# Electronic Supplementary Material (ESI) for CrystEngComm # 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_080113a _database_code_depnum_ccdc_archive 'CCDC 696713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H104 Cr2 Mn2 N20 O10' _chemical_formula_weight 2368.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1273(11) _cell_length_b 13.8348(14) _cell_length_c 20.0191(18) _cell_angle_alpha 73.539(6) _cell_angle_beta 73.108(6) _cell_angle_gamma 70.312(6) _cell_volume 2961.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1226 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9102 _exptl_absorpt_correction_T_max 0.9430 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33771 _diffrn_reflns_av_R_equivalents 0.1053 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10284 _reflns_number_gt 4633 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10284 _refine_ls_number_parameters 776 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1773 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2169 _refine_ls_wR_factor_gt 0.1617 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 4.897 _refine_ls_shift/su_max 1.541 _refine_ls_shift/su_mean 0.026 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 Mn1 Mn 1.0000 0.0000 1.0000 0.0413(16) Uani 1 2 d S . . Mn2 Mn 0.5000 0.5000 0.5000 0.0427(16) Uani 1 2 d S . . Cr1 Cr 0.6953(4) 0.1861(4) 0.8149(2) 0.0554(15) Uani 1 1 d . . . O1 O 0.936(3) 0.341(2) 0.6823(17) 0.121(10) Uani 1 1 d . . . O2 O 0.709(3) -0.100(2) 0.7883(15) 0.103(9) Uani 1 1 d . . . O3 O 0.5199(19) 0.5062(19) 0.6077(12) 0.059(6) Uani 1 1 d . . . O4 O 0.616(5) 0.642(4) -0.010(3) 0.20(2) Uani 1 1 d D . . H49 H 0.5994 0.6320 -0.0436 0.304 Uiso 1 1 calc R . . O5 O 0.769(6) 0.722(3) 0.881(3) 0.19(2) Uani 1 1 d D . . N1 N 0.519(3) 0.328(3) 0.7092(16) 0.093(10) Uani 1 1 d . . . N2 N 0.847(2) 0.064(2) 0.9390(13) 0.059(7) Uani 1 1 d . . . N3 N 0.741(2) 0.0623(19) 0.7734(13) 0.056(6) Uani 1 1 d . . . N4 N 0.834(2) 0.214(2) 0.7401(13) 0.057(6) Uani 1 1 d . . . N5 N 0.694(3) 0.327(2) 0.8315(16) 0.077(8) Uani 1 1 d . . . N6 N 0.560(2) 0.116(2) 0.8772(13) 0.064(7) Uani 1 1 d . . . N7 N 1.1046(18) 0.0399(16) 0.9035(11) 0.043(5) Uani 1 1 d . . . N8 N 1.0326(19) -0.1435(17) 0.9817(11) 0.045(6) Uani 1 1 d . . . N9 N 0.6325(18) 0.5684(18) 0.4486(11) 0.046(6) Uani 1 1 d . . . N10 N 0.6187(18) 0.3581(17) 0.5066(11) 0.047(6) Uani 1 1 d . . . C1 C 0.580(3) 0.274(3) 0.7472(17) 0.068(9) Uani 1 1 d . . . C3 C 0.841(3) 0.057(3) 0.7139(16) 0.059(8) Uani 1 1 d . . . C8 C 0.886(3) -0.018(3) 0.672(2) 0.078(10) Uani 1 1 d . . . H1 H 0.8529 -0.0740 0.6824 0.093 Uiso 1 1 calc R . . C7 C 0.980(4) -0.010(3) 0.614(2) 0.087(11) Uani 1 1 d . . . H2 H 1.0084 -0.0607 0.5860 0.104 Uiso 1 1 calc R . . C5 C 0.989(3) 0.142(3) 0.6376(17) 0.067(9) Uani 1 1 d . . . H6 H 1.0248 0.1958 0.6266 0.080 Uiso 1 1 calc R . . C4 C 0.892(3) 0.139(2) 0.6961(16) 0.057(8) Uani 1 1 d . . . C16 C 0.857(3) 0.306(3) 0.730(2) 0.078(10) Uani 1 1 d . . . C17 C 0.777(3) 0.369(3) 0.781(2) 0.076(10) Uani 1 1 d . . . C18 C 0.780(4) 0.470(4) 0.776(3) 0.120(16) Uani 1 1 d . . . H7 H 0.8366 0.4977 0.7406 0.143 Uiso 1 1 calc R . . C19 C 0.700(6) 0.527(4) 0.824(4) 0.16(2) Uani 1 1 d . . . H8 H 0.7009 0.5960 0.8200 0.189 Uiso 1 1 calc R . . C20 C 0.615(6) 0.483(6) 0.880(4) 0.17(2) Uani 1 1 d . . . H9 H 0.5639 0.5187 0.9159 0.198 Uiso 1 1 calc R . . C21 C 0.616(5) 0.384(4) 0.878(3) 0.119(16) Uani 1 1 d . . . H10 H 0.5580 0.3553 0.9108 0.143 Uiso 1 1 calc R . . C15 C 0.464(3) 0.151(3) 0.9264(18) 0.083(11) Uani 1 1 d . . . H11 H 0.4543 0.2121 0.9405 0.100 Uiso 1 1 calc R . . C14 C 0.377(3) 0.093(5) 0.958(2) 0.101(14) Uani 1 1 d . . . H12 H 0.3092 0.1176 0.9916 0.121 Uiso 1 1 calc R . . C13 C 0.394(4) 0.003(5) 0.937(2) 0.111(16) Uani 1 1 d . . . H13 H 0.3369 -0.0351 0.9567 0.133 Uiso 1 1 calc R . . C12 C 0.493(4) -0.032(3) 0.889(2) 0.093(13) Uani 1 1 d . . . H14 H 0.5047 -0.0952 0.8757 0.111 Uiso 1 1 calc R . . C11 C 0.576(3) 0.023(3) 0.8580(18) 0.071(10) Uani 1 1 d . . . C10 C 0.683(3) -0.011(3) 0.8039(18) 0.070(9) Uani 1 1 d . . . C9 C 1.135(3) 0.076(3) 0.533(2) 0.099(13) Uani 1 1 d . . . H5A H 1.1752 0.1223 0.5359 0.148 Uiso 1 1 calc R . . H3B H 1.1049 0.1012 0.4895 0.148 Uiso 1 1 calc R . . H4C H 1.1901 0.0070 0.5318 0.148 Uiso 1 1 calc R . . C2 C 0.795(3) 0.107(2) 0.8952(16) 0.057(8) Uani 1 1 d . . . C22 C 1.125(3) 0.136(2) 0.8726(15) 0.054(7) Uani 1 1 d . . . C23 C 1.084(3) 0.222(2) 0.9045(14) 0.050(7) Uani 1 1 d . . . C24 C 1.115(3) 0.321(3) 0.8642(17) 0.067(9) Uani 1 1 d D . . C25 C 1.034(7) 0.405(4) 0.838(3) 0.31(7) Uani 1 1 d D . . H28 H 0.9578 0.3972 0.8480 0.372 Uiso 1 1 calc R . . C26 C 1.044(7) 0.501(5) 0.799(3) 0.26(5) Uani 1 1 d D . . H27 H 0.9814 0.5560 0.7843 0.312 Uiso 1 1 calc R . . C27 C 1.161(6) 0.505(5) 0.786(2) 0.17(3) Uani 1 1 d D . . H26 H 1.1785 0.5659 0.7574 0.207 Uiso 1 1 calc R . . C28 C 1.240(5) 0.437(4) 0.808(4) 0.28(7) Uani 1 1 d D . . H25 H 1.3159 0.4462 0.8000 0.341 Uiso 1 1 calc R . . C29 C 1.214(5) 0.340(4) 0.848(4) 0.31(7) Uani 1 1 d D . . H24 H 1.2771 0.2859 0.8630 0.374 Uiso 1 1 calc R . . C30 C 1.199(4) 0.133(3) 0.8032(17) 0.092(13) Uani 1 1 d . . . H23 H 1.2272 0.1879 0.7722 0.111 Uiso 1 1 calc R . . C31 C 1.221(3) 0.038(3) 0.7903(17) 0.081(11) Uani 1 1 d . . . H22 H 1.2658 0.0145 0.7487 0.097 Uiso 1 1 calc R . . C32 C 1.161(2) -0.022(2) 0.8533(14) 0.049(7) Uani 1 1 d . . . C33 C 1.161(3) -0.124(2) 0.8604(14) 0.053(7) Uani 1 1 d . . . C34 C 1.224(3) -0.179(2) 0.7985(15) 0.055(8) Uani 1 1 d . . . C35 C 1.177(3) -0.149(3) 0.7385(17) 0.068(9) Uani 1 1 d . . . H15 H 1.1088 -0.0925 0.7346 0.082 Uiso 1 1 calc R . . C36 C 1.233(3) -0.203(3) 0.6838(18) 0.077(10) Uani 1 1 d . . . H16 H 1.2019 -0.1818 0.6431 0.092 Uiso 1 1 calc R . . C37 C 1.332(4) -0.286(3) 0.687(2) 0.080(11) Uani 1 1 d . . . H17 H 1.3670 -0.3217 0.6497 0.096 Uiso 1 1 calc R . . C38 C 1.379(4) -0.315(3) 0.747(2) 0.092(12) Uani 1 1 d . . . H18 H 1.4474 -0.3710 0.7499 0.110 Uiso 1 1 calc R . . C40 C 1.101(3) -0.181(2) 0.9216(15) 0.057(8) Uani 1 1 d . . . C41 C 1.100(4) -0.285(3) 0.9300(19) 0.095(14) Uani 1 1 d . . . H21 H 1.1381 -0.3275 0.8964 0.115 Uiso 1 1 calc R . . C42 C 1.034(4) -0.313(3) 0.9945(18) 0.091(13) Uani 1 1 d . . . H20 H 1.0195 -0.3782 1.0143 0.110 Uiso 1 1 calc R . . C43 C 0.989(3) -0.225(2) 1.0281(15) 0.053(7) Uani 1 1 d . . . C58 C 0.622(2) 0.674(2) 0.4230(14) 0.045(7) Uani 1 1 d . . . C60 C 0.522(2) 0.865(2) 0.3996(16) 0.052(7) Uani 1 1 d . . . C65 C 0.574(3) 0.909(3) 0.4324(18) 0.070(9) Uani 1 1 d . . . H29 H 0.6082 0.8698 0.4714 0.084 Uiso 1 1 calc R . . C64 C 0.574(3) 1.014(3) 0.404(2) 0.085(11) Uani 1 1 d D . . H30 H 0.6133 1.0424 0.4240 0.102 Uiso 1 1 calc R . . C63 C 0.522(3) 1.075(3) 0.351(2) 0.080(11) Uani 1 1 d . . . H31 H 0.5204 1.1454 0.3365 0.096 Uiso 1 1 calc R . . C62 C 0.472(3) 1.031(3) 0.319(2) 0.081(10) Uani 1 1 d . . . H32 H 0.4363 1.0720 0.2807 0.098 Uiso 1 1 calc R . . C61 C 0.473(3) 0.926(3) 0.3422(17) 0.066(9) Uani 1 1 d . . . H33 H 0.4405 0.8973 0.3186 0.080 Uiso 1 1 calc R . . C57 C 0.738(3) 0.689(3) 0.3873(15) 0.055(8) Uani 1 1 d . . . H34 H 0.7549 0.7530 0.3650 0.065 Uiso 1 1 calc R . . C56 C 0.818(3) 0.594(2) 0.3923(15) 0.056(8) Uani 1 1 d . . . H35 H 0.9003 0.5797 0.3742 0.067 Uiso 1 1 calc R . . C55 C 0.754(2) 0.517(2) 0.4303(14) 0.048(7) Uani 1 1 d . . . C48 C 0.807(2) 0.410(2) 0.4472(14) 0.049(7) Uani 1 1 d . . . C54 C 0.941(2) 0.370(2) 0.4257(16) 0.053(7) Uani 1 1 d . . . C49 C 0.995(3) 0.324(2) 0.3679(17) 0.065(9) Uani 1 1 d . . . H36 H 0.9483 0.3152 0.3418 0.078 Uiso 1 1 calc R . . C50 C 1.120(3) 0.289(3) 0.3476(19) 0.075(10) Uani 1 1 d . . . H37 H 1.1563 0.2577 0.3080 0.090 Uiso 1 1 calc R . . C51 C 1.189(3) 0.300(3) 0.386(2) 0.081(11) Uani 1 1 d . . . H38 H 1.2724 0.2765 0.3735 0.097 Uiso 1 1 calc R . . C52 C 1.136(3) 0.347(3) 0.444(2) 0.085(11) Uani 1 1 d . . . H39 H 1.1836 0.3558 0.4701 0.102 Uiso 1 1 calc R . . C53 C 1.013(3) 0.381(3) 0.4649(19) 0.070(9) Uani 1 1 d . . . H40 H 0.9773 0.4111 0.5047 0.084 Uiso 1 1 calc R . . C47 C 0.743(2) 0.336(2) 0.4844(14) 0.047(7) Uani 1 1 d . . . C46 C 0.797(3) 0.227(2) 0.5025(15) 0.056(8) Uani 1 1 d . . . H41 H 0.8782 0.1930 0.4931 0.068 Uiso 1 1 calc R . . C6 C 1.031(3) 0.069(3) 0.5963(18) 0.069(9) Uani 1 1 d . . . C66 C 0.624(3) 0.524(4) 0.617(2) 0.100(14) Uani 1 1 d . . . H43A H 0.6922 0.4654 0.6083 0.150 Uiso 1 1 calc R . . H45B H 0.6107 0.5331 0.6647 0.150 Uiso 1 1 calc R . . H44C H 0.6383 0.5865 0.5838 0.150 Uiso 1 1 calc R . . C67 C 0.708(9) 0.540(8) 0.023(8) 0.40(10) Uani 1 1 d . . . H48A H 0.7812 0.5255 -0.0124 0.596 Uiso 1 1 calc R . . H47B H 0.6741 0.4822 0.0365 0.596 Uiso 1 1 calc R . . H46C H 0.7242 0.5513 0.0637 0.596 Uiso 1 1 calc R . . C59 C 0.517(2) 0.753(2) 0.4289(14) 0.047(7) Uani 1 1 d . . . C44 C 0.597(2) 0.261(2) 0.5394(14) 0.048(7) Uani 1 1 d . . . C39A C 1.324(3) -0.261(3) 0.8026(18) 0.081(11) Uani 1 1 d . . . H19 H 1.3559 -0.2810 0.8429 0.098 Uiso 1 1 calc R . . C45A C 0.706(3) 0.182(2) 0.5368(15) 0.056(8) Uani 1 1 d . . . H42 H 0.7140 0.1106 0.5551 0.067 Uiso 1 1 calc R . . H50 H 0.752(16) 0.756(14) 0.843(5) 0.02(5) Uiso 1 1 d D . . H51 H 0.862(13) 0.697(18) 0.897(12) 0.09(7) Uiso 1 1 d D . . H52 H 0.505(19) 0.461(17) 0.636(12) 0.01(7) Uiso 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 Mn1 0.039(3) 0.047(4) 0.037(3) -0.001(3) -0.008(3) -0.018(3) Mn2 0.037(3) 0.049(4) 0.040(3) 0.000(3) -0.008(3) -0.019(3) Cr1 0.050(3) 0.065(3) 0.050(3) 0.004(2) -0.016(2) -0.023(3) O1 0.12(2) 0.11(2) 0.14(2) -0.029(18) 0.03(2) -0.079(19) O2 0.13(2) 0.08(2) 0.12(2) -0.016(16) -0.024(18) -0.060(18) O3 0.062(14) 0.070(16) 0.050(13) -0.003(12) -0.017(11) -0.026(13) O4 0.24(5) 0.21(5) 0.17(4) -0.09(3) 0.04(4) -0.09(4) O5 0.24(6) 0.13(3) 0.15(4) 0.02(3) -0.04(4) -0.04(4) N1 0.10(2) 0.10(2) 0.07(2) 0.013(17) -0.037(19) -0.02(2) N2 0.049(15) 0.083(19) 0.044(14) 0.007(13) -0.015(12) -0.029(14) N3 0.052(15) 0.059(17) 0.057(15) 0.003(12) -0.024(13) -0.018(13) N4 0.055(15) 0.055(17) 0.063(16) -0.001(13) -0.014(13) -0.027(13) N5 0.08(2) 0.08(2) 0.08(2) -0.021(17) -0.015(17) -0.027(18) N6 0.050(16) 0.09(2) 0.046(15) 0.014(14) -0.021(13) -0.024(15) N7 0.043(13) 0.040(14) 0.042(13) -0.001(11) -0.006(11) -0.017(11) N8 0.047(13) 0.048(14) 0.040(13) -0.002(11) -0.008(11) -0.019(11) N9 0.036(13) 0.052(16) 0.049(13) -0.004(11) -0.009(11) -0.014(11) N10 0.036(13) 0.058(16) 0.043(13) -0.003(11) -0.004(10) -0.021(11) C1 0.07(2) 0.07(2) 0.051(19) 0.006(17) -0.015(17) -0.024(19) C3 0.051(19) 0.07(2) 