# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_1(100K) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H84 B2 Cl2 Co2 Fe2 N26 O24' _chemical_formula_weight 2211.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.092(4) _cell_length_b 17.950(4) _cell_length_c 20.171(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.172(13) _cell_angle_gamma 90.00 _cell_volume 4876.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.45 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7749 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29876 _diffrn_reflns_av_R_equivalents 0.1390 _diffrn_reflns_av_sigmaI/netI 0.1270 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8523 _reflns_number_gt 3618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The disordered pyrazol ring of the Tp ligand (N8, N9, C10(C10'), C11(C11'), C12(C12')), ethoxycarbonly groups (C39(C39'), O5(O5'), O6(O6'), C40(C40'), C41(C41')) and (C26(C26'), O3(O3'), O4(O4'), C27(C27'), C28(C28')), and the ClO4 anion were treated with a two-site model with refined variable site occupancy factors. The distances for the disordered atoms of C39, C39', O5, O5', O6, O6' were restrained using DFIX commands. 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^)+(0.2000P)^2^+0.0000P] 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 8523 _refine_ls_number_parameters 824 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2522 _refine_ls_R_factor_gt 0.1277 _refine_ls_wR_factor_ref 0.3841 _refine_ls_wR_factor_gt 0.3074 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25590(10) 0.48455(8) 0.62884(8) 0.0498(5) Uani 1 1 d . . . Fe1 Fe 0.02175(11) 0.45515(8) 0.33800(9) 0.0545(5) Uani 1 1 d . A . B1 B 0.0339(9) 0.3293(7) 0.2391(8) 0.058(3) Uani 1 1 d . . . H1 H 0.0378 0.2885 0.2071 0.070 Uiso 1 1 d R . . N1 N 0.1583(6) 0.4767(4) 0.5136(5) 0.050(2) Uani 1 1 d . A . N2 N -0.1537(7) 0.4943(5) 0.3486(5) 0.061(3) Uani 1 1 d . . . N3 N 0.0446(13) 0.6259(6) 0.3351(10) 0.128(5) Uani 1 1 d . A . N4 N 0.0067(6) 0.3471(4) 0.3492(5) 0.048(2) Uani 1 1 d . . . N5 N 0.0106(6) 0.2978(5) 0.2987(5) 0.053(2) Uani 1 1 d . . . N6 N 0.1377(6) 0.4295(4) 0.3325(5) 0.052(2) Uani 1 1 d . . . N7 N 0.1317(7) 0.3714(5) 0.2867(6) 0.059(2) Uani 1 1 d . . . N8 N -0.0636(8) 0.4426(6) 0.2232(5) 0.075(3) Uani 1 1 d . . . N9 N -0.0468(8) 0.3865(6) 0.1858(6) 0.080(3) Uani 1 1 d . A . N10 N 0.3641(6) 0.5069(5) 0.7434(5) 0.051(2) Uani 1 1 d . . . N11 N 0.2661(5) 0.5971(4) 0.6232(4) 0.0345(17) Uani 1 1 d . B . N12 N 0.2418(6) 0.3736(5) 0.6327(5) 0.055(2) Uani 1 1 d . C . N13 N 0.3630(6) 0.4519(5) 0.6110(5) 0.055(2) Uani 1 1 d . . . C1 C 0.1050(7) 0.4655(5) 0.4469(6) 0.040(2) Uani 1 1 d . . . C2 C -0.0880(8) 0.4780(6) 0.3443(6) 0.049(3) Uani 1 1 d . . . C3 C 0.0340(9) 0.5604(8) 0.3348(7) 0.073(4) Uani 1 1 d . . . C4 C -0.0093(8) 0.3087(6) 0.3975(7) 0.059(3) Uani 1 1 d . . . H4 H -0.0191 0.3292 0.4362 0.071 Uiso 1 1 calc R . . C5 C -0.0092(9) 0.2316(6) 0.3813(8) 0.069(3) Uani 1 1 d . . . H5 H -0.0149 0.1907 0.4084 0.083 Uiso 1 1 calc R . . C6 C 0.0007(9) 0.2290(7) 0.3182(8) 0.068(3) Uani 1 1 d . . . H6 H 0.0006 0.1848 0.2922 0.082 Uiso 1 1 calc R . . C7 C 0.2313(10) 0.4544(7) 0.3694(8) 0.080(4) Uani 1 1 d . . . H7 H 0.2575 0.4954 0.4050 0.096 Uiso 1 1 calc R . . C8 C 0.2837(10) 0.4113(8) 0.3479(10) 0.096(5) Uani 1 1 d . . . H8 H 0.3509 0.4179 0.3642 0.115 Uiso 1 1 calc R . . C9 C 0.2218(9) 0.3589(6) 0.2998(8) 0.069(3) Uani 1 1 d . . . H9 H 0.2385 0.3191 0.2781 0.083 Uiso 1 1 calc R . . C10 C -0.158(6) 0.459(4) 0.164(4) 0.10(2) Uani 0.45(8) 1 d P A 1 H10 H -0.1943 0.4971 0.1692 0.118 Uiso 0.45(8) 1 calc PR A 1 C11 C -0.199(5) 0.418(4) 0.095(2) 0.10(2) Uani 0.45(8) 1 d P A 1 H11 H -0.2635 0.4229 0.0486 0.125 Uiso 0.45(8) 1 calc PR A 1 C12 C -0.123(7) 0.369(5) 0.111(5) 0.11(2) Uani 0.45(8) 1 d P A 1 H12 H -0.1239 0.3319 0.0768 0.131 Uiso 0.45(8) 1 calc PR A 1 C10' C -0.127(5) 0.492(4) 0.168(4) 0.094(16) Uani 0.55(8) 1 d P A 2 H10' H -0.1513 0.5360 0.1780 0.113 Uiso 0.55(8) 1 calc PR A 2 C11' C -0.152(3) 0.468(3) 0.0949(18) 0.098(18) Uani 0.55(8) 1 d P A 2 H11' H -0.1947 0.4922 0.0453 0.118 Uiso 0.55(8) 1 calc PR A 2 C12' C -0.101(6) 0.405(3) 0.108(4) 0.103(18) Uani 0.55(8) 1 d P A 2 H12' H -0.1040 0.3758 0.0679 0.124 Uiso 0.55(8) 1 calc PR A 2 C13 C 0.4175(9) 0.4561(6) 0.7989(8) 0.065(3) Uani 1 1 d . . . H13 H 0.4064 0.4047 0.7860 0.078 Uiso 1 1 calc R . . C14 C 0.4888(10) 0.4779(10) 0.8753(8) 0.091(4) Uani 1 1 d . . . H14 H 0.5295 0.4414 0.9137 0.109 Uiso 1 1 calc R . . C15 C 0.5014(9) 0.5515(8) 0.8959(7) 0.069(3) Uani 1 1 d . . . C16 C 0.4471(8) 0.6051(6) 0.8371(7) 0.060(3) Uani 1 1 d . . . H16 H 0.4575 0.6569 0.8489 0.071 Uiso 1 1 calc R . . C17 C 0.3769(7) 0.5798(6) 0.7604(6) 0.054(3) Uani 1 1 d . . . C23 C 0.5755(10) 0.5770(10) 0.9814(9) 0.080(4) Uani 1 1 d . . . O1 O 0.6183(6) 0.5299(6) 1.0318(6) 0.095(3) Uani 1 1 d . . . O2 O 0.5793(7) 0.6496(7) 0.9896(5) 0.096(3) Uani 1 1 d . . . C24 C 0.6414(12) 0.6758(10) 1.0732(9) 0.114(6) Uani 1 1 d . . . H24A H 0.6148 0.7236 1.0786 0.137 Uiso 1 1 calc R . . H24B H 0.6388 0.6388 1.1085 0.137 Uiso 1 1 calc R . . C25 C 0.7458(11) 0.6862(9) 1.0973(9) 0.101(5) Uani 1 1 d . . . H25A H 0.7693 0.6407 1.0857 0.151 Uiso 1 1 calc R . . H25B H 0.7874 0.6967 1.1542 0.151 Uiso 1 1 calc R . . H25C H 0.7496 0.7280 1.0678 0.151 Uiso 1 1 calc R . . C18 C 0.3146(7) 0.6306(5) 0.6934(6) 0.050(3) Uani 1 1 d . . . C19 C 0.3080(7) 0.7052(5) 0.7002(7) 0.059(3) Uani 1 1 d . B . H19 H 0.3431 0.7273 0.7514 0.071 Uiso 1 1 calc R . . C20 C 0.2521(8) 0.7494(6) 0.6353(7) 0.065(3) Uani 1 1 d . . . C21 C 0.2032(8) 0.7123(6) 0.5610(7) 0.062(3) Uani 1 1 d . B . H21 H 0.1616 0.7399 0.5139 0.075 Uiso 1 1 calc R . . C22 C 0.2146(8) 0.6389(7) 0.5564(7) 0.067(3) Uani 1 1 d . . . H22 H 0.1866 0.6160 0.5060 0.080 Uiso 1 1 calc R B . C26 C 0.249(3) 0.833(3) 0.636(3) 0.064(9) Uani 0.703(18) 1 d P B 1 O3 O 0.196(2) 0.8701(16) 0.5761(19) 0.063(6) Uani 0.703(18) 1 d P B 1 O4 O 0.2946(11) 0.8550(6) 0.7084(8) 0.060(4) Uani 0.703(18) 1 d P B 1 C27 C 0.2872(14) 0.9369(9) 0.7163(11) 0.069(6) Uani 0.703(18) 1 d P B 1 H27A H 0.3007 0.9475 0.7694 0.083 Uiso 0.703(18) 1 calc PR B 1 H27B H 0.2184 0.9530 0.6767 0.083 Uiso 0.703(18) 1 calc PR B 1 C28 C 0.3589(13) 0.9834(10) 0.7049(10) 0.075(6) Uani 0.703(18) 1 d P B 1 H28A H 0.4250 0.9608 0.7347 0.113 Uiso 0.703(18) 1 calc PR B 1 H28B H 0.3625 1.0342 0.7241 0.113 Uiso 0.703(18) 1 calc PR B 1 H28C H 0.3346 0.9850 0.6485 0.113 Uiso 0.703(18) 1 calc PR B 1 C26' C 0.221(8) 0.826(6) 0.647(8) 0.06(2) Uani 0.297(18) 1 d P B 2 O3' O 0.168(5) 0.863(4) 0.586(5) 0.065(14) Uani 0.297(18) 1 d P B 2 O4' O 0.239(3) 0.8478(15) 0.7146(19) 0.065(9) Uani 0.297(18) 1 d P B 2 C27' C 0.225(3) 0.926(2) 0.736(3) 0.071(13) Uani 0.297(18) 1 d P B 2 H27C H 0.2619 0.9300 0.7939 0.085 Uiso 0.297(18) 1 calc PR B 2 H27D H 0.2537 0.9618 0.7165 0.085 Uiso 0.297(18) 1 calc PR B 2 C28' C 0.119(3) 0.9458(18) 0.702(2) 0.065(13) Uani 0.297(18) 1 d P B 2 H28D H 0.0835 0.9475 0.6437 0.098 Uiso 0.297(18) 1 calc PR B 2 H28E H 0.1160 0.9948 0.7215 0.098 Uiso 0.297(18) 1 calc PR B 2 H28F H 0.0886 0.9085 0.7172 0.098 Uiso 0.297(18) 1 calc PR B 2 C29 C 0.1704(9) 0.3387(7) 0.6363(7) 0.066(3) Uani 1 1 d . . . H29 H 0.1329 0.3662 0.6514 0.079 Uiso 1 1 calc R . . C30 C 0.1500(9) 0.2639(8) 0.6185(8) 0.075(4) Uani 1 1 d . C . H30 H 0.0983 0.2410 0.6206 0.090 Uiso 1 1 calc R . . C31 C 0.2041(10) 0.2230(7) 0.5979(8) 0.069(3) Uani 1 1 d . . . C32 C 0.2769(9) 0.2578(6) 0.5923(7) 0.067(3) Uani 1 1 d . C . H32 H 0.3137 0.2315 0.5757 0.080 Uiso 1 1 calc R . . C33 C 0.2936(8) 0.3329(6) 0.6120(6) 0.054(3) Uani 1 1 d . . . C39 C 0.171(15) 0.144(8) 0.571(12) 0.12(3) Uani 0.55(4) 1 d PD C 1 O5 O 0.216(5) 0.112(4) 0.545(4) 0.111(17) Uani 0.55(4) 1 d PD C 1 O6 O 0.115(9) 0.112(7) 0.589(6) 0.12(2) Uani 0.55(4) 1 d PD C 1 C40 C 0.071(4) 0.035(2) 0.547(3) 0.136(17) Uani 0.55(4) 1 d P C 1 H40A H 0.0266 0.0411 0.4885 0.163 Uiso 0.55(4) 1 calc PR C 1 H40B H 0.1234 -0.0014 0.5593 0.163 Uiso 0.55(4) 1 calc PR C 1 C41 C 0.011(3) 0.012(2) 0.584(3) 0.16(2) Uani 0.55(4) 1 d P C 1 H41A H 0.0338 0.0421 0.6313 0.233 Uiso 0.55(4) 1 calc PR C 1 H41B H 0.0219 -0.0406 0.5975 0.233 Uiso 0.55(4) 1 calc PR C 1 H41C H -0.0598 0.0214 0.5452 0.233 Uiso 0.55(4) 1 calc PR C 1 C39' C 0.194(11) 0.140(11) 0.582(12) 0.12(6) Uani 0.45(4) 1 d PD C 2 O5' O 0.258(5) 0.111(4) 0.575(5) 0.11(2) Uani 0.45(4) 1 d PD C 2 O6' O 0.106(12) 0.119(9) 0.560(8) 0.13(3) Uani 0.45(4) 1 d PD C 2 C40' C 0.105(5) 0.047(3) 0.515(4) 0.15(2) Uani 0.45(4) 1 d P C 2 H40C H 0.1730 0.0367 0.5292 0.178 Uiso 0.45(4) 1 calc PR C 2 H40D H 0.0842 0.0040 0.5340 0.178 Uiso 0.45(4) 1 calc PR C 2 C41' C 0.035(4) 0.050(2) 0.423(4) 0.18(3) Uani 0.45(4) 1 d P C 2 H41D H 0.0657 0.0806 0.4020 0.264 Uiso 0.45(4) 1 calc PR C 2 H41E H -0.0287 0.0728 0.4085 0.264 Uiso 0.45(4) 1 calc PR C 2 H41F H 0.0230 -0.0001 0.4013 0.264 Uiso 0.45(4) 1 calc PR C 2 C34 C 0.3673(7) 0.3760(6) 0.6038(6) 0.054(3) Uani 1 1 d . C . C35 C 0.4357(9) 0.3441(7) 0.5915(6) 0.064(3) Uani 1 1 d . . . H35 H 0.4413 0.2916 0.5899 0.077 Uiso 1 1 calc R C . C36 C 0.4964(10) 0.3919(9) 0.5814(7) 0.078(4) Uani 1 1 d . C . C37 C 0.4877(9) 0.4665(8) 0.5840(7) 0.074(4) Uani 1 1 d . . . H37 H 0.5275 0.4994 0.5757 0.089 Uiso 1 1 calc R C . C38 C 0.4185(9) 0.4938(8) 0.5992(7) 0.072(4) Uani 1 1 d . C . H38 H 0.4119 0.5463 0.6008 0.086 Uiso 1 1 calc R . . C42 C 0.5717(10) 0.3623(11) 0.5663(8) 0.087(4) Uani 1 1 d . . . O7 O 0.6157(7) 0.4014(6) 0.5465(6) 0.102(3) Uani 1 1 d . C . O8 O 0.5871(7) 0.2898(7) 0.5784(6) 0.095(3) Uani 1 1 d . C . C43 C 0.6635(17) 0.2553(15) 0.5654(15) 0.170(10) Uani 1 1 d . . . H43A H 0.6484 0.2023 0.5497 0.205 Uiso 1 1 calc R C . H43B H 0.6676 0.2829 0.5248 0.205 Uiso 1 1 calc R . . C44 C 0.7535(17) 0.2631(19) 0.6429(19) 0.239(16) Uani 1 1 d . C . H44A H 0.7401 0.2930 0.6766 0.358 Uiso 1 1 calc R . . H44B H 0.8042 0.2879 0.6380 0.358 Uiso 1 1 calc R . . H44C H 0.7774 0.2138 0.6665 0.358 Uiso 1 1 calc R . . Cl1 Cl 0.528(4) 0.762(4) 0.193(3) 0.075(5) Uani 0.73(7) 1 d P D 1 O9 O 0.5239(17) 0.771(2) 0.2621(16) 0.114(11) Uani 0.73(7) 1 d P D 1 O10 O 0.497(3) 0.8260(19) 0.144(2) 0.125(10) Uani 0.73(7) 1 d P D 1 O11 O 0.625(4) 0.7376(16) 0.214(3) 0.066(7) Uani 0.73(7) 1 d P D 1 O12 O 0.4598(13) 0.7061(9) 0.147(2) 0.105(12) Uani 0.73(7) 1 d P D 1 Cl1' Cl 0.521(11) 0.776(10) 0.192(10) 0.09(3) Uani 0.27(7) 1 d P D 2 O9' O 0.541(5) 0.822(5) 0.256(4) 0.11(2) Uani 0.27(7) 1 d P D 2 O10' O 0.449(7) 0.814(5) 0.123(6) 0.12(3) Uani 0.27(7) 1 d P D 2 O11' O 0.622(9) 0.765(6) 0.219(8) 0.07(2) Uani 0.27(7) 1 d P D 2 O12' O 0.490(4) 0.713(3) 0.216(6) 0.10(3) Uani 0.27(7) 1 d P D 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 0.0487(8) 0.0419(8) 0.0471(9) -0.0085(6) 0.0187(7) 0.0010(6) Fe1 0.0585(10) 0.0390(9) 0.0533(10) 0.0017(7) 0.0225(8) 0.0069(7) B1 0.057(8) 0.058(8) 0.057(8) -0.023(6) 0.030(7) 0.001(6) N1 0.046(5) 0.050(5) 0.053(6) -0.012(4) 0.026(5) -0.005(4) N2 0.055(6) 0.050(6) 0.047(5) -0.019(4) 0.008(5) 0.014(4) N3 0.206(16) 0.038(7) 0.164(14) 0.024(8) 0.117(13) 0.021(8) N4 0.039(5) 0.035(5) 0.057(6) -0.009(4) 0.018(4) -0.002(3) N5 0.047(5) 0.046(5) 0.067(6) -0.023(4) 0.031(5) -0.024(4) N6 0.058(5) 0.039(5) 0.071(6) -0.004(4) 0.042(5) -0.008(4) N7 0.060(6) 0.042(5) 0.070(6) -0.007(5) 0.032(5) -0.009(4) N8 0.097(8) 0.080(7) 0.039(5) 0.007(5) 0.032(6) 0.040(6) N9 0.072(7) 0.104(9) 0.053(7) -0.002(6) 0.027(6) 0.025(6) N10 0.052(5) 0.057(6) 0.042(5) -0.005(4) 0.024(4) 0.015(4) N11 0.028(4) 0.027(4) 0.030(4) 0.007(3) 0.004(3) 0.002(3) N12 0.034(5) 0.081(7) 0.035(5) -0.011(4) 0.009(4) 0.001(4) N13 0.050(5) 0.057(6) 0.055(6) -0.013(4) 0.027(5) -0.010(4) C1 0.034(5) 0.039(6) 0.045(6) -0.004(4) 0.021(5) 0.003(4) C2 0.042(6) 0.042(6) 0.034(5) -0.013(4) 0.003(5) 0.008(4) C3 0.081(9) 0.076(10) 0.058(8) 0.024(7) 0.035(7) 0.023(7) C4 0.072(7) 0.044(6) 0.060(7) -0.004(5) 0.036(6) -0.005(5) C5 0.081(9) 0.035(6) 0.090(10) -0.017(6) 0.046(8) -0.029(6) C6 0.068(8) 0.058(8) 0.077(9) -0.019(6) 0.039(7) -0.017(6) C7 0.090(10) 0.060(8) 0.106(11) -0.019(7) 0.063(9) -0.021(7) C8 0.071(9) 0.081(10) 0.149(15) -0.019(9) 0.069(10) -0.025(8) C9 0.080(9) 0.049(7) 0.110(11) -0.007(7) 0.073(8) -0.014(6) C10 0.11(5) 0.09(5) 0.06(3) 0.00(4) 0.03(3) 0.03(3) C11 0.11(4) 0.09(4) 0.06(2) 0.00(2) 0.02(2) 0.04(3) C12 0.12(5) 0.09(5) 0.07(3) 0.00(4) 0.02(3) 0.04(4) C10' 0.11(4) 0.08(4) 0.06(2) 0.00(3) 0.03(2) 0.03(3) C11' 0.11(3) 0.09(3) 0.060(19) 0.005(17) 0.024(18) 0.04(3) C12' 0.12(4) 0.09(4) 0.06(2) 0.00(3) 0.02(2) 0.04(3) C13 0.083(9) 0.044(6) 0.076(9) 0.010(6) 0.049(8) 0.016(6) C14 0.075(10) 0.106(13) 0.060(9) 0.006(8) 0.016(8) 0.009(8) C15 0.058(7) 0.088(10) 0.052(7) 0.007(7) 0.024(6) 0.023(7) C16 0.051(6) 0.051(7) 0.081(9) -0.015(6) 0.039(6) 0.000(5) C17 0.041(6) 0.049(7) 0.060(7) 0.000(5) 0.021(5) 0.005(5) C23 0.073(9) 0.095(11) 0.082(11) 0.003(9) 0.049(8) -0.012(8) O1 0.065(6) 0.126(8) 0.075(6) 0.042(6) 0.026(5) 0.004(5) O2 0.089(7) 0.120(9) 0.048(5) -0.010(5) 0.017(5) 0.001(6) C24 0.097(12) 0.141(16) 0.068(10) -0.002(10) 0.021(9) 0.019(10) C25 0.086(11) 0.104(12) 0.077(10) -0.013(9) 0.022(8) -0.004(8) C18 0.046(6) 0.039(6) 0.048(7) -0.009(5) 0.015(5) -0.004(4) C19 0.043(6) 0.037(6) 0.066(8) -0.003(5) 0.010(6) -0.002(4) C20 0.048(6) 0.051(7) 0.065(8) 0.008(6) 0.010(6) 0.004(5) C21 0.065(7) 0.043(7) 0.060(8) 0.003(5) 0.023(6) -0.007(5) C22 0.065(7) 0.059(8) 0.055(8) -0.014(6) 0.020(6) 0.003(6) C26 0.06(2) 0.051(16) 0.06(2) -0.010(13) 0.018(16) -0.001(15) O3 0.062(15) 0.051(9) 0.062(13) 0.001(8) 0.024(10) -0.016(9) O4 0.052(8) 0.050(7) 0.061(8) -0.008(5) 0.020(7) 0.003(6) C27 0.062(12) 0.054(11) 0.060(11) -0.013(8) 0.014(9) 0.007(8) C28 0.064(11) 0.079(12) 0.061(12) -0.026(9) 0.020(9) -0.005(9) C26' 0.06(6) 0.05(3) 0.06(5) -0.01(3) 0.02(4) -0.01(3) O3' 0.06(4) 0.06(3) 0.07(3) 0.00(2) 0.03(2) -0.01(2) O4' 0.06(2) 0.050(17) 0.07(2) -0.011(14) 0.020(17) 0.003(14) C27' 0.07(3) 0.05(2) 0.07(3) -0.01(2) 0.02(2) 0.00(2) C28' 0.07(3) 0.03(2) 0.07(3) -0.015(17) 0.02(2) 0.000(16) C29 0.068(8) 0.075(9) 0.059(8) 0.008(6) 0.038(7) 0.002(6) C30 0.066(8) 0.084(10) 0.076(9) 0.032(7) 0.039(7) -0.010(7) C31 0.080(9) 0.057(8) 0.085(9) -0.009(6) 0.055(8) -0.007(6) C32 0.086(9) 0.054(7) 0.064(8) 0.000(6) 0.043(7) -0.013(6) C33 0.053(6) 0.054(7) 0.044(6) -0.002(5) 0.020(5) -0.003(5) C39 0.14(6) 0.07(5) 0.18(9) 0.01(5) 0.11(7) -0.02(5) O5 0.13(4) 0.09(2) 0.14(4) 0.00(2) 0.09(4) -0.02(3) O6 0.15(4) 0.06(3) 0.18(6) 0.01(4) 0.12(5) -0.03(2) C40 0.15(4) 0.07(2) 0.19(5) 0.01(2) 0.10(3) -0.03(2) C41 0.13(3) 0.10(3) 0.24(5) 0.01(3) 0.11(3) -0.05(2) C39' 0.14(12) 0.07(7) 0.18(11) 0.01(6) 0.11(9) -0.02(5) O5' 0.14(5) 0.049(18) 0.17(6) 0.02(3) 0.10(5) -0.02(3) O6' 0.15(4) 0.07(4) 0.19(9) 0.01(5) 0.11(6) -0.02(3) C40' 0.16(5) 0.08(3) 0.19(7) 0.00(4) 0.09(5) -0.02(3) C41' 0.18(5) 0.06(3) 0.20(6) -0.03(3) 0.05(4) -0.01(3) C34 0.043(6) 0.064(8) 0.051(7) -0.018(5) 0.022(5) -0.007(5) C35 0.063(7) 0.071(8) 0.046(7) -0.008(6) 0.022(6) -0.008(6) C36 0.066(8) 0.104(12) 0.046(7) 0.001(7) 0.018(6) 0.009(8) C37 0.061(8) 0.084(11) 0.067(8) -0.012(7) 0.029(7) -0.033(7) C38 0.072(8) 0.092(10) 0.049(7) -0.027(6) 0.032(7) -0.042(7) C42 0.055(8) 0.137(15) 0.050(8) -0.034(9) 0.017(7) -0.020(9) O7 0.068(6) 0.164(10) 0.078(7) -0.029(6) 0.043(5) -0.051(6) O8 0.072(6) 0.122(9) 0.086(7) -0.011(6) 0.040(6) -0.001(6) C43 0.122(18) 0.24(3) 0.17(2) 0.014(19) 0.097(18) 0.067(18) C44 0.085(17) 0.31(4) 0.27(4) 0.06(3) 0.07(2) 0.022(19) Cl1 0.070(10) 0.077(15) 0.082(8) 0.026(8) 0.045(7) 0.025(9) O9 0.094(14) 0.15(4) 0.110(17) 0.013(19) 0.061(12) 0.040(18) O10 0.086(19) 0.079(16) 0.13(2) 0.038(14) 0.008(18) 0.046(16) O11 0.075(11) 0.045(14) 0.076(11) 0.007(13) 0.041(8) 0.021(12) O12 0.067(10) 0.083(11) 0.14(3) -0.008(11) 0.039(13) 0.020(8) Cl1' 0.07(2) 0.09(6) 0.10(3) 0.01(3) 0.04(2) 0.03(3) O9' 0.10(3) 0.11(5) 0.12(4) 0.00(4) 0.06(3) 0.04(4) O10' 0.09(5) 0.10(4) 0.12(6) 0.03(4) 0.01(5) 0.03(4) O11' 0.07(3) 