.1596 0.9314 0.053 Uiso 1 1 calc R . . C42 C 0.5755(4) -0.0853(2) 0.8871(3) 0.0406(12) Uani 1 1 d . . . H42 H 0.5209 -0.0680 0.9064 0.049 Uiso 1 1 calc R . . C43 C 0.6361(3) -0.0553(2) 0.8437(2) 0.0346(11) Uani 1 1 d . . . H43 H 0.6223 -0.0175 0.8342 0.042 Uiso 1 1 calc R . . P1 P 0.14775(10) 0.23649(6) 0.46625(7) 0.0393(3) Uani 1 1 d . . . F1 F 0.1701(4) 0.21103(18) 0.5430(2) 0.0835(14) Uani 1 1 d . . . F2 F 0.0505(3) 0.20110(16) 0.4523(3) 0.0730(11) Uani 1 1 d . . . F3 F 0.1255(3) 0.26609(15) 0.39040(19) 0.0682(11) Uani 1 1 d . . . F4 F 0.2457(2) 0.27297(16) 0.47981(19) 0.0597(9) Uani 1 1 d . . . F5 F 0.2085(3) 0.19052(16) 0.4291(2) 0.0641(10) Uani 1 1 d . . . F6 F 0.0872(3) 0.28510(15) 0.5009(2) 0.0599(9) Uani 1 1 d . . . P2 P 0.45529(8) 0.07409(6) 0.87070(7) 0.0327(3) Uani 1 1 d . . . F7 F 0.5242(2) 0.03637(15) 0.92404(17) 0.0557(9) Uani 1 1 d . . . F8 F 0.3678(2) 0.03097(13) 0.87601(16) 0.0438(7) Uani 1 1 d . . . F9 F 0.3863(2) 0.11178(13) 0.81771(15) 0.0448(7) Uani 1 1 d . . . F10 F 0.5431(2) 0.11653(15) 0.86601(19) 0.0575(9) Uani 1 1 d . . . F11 F 0.4905(2) 0.04055(13) 0.80308(16) 0.0421(7) Uani 1 1 d . . . F12 F 0.4185(2) 0.10724(13) 0.93781(15) 0.0415(7) Uani 1 1 d . . . P3 P 0.26727(9) 0.87923(5) 0.48682(6) 0.0305(3) Uani 1 1 d D . . F13 F 0.2299(2) 0.87593(17) 0.40475(17) 0.0460(9) Uani 0.888(4) 1 d PD A 1 F14 F 0.2544(3) 0.94515(15) 0.4858(2) 0.0572(11) Uani 0.888(4) 1 d PD A 1 F15 F 0.3042(3) 0.88309(18) 0.56986(18) 0.0567(11) Uani 0.888(4) 1 d PD A 1 F16 F 0.2821(3) 0.81421(13) 0.48971(19) 0.0416(9) Uani 0.888(4) 1 d PD A 1 F13A F 0.2078(18) 0.9273(7) 0.4464(11) 0.0460(9) Uani 0.112(4) 1 d PD A 2 F14A F 0.279(2) 0.9141(9) 0.5601(8) 0.0572(11) Uani 0.112(4) 1 d PD A 2 F15A F 0.320(2) 0.8281(8) 0.5273(11) 0.0567(11) Uani 0.112(4) 1 d PD A 2 F16A F 0.249(2) 0.8420(8) 0.4164(8) 0.0416(9) Uani 0.112(4) 1 d PD A 2 F17 F 0.1568(2) 0.87163(15) 0.50874(19) 0.0547(9) Uani 1 1 d . A . F18 F 0.3765(2) 0.88718(13) 0.46427(16) 0.0447(7) Uani 1 1 d . A . C44 C 0.4167(5) 0.2607(3) 0.3743(4) 0.0643(17) Uani 1 1 d . . . H44A H 0.3496 0.2536 0.3886 0.077 Uiso 1 1 calc R . . H44B H 0.4224 0.3006 0.3642 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.50309(13) 0.24238(7) 0.44544(10) 0.0649(4) Uani 1 1 d . . . Cl2 Cl 0.43572(15) 0.22304(8) 0.29621(9) 0.0702(5) Uani 1 1 d . . . C45 C 0.3814(8) 0.1470(4) 0.5711(4) 0.068(2) Uani 0.841(4) 1 d PD B 1 H45A H 0.4477 0.1398 0.5551 0.082 Uiso 0.841(4) 1 calc PR B 1 H45B H 0.3466 0.1719 0.5356 0.082 Uiso 0.841(4) 1 calc PR B 1 Cl3 Cl 0.3158(2) 0.08386(12) 0.57450(19) 0.0889(10) Uani 0.841(4) 1 d PD B 1 Cl4 Cl 0.39259(17) 0.17921(14) 0.65479(11) 0.0802(9) Uani 0.841(4) 1 d PD B 1 C45A C 0.359(5) 0.1242(13) 0.5593(8) 0.068(2) Uani 0.159(4) 1 d PD B 2 H45C H 0.4198 0.1281 0.5347 0.082 Uiso 0.159(4) 1 calc PR B 2 H45D H 0.3116 0.1526 0.5399 0.082 Uiso 0.159(4) 1 calc PR B 2 Cl3A Cl 0.3077(11) 0.0575(6) 0.5421(9) 0.0889(10) Uani 0.159(4) 1 d PD B 2 Cl4A Cl 0.3836(9) 0.1341(8) 0.6513(6) 0.0802(9) Uani 0.159(4) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0153(3) 0.0287(3) 0.0166(3) 0.0004(2) 0.0022(2) 0.0011(2) Co2 0.0263(3) 0.0292(3) 0.0195(3) -0.0011(2) 0.0011(2) 0.0003(2) O1 0.0211(15) 0.0354(17) 0.0256(16) -0.0016(13) 0.0044(12) 0.0049(13) O2 0.0333(17) 0.0320(17) 0.0252(16) 0.0029(13) -0.0024(13) 0.0004(14) N1 0.0213(18) 0.037(2) 0.0192(18) -0.0025(15) 0.0031(14) 0.0028(15) N2 0.0186(17) 0.0267(19) 0.0212(18) -0.0007(14) 0.0052(14) 0.0013(14) N3 0.0209(18) 0.0288(19) 0.0210(18) 0.0011(14) 0.0034(14) -0.0003(14) N4 0.0178(16) 0.0295(19) 0.0197(17) 0.0029(14) 0.0053(13) 0.0013(14) N5 0.0186(17) 0.0267(18) 0.0209(18) -0.0001(14) 0.0049(14) 0.0002(14) N6 0.0195(17) 0.035(2) 0.0130(16) 0.0017(14) 0.0014(13) -0.0013(15) N7 0.036(2) 0.036(2) 0.0212(19) -0.0026(16) 0.0007(16) -0.0073(17) N8 0.029(2) 0.039(2) 0.027(2) -0.0045(17) 0.0023(16) 0.0017(17) N9 0.033(2) 0.0269(19) 0.0239(19) 0.0000(15) -0.0022(16) 0.0018(16) N10 0.033(2) 0.035(2) 0.0199(18) 0.0007(15) -0.0007(15) -0.0017(16) C1 0.027(2) 0.034(2) 0.026(2) 0.0007(18) 0.0050(18) 0.0022(19) C2 0.037(3) 0.038(3) 0.023(2) 0.0038(19) 0.0069(19) 0.004(2) C3 0.028(2) 0.042(3) 0.029(2) 0.000(2) 0.0109(19) -0.002(2) C4 0.023(2) 0.040(3) 0.030(2) 0.001(2) 0.0102(18) 0.0010(19) C5 0.019(2) 0.033(2) 0.025(2) -0.0032(18) 0.0018(17) 0.0022(17) C6 0.019(2) 0.028(2) 0.029(2) -0.0008(18) 0.0058(17) 0.0045(17) C7 0.019(2) 0.038(3) 0.029(2) -0.0004(19) 0.0025(17) 0.0014(18) C8 0.021(2) 0.043(3) 0.032(2) -0.003(2) -0.0026(18) 0.0005(19) C9 0.026(2) 0.033(2) 0.024(2) 0.0016(18) 0.0022(18) 0.0020(18) C10 0.024(2) 0.028(2) 0.020(2) 0.0010(17) 0.0030(16) 0.0021(17) C11 0.020(2) 0.027(2) 0.020(2) -0.0004(17) -0.0001(16) -0.0004(16) C12 0.026(2) 0.036(2) 0.018(2) 0.0001(18) 0.0008(17) -0.0003(18) C13 0.031(2) 0.044(3) 0.022(2) 0.0039(19) 0.0079(18) 0.000(2) C14 0.028(2) 0.046(3) 0.026(2) 0.006(2) 0.0110(19) -0.002(2) C15 0.019(2) 0.041(3) 0.026(2) 0.0002(19) 0.0021(17) -0.0039(18) C16 0.024(2) 0.039(3) 0.022(2) -0.0048(18) 0.0044(17) -0.0027(19) C17 0.035(3) 0.031(2) 0.036(3) -0.004(2) 0.009(2) 0.000(2) C18 0.035(3) 0.030(3) 0.054(3) -0.003(2) 0.012(2) 0.006(2) C19 0.026(2) 0.042(3) 0.037(3) 0.004(2) 0.003(2) 0.010(2) C20 0.022(2) 0.036(2) 0.021(2) 0.0028(18) 0.0083(17) 0.0042(18) C21 0.0159(19) 0.033(2) 0.018(2) 0.0084(17) 0.0062(15) 0.0008(16) C22 0.018(2) 0.034(2) 0.023(2) 0.0068(18) 0.0042(16) 0.0002(17) C23 0.023(2) 0.040(3) 0.016(2) 0.0039(18) 0.0024(17) -0.0039(18) C24 0.031(2) 0.040(3) 0.020(2) 0.0029(18) 0.0028(18) -0.004(2) C25 0.030(2) 0.050(3) 0.028(2) 0.007(2) -0.0062(19) -0.014(2) C26 0.039(3) 0.070(4) 0.037(3) 0.011(3) -0.010(2) -0.016(3) C27 0.058(4) 0.046(3) 0.035(3) -0.009(2) -0.013(3) -0.014(3) C28 0.049(3) 0.041(3) 0.027(2) -0.004(2) -0.004(2) -0.006(2) C29 0.044(3) 0.040(3) 0.032(3) -0.001(2) 0.011(2) -0.004(2) C30 0.055(3) 0.051(3) 0.033(3) 0.003(2) 0.015(2) 0.000(3) C31 0.043(3) 0.055(3) 0.038(3) -0.007(2) 0.013(2) -0.007(3) C32 0.044(3) 0.049(3) 0.038(3) -0.006(2) 0.005(2) 0.011(2) C33 0.038(3) 0.040(3) 0.026(2) -0.003(2) 0.002(2) 0.000(2) C34 0.034(3) 0.034(3) 0.031(2) -0.007(2) -0.002(2) 0.003(2) C35 0.053(3) 0.045(3) 0.039(3) -0.002(2) 0.008(2) 0.011(3) C36 0.066(4) 0.040(3) 0.050(3) 0.003(3) 0.004(3) 0.016(3) C37 0.060(4) 0.040(3) 0.041(3) 0.006(2) 0.004(3) 0.003(3) C38 0.042(3) 0.031(2) 0.027(2) -0.0010(19) -0.004(2) 0.001(2) C39 0.038(3) 0.038(3) 0.019(2) -0.0032(19) -0.0020(19) -0.005(2) C40 0.057(3) 0.041(3) 0.025(2) 0.001(2) 0.002(2) -0.013(2) C41 0.049(3) 0.055(3) 0.028(3) 0.005(2) 0.006(2) -0.018(3) C42 0.032(3) 0.052(3) 0.038(3) -0.004(2) 0.006(2) -0.008(2) C43 0.030(2) 0.046(3) 0.028(2) -0.002(2) -0.0011(19) -0.001(2) P1 0.0367(7) 0.0497(8) 0.0320(7) 0.0018(6) 0.0059(5) 0.0045(6) F1 0.119(4) 0.088(3) 0.045(2) 0.024(2) 0.017(2) 0.032(3) F2 0.059(2) 0.061(2) 0.102(3) -0.005(2) 0.024(2) -0.0136(18) F3 0.096(3) 0.058(2) 0.048(2) 0.0062(17) -0.013(2) -0.005(2) F4 0.0408(18) 0.081(3) 0.058(2) -0.0204(18) 0.0062(16) -0.0041(17) F5 0.060(2) 0.066(2) 0.070(2) -0.0172(19) 0.0216(19) 0.0077(18) F6 0.053(2) 0.063(2) 0.064(2) -0.0085(17) 0.0096(17) 0.0061(17) P2 0.0193(6) 0.0484(8) 0.0315(7) 0.0041(5) 0.0087(5) 0.0019(5) F7 0.0427(18) 0.079(2) 0.0435(18) -0.0006(16) -0.0062(14) 0.0210(17) F8 0.0349(15) 0.0530(18) 0.0451(17) 0.0043(14) 0.0130(13) -0.0101(13) F9 0.0454(17) 0.0567(19) 0.0330(15) 0.0098(14) 0.0075(13) 0.0101(14) F10 0.0327(16) 0.080(2) 0.063(2) -0.0159(18) 0.0244(15) -0.0169(16) F11 0.0304(15) 0.0572(19) 0.0403(16) -0.0037(14) 0.0127(12) 0.0033(13) F12 0.0277(14) 0.065(2) 0.0321(15) -0.0050(14) 0.0079(11) 0.0014(13) P3 0.0270(6) 0.0388(7) 0.0259(6) 0.0033(5) 0.0045(5) -0.0024(5) F13 0.0348(17) 0.074(3) 0.0282(17) 0.0157(16) -0.0055(13) -0.0074(17) F14 0.061(3) 0.042(2) 0.071(3) 0.0070(18) 0.018(2) 0.0002(18) F15 0.080(3) 0.062(3) 0.0281(18) -0.0061(16) 0.0021(17) -0.017(2) F16 0.047(2) 0.0374(18) 0.041(2) -0.0003(14) 0.0089(16) -0.0006(15) F13A 0.0348(17) 0.074(3) 0.0282(17) 