0.056(19) 0.000(17) -0.021(16) -0.017(17) C8 0.07(2) 0.07(2) 0.10(3) -0.02(2) -0.02(2) -0.014(19) C7 0.08(3) 0.09(3) 0.09(3) -0.03(2) -0.02(2) 0.00(2) C5 0.053(19) 0.08(2) 0.06(2) -0.006(18) -0.013(17) -0.017(18) C4 0.049(18) 0.06(2) 0.059(19) -0.009(16) -0.017(16) -0.014(16) C16 0.07(2) 0.08(3) 0.09(3) -0.01(2) -0.02(2) -0.03(2) C17 0.08(2) 0.07(2) 0.09(3) -0.02(2) -0.02(2) -0.03(2) C18 0.11(4) 0.10(4) 0.17(5) -0.05(3) -0.02(3) -0.05(3) C19 0.16(5) 0.11(4) 0.23(7) -0.09(5) -0.01(5) -0.05(4) C20 0.15(5) 0.19(6) 0.19(6) -0.12(5) 0.02(5) -0.06(5) C21 0.13(4) 0.11(4) 0.13(4) -0.05(3) 0.00(3) -0.04(3) C15 0.06(2) 0.12(3) 0.06(2) 0.01(2) -0.02(2) -0.03(2) C14 0.05(2) 0.15(4) 0.07(3) 0.02(3) -0.012(19) -0.02(3) C13 0.08(3) 0.17(5) 0.08(3) 0.02(3) -0.02(3) -0.07(3) C12 0.09(3) 0.11(3) 0.09(3) 0.02(2) -0.03(2) -0.07(3) C11 0.07(2) 0.09(3) 0.06(2) 0.018(19) -0.029(19) -0.04(2) C10 0.08(3) 0.08(3) 0.07(2) 0.001(19) -0.03(2) -0.04(2) C9 0.07(2) 0.13(4) 0.08(3) -0.04(2) 0.00(2) -0.01(2) C2 0.049(18) 0.07(2) 0.051(18) 0.003(16) -0.012(16) -0.029(16) C22 0.056(18) 0.054(19) 0.046(17) -0.003(15) 0.000(15) -0.025(16) C23 0.057(18) 0.052(19) 0.038(16) -0.001(14) -0.003(14) -0.026(15) C24 0.09(3) 0.05(2) 0.07(2) -0.008(16) 0.002(19) -0.036(19) C25 0.51(16) 0.20(7) 0.35(11) 0.21(8) -0.33(12) -0.28(10) C26 0.29(10) 0.22(8) 0.30(10) 0.17(7) -0.18(9) -0.18(8) C27 0.20(7) 0.22(8) 0.10(4) 0.03(4) 0.03(4) -0.16(7) C28 0.06(3) 0.09(5) 0.6(2) 0.03(6) 0.00(6) -0.01(3) C29 0.10(4) 0.06(4) 0.69(19) 0.06(6) -0.07(7) -0.05(3) C30 0.14(4) 0.07(2) 0.06(2) -0.016(18) 0.03(2) -0.06(2) C31 0.12(3) 0.08(3) 0.049(19) -0.025(18) 0.025(19) -0.05(2) C32 0.049(17) 0.053(19) 0.040(16) -0.001(14) -0.004(13) -0.021(15) C33 0.055(18) 0.05(2) 0.044(17) -0.002(14) -0.006(14) -0.017(15) C34 0.07(2) 0.043(18) 0.046(18) 0.000(14) -0.008(16) -0.020(17) C35 0.06(2) 0.08(2) 0.07(2) -0.028(19) -0.007(18) -0.019(18) C36 0.08(3) 0.10(3) 0.06(2) -0.04(2) 0.00(2) -0.04(2) C37 0.09(3) 0.07(3) 0.07(3) -0.03(2) 0.02(2) -0.05(2) C38 0.10(3) 0.05(2) 0.09(3) -0.01(2) 0.00(3) 0.00(2) C40 0.07(2) 0.05(2) 0.049(18) -0.008(15) -0.004(16) -0.020(16) C41 0.15(4) 0.05(2) 0.07(2) -0.025(18) 0.03(2) -0.05(2) C42 0.13(3) 0.06(2) 0.07(2) -0.010(18) 0.02(2) -0.05(2) C43 0.061(19) 0.051(19) 0.048(18) 0.002(14) -0.015(15) -0.024(16) C58 0.040(16) 0.054(19) 0.041(16) -0.001(13) -0.006(13) -0.021(15) C60 0.046(17) 0.052(19) 0.059(19) 0.000(15) -0.015(15) -0.021(15) C65 0.08(2) 0.07(2) 0.07(2) -0.003(18) -0.017(19) -0.033(19) C64 0.08(3) 0.08(3) 0.11(3) -0.02(2) -0.01(2) -0.04(2) C63 0.07(2) 0.06(2) 0.10(3) -0.01(2) 0.00(2) -0.02(2) C62 0.09(3) 0.07(3) 0.08(2) 0.008(19) -0.03(2) -0.04(2) C61 0.08(2) 0.06(2) 0.07(2) 0.002(17) -0.022(18) -0.031(18) C57 0.049(17) 0.06(2) 0.052(18) 0.002(14) -0.003(14) -0.025(17) C56 0.045(17) 0.07(2) 0.054(18) -0.003(15) -0.003(14) -0.028(17) C55 0.043(17) 0.05(2) 0.048(17) -0.001(14) -0.009(14) -0.022(15) C48 0.035(15) 0.06(2) 0.047(16) -0.005(14) -0.007(13) -0.020(15) C54 0.041(16) 0.055(19) 0.056(19) -0.002(15) -0.007(15) -0.018(14) C49 0.046(19) 0.08(2) 0.07(2) -0.018(18) -0.002(17) -0.024(17) C50 0.07(2) 0.08(2) 0.08(2) -0.019(19) 0.01(2) -0.030(19) C51 0.036(18) 0.09(3) 0.11(3) -0.02(2) -0.01(2) -0.019(18) C52 0.04(2) 0.11(3) 0.11(3) -0.02(3) -0.02(2) -0.02(2) C53 0.05(2) 0.08(2) 0.08(2) -0.024(19) -0.017(18) -0.017(18) C47 0.046(17) 0.05(2) 0.043(16) -0.004(13) -0.012(13) -0.020(15) C46 0.045(17) 0.05(2) 0.065(19) -0.005(15) -0.008(15) -0.012(15) C6 0.06(2) 0.08(3) 0.07(2) -0.02(2) -0.022(18) -0.005(19) C66 0.08(3) 0.17(4) 0.09(3) -0.03(3) -0.02(2) -0.07(3) C67 0.23(11) 0.18(9) 0.6(2) 0.09(11) -0.01(12) -0.01(8) C59 0.047(17) 0.052(18) 0.043(16) -0.001(13) -0.009(13) -0.022(15) C44 0.042(16) 0.051(19) 0.051(17) -0.003(14) -0.009(13) -0.017(15) C39A 0.10(3) 0.07(2) 0.06(2) -0.008(18) -0.01(2) 0.00(2) C45A 0.056(19) 0.046(18) 0.062(19) -0.002(14) -0.010(15) -0.020(16) _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 Mn1 N8 2.01(2) . ? Mn1 N8 2.01(2) 2_757 ? Mn1 N7 2.02(2) 2_757 ? Mn1 N7 2.02(2) . ? Mn1 N2 2.31(2) 2_757 ? Mn1 N2 2.31(2) . ? Mn2 N10 2.00(2) . ? Mn2 N10 2.00(2) 2_666 ? Mn2 N9 2.01(2) 2_666 ? Mn2 N9 2.01(2) . ? Mn2 O3 2.27(2) . ? Mn2 O3 2.27(2) 2_666 ? Cr1 N3 1.96(3) . ? Cr1 N4 1.97(2) . ? Cr1 N5 2.06(3) . ? Cr1 C1 2.07(4) . ? Cr1 N6 2.09(3) . ? Cr1 C2 2.12(3) . ? O1 C16 1.25(4) . ? O2 C10 1.27(4) . ? O3 C66 1.44(4) . ? O3 H52 0.8(2) . ? O4 C67 1.58(10) . ? O4 H49 0.8201 . ? O5 H50 0.81(5) . ? O5 H51 1.17(5) . ? N1 C1 1.15(4) . ? N2 C2 1.13(3) . ? N3 C10 1.33(4) . ? N3 C3 1.43(4) . ? N4 C16 1.34(4) . ? N4 C4 1.41(4) . ? N5 C21 1.33(5) . ? N5 C17 1.36(4) . ? N6 C15 1.33(4) . ? N6 C11 1.38(4) . ? N7 C22 1.37(3) . ? N7 C32 1.38(3) . ? N8 C40 1.37(3) . ? N8 C43 1.39(3) . ? N9 C58 1.38(3) . ? N9 C55 1.39(3) . ? N10 C44 1.39(3) . ? N10 C47 1.40(3) . ? C3 C4 1.39(4) . ? C3 C8 1.39(4) . ? C8 C7 1.37(5) . ? C8 H1 0.9300 . ? C7 C6 1.36(5) . ? C7 H2 0.9300 . ? C5 C6 1.36(4) . ? C5 C4 1.40(4) . ? C5 H6 0.9300 . ? C16 C17 1.46(5) . ? C17 C18 1.38(5) . ? C18 C19 1.37(7) . ? C18 H7 0.9300 . ? C19 C20 1.44(7) . ? C19 H8 0.9300 . ? C20 C21 1.38(7) . ? C20 H9 0.9300 . ? C21 H10 0.9300 . ? C15 C14 1.43(5) . ? C15 H11 0.9300 . ? C14 C13 1.36(6) . ? C14 H12 0.9300 . ? C13 C12 1.35(6) . ? C13 H13 0.9300 . ? C12 C11 1.38(4) . ? C12 H14 0.9300 . ? C11 C10 1.46(5) . ? C9 C6 1.51(5) . ? C9 H5A 0.9600 . ? C9 H3B 0.9600 . ? C9 H4C 0.9600 . ? C22 C23 1.39(4) . ? C22 C30 1.42(4) . ? C23 C43 1.39(4) 2_757 ? C23 C24 1.48(4) . ? C24 C29 1.25(5) . ? C24 C25 1.33(6) . ? C25 C26 1.35(6) . ? C25 H28 0.9300 . ? C26 C27 1.38(6) . ? C26 H27 0.9300 . ? C27 C28 1.19(6) . ? C27 H26 0.9300 . ? C28 C29 1.44(6) . ? C28 H25 0.9300 . ? C29 H24 0.9300 . ? C30 C31 1.34(4) . ? C30 H23 0.9300 . ? C31 C32 1.44(4) . ? C31 H22 0.9300 . ? C32 C33 1.39(4) . ? C33 C40 1.40(4) . ? C33 C34 1.51(4) . ? C34 C39A 1.36(4) . ? C34 C35 1.37(4) . ? C35 C36 1.39(4) . ? C35 H15 0.9300 . ? C36 C37 1.35(5) . ? C36 H16 0.9300 . ? C37 C38 1.37(5) . ? C37 H17 0.9300 . ? C38 C39A 1.41(5) . ? C38 H18 0.9300 . ? C40 C41 1.41(4) . ? C41 C42 1.33(4) . ? C41 H21 0.9300 . ? C42 C43 1.43(4) . ? C42 H20 0.9300 . ? C43 C23 1.39(4) 2_757 ? C58 C59 1.37(4) . ? C58 C57 1.44(4) . ? C60 C61 1.38(4) . ? C60 C65 1.39(4) . ? C60 C59 1.50(4) . ? C65 C64 1.40(5) . ? C65 H29 0.9300 . ? C64 C63 1.33(5) . ? C64 H30 0.9300 . ? C63 C62 1.37(5) . ? C63 H31 0.9300 . ? C62 C61 1.39(4) . ? C62 H32 0.9300 . ? C61 H33 0.9300 . ? C57 C56 1.35(4) . ? C57 H34 0.9300 . ? C56 C55 1.43(4) . ? C56 H35 0.9300 . ? C55 C48 1.40(4) . ? C48 C47 1.40(4) . ? C48 C54 1.50(4) . ? C54 C49 1.37(4) . ? C54 C53 1.39(4) . ? C49 C50 1.40(4) . ? C49 H36 0.9300 . ? C50 C51 1.37(5) . ? C50 H37 0.9300 . ? C51 C52 1.38(5) . ? C51 H38 0.9300 . ? C52 C53 1.38(4) . ? C52 H39 0.9300 . ? C53 H40 0.9300 . ? C47 C46 1.40(4) . ? C46 C45A 1.37(4) . ? C46 H41 0.9300 . ? C66 H43A 0.9600 . ? C66 H45B 0.9600 . ? C66 H44C 0.9600 . ? C67 H48A 0.9655 . ? C67 H47B 0.9655 . ? C67 H46C 0.9653 . ? C59 C44 1.41(4) 2_666 ? C44 C45A 1.40(4) . ? C44 C59 1.41(4) 2_666 ? C39A H19 0.9300 . ? C45A H42 0.9300 . ? 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 N8 Mn1 N8 180.000(4) . 2_757 ? N8 Mn1 N7 90.1(8) . 2_757 ? N8 Mn1 N7 89.9(8) 2_757 2_757 ? N8 Mn1 N7 89.9(8) . . ? N8 Mn1 N7 90.1(8) 2_757 . ? N7 Mn1 N7 180.000(2) 2_757 . ? N8 Mn1 N2 89.6(9) . 2_757 ? N8 Mn1 N2 90.4(9) 2_757 2_757 ? N7 Mn1 N2 84.6(8) 2_757 2_757 ? N7 Mn1 N2 95.4(8) . 2_757 ? N8 Mn1 N2 90.4(9) . . ? N8 Mn1 N2 89.6(9) 2_757 . ? N7 Mn1 N2 95.4(8) 2_757 . ? N7 Mn1 N2 84.6(8) . . ? N2 Mn1 N2 180.000(3) 2_757 . ? N10 Mn2 N10 180.000(3) . 2_666 ? N10 Mn2 N9 89.4(9) . 2_666 ? N10 Mn2 N9 90.6(9) 2_666 2_666 ? N10 Mn2 N9 90.6(9) . . ? N10 Mn2 N9 89.4(9) 2_666 . ? N9 Mn2 N9 180.0(19) 2_666 . ? N10 Mn2 O3 89.2(8) . . ? N10 Mn2 O3 90.8(8) 2_666 . ? N9 Mn2 O3 88.3(8) 2_666 . ? N9 Mn2 O3 91.7(8) . . ? N10 Mn2 O3 90.8(8) . 2_666 ? N10 Mn2 O3 89.2(8) 2_666 2_666 ? N9 Mn2 O3 91.7(8) 2_666 2_666 ? N9 Mn2 O3 88.3(8) . 2_666 ? O3 Mn2 O3 180.000(3) . 2_666 ? N3 Cr1 N4 80.8(11) . . ? N3 Cr1 N5 160.9(12) . . ? N4 Cr1 N5 80.1(12) . . ? N3 Cr1 C1 93.2(12) . . ? N4 Cr1 C1 91.0(11) . . ? N5 Cr1 C1 86.4(12) . . ? N3 Cr1 N6 80.3(12) . . ? N4 Cr1 N6 161.0(12) . . ? N5 Cr1 N6 118.8(13) . . ? C1 Cr1 N6 88.1(11) . . ? N3 Cr1 C2 93.4(11) . . ? N4 Cr1 C2 94.8(10) . . ? N5 Cr1 C2 89.0(12) . . ? C1 Cr1 C2 171.9(13) . . ? N6 Cr1 C2 88.3(10) . . ? C66 O3 Mn2 122(2) . . ? C66 O3 H52 109(10) . . ? Mn2 O3 H52 112(10) . . ? C67 O4 H49 109.3 . . ? H50 O5 H51 127(10) . . ? C2 N2 Mn1 161(2) . . ? C10 N3 C3 125(3) . . ? C10 N3 Cr1 119(2) . . ? C3 N3 Cr1 115(2) . . ? C16 N4 C4 125(3) . . ? C16 N4 Cr1 118(2) . . ? C4 N4 Cr1 115.9(19) . . ? C21 N5 C17 119(4) . . ? C21 N5 Cr1 129(3) . . ? C17 N5 Cr1 112(2) . . ? C15 N6 C11 120(3) . . ? C15 N6 Cr1 130(3) . . ? C11 N6 Cr1 110(2) . . ? C22 N7 C32 106(2) . . ? C22 N7 Mn1 126.9(18) . . ? C32 N7 Mn1 126.6(17) . . ? C40 N8 C43 107(2) . . ? C40 N8 Mn1 127.4(18) . . ? C43 N8 Mn1 126.1(19) . . ? C58 N9 C55 106(2) . . ? C58 N9 Mn2 127.4(17) . . ? C55 N9 Mn2 126.4(18) . . ? C44 N10 C47 105(2) . . ? C44 N10 Mn2 128.0(17) . . ? C47 N10 Mn2 127.2(18) . . ? N1 C1 Cr1 176(3) . . ? C4 C3 C8 119(3) . . ? C4 C3 N3 114(3) . . ? C8 C3 N3 127(3) . . ? C7 C8 C3 120(3) . . ? C7 C8 H1 120.0 . . ? C3 C8 H1 119.9 . . ? C6 C7 C8 122(4) . . ? C6 C7 H2 119.0 . . ? C8 C7 H2 119.0 . . ? C6 C5 C4 122(3) . . ? C6 C5 H6 118.9 . . ? C4 C5 H6 118.9 . . ? C3 C4 C5 119(3) . . ? C3 C4 N4 114(3) . . ? C5 C4 N4 128(3) . . ? O1 C16 N4 128(4) . . ? O1 C16 C17 119(4) . . ? N4 C16 C17 112(3) . . ? N5 C17 C18 121(4) . . ? N5 C17 C16 117(3) . . ? C18 C17 C16 121(4) . . ? C19 C18 C17 119(5) . . ? C19 C18 H7 120.2 . . ? C17 C18 H7 120.3 . . ? C18 C19 C20 121(5) . . ? C18 C19 H8 119.7 . . ? C20 C19 H8 119.7 . . ? C21 C20 C19 115(5) . . ? C21 C20 H9 122.7 . . ? C19 C20 H9 122.6 . . ? N5 C21 C20 125(5) . . ? N5 C21 H10 117.5 . . ? C20 C21 H10 117.4 . . ? N6 C15 C14 120(4) . . ? N6 C15 H11 119.9 . . ? C14 C15 H11 119.9 . . ? C13 C14 C15 119(4) . . ? C13 C14 H12 120.4 . . ? C15 C14 H12 120.4 . . ? C12 C13 C14 120(4) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.1 . . ? C13 C12 C11 121(4) . . ? C13 C12 H14 119.4 . . ? C11 C12 H14 119.4 . . ? C12 C11 N6 120(4) . . ? C12 C11 C10 123(4) . . ? N6 C11 C10 117(3) . . ? O2 C10 N3 127(3) . . ? O2 C10 C11 120(3) . . ? N3 C10 C11 112(3) . . ? C6 C9 H5A 109.5 . . ? C6 C9 H3B 109.5 . . ? H5A C9 H3B 109.5 . . ? C6 C9 H4C 109.4 . . ? H5A C9 H4C 109.5 . . ? H3B C9 H4C 109.5 . . ? N2 C2 Cr1 178(2) . . ? N7 C22 C23 126(2) . . ? N7 C22 C30 109(3) . . ? C23 C22 C30 125(3) . . ? C43 C23 C22 124(2) 2_757 . ? C43 C23 C24 117(3) 2_757 . ? C22 C23 C24 119(2) . . ? C29 C24 C25 109(4) . . ? C29 C24 C23 129(4) . . ? C25 C24 C23 122(4) . . ? C24 C25 C26 132(6) . . ? C24 C25 H28 114.2 . . ? C26 C25 H28 114.2 . . ? C25 C26 C27 110(6) . . ? C25 C26 H27 125.0 . . ? C27 C26 H27 124.9 . . ? C28 C27 C26 125(6) . . ? C28 C27 H26 117.2 . . ? C26 C27 H26 117.3 . . ? C27 C28 C29 117(6) . . ? C27 C28 H25 121.6 . . ? C29 C28 H25 121.8 . . ? C24 C29 C28 127(5) . . ? C24 C29 H24 116.4 . . ? C28 C29 H24 116.4 . . ? C31 C30 C22 108(3) . . ? C31 C30 H23 125.9 . . ? C22 C30 H23 125.8 . . ? C30 C31 C32 107(3) . . ? C30 C31 H22 126.7 . . ? C32 C31 H22 126.7 . . ? N7 C32 C33 126(2) . . ? N7 C32 C31 109(3) . . ? C33 C32 C31 124(3) . . ? C32 C33 C40 124(3) . . ? C32 C33 C34 120(2) . . ? C40 C33 C34 116(3) . . ? C39A C34 C35 119(3) . . ? C39A C34 C33 121(3) . . ? C35 C34 C33 120(3) . . ? C34 C35 C36 119(3) . . ? C34 C35 H15 120.5 . . ? C36 C35 H15 120.4 . . ? C37 C36 C35 123(4) . . ? C37 C36 H16 118.5 . . ? C35 C36 H16 118.6 . . ? C36 C37 C38 118(4) . . ? C36 C37 H17 121.1 . . ? C38 C37 H17 121.0 . . ? C37 C38 C39A 120(4) . . ? C37 C38 H18 119.9 . . ? C39A C38 H18 119.9 . . ? N8 C40 C33 126(3) . . ? N8 C40 C41 109(3) . . ? C33 C40 C41 125(3) . . ? C42 C41 C40 108(3) . . ? C42 C41 H21 126.0 . . ? C40 C41 H21 126.1 . . ? C41 C42 C43 108(3) . . ? C41 C42 H20 126.0 . . ? C43 C42 H20 126.0 . . ? N8 C43 C23 127(3) . 