0.08(6) 0.08(4) 0.02(5) 0.04(3) 0.02(5) O12' 0.07(3) 0.11(4) 0.13(9) 0.02(4) 0.06(4) 0.02(3) _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 1.968(10) 3_566 ? Co1 N1 1.973(9) . ? Co1 N12 2.012(10) . ? Co1 N13 2.031(9) . ? Co1 N10 2.032(8) . ? Co1 N11 2.035(7) . ? Fe1 C1 1.854(11) . ? Fe1 C2 1.885(11) . ? Fe1 C3 1.905(14) . ? Fe1 N8 1.955(9) . ? Fe1 N6 1.983(8) . ? Fe1 N4 1.983(8) . ? B1 N7 1.521(15) . ? B1 N9 1.539(16) . ? B1 N5 1.550(16) . ? B1 H1 1.0001 . ? N1 C1 1.150(12) . ? N2 C2 1.144(13) . ? N2 Co1 1.968(10) 3_566 ? N3 C3 1.187(16) . ? N4 C4 1.328(13) . ? N4 N5 1.375(11) . ? N5 C6 1.332(14) . ? N6 C7 1.339(15) . ? N6 N7 1.362(12) . ? N7 C9 1.343(14) . ? N8 C10' 1.35(6) . ? N8 C10 1.35(8) . ? N8 N9 1.370(13) . ? N9 C12' 1.35(7) . ? N9 C12 1.36(8) . ? N10 C13 1.330(13) . ? N10 C17 1.340(13) . ? N11 C18 1.330(11) . ? N11 C22 1.358(13) . ? N12 C33 1.335(13) . ? N12 C29 1.344(14) . ? N13 C38 1.286(13) . ? N13 C34 1.375(13) . ? C4 C5 1.423(15) . ? C4 H4 0.9500 . ? C5 C6 1.367(16) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.379(18) . ? C7 H7 0.9500 . ? C8 C9 1.327(17) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.36(8) . ? C10 H10 0.9500 . ? C11 C12 1.40(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C10' C11' 1.37(7) . ? C10' H10' 0.9500 . ? C11' C12' 1.34(7) . ? C11' H11' 0.9500 . ? C12' H12' 0.9500 . ? C13 C14 1.381(17) . ? C13 H13 0.9500 . ? C14 C15 1.366(18) . ? C14 H14 0.9500 . ? C15 C16 1.401(16) . ? C15 C23 1.534(18) . ? C16 C17 1.402(15) . ? C16 H16 0.9500 . ? C17 C18 1.477(14) . ? C23 O1 1.208(16) . ? C23 O2 1.310(17) . ? O2 C24 1.490(16) . ? C24 C25 1.48(2) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C18 C19 1.356(13) . ? C19 C20 1.365(14) . ? C19 H19 0.9500 . ? C20 C21 1.420(15) . ? C20 C26 1.50(5) . ? C20 C26' 1.53(12) . ? C21 C22 1.340(15) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C26 O3 1.22(6) . ? C26 O4 1.29(6) . ? O4 C27 1.491(19) . ? C27 C28 1.54(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26' O3' 1.23(14) . ? C26' O4' 1.29(12) . ? O4' C27' 1.51(5) . ? C27' C28' 1.49(5) . ? C27' H27C 0.9900 . ? C27' H27D 0.9900 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29 C30 1.381(17) . ? C29 H29 0.9500 . ? C30 C31 1.365(17) . ? C30 H30 0.9500 . ? C31 C32 1.386(16) . ? C31 C39 1.50(17) . ? C31 C39' 1.5(2) . ? C32 C33 1.390(15) . ? C32 H32 0.9500 . ? C33 C34 1.500(15) . ? C39 O5 1.237(10) . ? C39 O6 1.289(11) . ? O6 C40 1.57(14) . ? C40 C41 1.55(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C39' O5' 1.232(10) . ? C39' O6' 1.287(11) . ? O6' C40' 1.57(18) . ? C40' C41' 1.55(7) . ? C40' H40C 0.9900 . ? C40' H40D 0.9900 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C34 C35 1.378(15) . ? C35 C36 1.396(18) . ? C35 H35 0.9500 . ? C36 C37 1.351(18) . ? C36 C42 1.499(19) . ? C37 C38 1.397(18) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C42 O7 1.211(17) . ? C42 O8 1.322(18) . ? O8 C43 1.522(19) . ? C43 C44 1.44(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Cl1 O12 1.41(6) . ? Cl1 O10 1.42(6) . ? Cl1 O9 1.43(6) . ? Cl1 O11 1.44(7) . ? Cl1' O10' 1.41(17) . ? Cl1' O11' 1.41(19) . ? Cl1' O9' 1.4(2) . ? Cl1' O12' 1.43(14) . ? 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 N1 93.3(3) 3_566 . ? N2 Co1 N12 93.2(4) 3_566 . ? N1 Co1 N12 86.6(3) . . ? N2 Co1 N13 173.8(4) 3_566 . ? N1 Co1 N13 88.7(3) . . ? N12 Co1 N13 81.1(4) . . ? N2 Co1 N10 90.2(3) 3_566 . ? N1 Co1 N10 171.1(4) . . ? N12 Co1 N10 101.3(3) . . ? N13 Co1 N10 88.7(3) . . ? N2 Co1 N11 85.7(3) 3_566 . ? N1 Co1 N11 92.4(3) . . ? N12 Co1 N11 178.4(3) . . ? N13 Co1 N11 100.1(3) . . ? N10 Co1 N11 79.8(3) . . ? C1 Fe1 C2 89.7(4) . . ? C1 Fe1 C3 85.4(5) . . ? C2 Fe1 C3 84.5(5) . . ? C1 Fe1 N8 178.6(4) . . ? C2 Fe1 N8 91.6(4) . . ? C3 Fe1 N8 95.3(5) . . ? C1 Fe1 N6 89.9(4) . . ? C2 Fe1 N6 179.0(4) . . ? C3 Fe1 N6 96.3(4) . . ? N8 Fe1 N6 88.8(4) . . ? C1 Fe1 N4 91.0(4) . . ? C2 Fe1 N4 91.6(4) . . ? C3 Fe1 N4 174.7(5) . . ? N8 Fe1 N4 88.4(4) . . ? N6 Fe1 N4 87.5(3) . . ? N7 B1 N9 107.2(10) . . ? N7 B1 N5 107.3(9) . . ? N9 B1 N5 108.3(9) . . ? N7 B1 H1 111.3 . . ? N9 B1 H1 111.4 . . ? N5 B1 H1 111.1 . . ? C1 N1 Co1 173.5(8) . . ? C2 N2 Co1 171.8(9) . 3_566 ? C4 N4 N5 108.4(8) . . ? C4 N4 Fe1 132.5(7) . . ? N5 N4 Fe1 119.1(7) . . ? C6 N5 N4 108.5(9) . . ? C6 N5 B1 133.3(9) . . ? N4 N5 B1 118.0(8) . . ? C7 N6 N7 105.9(9) . . ? C7 N6 Fe1 134.2(8) . . ? N7 N6 Fe1 119.7(6) . . ? C9 N7 N6 109.0(9) . . ? C9 N7 B1 132.4(9) . . ? N6 N7 B1 118.3(8) . . ? C10' N8 C10 32(3) . . ? C10' N8 N9 108(3) . . ? C10 N8 N9 98(3) . . ? C10' N8 Fe1 129(3) . . ? C10 N8 Fe1 138(4) . . ? N9 N8 Fe1 120.9(7) . . ? C12' N9 C12 32(3) . . ? C12' N9 N8 105(3) . . ? C12 N9 N8 117(4) . . ? C12' N9 B1 137(3) . . ? C12 N9 B1 122(4) . . ? N8 N9 B1 116.9(9) . . ? C13 N10 C17 121.0(10) . . ? C13 N10 Co1 125.4(8) . . ? C17 N10 Co1 113.6(7) . . ? C18 N11 C22 119.4(8) . . ? C18 N11 Co1 114.0(6) . . ? C22 N11 Co1 125.5(7) . . ? C33 N12 C29 117.4(10) . . ? C33 N12 Co1 115.2(7) . . ? C29 N12 Co1 125.6(8) . . ? C38 N13 C34 118.7(10) . . ? C38 N13 Co1 127.3(9) . . ? C34 N13 Co1 113.7(7) . . ? N1 C1 Fe1 175.3(9) . . ? N2 C2 Fe1 177.7(10) . . ? N3 C3 Fe1 177.8(14) . . ? N4 C4 C5 108.0(10) . . ? N4 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? C6 C5 C4 105.3(10) . . ? C6 C5 H5 127.4 . . ? C4 C5 H5 127.4 . . ? N5 C6 C5 109.7(10) . . ? N5 C6 H6 125.2 . . ? C5 C6 H6 125.2 . . ? N6 C7 C8 109.5(12) . . ? N6 C7 H7 125.3 . . ? C8 C7 H7 125.3 . . ? C9 C8 C7 106.5(11) . . ? C9 C8 H8 126.7 . . ? C7 C8 H8 126.7 . . ? C8 C9 N7 108.9(11) . . ? C8 C9 H9 125.6 . . ? N7 C9 H9 125.6 . . ? N8 C10 C11 118(6) . . ? N8 C10 H10 120.9 . . ? C11 C10 H10 120.9 . . ? C10 C11 C12 103(5) . . ? C10 C11 H11 128.4 . . ? C12 C11 H11 128.4 . . ? N9 C12 C11 104(6) . . ? N9 C12 H12 127.9 . . ? C11 C12 H12 127.9 . . ? N8 C10' C11' 109(4) . . ? N8 C10' H10' 125.5 . . ? C11' C10' H10' 125.5 . . ? C12' C11' C10' 105(4) . . ? C12' C11' H11' 127.5 . . ? C10' C11' H11' 127.5 . . ? C11' C12' N9 112(5) . . ? C11' C12' H12' 123.8 . . ? N9 C12' H12' 123.8 . . ? N10 C13 C14 120.3(12) . . ? N10 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 120.5(13) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.2(12) . . ? C14 C15 C23 121.7(12) . . ? C16 C15 C23 119.1(13) . . ? C15 C16 C17 117.6(11) . . ? C15 C16 H16 121.2 . . ? C17 C16 H16 121.2 . . ? N10 C17 C16 121.2(9) . . ? N10 C17 C18 115.9(9) . . ? C16 C17 C18 122.9(10) . . ? O1 C23 O2 128.6(15) . . ? O1 C23 C15 118.1(15) . . ? O2 C23 C15 113.2(13) . . ? C23 O2 C24 114.5(12) . . ? C25 C24 O2 110.3(13) . . ? C25 C24 H24A 109.6 . . ? O2 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? O2 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N11 C18 C19 121.4(9) . . ? N11 C18 C17 113.8(8) . . ? C19 C18 C17 124.7(9) . . ? C18 C19 C20 121.5(10) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C19 C20 C21 115.7(10) . . ? C19 C20 C26 126(2) . . ? C21 C20 C26 118(2) . . ? C19 C20 C26' 118(5) . . ? C21 C20 C26' 123(5) . . ? C26 C20 C26' 23(3) . . ? C22 C21 C20 121.1(11) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 N11 120.4(10) . . ? C21 C22 H22 119.8 . . ? N11 C22 H22 119.8 . . ? O3 C26 O4 127(4) . . ? O3 C26 C20 123(4) . . ? O4 C26 C20 108(4) . . ? C26 O4 C27 113(3) . . ? O4 C27 C28 114.2(15) . . ? O4 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? O4 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3' C26' O4' 122(10) . . ? O3' C26' C20 116(10) . . ? O4' C26' C20 122(10) . . ? C26' O4' C27' 126(6) . . ? C28' C27' O4' 114(3) . . ? C28' C27' H27C 108.7 . . ? O4' C27' H27C 108.7 . . ? C28' C27' H27D 108.7 . . ? O4' C27' H27D 108.7 . . ? H27C C27' H27D 107.6 . . ? C27' C28' H28D 109.5 . . ? C27' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? N12 C29 C30 121.8(11) . . ? N12 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 120.1(11) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 119.3(11) . . ? C30 C31 C39 117(4) . . ? C32 C31 C39 123(3) . . ? C30 C31 C39' 126(4) . . ? C32 C31 C39' 115(4) . . ? C39 C31 C39' 12(10) . . ? C31 C32 C33 117.0(11) . . ? C31 C32 H32 121.5 . . ? C33 C32 H32 121.5 . . ? N12 C33 C32 124.3(10) . . ? N12 C33 C34 114.8(9) . . ? C32 C33 C34 120.7(10) . . ? O5 C39 O6 124(10) . . ? O5 C39 C31 115(9) . . ? O6 C39 C31 119(10) . . ? C39 O6 C40 115(10) . . ? C41 C40 O6 100(5) . . ? C41 C40 H40A 111.7 . . ? O6 C40 H40A 111.7 . . ? C41 C40 H40B 111.7 . . ? O6 C40 H40B 111.7 . . ? H40A C40 H40B 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O5' C39' O6' 131(10) . . ? O5' C39' C31 117(10) . . ? O6' C39' C31 110(10) . . ? C39' O6' C40' 97(10) . . ? C41' C40' O6' 115(6) . . ? C41' C40' H40C 108.5 . . ? O6' C40' H40C 108.5 . . ? C41' C40' H40D 108.5 . . ? O6' C40' H40D 108.5 . . ? H40C C40' H40D 107.5 . . ? C40' C41' H41D 109.5 . . ? C40' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C40' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? N13 C34 C35 121.5(10) . . ? N13 C34 C33 114.3(9) . . ? C35 C34 C33 124.3(10) . . ? C34 C35 C36 117.5(12) . . ? C34 C35 H35 121.2 . . ? C36 C35 H35 121.2 . . ? C37 C36 C35 120.6(13) . . ? C37 C36 C42 118.1(15) . . ? C35 C36 C42 121.3(15) . . ? C36 C37 C38 117.9(12) . . ? C36 C37 H37 121.0 . . ? C38 C37 H37 121.0 . . ? N13 C38 C37 123.6(13) . . ? N13 C38 H38 118.2 . . ? C37 C38 H38 118.2 . . ? O7 C42 O8 123.3(14) . . ? O7 C42 C36 123.0(18) . . ? O8 C42 C36 113.7(14) . . ? C42 O8 C43 117.1(15) . . ? C44 C43 O8 101.6(19) . . ? C44 C43 H43A 111.4 . . ? O8 C43 H43A 111.4 . . ? C44 C43 H43B 111.4 . . ? O8 C43 H43B 111.4 . . ? H43A C43 H43B 109.3 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O12 Cl1 O10 105(4) . . ? O12 Cl1 O9 107(2) . . ? O10 Cl1 O9 114(5) . . ? O12 Cl1 O11 107(4) . . ? O10 Cl1 O11 111(3) . . ? O9 Cl1 O11 112(4) . . ? O10' Cl1' O11' 127(10) . . ? O10' Cl1' O9' 106(10) . . ? O11' Cl1' O9' 95(10) . . ? O10' Cl1' O12' 118(10) . . ? O11' Cl1' O12' 107(10) . . ? O9' Cl1' O12' 95(10) . . ? 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 N1 C1 -124(7) 3_566 . . . ? N12 Co1 N1 C1 -31(7) . . . . ? N13 Co1 N1 C1 50(7) . . . . ? N10 Co1 N1 C1 123(7) . . . . ? N11 Co1 N1 C1 150(7) . . . . ? C1 Fe1 N4 C4 44.6(10) . . . . ? C2 Fe1 N4 C4 -45.1(10) . . . . ? C3 Fe1 N4 C4 -2(5) . . . . ? N8 Fe1 N4 C4 -136.6(10) . . . . ? N6 Fe1 N4 C4 134.5(10) . . . . ? C1 Fe1 N4 N5 -136.8(7) . . . . ? C2 Fe1 N4 N5 133.4(7) . . . . ? C3 Fe1 N4 N5 176(5) . . . . ? N8 Fe1 N4 N5 41.9(7) . . . . ? N6 Fe1 N4 N5 -47.0(7) . . . . ? C4 N4 N5 C6 -2.4(11) . . . . ? Fe1 N4 N5 C6 178.8(7) . . . . ? C4 N4 N5 B1 -177.0(9) . . . . ? Fe1 N4 N5 B1 4.1(11) . . . . ? N7 B1 N5 C6 -117.4(12) . . . . ? N9 B1 N5 C6 127.2(12) . . . . ? N7 B1 N5 N4 55.7(11) . . . . ? N9 B1 N5 N4 -59.8(12) . . . . ? C1 Fe1 N6 C7 -39.3(12) . . . . ? C2 Fe1 N6 C7 -102(24) . . . . ? C3 Fe1 N6 C7 46.1(12) . . . . ? N8 Fe1 N6 C7 141.3(12) . . . . ? N4 Fe1 N6 C7 -130.3(12) . . . . ? C1 Fe1 N6 N7 135.5(8) . . . . ? C2 Fe1 N6 N7 73(24) . . . . ? C3 Fe1 N6 N7 -139.1(8) . . . . ? N8 Fe1 N6 N7 -43.9(8) . . . . ? N4 Fe1 N6 N7 44.5(8) . . . . ? C7 N6 N7 C9 3.7(13) . . . . ? Fe1 N6 N7 C9 -172.5(7) . . . . ? C7 N6 N7 B1 177.9(10) . . . . ? Fe1 N6 N7 B1 1.8(13) . . . . ? N9 B1 N7 C9 -130.4(12) . . . . ? N5 B1 N7 C9 113.5(13) . . . . ? N9 B1 N7 N6 57.0(13) . . . . ? N5 B1 N7 N6 -59.2(12) . . . . ? C1 Fe1 N8 C10' -146(19) . . . . ? C2 Fe1 N8 C10' 57(4) . . . . ? C3 Fe1 N8 C10' -27(4) . . . . ? N6 Fe1 N8 C10' -123(4) . . . . ? N4 Fe1 N8 C10' 149(4) . . . . ? C1 Fe1 N8 C10 171(100) . . . . ? C2 Fe1 N8 C10 15(6) . . . . ? C3 Fe1 N8 C10 -70(6) . . . . ? N6 Fe1 N8 C10 -166(6) . . . . ? N4 Fe1 N8 C10 106(6) . . . . ? C1 Fe1 N8 N9 16(20) . . . . ? C2 Fe1 N8 N9 -140.0(10) . . . . ? C3 Fe1 N8 N9 135.4(10) . . . . ? N6 Fe1 N8 N9 39.1(10) . . . . ? N4 Fe1 N8 N9 -48.4(10) . . . . ? C10' N8 N9 C12' 0(4) . . . . ? C10 N8 N9 C12' 31(4) . . . . ? Fe1 N8 N9 C12' -165(4) . . . . ? C10' N8 N9 C12 -31(4) . . . . ? C10 N8 N9 C12 0(5) . . . . ? Fe1 N8 N9 C12 163(5) . . . . ? C10' N8 N9 B1 173(3) . . . . ? C10 N8 N9 B1 -156(4) . . . . ? Fe1 N8 N9 B1 6.8(15) . . . . ? N7 B1 N9 C12' 107(5) . . . . ? N5 B1 N9 C12' -138(5) . . . . ? N7 B1 N9 C12 143(5) . . . . ? N5 B1 N9 C12 -102(5) . . . . ? N7 B1 N9 N8 -62.1(14) . . . . ? N5 B1 N9 N8 53.4(14) . . . . ? N2 Co1 N10 C13 102.2(9) 3_566 . . . ? N1 Co1 N10 C13 -144.2(19) . . . . ? N12 Co1 N10 C13 8.9(9) . . . . ? N13 Co1 N10 C13 -71.8(9) . . . . ? N11 Co1 N10 C13 -172.3(9) . . . . ? N2 Co1 N10 C17 -76.3(7) 3_566 . . . ? N1 Co1 N10 C17 37(2) . . . . ? N12 Co1 N10 C17 -169.6(7) . . . . ? N13 Co1 N10 C17 109.8(7) . . . . ? N11 Co1 N10 C17 9.3(7) . . . . ? N2 Co1 N11 C18 75.7(7) 3_566 . . . ? N1 Co1 N11 C18 168.9(7) . . . . ? N12 Co1 N11 C18 119(11) . . . . ? N13 Co1 N11 C18 -102.0(7) . . . . ? N10 Co1 N11 C18 -15.3(6) . . . . ? N2 Co1 N11 C22 -92.4(8) 3_566 . . . ? N1 Co1 N11 C22 0.8(8) . . . . ? N12 Co1 N11 C22 -49(12) . . . . ? N13 Co1 N11 C22 89.9(8) . . . . ? N10 Co1 N11 C22 176.6(8) . . . . ? N2 Co1 N12 C33 173.5(7) 3_566 . . . ? N1 Co1 N12 C33 80.4(7) . . . . ? N13 Co1 N12 C33 -8.8(7) . . . . ? N10 Co1 N12 C33 -95.6(7) . . . . ? N11 Co1 N12 C33 131(11) . . . . ? N2 Co1 N12 C29 9.5(9) 3_566 . . . ? N1 Co1 N12 C29 -83.7(8) . . . . ? N13 Co1 N12 C29 -172.9(9) . . . . ? N10 Co1 N12 C29 100.3(8) . . . . ? N11 Co1 N12 C29 -33(12) . . . . ? N2 Co1 N13 C38 -159(3) 3_566 . . . ? N1 Co1 N13 C38 91.7(9) . . . . ? N12 Co1 N13 C38 178.5(10) . . . . ? N10 Co1 N13 C38 -79.9(9) . . . . ? N11 Co1 N13 C38 -0.5(10) . . . . ? N2 Co1 N13 C34 27(4) 3_566 . . . ? N1 Co1 N13 C34 -81.8(7) . . . . ? N12 Co1 N13 C34 5.1(7) . . . . ? N10 Co1 N13 C34 106.7(7) . . . . ? N11 Co1 N13 C34 -173.9(7) . . . . ? Co1 N1 C1 Fe1 -133(8) . . . . ? C2 Fe1 C1 N1 -100(10) . . . . ? C3 Fe1 C1 N1 -16(10) . . . . ? N8 Fe1 C1 N1 103(21) . . . . ? N6 Fe1 C1 N1 81(10) . . . . ? N4 Fe1 C1 N1 168(10) . . . . ? Co1 N2 C2 Fe1 -104(24) 3_566 . . . ? C1 Fe1 C2 N2 72(23) . . . . ? C3 Fe1 C2 N2 -13(23) . . . . ? N8 Fe1 C2 N2 -108(23) . . . . ? N6 Fe1 C2 N2 135(27) . . . . ? N4 Fe1 C2 N2 163(23) . . . . ? C1 Fe1 C3 N3 27(33) . . . . ? C2 Fe1 C3 N3 117(33) . . . . ? N8 Fe1 C3 N3 -152(33) . . . . ? N6 Fe1 C3 N3 -62(33) . . . . ? N4 Fe1 C3 N3 75(35) . . . . ? N5 N4 C4 C5 3.9(12) . . . . ? Fe1 N4 C4 C5 -177.4(7) . . . . ? N4 C4 C5 C6 -4.0(13) . . . . ? N4 N5 C6 C5 -0.3(13) . . . . ? B1 N5 C6 C5 173.2(11) . . . . ? C4 C5 C6 N5 2.6(13) . . . . ? N7 N6 C7 C8 -1.0(15) . . . . ? Fe1 N6 C7 C8 174.3(9) . . . . ? N6 C7 C8 C9 -2.0(17) . . . . ? C7 C8 C9 N7 4.3(17) . . . . ? N6 N7 C9 C8 -5.0(14) . . . . ? B1 N7 C9 C8 -178.2(13) . . . . ? C10' N8 C10 C11 113(14) . . . . ? N9 N8 C10 C11 0(6) . . . . ? Fe1 N8 C10 C11 -158(4) . . . . ? N8 C10 C11 C12 0(8) . . . . ? C12' N9 C12 C11 -74(11) . . . . ? N8 N9 C12 C11 0(6) . . . . ? B1 N9 C12 C11 155(3) . . . . ? C10 C11 C12 N9 0(7) . . . . ? C10 N8 C10' C11' -74(10) . . . . ? N9 N8 C10' C11' 0(5) . . . . ? Fe1 N8 C10' C11' 164(3) . . . . ? N8 C10' C11' C12' 0(6) . . . . ? C10' C11' C12' N9 0(7) . . . . ? C12 N9 C12' C11' 117(16) . . . . ? N8 N9 C12' C11' 0(6) . . . . ? B1 N9 C12' C11' -170(3) . . . . ? C17 N10 C13 C14 -1.2(17) . . . . ? Co1 N10 C13 C14 -179.6(9) . . . . ? N10 C13 C14 C15 4(2) . . . . ? C13 C14 C15 C16 -6(2) . . . . ? C13 C14 C15 C23 176.1(12) . . . . ? C14 C15 C16 C17 4.4(17) . . . . ? C23 C15 C16 C17 -177.2(10) . . . . ? C13 N10 C17 C16 0.2(15) . . . . ? Co1 N10 C17 C16 178.7(8) . . . . ? C13 N10 C17 C18 178.9(9) . . . . ? Co1 N10 C17 C18 -2.6(11) . . . . ? C15 C16 C17 N10 -1.7(15) . . . . ? C15 C16 C17 C18 179.6(10) . . . . ? C14 C15 C23 O1 -4.9(19) . . . . ? C16 C15 C23 O1 176.7(11) . . . . ? C14 C15 C23 O2 178.3(12) . . . . ? C16 C15 C23 O2 0.0(16) . . . . ? O1 C23 O2 C24 -3(2) . . . . ? C15 C23 O2 C24 173.1(11) . . . . ? C23 O2 C24 C25 89.3(16) . . . . ? C22 N11 C18 C19 4.9(14) . . . . ? Co1 N11 C18 C19 -163.9(8) . . . . ? C22 N11 C18 C17 -173.1(9) . . . . ? Co1 N11 C18 C17 