0.0157(16) -0.0055(13) -0.0074(17) F14A 0.061(3) 0.042(2) 0.071(3) 0.0070(18) 0.018(2) 0.0002(18) F15A 0.080(3) 0.062(3) 0.0281(18) -0.0061(16) 0.0021(17) -0.017(2) F16A 0.047(2) 0.0374(18) 0.041(2) -0.0003(14) 0.0089(16) -0.0006(15) F17 0.0328(16) 0.073(2) 0.061(2) 0.0041(17) 0.0242(15) -0.0027(15) F18 0.0274(14) 0.064(2) 0.0435(17) -0.0047(15) 0.0050(12) -0.0125(13) C44 0.063(4) 0.064(4) 0.067(4) 0.001(3) 0.011(3) 0.005(3) Cl1 0.0595(10) 0.0635(10) 0.0704(11) 0.0002(8) -0.0035(8) -0.0084(8) Cl2 0.0799(12) 0.0758(11) 0.0559(10) -0.0035(8) 0.0127(8) -0.0222(9) C45 0.073(7) 0.070(6) 0.064(5) 0.017(4) 0.027(4) 0.021(5) Cl3 0.0781(15) 0.0720(18) 0.122(3) 0.0268(16) 0.0448(16) 0.0269(14) Cl4 0.0656(12) 0.130(3) 0.0461(10) 0.0046(13) 0.0090(9) 0.0339(15) C45A 0.073(7) 0.070(6) 0.064(5) 0.017(4) 0.027(4) 0.021(5) Cl3A 0.0781(15) 0.0720(18) 0.122(3) 0.0268(16) 0.0448(16) 0.0269(14) Cl4A 0.0656(12) 0.130(3) 0.0461(10) 0.0046(13) 0.0090(9) 0.0339(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.859(3) . yes Co1 N5 1.877(3) . yes Co1 O1 1.918(3) . yes Co1 N3 1.934(3) . yes Co1 N1 1.955(4) . yes Co1 N4 2.017(4) . yes Co2 N9 1.887(4) . yes Co2 N6 1.900(4) . yes Co2 O2 1.905(3) . yes Co2 N8 1.942(4) . yes Co2 N10 1.979(4) . yes Co2 N7 2.042(4) . yes O1 O2 1.363(4) . ? N1 C1 1.342(6) . ? N1 C5 1.362(6) . ? N2 C10 1.337(5) . ? N2 C6 1.347(5) . ? N3 C15 1.344(6) . ? N3 C11 1.358(5) . ? N4 C16 1.335(6) . ? N4 C20 1.369(6) . ? N5 N6 1.321(5) . ? N5 C21 1.354(5) . ? N6 C23 1.351(6) . ? N7 C28 1.348(6) . ? N7 C24 1.358(6) . ? N8 C29 1.324(6) . ? N8 C33 1.373(6) . ? N9 C34 1.321(6) . ? N9 C38 1.350(6) . ? N10 C43 1.332(6) . ? N10 C39 1.369(6) . ? C1 C2 1.394(6) . ? C1 H1 0.9500 . ? C2 C3 1.377(7) . ? C2 H2 0.9500 . ? C3 C4 1.385(7) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.459(6) . ? C6 C7 1.381(6) . ? C7 C8 1.384(7) . ? C7 H7 0.9500 . ? C8 C9 1.392(6) . ? C8 H8 0.9500 . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.467(6) . ? C11 C12 1.383(6) . ? C12 C13 1.382(7) . ? C12 H12 0.9500 . ? C13 C14 1.382(7) . ? C13 H13 0.9500 . ? C14 C15 1.393(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.395(7) . ? C16 H16 0.9500 . ? C17 C18 1.369(7) . ? C17 H17 0.9500 . ? C18 C19 1.399(7) . ? C18 H18 0.9500 . ? C19 C20 1.375(6) . ? C19 H19 0.9500 . ? C20 C21 1.462(6) . ? C21 C22 1.376(6) . ? C22 C23 1.386(6) . ? C22 H22 0.9500 . ? C23 C24 1.447(6) . ? C24 C25 1.393(7) . ? C25 C26 1.347(8) . ? C25 H25 0.9500 . ? C26 C27 1.382(9) . ? C26 H26 0.9500 . ? C27 C28 1.397(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.394(7) . ? C29 H29 0.9500 . ? C30 C31 1.369(8) . ? C30 H30 0.9500 . ? C31 C32 1.375(8) . ? C31 H31 0.9500 . ? C32 C33 1.390(7) . ? C32 H32 0.9500 . ? C33 C34 1.457(7) . ? C34 C35 1.374(7) . ? C35 C36 1.383(8) . ? C35 H35 0.9500 . ? C36 C37 1.370(9) . ? C36 H36 0.9500 . ? C37 C38 1.389(7) . ? C37 H37 0.9500 . ? C38 C39 1.459(7) . ? C39 C40 1.389(7) . ? C40 C41 1.368(8) . ? C40 H40 0.9500 . ? C41 C42 1.359(8) . ? C41 H41 0.9500 . ? C42 C43 1.405(7) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? P1 F1 1.568(4) . ? P1 F5 1.581(4) . ? P1 F2 1.585(4) . ? P1 F3 1.595(4) . ? P1 F6 1.604(4) . ? P1 F4 1.607(4) . ? P2 F10 1.587(3) . ? P2 F8 1.597(3) . ? P2 F9 1.598(3) . ? P2 F12 1.601(3) . ? P2 F7 1.603(3) . ? P2 F11 1.606(3) . ? P3 F13 1.578(3) . ? P3 F13A 1.579(6) . ? P3 F16 1.590(3) . ? P3 F18 1.592(3) . ? P3 F15A 1.594(6) . ? P3 F15 1.594(4) . ? P3 F16A 1.597(6) . ? P3 F17 1.603(3) . ? P3 F14A 1.605(6) . ? P3 F14 1.608(4) . ? C44 Cl2 1.756(7) . ? C44 Cl1 1.763(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 Cl4 1.741(9) . ? C45 Cl3 1.778(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45A Cl4A 1.741(10) . ? C45A Cl3A 1.779(11) . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N5 177.99(15) . . yes N2 Co1 O1 86.84(14) . . yes N5 Co1 O1 91.31(14) . . yes N2 Co1 N3 81.99(15) . . yes N5 Co1 N3 97.47(15) . . yes O1 Co1 N3 96.58(14) . . yes N2 Co1 N1 82.07(15) . . yes N5 Co1 N1 98.58(15) . . yes O1 Co1 N1 86.28(14) . . yes N3 Co1 N1 163.62(15) . . yes N2 Co1 N4 101.48(14) . . yes N5 Co1 N4 80.45(14) . . yes O1 Co1 N4 169.65(13) . . yes N3 Co1 N4 90.73(14) . . yes N1 Co1 N4 88.76(14) . . yes N9 Co2 N6 177.19(16) . . yes N9 Co2 O2 87.50(15) . . yes N6 Co2 O2 90.10(14) . . yes N9 Co2 N8 81.60(17) . . yes N6 Co2 N8 97.14(16) . . yes O2 Co2 N8 94.40(15) . . yes N9 Co2 N10 81.51(16) . . yes N6 Co2 N10 99.84(15) . . yes O2 Co2 N10 87.46(14) . . yes N8 Co2 N10 162.91(17) . . yes N9 Co2 N7 103.45(16) . . yes N6 Co2 N7 79.13(15) . . yes O2 Co2 N7 166.83(15) . . yes N8 Co2 N7 94.44(16) . . yes N10 Co2 N7 86.95(15) . . yes O2 O1 Co1 115.5(2) . . ? O1 O2 Co2 115.4(2) . . ? C1 N1 C5 118.8(4) . . ? C1 N1 Co1 127.7(3) . . ? C5 N1 Co1 113.5(3) . . ? C10 N2 C6 122.4(4) . . ? C10 N2 Co1 118.8(3) . . ? C6 N2 Co1 118.1(3) . . ? C15 N3 C11 118.8(4) . . ? C15 N3 Co1 126.5(3) . . ? C11 N3 Co1 114.5(3) . . ? C16 N4 C20 119.1(4) . . ? C16 N4 Co1 126.8(3) . . ? C20 N4 Co1 114.0(3) . . ? N6 N5 C21 108.8(3) . . ? N6 N5 Co1 131.2(3) . . ? C21 N5 Co1 119.7(3) . . ? N5 N6 C23 108.5(4) . . ? N5 N6 Co2 131.8(3) . . ? C23 N6 Co2 119.6(3) . . ? C28 N7 C24 118.0(4) . . ? C28 N7 Co2 127.0(4) . . ? C24 N7 Co2 114.6(3) . . ? C29 N8 C33 119.2(4) . . ? C29 N8 Co2 127.0(3) . . ? C33 N8 Co2 113.8(3) . . ? C34 N9 C38 122.7(4) . . ? C34 N9 Co2 118.3(3) . . ? C38 N9 Co2 118.2(3) . . ? C43 N10 C39 119.0(4) . . ? C43 N10 Co2 126.9(3) . . ? C39 N10 Co2 113.9(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 118.7(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 113.3(4) . . ? C4 C5 C6 125.1(4) . . ? N2 C6 C7 120.0(4) . . ? N2 C6 C5 112.0(4) . . ? C7 C6 C5 128.0(4) . . ? C6 C7 C8 118.3(4) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C7 C8 C9 121.0(4) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 118.0(4) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N2 C10 C9 120.2(4) . . ? N2 C10 C11 111.4(4) . . ? C9 C10 C11 128.4(4) . . ? N3 C11 C12 122.2(4) . . ? N3 C11 C10 113.0(4) . . ? C12 C11 C10 124.8(4) . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N3 C15 C14 121.5(4) . . ? N3 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? N4 C16 C17 121.8(4) . . ? N4 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 119.3(4) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 119.0(4) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N4 C20 C19 121.4(4) . . ? N4 C20 C21 113.0(4) . . ? C19 C20 C21 125.5(4) . . ? N5 C21 C22 109.0(4) . . ? N5 C21 C20 112.5(4) . . ? C22 C21 C20 138.5(4) . . ? C21 C22 C23 104.6(4) . . ? C21 C22 H22 127.7 . . ? C23 C22 H22 127.7 . . ? N6 C23 C22 109.1(4) . . ? N6 C23 C24 113.4(4) . . ? C22 C23 C24 137.5(4) . . ? N7 C24 C25 122.0(4) . . ? N7 C24 C23 113.0(4) . . ? C25 C24 C23 125.0(5) . . ? C26 C25 C24 119.7(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 119.3(5) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? N7 C28 C27 121.4(5) . . ? N7 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? N8 C29 C30 121.8(5) . . ? N8 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 119.4(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 119.7(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 119.0(5) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? N8 C33 C32 120.9(5) . . ? N8 C33 C34 113.3(4) . . ? C32 C33 C34 125.8(5) . . ? N9 C34 C35 120.4(5) . . ? N9 C34 C33 112.3(4) . . ? C35 C34 C33 127.2(5) . . ? C34 C35 C36 118.1(5) . . ? C34 C35 H35 121.0 . . ? C36 C35 H35 121.0 . . ? C35 C36 C37 121.3(5) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? C36 C37 C38 118.2(5) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? N9 C38 C37 119.2(5) . . ? N9 C38 C39 112.6(4) . . ? C37 C38 C39 128.2(5) . . ? N10 C39 C40 121.0(5) . . ? N10 C39 C38 113.4(4) . . ? C40 C39 C38 125.6(5) . . ? C41 C40 C39 119.3(5) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C42 C41 C40 119.9(5) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 119.5(5) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? N10 