2_757 ? N8 C43 C42 108(3) . . ? C23 C43 C42 125(3) 2_757 . ? C59 C58 N9 126(2) . . ? C59 C58 C57 124(3) . . ? N9 C58 C57 110(2) . . ? C61 C60 C65 119(3) . . ? C61 C60 C59 123(3) . . ? C65 C60 C59 119(3) . . ? C60 C65 C64 117(3) . . ? C60 C65 H29 121.4 . . ? C64 C65 H29 121.5 . . ? C63 C64 C65 125(4) . . ? C63 C64 H30 117.8 . . ? C65 C64 H30 117.7 . . ? C64 C63 C62 118(4) . . ? C64 C63 H31 121.0 . . ? C62 C63 H31 121.0 . . ? C63 C62 C61 120(4) . . ? C63 C62 H32 119.9 . . ? C61 C62 H32 119.8 . . ? C60 C61 C62 121(3) . . ? C60 C61 H33 119.3 . . ? C62 C61 H33 119.3 . . ? C56 C57 C58 107(3) . . ? C56 C57 H34 126.5 . . ? C58 C57 H34 126.5 . . ? C57 C56 C55 108(3) . . ? C57 C56 H35 126.0 . . ? C55 C56 H35 126.0 . . ? N9 C55 C48 126(2) . . ? N9 C55 C56 109(3) . . ? C48 C55 C56 124(3) . . ? C55 C48 C47 124(2) . . ? C55 C48 C54 118(2) . . ? C47 C48 C54 118(3) . . ? C49 C54 C53 119(3) . . ? C49 C54 C48 121(3) . . ? C53 C54 C48 120(3) . . ? C54 C49 C50 121(3) . . ? C54 C49 H36 119.5 . . ? C50 C49 H36 119.5 . . ? C51 C50 C49 119(3) . . ? C51 C50 H37 120.3 . . ? C49 C50 H37 120.4 . . ? C50 C51 C52 120(3) . . ? C50 C51 H38 119.9 . . ? C52 C51 H38 119.8 . . ? C51 C52 C53 120(3) . . ? C51 C52 H39 119.8 . . ? C53 C52 H39 119.8 . . ? C52 C53 C54 120(3) . . ? C52 C53 H40 120.0 . . ? C54 C53 H40 120.0 . . ? N10 C47 C46 110(2) . . ? N10 C47 C48 125(3) . . ? C46 C47 C48 124(3) . . ? C45A C46 C47 107(3) . . ? C45A C46 H41 126.6 . . ? C47 C46 H41 126.6 . . ? C5 C6 C7 118(3) . . ? C5 C6 C9 121(4) . . ? C7 C6 C9 121(3) . . ? O3 C66 H43A 109.5 . . ? O3 C66 H45B 109.5 . . ? H43A C66 H45B 109.5 . . ? O3 C66 H44C 109.5 . . ? H43A C66 H44C 109.5 . . ? H45B C66 H44C 109.5 . . ? O4 C67 H48A 110.1 . . ? O4 C67 H47B 110.1 . . ? H48A C67 H47B 108.9 . . ? O4 C67 H46C 109.8 . . ? H48A C67 H46C 109.0 . . ? H47B C67 H46C 108.9 . . ? C58 C59 C44 124(3) . 2_666 ? C58 C59 C60 120(2) . . ? C44 C59 C60 116(3) 2_666 . ? N10 C44 C45A 110(2) . . ? N10 C44 C59 124(3) . 2_666 ? C45A C44 C59 125(3) . 2_666 ? C34 C39A C38 121(4) . . ? C34 C39A H19 119.7 . . ? C38 C39A H19 119.7 . . ? C46 C45A C44 108(3) . . ? C46 C45A H42 126.1 . . ? C44 C45A H42 126.1 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.658 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.069 data_080119e _database_code_depnum_ccdc_archive 'CCDC 696714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H104 Co2 Mn2 N20 O10' _chemical_formula_weight 2382.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0704(4) _cell_length_b 19.5784(5) _cell_length_c 20.9873(6) _cell_angle_alpha 70.3000(10) _cell_angle_beta 80.6750(10) _cell_angle_gamma 87.8770(10) _cell_volume 5751.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8387 _exptl_absorpt_correction_T_max 0.8707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49571 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 22361 _reflns_number_gt 17004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+4.8548P] 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 22361 _refine_ls_number_parameters 1543 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1577 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.468 _refine_ls_shift/su_mean 0.010 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 0.98515(2) 0.809509(18) 0.190136(18) 0.03346(10) Uani 1 1 d . . . Co2 Co 0.51661(2) 1.186442(18) 0.308538(17) 0.03284(10) Uani 1 1 d . . . Mn1 Mn 0.75074(2) 0.998859(16) 0.251582(17) 0.02701(10) Uani 1 1 d . . . Mn2 Mn 0.24261(2) 0.498592(17) 0.246525(17) 0.02653(10) Uani 1 1 d . . . O1 O 0.8424(2) 0.78748(16) 0.05364(16) 0.0869(9) Uani 1 1 d . . . O2 O 0.9505(3) 0.68369(19) 0.38671(13) 0.1086(11) Uani 1 1 d . . . O3 O 0.5689(3) 1.3041(2) 0.11072(14) 0.1186(13) Uani 1 1 d . . . O4 O 0.6255(2) 1.22402(16) 0.45477(15) 0.0921(9) Uani 1 1 d . . . O5 O 0.23073(13) 0.60954(10) 0.25761(11) 0.0421(4) Uani 1 1 d . . . O6 O 0.25826(14) 0.38804(11) 0.23232(11) 0.0440(4) Uani 1 1 d . . . O7 O 0.2648(3) -0.0169(2) 0.3728(2) 0.1220(13) Uani 1 1 d D . . O8 O 0.2123(3) 0.02817(18) 0.12494(19) 0.1038(10) Uani 1 1 d D . . O9 O 0.2512(3) 0.8578(2) 0.48574(19) 0.1134(11) Uani 1 1 d D . . O10 O 0.2831(3) 0.1265(2) 1.00268(19) 0.1146(12) Uani 1 1 d D . . N1 N 0.85621(15) 0.93107(12) 0.20582(12) 0.0405(5) Uani 1 1 d . . . N2 N 1.13017(19) 0.70245(15) 0.16929(15) 0.0585(7) Uani 1 1 d . . . N3 N 0.90169(15) 0.77127(12) 0.15231(13) 0.0420(5) Uani 1 1 d . . . N4 N 0.93295(17) 0.73979(13) 0.27361(13) 0.0473(6) Uani 1 1 d . . . N5 N 1.02256(15) 0.87110(12) 0.09318(12) 0.0423(5) Uani 1 1 d . . . N6 N 1.06192(16) 0.82949(14) 0.25018(13) 0.0479(6) Uani 1 1 d . . . N7 N 0.65840(13) 0.98396(10) 0.19823(11) 0.0320(4) Uani 1 1 d . . . N8 N 0.71489(13) 0.90265(10) 0.32525(11) 0.0317(4) Uani 1 1 d . . . N9 N 0.84115(14) 1.01484(11) 0.30630(11) 0.0326(4) Uani 1 1 d . . . N10 N 0.78532(13) 1.09515(10) 0.17760(10) 0.0300(4) Uani 1 1 d . . . N11 N 0.65159(15) 1.06701(12) 0.30108(12) 0.0406(5) Uani 1 1 d . . . N12 N 0.3652(2) 1.29320(16) 0.31325(17) 0.0687(8) Uani 1 1 d . . . N13 N 0.57323(16) 1.25507(13) 0.22638(12) 0.0445(5) Uani 1 1 d . . . N14 N 0.58616(15) 1.23120(12) 0.35115(12) 0.0413(5) Uani 1 1 d . . . N15 N 0.47090(16) 1.12679(12) 0.40444(12) 0.0459(6) Uani 1 1 d . . . N16 N 0.45849(17) 1.15584(14) 0.24436(14) 0.0508(6) Uani 1 1 d . . . N17 N 0.37209(13) 0.49414(11) 0.25959(10) 0.0306(4) Uani 1 1 d . . . N18 N 0.27866(13) 0.54892(10) 0.14536(10) 0.0294(4) Uani 1 1 d . . . N19 N 0.11254(12) 0.50411(10) 0.23398(10) 0.0283(4) Uani 1 1 d . . . N20 N 0.20629(13) 0.44834(11) 0.34774(10) 0.0307(4) Uani 1 1 d . . . C1 C 0.90255(17) 0.88417(14) 0.20162(13) 0.0358(6) Uani 1 1 d . . . C2 C 1.07397(18) 0.74124(14) 0.17611(14) 0.0397(6) Uani 1 1 d . . . C3 C 0.84923(19) 0.71259(16) 0.1998(2) 0.0543(8) Uani 1 1 d . . . C4 C 0.8664(2) 0.69582(16) 0.26695(18) 0.0541(8) Uani 1 1 d . . . C5 C 0.8205(3) 0.6378(2) 0.3196(2) 0.0798(13) Uani 1 1 d . . . H56 H 0.8303 0.6273 0.3645 0.096 Uiso 1 1 calc R . . C6 C 0.7612(3) 0.5968(2) 0.3046(3) 0.1035(19) Uani 1 1 d . . . H55 H 0.7315 0.5576 0.3395 0.124 Uiso 1 1 calc R . . C7 C 0.7448(3) 0.6125(2) 0.2390(3) 0.104(2) Uani 1 1 d . . . H54 H 0.7039 0.5839 0.2301 0.125 Uiso 1 1 calc R . . C8 C 0.7882(2) 0.6706(2) 0.1853(3) 0.0772(12) Uani 1 1 d . . . H53 H 0.7766 0.6809 0.1408 0.093 Uiso 1 1 calc R . . C9 C 0.8972(2) 0.80142(17) 0.08689(18) 0.0543(8) Uani 1 1 d . . . C10 C 0.9699(2) 0.85697(17) 0.05239(16) 0.0530(8) Uani 1 1 d . . . C11 C 0.9850(3) 0.8902(2) -0.01825(18) 0.0771(12) Uani 1 1 d . . . H48 H 0.9486 0.8788 -0.0452 0.092 Uiso 1 1 calc R . . C12 C 1.0543(3) 0.9401(2) -0.04797(19) 0.0887(15) Uani 1 1 d . . . H49 H 1.0652 0.9632 -0.0952 0.106 Uiso 1 1 calc R . . C13 C 1.1063(3) 0.9552(2) -0.0073(2) 0.0770(12) Uani 1 1 d . . . H50 H 1.1531 0.9892 -0.0264 0.092 Uiso 1 1 calc R . . C14 C 1.0895(2) 0.91952(17) 0.06347(18) 0.0589(9) Uani 1 1 d . . . H51 H 1.1263 0.9299 0.0907 0.071 Uiso 1 1 calc R . . C15 C 0.9708(3) 0.72971(19) 0.32969(17) 0.0622(9) Uani 1 1 d . . . C16 C 1.0452(2) 0.78168(19) 0.31462(16) 0.0562(8) Uani 1 1 d . . . C17 C 1.0975(3) 0.7813(2) 0.3636(2) 0.0797(12) Uani 1 1 d . . . H60 H 1.0860 0.7472 0.4075 0.096 Uiso 1 1 calc R . . C18 C 1.1661(3) 0.8314(3) 0.3470(3) 0.0997(17) Uani 1 1 d . . . H61 H 1.2015 0.8317 0.3793 0.120 Uiso 1 1 calc R . . C19 C 1.1812(3) 0.8803(3) 0.2830(3) 0.0981(15) Uani 1 1 d . . . H62 H 1.2263 0.9155 0.2709 0.118 Uiso 1 1 calc R . . C20 C 1.1287(3) 0.8775(2) 0.2352(2) 0.0774(11) Uani 1 1 d . . . H63 H 1.1408 0.9106 0.1909 0.093 Uiso 1 1 calc R . . C21 C 0.63956(17) 1.03034(13) 0.13622(13) 0.0352(5) Uani 1 1 d . . . C22 C 0.5613(2) 1.00354(16) 0.12052(16) 0.0487(7) Uani 1 1 d . . . H9 H 0.5337 1.0254 0.0822 0.058 Uiso 1 1 calc R . . C23 C 0.5353(2) 0.94115(16) 0.17113(16) 0.0490(7) Uani 1 1 d . . . H10 H 0.4863 0.9120 0.1743 0.059 Uiso 1 1 calc R . . C24 C 0.59633(17) 0.92749(14) 0.21924(14) 0.0370(6) Uani 1 1 d . . . C25 C 0.59730(17) 0.86385(13) 0.27496(14) 0.0376(6) Uani 1 1 d . . . C26 C 0.53570(19) 0.80297(14) 0.28019(15) 0.0422(6) Uani 1 1 d . . . C27 C 0.4457(2) 0.80148(17) 0.30542(19) 0.0595(9) Uani 1 1 d . . . H14 H 0.4218 0.8372 0.3228 0.071 Uiso 1 1 calc R . . C28 C 0.3898(2) 0.7461(2) 0.3050(2) 0.0713(11) Uani 1 1 d . . . H15 H 0.3289 0.7452 0.3223 0.086 Uiso 1 1 calc R . . C29 C 0.4244(3) 0.69347(18) 0.27916(19) 0.0663(10) Uani 1 1 d . . . H16 H 0.3867 0.6576 0.2779 0.080 Uiso 1 1 calc R . . C30 C 0.5137(3) 0.69371(19) 0.25550(19) 0.0679(10) Uani 1 1 d . . . H17 H 0.5375 0.6570 0.2394 0.082 Uiso 1 1 calc R . . C31 C 0.5698(2) 0.74864(17) 0.25520(17) 0.0579(8) Uani 1 1 d . . . H18 H 0.6308 0.7489 0.2381 0.069 Uiso 1 1 calc R . . C32 C 0.65584(17) 0.85216(13) 0.32212(14) 0.0367(6) Uani 1 1 d . . . C33 C 0.6641(2) 0.78472(16) 0.37552(17) 0.0579(9) Uani 1 1 d . . . H20 H 0.6318 0.7421 0.3845 0.069 Uiso 1 1 calc R . . C34 C 0.7272(2) 0.79447(16) 0.41023(18) 0.0601(9) Uani 1 1 d . . . H21 H 