18.0(10) . . . . ? N10 C17 C18 N11 -10.3(13) . . . . ? C16 C17 C18 N11 168.4(9) . . . . ? N10 C17 C18 C19 171.7(10) . . . . ? C16 C17 C18 C19 -9.6(16) . . . . ? N11 C18 C19 C20 -0.7(16) . . . . ? C17 C18 C19 C20 177.1(10) . . . . ? C18 C19 C20 C21 -0.8(16) . . . . ? C18 C19 C20 C26 -172.9(18) . . . . ? C18 C19 C20 C26' 161(4) . . . . ? C19 C20 C21 C22 -1.9(17) . . . . ? C26 C20 C21 C22 170.8(18) . . . . ? C26' C20 C21 C22 -162(4) . . . . ? C20 C21 C22 N11 6.2(17) . . . . ? C18 N11 C22 C21 -7.7(15) . . . . ? Co1 N11 C22 C21 159.9(8) . . . . ? C19 C20 C26 O3 -178(2) . . . . ? C21 C20 C26 O3 10(4) . . . . ? C26' C20 C26 O3 -99(17) . . . . ? C19 C20 C26 O4 -10(3) . . . . ? C21 C20 C26 O4 178.0(17) . . . . ? C26' C20 C26 O4 69(17) . . . . ? O3 C26 O4 C27 -6(5) . . . . ? C20 C26 O4 C27 -174.0(16) . . . . ? C26 O4 C27 C28 -79(2) . . . . ? C19 C20 C26' O3' -178(5) . . . . ? C21 C20 C26' O3' -18(8) . . . . ? C26 C20 C26' O3' 68(15) . . . . ? C19 C20 C26' O4' -5(8) . . . . ? C21 C20 C26' O4' 155(6) . . . . ? C26 C20 C26' O4' -120(22) . . . . ? O3' C26' O4' C27' -17(12) . . . . ? C20 C26' O4' C27' 171(4) . . . . ? C26' O4' C27' C28' 74(7) . . . . ? C33 N12 C29 C30 -0.7(16) . . . . ? Co1 N12 C29 C30 163.0(9) . . . . ? N12 C29 C30 C31 1.2(18) . . . . ? C29 C30 C31 C32 -2(2) . . . . ? C29 C30 C31 C39 -174(9) . . . . ? C29 C30 C31 C39' 176(10) . . . . ? C30 C31 C32 C33 3.1(18) . . . . ? C39 C31 C32 C33 174(9) . . . . ? C39' C31 C32 C33 -176(9) . . . . ? C29 N12 C33 C32 1.6(16) . . . . ? Co1 N12 C33 C32 -163.9(9) . . . . ? C29 N12 C33 C34 176.1(9) . . . . ? Co1 N12 C33 C34 10.6(11) . . . . ? C31 C32 C33 N12 -2.7(17) . . . . ? C31 C32 C33 C34 -176.9(10) . . . . ? C30 C31 C39 O5 173(11) . . . . ? C32 C31 C39 O5 1(20) . . . . ? C39' C31 C39 O5 -50(38) . . . . ? C30 C31 C39 O6 -19(16) . . . . ? C32 C31 C39 O6 169(7) . . . . ? C39' C31 C39 O6 119(59) . . . . ? O5 C39 O6 C40 -23(18) . . . . ? C31 C39 O6 C40 170(14) . . . . ? C39 O6 C40 C41 178(8) . . . . ? C30 C31 C39' O5' -170(9) . . . . ? C32 C31 C39' O5' 9(18) . . . . ? C39 C31 C39' O5' 143(62) . . . . ? C30 C31 C39' O6' 25(15) . . . . ? C32 C31 C39' O6' -156(7) . . . . ? C39 C31 C39' O6' -22(41) . . . . ? O5' C39' O6' C40' -5(17) . . . . ? C31 C39' O6' C40' 157(13) . . . . ? C39' O6' C40' C41' -109(9) . . . . ? C38 N13 C34 C35 6.0(15) . . . . ? Co1 N13 C34 C35 180.0(8) . . . . ? C38 N13 C34 C33 -175.0(10) . . . . ? Co1 N13 C34 C33 -1.0(11) . . . . ? N12 C33 C34 N13 -6.3(13) . . . . ? C32 C33 C34 N13 168.4(10) . . . . ? N12 C33 C34 C35 172.6(10) . . . . ? C32 C33 C34 C35 -12.6(16) . . . . ? N13 C34 C35 C36 -4.0(16) . . . . ? C33 C34 C35 C36 177.1(10) . . . . ? C34 C35 C36 C37 0.1(17) . . . . ? C34 C35 C36 C42 -179.0(10) . . . . ? C35 C36 C37 C38 1.8(18) . . . . ? C42 C36 C37 C38 -179.1(11) . . . . ? C34 N13 C38 C37 -4.0(17) . . . . ? Co1 N13 C38 C37 -177.1(9) . . . . ? C36 C37 C38 N13 0.2(18) . . . . ? C37 C36 C42 O7 -9.7(19) . . . . ? C35 C36 C42 O7 169.4(11) . . . . ? C37 C36 C42 O8 168.9(11) . . . . ? C35 C36 C42 O8 -12.0(17) . . . . ? O7 C42 O8 C43 -1(2) . . . . ? C36 C42 O8 C43 -179.2(14) . . . . ? C42 O8 C43 C44 89(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.122 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.188 # start Validation Reply Form _vrf_RFACR01_1100K ; PROBLEM: The value of the weighted R factor is > 0.35 RESPONSE: Due to the poor diffraction data. ; _vrf_PLAT084_1100K ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.38 RESPONSE: Due to the poor diffraction data. ; _vrf_PLAT220_1100K ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.0 Ratio RESPONSE: Due to the disordered terminal ethyl groups. ; _vrf_PLAT341_1100K ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0198 Ang. RESPONSE: Due to the poor diffraction data. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 967844' ####################################################################### # # 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_1(273K) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H84 B2 Cl2 Co2 Fe2 N26 O24' _chemical_formula_weight 2211.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.331(4) _cell_length_b 18.336(4) _cell_length_c 20.417(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.639(13) _cell_angle_gamma 90.00 _cell_volume 5090.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9113 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.95 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7828 _exptl_absorpt_correction_T_max 0.9435 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25948 _diffrn_reflns_av_R_equivalents 0.1150 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8810 _reflns_number_gt 4192 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The disordered pyrazol ring of the Tp ligand (N6, N7, C7(C7'), C8(C8'), C9(C9')), ethoxycarbonly group (C26(C26'), O3(O3'), O4(O4'), C27(C27'), C28(C28')) and the ClO4 anion were treated with a two-site model with refined variable site occupancy factors. The distances for the disordered atoms of C26, C26', O3, O3', O4, O4' were restrained using DFIX commands. 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^)+(0.2000P)^2^+0.0000P] 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 8810 _refine_ls_number_parameters 778 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2723 _refine_ls_R_factor_gt 0.1634 _refine_ls_wR_factor_ref 0.4416 _refine_ls_wR_factor_gt 0.3821 _refine_ls_goodness_of_fit_ref 1.359 _refine_ls_restrained_S_all 1.359 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25543(12) 0.51421(10) 0.62841(9) 0.0469(6) Uani 1 1 d . . . Fe1 Fe -0.01975(13) 0.45645(10) 0.66812(10) 0.0466(6) Uani 1 1 d . A . C1 C 0.0890(8) 0.4812(7) 0.6614(6) 0.044(3) Uani 1 1 d . . . N1 N 0.1526(8) 0.4931(6) 0.6537(6) 0.054(3) Uani 1 1 d . . . C2 C -0.1051(8) 0.4710(6) 0.5559(6) 0.038(3) Uani 1 1 d . . . N2 N -0.1535(7) 0.4786(5) 0.4915(5) 0.044(2) Uani 1 1 d . . . C3 C -0.0303(14) 0.5607(11) 0.6739(11) 0.084(5) Uani 1 1 d . . . N3 N -0.0447(15) 0.6231(11) 0.6735(12) 0.122(6) Uani 1 1 d . . . B1 B -0.0357(12) 0.3333(11) 0.7625(10) 0.067(5) Uani 1 1 d . . . H1 H -0.0386 0.2945 0.7942 0.080 Uiso 1 1 d R . . N4 N -0.0054(6) 0.3508(5) 0.6560(5) 0.039(2) Uani 1 1 d . . . N5 N -0.0135(8) 0.3018(6) 0.7022(6) 0.055(3) Uani 1 1 d . . . N6 N 0.0687(8) 0.4415(7) 0.7826(5) 0.060(3) Uani 1 1 d . . . N7 N 0.0470(9) 0.3879(8) 0.8148(7) 0.077(4) Uani 1 1 d . A . N8 N -0.1346(7) 0.4325(5) 0.6738(6) 0.045(2) Uani 1 1 d . . . N9 N -0.1311(8) 0.3735(6) 0.7157(6) 0.059(3) Uani 1 1 d . A . N10 N 0.3646(6) 0.5505(5) 0.6088(6) 0.041(2) Uani 1 1 d . . . N11 N 0.2438(7) 0.6287(6) 0.6306(5) 0.051(3) Uani 1 1 d . B . N12 N 0.2693(6) 0.3999(5) 0.6260(5) 0.033(2) Uani 1 1 d . . . N13 N 0.3693(7) 0.4887(6) 0.7458(5) 0.047(3) Uani 1 1 d . . . C4 C 0.0094(11) 0.3128(9) 0.6084(9) 0.069(4) Uani 1 1 d . . . H4 H 0.0170 0.3330 0.5703 0.083 Uiso 1 1 calc R . . C5 C 0.0121(12) 0.2404(9) 0.6229(10) 0.077(5) Uani 1 1 d . . . H5 H 0.0205 0.2024 0.5969 0.092 Uiso 1 1 calc R . . C6 C -0.0001(11) 0.2353(9) 0.6834(10) 0.073(4) Uani 1 1 d . . . H6 H 0.0007 0.1923 0.7078 0.088 Uiso 1 1 calc R . . C7 C 0.134(6) 0.488(5) 0.838(5) 0.073(16) Uani 0.52(10) 1 d P A 1 H7 H 0.1600 0.5298 0.8299 0.087 Uiso 0.52(10) 1 calc PR A 1 C8 C 0.155(4) 0.464(4) 0.906(2) 0.079(19) Uani 0.52(10) 1 d P A 1 H8 H 0.1980 0.4862 0.9545 0.095 Uiso 0.52(10) 1 calc PR A 1 C9 C 0.107(6) 0.408(5) 0.895(4) 0.080(17) Uani 0.52(10) 1 d P A 1 H9 H 0.1100 0.3817 0.9357 0.096 Uiso 0.52(10) 1 calc PR A 1 C7' C 0.159(7) 0.459(5) 0.842(5) 0.080(19) Uani 0.48(10) 1 d P A 2 H7' H 0.1962 0.4948 0.8379 0.096 Uiso 0.48(10) 1 calc PR A 2 C8' C 0.193(5) 0.420(4) 0.909(2) 0.08(2) Uani 0.48(10) 1 d P A 2 H8' H 0.2531 0.4236 0.9566 0.098 Uiso 0.48(10) 1 calc PR A 2 C9' C 0.119(7) 0.374(6) 0.890(5) 0.081(18) Uani 0.48(10) 1 d P A 2 H9' H 0.1174 0.3394 0.9231 0.097 Uiso 0.48(10) 1 calc PR A 2 C10 C -0.2296(12) 0.4531(9) 0.6322(10) 0.074(4) Uani 1 1 d . A . H10 H -0.2549 0.4903 0.5950 0.088 Uiso 1 1 calc R . . C11 C -0.2831(13) 0.4139(10) 0.6505(11) 0.079(5) Uani 1 1 d . . . H11 H -0.3496 0.4198 0.6305 0.095 Uiso 1 1 calc R A . C12 C -0.2201(11) 0.3629(9) 0.7050(10) 0.071(4) Uani 1 1 d . A . H12 H -0.2356 0.3280 0.7297 0.085 Uiso 1 1 calc R . . C13 C 0.4201(10) 0.5103(8) 0.5977(7) 0.053(3) Uani 1 1 d . . . H13 H 0.4146 0.4600 0.6003 0.063 Uiso 1 1 calc R . . C14 C 0.4870(10) 0.5353(8) 0.5823(8) 0.059(4) Uani 1 1 d . . . H14 H 0.5252 0.5037 0.5743 0.071 Uiso 1 1 calc R . . C15 C 0.4944(11) 0.6114(9) 0.5792(7) 0.064(4) Uani 1 1 d . . . C16 C 0.4333(10) 0.6563(7) 0.5888(7) 0.050(3) Uani 1 1 d . . . H16 H 0.4366 0.7068 0.5859 0.061 Uiso 1 1 calc R . . C17 C 0.3686(8) 0.6251(6) 0.6024(6) 0.041(3) Uani 1 1 d . . . C18 C 0.2954(8) 0.6672(6) 0.6110(6) 0.038(3) Uani 1 1 d . . . C19 C 0.2795(10) 0.7399(8) 0.5928(8) 0.061(4) Uani 1 1 d . B . H19 H 0.3164 0.7639 0.5774 0.073 Uiso 1 1 calc R . . C20 C 0.2095(13) 0.7783(8) 0.5969(10) 0.071(4) Uani 1 1 d . . . C21 C 0.1546(12) 0.7376(8) 0.6173(9) 0.067(4) Uani 1 1 d . B . H21 H 0.1046 0.7601 0.6189 0.081 Uiso 1 1 calc R . . C22 C 0.1733(10) 0.6650(8) 0.6351(8) 0.061(4) Uani 1 1 d . . . H22 H 0.1375 0.6396 0.6506 0.073 Uiso 1 1 calc R B . C23 C 0.5710(11) 0.6436(11) 0.5671(9) 0.073(5) Uani 1 1 d . . . C24 C 0.6574(17) 0.7423(15) 0.5639(18) 0.137(9) Uani 1 1 d . . . H24A H 0.6608 0.7136 0.5256 0.164 Uiso 1 1 calc R . . H24B H 0.6415 0.7924 0.5456 0.164 Uiso 1 1 calc R . . C25 C 0.751(2) 0.738(2) 0.643(2) 0.24(2) Uani 1 1 d . . . H25A H 0.7751 0.7865 0.6617 0.362 Uiso 1 1 calc R . . H25B H 0.7990 0.7116 0.6389 0.362 Uiso 1 1 calc R . . H25C H 0.7399 0.7136 0.6787 0.362 Uiso 1 1 calc R . . C26 C 0.174(19) 0.853(14) 0.573(15) 0.12(4) Uani 0.47(3) 1 d PD B 1 O3 O 0.121(12) 0.881(8) 0.591(6) 0.12(3) Uani 0.47(3) 1 d PD B 1 O4 O 0.211(7) 0.883(8) 0.538(9) 0.12(3) Uani 0.47(3) 1 d PD B 1 C27 C 0.154(4) 0.949(2) 0.492(4) 0.13(2) Uani 0.47(3) 1 d P B 1 H27A H 0.1345 0.9737 0.5237 0.161 Uiso 0.47(3) 1 calc PR B 1 H27B H 0.2001 0.9812 0.4908 0.161 Uiso 0.47(3) 1 calc PR B 1 C28 C 0.064(5) 0.946(3) 0.410(4) 0.14(2) Uani 0.47(3) 1 d P B 1 H28A H 0.0764 0.9715 0.3752 0.217 Uiso 0.47(3) 1 calc PR B 1 H28B H 0.0098 0.9687 0.4083 0.217 Uiso 0.47(3) 1 calc PR B 1 H28C H 0.0480 0.8962 0.3935 0.217 Uiso 0.47(3) 1 calc PR B 1 C26' C 0.197(11) 0.858(12) 0.574(13) 0.12(5) Uani 0.53(3) 1 d PD B 2 O3' O 0.256(5) 0.888(7) 0.565(7) 0.12(3) Uani 0.53(3) 1 d PD B 2 O4' O 0.115(10) 0.884(7) 0.559(6) 0.12(2) Uani 0.53(3) 1 d PD B 2 C27' C 0.083(4) 0.962(2) 0.536(4) 0.131(19) Uani 0.53(3) 1 d P B 2 H27C H 0.0534 0.9808 0.5634 0.157 Uiso 0.53(3) 1 calc PR B 2 H27D H 0.1368 0.9929 0.5475 0.157 Uiso 0.53(3) 1 calc PR B 2 C28' C 0.008(4) 0.955(2) 0.450(4) 0.14(2) Uani 0.53(3) 1 d P B 2 H28D H -0.0562 0.9473 0.4402 0.217 Uiso 0.53(3) 1 calc PR B 2 H28E H 0.0242 0.9138 0.4297 0.217 Uiso 0.53(3) 1 calc PR B 2 H28F H 0.0074 0.9983 0.4236 0.217 Uiso 0.53(3) 1 calc PR B 2 C29 C 0.2161(11) 0.3563(8) 0.5614(8) 0.065(4) Uani 1 1 d . . . H29 H 0.1848 0.3782 0.5121 0.078 Uiso 1 1 calc R . . C30 C 0.2062(12) 0.2845(8) 0.5643(9) 0.070(4) Uani 1 1 d . . . H30 H 0.1672 0.2573 0.5186 0.085 Uiso 1 1 calc R . . C31 C 0.2562(9) 0.2512(8) 0.6383(7) 0.061(4) Uani 1 1 d . . . C32 C 0.3127(10) 0.2927(7) 0.7016(7) 0.053(3) Uani 1 1 d . . . H32 H 0.3481 0.2712 0.7511 0.063 Uiso 1 1 calc R . . C33 C 0.3196(8) 0.3651(7) 0.6952(6) 0.048(3) Uani 1 1 d . . . C34 C 0.3830(8) 0.4172(7) 0.7631(6) 0.045(3) Uani 1 1 d . . . C35 C 0.4495(10) 0.3904(8) 0.8372(8) 0.054(3) Uani 1 1 d . . . H35 H 0.4574 0.3404 0.8468 0.065 Uiso 1 1 calc R . . C36 C 0.5050(10) 0.4409(8) 0.8980(8) 0.060(4) Uani 1 1 d . . . C37 C 0.4927(11) 0.5139(9) 0.8791(8) 0.074(5) Uani 1 1 d . . . H37 H 0.5306 0.5485 0.9176 0.089 Uiso 1 1 calc R . . C38 C 0.4235(11) 0.5356(8) 0.8024(8) 0.067(4) Uani 1 1 d . . . H38 H 0.4154 0.5852 0.7906 0.080 Uiso 1 1 calc R . . C39 C 0.2424(12) 0.1704(8) 0.6393(9) 0.082(5) Uani 1 1 d . . . C40 C 0.2817(16) 0.0649(11) 0.7204(12) 0.105(6) Uani 1 1 d . . . H40A H 0.2156 0.0479 0.6818 0.126 Uiso 1 1 calc R . . H40B H 0.2955 0.0549 0.7723 0.126 Uiso 1 1 calc R . . C41 C 0.3563(18) 0.0230(13) 0.7099(14) 0.127(8) Uani 1 1 d . . . H41A H 0.4217 0.0395 0.7484 0.190 Uiso 1 1 calc R . . H41B H 0.3417 0.0320 0.6581 0.190 Uiso 1 1 calc R . . H41C H 0.3515 -0.0283 0.7165 0.190 Uiso 1 1 calc R . . C42 C 0.5791(12) 0.4186(11) 0.9815(9) 0.072(4) Uani 1 1 d . . . C43 C 0.6442(16) 0.3219(12) 1.0741(10) 0.109(7) Uani 1 1 d . . . H43A H 0.6436 0.3589 1.1078 0.131 Uiso 1 1 calc R . . H43B H 0.6162 0.2777 1.0800 0.131 Uiso 1 1 calc R . . C44 C 0.7443(16) 0.3080(14) 1.0993(12) 0.124(8) Uani 1 1 d . . . H44A H 0.7458 0.2690 1.0686 0.186 Uiso 1 1 calc R . . H44B H 0.7822 0.2945 1.1538 0.186 Uiso 1 1 calc R . . H44C H 0.7718 0.3512 1.0921 0.186 Uiso 1 1 calc R . . O1 O 0.6180(8) 0.6016(7) 0.5523(7) 0.091(4) Uani 1 1 d . . . O2 O 0.5841(8) 0.7114(7) 0.5782(7) 0.083(3) Uani 1 1 d . . . O5 O 0.2874(10) 0.1467(6) 0.7109(7) 0.098(4) Uani 1 1 d . . . O6 O 0.1898(9) 0.1334(6) 0.5809(7) 0.092(4) Uani 1 1 d . . . O7 O 0.5820(8) 0.3468(6) 0.9909(5) 0.080(3) Uani 1 1 d . . . O8 O 0.6235(8) 0.4632(7) 1.0343(6) 0.091(4) Uani 1 1 d . . . Cl1 Cl 0.531(5) 0.264(8) 0.692(5) 0.085(12) Uani 0.60(11) 1 d P C 1 O9 O 0.521(2) 0.263(4) 0.757(2) 0.11(2) Uani 0.60(11) 1 d P C 1 O10 O 0.508(6) 0.327(3) 0.636(3) 0.135(17) Uani 0.60(11) 1 d P C 1 O11 O 0.627(7) 0.237(3) 0.712(5) 0.090(17) Uani 0.60(11) 1 d P C 1 O12 O 0.460(3) 0.2133(19) 0.636(4) 0.122(18) Uani 0.60(11) 1 d P C 1 Cl1' Cl 0.533(10) 0.278(14) 0.692(9) 0.11(4) Uani 0.40(11) 1 d P C 2 O9' O 0.490(4) 0.212(3) 0.697(6) 0.12(3) Uani 0.40(11) 1 d P C 2 O10' O 0.543(5) 0.316(6) 0.753(4) 0.12(3) Uani 0.40(11) 1 d P C 2 O11' O 0.624(12) 0.268(6) 0.711(8) 0.11(3) Uani 0.40(11) 1 d P C 2 O12' O 0.458(7) 0.316(4) 0.638(4) 0.11(2) Uani 0.40(11) 1 d P C 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 0.0432(10) 0.0435(11) 0.0348(9) 0.0042(8) 0.0096(7) -0.0028(8) Fe1 0.0473(11) 0.0440(11) 0.0346(10) -0.0028(8) 0.0141(8) -0.0054(8) C1 0.032(6) 0.049(8) 0.027(6) 0.006(5) 0.001(5) -0.006(6) N1 0.038(6) 0.064(8) 0.036(6) 0.024(5) 0.005(5) -0.009(5) C2 0.036(6) 0.032(7) 0.022(6) 0.011(5) 0.001(5) 0.011(5) N2 0.037(5) 0.041(6) 0.021(5) 0.013(4) -0.004(4) 0.007(4) C3 0.108(14) 0.078(13) 0.114(15) -0.015(11) 0.090(13) -0.021(11) N3 0.152(17) 0.080(13) 0.159(18) -0.025(12) 0.101(15) -0.020(12) B1 0.049(10) 0.089(14) 0.069(11) 0.033(10) 0.037(9) 0.006(9) N4 0.034(5) 0.033(6) 0.039(5) 0.005(5) 0.013(4) 0.013(4) N5 0.048(6) 0.054(8) 0.058(7) 0.031(6) 0.026(6) 0.018(5) N6 0.064(7) 0.083(9) 0.013(5) -0.003(5) 0.008(5) -0.022(6) N7 0.070(8) 0.112(12) 0.039(7) 0.007(7) 0.023(7) -0.006(8) N8 0.042(6) 0.040(6) 0.057(6) 0.009(5) 0.029(5) 0.003(5) N9 0.061(7) 0.046(7) 0.054(7) 0.005(6) 0.021(6) 0.002(6) N10 0.025(5) 0.041(6) 0.047(6) 0.002(5) 0.015(4) -0.006(4) N11 0.026(5) 0.080(9) 0.035(6) -0.004(5) 0.009(5) -0.016(5) N12 0.028(5) 0.028(5) 0.033(5) -0.004(4) 0.010(4) -0.010(4) N13 0.049(6) 0.047(7) 0.024(5) 0.022(5) 0.007(4) 0.001(5) C4 0.071(10) 0.053(10) 0.069(10) -0.002(8) 0.030(8) 0.002(8) C5 0.086(12) 0.060(11) 0.089(12) 0.012(9) 0.052(10) 0.021(9) C6 0.073(10) 0.054(10) 0.086(12) 0.018(8) 0.040(9) 0.027(8) C7 0.08(4) 0.08(5) 0.07(3) 0.00(3) 0.04(3) -0.01(3) C8 0.09(3) 0.08(4) 0.07(2) 0.00(2) 0.04(2) 0.00(3) C9 0.09(3) 0.08(5) 0.07(3) 0.00(3) 0.04(2) 0.00(4) C7' 0.08(5) 0.08(5) 0.07(3) 0.00(4) 0.03(3) 0.00(3) C8' 0.09(3) 0.08(5) 0.07(3) 0.00(2) 0.04(2) 0.00(3) C9' 0.09(4) 0.08(5) 0.06(3) 0.00(4) 0.04(2) 0.00(4) C10 0.074(11) 0.064(10) 0.080(11) 0.028(8) 0.041(9) 0.025(8) C11 0.073(11) 0.085(13) 0.102(13) -0.001(10) 0.063(11) 0.002(10) C12 0.061(10) 0.072(11) 0.091(12) -0.001(9) 0.049(9) 0.003(8) C13 0.057(8) 0.047(8) 0.055(8) 0.013(6) 0.031(7) 0.022(7) C14 0.051(8) 0.053(10) 0.049(8) -0.003(6) 0.012(7) 0.023(7) C15 0.066(9) 0.076(11) 