C43 C42 121.3(5) . . ? N10 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? F1 P1 F5 92.9(2) . . ? F1 P1 F2 92.2(3) . . ? F5 P1 F2 90.4(2) . . ? F1 P1 F3 176.4(2) . . ? F5 P1 F3 89.9(2) . . ? F2 P1 F3 89.9(2) . . ? F1 P1 F6 89.5(2) . . ? F5 P1 F6 177.2(2) . . ? F2 P1 F6 90.7(2) . . ? F3 P1 F6 87.6(2) . . ? F1 P1 F4 88.4(3) . . ? F5 P1 F4 89.9(2) . . ? F2 P1 F4 179.3(3) . . ? F3 P1 F4 89.5(2) . . ? F6 P1 F4 88.9(2) . . ? F10 P2 F8 179.3(2) . . ? F10 P2 F9 90.4(2) . . ? F8 P2 F9 90.30(17) . . ? F10 P2 F12 90.08(17) . . ? F8 P2 F12 89.94(16) . . ? F9 P2 F12 89.49(17) . . ? F10 P2 F7 89.7(2) . . ? F8 P2 F7 89.65(19) . . ? F9 P2 F7 179.8(2) . . ? F12 P2 F7 90.34(17) . . ? F10 P2 F11 90.67(17) . . ? F8 P2 F11 89.32(17) . . ? F9 P2 F11 90.11(17) . . ? F12 P2 F11 179.16(17) . . ? F7 P2 F11 90.06(17) . . ? F13 P3 F13A 57.2(8) . . ? F13 P3 F16 90.8(2) . . ? F13A P3 F16 143.9(9) . . ? F13 P3 F18 89.36(17) . . ? F13A P3 F18 104.0(10) . . ? F16 P3 F18 90.57(18) . . ? F13 P3 F15A 121.4(8) . . ? F13A P3 F15A 175.8(15) . . ? F16 P3 F15A 33.0(9) . . ? F18 P3 F15A 79.7(12) . . ? F13 P3 F15 179.4(2) . . ? F13A P3 F15 122.2(8) . . ? F16 P3 F15 89.7(2) . . ? F18 P3 F15 91.0(2) . . ? F15A P3 F15 59.2(8) . . ? F13 P3 F16A 32.3(8) . . ? F13A P3 F16A 89.0(8) . . ? F16 P3 F16A 58.6(8) . . ? F18 P3 F16A 86.6(10) . . ? F15A P3 F16A 89.2(8) . . ? F15 P3 F16A 148.2(8) . . ? F13 P3 F17 90.11(19) . . ? F13A P3 F17 75.4(10) . . ? F16 P3 F17 89.82(19) . . ? F18 P3 F17 179.3(2) . . ? F15A P3 F17 100.9(12) . . ? F15 P3 F17 89.5(2) . . ? F16A P3 F17 93.2(10) . . ? F13 P3 F14A 149.0(9) . . ? F13A P3 F14A 91.8(8) . . ? F16 P3 F14A 119.3(9) . . ? F18 P3 F14A 97.3(12) . . ? F15A P3 F14A 89.7(8) . . ? F15 P3 F14A 30.5(8) . . ? F16A P3 F14A 175.7(16) . . ? F17 P3 F14A 82.9(12) . . ? F13 P3 F14 90.7(2) . . ? F13A P3 F14 37.7(9) . . ? F16 P3 F14 178.4(2) . . ? F18 P3 F14 88.9(2) . . ? F15A P3 F14 145.4(10) . . ? F15 P3 F14 88.8(2) . . ? F16A P3 F14 122.8(9) . . ? F17 P3 F14 90.8(2) . . ? F14A P3 F14 59.3(9) . . ? Cl2 C44 Cl1 111.1(4) . . ? Cl2 C44 H44A 109.4 . . ? Cl1 C44 H44A 109.4 . . ? Cl2 C44 H44B 109.4 . . ? Cl1 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? Cl4 C45 Cl3 111.3(4) . . ? Cl4 C45 H45A 109.4 . . ? Cl3 C45 H45A 109.4 . . ? Cl4 C45 H45B 109.4 . . ? Cl3 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? Cl4A C45A Cl3A 110.4(10) . . ? Cl4A C45A H45C 109.6 . . ? Cl3A C45A H45C 109.6 . . ? Cl4A C45A H45D 109.6 . . ? Cl3A C45A H45D 109.6 . . ? H45C C45A H45D 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 O1 O2 128.1(3) . . . . ? N5 Co1 O1 O2 -51.1(3) . . . . ? N3 Co1 O1 O2 46.6(3) . . . . ? N1 Co1 O1 O2 -149.6(3) . . . . ? N4 Co1 O1 O2 -88.1(8) . . . . ? Co1 O1 O2 Co2 87.0(3) . . . . ? N9 Co2 O2 O1 123.7(3) . . . . ? N6 Co2 O2 O1 -54.8(3) . . . . ? N8 Co2 O2 O1 42.4(3) . . . . ? N10 Co2 O2 O1 -154.7(3) . . . . ? N7 Co2 O2 O1 -89.7(7) . . . . ? N2 Co1 N1 C1 -170.6(4) . . . . ? N5 Co1 N1 C1 11.3(4) . . . . ? O1 Co1 N1 C1 102.1(4) . . . . ? N3 Co1 N1 C1 -157.2(5) . . . . ? N4 Co1 N1 C1 -68.8(4) . . . . ? N2 Co1 N1 C5 8.2(3) . . . . ? N5 Co1 N1 C5 -169.9(3) . . . . ? O1 Co1 N1 C5 -79.1(3) . . . . ? N3 Co1 N1 C5 21.6(7) . . . . ? N4 Co1 N1 C5 110.0(3) . . . . ? O1 Co1 N2 C10 -93.3(3) . . . . ? N3 Co1 N2 C10 3.8(3) . . . . ? N1 Co1 N2 C10 -180.0(3) . . . . ? N4 Co1 N2 C10 92.9(3) . . . . ? O1 Co1 N2 C6 77.6(3) . . . . ? N3 Co1 N2 C6 174.7(3) . . . . ? N1 Co1 N2 C6 -9.1(3) . . . . ? N4 Co1 N2 C6 -96.2(3) . . . . ? N2 Co1 N3 C15 173.9(4) . . . . ? N5 Co1 N3 C15 -8.0(4) . . . . ? O1 Co1 N3 C15 -100.2(4) . . . . ? N1 Co1 N3 C15 160.5(5) . . . . ? N4 Co1 N3 C15 72.4(4) . . . . ? N2 Co1 N3 C11 0.0(3) . . . . ? N5 Co1 N3 C11 178.0(3) . . . . ? O1 Co1 N3 C11 85.8(3) . . . . ? N1 Co1 N3 C11 -13.4(7) . . . . ? N4 Co1 N3 C11 -101.5(3) . . . . ? N2 Co1 N4 C16 -2.0(4) . . . . ? N5 Co1 N4 C16 177.5(4) . . . . ? O1 Co1 N4 C16 -145.0(7) . . . . ? N3 Co1 N4 C16 80.0(4) . . . . ? N1 Co1 N4 C16 -83.6(4) . . . . ? N2 Co1 N4 C20 177.9(3) . . . . ? N5 Co1 N4 C20 -2.7(3) . . . . ? O1 Co1 N4 C20 34.9(9) . . . . ? N3 Co1 N4 C20 -100.1(3) . . . . ? N1 Co1 N4 C20 96.2(3) . . . . ? O1 Co1 N5 N6 4.2(4) . . . . ? N3 Co1 N5 N6 -92.7(4) . . . . ? N1 Co1 N5 N6 90.6(4) . . . . ? N4 Co1 N5 N6 177.9(4) . . . . ? O1 Co1 N5 C21 -168.4(3) . . . . ? N3 Co1 N5 C21 94.8(3) . . . . ? N1 Co1 N5 C21 -82.0(3) . . . . ? N4 Co1 N5 C21 5.3(3) . . . . ? C21 N5 N6 C23 0.2(4) . . . . ? Co1 N5 N6 C23 -172.9(3) . . . . ? C21 N5 N6 Co2 -175.6(3) . . . . ? Co1 N5 N6 Co2 11.2(5) . . . . ? O2 Co2 N6 N5 7.7(4) . . . . ? N8 Co2 N6 N5 -86.7(4) . . . . ? N10 Co2 N6 N5 95.2(4) . . . . ? N7 Co2 N6 N5 -179.9(4) . . . . ? O2 Co2 N6 C23 -167.7(3) . . . . ? N8 Co2 N6 C23 97.8(3) . . . . ? N10 Co2 N6 C23 -80.3(3) . . . . ? N7 Co2 N6 C23 4.6(3) . . . . ? N9 Co2 N7 C28 3.4(4) . . . . ? N6 Co2 N7 C28 -177.7(4) . . . . ? O2 Co2 N7 C28 -142.1(6) . . . . ? N8 Co2 N7 C28 85.9(4) . . . . ? N10 Co2 N7 C28 -77.1(4) . . . . ? N9 Co2 N7 C24 176.4(3) . . . . ? N6 Co2 N7 C24 -4.8(3) . . . . ? O2 Co2 N7 C24 30.8(8) . . . . ? N8 Co2 N7 C24 -101.2(3) . . . . ? N10 Co2 N7 C24 95.9(3) . . . . ? N9 Co2 N8 C29 174.8(4) . . . . ? N6 Co2 N8 C29 -7.7(4) . . . . ? O2 Co2 N8 C29 -98.4(4) . . . . ? N10 Co2 N8 C29 165.9(5) . . . . ? N7 Co2 N8 C29 71.8(4) . . . . ? N9 Co2 N8 C33 -6.6(3) . . . . ? N6 Co2 N8 C33 170.9(3) . . . . ? O2 Co2 N8 C33 80.2(3) . . . . ? N10 Co2 N8 C33 -15.5(7) . . . . ? N7 Co2 N8 C33 -109.6(3) . . . . ? O2 Co2 N9 C34 -86.4(3) . . . . ? N8 Co2 N9 C34 8.4(3) . . . . ? N10 Co2 N9 C34 -174.2(4) . . . . ? N7 Co2 N9 C34 101.0(3) . . . . ? O2 Co2 N9 C38 83.5(3) . . . . ? N8 Co2 N9 C38 178.3(4) . . . . ? N10 Co2 N9 C38 -4.3(3) . . . . ? N7 Co2 N9 C38 -89.1(3) . . . . ? N9 Co2 N10 C43 -174.3(4) . . . . ? N6 Co2 N10 C43 8.2(4) . . . . ? O2 Co2 N10 C43 97.9(4) . . . . ? N8 Co2 N10 C43 -165.4(5) . . . . ? N7 Co2 N10 C43 -70.2(4) . . . . ? N9 Co2 N10 C39 0.4(3) . . . . ? N6 Co2 N10 C39 -177.1(3) . . . . ? O2 Co2 N10 C39 -87.5(3) . . . . ? N8 Co2 N10 C39 9.3(7) . . . . ? N7 Co2 N10 C39 104.5(3) . . . . ? C5 N1 C1 C2 5.8(7) . . . . ? Co1 N1 C1 C2 -175.5(3) . . . . ? N1 C1 C2 C3 -0.5(7) . . . . ? C1 C2 C3 C4 -3.5(7) . . . . ? C2 C3 C4 C5 2.1(7) . . . . ? C1 N1 C5 C4 -7.2(6) . . . . ? Co1 N1 C5 C4 173.9(3) . . . . ? C1 N1 C5 C6 172.8(4) . . . . ? Co1 N1 C5 C6 -6.1(5) . . . . ? C3 C4 C5 N1 3.3(7) . . . . ? C3 C4 C5 C6 -176.6(4) . . . . ? C10 N2 C6 C7 -2.2(6) . . . . ? Co1 N2 C6 C7 -172.8(3) . . . . ? C10 N2 C6 C5 178.5(4) . . . . ? Co1 N2 C6 C5 8.0(5) . . . . ? N1 C5 C6 N2 -0.8(5) . . . . ? C4 C5 C6 N2 179.2(4) . . . . ? N1 C5 C6 C7 -179.9(4) . . . . ? C4 C5 C6 C7 0.0(8) . . . . ? N2 C6 C7 C8 1.6(7) . . . . ? C5 C6 C7 C8 -179.2(4) . . . . ? C6 C7 C8 C9 -1.2(7) . . . . ? C7 C8 C9 C10 1.2(7) . . . . ? C6 N2 C10 C9 2.3(6) . . . . ? Co1 N2 C10 C9 172.7(3) . . . . ? C6 N2 C10 C11 -176.9(4) . . . . ? Co1 N2 C10 C11 -6.4(5) . . . . ? C8 C9 C10 N2 -1.7(6) . . . . ? C8 C9 C10 C11 177.3(4) . . . . ? C15 N3 C11 C12 2.7(6) . . . . ? Co1 N3 C11 C12 177.2(3) . . . . ? C15 N3 C11 C10 -177.7(4) . . . . ? Co1 N3 C11 C10 -3.3(5) . . . . ? N2 C10 C11 N3 6.0(5) . . . . ? C9 C10 C11 N3 -173.0(4) . . . . ? N2 C10 C11 C12 -174.4(4) . . . . ? C9 C10 C11 C12 6.5(7) . . . . ? N3 C11 C12 C13 -1.5(7) . . . . ? C10 C11 C12 C13 179.0(4) . . . . ? C11 C12 C13 C14 0.1(7) . . . . ? C12 C13 C14 C15 0.0(7) . . . . ? C11 N3 C15 C14 -2.6(7) . . . . ? Co1 N3 C15 C14 -176.3(3) . . . . ? C13 C14 C15 N3 1.3(7) . . . . ? C20 N4 C16 C17 0.0(6) . . . . ? Co1 N4 C16 C17 179.8(3) . . . . ? N4 C16 C17 C18 1.1(7) . . . . ? C16 C17 C18 C19 -1.4(7) . . . . ? C17 C18 C19 C20 0.6(7) . . . . ? C16 N4 C20 C19 -0.8(6) . . . . ? Co1 N4 C20 C19 179.4(3) . . . . ? C16 N4 C20 C21 179.9(3) . . . . ? Co1 N4 C20 C21 0.0(4) . . . . ? C18 C19 C20 N4 0.5(7) . . . . ? C18 C19 C20 C21 179.8(4) . . . . ? N6 N5 C21 C22 0.0(4) . . . . ? Co1 N5 C21 C22 174.1(3) . . . . ? N6 N5 C21 C20 179.2(3) . . . . ? Co1 N5 C21 C20 -6.7(4) . . . . ? N4 C20 C21 N5 4.0(5) . . . . ? C19 