0.7466 0.7596 0.4476 0.072 Uiso 1 1 calc R . . C35 C 0.75923(18) 0.86793(13) 0.37956(14) 0.0377(6) Uani 1 1 d . . . C36 C 0.82328(17) 0.89881(13) 0.40291(13) 0.0362(6) Uani 1 1 d . . . C37 C 0.85761(19) 0.85555(15) 0.46719(14) 0.0414(6) Uani 1 1 d . . . C38 C 0.9488(2) 0.8442(2) 0.46578(17) 0.0645(9) Uani 1 1 d . . . H25 H 0.9881 0.8633 0.4248 0.077 Uiso 1 1 calc R . . C39 C 0.9823(3) 0.8045(3) 0.5248(2) 0.0864(13) Uani 1 1 d . . . H26 H 1.0438 0.7969 0.5230 0.104 Uiso 1 1 calc R . . C40 C 0.9260(3) 0.7766(2) 0.58530(19) 0.0804(12) Uani 1 1 d . . . H27 H 0.9492 0.7504 0.6247 0.097 Uiso 1 1 calc R . . C41 C 0.8371(3) 0.7868(2) 0.58827(18) 0.0744(11) Uani 1 1 d . . . H28 H 0.7989 0.7682 0.6299 0.089 Uiso 1 1 calc R . . C42 C 0.8018(2) 0.82523(18) 0.52888(16) 0.0593(8) Uani 1 1 d . . . H29 H 0.7399 0.8304 0.5310 0.071 Uiso 1 1 calc R . . C43 C 0.85799(18) 0.96929(14) 0.36897(13) 0.0367(6) Uani 1 1 d . . . C44 C 0.9165(2) 1.00536(17) 0.39519(16) 0.0549(8) Uani 1 1 d . . . H31 H 0.9380 0.9863 0.4367 0.066 Uiso 1 1 calc R . . C45 C 0.9346(2) 1.07158(17) 0.34890(16) 0.0557(8) Uani 1 1 d . . . H32 H 0.9710 1.1070 0.3525 0.067 Uiso 1 1 calc R . . C46 C 0.88831(18) 1.07823(14) 0.29288(14) 0.0386(6) Uani 1 1 d . . . C47 C 0.89125(17) 1.13951(13) 0.23431(13) 0.0353(5) Uani 1 1 d . . . C48 C 0.94697(18) 1.20293(14) 0.23100(14) 0.0389(6) Uani 1 1 d . . . C49 C 1.0390(2) 1.19864(17) 0.22760(17) 0.0512(7) Uani 1 1 d . . . H35 H 1.0678 1.1567 0.2246 0.061 Uiso 1 1 calc R . . C50 C 1.0893(2) 1.25633(19) 0.22858(17) 0.0575(8) Uani 1 1 d . . . H36 H 1.1515 1.2530 0.2257 0.069 Uiso 1 1 calc R . . C51 C 1.0479(2) 1.31780(17) 0.23382(16) 0.0563(8) Uani 1 1 d . . . H37 H 1.0816 1.3560 0.2352 0.068 Uiso 1 1 calc R . . C52 C 0.9569(2) 1.32290(17) 0.23702(16) 0.0555(8) Uani 1 1 d . . . H38 H 0.9286 1.3650 0.2401 0.067 Uiso 1 1 calc R . . C53 C 0.9058(2) 1.26561(15) 0.23574(16) 0.0477(7) Uani 1 1 d . . . H39 H 0.8437 1.2696 0.2381 0.057 Uiso 1 1 calc R . . C54 C 0.84557(17) 1.14531(13) 0.18010(13) 0.0332(5) Uani 1 1 d . . . C55 C 0.8557(2) 1.20458(15) 0.11644(15) 0.0447(7) Uani 1 1 d . . . H42 H 0.8919 1.2457 0.1051 0.054 Uiso 1 1 calc R . . C56 C 0.8036(2) 1.19036(15) 0.07603(15) 0.0456(7) Uani 1 1 d . . . H43 H 0.7991 1.2187 0.0312 0.055 Uiso 1 1 calc R . . C57 C 0.75615(17) 1.12304(13) 0.11511(13) 0.0351(5) Uani 1 1 d . . . C58 C 0.68860(17) 1.09311(13) 0.09395(13) 0.0358(6) Uani 1 1 d . . . C59 C 0.66806(19) 1.12610(15) 0.02265(14) 0.0425(6) Uani 1 1 d . . . C60 C 0.6461(2) 1.19765(17) -0.00495(17) 0.0587(8) Uani 1 1 d . . . H3 H 0.6406 1.2274 0.0218 0.070 Uiso 1 1 calc R . . C61 C 0.6320(3) 1.2258(2) -0.0728(2) 0.0789(12) Uani 1 1 d . . . H4 H 0.6181 1.2745 -0.0911 0.095 Uiso 1 1 calc R . . C62 C 0.6380(3) 1.1837(2) -0.1123(2) 0.0843(13) Uani 1 1 d . . . H5 H 0.6279 1.2035 -0.1574 0.101 Uiso 1 1 calc R . . C63 C 0.6591(3) 1.1115(2) -0.08651(18) 0.0697(10) Uani 1 1 d . . . H6 H 0.6627 1.0823 -0.1138 0.084 Uiso 1 1 calc R . . C64 C 0.6747(2) 1.08302(17) -0.01948(16) 0.0533(7) Uani 1 1 d . . . H7 H 0.6900 1.0345 -0.0020 0.064 Uiso 1 1 calc R . . C65 C 0.60539(17) 1.11375(13) 0.30447(13) 0.0344(5) Uani 1 1 d . . . C66 C 0.42160(18) 1.25334(15) 0.31269(15) 0.0438(6) Uani 1 1 d . . . C67 C 0.63085(19) 1.30393(16) 0.23637(17) 0.0487(7) Uani 1 1 d . . . C68 C 0.63785(19) 1.29162(15) 0.30494(18) 0.0484(7) Uani 1 1 d . . . C69 C 0.6890(2) 1.33808(19) 0.3223(2) 0.0696(10) Uani 1 1 d . . . H73 H 0.6937 1.3303 0.3679 0.084 Uiso 1 1 calc R . . C70 C 0.7334(2) 1.3969(2) 0.2697(3) 0.0937(17) Uani 1 1 d . . . H72 H 0.7671 1.4291 0.2805 0.112 Uiso 1 1 calc R . . C71 C 0.7280(3) 1.4079(2) 0.2022(3) 0.0902(15) Uani 1 1 d . . . H71 H 0.7590 1.4470 0.1680 0.108 Uiso 1 1 calc R . . C72 C 0.6777(2) 1.36247(19) 0.1845(2) 0.0718(11) Uani 1 1 d . . . H70 H 0.6746 1.3703 0.1387 0.086 Uiso 1 1 calc R . . C73 C 0.5452(3) 1.2597(2) 0.16774(17) 0.0660(9) Uani 1 1 d . . . C74 C 0.4797(2) 1.2014(2) 0.17944(17) 0.0633(9) Uani 1 1 d . . . C75 C 0.4426(3) 1.1924(3) 0.1262(2) 0.1006(16) Uani 1 1 d . . . H67 H 0.4566 1.2255 0.0820 0.121 Uiso 1 1 calc R . . C76 C 0.3862(4) 1.1358(4) 0.1384(3) 0.123(2) Uani 1 1 d . . . H66 H 0.3606 1.1297 0.1033 0.148 Uiso 1 1 calc R . . C77 C 0.3678(3) 1.0877(3) 0.2036(3) 0.1086(17) Uani 1 1 d . . . H65 H 0.3301 1.0478 0.2131 0.130 Uiso 1 1 calc R . . C78 C 0.4055(3) 1.0985(2) 0.2560(2) 0.0793(11) Uani 1 1 d . . . H64 H 0.3934 1.0650 0.3000 0.095 Uiso 1 1 calc R . . C79 C 0.5815(2) 1.20485(18) 0.41815(17) 0.0570(8) Uani 1 1 d . . . C80 C 0.5124(2) 1.14559(18) 0.44849(16) 0.0577(9) Uani 1 1 d . . . C81 C 0.4905(3) 1.1127(2) 0.51954(18) 0.0877(15) Uani 1 1 d . . . H77 H 0.5203 1.1265 0.5489 0.105 Uiso 1 1 calc R . . C82 C 0.4243(4) 1.0598(2) 0.5453(2) 0.103(2) Uani 1 1 d . . . H78 H 0.4081 1.0375 0.5924 0.124 Uiso 1 1 calc R . . C83 C 0.3833(3) 1.0406(2) 0.5010(2) 0.0964(17) Uani 1 1 d . . . H79 H 0.3391 1.0043 0.5176 0.116 Uiso 1 1 calc R . . C84 C 0.4069(2) 1.07537(18) 0.4300(2) 0.0661(10) Uani 1 1 d . . . H80 H 0.3772 1.0622 0.4003 0.079 Uiso 1 1 calc R . . C85 C 0.40565(16) 0.46685(13) 0.32034(13) 0.0331(5) Uani 1 1 d . . . C86 C 0.50206(17) 0.47448(15) 0.30651(14) 0.0409(6) Uani 1 1 d . . . H117 H 0.5407 0.4610 0.3388 0.049 Uiso 1 1 calc R . . C87 C 0.52609(17) 0.50458(15) 0.23843(14) 0.0406(6) Uani 1 1 d . . . H116 H 0.5846 0.5146 0.2149 0.049 Uiso 1 1 calc R . . C88 C 0.44538(16) 0.51856(13) 0.20850(13) 0.0328(5) Uani 1 1 d . . . C89 C 0.44357(16) 0.55289(13) 0.13903(13) 0.0338(5) Uani 1 1 d . . . C90 C 0.53225(17) 0.57548(14) 0.09265(13) 0.0363(6) Uani 1 1 d . . . C91 C 0.5725(2) 0.64078(18) 0.08272(18) 0.0595(9) Uani 1 1 d . . . H114 H 0.5437 0.6723 0.1037 0.071 Uiso 1 1 calc R . . C92 C 0.6565(2) 0.6604(2) 0.0415(2) 0.0715(11) Uani 1 1 d . . . H113 H 0.6829 0.7049 0.0348 0.086 Uiso 1 1 calc R . . C93 C 0.6991(2) 0.6147(2) 0.01145(19) 0.0685(10) Uani 1 1 d . . . H112 H 0.7552 0.6274 -0.0156 0.082 Uiso 1 1 calc R . . C94 C 0.6596(3) 0.5498(2) 0.0208(2) 0.0793(12) Uani 1 1 d . . . H111 H 0.6889 0.5185 -0.0004 0.095 Uiso 1 1 calc R . . C95 C 0.5762(2) 0.52977(19) 0.0613(2) 0.0639(10) Uani 1 1 d . . . H110 H 0.5501 0.4853 0.0673 0.077 Uiso 1 1 calc R . . C96 C 0.36491(16) 0.56807(13) 0.11011(12) 0.0316(5) Uani 1 1 d . . . C97 C 0.36199(18) 0.60608(14) 0.03903(13) 0.0381(6) Uani 1 1 d . . . H106 H 0.4111 0.6244 0.0048 0.046 Uiso 1 1 calc R . . C98 C 0.27498(18) 0.61039(14) 0.03095(13) 0.0384(6) Uani 1 1 d . . . H105 H 0.2530 0.6328 -0.0099 0.046 Uiso 1 1 calc R . . C99 C 0.22216(16) 0.57442(12) 0.09634(12) 0.0311(5) Uani 1 1 d . . . C100 C 0.12873(16) 0.56703(13) 0.10877(12) 0.0311(5) Uani 1 1 d . . . C101 C 0.07877(17) 0.59520(14) 0.04907(13) 0.0360(6) Uani 1 1 d . . . C102 C 0.0910(2) 0.56504(16) -0.00259(15) 0.0468(7) Uani 1 1 d . . . H102 H 0.1328 0.5287 -0.0015 0.056 Uiso 1 1 calc R . . C103 C 0.0412(2) 0.58847(18) -0.05605(16) 0.0566(8) Uani 1 1 d . . . H101 H 0.0506 0.5686 -0.0910 0.068 Uiso 1 1 calc R . . C104 C -0.0217(2) 0.64096(19) -0.05707(16) 0.0572(8) Uani 1 1 d . . . H100 H -0.0563 0.6556 -0.0921 0.069 Uiso 1 1 calc R . . C105 C -0.0340(2) 0.67192(18) -0.00695(16) 0.0527(8) Uani 1 1 d . . . H99 H -0.0767 0.7077 -0.0082 0.063 Uiso 1 1 calc R . . C106 C 0.01673(19) 0.65022(16) 0.04568(15) 0.0442(6) Uani 1 1 d . . . H98 H 0.0093 0.6725 0.0789 0.053 Uiso 1 1 calc R . . C107 C 0.07831(16) 0.53501(13) 0.17368(13) 0.0319(5) Uani 1 1 d . . . C108 C -0.01797(16) 0.53124(14) 0.18843(14) 0.0376(6) Uani 1 1 d . . . H95 H -0.0570 0.5474 0.1565 0.045 Uiso 1 1 calc R . . C109 C -0.04189(16) 0.50032(14) 0.25637(14) 0.0370(6) Uani 1 1 d . . . H94 H -0.1003 0.4923 0.2802 0.044 Uiso 1 1 calc R . . C110 C 0.03913(15) 0.48182(13) 0.28567(13) 0.0311(5) Uani 1 1 d . . . C111 C 0.04130(16) 0.44607(13) 0.35455(13) 0.0326(5) Uani 1 1 d . . . C112 C -0.04647(16) 0.42613(14) 0.40258(13) 0.0345(5) Uani 1 1 d . . . C113 C -0.09706(19) 0.36666(16) 0.40803(15) 0.0466(7) Uani 1 1 d . . . H92 H -0.0776 0.3386 0.3806 0.056 Uiso 1 1 calc R . . C114 C -0.1773(2) 0.34798(19) 0.45430(17) 0.0578(8) Uani 1 1 d . . . H91 H -0.2106 0.3074 0.4580 0.069 Uiso 1 1 calc R . . C115 C -0.2067(2) 0.3895(2) 0.49407(18) 0.0617(9) Uani 1 1 d . . . H90 H -0.2602 0.3772 0.5248 0.074 Uiso 1 1 calc R . . C116 C -0.1575(2) 0.4490(2) 0.4888(2) 0.0709(11) Uani 1 1 d . . . H89 H -0.1780 0.4772 0.5158 0.085 Uiso 1 1 calc R . . C117 C -0.0776(2) 0.46760(18) 0.44353(18) 0.0569(8) Uani 1 1 d . . . H88 H -0.0446 0.5081 0.4405 0.068 Uiso 1 1 calc R . . C118 C 0.12003(16) 0.42871(13) 0.38297(13) 0.0323(5) Uani 1 1 d . . . C134 C 0.12320(18) 0.39067(14) 0.45403(13) 0.0392(6) Uani 1 1 d . . . H84 H 0.0744 0.3711 0.4881 0.047 Uiso 1 1 calc R . . C119 C 0.40320(17) 0.41222(15) 0.44598(13) 0.0380(6) Uani 1 1 d . . . C120 C 0.20984(18) 0.38853(14) 0.46225(13) 0.0382(6) Uani 1 1 d . . . H83 H 0.2318 0.3673 0.5033 0.046 Uiso 1 1 calc R . . C121 C 0.26256(16) 0.42460(13) 0.39686(12) 0.0327(5) Uani 1 1 d . . . C122 C 0.35547(16) 0.43513(13) 0.38521(13) 0.0327(5) Uani 1 1 d . . . C123 C 0.3871(2) 0.44732(19) 0.49367(16) 0.0530(8) Uani 1 1 d . . . H124 H 0.3449 0.4839 0.4886 0.064 Uiso 1 1 calc R . . C124 C 0.4332(2) 0.4287(2) 0.54912(17) 0.0676(10) Uani 1 1 d . . . H123 H 0.4212 0.4520 0.5815 0.081 Uiso 1 1 calc R . . C125 C 0.4966(2) 0.3756(2) 0.55586(17) 0.0684(10) Uani 1 1 d . . . H122 H 0.5286 0.3638 0.5924 0.082 Uiso 1 1 calc R . . C126 C 0.5130(2) 0.3401(2) 0.50959(18) 0.0645(9) Uani 1 1 d . . . H121 H 0.5559 0.3041 0.5147 0.077 Uiso 1 1 calc R . . C127 C 0.4660(2) 0.35756(17) 0.45490(16) 0.0514(7) Uani 1 1 d . . . H120 H 0.4766 0.3324 0.4240 0.062 Uiso 1 1 calc R . . C128 C 0.2951(3) 0.3795(2) 0.16867(19) 0.0765(11) Uani 1 1 d . . . H12D H 0.2586 0.4044 0.1347 0.115 Uiso 1 1 calc R . . H12E H 0.2964 0.3288 0.1739 0.115 Uiso 1 1 calc R . . H12F H 0.3551 0.3995 0.1544 0.115 Uiso 1 1 calc R . . C129 C 0.1880(3) 0.6202(2) 0.31907(19) 0.0682(10) Uani 1 1 d . . . H12A H 0.1262 0.6045 0.3285 0.102 Uiso 1 1 calc R . . H12B H 0.1910 0.6707 0.3138 0.102 Uiso 1 1 calc R . . H12C H 0.2180 0.5925 0.3564 0.102 Uiso 1 1 calc R . . C130 C 0.2048(4) 0.8667(4) 0.5438(4) 0.150(3) Uani 1 1 d D . . H12M H 0.2463 0.8738 0.5712 0.224 Uiso 1 1 calc R . . H12N H 0.1680 0.8243 0.5694 0.224 Uiso 1 1 calc R . . H12O H 0.1672 0.9083 0.5315 0.224 Uiso 1 1 calc R . . C131 C 0.1825(5) 0.0186(4) 0.3773(4) 0.152(3) Uani 1 1 d . . . H12J H 0.1339 -0.0157 0.3875 0.228 Uiso 1 1 calc R . . H12K H 0.1791 0.0563 0.3344 0.228 Uiso 1 1 calc R . . H12L