0.029(7) -0.003(7) 0.014(7) -0.031(8) C16 0.061(8) 0.032(7) 0.046(7) 0.006(6) 0.022(7) 0.010(6) C17 0.033(6) 0.038(7) 0.032(6) 0.006(5) 0.006(5) -0.004(5) C18 0.037(6) 0.027(7) 0.037(6) -0.012(5) 0.012(5) -0.005(5) C19 0.056(9) 0.064(10) 0.060(9) -0.005(7) 0.030(7) 0.005(7) C20 0.092(12) 0.049(10) 0.083(11) 0.012(8) 0.055(10) 0.013(9) C21 0.093(11) 0.037(9) 0.090(11) -0.012(8) 0.062(10) 0.026(8) C22 0.050(8) 0.073(11) 0.060(9) -0.014(7) 0.031(7) -0.017(7) C23 0.058(10) 0.095(14) 0.057(9) 0.025(9) 0.027(8) 0.011(10) C24 0.106(18) 0.14(2) 0.19(3) -0.008(19) 0.10(2) -0.033(16) C25 0.14(3) 0.33(6) 0.22(4) -0.05(4) 0.08(3) -0.10(3) C26 0.15(10) 0.06(7) 0.18(11) 0.02(6) 0.11(9) 0.04(7) O3 0.16(5) 0.06(3) 0.17(7) 0.02(5) 0.12(6) 0.04(3) O4 0.15(7) 0.06(4) 0.18(8) 0.02(5) 0.11(7) 0.04(6) C27 0.16(5) 0.07(3) 0.18(6) 0.02(3) 0.10(5) 0.03(3) C28 0.17(6) 0.08(4) 0.19(6) 0.03(4) 0.10(6) 0.03(3) C26' 0.15(11) 0.06(7) 0.18(12) 0.02(7) 0.11(9) 0.04(6) O3' 0.15(6) 0.06(3) 0.19(8) 0.02(4) 0.12(6) 0.03(5) O4' 0.15(4) 0.06(3) 0.18(8) 0.02(5) 0.11(6) 0.04(2) C27' 0.15(4) 0.06(3) 0.19(6) 0.02(3) 0.10(4) 0.03(3) C28' 0.16(5) 0.08(3) 0.19(6) 0.02(3) 0.10(5) 0.03(3) C29 0.069(10) 0.057(10) 0.052(8) -0.004(7) 0.023(7) -0.010(7) C30 0.100(12) 0.050(10) 0.052(9) -0.006(7) 0.037(9) -0.007(8) C31 0.044(7) 0.061(10) 0.031(7) -0.001(6) -0.009(6) 0.010(6) C32 0.062(8) 0.033(8) 0.035(7) 0.007(6) 0.009(6) 0.014(6) C33 0.039(7) 0.064(10) 0.020(6) 0.010(5) 0.004(5) 0.014(6) C34 0.038(7) 0.060(9) 0.016(5) 0.009(5) 0.002(5) 0.005(6) C35 0.063(8) 0.046(8) 0.053(8) 0.003(7) 0.032(7) -0.006(7) C36 0.044(8) 0.068(11) 0.049(8) -0.001(7) 0.014(6) 0.001(7) C37 0.065(10) 0.067(11) 0.049(9) -0.016(8) 0.006(7) -0.001(8) C38 0.086(11) 0.055(10) 0.046(8) -0.009(7) 0.029(8) -0.016(8) C39 0.082(11) 0.049(10) 0.040(8) 0.010(7) -0.012(8) 0.007(8) C40 0.112(16) 0.097(16) 0.091(14) 0.016(12) 0.048(13) -0.008(12) C41 0.126(19) 0.13(2) 0.112(18) 0.010(15) 0.056(16) -0.006(16) C42 0.066(10) 0.089(14) 0.057(10) 0.011(10) 0.032(8) 0.007(9) C43 0.113(17) 0.110(16) 0.063(12) 0.014(11) 0.022(11) -0.021(13) C44 0.103(17) 0.14(2) 0.089(14) 0.044(14) 0.031(13) 0.001(14) O1 0.066(7) 0.119(10) 0.106(9) 0.018(8) 0.059(7) 0.020(7) O2 0.082(8) 0.068(8) 0.112(9) -0.007(7) 0.062(7) -0.013(6) O5 0.112(10) 0.056(7) 0.081(8) 0.003(6) 0.025(7) -0.017(6) O6 0.112(10) 0.058(7) 0.068(8) 0.002(6) 0.025(7) -0.001(6) O7 0.081(7) 0.077(8) 0.038(5) 0.013(5) 0.005(5) 0.001(6) O8 0.086(8) 0.090(9) 0.040(6) -0.016(6) 0.000(5) 0.003(6) Cl1 0.071(18) 0.10(3) 0.077(19) 0.03(2) 0.036(14) 0.027(18) O9 0.10(2) 0.14(6) 0.10(2) 0.01(3) 0.059(17) 0.03(2) O10 0.12(4) 0.13(3) 0.13(3) 0.01(2) 0.06(3) 0.01(3) O11 0.09(3) 0.09(4) 0.085(19) 0.02(3) 0.047(17) 0.04(3) O12 0.10(2) 0.13(2) 0.11(4) -0.01(2) 0.04(3) -0.001(18) Cl1' 0.09(4) 0.12(8) 0.10(4) 0.01(3) 0.04(3) 0.02(3) O9' 0.10(3) 0.12(4) 0.12(9) 0.01(4) 0.04(4) 0.00(3) O10' 0.11(3) 0.12(6) 0.11(4) 0.00(4) 0.04(3) 0.03(4) O11' 0.10(5) 0.11(7) 0.10(4) 0.00(6) 0.05(4) 0.00(7) O12' 0.11(5) 0.12(4) 0.11(3) 0.02(3) 0.06(4) 0.01(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.049(11) . ? Co1 N2 2.065(9) 3_566 ? Co1 N11 2.110(12) . ? Co1 N12 2.111(9) . ? Co1 N13 2.117(9) . ? Co1 N10 2.138(9) . ? Fe1 C1 1.910(13) . ? Fe1 C3 1.93(2) . ? Fe1 C2 1.930(11) . ? Fe1 N6 1.971(9) . ? Fe1 N4 1.983(9) . ? Fe1 N8 1.993(9) . ? C1 N1 1.154(15) . ? C2 N2 1.105(13) . ? N2 Co1 2.065(9) 3_566 ? C3 N3 1.17(2) . ? B1 N9 1.50(2) . ? B1 N7 1.54(2) . ? B1 N5 1.57(2) . ? B1 H1 0.9800 . ? N4 C4 1.321(17) . ? N4 N5 1.361(13) . ? N5 C6 1.332(18) . ? N6 C7' 1.33(9) . ? N6 N7 1.333(16) . ? N6 C7 1.35(8) . ? N7 C9' 1.35(9) . ? N7 C9 1.42(8) . ? N8 C10 1.345(17) . ? N8 N9 1.360(14) . ? N9 C12 1.359(17) . ? N10 C13 1.284(15) . ? N10 C17 1.378(15) . ? N11 C18 1.320(14) . ? N11 C22 1.376(17) . ? N12 C33 1.339(14) . ? N12 C29 1.366(16) . ? N13 C38 1.314(16) . ? N13 C34 1.343(16) . ? C4 C5 1.35(2) . ? C4 H4 0.9300 . ? C5 C6 1.36(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.31(8) . ? C7 H7 0.9300 . ? C8 C9 1.24(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C7' C8' 1.36(9) . ? C7' H7' 0.9300 . ? C8' C9' 1.34(11) . ? C8' H8' 0.9300 . ? C9' H9' 0.9300 . ? C10 C11 1.34(2) . ? C10 H10 0.9300 . ? C11 C12 1.38(2) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.371(19) . ? C13 H13 0.9300 . ? C14 C15 1.40(2) . ? C14 H14 0.9300 . ? C15 C16 1.39(2) . ? C15 C23 1.52(2) . ? C16 C17 1.361(17) . ? C16 H16 0.9300 . ? C17 C18 1.513(16) . ? C18 C19 1.370(18) . ? C19 C20 1.383(19) . ? C19 H19 0.9300 . ? C20 C21 1.40(2) . ? C20 C26 1.5(2) . ? C20 C26' 1.5(2) . ? C21 C22 1.37(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O1 1.24(2) . ? C23 O2 1.26(2) . ? C24 C25 1.49(4) . ? C24 O2 1.49(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O3 1.223(10) . ? C26 O4 1.286(11) . ? O4 C27 1.50(15) . ? C27 C28 1.50(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C26' O3' 1.224(10) . ? C26' O4' 1.284(10) . ? O4' C27' 1.50(12) . ? C27' C28' 1.50(7) . ? C27' H27C 0.9700 . ? C27' H27D 0.9700 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29 C30 1.33(2) . ? C29 H29 0.9300 . ? C30 C31 1.398(18) . ? C30 H30 0.9300 . ? C31 C32 1.333(17) . ? C31 C39 1.50(2) . ? C32 C33 1.345(18) . ? C32 H32 0.9300 . ? C33 C34 1.523(17) . ? C34 C35 1.376(17) . ? C35 C36 1.405(19) . ? C35 H35 0.9300 . ? C36 C37 1.38(2) . ? C36 C42 1.50(2) . ? C37 C38 1.39(2) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 O6 1.219(17) . ? C39 O5 1.293(17) . ? C40 O5 1.52(2) . ? C40 C41 1.55(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 O8 1.220(19) . ? C42 O7 1.33(2) . ? C43 C44 1.44(3) . ? C43 O7 1.488(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? Cl1 O9 1.43(9) . ? Cl1 O12 1.43(14) . ? Cl1 O11 1.47(11) . ? Cl1 O10 1.52(12) . ? Cl1' O12' 1.31(14) . ? Cl1' O11' 1.32(19) . ? Cl1' O10' 1.36(19) . ? Cl1' O9' 1.4(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N2 94.3(4) . 3_566 ? N1 Co1 N11 95.0(4) . . ? N2 Co1 N11 86.5(4) 3_566 . ? N1 Co1 N12 86.1(4) . . ? N2 Co1 N12 93.5(4) 3_566 . ? N11 Co1 N12 178.9(4) . . ? N1 Co1 N13 90.1(4) . . ? N2 Co1 N13 169.0(4) 3_566 . ? N11 Co1 N13 103.2(4) . . ? N12 Co1 N13 76.7(4) . . ? N1 Co1 N10 172.2(4) . . ? N2 Co1 N10 88.1(4) 3_566 . ? N11 Co1 N10 77.8(4) . . ? N12 Co1 N10 101.1(3) . . ? N13 Co1 N10 88.9(4) . . ? C1 Fe1 C3 83.5(6) . . ? C1 Fe1 C2 88.3(5) . . ? C3 Fe1 C2 84.6(7) . . ? C1 Fe1 N6 91.1(5) . . ? C3 Fe1 N6 95.6(7) . . ? C2 Fe1 N6 179.4(5) . . ? C1 Fe1 N4 92.5(5) . . ? C3 Fe1 N4 175.1(5) . . ? C2 Fe1 N4 92.5(4) . . ? N6 Fe1 N4 87.3(5) . . ? C1 Fe1 N8 178.8(5) . . ? C3 Fe1 N8 95.5(5) . . ? C2 Fe1 N8 90.9(5) . . ? N6 Fe1 N8 89.7(5) . . ? N4 Fe1 N8 88.4(4) . . ? N1 C1 Fe1 175.8(12) . . ? C1 N1 Co1 174.4(9) . . ? N2 C2 Fe1 179.2(12) . . ? C2 N2 Co1 173.5(10) . 3_566 ? N3 C3 Fe1 174.6(19) . . ? N9 B1 N7 109.0(14) . . ? N9 B1 N5 107.0(12) . . ? N7 B1 N5 106.7(11) . . ? N9 B1 H1 111.4 . . ? N7 B1 H1 111.0 . . ? N5 B1 H1 111.5 . . ? C4 N4 N5 106.8(11) . . ? C4 N4 Fe1 133.6(10) . . ? N5 N4 Fe1 119.6(8) . . ? C6 N5 N4 108.0(12) . . ? C6 N5 B1 135.0(12) . . ? N4 N5 B1 117.0(11) . . ? C7' N6 N7 101(4) . . ? C7' N6 C7 28(3) . . ? N7 N6 C7 111(3) . . ? C7' N6 Fe1 139(4) . . ? N7 N6 Fe1 117.8(8) . . ? C7 N6 Fe1 129(4) . . ? N6 N7 C9' 114(4) . . ? N6 N7 C9 100(3) . . ? C9' N7 C9 28(3) . . ? N6 N7 B1 120.5(11) . . ? C9' N7 B1 123(5) . . ? C9 N7 B1 138(3) . . ? C10 N8 N9 104.7(11) . . ? C10 N8 Fe1 134.0(10) . . ? N9 N8 Fe1 119.9(8) . . ? C12 N9 N8 110.1(11) . . ? C12 N9 B1 132.5(13) . . ? N8 N9 B1 117.4(11) . . ? C13 N10 C17 118.5(10) . . ? C13 N10 Co1 126.8(9) . . ? C17 N10 Co1 114.5(7) . . ? C18 N11 C22 117.3(12) . . ? C18 N11 Co1 116.5(8) . . ? C22 N11 Co1 124.8(9) . . ? C33 N12 C29 115.5(11) . . ? C33 N12 Co1 117.4(8) . . ? C29 N12 Co1 125.8(9) . . ? C38 N13 C34 118.3(11) . . ? C38 N13 Co1 126.3(10) . . ? C34 N13 Co1 115.3(8) . . ? N4 C4 C5 110.7(15) . . ? N4 C4 H4 124.6 . . ? C5 C4 H4 124.6 . . ? C4 C5 C6 105.2(15) . . ? C4 C5 H5 127.4 . . ? C6 C5 H5 127.4 . . ? N5 C6 C5 109.2(14) . . ? N5 C6 H6 125.4 . . ? C5 C6 H6 125.4 . . ? C8 C7 N6 107(6) . . ? C8 C7 H7 126.4 . . ? N6 C7 H7 126.4 . . ? C9 C8 C7 109(6) . . ? C9 C8 H8 125.4 . . ? C7 C8 H8 125.4 . . ? C8 C9 N7 112(6) . . ? C8 C9 H9 123.8 . . ? N7 C9 H9 123.8 . . ? N6 C7' C8' 114(7) . . ? N6 C7' H7' 122.8 . . ? C8' C7' H7' 122.8 . . ? C9' C8' C7' 104(6) . . ? C9' C8' H8' 127.8 . . ? C7' C8' H8' 127.8 . . ? C8' C9' N7 106(6) . . ? C8' C9' H9' 126.9 . . ? N7 C9' H9' 126.9 . . ? C11 C10 N8 112.1(14) . . ? C11 C10 H10 123.9 . . ? N8 C10 H10 123.9 . . ? C10 C11 C12 106.2(14) . . ? C10 C11 H11 126.9 . . ? C12 C11 H11 126.9 . . ? N9 C12 C11 106.6(14) . . ? N9 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? N10 C13 C14 125.3(13) . . ? N10 C13 H13 117.3 . . ? C14 C13 H13 117.3 . . ? C13 C14 C15 116.3(12) . . ? C13 C14 H14 121.9 . . ? C15 C14 H14 121.9 . . ? C16 C15 C14 119.7(13) . . ? C16 C15 C23 120.8(15) . . ? C14 C15 C23 119.5(16) . . ? C17 C16 C15 118.6(12) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 N10 121.3(11) . . ? C16 C17 C18 124.2(11) . . ? N10 C17 C18 114.5(10) . . ? N11 C18 C19 123.1(12) . . ? N11 C18 C17 116.1(10) . . ? C19 C18 C17 120.6(11) . . ? C18 C19 C20 121.1(14) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C21 115.8(14) . . ? C19 C20 C26 130(5) . . ? C21 C20 C26 114(6) . . ? C19 C20 C26' 117(4) . . ? C21 C20 C26' 127(4) . . ? C26 C20 C26' 14(10) . . ? C22 C21 C20 120.8(12) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 N11 121.7(13) . . ? C21 C22 H22 119.2 . . ? N11 C22 H22 119.2 . . ? O1 C23 O2 126.2(15) . . ? O1 C23 C15 118.4(17) . . ? O2 C23 C15 115.3(15) . . ? C25 C24 O2 103(2) . . ? C25 C24 H24A 111.2 . . ? O2 C24 H24A 111.2 . . ? C25 C24 H24B 111.2 . . ? O2 C24 H24B 111.2 . . ? H24A C24 H24B 109.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O3 C26 O4 129(10) . . ? O3 C26 C20 120(10) . . ? O4 C26 C20 111(10) . . ? C26 O4 C27 111(10) . . ? C28 C27 O4 124(7) . . ? C28 C27 H27A 106.4 . . ? O4 C27 H27A 106.4 . . ? C28 C27 H27B 106.4 . . ? O4 C27 H27B 106.4 . . ? H27A C27 H27B 106.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3' C26' O4' 127(10) . . ? O3' C26' C20 120(10) . . ? O4' C26' C20 113(10) . . ? C26' O4' C27' 125(10) . . ? C28' C27' O4' 102(6) . . ? C28' C27' H27C 111.5 . . ? O4' C27' H27C 111.5 . . ? C28' C27' H27D 111.5 . . ? O4' C27' H27D 111.5 . . ? H27C C27' H27D 109.3 . . ? C27' C28' H28D 109.5 . . ? C27' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C30 C29 N12 124.3(14) . . ? C30 C29 H29 117.8 . . ? N12 C29 H29 117.8 . . ? C29 C30 C31 117.9(14) . . ? C29 C30 H30 121.1 . . ? C31 C30 H30 121.1 . . ? C32 C31 C30 118.3(14) . . ? C32 C31 C39 125.4(12) . . ? C30 C31 C39 116.3(12) . . ? C31 C32 C33 121.3(12) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? N12 C33 C32 122.6(11) . . ? N12 C33 C34 111.8(11) . . ? C32 C33 C34 125.6(10) . . ? N13 C34 C35 123.6(11) . . ? N13 C34 C33 116.3(9) . . ? C35 C34 C33 120.1(12) . . ? C34 C35 C36 117.8(13) . . ? C34 C35 H35 121.1 . . ? C36 C35 H35 121.1 . . ? C37 C36 C35 118.1(13) . . ? C37 C36 C42 118.9(14) . . ? C35 C36 C42 123.0(14) . . ? C36 C37 C38 119.7(13) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? N13 C38 C37 122.4(14) . . ? N13 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? O6 C39 O5 124.7(15) . . ? O6 C39 C31 124.4(13) . . ? O5 C39 C31 110.6(13) . . ? O5 C40 C41 111.1(16) . . ? O5 C40 H40A 109.4 . . ? C41 C40 H40A 109.4 . . ? O5 C40 H40B 109.4 . . ? C41 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O8 C42 O7 125.4(15) . . ? O8 C42 C36 122.2(16) . . ? O7 C42 C36 112.1(14) . . ? C44 C43 O7 112.5(17) . . ? C44 C43 H43A 109.1 . . ? O7 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? O7 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C23 O2 C24 114.5(15) . . ? C39 O5 C40 116.1(13) . . ? C42 O7 C43 114.6(13) . . ? O9 Cl1 O12 106(7) . . ? O9 Cl1 O11 113(6) . . ? O12 Cl1 O11 106(9) . . ? O9 Cl1 O10 128(10) . . ? O12 Cl1 O10 98(5) . . ? O11 Cl1 O10 104(7) . . ? O12' Cl1' O11' 133(10) . . ? O12' Cl1' O10' 95(10) . . ? O11' Cl1' O10' 105(10) . . ? O12' Cl1' O9' 105(10) . . ? O11' Cl1' O9' 113(10) . . ? O10' Cl1' O9' 101(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 C1 N1 -135(15) . . . . ? C2 Fe1 C1 N1 -51(15) . . . . ? N6 Fe1 C1 N1 129(15) . . . . ? N4 Fe1 C1 N1 42(15) . . . . ? N8 Fe1 C1 N1 -100(29) . . . . ? Fe1 C1 N1 Co1 44(25) . . . . ? N2 Co1 N1 C1 3(12) 3_566 . . . ? N11 Co1 N1 C1 90(12) . . . . ? N12 Co1 N1 C1 -90(12) . . . . ? N13 Co1 N1 C1 -166(12) . . . . ? N10 Co1 N1 C1 111(11) . . . . ? C1 Fe1 C2 N2 65(100) . . . . ? C3 Fe1 C2 N2 149(100) . . . . ? N6 Fe1 C2 N2 43(100) . . . . ? N4 Fe1 C2 N2 -27(100) . . . . ? N8 Fe1 C2 N2 -116(100) . . . . ? Fe1 C2 N2 Co1 95(100) . . . 3_566 ? C1 Fe1 C3 N3 139(17) . . . . ? C2 Fe1 C3 N3 50(17) . . . . ? N6 Fe1 C3 N3 -131(17) . . . . ? N4 Fe1 C3 N3 104(16) . . . . ? N8 Fe1 C3 N3 -41(17) . . . . ? C1 Fe1 N4 C4 -44.8(12) . . . . ? C3 Fe1 N4 C4 -10(8) . . . . ? C2 Fe1 N4 C4 43.6(13) . . . . ? N6 Fe1 N4 C4 -135.8(12) . . . . ? N8 Fe1 N4 C4 134.4(12) . . . . ? C1 Fe1 N4 N5 137.1(8) . . . . ? C3 Fe1 N4 N5 172(8) . . . . ? C2 Fe1 N4 N5 -134.5(8) . . . . ? N6 Fe1 N4 N5 46.1(8) . . . . ? N8 Fe1 N4 N5 -43.7(8) . . . . ? C4 N4 N5 C6 2.0(14) . . . . ? Fe1 N4 N5 C6 -179.4(9) . . . . ? C4 N4 N5 B1 -177.7(12) . . . . ? Fe1 N4 N5 B1 0.9(14) . . . . ? N9 B1 N5 C6 -120.2(17) . . . . ? N7 B1 N5 C6 123.3(17) . . . . ? N9 B1 N5 N4 59.4(15) . . . . ? N7 B1 N5 N4 -57.1(15) . . . . ? C1 Fe1 N6 C7' 19(6) . . . . ? C3 Fe1 N6 C7' -65(6) . . . . ? C2 Fe1 N6 C7' 41(47) . . . . ? N4 Fe1 N6 C7' 111(6) . . . . ? N8 Fe1 N6 C7' -160(6) . . . . ? C1 Fe1 N6 N7 -143.6(12) . . . . ? C3 Fe1 N6 N7 132.8(12) . . . . ? C2 Fe1 N6 N7 -122(45) . . . . ? N4 Fe1 N6 N7 -51.1(11) . . . . ? N8 Fe1 N6 N7 37.3(11) . . . . ? C1 Fe1 N6 C7 56(4) . . . . ? C3 Fe1 N6 C7 -28(4) . . . . ? C2 Fe1 N6 C7 78(46) . . . . ? N4 Fe1 N6 C7 148(4) . . . . ? N8 Fe1 N6 C7 -123(4) . . . . ? C7' N6 N7 C9' 1(4) . . . . ? C7 N6 N7 C9' -26(4) . . . . ? Fe1 N6 N7 C9' 170(4) . . . . ? C7' N6 N7 C9 28(4) . . . . ? C7 N6 N7 C9 0(4) . . . . ? Fe1 N6 N7 C9 -164(4) . . . . ? C7' N6 N7 B1 -160(4) . . . . ? C7 N6 N7 B1 172(4) . . . . ? Fe1 N6 N7 B1 8.3(19) . . . . ? N9 B1 N7 N6 -62.4(18) . . . . ? N5 B1 N7 N6 52.7(18) . . . . ? N9 B1 N7 C9' 138(4) . . . . ? N5 B1 N7 C9' -107(4) . . . . ? N9 B1 N7 C9 106(6) . . . . ? N5 B1 N7 C9 -139(6) . . . . ? C1 Fe1 N8 C10 19(24) . . . . ? C3 Fe1 N8 C10 54.3(15) . . . . ? C2 Fe1 N8 C10 -30.3(14) . . . . ? N6 Fe1 N8 C10 149.9(14) . . . . ? N4 Fe1 N8 C10 -122.8(14) . . . . ? C1 Fe1 N8 N9 -177(100) . . . . ? C3 Fe1 N8 N9 -141.6(10) . . . . ? C2 Fe1 N8 N9 133.8(9) . . . . ? N6 Fe1 N8 N9 -46.0(10) . . . . ? N4 Fe1 N8 N9 41.3(9) . . . . ? C10 N8 N9 C12 -5.5(15) . . . . ? Fe1 N8 N9 C12 -173.7(9) . . . . ? C10 N8 N9 B1 174.1(14) . . . . ? Fe1 N8 N9 B1 5.9(16) . . . . ? N7 B1 N9 C12 -128.5(15) . . . . ? N5 B1 N9 C12 116.5(16) . . . . ? N7 B1 N9 N8 52.1(16) . . . . ? N5 B1 N9 N8 -62.9(16) . . . . ? N1 Co1 N10 C13 159(2) . . . . ? N2 Co1 N10 C13 -92.3(10) 3_566 . . . ? N11 Co1 N10 C13 -179.1(11) . . . . ? N12 Co1 N10 C13 1.0(10) . . . . ? N13 Co1 N10 C13 77.1(10) . . . . ? N1 Co1 N10 C17 -25(3) . . . . ? N2 Co1 N10 C17 82.9(8) 3_566 . . . ? N11 Co1 N10 C17 -3.9(7) . . . . ? N12 Co1 N10 C17 176.2(7) . . . . ? N13 Co1 N10 C17 -107.7(8) . . . . ? N1 Co1 N11 C18 -175.3(8) . . . . ? N2 Co1 N11 C18 -81.3(8) 3_566 . . . ? N12 Co1 N11 C18 11(21) . . . . ? N13 Co1 N11 C18 93.4(8) . . . . ? N10 Co1 N11 C18 7.5(8) . . . . ? N1 Co1 N11 C22 -9.1(10) . . . . ? N2 Co1 N11 C22 85.0(10) 3_566 . . . ? N12 Co1 N11 C22 177(100) . . . . ? N13 Co1 N11 C22 -100.3(10) . . . . ? N10 Co1 N11 C22 173.8(10) . . . . ? N1 Co1 N12 C33 -76.0(8) . . . . ? N2 Co1 N12 C33 -170.1(8) 3_566 . . . ? N11 Co1 N12 C33 98(20) . . . . ? N13 Co1 N12 C33 15.1(8) . . . . ? N10 Co1 N12 C33 101.2(8) . . . . ? N1 Co1 N12 C29 