C20 C21 N5 -175.3(4) . . . . ? N4 C20 C21 C22 -177.1(5) . . . . ? C19 C20 C21 C22 3.6(8) . . . . ? N5 C21 C22 C23 -0.2(4) . . . . ? C20 C21 C22 C23 -179.1(5) . . . . ? N5 N6 C23 C22 -0.3(4) . . . . ? Co2 N6 C23 C22 176.1(3) . . . . ? N5 N6 C23 C24 179.9(3) . . . . ? Co2 N6 C23 C24 -3.7(5) . . . . ? C21 C22 C23 N6 0.3(4) . . . . ? C21 C22 C23 C24 -179.9(5) . . . . ? C28 N7 C24 C25 -1.0(7) . . . . ? Co2 N7 C24 C25 -174.6(3) . . . . ? C28 N7 C24 C23 177.8(4) . . . . ? Co2 N7 C24 C23 4.2(5) . . . . ? N6 C23 C24 N7 -0.6(5) . . . . ? C22 C23 C24 N7 179.7(5) . . . . ? N6 C23 C24 C25 178.2(4) . . . . ? C22 C23 C24 C25 -1.6(8) . . . . ? N7 C24 C25 C26 1.5(7) . . . . ? C23 C24 C25 C26 -177.1(5) . . . . ? C24 C25 C26 C27 -0.4(8) . . . . ? C25 C26 C27 C28 -1.0(9) . . . . ? C24 N7 C28 C27 -0.5(7) . . . . ? Co2 N7 C28 C27 172.2(4) . . . . ? C26 C27 C28 N7 1.6(8) . . . . ? C33 N8 C29 C30 -2.9(7) . . . . ? Co2 N8 C29 C30 175.7(4) . . . . ? N8 C29 C30 C31 1.3(8) . . . . ? C29 C30 C31 C32 0.7(9) . . . . ? C30 C31 C32 C33 -1.0(8) . . . . ? C29 N8 C33 C32 2.6(7) . . . . ? Co2 N8 C33 C32 -176.1(4) . . . . ? C29 N8 C33 C34 -177.1(4) . . . . ? Co2 N8 C33 C34 4.2(5) . . . . ? C31 C32 C33 N8 -0.7(8) . . . . ? C31 C32 C33 C34 179.0(5) . . . . ? C38 N9 C34 C35 1.8(7) . . . . ? Co2 N9 C34 C35 171.2(4) . . . . ? C38 N9 C34 C33 -177.6(4) . . . . ? Co2 N9 C34 C33 -8.1(5) . . . . ? N8 C33 C34 N9 2.3(6) . . . . ? C32 C33 C34 N9 -177.4(5) . . . . ? N8 C33 C34 C35 -177.1(5) . . . . ? C32 C33 C34 C35 3.3(8) . . . . ? N9 C34 C35 C36 -0.7(8) . . . . ? C33 C34 C35 C36 178.6(5) . . . . ? C34 C35 C36 C37 -1.6(9) . . . . ? C35 C36 C37 C38 2.7(9) . . . . ? C34 N9 C38 C37 -0.6(7) . . . . ? Co2 N9 C38 C37 -170.0(4) . . . . ? C34 N9 C38 C39 176.6(4) . . . . ? Co2 N9 C38 C39 7.1(5) . . . . ? C36 C37 C38 N9 -1.7(8) . . . . ? C36 C37 C38 C39 -178.3(5) . . . . ? C43 N10 C39 C40 -0.8(7) . . . . ? Co2 N10 C39 C40 -175.9(4) . . . . ? C43 N10 C39 C38 178.3(4) . . . . ? Co2 N10 C39 C38 3.2(5) . . . . ? N9 C38 C39 N10 -6.5(6) . . . . ? C37 C38 C39 N10 170.3(5) . . . . ? N9 C38 C39 C40 172.6(4) . . . . ? C37 C38 C39 C40 -10.6(8) . . . . ? N10 C39 C40 C41 0.2(7) . . . . ? C38 C39 C40 C41 -178.8(5) . . . . ? C39 C40 C41 C42 0.9(8) . . . . ? C40 C41 C42 C43 -1.3(8) . . . . ? C39 N10 C43 C42 0.4(7) . . . . ? Co2 N10 C43 C42 174.8(4) . . . . ? C41 C42 C43 N10 0.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.217 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.130 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.270 0.641 0.328 261 62 ' ' 2 0.270 0.859 0.828 261 62 ' ' 3 0.730 0.141 0.172 261 62 ' ' 4 0.730 0.359 0.672 261 62 ' ' _platon_squeeze_details ; The volume occupied by solvent is 17.2 percent of the unit cell. ; data_stahl125 _database_code_depnum_ccdc_archive 'CCDC 885443' #TrackingRef 'stahl125_MOD.cif' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C39 H35 Co2 N14 O2, 0.5(C10 H24), 3(F6 P), C3 H6 O ; _chemical_formula_sum 'C47 H53 Co2 F18 N14 O3 P3' _chemical_formula_weight 1414.80 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' 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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.150(4) _cell_length_b 13.310(4) _cell_length_c 17.433(5) _cell_angle_alpha 95.70(2) _cell_angle_beta 96.001(19) _cell_angle_gamma 107.53(3) _cell_volume 2648.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 0.840 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; SADABS (Bruker-AXS, 2007) ; _exptl_absorpt_correction_T_min 0.8112 _exptl_absorpt_correction_T_max 0.8500 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source . _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.50\% \w and 0.5\% \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29785 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9227 _reflns_number_gt 8186 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 Ver. 2010.11-3 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT Ver. 7.68A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT Ver. 7.68A' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL, OLEX2 (Dolomanov et al., 2009)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+2.8750P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9227 _refine_ls_number_parameters 746 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1095 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.23028(3) 0.07937(3) 0.310408(19) 0.01184(10) Uani 1 1 d . . . Co2 Co 0.05281(3) 0.19954(3) 0.177725(18) 0.01098(10) Uani 1 1 d . . . O1 O 0.13984(16) 0.03691(14) 0.21116(10) 0.0155(4) Uani 1 1 d . . . O2 O 0.15652(16) 0.11930(14) 0.16596(10) 0.0149(4) Uani 1 1 d . . . N1 N 0.10691(19) -0.02004(18) 0.34951(12) 0.0160(5) Uani 1 1 d . . . N2 N 0.0213(2) -0.18516(19) 0.36785(13) 0.0191(5) Uani 1 1 d . . . N3 N 0.28460(18) -0.03964(17) 0.29803(12) 0.0133(4) Uani 1 1 d . . . N4 N 0.52325(19) 0.12703(18) 0.21686(13) 0.0177(5) Uani 1 1 d . . . N5 N 0.36881(19) 0.14401(17) 0.26595(12) 0.0150(5) Uani 1 1 d . . . N6 N 0.31232(18) 0.14186(17) 0.42004(12) 0.0137(4) Uani 1 1 d . . . N7 N 0.16808(19) 0.19048(17) 0.32889(12) 0.0136(4) Uani 1 1 d . . . N8 N 0.08458(18) 0.21393(17) 0.28635(12) 0.0128(4) Uani 1 1 d . . . N9 N -0.04756(18) 0.29143(17) 0.20854(12) 0.0132(4) Uani 1 1 d . . . N10 N 0.18036(19) 0.32456(17) 0.17245(12) 0.0147(4) Uani 1 1 d . . . N11 N 0.2991(2) 0.42171(18) 0.10156(14) 0.0191(5) Uani 1 1 d . . . N12 N 0.03686(18) 0.19651(17) 0.06800(12) 0.0122(4) Uani 1 1 d . . . N13 N -0.21903(18) -0.03039(17) 0.05772(13) 0.0147(4) Uani 1 1 d . . . N14 N -0.08289(18) 0.07416(17) 0.15018(12) 0.0134(4) Uani 1 1 d . . . C1 C 0.0048(2) -0.0240(2) 0.37770(15) 0.0192(6) Uani 1 1 d . . . H1 H -0.0238 0.0344 0.3874 0.023 Uiso 1 1 calc R . . C2 C -0.0486(2) -0.1257(2) 0.38940(16) 0.0222(6) Uani 1 1 d . . . H2 H -0.1207 -0.1510 0.4088 0.027 Uiso 1 1 calc R . . C3 C -0.0051(3) -0.2996(2) 0.36930(17) 0.0256(6) Uani 1 1 d . . . H3A H 0.0556 -0.3127 0.4048 0.038 Uiso 1 1 calc R . . H3B H -0.0079 -0.3351 0.3168 0.038 Uiso 1 1 calc R . . H3C H -0.0808 -0.3278 0.3873 0.038 Uiso 1 1 calc R . . C4 C 0.1152(2) -0.1181(2) 0.34481(15) 0.0161(5) Uani 1 1 d . . . C5 C 0.2186(2) -0.1331(2) 0.31626(14) 0.0156(5) Uani 1 1 d . . . C6 C 0.2539(2) -0.2230(2) 0.30539(15) 0.0197(6) Uani 1 1 d . . . H6 H 0.2085 -0.2892 0.3183 0.024 Uiso 1 1 calc R . . C7 C 0.3573(3) -0.2133(2) 0.27518(15) 0.0206(6) Uani 1 1 d . . . H7 H 0.3828 -0.2739 0.2674 0.025 Uiso 1 1 calc R . . C8 C 0.4240(2) -0.1174(2) 0.25614(15) 0.0194(6) Uani 1 1 d . . . H8 H 0.4948 -0.1114 0.2357 0.023 Uiso 1 1 calc R . . C9 C 0.3844(2) -0.0301(2) 0.26786(14) 0.0150(5) Uani 1 1 d . . . C10 C 0.4301(2) 0.0781(2) 0.25041(14) 0.0161(5) Uani 1 1 d . . . C11 C 0.6141(2) 0.0839(2) 0.19355(17) 0.0223(6) Uani 1 1 d . . . H11A H 0.6464 0.0563 0.2377 0.033 Uiso 1 1 calc R . . H11B H 0.6763 0.1403 0.1773 0.033 Uiso 1 1 calc R . . H11C H 0.5805 0.0262 0.1501 0.033 Uiso 1 1 calc R . . C12 C 0.5195(2) 0.2277(2) 0.21012(16) 0.0219(6) Uani 1 1 d . . . H12 H 0.5734 0.2808 0.1881 0.026 Uiso 1 1 calc R . . C13 C 0.4239(2) 0.2374(2) 0.24093(16) 0.0191(6) Uani 1 1 d . . . H13 H 0.3998 0.2991 0.2443 0.023 Uiso 1 1 calc R . . C14 C 0.3976(2) 0.1161(2) 0.46050(15) 0.0167(5) Uani 1 1 d . . . H14 H 0.4265 0.0638 0.4366 0.020 Uiso 1 1 calc R . . C15 C 0.4447(2) 0.1630(2) 0.53565(15) 0.0184(6) Uani 1 1 d . . . H15 H 0.5054 0.1435 0.5628 0.022 Uiso 1 1 calc R . . C16 C 0.4028(2) 0.2389(2) 0.57117(15) 0.0193(6) Uani 1 1 d . . . H16 H 0.4327 0.2705 0.6235 0.023 Uiso 1 1 calc R . . C17 C 0.3164(2) 0.2683(2) 0.52935(15) 0.0173(5) Uani 1 1 d . . . H17 H 0.2875 0.3214 0.5521 0.021 Uiso 1 1 calc R . . C18 C 0.2733(2) 0.2187(2) 0.45407(15) 0.0143(5) Uani 1 1 d . . . C19 C 0.1850(2) 0.2431(2) 0.40180(14) 0.0136(5) Uani 1 1 d . . . C20 C 0.1113(2) 0.3052(2) 0.40552(15) 0.0148(5) Uani 1 1 d . . . H20 H 0.1043 0.3507 0.4490 0.018 Uiso 1 1 calc R . . C21 C 0.0502(2) 0.2850(2) 0.33057(15) 0.0134(5) Uani 1 1 d . . . C22 C -0.0327(2) 0.3248(2) 0.28645(15) 0.0140(5) Uani 1 1 d . . . C23 C -0.0918(2) 0.3895(2) 0.31796(15) 0.0170(5) Uani 1 1 d . . . H23 H -0.0808 0.4112 0.3726 0.020 Uiso 1 1 calc R . . C24 C -0.1672(2) 0.4220(2) 0.26844(16) 0.0184(6) Uani 1 1 d . . . H24 H -0.2079 0.4672 0.2886 0.022 Uiso 1 1 calc R . . C25 C -0.1827(2) 0.3878(2) 0.18914(15) 0.0166(5) Uani 1 1 d . . . H25 H -0.2340 0.4093 0.1543 0.020 Uiso 1 1 calc R . . C26 C -0.1223(2) 0.3219(2) 0.16142(15) 0.0152(5) Uani 1 1 d . . . H26 H -0.1342 0.2974 0.1072 0.018 Uiso 1 1 calc R . . C27 C 0.2603(2) 0.4074(2) 0.22137(16) 0.0183(6) Uani 1 1 d . . . H27 H 0.2636 0.4206 0.2763 0.022 Uiso 1 1 calc R . . C28 C 0.3340(2) 0.4677(2) 0.17766(17) 0.0212(6) Uani 1 1 d . . . H28 H 0.3978 0.5300 0.1965 0.025 Uiso 1 1 calc R . . C29 C 0.3574(3) 0.4593(2) 0.03568(18) 0.0277(7) Uani 1 1 d . . . H29A H 0.3853 0.4039 0.0111 0.042 Uiso 1 1 calc R . . H29B H 0.4237 0.5236 0.0542 0.042 Uiso 1 1 calc R . . H29C H 0.3023 0.4756 -0.0024 0.042 Uiso 1 1 calc R . . C30 C 0.2049(2) 0.3360(2) 0.10037(15) 0.0154(5) Uani 1 1 d . . . C31 C 0.1236(2) 0.2623(2) 0.03728(15) 0.0150(5) Uani 1 1 d . . . C32 C 0.1231(2) 0.2538(2) -0.04276(16) 0.0192(6) Uani 1 1 d . . . H32 H 0.1844 0.2990 -0.0649 0.023 Uiso 1 1 calc R . . C33 C 0.0301(2) 0.1774(2) -0.08933(15) 0.0182(6) Uani 1 1 d . . . H33 H 0.0272 0.1711 -0.1443 0.022 Uiso 1 1 calc R . . C34 C -0.0591(2) 0.1099(2) -0.05738(15) 0.0155(5) Uani 1 1 d . . . H34 H -0.1230 0.0584 -0.0897 0.019 Uiso 1 1 calc R . . C35 C -0.0521(2) 0.1199(2) 0.02315(15) 0.0132(5) Uani 1 1 d . . . C36 C -0.1221(2) 0.0546(2) 0.07328(14) 0.0137(5) Uani 1 1 d . . . C37 C -0.2931(2) -0.0737(2) -0.01784(16) 0.0206(6) Uani 1 1 d . . . H37A H -0.3590 -0.1348 -0.0113 0.031 Uiso 1 1 calc R . . H37B H -0.2472 -0.0964 -0.0550 0.031 Uiso 1 1 calc R . . H37C H -0.3224 -0.0188 -0.0375 0.031 Uiso 1 1 calc R . . C38 C -0.2412(2) -0.0674(2) 0.12726(15) 0.0171(5) Uani 1 1 d . . . H38 H -0.3037 -0.1271 0.1346 0.021 Uiso 1 1 calc R . . C39 C -0.1561(2) -0.0021(2) 0.18398(15) 0.0160(5) Uani 1 1 d . . . H39 H -0.1493 -0.0089 0.2379 0.019 Uiso 1 1 calc R . . P1 P 0.74658(6) 0.12730(6) 0.42552(4) 0.02148(17) Uani 1 1 d . . . F1 F 0.68407(18) 0.13174(17) 0.50175(11) 0.0402(5) Uani 1 1 d . . . F2 F 0.85586(19) 0.22374(18) 0.46755(11) 0.0486(6) Uani 1 1 d . . . F3 F 0.68909(19) 0.20976(17) 0.39140(12) 0.0440(5) Uani 1 1 d . . . F4 F 0.63533(16) 0.03304(16) 0.38309(11) 0.0388(5) Uani 1 1 d . . . F5 F 0.80275(17) 0.04443(17) 0.45968(11) 0.0380(5) Uani 1 1 d . . . F6 F 0.80994(16) 0.12270(15) 0.35010(10) 0.0327(4) Uani 1 1 d . . . P2 P 0.67955(6) 0.64931(6) 0.22136(4) 0.01740(16) Uani 1 1 d . . . F7 F 0.80013(15) 0.63971(17) 0.19786(10) 0.0353(4) Uani 1 1 d . . . F8 F 0.61998(17) 0.52461(14) 0.19442(11) 0.0349(4) Uani 1 1 d . . . F9 F 0.71497(15) 0.62693(15) 0.30750(9) 0.0290(4) Uani 1 1 d . . . F10 F 0.73788(17) 0.77336(14) 0.24858(11) 0.0370(5) Uani 1 1 d . . . F11 F 0.64328(16) 0.67174(15) 0.13557(9) 0.0312(4) Uani 1 1 d . . . F12 F 0.55823(14) 0.65852(14) 0.24491(9) 0.0253(4) Uani 1 1 d . . . P3 P 0.36761(7) 0.76679(6) 0.03441(4) 0.02564(18) Uani 1 1 d . . . F13 F 0.28470(19) 0.81523(19) 0.07976(15) 0.0538(6) Uani 1 1 d . . . F14 F 0.47575(18) 0.86613(17) 0.07343(12) 0.0482(6) Uani 1 1 d . . . F15 F 0.3485(3) 0.82851(19) -0.03671(13) 0.0757(9) Uani 1 1 d . . . F16 F 0.26094(19) 0.66592(17) -0.00517(12) 0.0499(6) Uani 1 1 d . . . F17 F 0.38536(18) 0.70392(15) 0.10526(10) 0.0364(5) Uani 1 1 d . . . F18 F 0.4524(2) 0.71772(19) -0.01025(14) 0.0618(7) Uani 1 1 d . . . O3 O 0.20815(19) 0.49565(16) 0.55202(12) 0.0284(5) Uani 1 1 d . . . C40 C 0.2875(3) 0.5941(3) 0.45366(19) 0.0362(8) Uani 1 1 d . . . H40A H 0.2094 0.5605 0.4243 0.054 Uiso 1 1 calc R . . H40B H 0.3453 0.5768 0.4241 0.054 Uiso 1 1 calc R . . H40C H 0.3040 0.6714 0.4622 0.054 Uiso 1 1 calc R . . C41 C 0.2934(3) 0.5534(2) 0.53096(17) 0.0255(6) Uani 1 1 d . . . C42 C 0.4102(3) 0.5889(3) 0.5807(2) 0.0356(8) Uani 1 1 d . . . H42A H 0.4336 0.6659 0.5972 0.053 Uiso 1 1 calc R . . H42B H 0.4679 0.5724 0.5508 0.053 Uiso 1 1 calc R . . H42C H 0.4055 0.5519 0.6267 0.053 Uiso 1 1 calc R . . C43 C -0.0645(3) 0.3951(14) -0.1454(2) 0.1107(11) Uiso 0.50 1 d PR A -1 H43D H -0.0851 0.4182 -0.1950 0.166 Uiso 0.50 1 calc PR B -1 H43E H -0.1199 0.3255 -0.1417 0.166 Uiso 0.50 1 calc PR C -1 H43F H 0.0144 0.3896 -0.1426 0.166 Uiso 0.50 1 calc PR D -1 C44 C -0.0690(3) 0.4762(13) -0.0780(3) 0.1107(11) Uiso 0.50 1 d PR A -1 H44C H -0.1500 0.4589 -0.0661 0.133 Uiso 0.50 1 calc PR E -1 H44D H -0.0474 0.5478 -0.0946 0.133 Uiso 0.50 1 calc PR F -1 C45 C 0.0123(3) 0.4791(14) -0.0039(2) 0.1107(11) Uiso 0.50 1 d PR A -1 H45C H 0.0932 0.4963 -0.0159 0.133 Uiso 0.50 1 calc PR G -1 H45D H -0.0093 0.4075 0.0126 0.133 Uiso 0.50 1 calc PR H -1 C46 C 0.0087(3) 0.5601(13) 0.0641(3) 0.1107(11) Uiso 0.50 1 d PR A -1 H46C H 0.0304 0.6318 0.0478 0.133 Uiso 0.50 1 calc PR I -1 H46D H -0.0722 0.5429 0.0763 0.133 Uiso 0.50 1 calc PR J -1 C47 C 0.0902(3) 0.5621(13) 0.1378(3) 0.1107(11) Uiso 0.50 1 d PR A -1 H47D H 0.1598 0.5466 0.1232 0.166 Uiso 0.50 1 calc PR K -1 H47E H 0.0498 0.5085 0.1686 0.166 Uiso 0.50 1 calc PR L -1 H47F H 0.1134 0.6327 0.1687 0.166 Uiso 0.50 1 calc PR M -1 C43A C -0.0903(3) 0.4372(14) -0.1378(2) 0.1107(11) Uiso 0.50 1 d PR N -2 H43A H -0.0553 0.4213 -0.1838 0.166 Uiso 0.50 1 calc PR O -2 H43B H -0.1024 0.5067 -0.1381 0.166 Uiso 0.50 1 calc PR P -2 H43C H -0.1654 0.3822 -0.1386 0.166 Uiso 0.50 1 calc PR Q -2 C44A C -0.0087(3) 0.4392(14) -0.0641(2) 0.1107(11) Uiso 0.50 1 d PR N -2 H44A H 0.0721 0.4563 -0.0763 0.133 Uiso 0.50 1 calc PR R -2 H44B H -0.0305 0.3675 -0.0478 0.133 Uiso 0.50 1 calc PR S -2 C45A C -0.0123(3) 0.5201(13) 0.0038(3) 0.1107(11) Uiso 0.50 1 d PR N -2 H45A H 0.0093 0.5918 -0.0126 0.133 Uiso 0.50 1 calc PR T -2 H45B H -0.0932 0.5030 0.0159 0.133 Uiso 0.50 1 calc PR U -2 C46A C 0.0689(3) 0.5230(13) 0.0780(3) 0.1107(11) Uiso 0.50 1 d PR N -2 H46A H 0.0474 0.4515 0.0946 0.133 Uiso 0.50 1 calc PR V -2 H46B H 0.1499 0.5404 0.0661 0.133 Uiso 0.50 1 calc PR W -2 C47A C 0.0644(4) 0.6042(12) 0.1454(4) 0.1107(11) Uiso 0.50 1 d PR N -2 H47A H 0.0415 0.6617 0.1245 0.166 Uiso 0.50 1 calc PR X -2 H47B H 0.1416 0.6336 0.1768 0.166 Uiso 0.50 1 calc PR Y -2 H47C H 0.0074 0.5691 0.1779 0.166 Uiso 0.50 1 calc PR Z -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01075(18) 0.01416(19) 0.01098(18) 0.00020(13) 0.00224(13) 0.00472(14) Co2 0.01058(18) 0.01193(18) 0.00946(17) -0.00021(13) 0.00199(13) 0.00247(14) O1 0.0173(9) 0.0144(9) 0.0141(9) 0.0006(7) 0.0004(7) 0.0049(8) O2 0.0162(9) 0.0171(9) 0.0135(9) 0.0036(7) 0.0051(7) 0.0069(8) N1 0.0142(11) 0.0204(12) 0.0131(10) 0.0009(9) 0.0017(9) 0.0056(9) N2 0.0155(11) 0.0212(12) 0.0180(11) 0.0039(9) 0.0016(9) 0.0017(10) N3 0.0120(11) 0.0167(11) 0.0101(10) -0.0006(8) -0.0009(8) 0.0046(9) N4 0.0132(11) 0.0239(12) 0.0164(11) 0.0024(9) 0.0043(9) 0.0059(10) N5 0.0137(11) 0.0173(11) 0.0134(10) 0.0007(8) 0.0010(8) 0.0047(9) N6 0.0131(11) 0.0171(11) 0.0111(10) 0.0026(8) 0.0035(8) 0.0043(9) N7 0.0134(11) 0.0166(11) 0.0109(10) 0.0005(8) 0.0014(8) 0.0053(9) N8 0.0104(10) 0.0150(11) 0.0135(10) 0.0016(8) 0.0016(8) 0.0048(9) N9 0.0118(10) 0.0126(11) 0.0136(10) 0.0009(8) 0.0017(8) 0.0016(9) N10 0.0133(11) 0.0154(11) 0.0148(11) 0.0000(9) 0.0019(8) 0.0042(9) N11 0.0143(11) 0.0162(11) 0.0255(12) 0.0027(9) 0.0077(9) 0.0014(9) N12 0.0107(10) 0.0129(10) 0.0126(10) 0.0005(8) 0.0023(8) 0.0035(9) N13 0.0114(11) 0.0124(11) 0.0188(11) -0.0016(8) 0.0027(9) 0.0027(9) N14 0.0129(11) 0.0146(11) 0.0130(10) 0.0006(8) 0.0032(8) 0.0045(9) C1 0.0139(13) 0.0267(15) 0.0177(13) 0.0031(11) 0.0032(10) 0.0072(12) C2 0.0131(13) 0.0313(16) 0.0211(14) 0.0054(12) 0.0053(11) 0.0037(12) C3 0.0262(16) 0.0191(15) 0.0262(15) 0.0061(12) 0.0016(12) -0.0009(12) C4 0.0155(13) 0.0170(13) 0.0138(12) 0.0025(10) -0.0012(10) 0.0034(11) C5 0.0157(13) 0.0169(13) 0.0118(12) 0.0008(10) -0.0012(10) 0.0031(11) C6 0.0245(15) 0.0185(14) 0.0166(13) 0.0020(10) -0.0004(11) 0.0085(12) C7 