H 0.1783 0.0395 0.4130 0.228 Uiso 1 1 calc R . . C132 C 0.1545(4) 0.0701(3) 0.1561(3) 0.123(2) Uani 1 1 d . . . H12G H 0.1673 0.0621 0.2014 0.184 Uiso 1 1 calc R . . H12H H 0.0932 0.0562 0.1589 0.184 Uiso 1 1 calc R . . H12I H 0.1637 0.1205 0.1292 0.184 Uiso 1 1 calc R . . C133 C 0.3590(5) 0.1360(3) 0.9550(3) 0.156(3) Uani 1 1 d . . . H13A H 0.3800 0.1854 0.9406 0.234 Uiso 1 1 calc R . . H13B H 0.3456 0.1252 0.9162 0.234 Uiso 1 1 calc R . . H13C H 0.4046 0.1041 0.9748 0.234 Uiso 1 1 calc R . . H131 H 0.208(2) 0.6285(18) 0.2298(17) 0.054(10) Uiso 1 1 d . . . H132 H 0.282(2) 0.371(2) 0.2565(19) 0.066(12) Uiso 1 1 d . . . H133 H 0.236(3) 0.140(3) 0.976(3) 0.18(3) Uiso 1 1 d D . . H134 H 0.246(4) 0.067(3) 0.085(3) 0.21(3) Uiso 1 1 d D . . H135 H 0.266(5) -0.063(2) 0.409(3) 0.23(4) Uiso 1 1 d D . . H136 H 0.297(15) 0.879(17) 0.460(12) 1.5(4) Uiso 1 1 d 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 0.03566(19) 0.03018(18) 0.0343(2) -0.01088(15) -0.00539(15) 0.00376(14) Co2 0.03474(18) 0.03001(18) 0.03014(19) -0.00637(14) -0.00366(14) 0.00369(13) Mn1 0.03091(19) 0.02178(18) 0.0268(2) -0.00545(15) -0.00574(15) -0.00048(14) Mn2 0.02700(18) 0.02504(18) 0.02365(19) -0.00333(15) -0.00345(14) 0.00014(13) O1 0.106(2) 0.0851(19) 0.096(2) -0.0422(17) -0.0661(18) 0.0173(16) O2 0.157(3) 0.109(2) 0.0332(14) 0.0055(15) -0.0023(17) -0.002(2) O3 0.150(3) 0.141(3) 0.0310(14) 0.0178(17) -0.0101(17) -0.035(2) O4 0.138(3) 0.087(2) 0.0751(19) -0.0394(16) -0.0624(19) 0.0203(18) O5 0.0468(11) 0.0331(9) 0.0498(12) -0.0152(9) -0.0151(10) 0.0049(8) O6 0.0477(11) 0.0350(10) 0.0491(12) -0.0138(9) -0.0087(10) 0.0058(8) O7 0.098(3) 0.109(3) 0.152(4) -0.033(3) -0.019(2) -0.020(2) O8 0.125(3) 0.086(2) 0.103(3) -0.045(2) 0.002(2) -0.008(2) O9 0.112(3) 0.126(3) 0.106(3) -0.038(2) -0.035(2) 0.024(2) O10 0.100(2) 0.134(3) 0.084(2) -0.002(2) -0.022(2) 0.016(2) N1 0.0411(12) 0.0380(12) 0.0400(13) -0.0120(10) -0.0024(10) 0.0033(10) N2 0.0629(17) 0.0525(15) 0.0661(18) -0.0252(14) -0.0204(14) 0.0218(13) N3 0.0412(12) 0.0384(12) 0.0508(15) -0.0174(11) -0.0155(11) 0.0060(10) N4 0.0538(14) 0.0401(13) 0.0407(14) -0.0081(11) 0.0008(11) 0.0034(11) N5 0.0443(13) 0.0365(12) 0.0395(13) -0.0086(10) 0.0008(10) 0.0114(10) N6 0.0494(14) 0.0511(14) 0.0514(15) -0.0263(13) -0.0131(12) 0.0081(11) N7 0.0360(11) 0.0253(10) 0.0328(11) -0.0061(9) -0.0078(9) -0.0013(8) N8 0.0355(11) 0.0264(10) 0.0314(11) -0.0064(9) -0.0073(9) 0.0001(8) N9 0.0381(11) 0.0266(10) 0.0322(11) -0.0073(9) -0.0081(9) -0.0001(8) N10 0.0359(11) 0.0251(10) 0.0280(11) -0.0076(8) -0.0046(8) -0.0020(8) N11 0.0425(12) 0.0363(12) 0.0388(13) -0.0100(10) -0.0017(10) 0.0054(10) N12 0.0608(17) 0.0556(17) 0.082(2) -0.0151(16) -0.0133(16) 0.0246(14) N13 0.0485(13) 0.0412(13) 0.0343(13) -0.0024(10) -0.0024(10) 0.0007(10) N14 0.0461(13) 0.0383(12) 0.0424(13) -0.0139(11) -0.0163(11) 0.0089(10) N15 0.0483(13) 0.0371(12) 0.0395(13) -0.0036(11) 0.0071(11) 0.0119(10) N16 0.0507(14) 0.0527(15) 0.0524(16) -0.0200(13) -0.0133(12) 0.0023(11) N17 0.0293(10) 0.0304(10) 0.0279(11) -0.0050(9) -0.0030(8) 0.0006(8) N18 0.0298(10) 0.0277(10) 0.0266(10) -0.0038(8) -0.0047(8) 0.0003(8) N19 0.0292(10) 0.0274(10) 0.0263(10) -0.0066(8) -0.0039(8) -0.0009(8) N20 0.0318(10) 0.0306(10) 0.0252(10) -0.0036(8) -0.0042(8) 0.0014(8) C1 0.0370(13) 0.0332(13) 0.0351(14) -0.0100(11) -0.0035(11) 0.0021(11) C2 0.0456(15) 0.0371(14) 0.0388(15) -0.0144(12) -0.0120(12) 0.0073(12) C3 0.0389(15) 0.0398(16) 0.086(3) -0.0266(17) -0.0041(15) 0.0017(12) C4 0.0484(17) 0.0390(16) 0.069(2) -0.0189(15) 0.0102(15) 0.0002(13) C5 0.076(3) 0.052(2) 0.086(3) -0.011(2) 0.031(2) -0.0037(18) C6 0.072(3) 0.058(2) 0.160(5) -0.033(3) 0.039(3) -0.022(2) C7 0.047(2) 0.063(3) 0.205(6) -0.054(4) 0.000(3) -0.0138(18) C8 0.051(2) 0.061(2) 0.132(4) -0.045(2) -0.022(2) 0.0005(16) C9 0.0639(19) 0.0492(18) 0.061(2) -0.0267(16) -0.0282(17) 0.0155(15) C10 0.070(2) 0.0495(17) 0.0407(17) -0.0169(14) -0.0146(15) 0.0251(15) C11 0.115(3) 0.073(3) 0.0404(19) -0.0161(18) -0.019(2) 0.037(2) C12 0.123(4) 0.075(3) 0.039(2) 0.0023(19) 0.011(2) 0.048(3) C13 0.069(2) 0.060(2) 0.067(3) 0.0058(19) 0.025(2) 0.0190(18) C14 0.0515(18) 0.0491(18) 0.059(2) -0.0042(16) 0.0068(15) 0.0064(14) C15 0.085(3) 0.057(2) 0.0387(18) -0.0121(16) -0.0044(17) 0.0099(18) C16 0.071(2) 0.065(2) 0.0422(17) -0.0287(16) -0.0178(15) 0.0218(17) C17 0.100(3) 0.099(3) 0.060(2) -0.046(2) -0.036(2) 0.042(2) C18 0.094(3) 0.140(5) 0.112(4) -0.088(4) -0.057(3) 0.037(3) C19 0.089(3) 0.122(4) 0.110(4) -0.060(3) -0.041(3) -0.009(3) C20 0.076(2) 0.089(3) 0.079(3) -0.039(2) -0.017(2) -0.018(2) C21 0.0415(14) 0.0282(12) 0.0344(14) -0.0058(11) -0.0125(11) 0.0007(10) C22 0.0506(16) 0.0444(16) 0.0488(18) -0.0049(14) -0.0229(14) -0.0060(13) C23 0.0504(16) 0.0425(16) 0.0505(18) -0.0042(14) -0.0201(14) -0.0112(13) C24 0.0393(14) 0.0327(13) 0.0390(15) -0.0102(11) -0.0094(11) -0.0037(10) C25 0.0391(14) 0.0298(13) 0.0411(15) -0.0072(11) -0.0082(11) -0.0038(10) C26 0.0470(15) 0.0320(13) 0.0426(16) -0.0017(12) -0.0141(13) -0.0091(11) C27 0.0472(17) 0.0456(17) 0.082(2) -0.0146(17) -0.0121(16) -0.0051(13) C28 0.0460(18) 0.066(2) 0.093(3) -0.008(2) -0.0232(18) -0.0137(16) C29 0.083(3) 0.0482(19) 0.065(2) -0.0003(17) -0.039(2) -0.0234(17) C30 0.093(3) 0.0514(19) 0.064(2) -0.0226(18) -0.014(2) -0.0195(18) C31 0.067(2) 0.0489(18) 0.057(2) -0.0193(16) -0.0033(16) -0.0134(15) C32 0.0393(13) 0.0278(12) 0.0390(15) -0.0047(11) -0.0079(11) -0.0052(10) C33 0.072(2) 0.0326(15) 0.061(2) 0.0053(14) -0.0282(17) -0.0145(14) C34 0.078(2) 0.0321(15) 0.061(2) 0.0072(14) -0.0332(18) -0.0078(14) C35 0.0418(14) 0.0287(12) 0.0382(15) -0.0047(11) -0.0079(11) 0.0013(10) C36 0.0418(14) 0.0307(13) 0.0327(14) -0.0050(11) -0.0098(11) 0.0041(10) C37 0.0487(15) 0.0379(14) 0.0351(15) -0.0071(12) -0.0116(12) 0.0039(12) C38 0.0571(19) 0.083(2) 0.0451(19) -0.0111(18) -0.0126(15) 0.0179(17) C39 0.068(2) 0.119(4) 0.063(3) -0.014(2) -0.026(2) 0.033(2) C40 0.097(3) 0.093(3) 0.045(2) -0.010(2) -0.028(2) 0.029(2) C41 0.089(3) 0.077(3) 0.0386(19) 0.0006(18) -0.0048(18) 0.017(2) C42 0.0567(19) 0.061(2) 0.0450(18) -0.0009(16) -0.0053(15) 0.0078(15) C43 0.0433(14) 0.0334(13) 0.0325(14) -0.0073(11) -0.0112(11) 0.0004(11) C44 0.072(2) 0.0491(17) 0.0426(17) -0.0056(14) -0.0257(15) -0.0118(15) C45 0.075(2) 0.0447(17) 0.0480(18) -0.0069(14) -0.0251(16) -0.0178(15) C46 0.0442(14) 0.0341(13) 0.0393(15) -0.0131(12) -0.0093(12) -0.0031(11) C47 0.0393(13) 0.0292(12) 0.0370(14) -0.0096(11) -0.0072(11) -0.0039(10) C48 0.0479(15) 0.0327(13) 0.0342(14) -0.0072(11) -0.0085(12) -0.0077(11) C49 0.0493(17) 0.0447(16) 0.059(2) -0.0146(15) -0.0137(14) -0.0018(13) C50 0.0503(18) 0.065(2) 0.056(2) -0.0113(17) -0.0184(15) -0.0133(15) C51 0.079(2) 0.0489(18) 0.0425(17) -0.0118(14) -0.0146(16) -0.0243(16) C52 0.077(2) 0.0425(16) 0.0508(19) -0.0203(15) -0.0073(16) -0.0091(15) C53 0.0532(17) 0.0403(15) 0.0503(18) -0.0166(14) -0.0056(14) -0.0061(13) C54 0.0366(13) 0.0264(12) 0.0346(14) -0.0072(10) -0.0062(11) -0.0026(10) C55 0.0527(16) 0.0323(14) 0.0424(16) -0.0014(12) -0.0100(13) -0.0116(12) C56 0.0578(17) 0.0356(14) 0.0374(15) -0.0015(12) -0.0114(13) -0.0096(12) C57 0.0434(14) 0.0276(12) 0.0321(13) -0.0071(10) -0.0056(11) -0.0014(10) C58 0.0424(14) 0.0297(12) 0.0340(14) -0.0071(11) -0.0103(11) 0.0011(10) C59 0.0489(15) 0.0398(15) 0.0348(15) -0.0033(12) -0.0142(12) -0.0054(12) C60 0.080(2) 0.0432(17) 0.0511(19) -0.0056(15) -0.0272(17) 0.0030(15) C61 0.117(3) 0.051(2) 0.065(2) -0.0005(18) -0.045(2) 0.008(2) C62 0.113(3) 0.086(3) 0.047(2) -0.001(2) -0.039(2) 0.003(2) C63 0.086(3) 0.081(3) 0.050(2) -0.0251(19) -0.0256(19) 0.000(2) C64 0.0633(19) 0.0515(18) 0.0474(18) -0.0139(15) -0.0215(15) 0.0024(14) C65 0.0369(13) 0.0331(13) 0.0285(13) -0.0059(11) -0.0009(10) 0.0001(11) C66 0.0404(15) 0.0407(15) 0.0451(16) -0.0083(13) -0.0065(12) 0.0059(12) C67 0.0407(15) 0.0385(15) 0.059(2) -0.0079(14) -0.0033(14) 0.0032(12) C68 0.0371(14) 0.0367(15) 0.072(2) -0.0187(15) -0.0116(14) 0.0052(11) C69 0.0534(19) 0.057(2) 0.111(3) -0.037(2) -0.030(2) 0.0072(16) C70 0.045(2) 0.054(2) 0.187(5) -0.046(3) -0.018(3) -0.0056(16) C71 0.056(2) 0.050(2) 0.142(5) -0.015(3) 0.009(3) -0.0106(17) C72 0.057(2) 0.052(2) 0.081(3) 0.0001(19) 0.0124(19) -0.0010(16) C73 0.079(2) 0.073(2) 0.0346(17) -0.0039(17) -0.0070(16) -0.0031(19) C74 0.066(2) 0.086(3) 0.0420(18) -0.0223(18) -0.0190(16) 0.0029(18) C75 0.099(3) 0.155(5) 0.059(3) -0.041(3) -0.028(2) -0.005(3) C76 0.112(4) 0.182(6) 0.110(4) -0.081(4) -0.044(4) -0.015(4) C77 0.108(4) 0.126(4) 0.122(4) -0.068(4) -0.037(3) -0.029(3) C78 0.079(3) 0.077(3) 0.091(3) -0.033(2) -0.024(2) -0.015(2) C79 0.078(2) 0.0506(18) 0.0496(19) -0.0210(16) -0.0269(17) 0.0203(16) C80 0.081(2) 0.0516(18) 0.0342(16) -0.0106(14) -0.0047(15) 0.0299(17) C81 0.132(4) 0.079(3) 0.0357(19) -0.0081(19) 0.000(2) 0.046(3) C82 0.141(4) 0.081(3) 0.044(2) 0.008(2) 0.033(3) 0.050(3) C83 0.090(3) 0.059(2) 0.088(3) 0.015(2) 0.047(3) 0.016(2) C84 0.058(2) 0.0502(19) 0.067(2) -0.0020(17) 0.0156(17) 0.0038(15) C85 0.0323(12) 0.0332(13) 0.0320(13) -0.0072(11) -0.0084(10) 0.0024(10) C86 0.0321(13) 0.0514(16) 0.0364(15) -0.0088(13) -0.0108(11) 0.0014(11) C87 0.0299(13) 0.0483(16) 0.0386(15) -0.0081(13) -0.0058(11) 0.0001(11) C88 0.0303(12) 0.0340(13) 0.0327(13) -0.0092(11) -0.0055(10) 0.0008(10) C89 0.0324(12) 0.0335(13) 0.0330(13) -0.0089(11) -0.0026(10) -0.0014(10) C90 0.0339(13) 0.0422(14) 0.0278(13) -0.0056(11) -0.0039(10) -0.0009(11) C91 0.0581(19) 0.0517(18) 0.065(2) -0.0255(17) 0.0164(16) -0.0150(15) C92 0.062(2) 0.072(2) 0.073(3) -0.025(2) 0.0173(18) -0.0331(18) C93 0.0401(17) 0.096(3) 0.062(2) -0.025(2) 0.0158(16) -0.0157(17) C94 0.060(2) 0.085(3) 0.090(3) -0.042(2) 0.023(2) -0.002(2) C95 0.0527(19) 0.057(2) 0.081(3) -0.0340(19) 0.0169(17) -0.0111(15) C96 0.0350(12) 0.0296(12) 0.0263(12) -0.0053(10) -0.0025(10) -0.0017(10) C97 0.0405(14) 0.0367(14) 0.0283(13) -0.0015(11) -0.0003(11) -0.0046(11) C98 0.0440(14) 0.0377(14) 0.0276(13) -0.0028(11) -0.0061(11) -0.0030(11) C99 0.0376(13) 0.0250(11) 0.0270(12) -0.0038(10) -0.0056(10) -0.0010(9) C100 0.0366(12) 0.0278(12) 0.0274(12) -0.0055(10) -0.0086(10) 0.0008(10) C101 0.0360(13) 0.0382(14) 0.0298(13) -0.0043(11) -0.0083(11) -0.0061(10) C102 0.0540(17) 0.0503(17) 0.0368(15) -0.0137(13) -0.0103(13) -0.0029(13) C103 0.073(2) 0.064(2) 0.0346(16) -0.0142(15) -0.0143(15) -0.0139(17) C104 0.0588(19) 0.068(2) 0.0376(17) -0.0006(15) -0.0211(14) -0.0141(16) C105 0.0445(16) 0.0573(19) 0.0479(18) -0.0029(15) -0.0166(14) 0.0032(14) C106 