90.1(10) . . . . ? N2 Co1 N12 C29 -4.0(10) 3_566 . . . ? N11 Co1 N12 C29 -96(20) . . . . ? N13 Co1 N12 C29 -178.9(10) . . . . ? N10 Co1 N12 C29 -92.8(10) . . . . ? N1 Co1 N13 C38 -100.7(12) . . . . ? N2 Co1 N13 C38 145.7(19) 3_566 . . . ? N11 Co1 N13 C38 -5.6(12) . . . . ? N12 Co1 N13 C38 173.4(12) . . . . ? N10 Co1 N13 C38 71.6(11) . . . . ? N1 Co1 N13 C34 76.6(9) . . . . ? N2 Co1 N13 C34 -37(2) 3_566 . . . ? N11 Co1 N13 C34 171.7(8) . . . . ? N12 Co1 N13 C34 -9.4(8) . . . . ? N10 Co1 N13 C34 -111.1(9) . . . . ? N5 N4 C4 C5 -0.5(16) . . . . ? Fe1 N4 C4 C5 -178.8(10) . . . . ? N4 C4 C5 C6 -1.1(18) . . . . ? N4 N5 C6 C5 -2.8(16) . . . . ? B1 N5 C6 C5 176.9(15) . . . . ? C4 C5 C6 N5 2.4(18) . . . . ? C7' N6 C7 C8 -74(13) . . . . ? N7 N6 C7 C8 0(5) . . . . ? Fe1 N6 C7 C8 162(3) . . . . ? N6 C7 C8 C9 0(7) . . . . ? C7 C8 C9 N7 0(8) . . . . ? N6 N7 C9 C8 0(6) . . . . ? C9' N7 C9 C8 122(18) . . . . ? B1 N7 C9 C8 -170(4) . . . . ? N7 N6 C7' C8' -1(6) . . . . ? C7 N6 C7' C8' 112(16) . . . . ? Fe1 N6 C7' C8' -166(4) . . . . ? N6 C7' C8' C9' 1(8) . . . . ? C7' C8' C9' N7 0(7) . . . . ? N6 N7 C9' C8' -1(6) . . . . ? C9 N7 C9' C8' -67(13) . . . . ? B1 N7 C9' C8' 160(3) . . . . ? N9 N8 C10 C11 4.9(18) . . . . ? Fe1 N8 C10 C11 170.6(11) . . . . ? N8 C10 C11 C12 -2(2) . . . . ? N8 N9 C12 C11 4.1(17) . . . . ? B1 N9 C12 C11 -175.3(16) . . . . ? C10 C11 C12 N9 -1.1(19) . . . . ? C17 N10 C13 C14 2.4(19) . . . . ? Co1 N10 C13 C14 177.4(10) . . . . ? N10 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C16 -2.2(18) . . . . ? C13 C14 C15 C23 176.5(12) . . . . ? C14 C15 C16 C17 1.2(18) . . . . ? C23 C15 C16 C17 -177.5(11) . . . . ? C15 C16 C17 N10 1.6(17) . . . . ? C15 C16 C17 C18 -177.7(11) . . . . ? C13 N10 C17 C16 -3.4(16) . . . . ? Co1 N10 C17 C16 -179.0(9) . . . . ? C13 N10 C17 C18 176.0(10) . . . . ? Co1 N10 C17 C18 0.3(11) . . . . ? C22 N11 C18 C19 -2.2(16) . . . . ? Co1 N11 C18 C19 165.1(10) . . . . ? C22 N11 C18 C17 -176.9(10) . . . . ? Co1 N11 C18 C17 -9.6(12) . . . . ? C16 C17 C18 N11 -174.6(11) . . . . ? N10 C17 C18 N11 6.1(14) . . . . ? C16 C17 C18 C19 10.6(17) . . . . ? N10 C17 C18 C19 -168.8(11) . . . . ? N11 C18 C19 C20 2(2) . . . . ? C17 C18 C19 C20 177.0(12) . . . . ? C18 C19 C20 C21 -3(2) . . . . ? C18 C19 C20 C26 -173(15) . . . . ? C18 C19 C20 C26' -179(10) . . . . ? C19 C20 C21 C22 3(2) . . . . ? C26 C20 C21 C22 175(12) . . . . ? C26' C20 C21 C22 179(11) . . . . ? C20 C21 C22 N11 -3(2) . . . . ? C18 N11 C22 C21 2.3(18) . . . . ? Co1 N11 C22 C21 -163.9(11) . . . . ? C16 C15 C23 O1 -174.0(13) . . . . ? C14 C15 C23 O1 7(2) . . . . ? C16 C15 C23 O2 10.1(19) . . . . ? C14 C15 C23 O2 -168.6(13) . . . . ? C19 C20 C26 O3 -170(14) . . . . ? C21 C20 C26 O3 19(27) . . . . ? C26' C20 C26 O3 -149(96) . . . . ? C19 C20 C26 O4 6(30) . . . . ? C21 C20 C26 O4 -165(16) . . . . ? C26' C20 C26 O4 27(58) . . . . ? O3 C26 O4 C27 -22(37) . . . . ? C20 C26 O4 C27 162(14) . . . . ? C26 O4 C27 C28 -85(21) . . . . ? C19 C20 C26' O3' -11(24) . . . . ? C21 C20 C26' O3' 173(13) . . . . ? C26 C20 C26' O3' -173(94) . . . . ? C19 C20 C26' O4' 162(11) . . . . ? C21 C20 C26' O4' -14(21) . . . . ? C26 C20 C26' O4' 0(63) . . . . ? O3' C26' O4' C27' -8(31) . . . . ? C20 C26' O4' C27' 179(11) . . . . ? C26' O4' C27' C28' 104(14) . . . . ? C33 N12 C29 C30 5(2) . . . . ? Co1 N12 C29 C30 -160.9(12) . . . . ? N12 C29 C30 C31 -2(2) . . . . ? C29 C30 C31 C32 -2(2) . . . . ? C29 C30 C31 C39 179.4(15) . . . . ? C30 C31 C32 C33 2(2) . . . . ? C39 C31 C32 C33 -179.0(14) . . . . ? C29 N12 C33 C32 -4.9(17) . . . . ? Co1 N12 C33 C32 162.6(10) . . . . ? C29 N12 C33 C34 175.3(10) . . . . ? Co1 N12 C33 C34 -17.2(12) . . . . ? C31 C32 C33 N12 1(2) . . . . ? C31 C32 C33 C34 -178.9(13) . . . . ? C38 N13 C34 C35 1.4(19) . . . . ? Co1 N13 C34 C35 -176.1(10) . . . . ? C38 N13 C34 C33 -179.0(11) . . . . ? Co1 N13 C34 C33 3.5(13) . . . . ? N12 C33 C34 N13 8.8(15) . . . . ? C32 C33 C34 N13 -171.0(12) . . . . ? N12 C33 C34 C35 -171.6(11) . . . . ? C32 C33 C34 C35 8.6(19) . . . . ? N13 C34 C35 C36 0.7(19) . . . . ? C33 C34 C35 C36 -178.9(11) . . . . ? C34 C35 C36 C37 -3(2) . . . . ? C34 C35 C36 C42 179.4(12) . . . . ? C35 C36 C37 C38 3(2) . . . . ? C42 C36 C37 C38 -179.2(14) . . . . ? C34 N13 C38 C37 -1(2) . . . . ? Co1 N13 C38 C37 175.9(11) . . . . ? C36 C37 C38 N13 -1(2) . . . . ? C32 C31 C39 O6 179.4(17) . . . . ? C30 C31 C39 O6 -2(3) . . . . ? C32 C31 C39 O5 5(2) . . . . ? C30 C31 C39 O5 -176.3(15) . . . . ? C37 C36 C42 O8 6(2) . . . . ? C35 C36 C42 O8 -176.6(14) . . . . ? C37 C36 C42 O7 179.4(14) . . . . ? C35 C36 C42 O7 -3(2) . . . . ? O1 C23 O2 C24 6(2) . . . . ? C15 C23 O2 C24 -178.4(15) . . . . ? C25 C24 O2 C23 -91(3) . . . . ? O6 C39 O5 C40 7(3) . . . . ? C31 C39 O5 C40 -178.4(14) . . . . ? C41 C40 O5 C39 80(2) . . . . ? O8 C42 O7 C43 1(2) . . . . ? C36 C42 O7 C43 -172.2(14) . . . . ? C44 C43 O7 C42 -91(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.073 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.221 # start Validation Reply Form _vrf_RFACG01_1273K ; PROBLEM: The value of the R factor is > 0.15 RESPONSE: Due to the poor diffraction data. ; _vrf_RFACR01_1273K ; PROBLEM: The value of the weighted R factor is > 0.35 RESPONSE: Due to the poor diffraction data. ; _vrf_PLAT082_1273K ; PROBLEM: High R1 Value .................................. 0.16 RESPONSE: Due to the poor diffraction data. ; _vrf_PLAT084_1273K ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.44 RESPONSE: Due to the poor diffraction data. ; _vrf_PLAT220_1273K ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.3 Ratio RESPONSE: Due to the disordered terminal ethyl groups. ; _vrf_PLAT341_1273K ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0246 Ang. RESPONSE: Due to the poor diffraction data. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 967845' ####################################################################### # # 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_1.2MeOH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H92 B2 Cl2 Co2 Fe2 N26 O26' _chemical_formula_weight 2275.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.6722(11) _cell_length_b 17.9250(12) _cell_length_c 20.6405(11) _cell_angle_alpha 90.00 _cell_angle_beta 119.458(4) _cell_angle_gamma 90.00 _cell_volume 5048.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9847 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.37 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7804 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34637 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8863 _reflns_number_gt 7591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0454P)^2^+7.1875P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8863 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.24928(2) 0.501397(16) 0.619506(16) 0.01433(9) Uani 1 1 d . . . Fe1 Fe -0.03743(2) 0.579411(18) 0.634959(17) 0.01505(9) Uani 1 1 d . . . O1 O 0.59737(14) 0.38645(10) 0.52822(11) 0.0326(4) Uani 1 1 d . . . O2 O 0.55410(13) 0.27806(9) 0.55840(10) 0.0239(4) Uani 1 1 d . . . O3 O 0.23406(14) 0.11964(9) 0.62884(11) 0.0302(4) Uani 1 1 d . . . O4 O 0.11998(13) 0.14947(9) 0.66110(10) 0.0241(4) Uani 1 1 d . . . O5 O 0.21930(14) 0.87559(10) 0.53369(10) 0.0317(4) Uani 1 1 d . . . O6 O 0.29655(12) 0.87275(9) 0.65850(9) 0.0208(4) Uani 1 1 d . . . O7 O 0.61267(12) 0.66527(9) 0.93658(9) 0.0235(4) Uani 1 1 d . . . O8 O 0.64279(13) 0.54398(10) 0.96706(10) 0.0301(4) Uani 1 1 d . . . N1 N 0.15106(14) 0.53484(11) 0.64003(10) 0.0176(4) Uani 1 1 d . . . N2 N -0.15681(14) 0.51672(11) 0.48048(11) 0.0186(4) Uani 1 1 d . . . N3 N -0.0378(2) 0.42310(15) 0.69452(18) 0.0496(7) Uani 1 1 d . . . N4 N -0.03480(14) 0.68043(11) 0.59370(11) 0.0190(4) Uani 1 1 d . . . N5 N -0.05451(15) 0.74256(11) 0.62169(12) 0.0235(5) Uani 1 1 d . . . N6 N 0.03361(14) 0.62510(12) 0.73610(11) 0.0211(4) Uani 1 1 d . . . N7 N 0.00640(15) 0.69342(12) 0.74843(11) 0.0237(5) Uani 1 1 d . . . N8 N -0.16136(14) 0.60903(11) 0.63372(11) 0.0195(4) Uani 1 1 d . . . N9 N -0.16950(14) 0.67958(12) 0.65498(11) 0.0224(4) Uani 1 1 d . . . N10 N 0.34872(14) 0.46070(10) 0.60022(10) 0.0158(4) Uani 1 1 d . . . N11 N 0.23152(13) 0.39861(10) 0.63746(10) 0.0158(4) Uani 1 1 d . . . N12 N 0.26461(13) 0.60499(11) 0.60063(10) 0.0163(4) Uani 1 1 d . . . N13 N 0.34928(13) 0.52533(10) 0.71991(10) 0.0150(4) Uani 1 1 d . . . C1 C 0.07867(17) 0.55368(12) 0.63755(12) 0.0157(5) Uani 1 1 d . . . C2 C -0.10931(16) 0.54101(12) 0.53968(13) 0.0171(5) Uani 1 1 d . . . C3 C -0.03819(18) 0.48299(15) 0.67378(15) 0.0264(6) Uani 1 1 d . . . C4 C -0.00833(18) 0.70348(15) 0.54480(14) 0.0249(5) Uani 1 1 d . . . H4 H 0.0089 0.6715 0.5164 0.030 Uiso 1 1 calc R . . C5 C -0.0095(2) 0.78126(16) 0.54122(16) 0.0327(6) Uani 1 1 d . . . H5 H 0.0064 0.8119 0.5111 0.039 Uiso 1 1 calc R . . C6 C -0.03858(19) 0.80358(14) 0.59041(16) 0.0318(6) Uani 1 1 d . . . H6 H -0.0464 0.8539 0.6011 0.038 Uiso 1 1 calc R . . C7 C 0.10856(18) 0.60307(16) 0.80081(14) 0.0275(6) Uani 1 1 d . . . H7 H 0.1425 0.5572 0.8085 0.033 Uiso 1 1 calc R . . C8 C 0.1302(2) 0.65677(17) 0.85554(15) 0.0332(6) Uani 1 1 d . . . H8 H 0.1796 0.6547 0.9064 0.040 Uiso 1 1 calc R . . C9 C 0.06391(19) 0.71368(17) 0.81974(15) 0.0308(6) Uani 1 1 d . . . H9 H 0.0597 0.7591 0.8417 0.037 Uiso 1 1 calc R . . C10 C -0.24490(17) 0.57396(15) 0.61678(13) 0.0233(5) Uani 1 1 d . . . H10 H -0.2596 0.5238 0.6000 0.028 Uiso 1 1 calc R . . C11 C -0.30757(18) 0.62155(15) 0.62731(14) 0.0263(6) Uani 1 1 d . . . H11 H -0.3713 0.6106 0.6194 0.032 Uiso 1 1 calc R . . C12 C -0.25727(18) 0.68733(16) 0.65156(14) 0.0273(6) Uani 1 1 d . . . H12 H -0.2803 0.7311 0.6639 0.033 Uiso 1 1 calc R . . C13 C 0.41157(17) 0.49988(13) 0.58728(12) 0.0178(5) Uani 1 1 d . . . H13 H 0.4101 0.5528 0.5885 0.021 Uiso 1 1 calc R . . C14 C 0.47843(17) 0.46511(13) 0.57224(12) 0.0185(5) Uani 1 1 d . . . H14 H 0.5232 0.4938 0.5640 0.022 Uiso 1 1 calc R . . C15 C 0.47977(17) 0.38768(13) 0.56925(12) 0.0186(5) Uani 1 1 d . . . C16 C 0.41448(17) 0.34697(13) 0.58274(12) 0.0183(5) Uani 1 1 d . . . H16 H 0.4142 0.2940 0.5812 0.022 Uiso 1 1 calc R . . C17 C 0.34993(16) 0.38519(12) 0.59848(12) 0.0165(5) Uani 1 1 d . . . C18 C 0.27979(16) 0.34971(13) 0.61676(12) 0.0169(5) Uani 1 1 d . . . C19 C 0.26483(16) 0.27355(13) 0.61661(12) 0.0181(5) Uani 1 1 d . . . H19 H 0.2982 0.2397 0.6014 0.022 Uiso 1 1 calc R . . C20 C 0.20018(17) 0.24761(13) 0.63912(13) 0.0190(5) Uani 1 1 d . . . C21 C 0.15214(17) 0.29817(13) 0.66113(13) 0.0197(5) Uani 1 1 d . . . H21 H 0.1087 0.2811 0.6776 0.024 Uiso 1 1 calc R . . C22 C 0.16842(17) 0.37353(13) 0.65870(13) 0.0188(5) Uani 1 1 d . . . H22 H 0.1343 0.4083 0.6723 0.023 Uiso 1 1 calc R . . C23 C 0.55052(17) 0.35139(14) 0.54966(13) 0.0216(5) Uani 1 1 d . . . C24 C 0.61739(19) 0.23849(14) 0.53590(15) 0.0264(6) Uani 1 1 d . . . H24A H 0.6869 0.2517 0.5694 0.032 Uiso 1 1 calc R . . H24B H 0.5999 0.2523 0.4844 0.032 Uiso 1 1 calc R . . C25 C 0.6019(2) 0.15617(15) 0.54070(17) 0.0336(6) Uani 1 1 d . . . H25A H 0.5322 0.1443 0.5098 0.050 Uiso 1 1 calc R . . H25B H 0.6234 0.1427 0.5925 0.050 Uiso 1 1 calc R . . H25C H 0.6399 0.1280 0.5230 0.050 Uiso 1 1 calc R . . C26 C 0.18733(18) 0.16468(13) 0.64171(13) 0.0217(5) Uani 1 1 d . . . C27 C 0.1038(2) 0.07087(14) 0.67129(15) 0.0276(6) Uani 1 1 d . . . H27A H 0.0750 0.0672 0.7044 0.033 Uiso 1 1 calc R . . H27B H 0.1673 0.0442 0.6953 0.033 Uiso 1 1 calc R . . C28 C 0.0362(2) 0.03497(16) 0.59782(17) 0.0382(7) Uani 1 1 d . . . H28A H 0.0680 0.0337 0.5671 0.057 Uiso 1 1 calc R . . H28B H -0.0246 0.0638 0.5723 0.057 Uiso 1 1 calc R . . H28C H 0.0212 -0.0160 0.6061 0.057 Uiso 1 1 calc R . . C29 C 0.21367(17) 0.64037(13) 0.53545(13) 0.0199(5) Uani 1 1 d . . . H29 H 0.1785 0.6120 0.4912 0.024 Uiso 1 1 calc R . . C30 C 0.21122(17) 0.71711(13) 0.53126(13) 0.0207(5) Uani 1 1 d . . . H30 H 0.1760 0.7414 0.4845 0.025 Uiso 1 1 calc R . . C31 C 0.26081(17) 0.75867(13) 0.59617(13) 0.0189(5) Uani 1 1 d . . . C32 C 0.31542(17) 0.72193(13) 0.66333(13) 0.0182(5) Uani 1 1 d . . . H32 H 0.3508 0.7492 0.7083 0.022 Uiso 1 1 calc R . . C33 C 0.31741(16) 0.64488(13) 0.66366(12) 0.0165(5) Uani 1 1 d . . . C34 C 0.37525(16) 0.59876(13) 0.73025(12) 0.0167(5) Uani 1 1 d . . . C35 C 0.45265(17) 0.62428(13) 0.79632(13) 0.0188(5) Uani 1 1 d . . . H35 H 0.4704 0.6755 0.8026 0.023 Uiso 1 1 calc R . . C36 C 0.50410(18) 0.57327(13) 0.85350(13) 0.0198(5) Uani 1 1 d . . . C37 C 0.47427(18) 0.49939(13) 0.84328(14) 0.0215(5) Uani 1 1 d . . . H37 H 0.5068 0.4643 0.8824 0.026 Uiso 1 1 calc R . . C38 C 0.39702(17) 0.47729(13) 0.77592(13) 0.0190(5) Uani 1 1 d . . . H38 H 0.3772 0.4265 0.7691 0.023 Uiso 1 1 calc R . . C39 C 0.25595(17) 0.84228(13) 0.59151(13) 0.0202(5) Uani 1 1 d . . . C40 C 0.29988(19) 0.95405(13) 0.66051(14) 0.0247(5) Uani 1 1 d . . . H40A H 0.2334 0.9747 0.6423 0.030 Uiso 1 1 calc R . . H40B H 0.3258 0.9731 0.6286 0.030 Uiso 1 1 calc R . . C41 C 0.3660(2) 0.97620(15) 0.74003(14) 0.0294(6) Uani 1 1 d . . . H41A H 0.4298 0.9519 0.7586 0.044 Uiso 1 1 calc R . . H41B H 0.3366 0.9607 0.7703 0.044 Uiso 1 1 calc R . . H41C H 0.3746 1.0305 0.7432 0.044 Uiso 1 1 calc R . . C42 C 0.59189(18) 0.60042(14) 0.92369(13) 0.0219(5) Uani 1 1 d . . . C43 C 0.7361(2) 0.56235(17) 1.03391(15) 0.0352(7) Uani 1 1 d . . . H43A H 0.7655 0.6067 1.0240 0.042 Uiso 1 1 calc R . . H43B H 0.7823 0.5201 1.0463 0.042 Uiso 1 1 calc R . . C44 C 0.7200(3) 0.5779(2) 1.09802(17) 0.0501(8) Uani 1 1 d . . . H44A H 0.6875 0.5350 1.1061 0.075 Uiso 1 1 calc R . . H44B H 0.6786 0.6222 1.0873 0.075 Uiso 1 1 calc R . . H44C H 0.7832 0.5866 1.1428 0.075 Uiso 1 1 calc R . . B1 B -0.0811(2) 0.73311(17) 0.68343(17) 0.0254(6) Uani 1 1 d . . . H1 H -0.0953 0.7822 0.6992 0.030 Uiso 1 1 d R . . O1S O 0.1592(2) 0.90076(16) 0.73882(18) 0.0747(8) Uani 1 1 d . . . H1S H 0.1025 0.9009 0.7335 0.112 Uiso 1 1 d R . . C1S C 0.2039(3) 0.8309(2) 0.7677(2) 0.0540(9) Uani 1 1 d . . . H1SA H 0.2149 0.8251 0.8185 0.065 Uiso 1 1 d R . . H1SB H 0.1611 0.7907 0.7363 0.065 Uiso 1 1 d R . . H1SC H 0.2667 0.8285 0.7684 0.065 Uiso 1 1 d R . . Cl1 Cl 0.53484(4) 0.77843(3) 0.68865(3) 0.02251(13) Uani 1 1 d . . . O9 O 0.46243(13) 0.82469(10) 0.63056(10) 0.0301(4) Uani 1 1 d . . . O10 O 0.51957(15) 0.70179(10) 0.66531(12) 0.0372(5) Uani 1 1 d . . . O11 O 0.52602(13) 0.78681(11) 0.75462(10) 0.0317(4) Uani 1 1 d . . . O12 O 0.63122(13) 0.80275(10) 0.70466(10) 0.0280(4) 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 Co1 0.01441(16) 0.01234(16) 0.01649(16) -0.00221(11) 0.00778(13) -0.00032(12) Fe1 0.01485(17) 0.01469(17) 0.01577(17) -0.00112(12) 0.00764(13) 0.00116(12) O1 0.0396(11) 0.0242(10) 0.0527(12) 0.0074(9) 0.0371(10) 0.0038(8) O2 0.0277(9) 0.0193(9) 0.0322(10) 0.0010(7) 0.0206(8) 0.0029(7) O3 0.0384(11) 0.0149(9) 0.0489(12) 0.0014(8) 0.0305(10) 0.0004(8) O4 0.0271(9) 0.0152(8) 0.0368(10) 0.0004(7) 0.0209(8) -0.0031(7) O5 0.0449(11) 0.0177(9) 0.0213(9) 0.0033(7) 0.0078(8) 0.0007(8) O6 0.0265(9) 0.0133(8) 0.0200(8) 0.0004(6) 0.0095(7) 0.0009(7) O7 0.0259(9) 0.0181(9) 0.0241(9) -0.0008(7) 0.0105(7) -0.0039(7) O8 0.0311(10) 0.0225(10) 0.0242(9) 0.0013(7) 0.0040(8) 0.0007(8) N1 0.0178(10) 0.0138(10) 0.0200(10) -0.0018(8) 0.0084(8) -0.0004(8) N2 0.0174(9) 0.0170(10) 0.0207(11) -0.0031(8) 0.0089(9) -0.0013(8) N3 0.0466(16) 0.0329(15) 0.077(2) 0.0249(14) 0.0363(15) 0.0076(12) N4 0.0156(9) 0.0181(10) 0.0220(10) -0.0014(8) 0.0084(8) 0.0014(8) N5 0.0211(10) 0.0151(10) 0.0304(11) -0.0033(8) 0.0097(9) 0.0003(8) N6 0.0178(10) 0.0280(11) 0.0180(10) -0.0026(8) 0.0091(8) 0.0000(8) N7 0.0207(10) 0.0279(11) 0.0233(11) -0.0105(9) 0.0114(9) -0.0027(9) N8 0.0207(10) 0.0186(10) 0.0194(10) -0.0033(8) 0.0100(8) 0.0008(8) N9 0.0180(10) 0.0242(11) 0.0256(11) -0.0075(9) 0.0112(9) 0.0019(8) N10 0.0179(9) 0.0138(10) 0.0150(9) -0.0004(7) 0.0077(8) -0.0005(8) N11 0.0146(9) 0.0139(9) 0.0182(9) -0.0022(7) 0.0074(8) 0.0001(7) N12 0.0163(9) 0.0157(10) 0.0184(10) -0.0020(8) 