0.0265(15) 0.0193(14) 0.0179(13) 0.0000(11) 0.0004(11) 0.0118(12) C8 0.0190(14) 0.0261(15) 0.0157(13) -0.0004(11) 0.0024(11) 0.0117(12) C9 0.0138(13) 0.0212(14) 0.0096(12) -0.0012(10) -0.0011(10) 0.0070(11) C10 0.0134(13) 0.0241(14) 0.0110(12) 0.0003(10) 0.0019(10) 0.0071(11) C11 0.0159(14) 0.0314(16) 0.0230(14) 0.0028(12) 0.0085(11) 0.0107(12) C12 0.0185(14) 0.0231(15) 0.0232(14) 0.0067(11) 0.0049(11) 0.0036(12) C13 0.0170(13) 0.0187(14) 0.0228(14) 0.0052(11) 0.0033(11) 0.0064(11) C14 0.0138(13) 0.0183(13) 0.0182(13) 0.0032(10) 0.0037(10) 0.0047(11) C15 0.0144(13) 0.0252(15) 0.0169(13) 0.0073(11) 0.0012(10) 0.0068(11) C16 0.0175(14) 0.0266(15) 0.0109(12) 0.0016(11) 0.0008(10) 0.0035(12) C17 0.0175(13) 0.0204(14) 0.0134(12) -0.0009(10) 0.0029(10) 0.0062(11) C18 0.0114(12) 0.0173(13) 0.0138(12) 0.0017(10) 0.0030(10) 0.0035(10) C19 0.0125(12) 0.0157(13) 0.0111(12) -0.0002(10) 0.0014(10) 0.0032(10) C20 0.0155(13) 0.0145(13) 0.0144(12) 0.0005(10) 0.0045(10) 0.0043(11) C21 0.0122(12) 0.0129(12) 0.0152(12) 0.0016(10) 0.0048(10) 0.0032(10) C22 0.0112(12) 0.0143(13) 0.0150(12) 0.0017(10) 0.0024(10) 0.0017(10) C23 0.0171(13) 0.0159(13) 0.0173(13) -0.0003(10) 0.0036(10) 0.0047(11) C24 0.0171(13) 0.0166(13) 0.0243(14) 0.0036(11) 0.0059(11) 0.0085(11) C25 0.0146(13) 0.0167(13) 0.0189(13) 0.0055(10) 0.0025(10) 0.0045(11) C26 0.0151(13) 0.0135(13) 0.0147(12) 0.0030(10) 0.0014(10) 0.0011(10) C27 0.0150(13) 0.0164(13) 0.0204(13) -0.0031(11) -0.0010(11) 0.0033(11) C28 0.0162(14) 0.0160(14) 0.0281(15) -0.0028(11) 0.0018(11) 0.0025(11) C29 0.0256(16) 0.0229(15) 0.0325(16) 0.0050(12) 0.0160(13) 0.0002(13) C30 0.0126(13) 0.0144(13) 0.0189(13) 0.0029(10) 0.0058(10) 0.0024(11) C31 0.0148(13) 0.0133(13) 0.0189(13) 0.0030(10) 0.0053(10) 0.0060(11) C32 0.0216(14) 0.0195(14) 0.0188(13) 0.0043(11) 0.0104(11) 0.0071(12) C33 0.0249(15) 0.0205(14) 0.0122(12) 0.0024(10) 0.0055(11) 0.0109(12) C34 0.0177(13) 0.0160(13) 0.0131(12) -0.0026(10) -0.0006(10) 0.0082(11) C35 0.0122(12) 0.0116(12) 0.0171(12) 0.0003(10) 0.0024(10) 0.0062(10) C36 0.0129(12) 0.0136(13) 0.0148(12) -0.0018(10) 0.0020(10) 0.0059(10) C37 0.0150(13) 0.0218(14) 0.0191(14) -0.0058(11) -0.0006(11) 0.0008(11) C38 0.0153(13) 0.0145(13) 0.0230(14) 0.0039(10) 0.0088(11) 0.0043(11) C39 0.0170(13) 0.0159(13) 0.0175(13) 0.0040(10) 0.0070(10) 0.0065(11) P1 0.0183(4) 0.0273(4) 0.0185(4) 0.0036(3) 0.0043(3) 0.0059(3) F1 0.0439(12) 0.0562(13) 0.0313(10) 0.0124(9) 0.0202(9) 0.0248(10) F2 0.0440(13) 0.0504(13) 0.0307(10) -0.0053(9) 0.0003(9) -0.0107(10) F3 0.0540(13) 0.0440(12) 0.0467(12) 0.0199(10) 0.0139(10) 0.0278(11) F4 0.0270(10) 0.0418(11) 0.0360(10) 0.0109(9) -0.0015(8) -0.0061(9) F5 0.0347(11) 0.0563(13) 0.0358(10) 0.0178(9) 0.0105(8) 0.0278(10) F6 0.0305(10) 0.0431(11) 0.0231(9) 0.0033(8) 0.0113(7) 0.0071(8) P2 0.0156(3) 0.0214(4) 0.0155(3) 0.0032(3) 0.0026(3) 0.0059(3) F7 0.0217(9) 0.0649(13) 0.0287(9) 0.0176(9) 0.0124(7) 0.0210(9) F8 0.0395(11) 0.0228(9) 0.0418(11) -0.0050(8) 0.0099(9) 0.0105(8) F9 0.0325(10) 0.0443(11) 0.0180(8) 0.0114(7) 0.0071(7) 0.0203(9) F10 0.0358(11) 0.0223(9) 0.0415(11) 0.0044(8) -0.0055(8) -0.0042(8) F11 0.0330(10) 0.0462(11) 0.0184(8) 0.0074(8) 0.0012(7) 0.0182(9) F12 0.0183(8) 0.0316(9) 0.0245(8) -0.0070(7) 0.0022(7) 0.0094(7) P3 0.0242(4) 0.0272(4) 0.0177(4) 0.0037(3) -0.0023(3) -0.0020(3) F13 0.0411(13) 0.0552(14) 0.0781(17) 0.0212(12) 0.0159(12) 0.0283(11) F14 0.0383(12) 0.0436(12) 0.0415(12) -0.0108(9) 0.0045(9) -0.0127(10) F15 0.124(2) 0.0393(13) 0.0353(12) 0.0204(10) -0.0215(14) -0.0112(14) F16 0.0451(13) 0.0394(12) 0.0432(12) 0.0132(9) -0.0211(10) -0.0124(10) F17 0.0500(12) 0.0419(11) 0.0202(9) 0.0033(8) -0.0031(8) 0.0218(10) F18 0.0704(17) 0.0515(14) 0.0550(14) -0.0116(11) 0.0385(13) 0.0025(12) O3 0.0323(12) 0.0231(11) 0.0259(11) -0.0001(9) 0.0076(9) 0.0031(10) C40 0.046(2) 0.0285(17) 0.0294(17) 0.0062(13) 0.0068(15) 0.0040(15) C41 0.0329(17) 0.0187(15) 0.0244(15) -0.0033(12) 0.0049(13) 0.0091(13) C42 0.0313(18) 0.0358(19) 0.0367(18) 0.0049(14) 0.0008(14) 0.0074(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N7 1.869(2) . yes Co1 O1 1.8853(18) . yes Co1 N3 1.893(2) . yes Co1 N1 1.913(2) . yes Co1 N5 1.925(2) . yes Co1 N6 2.031(2) . yes Co2 N8 1.871(2) . yes Co2 O2 1.8951(18) . yes Co2 N12 1.897(2) . yes Co2 N10 1.920(2) . yes Co2 N14 1.937(2) . yes Co2 N9 2.044(2) . yes O1 O2 1.391(3) . ? N1 C4 1.335(3) . ? N1 C1 1.370(3) . ? N2 C4 1.347(4) . ? N2 C2 1.379(4) . ? N2 C3 1.463(4) . ? N3 C9 1.348(3) . ? N3 C5 1.350(3) . ? N4 C10 1.348(4) . ? N4 C12 1.370(4) . ? N4 C11 1.464(3) . ? N5 C10 1.337(3) . ? N5 C13 1.360(4) . ? N6 C14 1.341(3) . ? N6 C18 1.362(3) . ? N7 N8 1.325(3) . ? N7 C19 1.353(3) . ? N8 C21 1.350(3) . ? N9 C26 1.340(3) . ? N9 C22 1.362(3) . ? N10 C30 1.334(3) . ? N10 C27 1.372(3) . ? N11 C30 1.348(3) . ? N11 C28 1.371(4) . ? N11 C29 1.463(4) . ? N12 C31 1.349(3) . ? N12 C35 1.349(3) . ? N13 C36 1.346(3) . ? N13 C38 1.375(3) . ? N13 C37 1.472(3) . ? N14 C36 1.347(3) . ? N14 C39 1.361(3) . ? C1 C2 1.359(4) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.458(4) . ? C5 C6 1.391(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9500 . ? C7 C8 1.383(4) . ? C7 H7 0.9500 . ? C8 C9 1.391(4) . ? C8 H8 0.9500 . ? C9 C10 1.454(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.364(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.378(4) . ? C14 H14 0.9500 . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.389(4) . ? C16 H16 0.9500 . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.466(4) . ? C19 C20 1.391(4) . ? C20 C21 1.392(4) . ? C20 H20 0.9500 . ? C21 C22 1.459(4) . ? C22 C23 1.385(4) . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 C25 1.387(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.363(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.457(4) . ? C31 C32 1.388(4) . ? C32 C33 1.387(4) . ? C32 H32 0.9500 . ? C33 C34 1.389(4) . ? C33 H33 0.9500 . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.450(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.370(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? P1 F4 1.592(2) . yes P1 F2 1.591(2) . yes P1 F5 1.592(2) . yes P1 F6 1.5965(18) . yes P1 F3 1.597(2) . yes P1 F1 1.6028(19) . yes P2 F10 1.588(2) . yes P2 F8 1.5967(19) . yes P2 F11 1.5969(18) . yes P2 F7 1.5994(18) . yes P2 F9 1.5999(17) . yes P2 F12 1.6069(17) . yes P3 F13 1.585(2) . yes P3 F15 1.588(2) . yes P3 F14 1.589(2) . yes P3 F17 1.5908(19) . yes P3 F16 1.593(2) . yes P3 F18 1.602(2) . yes O3 C41 1.206(4) . ? C40 C41 1.504(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.500(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.5314(17) . ? C43 H43D 0.9800 . ? C43 H43E 0.9800 . ? C43 H43F 0.9800 . ? C44 C45 1.5328 . ? C44 H44C 0.9900 . ? C44 H44D 0.9900 . ? C45 C46 1.534(2) . ? C45 H45C 0.9900 . ? C45 H45D 0.9900 . ? C46 C47 1.5310 . ? C46 H46C 0.9900 . ? C46 H46D 0.9900 . ? C47 H47D 0.9800 . ? C47 H47E 0.9800 . ? C47 H47F 0.9800 . ? C43A C44A 1.5310 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A C45A 1.5331(18) . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.5328 . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A C47A 1.531(2) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? 