0.0473(15) 0.0477(16) 0.0359(15) -0.0084(13) -0.0148(12) 0.0034(12) C107 0.0326(12) 0.0306(12) 0.0334(13) -0.0111(11) -0.0067(10) -0.0004(10) C108 0.0309(12) 0.0431(14) 0.0377(15) -0.0091(12) -0.0120(11) -0.0002(10) C109 0.0283(12) 0.0404(14) 0.0419(15) -0.0133(12) -0.0050(11) -0.0010(10) C110 0.0296(12) 0.0299(12) 0.0348(13) -0.0125(11) -0.0038(10) -0.0016(9) C111 0.0327(12) 0.0312(12) 0.0315(13) -0.0090(11) -0.0002(10) -0.0036(10) C112 0.0308(12) 0.0382(14) 0.0299(13) -0.0060(11) -0.0027(10) -0.0021(10) C113 0.0491(16) 0.0443(16) 0.0432(16) -0.0143(13) 0.0030(13) -0.0102(12) C114 0.0509(18) 0.062(2) 0.054(2) -0.0122(16) 0.0018(15) -0.0235(15) C115 0.0416(16) 0.081(2) 0.051(2) -0.0159(18) 0.0143(14) -0.0091(16) C116 0.061(2) 0.079(3) 0.072(3) -0.040(2) 0.0207(18) -0.0042(18) C117 0.0508(18) 0.0554(19) 0.068(2) -0.0329(17) 0.0113(16) -0.0128(14) C118 0.0324(12) 0.0297(12) 0.0308(13) -0.0059(10) -0.0027(10) -0.0033(9) C134 0.0395(14) 0.0404(14) 0.0295(13) -0.0031(11) 0.0001(11) -0.0067(11) C119 0.0353(13) 0.0445(15) 0.0302(14) -0.0060(12) -0.0072(11) -0.0028(11) C120 0.0434(14) 0.0362(14) 0.0278(13) -0.0005(11) -0.0070(11) -0.0017(11) C121 0.0372(13) 0.0288(12) 0.0284(13) -0.0037(10) -0.0073(10) -0.0001(10) C122 0.0364(13) 0.0301(12) 0.0280(13) -0.0039(10) -0.0079(10) 0.0026(10) C123 0.0471(16) 0.070(2) 0.0460(18) -0.0229(16) -0.0091(14) -0.0031(15) C124 0.065(2) 0.102(3) 0.0409(18) -0.0299(19) -0.0066(16) -0.022(2) C125 0.063(2) 0.091(3) 0.0410(18) 0.0007(18) -0.0232(16) -0.0181(19) C126 0.064(2) 0.064(2) 0.056(2) 0.0005(17) -0.0294(17) 0.0074(17) C127 0.0551(18) 0.0524(18) 0.0436(17) -0.0084(14) -0.0173(14) 0.0089(14) C128 0.110(3) 0.055(2) 0.064(2) -0.0300(19) 0.011(2) -0.006(2) C129 0.093(3) 0.058(2) 0.063(2) -0.0366(19) -0.003(2) 0.0013(19) C130 0.116(5) 0.145(6) 0.194(8) -0.080(6) 0.005(5) 0.007(4) C131 0.146(6) 0.152(6) 0.169(7) -0.061(5) -0.049(5) 0.039(5) C132 0.124(4) 0.158(5) 0.113(4) -0.076(4) -0.035(4) 0.039(4) C133 0.181(7) 0.114(5) 0.145(6) -0.041(4) 0.040(5) 0.040(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 N3 1.889(2) . ? Co1 N4 1.890(2) . ? Co1 C2 1.916(3) . ? Co1 C1 1.937(3) . ? Co1 N6 1.979(2) . ? Co1 N5 1.984(2) . ? Co2 N13 1.885(2) . ? Co2 N14 1.888(2) . ? Co2 C66 1.916(3) . ? Co2 C65 1.930(3) . ? Co2 N16 1.976(3) . ? Co2 N15 1.979(2) . ? Mn1 N7 2.008(2) . ? Mn1 N9 2.014(2) . ? Mn1 N8 2.018(2) . ? Mn1 N10 2.018(2) . ? Mn1 N11 2.319(2) . ? Mn1 N1 2.328(2) . ? Mn2 N18 2.007(2) . ? Mn2 N20 2.008(2) . ? Mn2 N17 2.0087(19) . ? Mn2 N19 2.0139(19) . ? Mn2 O5 2.2590(19) . ? Mn2 O6 2.281(2) . ? O1 C9 1.256(4) . ? O2 C15 1.230(4) . ? O3 C73 1.224(4) . ? O4 C79 1.245(4) . ? O5 C129 1.422(4) . ? O5 H131 0.71(3) . ? O6 C128 1.423(4) . ? O6 H132 0.66(4) . ? O7 C131 1.404(7) . ? O7 H135 0.97(2) . ? O8 C132 1.408(6) . ? O8 H134 1.01(2) . ? O9 H136 0.83(3) . ? O9 C130 1.365(7) . ? O9 H136 0.83(3) . ? O10 C133 1.364(6) . ? O10 H133 0.95(2) . ? N1 C1 1.151(3) . ? N2 C2 1.141(4) . ? N3 C9 1.311(4) . ? N3 C3 1.406(4) . ? N4 C15 1.342(4) . ? N4 C4 1.399(4) . ? N5 C14 1.332(4) . ? N5 C10 1.354(4) . ? N6 C20 1.327(4) . ? N6 C16 1.350(4) . ? N7 C21 1.379(3) . ? N7 C24 1.381(3) . ? N8 C35 1.378(3) . ? N8 C32 1.379(3) . ? N9 C46 1.374(3) . ? N9 C43 1.375(3) . ? N10 C57 1.378(3) . ? N10 C54 1.381(3) . ? N11 C65 1.144(3) . ? N12 C66 1.133(4) . ? N13 C73 1.339(4) . ? N13 C67 1.403(4) . ? N14 C79 1.315(4) . ? N14 C68 1.413(4) . ? N15 C84 1.331(4) . ? N15 C80 1.347(4) . ? N16 C78 1.332(4) . ? N16 C74 1.347(4) . ? N17 C85 1.377(3) . ? N17 C88 1.381(3) . ? N18 C96 1.384(3) . ? N18 C99 1.392(3) . ? N19 C107 1.381(3) . ? N19 C110 1.385(3) . ? N20 C118 1.385(3) . ? N20 C121 1.389(3) . ? C3 C8 1.390(5) . ? C3 C4 1.401(5) . ? C4 C5 1.398(5) . ? C5 C6 1.362(7) . ? C5 H56 0.9300 . ? C6 C7 1.368(8) . ? C6 H55 0.9300 . ? C7 C8 1.394(6) . ? C7 H54 0.9300 . ? C8 H53 0.9300 . ? C9 C10 1.486(5) . ? C10 C11 1.387(5) . ? C11 C12 1.375(7) . ? C11 H48 0.9300 . ? C12 C13 1.355(6) . ? C12 H49 0.9300 . ? C13 C14 1.395(5) . ? C13 H50 0.9300 . ? C14 H51 0.9300 . ? C15 C16 1.464(5) . ? C16 C17 1.392(5) . ? C17 C18 1.371(7) . ? C17 H60 0.9300 . ? C18 C19 1.351(7) . ? C18 H61 0.9300 . ? C19 C20 1.390(5) . ? C19 H62 0.9300 . ? C20 H63 0.9300 . ? C21 C58 1.401(4) . ? C21 C22 1.436(4) . ? C22 C23 1.342(4) . ? C22 H9 0.9300 . ? C23 C24 1.427(4) . ? C23 H10 0.9300 . ? C24 C25 1.394(4) . ? C25 C32 1.388(4) . ? C25 C26 1.502(3) . ? C26 C27 1.371(4) . ? C26 C31 1.385(4) . ? C27 C28 1.401(4) . ? C27 H14 0.9300 . ? C28 C29 1.368(6) . ? C28 H15 0.9300 . ? C29 C30 1.357(5) . ? C29 H16 0.9300 . ? C30 C31 1.390(4) . ? C30 H17 0.9300 . ? C31 H18 0.9300 . ? C32 C33 1.432(4) . ? C33 C34 1.343(4) . ? C33 H20 0.9300 . ? C34 C35 1.429(4) . ? C34 H21 0.9300 . ? C35 C36 1.390(4) . ? C36 C43 1.398(4) . ? C36 C37 1.493(4) . ? C37 C42 1.379(4) . ? C37 C38 1.381(4) . ? C38 C39 1.384(5) . ? C38 H25 0.9300 . ? C39 C40 1.360(6) . ? C39 H26 0.9300 . ? C40 C41 1.342(6) . ? C40 H27 0.9300 . ? C41 C42 1.398(5) . ? C41 H28 0.9300 . ? C42 H29 0.9300 . ? C43 C44 1.430(4) . ? C44 C45 1.338(4) . ? C44 H31 0.9300 . ? C45 C46 1.429(4) . ? C45 H32 0.9300 . ? C46 C47 1.394(4) . ? C47 C54 1.394(4) . ? C47 C48 1.500(3) . ? C48 C49 1.379(4) . ? C48 C53 1.381(4) . ? C49 C50 1.391(4) . ? C49 H35 0.9300 . ? C50 C51 1.364(5) . ? C50 H36 0.9300 . ? C51 C52 1.365(5) . ? C51 H37 0.9300 . ? C52 C53 1.394(4) . ? C52 H38 0.9300 . ? C53 H39 0.9300 . ? C54 C55 1.434(4) . ? C55 C56 1.343(4) . ? C55 H42 0.9300 . ? C56 C57 1.440(4) . ? C56 H43 0.9300 . ? C57 C58 1.394(4) . ? C58 C59 1.495(4) . ? C59 C60 1.374(4) . ? C59 C64 1.404(4) . ? C60 C61 1.392(5) . ? C60 H3 0.9300 . ? C61 C62 1.343(6) . ? C61 H4 0.9300 . ? C62 C63 1.379(5) . ? C62 H5 0.9300 . ? C63 C64 1.384(4) . ? C63 H6 0.9300 . ? C64 H7 0.9300 . ? C67 C68 1.398(5) . ? C67 C72 1.402(4) . ? C68 C69 1.386(4) . ? C69 C70 1.398(6) . ? C69 H73 0.9300 . ? C70 C71 1.375(7) . ? C70 H72 0.9300 . ? C71 C72 1.367(6) . ? C71 H71 0.9300 . ? C72 H70 0.9300 . ? C73 C74 1.467(5) . ? C74 C75 1.392(5) . ? C75 C76 1.350(7) . ? C75 H67 0.9300 . ? C76 C77 1.364(7) . ? C76 H66 0.9300 . ? C77 C78 1.395(6) . ? C77 H65 0.9300 . ? C78 H64 0.9300 . ? C79 C80 1.487(5) . ? C80 C81 1.399(5) . ? C81 C82 1.373(7) . ? C81 H77 0.9300 . ? C82 C83 1.352(7) . ? C82 H78 0.9300 . ? C83 C84 1.404(6) . ? C83 H79 0.9300 . ? C84 H80 0.9300 . ? C85 C122 1.394(4) . ? C85 C86 1.438(3) . ? C86 C87 1.342(4) . ? C86 H117 0.9300 . ? C87 C88 1.434(3) . ? C87 H116 0.9300 . ? C88 C89 1.389(4) . ? C89 C96 1.396(3) . ? C89 C90 1.504(3) . ? C90 C91 1.372(4) . ? C90 C95 1.373(4) . ? C91 C92 1.398(4) . ? C91 H114 0.9300 . ? C92 C93 1.347(5) . ? C92 H113 0.9300 . ? C93 C94 1.363(5) . ? C93 H112 0.9300 . ? C94 C95 1.386(5) . ? C94 H111 0.9300 . ? C95 H110 0.9300 . ? C96 C97 1.432(3) . ? C97 C98 1.345(4) . ? C97 H106 0.9300 . ? C98 C99 1.431(3) . ? C98 H105 0.9300 . ? C99 C100 1.394(3) . ? C100 C107 1.396(3) . ? C100 C101 1.500(3) . ? C101 C102 1.384(4) . ? C101 C106 1.391(4) . ? C102 C103 1.390(4) . ? C102 H102 0.9300 . ? C103 C104 1.370(5) . ? C103 H101 0.9300 . ? C104 C105 1.366(5) . ? C104 H100 0.9300 . ? C105 C106 1.386(4) . ? C105 H99 0.9300 . ? C106 H98 0.9300 . ? C107 C108 1.433(3) . ? C108 C109 1.341(4) . ? C108 H95 0.9300 . ? C109 C110 1.435(3) . ? C109 H94 0.9300 . ? C110 C111 1.383(3) . ? C111 C118 1.394(3) . ? C111 C112 1.503(3) . ? C112 C113 1.378(4) . ? C112 C117 1.389(4) . ? C113 C114 1.397(4) . ? C113 H92 0.9300 . ? C114 C115 1.365(5) . ? C114 H91 0.9300 . ? C115 C116 1.368(5) . ? C115 H90 0.9300 . ? C116 C117 1.383(4) . ? C116 H89 0.9300 . ? C117 H88 0.9300 . ? C118 C134 1.433(3) . ? C134 C120 1.342(4) . ? C134 H84 0.9300 . ? C119 C123 1.380(4) . ? C119 C127 1.387(4) . ? C119 C122 1.494(3) . ? C120 C121 1.431(3) . ? C120 H83 0.9300 . ? C121 C122 1.393(3) . ? C123 C124 1.388(4) . ? C123 H124 0.9300 . ? C124 C125 1.373(5) . ? C124 H123 0.9300 . ? C125 C126 1.360(5) . ? C125 H122 0.9300 . ? C126 C127 1.384(4) . ? C126 H121 0.9300 . ? C127 H120 0.9300 . ? C128 H12D 0.9600 . ? C128 H12E 0.9600 . ? C128 H12F 0.9600 . ? C129 H12A 0.9600 . ? C129 H12B 0.9600 . ? C129 H12C 0.9600 . ? C130 H12M 0.9600 . ? C130 H12N 0.9600 . ? C130 H12O 0.9600 . ? C131 H12J 0.9600 . ? C131 H12K 0.9600 . ? C131 H12L 0.9600 . ? C132 H12G 0.9600 . ? C132 H12H 0.9600 . ? C132 H12I 0.9600 . ? C133 H13A 0.9600 . ? C133 H13B 0.9600 . ? C133 H13C 0.9600 . ? 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 N3 Co1 N4 83.99(11) . . ? N3 Co1 C2 91.65(11) . . ? N4 Co1 C2 90.15(11) . . ? N3 Co1 C1 91.48(10) . . ? N4 Co1 C1 93.21(11) . . ? C2 Co1 C1 175.63(11) . . ? N3 Co1 N6 165.99(11) . . ? N4 Co1 N6 82.12(11) . . ? C2 Co1 N6 86.55(11) . . ? C1 Co1 N6 91.14(10) . . ? N3 Co1 N5 82.87(11) . . ? N4 Co1 N5 166.75(11) . . ? C2 Co1 N5 88.45(10) . . ? C1 Co1 N5 88.91(10) . . ? N6 Co1 N5 110.93(11) . . ? N13 Co2 N14 84.58(11) . . ? N13 Co2 C66 89.23(11) . . ? N14 Co2 C66 90.68(11) . . ? N13 Co2 C65 93.13(10) . . ? N14 Co2 C65 93.27(10) . . ? C66 Co2 C65 175.57(12) . . ? N13 Co2 N16 82.22(11) . . ? N14 Co2 N16 166.80(11) . . ? C66 Co2 N16 89.55(12) . . ? C65 Co2 N16 87.06(11) . . ? N13 Co2 N15 167.25(11) . . ? N14 Co2 N15 82.76(11) . . ? C66 Co2 N15 89.42(11) . . ? C65 Co2 N15 89.09(10) . . ? N16 Co2 N15 110.45(11) . . ? N7 Mn1 N9 178.67(8) . . ? N7 Mn1 N8 90.27(8) . . ? N9 Mn1 N8 89.67(8) . . ? N7 Mn1 N10 89.19(8) . . ? N9 Mn1 N10 90.87(8) . . ? N8 Mn1 N10 179.40(8) . . ? N7 Mn1 N11 91.17(8) . . ? N9 Mn1 N11 87.52(8) . . ? N8 Mn1 N11 95.54(8) . . ? N10 Mn1 N11 84.22(8) . . ? N7 Mn1 N1 92.14(8) . . ? N9 Mn1 N1 89.17(8) . . ? N8 Mn1 N1 84.23(8) . . ? N10 Mn1 N1 96.03(8) . . ? N11 Mn1 N1 176.68(8) . . ? N18 Mn2 N20 179.88(9) . . ? N18 Mn2 N17 90.46(8) . . ? N20 Mn2 N17 89.65(8) . . ? N18 Mn2 N19 89.75(8) . . ? N20 Mn2 N19 90.14(8) . . ? N17 Mn2 N19 179.24(8) . . ? N18 Mn2 O5 87.59(8) . . ? N20 Mn2 O5 92.35(8) . . ? N17 Mn2 O5 90.73(8) . . ? N19 Mn2 O5 88.55(7) . . ? N18 Mn2 O6 90.79(8) . . ? N20 Mn2 O6 89.27(8) . . ? N17 Mn2 O6 88.31(8) . . ? N19 Mn2 O6 92.41(8) . . ? O5 Mn2 O6 178.12(7) . . ? C129 O5 Mn2 122.21(19) . . ? C129 O5 H131 111(3) . . ? Mn2 O5 H131 101(3) . . ? C128 O6 Mn2 122.8(2) . . ? C128 O6 H132 112(3) . . ? Mn2 O6 H132 100(3) . . ? C131 O7 H135 114(5) . . ? C132 O8 H134 101(4) . . ? H136 O9 C130 131(4) . . ? H136 O9 H136 0(10) . . ? C130 O9 H136 131(4) . . ? C133 O10 H133 104(4) . . ? C1 N1 Mn1 160.7(2) . . ? C9 N3 C3 127.1(3) . . ? C9 N3 Co1 118.6(2) . . ? C3 N3 Co1 114.3(2) . . ? C15 N4 C4 126.4(3) . . ? C15 N4 Co1 118.6(2) . . ? C4 N4 Co1 114.2(2) . . ? C14 N5 C10 117.8(3) . . ? C14 N5 Co1 131.5(2) . . ? C10 N5 Co1 110.6(2) . . ? C20 N6 C16 118.0(3) . . ? C20 N6 Co1 130.2(3) . . ? C16 N6 Co1 111.6(2) . . ? C21 N7 C24 106.3(2) . . ? C21 N7 Mn1 127.19(16) . . ? C24 N7 Mn1 126.33(17) . . ? C35 N8 C32 106.4(2) . . ? C35 N8 Mn1 126.11(17) . . ? C32 N8 Mn1 125.92(17) . . ? C46 N9 C43 106.4(2) . . ? C46 N9 Mn1 125.95(17) . . ? C43 N9 Mn1 127.00(17) . . ? C57 N10 C54 106.8(2) . . ? C57 N10 Mn1 127.61(16) . . ? C54 N10 Mn1 125.55(17) . . ? C65 N11 Mn1 158.6(2) . . ? C73 N13 C67 126.9(3) . . ? C73 N13 Co2 118.5(2) . . ? C67 N13 Co2 113.7(2) . . ? C79 N14 C68 127.4(3) . . ? C79 N14 Co2 118.8(2) . . ? C68 N14 Co2 113.8(2) . . ? C84 N15 C80 118.3(3) . . ? C84 N15 Co2 130.7(3) . . ? C80 N15 Co2 110.9(2) . . ? C78 N16 C74 118.3(3) . . ? C78 N16 Co2 130.2(3) . . ? C74 N16 Co2 111.6(2) . . ? C85 N17 C88 106.43(19) . . ? C85 N17 Mn2 127.43(16) . . ? C88 N17 Mn2 126.14(16) . . ? C96 N18 C99 105.52(19) . . ? C96 N18 Mn2 127.08(16) . . ? C99 N18 Mn2 127.36(16) . . ? C107 N19 C110 106.37(19) . . ? C107 N19 Mn2 127.38(16) . . ? C110 N19 Mn2 126.11(16) . . ? C118 N20 C121 105.56(19) . . ? C118 N20 Mn2 127.21(16) . . ? C121 N20 Mn2 127.21(16) . . ? N1 C1 Co1 176.6(2) . . ? N2 C2 Co1 176.0(3) . . ? C8 C3 C4 120.0(3) . . ? C8 C3 N3 126.5(4) . . ? C4 C3 N3 113.3(3) . . ? C5 C4 N4 126.1(4) . . ? C5 C4 C3 119.8(4) . . ? N4 C4 C3 114.1(3) . . ? C6 C5 C4 119.5(5) . . ? C6 C5 H56 120.2 . . ? C4 C5 H56 120.2 . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H55 119.6 . . ? C7 C6 H55 119.6 . . ? C6 C7 C8 121.4(4) . . ? C6 C7 H54 119.3 . . ? C8 C7 H54 119.3 . . ? C3 C8 C7 118.3(5) . . ? C3 C8 H53 120.8 . . ? C7 C8 H53 120.8 . . ? O1 C9 N3 128.0(3) . . ? O1 C9 C10 120.9(3) . . ? N3 C9 C10 111.1(3) . . ? N5 C10 C11 122.1(4) . . ? N5 C10 C9 116.5(3) . . ? C11 C10 C9 121.4(3) . . ? C12 C11 C10 119.2(4) . . ? C12 C11 H48 120.4 . . ? C10 C11 H48 120.4 . . ? C13 C12 C11 118.8(4) . . ? C13 C12 H49 120.6 . . ? C11 C12 H49 120.6 . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H50 120.1 . . ? C14 C13 H50 120.1 . . ? N5 C14 C13 122.1(4) . . ? N5 C14 H51 118.9 . . ? C13 C14 H51 118.9 . . ? O2 C15 N4 127.7(4) . . ? O2 C15 C16 121.8(4) . . ? N4 C15 C16 110.5(3) . . ? N6 C16 C17 121.2(4) . . ? N6 C16 C15 116.7(3) . . ? C17 C16 C15 122.0(4) . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H60 120.1 . . ? C16 C17 H60 120.1 . . ? C19 C18 C17 118.8(4) . . ? C19 C18 H61 120.6 . . ? C17 C18 H61 120.6 . . ? C18 C19 C20 119.5(5) . . ? C18 C19 H62 120.3 . . ? C20 C19 H62 120.3 . . ? N6 C20 C19 122.7(4) . . ? N6 C20 H63 118.6 . . ? C19 C20 H63 118.6 . . ? N7 C21 C58 126.4(2) . . ? N7 C21 C22 109.0(2) . . ? C58 C21 C22 124.6(2) . . ? C23 C22 C21 107.5(3) . . ? C23 C22 H9 126.2 . . ? C21 C22 H9 126.2 . . ? C22 C23 C24 107.7(2) . . ? C22 C23 H10 126.1 . . ? C24 C23 H10 126.1 . . ? N7 C24 C25 125.8(2) . . ? N7 C24 C23 109.3(2) . . ? C25 C24 C23 124.7(2) . . ? C32 C25 C24 123.9(2) . . ? C32 C25 C26 118.9(2) . . ? C24 C25 C26 117.0(2) . . ? C27 C26 C31 118.8(3) . . ? C27 C26 C25 122.1(3) . . ? C31 C26 C25 118.9(3) . . ? C26 C27 C28 120.0(3) . . ? C26 C27 H14 120.0 . . ? C28 C27 H14 120.0 . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H15 119.8 . . ? C27 C28 H15 119.8 . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H16 120.0 . . ? C28 C29 H16 120.0 . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H17 119.9 . . ? C31 C30 H17 119.9 . . ? C26 C31 C30 120.5(3) . . ? C26 C31 H18 119.7 . . ? C30 C31 H18 119.7 . . ? N8 C32 C25 126.0(2) . . ? N8 C32 C33 109.3(2) . . ? C25 C32 C33 124.7(2) . . ? C34 C33 C32 107.3(3) . . ? C34 C33 H20 126.3 . . ? C32 C33 H20 126.3 . . ? C33 C34 C35 107.8(3) . . ? C33 C34 H21 126.1 . . ? C35 C34 H21 126.1 . . ? N8 C35 C36 126.3(2) . . ? N8 C35 C34 109.2(2) . . ? C36 C35 C34 124.5(3) . . ? C35 C36 C43 123.2(2) . . ? C35 C36 C37 119.3(2) . . ? C43 C36 C37 117.5(2) . . ? C42 C37 C38 117.6(3) . . ? C42 C37 C36 122.8(3) . . ? C38 C37 C36 119.6(3) . . ? C37 C38 C39 120.6(3) . . ? C37 C38 H25 119.7 . . ? C39 C38 H25 119.7 . . ? C40 C39 C38 120.6(4) . . ? C40 C39 H26 119.7 . . ? C38 C39 H26 119.7 . . ? C41 C40 C39 120.2(3) . . ? C41 C40 H27 119.9 . . ? C39 C40 H27 119.9 . . ? C40 C41 C42 120.1(3) . . ? C40 C41 H28 120.0 . . ? C42 C41 H28 120.0 . . ? C37 C42 C41 120.9(3) . . ? C37 C42 H29 119.6 . . ? C41 C42 H29 119.6 . . ? N9 C43 C36 126.0(2) . . ? N9 C43 C44 109.4(2) . . ? C36 C43 C44 124.5(2) . . ? C45 C44 C43 107.2(3) . . ? C45 C44 H31 126.4 . . ? C43 C44 H31 126.4 . . ? C44 C45 C46 108.0(3) . . ? C44 C45 H32 126.0 . . ? C46 C45 H32 126.0 . . ? N9 C46 C47 126.1(2) . . ? N9 C46 C45 109.0(2) . . ? C47 C46 C45 124.9(2) . . ? C54 C47 C46 124.3(2) . . ? C54 C47 C48 118.9(2) . . ? C46 C47 C48 116.7(2) . . ? C49 C48 C53 118.5(3) . . ? C49 C48 C47 121.3(3) . . ? C53 C48 C47 120.1(3) . . ? C48 C49 C50 120.7(3) . . ? C48 C49 H35 119.7 . . ? C50 C49 H35 119.7 . . ? C51 C50 C49 120.3(3) . . ? C51 C50 H36 119.8 . . ? C49 C50 H36 119.8 . . ? C50 C51 C52 119.6(3) . . ? C50 C51 H37 120.2 . . ? C52 C51 H37 120.2 . . ? C51 C52 C53 120.6(3) . . ? C51 C52 H38 119.7 . . ? C53 C52 H38 119.7 . . ? C48 C53 C52 120.2(3) . . ? C48 C53 H39 119.9 . . ? C52 C53 H39 119.9 . . ? N10 C54 C47 126.4(2) . . ? N10 C54 C55 108.7(2) . . ? C47 C54 C55 124.9(2) . . ? C56 C55 C54 108.1(2) . . ? C56 C55 H42 125.9 . . ? C54 C55 H42 125.9 . . ? C55 C56 C57 107.2(2) . . ? C55 C56 H43 126.4 . . ? C57 C56 H43 126.4 . . ? N10 C57 C58 125.8(2) . . ? N10 C57 C56 109.0(2) . . ? C58 C57 C56 125.1(2) . . ? C57 C58 C21 122.7(2) . . ? C57 C58 C59 120.3(2) . . ? C21 C58 C59 116.9(2) . . ? C60 C59 C64 117.9(3) . . ? C60 C59 C58 123.2(3) . . ? C64 C59 C58 118.8(2) . . ? C59 C60 C61 120.3(3) . . ? C59 C60 H3 119.8 . . ? C61 C60 H3 119.8 . . ? C62 C61 C60 121.1(3) . . ? C62 C61 H4 119.5 . . ? C60 C61 H4 119.5 . . ? C61 C62 C63 120.6(3) . . ? C61 C62 H5 119.7 . . ? C63 C62 H5 119.7 . . ? C62 C63 C64 119.0(4) . . ? C62 C63 H6 120.5 . . ? C64 C63 H6 120.5 . . ? C63 C64 C59 121.1(3) . . ? C63 C64 H7 119.4 . . ? C59 C64 H7 119.4 . . ? N11 C65 Co2 173.5(2) . . ? N12 C66 Co2 178.1(3) . . ? C68 C67 C72 120.0(3) . . ? C68 C67 N13 114.5(3) . . ? C72 C67 N13 125.5(3) . . ? C69 C68 C67 120.4(3) . . ? C69 C68 N14 126.1(3) . . ? C67 C68 N14 113.4(3) . . ? C68 C69 C70 118.3(4) . . ? C68 C69 H73 120.8 . . ? C70 C69 H73 120.8 . . ? C71 C70 C69 121.1(4) . . ? C71 C70 H72 119.5 . . ? C69 C70 H72 119.5 . . ? C72 C71 C70 121.1(4) . . ? C72 C71 H71 119.5 . . ? C70 C71 H71 119.5 . . ? C71 C72 C67 119.1(4) . . ? C71 C72 H70 120.5 . . ? C67 C72 H70 120.5 . . ? O3 C73 N13 127.7(4) . . ? O3 C73 C74 121.9(4) . . ? N13 C73 C74 110.5(3) . . ? N16 C74 C75 121.4(4) . . ? N16 C74 C73 116.6(3) . . ? C75 C74 C73 122.0(4) . . ? C76 C75 C74 120.2(5) . . ? C76 C75 H67 119.9 . . ? C74 C75 H67 119.9 . . ? C75 C76 C77 118.6(4) . . ? C75 C76 H66 120.7 . . ? C77 C76 H66 120.7 . . ? C76 C77 C78 119.9(5) . . ? C76 C77 H65 120.1 . . ? C78 C77 H65 120.1 . . ? N16 C78 C77 121.6(4) . . ? N16 C78 H64 119.2 . . ? C77 C78 H64 119.2 . . ? O4 C79 N14 128.2(4) . . ? O4 C79 C80 121.3(3) . . ? N14 C79 C80 110.5(3) . . ? N15 C80 C81 122.1(4) . . ? N15 C80 C79 116.8(3) . . ? C81 C80 C79 121.0(4) . . ? C82 C81 C80 119.0(5) . . ? C82 C81 H77 120.5 . . ? C80 C81 H77 120.5 . . ? C83 C82 C81 118.7(4) . . ? C83 C82 H78 120.6 . . ? C81 C82 H78 120.6 . . ? C82 C83 C84 120.4(4) . . ? C82 C83 H79 119.8 . . ? C84 C83 H79 119.8 . . ? N15 C84 C83 121.4(4) . . ? N15 C84 H80 119.3 . . ? C83 C84 H80 119.3 . . ? N17 C85 C122 126.1(2) . . ? N17 C85 C86 109.2(2) . . ? C122 C85 C86 124.6(2) . . ? C87 C86 C85 107.5(2) . . ? C87 C86 H117 126.3 . . ? C85 C86 H117 126.3 . . ? C86 C87 C88 107.7(2) . . ? C86 C87 H116 126.2 . . ? C88 C87 H116 126.2 . . ? N17 C88 C89 126.7(2) . . ? N17 C88 C87 109.2(2) . . ? C89 C88 C87 124.1(2) . . ? C88 C89 C96 124.1(2) . . ? C88 C89 C90 117.5(2) . . ? C96 C89 C90 118.4(2) . . ? C91 C90 C95 118.6(3) . . ? C91 C90 C89 121.0(2) . . ? C95 C90 C89 120.4(2) . . ? C90 C91 C92 120.7(3) . . ? C90 C91 H114 119.7 . . ? C92 C91 H114 119.7 . . ? C93 C92 C91 120.0(3) . . ? C93 C92 H113 120.0 . . ? C91 C92 H113 120.0 . . ? C92 C93 C94 119.8(3) . . ? C92 C93 H112 120.1 . . ? C94 C93 H112 120.1 . . ? C93 C94 C95 120.8(3) . . ? C93 C94 H111 119.6 . . ? C95 C94 H111 119.6 . . ? C90 C95 C94 120.1(3) . . ? C90 C95 H110 119.9 . . ? C94 C95 H110 119.9 . . ? N18 C96 C89 125.4(2) . . ? N18 C96 C97 110.0(2) . . ? C89 C96 C97 124.6(2) . . ? C98 C97 C96 107.2(2) . . ? C98 C97 H106 126.4 . . ? C96 C97 H106 126.4 . . ? C97 C98 C99 107.9(2) . . ? C97 C98 H105 126.0 . . ? C99 C98 H105 126.0 . . ? N18 C99 C100 125.6(2) . . ? N18 C99 C98 109.3(2) . . ? C100 C99 C98 125.1(2) . . ? C99 C100 C107 124.0(2) . . ? C99 C100 C101 118.3(2) . . ? C107 C100 C101 117.7(2) . . ? C102 C101 C106 118.5(3) . . ? C102 C101 C100 120.6(2) . . ? C106 C101 C100 120.8(2) . . ? C101 C102 C103 120.7(3) . . ? C101 C102 H102 119.7 . . ? C103 C102 H102 119.7 . . ? C104 C103 C102 119.8(3) . . ? C104 C103 H101 120.1 . . ? C102 C103 H101 120.1 . . ? C105 C104 C103 120.4(3) . . ? C105 C104 H100 119.8 . . ? C103 C104 H100 119.8 . . ? C104 C105 C106 120.3(3) . . ? C104 C105 H99 119.9 . . ? C106 C105 H99 119.9 . . ? C105 C106 C101 120.3(3) . . ? C105 C106 H98 119.9 . . ? C101 C106 H98 119.9 . . ? N19 C107 C100 125.9(2) . . ? N19 C107 C108 109.1(2) . . ? C100 C107 C108 125.0(2) . . ? C109 C108 C107 107.9(2) . . ? C109 C108 H95 126.0 . . ? C107 C108 H95 126.0 . . ? C108 C109 C110 107.5(2) . . ? C108 C109 H94 126.2 . . ? C110 C109 H94 126.2 . . ? C111 C110 N19 126.7(2) . . ? C111 C110 C109 124.3(2) . . ? N19 C110 C109 109.1(2) . . ? C110 C111 C118 124.2(2) . . ? C110 C111 C112 118.4(2) . . ? C118 C111 C112 117.4(2) . . ? C113 C112 C117 118.5(3) . . ? C113 C112 C111 121.7(2) . . ? C117 C112 C111 119.9(2) . . ? C112 C113 C114 120.7(3) . . ? C112 C113 H92 119.6 . . ? C114 C113 H92 119.6 . . ? C115 C114 C113 119.9(3) . . ? C115 C114 H91 120.1 . . ? C113 C114 H91 120.1 . . ? C114 C115 C116 120.0(3) . . ? C114 C115 H90 120.0 . . ? C116 C115 H90 120.0 . . ? C115 C116 C117 120.6(3) . . ? C115 C116 H89 119.7 . . ? C117 C116 H89 119.7 . . ? C116 C117 C112 120.3(3) . . ? C116 C117 H88 119.8 . . ? C112 C117 H88 119.8 . . ? N20 C118 C111 125.3(2) . . ? N20 C118 C134 109.9(2) . . ? C111 C118 C134 124.7(2) . . ? C120 C134 C118 107.2(2) . . ? C120 C134 H84 126.4 . . ? C118 C134 H84 126.4 . . ? C123 C119 C127 118.6(3) . . ? C123 C119 C122 119.8(3) . . ? C127 