0.0098(8) 0.0001(8) N13 0.0168(9) 0.0120(9) 0.0196(10) -0.0016(7) 0.0115(8) -0.0009(7) C1 0.0190(12) 0.0121(11) 0.0145(11) -0.0021(8) 0.0070(9) -0.0024(9) C2 0.0175(11) 0.0130(11) 0.0245(13) 0.0013(9) 0.0131(10) 0.0022(9) C3 0.0218(13) 0.0281(15) 0.0321(14) 0.0047(11) 0.0154(11) 0.0033(11) C4 0.0220(12) 0.0270(14) 0.0233(12) 0.0047(10) 0.0092(10) 0.0000(10) C5 0.0280(14) 0.0283(15) 0.0348(15) 0.0106(12) 0.0100(12) -0.0026(11) C6 0.0242(13) 0.0155(13) 0.0444(16) 0.0048(11) 0.0083(12) -0.0005(10) C7 0.0213(12) 0.0402(16) 0.0202(12) 0.0013(11) 0.0096(11) 0.0017(11) C8 0.0263(14) 0.0525(18) 0.0192(13) -0.0077(12) 0.0099(11) -0.0055(13) C9 0.0225(13) 0.0440(17) 0.0275(14) -0.0162(12) 0.0134(11) -0.0071(12) C10 0.0204(12) 0.0255(13) 0.0242(13) -0.0040(10) 0.0111(10) -0.0044(10) C11 0.0165(12) 0.0345(15) 0.0293(13) -0.0036(11) 0.0123(11) -0.0005(11) C12 0.0193(12) 0.0339(15) 0.0300(14) -0.0068(11) 0.0131(11) 0.0054(11) C13 0.0208(12) 0.0145(11) 0.0182(11) 0.0014(9) 0.0096(10) -0.0012(9) C14 0.0196(11) 0.0177(12) 0.0194(11) 0.0018(9) 0.0105(10) -0.0020(9) C15 0.0185(11) 0.0205(12) 0.0158(11) 0.0018(9) 0.0077(9) 0.0023(9) C16 0.0200(11) 0.0159(11) 0.0186(11) 0.0015(9) 0.0091(10) 0.0010(9) C17 0.0173(11) 0.0150(11) 0.0162(11) 0.0000(9) 0.0074(9) -0.0006(9) C18 0.0167(11) 0.0160(12) 0.0169(11) 0.0005(9) 0.0075(9) 0.0017(9) C19 0.0177(11) 0.0160(12) 0.0204(12) -0.0004(9) 0.0092(10) 0.0014(9) C20 0.0192(11) 0.0155(12) 0.0206(12) 0.0008(9) 0.0085(10) 0.0004(9) C21 0.0173(11) 0.0198(12) 0.0225(12) 0.0012(9) 0.0102(10) -0.0013(9) C22 0.0183(11) 0.0189(12) 0.0215(12) -0.0022(9) 0.0115(10) 0.0014(9) C23 0.0222(12) 0.0218(13) 0.0209(12) 0.0025(10) 0.0107(10) 0.0038(10) C24 0.0278(13) 0.0260(13) 0.0331(14) -0.0006(11) 0.0210(12) 0.0046(11) C25 0.0376(16) 0.0272(15) 0.0457(17) 0.0016(12) 0.0280(14) 0.0041(12) C26 0.0244(12) 0.0165(12) 0.0255(13) 0.0010(10) 0.0133(11) -0.0005(10) C27 0.0353(15) 0.0170(13) 0.0375(15) 0.0018(11) 0.0234(13) -0.0032(11) C28 0.0413(17) 0.0246(15) 0.0462(17) -0.0019(13) 0.0196(14) -0.0089(13) C29 0.0232(12) 0.0184(12) 0.0176(11) -0.0008(9) 0.0096(10) 0.0006(10) C30 0.0222(12) 0.0207(12) 0.0176(12) 0.0017(9) 0.0086(10) 0.0001(10) C31 0.0190(11) 0.0165(12) 0.0226(12) 0.0000(9) 0.0112(10) -0.0002(9) C32 0.0177(11) 0.0168(12) 0.0191(11) -0.0010(9) 0.0083(9) -0.0010(9) C33 0.0156(11) 0.0155(11) 0.0199(11) -0.0010(9) 0.0098(9) -0.0013(9) C34 0.0177(11) 0.0148(11) 0.0197(11) -0.0008(9) 0.0109(10) 0.0005(9) C35 0.0230(12) 0.0121(11) 0.0211(12) -0.0003(9) 0.0106(10) -0.0004(9) C36 0.0233(12) 0.0177(12) 0.0203(12) -0.0011(9) 0.0122(10) 0.0004(10) C37 0.0265(13) 0.0158(12) 0.0234(12) 0.0036(9) 0.0132(10) 0.0013(10) C38 0.0222(12) 0.0137(11) 0.0234(12) 0.0008(9) 0.0129(10) -0.0006(9) C39 0.0190(11) 0.0183(12) 0.0208(12) 0.0015(10) 0.0079(10) 0.0005(10) C40 0.0312(14) 0.0124(12) 0.0263(13) 0.0003(10) 0.0111(11) 0.0002(10) C41 0.0338(15) 0.0248(13) 0.0252(13) -0.0021(11) 0.0110(12) -0.0005(11) C42 0.0240(12) 0.0211(13) 0.0215(12) 0.0022(10) 0.0119(10) 0.0024(10) C43 0.0298(15) 0.0336(16) 0.0282(14) 0.0008(12) 0.0035(12) -0.0014(12) C44 0.050(2) 0.056(2) 0.0319(16) -0.0036(15) 0.0106(15) -0.0029(16) B1 0.0197(14) 0.0227(15) 0.0322(16) -0.0114(12) 0.0115(12) 0.0004(11) O1S 0.095(2) 0.0593(18) 0.097(2) 0.0197(16) 0.068(2) 0.0137(16) C1S 0.048(2) 0.057(2) 0.065(2) 0.0194(18) 0.0341(18) 0.0055(17) Cl1 0.0212(3) 0.0199(3) 0.0262(3) -0.0032(2) 0.0115(2) -0.0006(2) O9 0.0270(10) 0.0282(10) 0.0298(10) 0.0026(8) 0.0100(8) 0.0017(8) O10 0.0368(11) 0.0204(10) 0.0566(13) -0.0079(9) 0.0247(10) -0.0018(8) O11 0.0236(9) 0.0466(12) 0.0253(9) -0.0036(8) 0.0123(8) -0.0030(8) O12 0.0239(9) 0.0249(10) 0.0385(10) -0.0049(8) 0.0179(8) -0.0014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.877(2) 3_566 ? Co1 N1 1.884(2) . ? Co1 N11 1.9263(19) . ? Co1 N10 1.9311(19) . ? Co1 N13 1.9340(19) . ? Co1 N12 1.9363(19) . ? Fe1 C1 1.852(2) . ? Fe1 C2 1.852(2) . ? Fe1 C3 1.908(3) . ? Fe1 N6 1.996(2) . ? Fe1 N8 2.001(2) . ? Fe1 N4 2.010(2) . ? O1 C23 1.204(3) . ? O2 C23 1.324(3) . ? O2 C24 1.468(3) . ? O3 C26 1.204(3) . ? O4 C26 1.328(3) . ? O4 C27 1.465(3) . ? O5 C39 1.199(3) . ? O6 C39 1.323(3) . ? O6 C40 1.458(3) . ? O7 C42 1.201(3) . ? O8 C42 1.326(3) . ? O8 C43 1.472(3) . ? N1 C1 1.161(3) . ? N2 C2 1.159(3) . ? N2 Co1 1.877(2) 3_566 ? N3 C3 1.155(4) . ? N4 C4 1.332(3) . ? N4 N5 1.358(3) . ? N5 C6 1.354(3) . ? N5 B1 1.532(4) . ? N6 C7 1.333(3) . ? N6 N7 1.361(3) . ? N7 C9 1.344(3) . ? N7 B1 1.541(4) . ? N8 C10 1.335(3) . ? N8 N9 1.365(3) . ? N9 C12 1.349(3) . ? N9 B1 1.545(3) . ? N10 C13 1.339(3) . ? N10 C17 1.354(3) . ? N11 C22 1.341(3) . ? N11 C18 1.357(3) . ? N12 C29 1.339(3) . ? N12 C33 1.353(3) . ? N13 C38 1.337(3) . ? N13 C34 1.363(3) . ? C4 C5 1.396(4) . ? C4 H4 0.9500 . ? C5 C6 1.361(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.393(4) . ? C7 H7 0.9500 . ? C8 C9 1.382(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 C12 1.369(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(3) . ? C14 H14 0.9500 . ? C15 C16 1.392(3) . ? C15 C23 1.502(3) . ? C16 C17 1.386(3) . ? C16 H16 0.9500 . ? C17 C18 1.471(3) . ? C18 C19 1.385(3) . ? C19 C20 1.386(3) . ? C19 H19 0.9500 . ? C20 C21 1.390(3) . ? C20 C26 1.505(3) . ? C21 C22 1.380(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C24 C25 1.507(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.502(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.378(3) . ? C29 H29 0.9500 . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 C39 1.501(3) . ? C32 C33 1.382(3) . ? C32 H32 0.9500 . ? C33 C34 1.473(3) . ? C34 C35 1.383(3) . ? C35 C36 1.394(3) . ? C35 H35 0.9500 . ? C36 C37 1.386(3) . ? C36 C42 1.506(3) . ? C37 C38 1.378(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 C41 1.501(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C43 C44 1.490(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? B1 H1 1.0001 . ? O1S C1S 1.416(4) . ? O1S H1S 0.8400 . ? C1S H1SA 0.9799 . ? C1S H1SB 0.9801 . ? C1S H1SC 0.9800 . ? Cl1 O10 1.4363(19) . ? Cl1 O9 1.4405(19) . ? Cl1 O11 1.4425(19) . ? Cl1 O12 1.4456(18) . ? 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 N1 91.59(8) 3_566 . ? N2 Co1 N11 86.54(8) 3_566 . ? N1 Co1 N11 92.85(8) . . ? N2 Co1 N10 88.45(8) 3_566 . ? N1 Co1 N10 176.29(8) . . ? N11 Co1 N10 83.45(8) . . ? N2 Co1 N13 175.68(8) 3_566 . ? N1 Co1 N13 90.55(8) . . ? N11 Co1 N13 97.10(8) . . ? N10 Co1 N13 89.65(8) . . ? N2 Co1 N12 92.85(8) 3_566 . ? N1 Co1 N12 86.33(8) . . ? N11 Co1 N12 178.97(8) . . ? N10 Co1 N12 97.37(8) . . ? N13 Co1 N12 83.54(8) . . ? C1 Fe1 C2 90.80(10) . . ? C1 Fe1 C3 88.35(10) . . ? C2 Fe1 C3 89.03(11) . . ? C1 Fe1 N6 92.13(9) . . ? C2 Fe1 N6 176.61(9) . . ? C3 Fe1 N6 92.75(10) . . ? C1 Fe1 N8 178.75(9) . . ? C2 Fe1 N8 90.30(9) . . ? C3 Fe1 N8 92.25(10) . . ? N6 Fe1 N8 86.74(8) . . ? C1 Fe1 N4 90.69(9) . . ? C2 Fe1 N4 90.77(9) . . ? C3 Fe1 N4 179.02(10) . . ? N6 Fe1 N4 87.50(8) . . ? N8 Fe1 N4 88.72(8) . . ? C23 O2 C24 115.23(19) . . ? C26 O4 C27 117.39(19) . . ? C39 O6 C40 115.75(18) . . ? C42 O8 C43 116.9(2) . . ? C1 N1 Co1 166.37(18) . . ? C2 N2 Co1 166.63(19) . 3_566 ? C4 N4 N5 106.8(2) . . ? C4 N4 Fe1 132.81(17) . . ? N5 N4 Fe1 120.14(15) . . ? C6 N5 N4 109.0(2) . . ? C6 N5 B1 132.5(2) . . ? N4 N5 B1 118.3(2) . . ? C7 N6 N7 106.4(2) . . ? C7 N6 Fe1 133.63(18) . . ? N7 N6 Fe1 119.99(15) . . ? C9 N7 N6 110.2(2) . . ? C9 N7 B1 131.2(2) . . ? N6 N7 B1 118.60(19) . . ? C10 N8 N9 106.61(19) . . ? C10 N8 Fe1 134.36(17) . . ? N9 N8 Fe1 119.02(15) . . ? C12 N9 N8 109.4(2) . . ? C12 N9 B1 131.1(2) . . ? N8 N9 B1 119.31(19) . . ? C13 N10 C17 119.8(2) . . ? C13 N10 Co1 126.17(16) . . ? C17 N10 Co1 113.97(15) . . ? C22 N11 C18 120.1(2) . . ? C22 N11 Co1 125.66(16) . . ? C18 N11 Co1 113.68(15) . . ? C29 N12 C33 119.8(2) . . ? C29 N12 Co1 125.78(16) . . ? C33 N12 Co1 113.02(15) . . ? C38 N13 C34 119.3(2) . . ? C38 N13 Co1 126.71(16) . . ? C34 N13 Co1 113.84(15) . . ? N1 C1 Fe1 177.4(2) . . ? N2 C2 Fe1 177.8(2) . . ? N3 C3 Fe1 176.5(3) . . ? N4 C4 C5 110.4(2) . . ? N4 C4 H4 124.8 . . ? C5 C4 H4 124.8 . . ? C6 C5 C4 104.8(2) . . ? C6 C5 H5 127.6 . . ? C4 C5 H5 127.6 . . ? N5 C6 C5 109.0(2) . . ? N5 C6 H6 125.5 . . ? C5 C6 H6 125.5 . . ? N6 C7 C8 110.5(3) . . ? N6 C7 H7 124.7 . . ? C8 C7 H7 124.7 . . ? C9 C8 C7 104.9(2) . . ? C9 C8 H8 127.5 . . ? C7 C8 H8 127.5 . . ? N7 C9 C8 108.0(2) . . ? N7 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? N8 C10 C11 110.2(2) . . ? N8 C10 H10 124.9 . . ? C11 C10 H10 124.9 . . ? C12 C11 C10 105.1(2) . . ? C12 C11 H11 127.4 . . ? C10 C11 H11 127.4 . . ? N9 C12 C11 108.6(2) . . ? N9 C12 H12 125.7 . . ? C11 C12 H12 125.7 . . ? N10 C13 C14 121.5(2) . . ? N10 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 119.1(2) . . ? C14 C15 C23 118.3(2) . . ? C16 C15 C23 122.6(2) . . ? C17 C16 C15 118.7(2) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? N10 C17 C16 121.4(2) . . ? N10 C17 C18 113.8(2) . . ? C16 C17 C18 124.8(2) . . ? N11 C18 C19 121.2(2) . . ? N11 C18 C17 113.8(2) . . ? C19 C18 C17 124.9(2) . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C19 C20 C21 119.6(2) . . ? C19 C20 C26 118.4(2) . . ? C21 C20 C26 122.0(2) . . ? C22 C21 C20 119.1(2) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N11 C22 C21 121.3(2) . . ? N11 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? O1 C23 O2 125.1(2) . . ? O1 C23 C15 122.5(2) . . ? O2 C23 C15 112.4(2) . . ? O2 C24 C25 107.2(2) . . ? O2 C24 H24A 110.3 . . ? C25 C24 H24A 110.3 . . ? O2 C24 H24B 110.3 . . ? C25 C24 H24B 110.3 . . ? H24A C24 H24B 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O3 C26 O4 126.1(2) . . ? O3 C26 C20 123.2(2) . . ? O4 C26 C20 110.7(2) . . ? O4 C27 C28 110.7(2) . . ? O4 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C29 C30 121.4(2) . . ? N12 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C31 119.3(2) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 119.2(2) . . ? C32 C31 C39 121.7(2) . . ? C30 C31 C39 119.1(2) . . ? C33 C32 C31 118.8(2) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? N12 C33 C32 121.5(2) . . ? N12 C33 C34 113.9(2) . . ? C32 C33 C34 124.6(2) . . ? N13 C34 C35 121.6(2) . . ? N13 C34 C33 113.36(19) . . ? C35 C34 C33 125.0(2) . . ? C34 C35 C36 118.6(2) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C37 C36 C35 119.1(2) . . ? C37 C36 C42 122.4(2) . . ? C35 C36 C42 118.5(2) . . ? C38 C37 C36 119.4(2) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? N13 C38 C37 121.8(2) . . ? N13 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? O5 C39 O6 125.7(2) . . ? O5 C39 C31 123.1(2) . . ? O6 C39 C31 111.22(19) . . ? O6 C40 C41 106.9(2) . . ? O6 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? O6 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O7 C42 O8 125.5(2) . . ? O7 C42 C36 123.1(2) . . ? O8 C42 C36 111.4(2) . . ? O8 C43 C44 110.5(3) . . ? O8 C43 H43A 109.6 . . ? C44 C43 H43A 109.6 . . ? O8 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 B1 N7 106.6(2) . . ? N5 B1 N9 108.2(2) . . ? N7 B1 N9 107.0(2) . . ? N5 B1 H1 111.6 . . ? N7 B1 H1 111.6 . . ? N9 B1 H1 111.6 . . ? C1S O1S H1S 109.3 . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 109.6 . . ? H1SA C1S H1SB 109.5 . . ? O1S C1S H1SC 109.3 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O10 Cl1 O9 109.77(12) . . ? O10 Cl1 O11 109.79(12) . . ? O9 Cl1 O11 108.89(11) . . ? O10 Cl1 O12 110.38(11) . . ? O9 Cl1 O12 108.88(11) . . ? O11 Cl1 O12 109.10(11) . . ? 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 N1 C1 -5.3(8) 3_566 . . . ? N11 Co1 N1 C1 -91.9(8) . . . . ? N10 Co1 N1 C1 -96.0(14) . . . . ? N13 Co1 N1 C1 170.9(8) . . . . ? N12 Co1 N1 C1 87.4(8) . . . . ? C1 Fe1 N4 C4 38.2(2) . . . . ? C2 Fe1 N4 C4 -52.7(2) . . . . ? C3 Fe1 N4 C4 26(6) . . . . ? N6 Fe1 N4 C4 130.3(2) . . . . ? N8 Fe1 N4 C4 -142.9(2) . . . . ? C1 Fe1 N4 N5 -135.00(17) . . . . ? C2 Fe1 N4 N5 134.18(17) . . . . ? C3 Fe1 N4 N5 -147(6) . . . . ? N6 Fe1 N4 N5 -42.90(17) . . . . ? N8 Fe1 N4 N5 43.90(17) . . . . ? C4 N4 N5 C6 -0.9(3) . . . . ? Fe1 N4 N5 C6 173.90(16) . . . . ? C4 N4 N5 B1 -176.3(2) . . . . ? Fe1 N4 N5 B1 -1.5(3) . . . . ? C1 Fe1 N6 C7 -46.5(2) . . . . ? C2 Fe1 N6 C7 163.5(15) . . . . ? C3 Fe1 N6 C7 41.9(2) . . . . ? N8 Fe1 N6 C7 134.0(2) . . . . ? N4 Fe1 N6 C7 -137.1(2) . . . . ? C1 Fe1 N6 N7 133.31(18) . . . . ? C2 Fe1 N6 N7 -16.6(17) . . . . ? C3 Fe1 N6 N7 -138.24(18) . . . . ? N8 Fe1 N6 N7 -46.15(17) . . . . ? N4 Fe1 N6 N7 42.71(17) . . . . ? C7 N6 N7 C9 0.2(3) . . . . ? Fe1 N6 N7 C9 -179.64(17) . . . . ? C7 N6 N7 B1 -178.8(2) . . . . ? Fe1 N6 N7 B1 1.3(3) . . . . ? C1 Fe1 N8 C10 -158(4) . . . . ? C2 Fe1 N8 C10 49.6(2) . . . . ? C3 Fe1 N8 C10 -39.4(2) . . . . ? N6 Fe1 N8 C10 -132.0(2) . . . . ? N4 Fe1 N8 C10 140.4(2) . . . . ? C1 Fe1 N8 N9 21(4) . . . . ? C2 Fe1 N8 N9 -131.45(17) . . . . ? C3 Fe1 N8 N9 139.50(18) . . . . ? N6 Fe1 N8 N9 46.88(17) . . . . ? N4 Fe1 N8 N9 -40.69(17) . . . . ? C10 N8 N9 C12 0.4(3) . . . . ? Fe1 N8 N9 C12 -178.73(16) . . . . ? C10 N8 N9 B1 175.9(2) . . . . ? Fe1 N8 N9 B1 -3.3(3) . . . . ? N2 Co1 N10 C13 99.51(19) 3_566 . . . ? N1 Co1 N10 C13 -169.7(12) . . . . ? N11 Co1 N10 C13 -173.80(19) . . . . ? N13 Co1 N10 C13 -76.61(19) . . . . ? N12 Co1 N10 C13 6.83(19) . . . . ? N2 Co1 N10 C17 -78.78(16) 3_566 . . . ? N1 Co1 N10 C17 12.0(13) . . . . ? N11 Co1 N10 C17 7.91(15) . . . . ? N13 Co1 N10 C17 105.10(16) . . . . ? N12 Co1 N10 C17 -171.46(15) . . . . ? N2 Co1 N11 C22 -92.96(19) 3_566 . . . ? N1 Co1 N11 C22 -1.53(19) . . . . ? N10 Co1 N11 C22 178.20(19) . . . . ? N13 Co1 N11 C22 89.38(19) . . . . ? N12 Co1 N11 C22 -39(4) . . . . ? N2 Co1 N11 C18 78.32(16) 3_566 . . . ? N1 Co1 N11 C18 169.74(16) . . . . ? N10 Co1 N11 C18 -10.52(15) . . . . ? N13 Co1 N11 C18 -99.35(16) . . . . ? N12 Co1 N11 C18 132(4) . . . . ? N2 Co1 N12 C29 4.0(2) 3_566 . . . ? N1 Co1 N12 C29 -87.40(19) . . . . ? N11 Co1 N12 C29 -50(4) . . . . ? N10 Co1 N12 C29 92.82(19) . . . . ? N13 Co1 N12 C29 -178.4(2) . . . . ? N2 Co1 N12 C33 170.22(16) 3_566 . . . ? N1 Co1 N12 C33 78.80(16) . . . . ? N11 Co1 N12 C33 117(4) . . . . ? N10 Co1 N12 C33 -100.97(16) . . . . ? N13 Co1 N12 C33 -12.17(15) . . . . ? N2 Co1 N13 C38 -137.5(10) 3_566 . . . ? N1 Co1 N13 C38 102.72(19) . . . . ? N11 Co1 N13 C38 9.8(2) . . . . ? N10 Co1 N13 C38 -73.58(19) . . . . ? N12 Co1 N13 C38 -171.0(2) . . . . ? N2 Co1 N13 C34 38.1(12) 3_566 . . . ? N1 Co1 N13 C34 -81.69(16) . . . . ? N11 Co1 N13 C34 -174.63(15) . . . . ? N10 Co1 N13 C34 102.01(16) . . . . ? N12 Co1 N13 C34 4.56(16) . . . . ? Co1 N1 C1 Fe1 98(4) . . . . ? C2 Fe1 C1 N1 -84(5) . . . . ? C3 Fe1 C1 N1 5(5) . . . . ? N6 Fe1 C1 N1 97(5) . . . . ? N8 Fe1 C1 N1 123(5) . . . . ? N4 Fe1 C1 N1 -175(100) . . . . ? Co1 N2 C2 Fe1 70(6) 3_566 . . . ? C1 Fe1 C2 N2 157(5) . . . . ? C3 Fe1 C2 N2 69(5) . . . . ? N6 Fe1 C2 N2 -53(6) . . . . ? N8 Fe1 C2 N2 -24(5) . . . . ? N4 Fe1 C2 N2 -112(5) . . . . ? C1 Fe1 C3 N3 -49(4) . . . . ? C2 Fe1 C3 N3 42(4) . . . . ? N6 Fe1 C3 N3 -141(4) . . . . ? N8 Fe1 C3 N3 132(4) . . . . ? N4 Fe1 C3 N3 -37(9) . . . . ? N5 N4 C4 C5 0.7(3) . . . . ? Fe1 N4 C4 C5 -173.13(18) . . . . ? N4 C4 C5 C6 -0.3(3) . . . . ? N4 N5 C6 C5 0.7(3) . . . . ? B1 N5 C6 C5 175.3(2) . . . . ? C4 C5 C6 N5 -0.3(3) . . . . ? N7 N6 C7 C8 0.2(3) . . . . ? Fe1 N6 C7 C8 -179.89(18) . . . . ? N6 C7 C8 C9 -0.6(3) . . . . ? N6 N7 C9 C8 -0.6(3) . . . . ? B1 N7 C9 C8 178.2(3) . . . . ? C7 C8 C9 N7 0.7(3) . . . . ? N9 N8 C10 C11 -0.3(3) . . . . ? Fe1 N8 C10 C11 178.73(18) . . . . ? N8 C10 C11 C12 0.0(3) . . . . ? N8 N9 C12 C11 -0.5(3) . . . . ? B1 N9 C12 C11 -175.2(3) . . . . ? C10 C11 C12 N9 0.3(3) . . . . ? C17 N10 C13 C14 -0.2(3) . . . . ? Co1 N10 C13 C14 -178.36(16) . . . . ? N10 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C13 C14 C15 C23 177.5(2) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C23 C15 C16 C17 -178.3(2) . . . . ? C13 N10 C17 C16 -0.7(3) . . . . ? Co1 N10 C17 C16 177.73(17) . . . . ? C13 N10 C17 C18 