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 N7 Co1 O1 90.48(9) . . yes N7 Co1 N3 174.79(9) . . yes O1 Co1 N3 90.93(8) . . yes N7 Co1 N1 93.07(10) . . yes O1 Co1 N1 87.77(9) . . yes N3 Co1 N1 81.98(10) . . yes N7 Co1 N5 103.42(10) . . yes O1 Co1 N5 91.64(9) . . yes N3 Co1 N5 81.55(10) . . yes N1 Co1 N5 163.51(9) . . yes N7 Co1 N6 80.17(9) . . yes O1 Co1 N6 170.56(8) . . yes N3 Co1 N6 98.27(9) . . yes N1 Co1 N6 91.42(9) . . yes N5 Co1 N6 91.79(9) . . yes N8 Co2 O2 91.48(8) . . yes N8 Co2 N12 173.67(9) . . yes O2 Co2 N12 87.00(8) . . yes N8 Co2 N10 92.46(9) . . yes O2 Co2 N10 87.94(9) . . yes N12 Co2 N10 81.35(9) . . yes N8 Co2 N14 104.50(9) . . yes O2 Co2 N14 92.36(9) . . yes N12 Co2 N14 81.71(9) . . yes N10 Co2 N14 163.02(9) . . yes N8 Co2 N9 79.63(9) . . yes O2 Co2 N9 170.92(8) . . yes N12 Co2 N9 101.64(9) . . yes N10 Co2 N9 90.59(9) . . yes N14 Co2 N9 91.66(9) . . yes O2 O1 Co1 112.61(13) . . ? O1 O2 Co2 113.67(13) . . ? C4 N1 C1 107.0(2) . . ? C4 N1 Co1 113.75(18) . . ? C1 N1 Co1 139.1(2) . . ? C4 N2 C2 106.9(2) . . ? C4 N2 C3 127.7(2) . . ? C2 N2 C3 125.4(2) . . ? C9 N3 C5 122.1(2) . . ? C9 N3 Co1 119.31(18) . . ? C5 N3 Co1 118.51(18) . . ? C10 N4 C12 107.0(2) . . ? C10 N4 C11 127.5(2) . . ? C12 N4 C11 125.5(2) . . ? C10 N5 C13 106.8(2) . . ? C10 N5 Co1 113.46(18) . . ? C13 N5 Co1 139.60(19) . . ? C14 N6 C18 118.6(2) . . ? C14 N6 Co1 127.70(18) . . ? C18 N6 Co1 113.74(17) . . ? N8 N7 C19 108.7(2) . . ? N8 N7 Co1 129.85(17) . . ? C19 N7 Co1 119.43(17) . . ? N7 N8 C21 108.6(2) . . ? N7 N8 Co2 128.03(17) . . ? C21 N8 Co2 119.73(17) . . ? C26 N9 C22 118.6(2) . . ? C26 N9 Co2 127.56(17) . . ? C22 N9 Co2 113.81(17) . . ? C30 N10 C27 106.9(2) . . ? C30 N10 Co2 113.59(17) . . ? C27 N10 Co2 139.43(19) . . ? C30 N11 C28 107.1(2) . . ? C30 N11 C29 127.7(2) . . ? C28 N11 C29 125.2(2) . . ? C31 N12 C35 122.0(2) . . ? C31 N12 Co2 118.28(17) . . ? C35 N12 Co2 119.09(17) . . ? C36 N13 C38 107.1(2) . . ? C36 N13 C37 127.6(2) . . ? C38 N13 C37 125.3(2) . . ? C36 N14 C39 106.9(2) . . ? C36 N14 Co2 112.66(17) . . ? C39 N14 Co2 140.42(18) . . ? C2 C1 N1 108.4(2) . . ? C2 C1 H1 125.8 . . ? N1 C1 H1 125.8 . . ? C1 C2 N2 107.3(2) . . ? C1 C2 H2 126.4 . . ? N2 C2 H2 126.4 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 N2 110.4(2) . . ? N1 C4 C5 116.8(2) . . ? N2 C4 C5 132.8(2) . . ? N3 C5 C6 120.1(2) . . ? N3 C5 C4 108.8(2) . . ? C6 C5 C4 131.1(3) . . ? C7 C6 C5 118.1(3) . . ? C7 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? C8 C7 C6 121.5(3) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C9 118.1(3) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? N3 C9 C8 120.2(2) . . ? N3 C9 C10 108.4(2) . . ? C8 C9 C10 131.4(2) . . ? N5 C10 N4 110.4(2) . . ? N5 C10 C9 117.3(2) . . ? N4 C10 C9 132.3(2) . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 N4 107.1(2) . . ? C13 C12 H12 126.4 . . ? N4 C12 H12 126.4 . . ? N5 C13 C12 108.7(2) . . ? N5 C13 H13 125.7 . . ? C12 C13 H13 125.7 . . ? N6 C14 C15 122.2(2) . . ? N6 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 119.1(2) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 118.7(2) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N6 C18 C17 122.1(2) . . ? N6 C18 C19 112.7(2) . . ? C17 C18 C19 125.2(2) . . ? N7 C19 C20 109.3(2) . . ? N7 C19 C18 112.6(2) . . ? C20 C19 C18 138.1(2) . . ? C19 C20 C21 103.8(2) . . ? C19 C20 H20 128.1 . . ? C21 C20 H20 128.1 . . ? N8 C21 C20 109.5(2) . . ? N8 C21 C22 112.8(2) . . ? C20 C21 C22 137.5(2) . . ? N9 C22 C23 122.0(2) . . ? N9 C22 C21 112.6(2) . . ? C23 C22 C21 125.4(2) . . ? C24 C23 C22 118.8(2) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 119.2(2) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 119.1(2) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? N9 C26 C25 122.2(2) . . ? N9 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C28 C27 N10 108.2(2) . . ? C28 C27 H27 125.9 . . ? N10 C27 H27 125.9 . . ? C27 C28 N11 107.4(2) . . ? C27 C28 H28 126.3 . . ? N11 C28 H28 126.3 . . ? N11 C29 H29A 109.5 . . ? N11 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N11 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 N11 110.3(2) . . ? N10 C30 C31 116.6(2) . . ? N11 C30 C31 132.8(2) . . ? N12 C31 C32 120.4(2) . . ? N12 C31 C30 108.7(2) . . ? C32 C31 C30 130.9(3) . . ? C31 C32 C33 117.8(2) . . ? C31 C32 H32 121.1 . . ? C33 C32 H32 121.1 . . ? C32 C33 C34 121.5(2) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 118.1(2) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? N12 C35 C34 120.0(2) . . ? N12 C35 C36 108.7(2) . . ? C34 C35 C36 131.1(2) . . ? N13 C36 N14 110.3(2) . . ? N13 C36 C35 132.1(2) . . ? N14 C36 C35 117.5(2) . . ? N13 C37 H37A 109.5 . . ? N13 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N13 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 N13 107.2(2) . . ? C39 C38 H38 126.4 . . ? N13 C38 H38 126.4 . . ? N14 C39 C38 108.6(2) . . ? N14 C39 H39 125.7 . . ? C38 C39 H39 125.7 . . ? F4 P1 F2 178.43(13) . . yes F4 P1 F5 90.91(12) . . yes F2 P1 F5 90.61(13) . . yes F4 P1 F6 90.45(11) . . yes F2 P1 F6 89.94(11) . . yes F5 P1 F6 90.37(11) . . yes F4 P1 F3 88.68(12) . . yes F2 P1 F3 89.80(13) . . yes F5 P1 F3 179.47(12) . . yes F6 P1 F3 89.97(11) . . yes F4 P1 F1 89.87(12) . . yes F2 P1 F1 89.75(12) . . yes F5 P1 F1 89.15(11) . . yes F6 P1 F1 179.43(11) . . yes F3 P1 F1 90.51(11) . . yes F10 P2 F8 179.48(12) . . yes F10 P2 F11 90.22(11) . . yes F8 P2 F11 89.93(11) . . yes F10 P2 F7 90.85(12) . . yes F8 P2 F7 89.65(11) . . yes F11 P2 F7 90.37(10) . . yes F10 P2 F9 89.76(11) . . yes F8 P2 F9 90.09(11) . . yes F11 P2 F9 179.56(10) . . yes F7 P2 F9 90.07(10) . . yes F10 P2 F12 89.34(11) . . yes F8 P2 F12 90.16(10) . . yes F11 P2 F12 89.65(10) . . yes F7 P2 F12 179.81(12) . . yes F9 P2 F12 89.90(9) . . yes F13 P3 F15 90.44(16) . . yes F13 P3 F14 89.36(13) . . yes F15 P3 F14 90.02(13) . . yes F13 P3 F17 89.48(12) . . yes F15 P3 F17 179.34(14) . . yes F14 P3 F17 90.64(12) . . yes F13 P3 F16 91.75(14) . . yes F15 P3 F16 90.31(12) . . yes F14 P3 F16 178.85(14) . . yes F17 P3 F16 89.03(11) . . yes F13 P3 F18 179.17(15) . . yes F15 P3 F18 90.30(17) . . yes F14 P3 F18 90.26(13) . . yes F17 P3 F18 89.79(13) . . yes F16 P3 F18 88.63(14) . . yes C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O3 C41 C42 121.7(3) . . ? O3 C41 C40 121.6(3) . . ? C42 C41 C40 116.7(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 H43D 109.5 . . ? C44 C43 H43E 109.5 . . ? H43D C43 H43E 109.5 . . ? C44 C43 H43F 109.5 . . ? H43D C43 H43F 109.5 . . ? H43E C43 H43F 109.5 . . ? C43 C44 C45 113.3 . . ? C43 C44 H44C 108.9 . . ? C45 C44 H44C 108.9 . . ? C43 C44 H44D 108.9 . . ? C45 C44 H44D 108.9 . . ? H44C C44 H44D 107.7 . . ? C44 C45 C46 113.8 . . ? C44 C45 H45C 108.8 . . ? C46 C45 H45C 108.8 . . ? C44 C45 H45D 108.8 . . ? C46 C45 H45D 108.8 . . ? H45C C45 H45D 107.7 . . ? C47 C46 C45 113.3 . . ? C47 C46 H46C 108.9 . . ? C45 C46 H46C 108.9 . . ? C47 C46 H46D 108.9 . . ? C45 C46 H46D 108.9 . . ? H46C C46 H46D 107.7 . . ? C46 C47 H47D 109.5 . . ? C46 C47 H47E 109.5 . . ? H47D C47 H47E 109.5 . . ? C46 C47 H47F 109.5 . . ? H47D C47 H47F 109.5 . . ? H47E C47 H47F 109.5 . . ? C44A C43A H43A 109.5 . . ? C44A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C44A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C43A C44A C45A 113.3 . . ? C43A C44A H44A 108.9 . . ? C45A C44A H44A 108.9 . . ? C43A C44A H44B 108.9 . . ? C45A C44A H44B 108.9 . . ? H44A C44A H44B 107.7 . . ? C46A C45A C44A 113.8 . . ? C46A C45A H45A 108.8 . . ? C44A C45A H45A 108.8 . . ? C46A C45A H45B 108.8 . . ? C44A C45A H45B 108.8 . . ? H45A C45A H45B 107.7 . . ? C47A C46A C45A 113.3 . . ? C47A C46A H46A 108.9 . . ? C45A C46A H46A 108.9 . . ? C47A C46A H46B 108.9 . . ? C45A C46A H46B 108.9 . . ? H46A C46A H46B 107.7 . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? 