177.59(19) . . . . ? Co1 N10 C17 C18 -4.0(2) . . . . ? C15 C16 C17 N10 0.6(3) . . . . ? C15 C16 C17 C18 -177.4(2) . . . . ? C22 N11 C18 C19 0.4(3) . . . . ? Co1 N11 C18 C19 -171.42(17) . . . . ? C22 N11 C18 C17 -177.17(19) . . . . ? Co1 N11 C18 C17 11.0(2) . . . . ? N10 C17 C18 N11 -4.6(3) . . . . ? C16 C17 C18 N11 173.6(2) . . . . ? N10 C17 C18 C19 177.9(2) . . . . ? C16 C17 C18 C19 -3.9(4) . . . . ? N11 C18 C19 C20 -0.9(3) . . . . ? C17 C18 C19 C20 176.4(2) . . . . ? C18 C19 C20 C21 0.0(3) . . . . ? C18 C19 C20 C26 -177.6(2) . . . . ? C19 C20 C21 C22 1.3(3) . . . . ? C26 C20 C21 C22 178.8(2) . . . . ? C18 N11 C22 C21 1.0(3) . . . . ? Co1 N11 C22 C21 171.74(17) . . . . ? C20 C21 C22 N11 -1.8(3) . . . . ? C24 O2 C23 O1 -3.2(4) . . . . ? C24 O2 C23 C15 176.44(19) . . . . ? C14 C15 C23 O1 -8.9(4) . . . . ? C16 C15 C23 O1 169.7(2) . . . . ? C14 C15 C23 O2 171.5(2) . . . . ? C16 C15 C23 O2 -10.0(3) . . . . ? C23 O2 C24 C25 -172.9(2) . . . . ? C27 O4 C26 O3 3.1(4) . . . . ? C27 O4 C26 C20 -175.8(2) . . . . ? C19 C20 C26 O3 3.9(4) . . . . ? C21 C20 C26 O3 -173.7(2) . . . . ? C19 C20 C26 O4 -177.2(2) . . . . ? C21 C20 C26 O4 5.2(3) . . . . ? C26 O4 C27 C28 -82.5(3) . . . . ? C33 N12 C29 C30 -2.1(3) . . . . ? Co1 N12 C29 C30 163.28(18) . . . . ? N12 C29 C30 C31 -1.5(4) . . . . ? C29 C30 C31 C32 3.0(4) . . . . ? C29 C30 C31 C39 -178.6(2) . . . . ? C30 C31 C32 C33 -1.1(3) . . . . ? C39 C31 C32 C33 -179.5(2) . . . . ? C29 N12 C33 C32 4.1(3) . . . . ? Co1 N12 C33 C32 -163.04(18) . . . . ? C29 N12 C33 C34 -175.8(2) . . . . ? Co1 N12 C33 C34 17.0(2) . . . . ? C31 C32 C33 N12 -2.5(3) . . . . ? C31 C32 C33 C34 177.4(2) . . . . ? C38 N13 C34 C35 2.8(3) . . . . ? Co1 N13 C34 C35 -173.15(17) . . . . ? C38 N13 C34 C33 179.25(19) . . . . ? Co1 N13 C34 C33 3.3(2) . . . . ? N12 C33 C34 N13 -13.5(3) . . . . ? C32 C33 C34 N13 166.6(2) . . . . ? N12 C33 C34 C35 162.9(2) . . . . ? C32 C33 C34 C35 -17.1(4) . . . . ? N13 C34 C35 C36 -0.6(3) . . . . ? C33 C34 C35 C36 -176.6(2) . . . . ? C34 C35 C36 C37 -2.1(3) . . . . ? C34 C35 C36 C42 176.5(2) . . . . ? C35 C36 C37 C38 2.6(4) . . . . ? C42 C36 C37 C38 -175.9(2) . . . . ? C34 N13 C38 C37 -2.3(3) . . . . ? Co1 N13 C38 C37 173.10(18) . . . . ? C36 C37 C38 N13 -0.4(4) . . . . ? C40 O6 C39 O5 -2.9(4) . . . . ? C40 O6 C39 C31 177.3(2) . . . . ? C32 C31 C39 O5 170.8(2) . . . . ? C30 C31 C39 O5 -7.6(4) . . . . ? C32 C31 C39 O6 -9.4(3) . . . . ? C30 C31 C39 O6 172.2(2) . . . . ? C39 O6 C40 C41 -168.5(2) . . . . ? C43 O8 C42 O7 -4.5(4) . . . . ? C43 O8 C42 C36 173.9(2) . . . . ? C37 C36 C42 O7 -172.0(2) . . . . ? C35 C36 C42 O7 9.4(4) . . . . ? C37 C36 C42 O8 9.5(3) . . . . ? C35 C36 C42 O8 -169.0(2) . . . . ? C42 O8 C43 C44 89.3(3) . . . . ? C6 N5 B1 N7 -115.2(3) . . . . ? N4 N5 B1 N7 59.0(3) . . . . ? C6 N5 B1 N9 130.0(3) . . . . ? N4 N5 B1 N9 -55.8(3) . . . . ? C9 N7 B1 N5 122.1(3) . . . . ? N6 N7 B1 N5 -59.2(3) . . . . ? C9 N7 B1 N9 -122.4(3) . . . . ? N6 N7 B1 N9 56.4(3) . . . . ? C12 N9 B1 N5 -126.6(3) . . . . ? N8 N9 B1 N5 59.2(3) . . . . ? C12 N9 B1 N7 118.9(3) . . . . ? N8 N9 B1 N7 -55.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.020 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.064 _database_code_depnum_ccdc_archive 'CCDC 967846' ####################################################################### # # 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_1.2MeOH' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H92 B2 Cl2 Co2 Fe2 N26 O26' _chemical_formula_weight 2275.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 15.698(3) _cell_length_b 17.923(4) _cell_length_c 20.679(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.442(11) _cell_angle_gamma 90.00 _cell_volume 5066.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.54 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7811 _exptl_absorpt_correction_T_max 0.9430 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35078 _diffrn_reflns_av_R_equivalents 0.1302 _diffrn_reflns_av_sigmaI/netI 0.1127 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8852 _reflns_number_gt 5045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0532P)^2^+137.3994P] 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 8852 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2181 _refine_ls_R_factor_gt 0.1286 _refine_ls_wR_factor_ref 0.3149 _refine_ls_wR_factor_gt 0.2786 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.24897(10) 0.50134(8) 0.61958(8) 0.0229(4) Uani 1 1 d . . . Fe1 Fe -0.03774(11) 0.57886(9) 0.63480(8) 0.0242(4) Uani 1 1 d . . . O1 O 0.5958(7) 0.3870(5) 0.5282(5) 0.043(2) Uani 1 1 d . . . O2 O 0.5550(5) 0.2786(4) 0.5590(4) 0.0302(18) Uani 1 1 d . . . O3 O 0.2350(6) 0.1198(5) 0.6286(5) 0.041(2) Uani 1 1 d . . . O4 O 0.1203(5) 0.1491(4) 0.6614(4) 0.0307(19) Uani 1 1 d . . . O5 O 0.2205(6) 0.8755(4) 0.5343(4) 0.040(2) Uani 1 1 d . . . O6 O 0.2966(5) 0.8732(4) 0.6580(4) 0.0291(18) Uani 1 1 d . . . O7 O 0.6123(6) 0.6654(4) 0.9362(4) 0.0302(19) Uani 1 1 d . . . O8 O 0.6417(6) 0.5444(5) 0.9667(5) 0.043(2) Uani 1 1 d . . . N1 N 0.1505(6) 0.5341(5) 0.6390(4) 0.020(2) Uani 1 1 d . . . N2 N -0.1559(6) 0.5179(5) 0.4810(4) 0.0199(19) Uani 1 1 d . . . N3 N -0.0396(10) 0.4218(7) 0.6930(9) 0.069(4) Uani 1 1 d . . . N4 N -0.0340(6) 0.6812(5) 0.5967(5) 0.024(2) Uani 1 1 d . . . N5 N -0.0542(7) 0.7428(5) 0.6219(6) 0.035(2) Uani 1 1 d . . . N6 N 0.0347(7) 0.6228(5) 0.7363(5) 0.031(2) Uani 1 1 d . . . N7 N 0.0070(7) 0.6920(6) 0.7497(5) 0.032(2) Uani 1 1 d . . . N8 N -0.1604(7) 0.6085(5) 0.6344(5) 0.025(2) Uani 1 1 d . . . N9 N -0.1709(7) 0.6794(5) 0.6545(5) 0.034(2) Uani 1 1 d . . . N10 N 0.3486(6) 0.4619(4) 0.6012(4) 0.0183(19) Uani 1 1 d . . . N11 N 0.2317(6) 0.3986(5) 0.6379(5) 0.021(2) Uani 1 1 d . . . N12 N 0.2643(5) 0.6042(5) 0.6004(4) 0.0140(17) Uani 1 1 d . . . N13 N 0.3487(6) 0.5255(5) 0.7200(4) 0.023(2) Uani 1 1 d . . . C1 C 0.0771(8) 0.5531(5) 0.6355(6) 0.021(2) Uani 1 1 d . . . C2 C -0.1118(7) 0.5404(5) 0.5384(5) 0.014(2) Uani 1 1 d . . . C3 C -0.0380(8) 0.4819(6) 0.6729(6) 0.025(2) Uani 1 1 d . . . C4 C -0.0084(8) 0.7042(7) 0.5453(6) 0.033(3) Uani 1 1 d . . . H4 H 0.0076 0.6724 0.5161 0.039 Uiso 1 1 calc R . . C5 C -0.0098(9) 0.7816(6) 0.5430(7) 0.034(3) Uani 1 1 d . . . H5 H 0.0059 0.8128 0.5132 0.041 Uiso 1 1 calc R . . C6 C -0.0373(9) 0.8025(7) 0.5908(8) 0.048(4) Uani 1 1 d . . . H6 H -0.0443 0.8529 0.6017 0.058 Uiso 1 1 calc R . . C7 C 0.1072(8) 0.6018(7) 0.7996(6) 0.032(3) Uani 1 1 d . . . H7 H 0.1407 0.5557 0.8073 0.039 Uiso 1 1 calc R . . C8 C 0.1302(9) 0.6558(8) 0.8554(7) 0.045(3) Uani 1 1 d . . . H8 H 0.1805 0.6537 0.9058 0.053 Uiso 1 1 calc R . . C9 C 0.0627(9) 0.7125(8) 0.8203(7) 0.043(3) Uani 1 1 d . . . H9 H 0.0573 0.7575 0.8424 0.052 Uiso 1 1 calc R . . C10 C -0.2458(8) 0.5740(6) 0.6163(6) 0.030(3) Uani 1 1 d . . . H10 H -0.2613 0.5243 0.5983 0.036 Uiso 1 1 calc R . . C11 C -0.3084(9) 0.6208(7) 0.6275(7) 0.040(3) Uani 1 1 d . . . H11 H -0.3720 0.6099 0.6197 0.048 Uiso 1 1 calc R . . C12 C -0.2568(8) 0.6866(7) 0.6524(6) 0.032(3) Uani 1 1 d . . . H12 H -0.2789 0.7301 0.6660 0.039 Uiso 1 1 calc R . . C13 C 0.4105(8) 0.4995(6) 0.5872(6) 0.024(2) Uani 1 1 d . . . H13 H 0.4081 0.5525 0.5873 0.029 Uiso 1 1 calc R . . C14 C 0.4778(8) 0.4660(6) 0.5726(6) 0.021(2) Uani 1 1 d . . . H14 H 0.5222 0.4947 0.5641 0.026 Uiso 1 1 calc R . . C15 C 0.4788(8) 0.3876(6) 0.5709(6) 0.026(3) Uani 1 1 d . . . C16 C 0.4137(7) 0.3467(6) 0.5833(5) 0.023(2) Uani 1 1 d . . . H16 H 0.4128 0.2938 0.5812 0.028 Uiso 1 1 calc R . . C17 C 0.3492(7) 0.3860(6) 0.5990(5) 0.019(2) Uani 1 1 d . . . C18 C 0.2792(7) 0.3497(6) 0.6182(5) 0.017(2) Uani 1 1 d . . . C19 C 0.2650(8) 0.2738(6) 0.6171(6) 0.026(3) Uani 1 1 d . . . H19 H 0.2981 0.2404 0.6014 0.032 Uiso 1 1 calc R . . C20 C 0.2011(8) 0.2480(6) 0.6396(6) 0.025(2) Uani 1 1 d . . . C21 C 0.1514(7) 0.2972(6) 0.6601(6) 0.026(3) Uani 1 1 d . . . H21 H 0.1067 0.2797 0.6752 0.031 Uiso 1 1 calc R . . C22 C 0.1683(8) 0.3738(6) 0.6582(6) 0.026(3) Uani 1 1 d . . . H22 H 0.1340 0.4086 0.6717 0.031 Uiso 1 1 calc R . . C23 C 0.5496(7) 0.3511(7) 0.5502(6) 0.025(2) Uani 1 1 d . . . C24 C 0.6160(9) 0.2389(7) 0.5358(7) 0.034(3) Uani 1 1 d . . . H24A H 0.6855 0.2521 0.5685 0.041 Uiso 1 1 calc R . . H24B H 0.5976 0.2529 0.4842 0.041 Uiso 1 1 calc R . . C25 C 0.6017(10) 0.1571(7) 0.5402(8) 0.041(3) Uani 1 1 d . . . H25A H 0.5324 0.1447 0.5090 0.062 Uiso 1 1 calc R . . H25B H 0.6230 0.1433 0.5918 0.062 Uiso 1 1 calc R . . H25C H 0.6405 0.1295 0.5227 0.062 Uiso 1 1 calc R . . C26 C 0.1870(8) 0.1646(7) 0.6418(6) 0.028(3) Uani 1 1 d . . . C27 C 0.1048(9) 0.0699(6) 0.6710(7) 0.034(3) Uani 1 1 d . . . H27A H 0.0758 0.0655 0.7039 0.041 Uiso 1 1 calc R . . H27B H 0.1685 0.0436 0.6949 0.041 Uiso 1 1 calc R . . C28 C 0.0384(10) 0.0346(7) 0.5978(8) 0.053(4) Uani 1 1 d . . . H28A H 0.0689 0.0365 0.5663 0.079 Uiso 1 1 calc R . . H28B H -0.0239 0.0615 0.5736 0.079 Uiso 1 1 calc R . . H28C H 0.0267 -0.0176 0.6055 0.079 Uiso 1 1 calc R . . C29 C 0.2137(8) 0.6410(6) 0.5357(6) 0.026(3) Uani 1 1 d . . . H29 H 0.1792 0.6131 0.4912 0.031 Uiso 1 1 calc R . . C30 C 0.2104(8) 0.7170(6) 0.5319(6) 0.022(2) Uani 1 1 d . . . H30 H 0.1732 0.7413 0.4854 0.027 Uiso 1 1 calc R . . C31 C 0.2614(8) 0.7580(6) 0.5960(5) 0.026(3) Uani 1 1 d . . . C32 C 0.3151(7) 0.7221(6) 0.6628(6) 0.022(2) Uani 1 1 d . . . H32 H 0.3500 0.7496 0.7076 0.027 Uiso 1 1 calc R . . C33 C 0.3170(7) 0.6444(6) 0.6631(5) 0.019(2) Uani 1 1 d . . . C34 C 0.3749(8) 0.5984(6) 0.7296(6) 0.022(2) Uani 1 1 d . . . C35 C 0.4516(8) 0.6236(6) 0.7957(6) 0.024(2) Uani 1 1 d . . . H35 H 0.4680 0.6751 0.8022 0.029 Uiso 1 1 calc R . . C36 C 0.5050(8) 0.5734(6) 0.8531(6) 0.028(3) Uani 1 1 d . . . C37 C 0.4743(8) 0.4994(6) 0.8433(6) 0.028(3) Uani 1 1 d . . . H37 H 0.5058 0.4644 0.8824 0.034 Uiso 1 1 calc R . . C38 C 0.3963(7) 0.4776(6) 0.7750(6) 0.026(3) Uani 1 1 d . . . H38 H 0.3767 0.4267 0.7677 0.031 Uiso 1 1 calc R . . C39 C 0.2561(7) 0.8423(6) 0.5920(5) 0.019(2) Uani 1 1 d . . . C40 C 0.3020(9) 0.9542(6) 0.6606(6) 0.034(3) Uani 1 1 d . . . H40A H 0.2358 0.9757 0.6414 0.041 Uiso 1 1 calc R . . H40B H 0.3295 0.9726 0.6296 0.041 Uiso 1 1 calc R . . C41 C 0.3661(9) 0.9770(7) 0.7395(7) 0.040(3) Uani 1 1 d . . . H41A H 0.4305 0.9537 0.7588 0.060 Uiso 1 1 calc R . . H41B H 0.3365 0.9609 0.7693 0.060 Uiso 1 1 calc R . . H41C H 0.3734 1.0314 0.7424 0.060 Uiso 1 1 calc R . . C42 C 0.5910(8) 0.6004(7) 0.9242(6) 0.029(3) Uani 1 1 d . . . C43 C 0.7340(10) 0.5633(7) 1.0343(7) 0.045(4) Uani 1 1 d . . . H43A H 0.7809 0.5217 1.0460 0.054 Uiso 1 1 calc R . . H43B H 0.7626 0.6083 1.0245 0.054 Uiso 1 1 calc R . . C44 C 0.7207(13) 0.5772(9) 1.0987(8) 0.065(5) Uani 1 1 d . . . H44A H 0.6892 0.5339 1.1070 0.097 Uiso 1 1 calc R . . H44B H 0.6795 0.6214 1.0893 0.097 Uiso 1 1 calc R . . H44C H 0.7846 0.5857 1.1427 0.097 Uiso 1 1 calc R . . B1 B -0.0806(9) 0.7325(8) 0.6849(7) 0.031(3) Uani 1 1 d . . . H1 H -0.0948 0.7815 0.7007 0.037 Uiso 1 1 d R . . O1S O 0.1606(11) 0.9010(7) 0.7399(9) 0.100(5) Uani 1 1 d . . . H1S H 0.1039 0.9012 0.7346 0.150 Uiso 1 1 d R . . C1S C 0.2042(11) 0.8293(10) 0.7687(9) 0.063(4) Uani 1 1 d . . . H1SA H 0.2152 0.8235 0.8195 0.075 Uiso 1 1 d R . . H1SB H 0.1614 0.7891 0.7373 0.075 Uiso 1 1 d R . . H1SC H 0.2671 0.8268 0.7694 0.075 Uiso 1 1 d R . . Cl1 Cl 0.5353(2) 0.77813(16) 0.68905(16) 0.0310(7) Uani 1 1 d . . . O9 O 0.4637(6) 0.8237(5) 0.6297(5) 0.038(2) Uani 1 1 d . . . O10 O 0.5207(6) 0.7012(5) 0.6672(6) 0.047(2) Uani 1 1 d . . . O11 O 0.5259(5) 0.7862(5) 0.7540(4) 0.036(2) Uani 1 1 d . . . O12 O 0.6312(6) 0.8016(4) 0.7040(5) 0.038(2) 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 Co1 0.0160(7) 0.0196(8) 0.0234(7) -0.0026(6) 0.0024(6) 0.0002(6) Fe1 0.0182(8) 0.0231(9) 0.0232(8) -0.0013(7) 0.0039(6) 0.0008(7) O1 0.047(5) 0.028(5) 0.062(6) 0.005(4) 0.032(5) 0.006(4) O2 0.027(4) 0.018(4) 0.041(5) 0.000(3) 0.013(4) 0.007(3) O3 0.044(5) 0.022(5) 0.062(6) -0.006(4) 0.030(5) -0.006(4) O4 0.022(4) 0.023(4) 0.047(5) -0.002(4) 0.017(4) -0.004(3) O5 0.048(5) 0.022(5) 0.026(4) -0.002(4) 0.000(4) 0.001(4) O6 0.025(4) 0.021(4) 0.029(4) 0.003(3) 0.004(3) 0.004(3) O7 0.028(4) 0.023(5) 0.029(4) -0.001(3) 0.006(3) -0.005(3) O8 0.041(5) 0.023(5) 0.039(5) 0.006(4) -0.002(4) 0.002(4) N1 0.022(5) 0.011(4) 0.015(4) -0.001(3) -0.001(4) 0.001(4) N2 0.016(4) 0.029(5) 0.007(4) -0.003(4) 0.000(4) -0.002(4) N3 0.055(8) 0.048(8) 0.125(12) 0.042(8) 0.061(9) 0.022(7) N4 0.015(4) 0.016(5) 0.035(5) -0.008(4) 0.007(4) -0.003(4) N5 0.026(5) 0.017(5) 0.054(7) -0.009(5) 0.014(5) 0.000(4) N6 0.028(5) 0.033(6) 0.015(5) -0.007(4) -0.002(4) -0.004(4) N7 0.019(5) 0.040(6) 0.034(5) -0.010(5) 0.012(4) -0.005(4) N8 0.025(5) 0.021(5) 0.031(5) -0.005(4) 0.015(4) 0.002(4) N9 0.023(5) 0.024(5) 0.040(6) -0.016(4) 0.005(4) -0.011(4) N10 0.021(5) 0.009(4) 0.015(4) -0.002(3) 0.001(4) 0.001(4) N11 0.012(4) 0.017(5) 0.021(5) -0.006(4) -0.002(4) 0.004(4) N12 0.007(4) 0.018(4) 0.019(4) -0.003(3) 0.008(3) 0.003(3) N13 0.019(5) 0.020(5) 0.012(4) -0.006(3) -0.005(4) -0.009(4) C1 0.035(7) 0.006(5) 0.023(6) -0.003(4) 0.014(5) -0.006(5) C2 0.019(5) 0.011(5) 0.013(5) 0.001(4) 0.007(4) -0.008(4) C3 0.025(6) 0.026(7) 0.034(6) 0.006(5) 0.022(5) 0.001(5) C4 0.026(6) 0.031(7) 0.024(6) 0.000(5) -0.001(5) 0.003(5) C5 0.029(6) 0.019(6) 0.049(8) 0.008(6) 0.015(6) -0.001(5) C6 0.036(7) 0.017(7) 0.056(9) 0.012(6) -0.004(7) 0.003(6) C7 0.019(6) 0.053(8) 0.015(5) -0.006(5) 0.001(5) -0.001(5) C8 0.031(7) 0.062(10) 0.034(7) -0.009(7) 0.011(6) -0.003(7) C9 0.031(7) 0.055(9) 0.038(7) -0.011(6) 0.012(6) 0.003(6) C10 0.016(5) 0.024(6) 0.040(7) -0.006(5) 0.007(5) 0.002(5) C11 0.026(6) 0.039(8) 0.042(7) 0.005(6) 0.006(6) -0.001(6) C12 0.018(6) 0.043(8) 0.028(6) -0.007(5) 0.005(5) -0.006(5) C13 0.029(6) 0.017(5) 0.027(6) -0.002(5) 0.014(5) -0.005(5) C14 0.021(5) 0.013(5) 0.022(5) 0.006(4) 0.005(5) 0.000(4) C15 0.023(6) 0.022(6) 0.025(6) -0.001(5) 0.005(5) 0.004(5) C16 0.015(5) 0.025(6) 0.016(5) -0.001(4) -0.003(4) -0.005(5) C17 0.009(5) 0.027(6) 0.010(5) 0.003(4) -0.003(4) 0.001(4) C18 0.007(5) 0.021(6) 0.012(5) -0.003(4) -0.003(4) 0.001(4) C19 0.023(6) 0.017(6) 0.020(5) -0.003(4) -0.004(5) 0.001(5) C20 0.024(6) 0.020(6) 0.025(6) -0.001(5) 0.007(5) 0.002(5) C21 0.013(5) 0.026(6) 0.027(6) 0.006(5) 0.001(4) 0.002(5) C22 0.018(5) 0.020(6) 0.030(6) -0.006(5) 0.005(5) 0.003(5) C23 0.014(5) 0.034(7) 0.028(6) -0.001(5) 0.011(5) 0.000(5) C24 0.035(7) 0.033(7) 0.032(6) -0.001(5) 0.014(6) 0.006(6) C25 0.042(8) 0.029(7) 0.053(8) 0.005(6) 0.023(7) -0.001(6) C26 0.022(6) 0.031(7) 0.023(6) -0.009(5) 0.004(5) -0.005(5) C27 0.039(7) 0.020(6) 0.046(7) -0.003(5) 0.024(6) -0.002(5) C28 0.048(8) 0.016(7) 0.070(10) -0.003(6) 0.011(7) -0.005(6) C29 0.026(6) 0.031(7) 0.019(5) -0.007(5) 0.010(5) 0.002(5) C30 0.023(6) 0.013(5) 0.028(6) 0.001(4) 0.011(5) 0.005(4) C31 0.017(5) 0.032(7) 0.013(5) -0.002(5) -0.006(4) 0.001(5) C32 0.014(5) 0.017(6) 0.028(6) -0.005(4) 0.005(4) -0.001(4) C33 0.007(5) 0.028(6) 0.020(5) -0.003(4) 0.004(4) -0.005(4) C34 0.023(6) 0.010(5) 0.034(6) -0.003(4) 0.015(5) -0.001(4) C35 0.020(5) 0.014(6) 0.033(6) -0.001(5) 0.008(5) -0.003(4) C36 0.033(6) 0.018(6) 0.039(7) 0.007(5) 0.023(6) -0.001(5) C37 0.031(6) 0.012(5) 0.034(6) 0.002(5) 0.010(5) 0.000(5) C38 0.014(5) 0.028(6) 0.030(6) 0.004(5) 0.006(5) -0.003(4) C39 0.015(5) 0.018(5) 0.012(5) 0.001(4) -0.002(4) 0.002(4) C40 0.033(7) 0.024(6) 0.029(6) 0.002(5) 0.003(5) -0.003(5) C41 0.041(7) 0.028(7) 0.043(8) -0.001(6) 0.014(6) -0.004(6) C42 0.029(6) 0.030(7) 0.024(6) 0.000(5) 0.010(5) 0.000(5) C43 0.043(8) 0.033(8) 0.035(7) -0.001(6) 0.000(6) -0.007(6) C44 0.073(11) 0.056(10) 0.049(9) 0.006(8) 0.017(8) 0.007(9) B1 0.026(7) 0.031(8) 0.022(7) -0.013(6) 0.002(6) 0.001(6) O1S 0.108(11) 0.067(9) 0.152(14) 0.006(9) 0.085(11) 0.007(8) C1S 0.049(9) 0.070(12) 0.070(11) 0.020(9) 0.031(8) 0.019(8) Cl1 0.0212(14) 0.0272(15) 0.0337(15) -0.0034(12) 0.0052(12) -0.0031(11) O9 0.035(5) 0.031(5) 0.041(5) 0.011(4) 0.012(4) 0.002(4) O10 0.040(5) 0.019(5) 0.080(7) -0.005(4) 0.027(5) -0.002(4) O11 0.020(4) 0.045(5) 0.035(5) -0.003(4) 0.006(4) 0.000(4) O12 0.026(4) 0.022(4) 0.064(6) -0.002(4) 0.021(4) 0.008(3) _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 N1 1.872(10) . ? Co1 N2 1.895(8) 3_566 ? Co1 N10 1.917(9) . ? Co1 N12 1.925(8) . ? Co1 N11 1.926(9) . ? Co1 N13 1.937(8) . ? Fe1 C1 1.854(12) . ? Fe1 C2 1.876(9) . ? Fe1 C3 1.909(11) . ? Fe1 N6 1.994(9) . ? Fe1 N8 1.995(9) . ? Fe1 N4 2.009(9) . ? O1 C23 1.212(14) . ? O2 C23 1.309(14) . ? O2 C24 1.452(14) . ? O3 C26 1.220(14) . ? O4 C26 1.325(14) . ? O4 C27 1.469(13) . ? O5 C39 1.198(12) . ? O6 C39 1.311(12) . ? O6 C40 1.454(13) . ? O7 C42 1.204(13) . ? O8 C42 1.313(14) . ? O8 C43 1.475(14) . ? N1 C1 1.169(14) . ? N2 C2 1.116(12) . ? N2 Co1 1.895(8) 3_566 ? N3 C3 1.160(15) . ? N4 N5 1.325(13) . ? N4 C4 1.372(15) . ? N5 C6 1.340(16) . ? N5 B1 1.560(18) . ? N6 C7 1.297(14) . ? N6 N7 1.386(14) . ? N7 C9 1.333(15) . ? N7 B1 1.549(16) . ? N8 C10 1.351(14) . ? N8 N9 1.372(13) . ? N9 C12 1.335(15) . ? N9 B1 1.560(16) . ? N10 C13 1.326(13) . ? N10 C17 1.362(13) . ? N11 C22 1.333(14) . ? N11 C18 1.337(13) . ? N12 C29 1.346(13) . ? N12 C33 1.353(12) . ? N13 C38 1.325(13) . ? N13 C34 1.355(13) . ? C4 C5 1.388(16) . ? C4 H4 0.9500 . ? C5 C6 1.31(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.410(17) . ? C7 H7 0.9500 . ? C8 C9 1.389(19) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.395(17) . ? C10 H10 0.9500 . ? C11 C12 1.378(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.372(15) . ? C13 H13 0.9500 . ? C14 C15 1.406(15) . ? C14 H14 0.9500 . ? C15 C16 1.380(16) . ? C15 C23 1.520(15) . ? C16 C17 1.396(15) . ? C16 H16 0.9500 . ? C17 C18 1.489(14) . ? C18 C19 1.377(15) . ? C19 C20 1.376(16) . ? C19 H19 0.9500 . ? C20 C21 1.375(16) . ? C20 C26 1.515(16) . ? C21 C22 1.404(15) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C24 C25 1.493(17) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C27 C28 1.493(17) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.364(15) . ? C29 H29 0.9500 . ? C30 C31 1.378(14) . ? C30 H30 0.9500 . ? C31 C32 1.374(14) . ? C31 C39 1.512(15) . ? C32 C33 1.393(15) . ? C32 H32 0.9500 . ? C33 C34 1.472(14) . ? C34 C35 1.381(15) . ? C35 C36 1.394(15) . ? C35 H35 0.9500 . ? C36 C37 1.390(15) . ? C36 C42 1.507(16) . ? C37 C38 1.395(15) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 C41 1.493(16) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C43 C44 1.47(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? B1 H1 1.0004 . ? O1S C1S 1.441(19) . ? O1S H1S 0.8414 . ? C1S H1SA 0.9818 . ? C1S H1SB 0.9809 . ? C1S H1SC 0.9816 . ? Cl1 O11 1.429(9) . ? Cl1 O10 1.433(9) . ? Cl1 O12 1.442(9) . ? Cl1 O9 1.443(8) . ? 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 N1 Co1 N2 91.2(4) . 3_566 ? N1 Co1 N10 176.6(4) . . ? N2 Co1 N10 88.8(4) 3_566 . ? N1 Co1 N12 86.8(3) . . ? N2 Co1 N12 93.2(4) 3_566 . ? N10 Co1 N12 96.6(3) . . ? N1 Co1 N11 92.7(4) . . ? N2 Co1 N11 86.2(4) 3_566 . ? N10 Co1 N11 83.9(4) . . ? N12 Co1 N11 179.2(4) . . ? N1 Co1 N13 91.0(4) . . ? N2 Co1 N13 176.0(4) 3_566 . ? N10 Co1 N13 89.2(4) . . ? N12 Co1 N13 83.6(3) . . ? N11 Co1 N13 97.0(4) . . ? C1 Fe1 C2 90.5(4) . . ? C1 Fe1 C3 88.3(4) . . ? C2 Fe1 C3 88.7(4) . . ? C1 Fe1 N6 92.4(4) . . ? C2 Fe1 N6 177.0(4) . . ? C3 Fe1 N6 92.3(4) . . ? C1 Fe1 N8 179.0(4) . . ? C2 Fe1 N8 90.0(4) . . ? C3 Fe1 N8 92.6(4) . . ? N6 Fe1 N8 87.1(4) . . ? C1 Fe1 N4 90.8(4) . . ? C2 Fe1 N4 92.4(4) . . ? C3 Fe1 N4 178.6(4) . . ? N6 Fe1 N4 86.6(4) . . ? N8 Fe1 N4 88.3(4) . . ? C23 O2 C24 116.7(9) . . ? C26 O4 C27 116.9(9) . . ? C39 O6 C40 116.8(8) . . ? C42 O8 C43 116.6(9) . . ? C1 N1 Co1 166.1(8) . . ? C2 N2 Co1 167.1(9) . 3_566 ? N5 N4 C4 105.8(9) . . ? N5 N4 Fe1 123.3(8) . . ? C4 N4 Fe1 130.9(8) . . ? N4 N5 C6 109.5(11) . . ? N4 N5 B1 116.3(10) . . ? C6 N5 B1 133.8(11) . . ? C7 N6 N7 105.3(9) . . ? C7 N6 Fe1 135.3(9) . . ? N7 N6 Fe1 119.4(7) . . ? C9 N7 N6 111.3(10) . . ? C9 N7 B1 130.0(11) . . ? N6 N7 B1 118.7(9) . . ? C10 N8 N9 104.9(9) . . ? C10 N8 Fe1 134.8(8) . . ? N9 N8 Fe1 120.3(7) . . ? C12 N9 N8 110.4(9) . . ? C12 N9 B1 131.2(10) . . ? N8 N9 B1 117.9(9) . . ? C13 N10 C17 118.9(9) . . ? C13 N10 Co1 127.8(7) . . ? C17 N10 Co1 113.3(7) . . ? C22 N11 C18 119.6(9) . . ? C22 N11 Co1 125.4(7) . . ? C18 N11 Co1 114.4(7) . . ? C29 N12 C33 118.3(9) . . ? C29 N12 Co1 127.0(7) . . ? C33 N12 Co1 113.1(7) . . ? C38 N13 C34 119.8(9) . . ? C38 N13 Co1 126.3(7) . . ? C34 N13 Co1 113.6(7) . . ? N1 C1 Fe1 176.3(9) . . ? N2 C2 Fe1 179.6(11) . . ? N3 C3 Fe1 177.0(12) . . ? N4 C4 C5 108.7(11) . . ? N4 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? C6 C5 C4 105.3(12) . . ? C6 C5 H5 127.3 . . ? C4 C5 H5 127.3 . . ? C5 C6 N5 110.5(12) . . ? C5 C6 H6 124.8 . . ? N5 C6 H6 124.8 . . ? N6 C7 C8 111.8(12) . . ? N6 C7 H7 124.1 . . ? C8 C7 H7 124.1 . . ? C9 C8 C7 104.6(11) . . ? C9 C8 H8 127.7 . . ? C7 C8 H8 127.7 . . ? N7 C9 C8 107.0(12) . . ? N7 C9 H9 126.5 . . ? C8 C9 H9 126.5 . . ? N8 C10 C11 111.3(10) . . ? N8 C10 H10 124.4 . . ? C11 C10 H10 124.4 . . ? C12 C11 C10 104.1(11) . . ? C12 C11 H11 128.0 . . ? C10 C11 H11 128.0 . . ? N9 C12 C11 109.2(11) . . ? N9 C12 H12 125.4 . . ? C11 C12 H12 125.4 . . ? N10 C13 C14 123.4(10) . . ? N10 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C13 C14 C15 117.6(10) . . ? C13 C14 H14 121.2 . . ? C15 C14 H14 121.2 . . ? C16 C15 C14 120.4(11) . . ? C16 C15 C23 122.4(10) . . ? C14 C15 C23 117.1(10) . . ? C15 C16 C17 117.7(10) . . ? C15 C16 H16 121.2 . . ? C17 C16 H16 121.2 . . ? N10 C17 C16 122.0(10) . . ? N10 C17 C18 114.1(9) . . ? C16 C17 C18 123.8(10) . . ? N11 C18 C19 122.8(10) . . ? N11 C18 C17 113.0(9) . . ? C19 C18 C17 124.2(10) . . ? C20 C19 C18 117.8(11) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C21 C20 C19 120.5(11) . . ? C21 C20 C26 120.6(11) . . ? C19 C20 C26 118.9(10) . . ? C20 C21 C22 118.3(11) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N11 C22 C21 121.0(10) . . ? N11 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? O1 C23 O2 124.7(11) . . ? O1 C23 C15 122.2(11) . . ? O2 C23 C15 113.2(10) . . ? O2 C24 C25 108.6(10) . . ? O2 C24 H24A 110.0 . . ? C25 C24 H24A 110.0 . . ? O2 C24 H24B 110.0 . . ? C25 C24 H24B 110.0 . . ? H24A C24 H24B 108.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O3 C26 O4 126.7(11) . . ? O3 C26 C20 121.9(11) . . ? O4 C26 C20 111.4(10) . . ? O4 C27 C28 110.6(10) . . ? O4 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C29 C30 122.3(10) . . ? N12 C29 H29 118.8 . . ? C30 C29 H29 118.8 . . ? C29 C30 C31 119.3(10) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 119.7(10) . . ? C32 C31 C39 120.9(9) . . ? C30 C31 C39 119.4(9) . . ? C31 C32 C33 118.3(10) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? N12 C33 C32 121.8(9) . . ? N12 C33 C34 113.7(9) . . ? C32 C33 C34 124.5(9) . . ? N13 C34 C35 120.9(10) . . ? N13 C34 C33 113.6(9) . . ? C35 C34 C33 125.5(9) . . ? C34 C35 C36 120.0(10) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 118.1(10) . . ? C37 C36 C42 122.0(10) . . ? C35 C36 C42 119.9(10) . . ? C36 C37 C38 119.0(10) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N13 C38 C37 122.1(10) . . ? N13 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? O5 C39 O6 125.2(10) . . ? O5 C39 C31 122.5(9) . . ? O6 C39 C31 112.3(8) . . ? O6 C40 C41 108.1(9) . . ? O6 C40 H40A 110.1 . . ? C41 C40 H40A 110.1 . . ? O6 C40 H40B 110.1 . . ? C41 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O7 C42 O8 125.9(10) . . ? O7 C42 C36 122.5(10) . . ? O8 C42 C36 111.4(10) . . ? C44 C43 O8 112.8(13) . . ? C44 C43 H43A 109.0 . . ? O8 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? O8 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 B1 N5 106.9(10) . . ? N7 B1 N9 107.9(10) . . ? N5 B1 N9 107.3(9) . . ? N7 B1 H1 112.0 . . ? N5 B1 H1 111.2 . . ? N9 B1 H1 111.3 . . ? C1S O1S H1S 108.3 . . ? O1S C1S H1SA 109.5 . . ? O1S C1S H1SB 110.5 . . ? H1SA C1S H1SB 109.5 . . ? O1S C1S H1SC 108.4 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O11 Cl1 O10 108.6(6) . . ? O11 Cl1 O12 110.4(5) . . ? O10 Cl1 O12 109.7(5) . . ? O11 Cl1 O9 110.2(5) . . ? O10 Cl1 O9 109.8(5) . . ? O12 Cl1 O9 108.1(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 N2 Co1 N1 C1 -7(3) 3_566 . . . ? N10 Co1 N1 C1 -97(7) . . . . ? N12 Co1 N1 C1 86(3) . . . . ? N11 Co1 N1 C1 -94(3) . . . . ? N13 Co1 N1 C1 169(3) . . . . ? C1 Fe1 N4 N5 -137.5(8) . . . . ? C2 Fe1 N4 N5 132.0(8) . . . . ? C3 Fe1 N4 N5 -86(18) . . . . ? N6 Fe1 N4 N5 -45.2(8) . . . . ? N8 Fe1 N4 N5 42.0(8) . . . . ? C1 Fe1 N4 C4 39.5(9) . . . . ? C2 Fe1 N4 C4 -51.0(9) . . . . ? C3 Fe1 N4 C4 91(18) . . . . ? N6 Fe1 N4 C4 131.8(9) . . . . ? N8 Fe1 N4 C4 -141.0(9) . . . . ? C4 N4 N5 C6 -3.0(12) . . . . ? Fe1 N4 N5 C6 174.6(8) . . . . ? C4 N4 N5 B1 -177.0(9) . . . . ? Fe1 N4 N5 B1 0.7(12) . . . . ? C1 Fe1 N6 C7 -47.4(13) . . . . ? C2 Fe1 N6 C7 152(7) . . . . ? C3 Fe1 N6 C7 41.0(13) . . . . ? N8 Fe1 N6 C7 133.5(13) . . . . ? N4 Fe1 N6 C7 -138.0(13) . . . . ? C1 Fe1 N6 N7 133.6(9) . . . . ? C2 Fe1 N6 N7 -27(8) . . . . ? C3 Fe1 N6 N7 -138.0(9) . . . . ? N8 Fe1 N6 N7 -45.5(8) . . . . ? N4 Fe1 N6 N7 42.9(8) . . . . ? C7 N6 N7 C9 0.4(14) . . . . ? Fe1 N6 N7 C9 179.7(9) . . . . ? C7 N6 N7 B1 -178.7(11) . . . . ? Fe1 N6 N7 B1 0.6(14) . . . . ? C1 Fe1 N8 C10 171(100) . . . . ? C2 Fe1 N8 C10 47.9(11) . . . . ? C3 Fe1 N8 C10 -40.8(11) . . . . ? N6 Fe1 N8 C10 -133.0(11) . . . . ? N4 Fe1 N8 C10 140.3(11) . . . . ? C1 Fe1 N8 N9 -7(23) . . . . ? C2 Fe1 N8 N9 -130.2(8) . . . . ? C3 Fe1 N8 N9 141.1(8) . . . . ? N6 Fe1 N8 N9 48.9(8) . . . . ? N4 Fe1 N8 N9 -37.8(8) . . . . ? C10 N8 N9 C12 3.2(12) . . . . ? Fe1 N8 N9 C12 -178.2(7) . . . . ? C10 N8 N9 B1 175.2(10) . . . . ? Fe1 N8 N9 B1 -6.1(13) . . . . ? N1 Co1 N10 C13 -172(5) . . . . ? N2 Co1 N10 C13 98.6(9) 3_566 . . . ? N12 Co1 N10 C13 5.6(9) . . . . ? N11 Co1 N10 C13 -175.0(9) . . . . ? N13 Co1 N10 C13 -77.9(9) . . . . ? N1 Co1 N10 C17 11(6) . . . . ? N2 Co1 N10 C17 -77.6(7) 3_566 . . . ? N12 Co1 N10 C17 -170.7(6) . . . . ? N11 Co1 N10 C17 8.7(7) . . . . ? N13 Co1 N10 C17 105.8(7) . . . . ? N1 Co1 N11 C22 -1.2(8) . . . . ? N2 Co1 N11 C22 -92.2(8) 3_566 . . . ? N10 Co1 N11 C22 178.6(8) . . . . ? N12 Co1 N11 C22 -50(27) . . . . ? N13 Co1 N11 C22 90.1(8) . . . . ? N1 Co1 N11 C18 169.4(7) . . . . ? N2 Co1 N11 C18 78.4(7) 3_566 . . . ? N10 Co1 N11 C18 -10.8(6) . . . . ? N12 Co1 N11 C18 121(27) . . . . ? N13 Co1 N11 C18 -99.2(7) . . . . ? N1 Co1 N12 C29 -86.2(8) . . . . ? N2 Co1 N12 C29 4.8(8) 3_566 . . . ? N10 Co1 N12 C29 93.9(8) . . . . ? N11 Co1 N12 C29 -38(27) . . . . ? N13 Co1 N12 C29 -177.6(9) . . . . ? N1 Co1 N12 C33 79.4(7) . . . . ? N2 Co1 N12 C33 170.3(7) 3_566 . . . ? N10 Co1 N12 C33 -100.5(7) . . . . ? N11 Co1 N12 C33 128(27) . . . . ? N13 Co1 N12 C33 -12.0(7) . . . . ? N1 Co1 N13 C38 103.3(9) . . . . ? N2 Co1 N13 C38 -133(5) 3_566 . . . ? N10 Co1 N13 C38 -73.3(9) . . . . ? N12 Co1 N13 C38 -170.1(10) . . . . ? N11 Co1 N13 C38 10.4(10) . . . . ? N1 Co1 N13 C34 -82.6(8) . . . . ? N2 Co1 N13 C34 41(6) 3_566 . . . ? N10 Co1 N13 C34 100.8(8) . . . . ? N12 Co1 N13 C34 4.1(8) . . . . ? N11 Co1 N13 C34 -175.4(8) . . . . ? Co1 N1 C1 Fe1 130(13) . . . . ? C2 Fe1 C1 N1 -114(14) . . . . ? C3 Fe1 C1 N1 -26(14) . . . . ? N6 Fe1 C1 N1 67(14) . . . . ? N8 Fe1 C1 N1 123(22) . . . . ? N4 Fe1 C1 N1 153(14) . . . . ? Co1 N2 C2 Fe1 -36(100) 3_566 . . . ? C1 Fe1 C2 N2 -106(100) . . . . ? C3 Fe1 C2 N2 166(100) . . . . ? N6 Fe1 C2 N2 55(100) . . . . ? N8 Fe1 C2 N2 73(100) . . . . ? N4 Fe1 C2 N2 -15(100) . . . . ? C1 Fe1 C3 N3 -76(21) . . . . ? C2 Fe1 C3 N3 15(21) . . . . ? N6 Fe1 C3 N3 -168(21) . . . . ? N8 Fe1 C3 N3 105(21) . . . . ? N4 Fe1 C3 N3 -127(22) . . . . ? N5 N4 C4 C5 2.6(12) . . . . ? Fe1 N4 C4 C5 -174.8(8) . . . . ? N4 C4 C5 C6 -1.2(13) . . . . ? C4 C5 C6 N5 -0.7(14) . . . . ? N4 N5 C6 C5 2.4(14) . . . . ? B1 N5 C6 C5 174.9(12) . . . . ? N7 N6 C7 C8 -0.9(14) . . . . ? Fe1 N6 C7 C8 -180.0(9) . . . . ? N6 C7 C8 C9 1.0(16) . . . . ? N6 N7 C9 C8 0.2(15) . . . . ? B1 N7 C9 C8 179.2(12) . . . . ? C7 C8 C9 N7 -0.7(15) . . . . ? N9 N8 C10 C11 -2.5(13) . . . . ? Fe1 N8 C10 C11 179.2(8) . . . . ? N8 C10 C11 C12 1.0(14) . . . . ? N8 N9 C12 C11 -2.7(14) . . . . ? B1 N9 C12 C11 -173.4(12) . . . . ? C10 C11 C12 N9 1.0(14) . . . . ? C17 N10 C13 C14 -2.0(15) . . . . ? Co1 N10 C13 C14 -178.1(7) . . . . ? N10 C13 C14 C15 1.6(16) . . . . ? C13 C14 C15 C16 0.2(15) . . . . ? C13 C14 C15 C23 176.5(9) . . . . ? C14 C15 C16 C17 -1.3(15) . . . . ? C23 C15 C16 C17 -177.4(9) . . . . ? C13 N10 C17 C16 0.7(14) . . . . ? Co1 N10 C17 C16 177.4(7) . . . . ? C13 N10 C17 C18 177.9(8) . . . . ? Co1 N10 C17 C18 -5.4(10) . . . . ? C15 C16 C17 N10 0.9(14) . . . . ? C15 C16 C17 C18 -176.0(9) . . . . ? C22 N11 C18 C19 0.7(14) . . . . ? Co1 N11 C18 C19 -170.5(7) . . . . ? C22 N11 C18 C17 -178.5(8) . . . . ? Co1 N11 C18 C17 10.3(10) . . . . ? N10 C17 C18 N11 -3.2(11) . . . . ? C16 C17 C18 N11 174.0(9) . . . . ? N10 C17 C18 C19 177.7(9) . . . . ? C16 C17 C18 C19 -5.2(14) . . . . ? N11 C18 C19 C20 -2.1(14) . . . . ? C17 C18 C19 C20 177.0(9) . . . . ? C18 C19 C20 C21 2.0(15) . . . . ? C18 C19 C20 C26 -177.7(9) . . . . ? C19 C20 C21 C22 -0.6(15) . . . . ? C26 C20 C21 C22 179.0(9) . . . . ? C18 N11 C22 C21 0.7(14) . . . . ? Co1 N11 C22 C21 170.9(7) . . . . ? C20 C21 C22 N11 -0.8(15) . . . . ? C24 O2 C23 O1 -4.3(16) . . . . ? C24 O2 C23 C15 176.0(9) . . . . ? C16 C15 C23 O1 168.3(11) . . . . ? C14 C15 C23 O1 -7.9(16) . . . . ? C16 C15 C23 O2 -12.0(14) . . . . ? C14 C15 C23 O2 171.8(9) . . . . ? C23 O2 C24 C25 -172.2(10) . . . . ? C27 O4 C26 O3 2.5(16) . . . . ? C27 O4 C26 C20 -175.6(9) . . . . ? C21 C20 C26 O3 -175.1(10) . . . . ? C19 C20 C26 O3 4.6(16) . . . . ? C21 C20 C26 O4 3.2(14) . . . . ? C19 C20 C26 O4 -177.2(9) . . . . ? C26 O4 C27 C28 -82.0(13) . . . . ? C33 N12 C29 C30 -3.1(15) . . . . ? Co1 N12 C29 C30 161.8(8) . . . . ? N12 C29 C30 C31 1.0(17) . . . . ? C29 C30 C31 C32 0.2(17) . . . . ? C29 C30 C31 C39 -178.8(10) . . . . ? C30 C31 C32 C33 0.8(16) . . . . ? C39 C31 C32 C33 179.8(10) . . . . ? C29 N12 C33 C32 4.2(14) . . . . ? Co1 N12 C33 C32 -162.8(8) . . . . ? C29 N12 C33 C34 -175.8(9) . . . . ? Co1 N12 C33 C34 17.2(10) . . . . ? C31 C32 C33 N12 -3.1(16) . . . . ? C31 C32 C33 C34 176.9(10) . . . . ? C38 N13 C34 C35 0.9(16) . . . . ? Co1 N13 C34 C35 -173.6(9) . . . . ? C38 N13 C34 C33 178.6(9) . . . . ? Co1 N13 C34 C33 4.1(12) . . . . ? N12 C33 C34 N13 -14.1(13) . . . . ? C32 C33 C34 N13 166.0(10) . . . . ? N12 C33 C34 C35 163.5(10) . . . . ? C32 C33 C34 C35 -16.5(17) . . . . ? N13 C34 C35 C36 1.7(17) . . . . ? C33 C34 C35 C36 -175.7(10) . . . . ? C34 C35 C36 C37 -4.5(17) . . . . ? C34 C35 C36 C42 177.7(11) . . . . ? C35 C36 C37 C38 4.6(17) . . . . ? C42 C36 C37 C38 -177.7(11) . . . . ? C34 N13 C38 C37 -0.7(17) . . . . ? Co1 N13 C38 C37 173.1(9) . . . . ? C36 C37 C38 N13 -2.1(18) . . . . ? C40 O6 C39 O5 -2.8(16) . . . . ? C40 O6 C39 C31 175.6(10) . . . . ? C32 C31 C39 O5 170.4(11) . . . . ? C30 C31 C39 O5 -10.6(17) . . . . ? C32 C31 C39 O6 -8.0(15) . . . . ? C30 C31 C39 O6 171.0(10) . . . . ? C39 O6 C40 C41 -169.6(10) . . . . ? C43 O8 C42 O7 -1.2(19) . . . . ? C43 O8 C42 C36 173.5(11) . . . . ? C37 C36 C42 O7 -172.4(12) . . . . ? C35 C36 C42 O7 5.3(18) . . . . ? C37 C36 C42 O8 12.6(16) . . . . ? C35 C36 C42 O8 -169.7(11) . . . . ? C42 O8 C43 C44 89.5(14) . . . . ? C9 N7 B1 N5 122.5(13) . . . . ? N6 N7 B1 N5 -58.6(13) . . . . ? C9 N7 B1 N9 -122.4(13) . . . . ? N6 N7 B1 N9 56.6(13) . . . . ? N4 N5 B1 N7 57.5(12) . . . . ? C6 N5 B1 N7 -114.6(14) . . . . ? N4 N5 B1 N9 -58.0(12) . . . . ? C6 N5 B1 N9 129.9(13) . . . . ? C12 N9 B1 N7 116.9(13) . . . . ? N8 N9 B1 N7 -53.2(13) . . . . ? C12 N9 B1 N5 -128.3(13) . . . . ? N8 N9 B1 N5 61.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.813 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.193 _database_code_depnum_ccdc_archive 'CCDC 967847'