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 N7 Co1 O1 O2 54.48(15) . . . . ? N3 Co1 O1 O2 -130.53(14) . . . . ? N1 Co1 O1 O2 147.53(15) . . . . ? N5 Co1 O1 O2 -48.96(15) . . . . ? N6 Co1 O1 O2 62.3(6) . . . . ? Co1 O1 O2 Co2 -90.08(14) . . . . ? N8 Co2 O2 O1 48.82(15) . . . . ? N12 Co2 O2 O1 -137.33(15) . . . . ? N10 Co2 O2 O1 141.24(15) . . . . ? N14 Co2 O2 O1 -55.76(15) . . . . ? N9 Co2 O2 O1 60.4(6) . . . . ? N7 Co1 N1 C4 178.02(18) . . . . ? O1 Co1 N1 C4 87.66(18) . . . . ? N3 Co1 N1 C4 -3.60(18) . . . . ? N5 Co1 N1 C4 -0.6(4) . . . . ? N6 Co1 N1 C4 -101.75(18) . . . . ? N7 Co1 N1 C1 3.4(3) . . . . ? O1 Co1 N1 C1 -87.0(3) . . . . ? N3 Co1 N1 C1 -178.3(3) . . . . ? N5 Co1 N1 C1 -175.2(3) . . . . ? N6 Co1 N1 C1 83.6(3) . . . . ? N7 Co1 N3 C9 -162.3(9) . . . . ? O1 Co1 N3 C9 91.92(19) . . . . ? N1 Co1 N3 C9 179.54(19) . . . . ? N5 Co1 N3 C9 0.41(18) . . . . ? N6 Co1 N3 C9 -90.19(19) . . . . ? N7 Co1 N3 C5 20.9(11) . . . . ? O1 Co1 N3 C5 -84.82(18) . . . . ? N1 Co1 N3 C5 2.79(18) . . . . ? N5 Co1 N3 C5 -176.34(19) . . . . ? N6 Co1 N3 C5 93.06(19) . . . . ? N7 Co1 N5 C10 177.84(17) . . . . ? O1 Co1 N5 C10 -91.27(18) . . . . ? N3 Co1 N5 C10 -0.57(17) . . . . ? N1 Co1 N5 C10 -3.6(4) . . . . ? N6 Co1 N5 C10 97.52(18) . . . . ? N7 Co1 N5 C13 -6.3(3) . . . . ? O1 Co1 N5 C13 84.6(3) . . . . ? N3 Co1 N5 C13 175.3(3) . . . . ? N1 Co1 N5 C13 172.2(3) . . . . ? N6 Co1 N5 C13 -86.7(3) . . . . ? N7 Co1 N6 C14 -172.3(2) . . . . ? O1 Co1 N6 C14 179.7(4) . . . . ? N3 Co1 N6 C14 12.7(2) . . . . ? N1 Co1 N6 C14 94.8(2) . . . . ? N5 Co1 N6 C14 -69.0(2) . . . . ? N7 Co1 N6 C18 7.58(18) . . . . ? O1 Co1 N6 C18 -0.4(6) . . . . ? N3 Co1 N6 C18 -167.39(18) . . . . ? N1 Co1 N6 C18 -85.29(18) . . . . ? N5 Co1 N6 C18 110.89(18) . . . . ? O1 Co1 N7 N8 5.6(2) . . . . ? N3 Co1 N7 N8 -100.2(10) . . . . ? N1 Co1 N7 N8 -82.2(2) . . . . ? N5 Co1 N7 N8 97.4(2) . . . . ? N6 Co1 N7 N8 -173.1(2) . . . . ? O1 Co1 N7 C19 167.5(2) . . . . ? N3 Co1 N7 C19 61.8(11) . . . . ? N1 Co1 N7 C19 79.7(2) . . . . ? N5 Co1 N7 C19 -100.7(2) . . . . ? N6 Co1 N7 C19 -11.16(19) . . . . ? C19 N7 N8 C21 2.3(3) . . . . ? Co1 N7 N8 C21 165.78(18) . . . . ? C19 N7 N8 Co2 160.34(18) . . . . ? Co1 N7 N8 Co2 -36.2(3) . . . . ? O2 Co2 N8 N7 11.1(2) . . . . ? N12 Co2 N8 N7 -64.9(9) . . . . ? N10 Co2 N8 N7 -76.9(2) . . . . ? N14 Co2 N8 N7 103.9(2) . . . . ? N9 Co2 N8 N7 -167.1(2) . . . . ? O2 Co2 N8 C21 166.96(19) . . . . ? N12 Co2 N8 C21 91.0(8) . . . . ? N10 Co2 N8 C21 79.0(2) . . . . ? N14 Co2 N8 C21 -100.2(2) . . . . ? N9 Co2 N8 C21 -11.19(19) . . . . ? N8 Co2 N9 C26 -174.5(2) . . . . ? O2 Co2 N9 C26 173.7(4) . . . . ? N12 Co2 N9 C26 11.8(2) . . . . ? N10 Co2 N9 C26 93.1(2) . . . . ? N14 Co2 N9 C26 -70.0(2) . . . . ? N8 Co2 N9 C22 6.44(17) . . . . ? O2 Co2 N9 C22 -5.4(6) . . . . ? N12 Co2 N9 C22 -167.24(17) . . . . ? N10 Co2 N9 C22 -85.95(18) . . . . ? N14 Co2 N9 C22 110.88(18) . . . . ? N8 Co2 N10 C30 168.55(18) . . . . ? O2 Co2 N10 C30 77.15(18) . . . . ? N12 Co2 N10 C30 -10.12(18) . . . . ? N14 Co2 N10 C30 -14.2(4) . . . . ? N9 Co2 N10 C30 -111.81(18) . . . . ? N8 Co2 N10 C27 -8.3(3) . . . . ? O2 Co2 N10 C27 -99.7(3) . . . . ? N12 Co2 N10 C27 173.0(3) . . . . ? N14 Co2 N10 C27 169.0(3) . . . . ? N9 Co2 N10 C27 71.3(3) . . . . ? N8 Co2 N12 C31 -0.9(9) . . . . ? O2 Co2 N12 C31 -77.11(19) . . . . ? N10 Co2 N12 C31 11.26(18) . . . . ? N14 Co2 N12 C31 -169.9(2) . . . . ? N9 Co2 N12 C31 100.07(19) . . . . ? N8 Co2 N12 C35 170.4(7) . . . . ? O2 Co2 N12 C35 94.16(18) . . . . ? N10 Co2 N12 C35 -177.47(19) . . . . ? N14 Co2 N12 C35 1.34(18) . . . . ? N9 Co2 N12 C35 -88.66(19) . . . . ? N8 Co2 N14 C36 176.84(17) . . . . ? O2 Co2 N14 C36 -91.02(17) . . . . ? N12 Co2 N14 C36 -4.41(17) . . . . ? N10 Co2 N14 C36 -0.4(4) . . . . ? N9 Co2 N14 C36 97.12(17) . . . . ? N8 Co2 N14 C39 -1.0(3) . . . . ? O2 Co2 N14 C39 91.1(3) . . . . ? N12 Co2 N14 C39 177.7(3) . . . . ? N10 Co2 N14 C39 -178.3(3) . . . . ? N9 Co2 N14 C39 -80.8(3) . . . . ? C4 N1 C1 C2 -0.4(3) . . . . ? Co1 N1 C1 C2 174.5(2) . . . . ? N1 C1 C2 N2 -0.2(3) . . . . ? C4 N2 C2 C1 0.8(3) . . . . ? C3 N2 C2 C1 -178.4(2) . . . . ? C1 N1 C4 N2 0.9(3) . . . . ? Co1 N1 C4 N2 -175.40(16) . . . . ? C1 N1 C4 C5 -179.7(2) . . . . ? Co1 N1 C4 C5 3.9(3) . . . . ? C2 N2 C4 N1 -1.1(3) . . . . ? C3 N2 C4 N1 178.0(2) . . . . ? C2 N2 C4 C5 179.7(3) . . . . ? C3 N2 C4 C5 -1.2(5) . . . . ? C9 N3 C5 C6 1.2(4) . . . . ? Co1 N3 C5 C6 177.83(18) . . . . ? C9 N3 C5 C4 -178.0(2) . . . . ? Co1 N3 C5 C4 -1.4(3) . . . . ? N1 C4 C5 N3 -1.7(3) . . . . ? N2 C4 C5 N3 177.4(3) . . . . ? N1 C4 C5 C6 179.2(3) . . . . ? N2 C4 C5 C6 -1.6(5) . . . . ? N3 C5 C6 C7 -0.4(4) . . . . ? C4 C5 C6 C7 178.6(3) . . . . ? C5 C6 C7 C8 -0.1(4) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C5 N3 C9 C8 -1.5(4) . . . . ? Co1 N3 C9 C8 -178.09(18) . . . . ? C5 N3 C9 C10 176.5(2) . . . . ? Co1 N3 C9 C10 -0.2(3) . . . . ? C7 C8 C9 N3 1.0(4) . . . . ? C7 C8 C9 C10 -176.4(3) . . . . ? C13 N5 C10 N4 0.5(3) . . . . ? Co1 N5 C10 N4 177.72(16) . . . . ? C13 N5 C10 C9 -176.5(2) . . . . ? Co1 N5 C10 C9 0.7(3) . . . . ? C12 N4 C10 N5 -0.8(3) . . . . ? C11 N4 C10 N5 177.6(2) . . . . ? C12 N4 C10 C9 175.7(3) . . . . ? C11 N4 C10 C9 -5.9(4) . . . . ? N3 C9 C10 N5 -0.3(3) . . . . ? C8 C9 C10 N5 177.3(3) . . . . ? N3 C9 C10 N4 -176.6(3) . . . . ? C8 C9 C10 N4 1.0(5) . . . . ? C10 N4 C12 C13 0.7(3) . . . . ? C11 N4 C12 C13 -177.8(2) . . . . ? C10 N5 C13 C12 -0.1(3) . . . . ? Co1 N5 C13 C12 -176.1(2) . . . . ? N4 C12 C13 N5 -0.4(3) . . . . ? C18 N6 C14 C15 1.6(4) . . . . ? Co1 N6 C14 C15 -178.5(2) . . . . ? N6 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 -1.9(4) . . . . ? C15 C16 C17 C18 1.5(4) . . . . ? C14 N6 C18 C17 -2.0(4) . . . . ? Co1 N6 C18 C17 178.1(2) . . . . ? C14 N6 C18 C19 176.7(2) . . . . ? Co1 N6 C18 C19 -3.3(3) . . . . ? C16 C17 C18 N6 0.4(4) . . . . ? C16 C17 C18 C19 -178.0(2) . . . . ? N8 N7 C19 C20 -1.6(3) . . . . ? Co1 N7 C19 C20 -167.10(17) . . . . ? N8 N7 C19 C18 177.8(2) . . . . ? Co1 N7 C19 C18 12.4(3) . . . . ? N6 C18 C19 N7 -5.1(3) . . . . ? C17 C18 C19 N7 173.4(2) . . . . ? N6 C18 C19 C20 174.1(3) . . . . ? C17 C18 C19 C20 -7.3(5) . . . . ? N7 C19 C20 C21 0.3(3) . . . . ? C18 C19 C20 C21 -179.0(3) . . . . ? N7 N8 C21 C20 -2.2(3) . . . . ? Co2 N8 C21 C20 -162.31(17) . . . . ? N7 N8 C21 C22 173.7(2) . . . . ? Co2 N8 C21 C22 13.5(3) . . . . ? C19 C20 C21 N8 1.1(3) . . . . ? C19 C20 C21 C22 -173.2(3) . . . . ? C26 N9 C22 C23 -0.4(4) . . . . ? Co2 N9 C22 C23 178.8(2) . . . . ? C26 N9 C22 C21 179.5(2) . . . . ? Co2 N9 C22 C21 -1.3(3) . . . . ? N8 C21 C22 N9 -7.1(3) . . . . ? C20 C21 C22 N9 167.1(3) . . . . ? N8 C21 C22 C23 172.8(2) . . . . ? C20 C21 C22 C23 -13.0(5) . . . . ? N9 C22 C23 C24 -0.7(4) . . . . ? C21 C22 C23 C24 179.3(2) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C23 C24 C25 C26 0.0(4) . . . . ? C22 N9 C26 C25 1.4(4) . . . . ? Co2 N9 C26 C25 -177.62(19) . . . . ? C24 C25 C26 N9 -1.2(4) . . . . ? C30 N10 C27 C28 -0.9(3) . . . . ? Co2 N10 C27 C28 176.1(2) . . . . ? N10 C27 C28 N11 0.1(3) . . . . ? C30 N11 C28 C27 0.7(3) . . . . ? C29 N11 C28 C27 -177.8(3) . . . . ? C27 N10 C30 N11 1.4(3) . . . . ? Co2 N10 C30 N11 -176.50(17) . . . . ? C27 N10 C30 C31 -174.1(2) . . . . ? Co2 N10 C30 C31 8.0(3) . . . . ? C28 N11 C30 N10 -1.3(3) . . . . ? C29 N11 C30 N10 177.1(3) . . . . ? C28 N11 C30 C31 173.2(3) . . . . ? C29 N11 C30 C31 -8.4(5) . . . . ? C35 N12 C31 C32 0.9(4) . . . . ? Co2 N12 C31 C32 171.93(19) . . . . ? C35 N12 C31 C30 179.5(2) . . . . ? Co2 N12 C31 C30 -9.5(3) . . . . ? N10 C30 C31 N12 0.7(3) . . . . ? N11 C30 C31 N12 -173.6(3) . . . . ? N10 C30 C31 C32 179.0(3) . . . . ? N11 C30 C31 C32 4.8(5) . . . . ? N12 C31 C32 C33 1.1(4) . . . . ? C30 C31 C32 C33 -177.1(3) . . . . ? C31 C32 C33 C34 -1.1(4) . . . . ? C32 C33 C34 C35 -0.8(4) . . . . ? C31 N12 C35 C34 -2.9(4) . . . . ? Co2 N12 C35 C34 -173.84(18) . . . . ? C31 N12 C35 C36 172.7(2) . . . . ? Co2 N12 C35 C36 1.8(3) . . . . ? C33 C34 C35 N12 2.8(4) . . . . ? C33 C34 C35 C36 -171.7(3) . . . . ? C38 N13 C36 N14 -1.1(3) . . . . ? C37 N13 C36 N14 175.7(2) . . . . ? C38 N13 C36 C35 173.8(3) . . . . ? C37 N13 C36 C35 -9.4(4) . . . . ? C39 N14 C36 N13 1.2(3) . . . . ? Co2 N14 C36 N13 -177.39(16) . . . . ? C39 N14 C36 C35 -174.6(2) . . . . ? Co2 N14 C36 C35 6.9(3) . . . . ? N12 C35 C36 N13 179.7(2) . . . . ? C34 C35 C36 N13 -5.3(5) . . . . ? N12 C35 C36 N14 -5.7(3) . . . . ? C34 C35 C36 N14 169.3(2) . . . . ? C36 N13 C38 C39 0.5(3) . . . . ? C37 N13 C38 C39 -176.3(2) . . . . ? C36 N14 C39 C38 -0.8(3) . . . . ? Co2 N14 C39 C38 177.1(2) . . . . ? N13 C38 C39 N14 0.2(3) . . . . ? C43 C44 C45 C46 -180.0 . . . . ? C44 C45 C46 C47 180.0 . . . . ? C43A C44A C45A C46A -180.0 . . . . ? C44A C45A C46A C47A 180.00(5) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.871 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.090 # File processed with modiCIFer (v.3-27-2007). I.A.Guzei, UW-Madison.