C119 C122 121.5(3) . . ? C134 C120 C121 108.1(2) . . ? C134 C120 H83 126.0 . . ? C121 C120 H83 126.0 . . ? N20 C121 C122 125.8(2) . . ? N20 C121 C120 109.3(2) . . ? C122 C121 C120 124.9(2) . . ? C121 C122 C85 123.6(2) . . ? C121 C122 C119 117.8(2) . . ? C85 C122 C119 118.6(2) . . ? C119 C123 C124 120.8(3) . . ? C119 C123 H124 119.6 . . ? C124 C123 H124 119.6 . . ? C125 C124 C123 119.5(3) . . ? C125 C124 H123 120.3 . . ? C123 C124 H123 120.2 . . ? C126 C125 C124 120.5(3) . . ? C126 C125 H122 119.7 . . ? C124 C125 H122 119.7 . . ? C125 C126 C127 120.2(3) . . ? C125 C126 H121 119.9 . . ? C127 C126 H121 119.9 . . ? C126 C127 C119 120.4(3) . . ? C126 C127 H120 119.8 . . ? C119 C127 H120 119.8 . . ? O6 C128 H12D 109.5 . . ? O6 C128 H12E 109.5 . . ? H12D C128 H12E 109.5 . . ? O6 C128 H12F 109.5 . . ? H12D C128 H12F 109.5 . . ? H12E C128 H12F 109.5 . . ? O5 C129 H12A 109.5 . . ? O5 C129 H12B 109.5 . . ? H12A C129 H12B 109.5 . . ? O5 C129 H12C 109.5 . . ? H12A C129 H12C 109.5 . . ? H12B C129 H12C 109.5 . . ? O9 C130 H12M 109.5 . . ? O9 C130 H12N 109.5 . . ? H12M C130 H12N 109.5 . . ? O9 C130 H12O 109.5 . . ? H12M C130 H12O 109.5 . . ? H12N C130 H12O 109.5 . . ? O7 C131 H12J 109.5 . . ? O7 C131 H12K 109.5 . . ? H12J C131 H12K 109.5 . . ? O7 C131 H12L 109.5 . . ? H12J C131 H12L 109.5 . . ? H12K C131 H12L 109.5 . . ? O8 C132 H12G 109.5 . . ? O8 C132 H12H 109.5 . . ? H12G C132 H12H 109.5 . . ? O8 C132 H12I 109.5 . . ? H12G C132 H12I 109.5 . . ? H12H C132 H12I 109.5 . . ? O10 C133 H13A 109.4 . . ? O10 C133 H13B 109.5 . . ? H13A C133 H13B 109.5 . . ? O10 C133 H13C 109.5 . . ? H13A C133 H13C 109.5 . . ? H13B C133 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.945 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.066 data_dp1 _database_code_depnum_ccdc_archive 'CCDC 696719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H104 Cr2 Mn2 N20 O10' _chemical_formula_weight 2368.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.0924(7) _cell_length_b 19.7862(9) _cell_length_c 21.0071(11) _cell_angle_alpha 70.461(3) _cell_angle_beta 81.220(3) _cell_angle_gamma 88.865(3) _cell_volume 5839.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9090 _exptl_absorpt_correction_T_max 0.9296 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 135612 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 22885 _reflns_number_gt 17696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+3.7868P] 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 22885 _refine_ls_number_parameters 1531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.014 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 H136 H 0.218(2) 0.1329(17) 0.2283(15) 0.064(9) Uiso 1 1 d . . . H135 H 0.278(2) -0.1333(16) 0.2607(15) 0.062(9) Uiso 1 1 d . . . Cr1 Cr 0.51232(2) 0.686284(18) 0.310701(17) 0.03570(10) Uani 1 1 d . . . Cr2 Cr 0.99379(2) 0.307983(18) 0.190330(18) 0.03553(10) Uani 1 1 d . . . Mn1 Mn 0.754022(19) 0.499014(14) 0.251347(14) 0.02861(9) Uani 1 1 d . . . Mn2 Mn 0.244391(18) -0.001279(14) 0.246713(14) 0.02796(9) Uani 1 1 d . . . O1 O 0.63700(18) 0.73465(13) 0.44972(12) 0.0796(7) Uani 1 1 d . . . O2 O 0.5636(2) 0.80559(19) 0.10966(12) 0.1309(13) Uani 1 1 d . . . O3 O 0.9521(2) 0.17600(15) 0.38898(11) 0.1035(9) Uani 1 1 d . . . O4 O 0.84397(17) 0.28074(13) 0.05447(13) 0.0831(7) Uani 1 1 d . . . O5 O 0.25580(12) -0.10992(9) 0.23149(9) 0.0462(4) Uani 1 1 d . . . O6 O 0.23784(12) 0.10766(9) 0.25934(9) 0.0442(4) Uani 1 1 d . . . O7 O 0.7531(2) 0.64353(19) 0.50758(16) 0.1077(9) Uani 1 1 d . . . H7 H 0.7113 0.6146 0.5271 0.162 Uiso 1 1 calc R . . O8 O 0.7285(2) 0.3743(2) -0.00621(15) 0.1134(10) Uani 1 1 d . . . H8 H 0.7681 0.3481 0.0099 0.170 Uiso 1 1 calc R . . O9 O 0.2055(3) 0.52258(16) 0.12871(17) 0.1174(11) Uani 1 1 d . . . H9 H 0.2253 0.5506 0.0907 0.176 Uiso 1 1 calc R . . O10 O 0.2704(2) 0.48302(19) 0.3807(2) 0.1269(12) Uani 1 1 d . . . H10 H 0.2676 0.4465 0.4143 0.190 Uiso 1 1 calc R . . N9 N 0.66291(12) 0.48207(9) 0.19763(9) 0.0341(4) Uani 1 1 d . . . N10 N 0.78661(12) 0.59550(9) 0.17848(9) 0.0325(4) Uani 1 1 d . . . N7 N 0.84402(12) 0.51678(9) 0.30581(9) 0.0345(4) Uani 1 1 d . . . N8 N 0.72054(12) 0.40229(9) 0.32398(9) 0.0332(4) Uani 1 1 d . . . N1 N 0.65173(14) 0.56167(11) 0.30192(10) 0.0454(5) Uani 1 1 d . . . N2 N 0.34705(19) 0.79003(15) 0.31885(17) 0.0819(9) Uani 1 1 d . . . N3 N 0.56939(15) 0.75813(12) 0.22531(10) 0.0487(5) Uani 1 1 d . . . N4 N 0.58760(13) 0.73732(10) 0.34983(10) 0.0416(4) Uani 1 1 d . . . N5 N 0.47538(14) 0.62836(10) 0.41478(10) 0.0433(5) Uani 1 1 d . . . N6 N 0.45300(17) 0.65635(14) 0.24126(12) 0.0631(6) Uani 1 1 d . . . N11 N 0.86170(13) 0.43551(10) 0.20528(10) 0.0430(4) Uani 1 1 d . . . N12 N 1.15289(18) 0.20498(13) 0.16431(14) 0.0672(7) Uani 1 1 d . . . N13 N 0.90673(14) 0.26628(11) 0.15173(11) 0.0437(5) Uani 1 1 d . . . N14 N 0.93808(15) 0.23373(11) 0.27518(10) 0.0470(5) Uani 1 1 d . . . N16 N 1.07082(15) 0.32321(12) 0.25898(11) 0.0504(5) Uani 1 1 d . . . N15 N 1.02485(14) 0.37112(10) 0.08713(10) 0.0433(5) Uani 1 1 d . . . N17 N 0.11459(11) 0.00542(9) 0.23392(8) 0.0298(4) Uani 1 1 d . . . N18 N 0.20782(11) -0.05180(9) 0.34756(8) 0.0320(4) Uani 1 1 d . . . N19 N 0.37390(11) -0.00692(9) 0.26009(9) 0.0325(4) Uani 1 1 d . . . N20 N 0.28030(11) 0.04938(9) 0.14584(8) 0.0315(4) Uani 1 1 d . . . C67 C 0.85403(17) 0.20759(14) 0.19989(16) 0.0522(6) Uani 1 1 d . . . C72 C 0.7917(2) 0.16578(17) 0.1850(2) 0.0718(9) Uani 1 1 d . . . H2 H 0.7800 0.1762 0.1405 0.086 Uiso 1 1 calc R . . C71 C 0.7476(2) 0.10848(18) 0.2380(3) 0.0906(13) Uani 1 1 d . . . H3 H 0.7065 0.0802 0.2286 0.109 Uiso 1 1 calc R . . C70 C 0.7632(2) 0.09265(19) 0.3036(3) 0.0928(13) Uani 1 1 d . . . H4 H 0.7325 0.0539 0.3380 0.111 Uiso 1 1 calc R . . C69 C 0.8233(2) 0.13305(17) 0.31932(19) 0.0752(10) Uani 1 1 d . . . H5 H 0.8326 0.1225 0.3643 0.090 Uiso 1 1 calc R . . C68 C 0.87083(18) 0.19048(14) 0.26721(15) 0.0523(6) Uani 1 1 d . . . C79 C 0.9736(2) 0.22214(16) 0.33266(13) 0.0607(7) Uani 1 1 d . . . C80 C 1.0502(2) 0.27359(15) 0.32177(13) 0.0554(7) Uani 1 1 d . . . C81 C 1.0996(3) 0.2687(2) 0.37349(17) 0.0794(10) Uani 1 1 d . . . H9A H 1.0854 0.2336 0.4162 0.095 Uiso 1 1 calc R . . C82 C 1.1708(3) 0.3175(2) 0.3601(2) 0.0944(13) Uani 1 1 d . . . H10A H 1.2046 0.3156 0.3941 0.113 Uiso 1 1 calc R . . C83 C 1.1907(3) 0.3678(2) 0.2973(2) 0.0947(12) Uani 1 1 d . . . H11 H 1.2377 0.4010 0.2879 0.114 Uiso 1 1 calc R . . C84 C 1.1401(2) 0.36921(19) 0.24713(19) 0.0719(9) Uani 1 1 d . . . H12 H 1.1548 0.4032 0.2038 0.086 Uiso 1 1 calc R . . C66 C 1.09478(17) 0.24090(13) 0.17142(13) 0.0454(6) Uani 1 1 d . . . C73 C 0.90002(19) 0.29594(15) 0.08612(14) 0.0530(6) Uani 1 1 d . . . C74 C 0.97094(19) 0.35293(14) 0.04917(13) 0.0499(6) Uani 1 1 d . . . C75 C 0.9821(2) 0.38475(18) -0.02099(15) 0.0690(9) Uani 1 1 d . . . H16 H 0.9446 0.3712 -0.0462 0.083 Uiso 1 1 calc R . . C76 C 1.0485(2) 0.43630(18) -0.05344(16) 0.0732(9) Uani 1 1 d . . . H17 H 1.0572 0.4575 -0.1008 0.088 Uiso 1 1 calc R . . C77 C 1.1014(2) 0.45597(16) -0.01557(17) 0.0690(9) Uani 1 1 d . . . H18 H 1.1459 0.4917 -0.0366 0.083 Uiso 1 1 calc R . . C78 C 1.08866(19) 0.42189(14) 0.05568(15) 0.0552(7) Uani 1 1 d . . . H19 H 1.1256 0.4351 0.0815 0.066 Uiso 1 1 calc R . . C65 C 0.90766(15) 0.38992(12) 0.20198(11) 0.0391(5) Uani 1 1 d . . . C47 C 0.68928(16) 0.59200(12) 0.09506(12) 0.0396(5) Uani 1 1 d . . . C48 C 0.66688(19) 0.62556(14) 0.02461(13) 0.0526(7) Uani 1 1 d . . . C53 C 0.6766(2) 0.58395(17) -0.01949(15) 0.0644(8) Uani 1 1 d . . . H23 H 0.6958 0.5371 -0.0038 0.077 Uiso 1 1 calc R . . C52 C 0.6578(3) 0.6126(2) -0.08557(17) 0.0831(10) Uani 1 1 d . . . H24 H 0.6633 0.5851 -0.1142 0.100 Uiso 1 1 calc R . . C51 C 0.6306(3) 0.6827(2) -0.10824(19) 0.1020(15) Uani 1 1 d . . . H25 H 0.6162 0.7023 -0.1521 0.122 Uiso 1 1 calc R . . C50 C 0.6249(3) 0.72183(19) -0.06839(19) 0.0970(14) Uani 1 1 d . . . H26 H 0.6089 0.7694 -0.0853 0.116 Uiso 1 1 calc R . . C49 C 0.6424(2) 0.69393(16) -0.00107(17) 0.0756(10) Uani 1 1 d . . . H27 H 0.6370 0.7229 0.0261 0.091 Uiso 1 1 calc R . . C54 C 0.75597(16) 0.62302(12) 0.11676(11) 0.0391(5) Uani 1 1 d . . . C55 C 0.80166(19) 0.69082(13) 0.07831(13) 0.0542(7) Uani 1 1 d . . . H29 H 0.7960 0.7190 0.0338 0.065 Uiso 1 1 calc R . . C56 C 0.85391(18) 0.70597(13) 0.11825(13) 0.0502(6) Uani 1 1 d . . . H30 H 0.8893 0.7475 0.1072 0.060 Uiso 1 1 calc R . . C57 C 0.84543(15) 0.64659(11) 0.18109(11) 0.0365(5) Uani 1 1 d . . . C58 C 0.89254(15) 0.64128(11) 0.23447(12) 0.0379(5) Uani 1 1 d . . . C59 C 0.94778(16) 0.70479(12) 0.23153(12) 0.0403(5) Uani 1 1 d . . . C60 C 0.90603(18) 0.76596(13) 0.23710(13) 0.0482(6) Uani 1 1 d . . . H34 H 0.8440 0.7686 0.2400 0.058 Uiso 1 1 calc R . . C61 C 0.9564(2) 0.82329(14) 0.23841(14) 0.0562(7) Uani 1 1 d . . . H35 H 0.9277 0.8641 0.2421 0.067 Uiso 1 1 calc R . . C62 C 1.0473(2) 0.82064(14) 0.23434(13) 0.0571(7) Uani 1 1 d . . . H36 H 1.0804 0.8592 0.2354 0.069 Uiso 1 1 calc R . . C63 C 1.08949(19) 0.76021(16) 0.22857(15) 0.0600(7) Uani 1 1 d . . . H37 H 1.1515 0.7579 0.2258 0.072 Uiso 1 1 calc R . . C64 C 1.04022(18) 0.70300(14) 0.22692(14) 0.0530(6) Uani 1 1 d . . . H38 H 1.0696 0.6626 0.2226 0.064 Uiso 1 1 calc R . . C21 C 0.89174(16) 0.57995(12) 0.29241(12) 0.0393(5) Uani 1 1 d . . . C22 C 0.94038(19) 0.57364(14) 0.34720(14) 0.0552(7) Uani 1 1 d . . . H40 H 0.9772 0.6090 0.3506 0.066 Uiso 1 1 calc R . . C23 C 0.92324(19) 0.50713(14) 0.39304(13) 0.0538(7) Uani 1 1 d . . . H41 H 0.9464 0.4881 0.4337 0.065 Uiso 1 1 calc R . . C24 C 0.86294(16) 0.47121(12) 0.36759(11) 0.0381(5) Uani 1 1 d . . . C25 C 0.82892(15) 0.40115(12) 0.40141(11) 0.0387(5) Uani 1 1 d . . . C26 C 0.86493(17) 0.35868(12) 0.46499(12) 0.0438(5) Uani 1 1 d . . . C27 C 0.9562(2) 0.34726(18) 0.46194(15) 0.0672(8) Uani 1 1 d . . . H45 H 0.9938 0.3651 0.4202 0.081 Uiso 1 1 calc R . . C28 C 0.9922(2) 0.3097(2) 0.51999(18) 0.0866(11) Uani 1 1 d . . . H46 H 1.0536 0.3024 0.5171 0.104 Uiso 1 1 calc R . . C29 C 0.9374(3) 0.28356(19) 0.58143(16) 0.0791(10) Uani 1 1 d . . . H47 H 0.9616 0.2588 0.6206 0.095 Uiso 1 1 calc R . . C30 C 0.8485(2) 0.29349(19) 0.58560(16) 0.0769(10) Uani 1 1 d . . . H48 H 0.8114 0.2759 0.6276 0.092 Uiso 1 1 calc R . . C31 C 0.8119(2) 0.33002(17) 0.52701(15) 0.0659(8) Uani 1 1 d . . . H49 H 0.7501 0.3350 0.5302 0.079 Uiso 1 1 calc R . . C32 C 0.76413(16) 0.36923(11) 0.37853(12) 0.0395(5) Uani 1 1 d . . . C33 C 0.7328(2) 0.29632(14) 0.40964(15) 0.0640(8) Uani 1 1 d . . . H51 H 0.7524 0.2625 0.4471 0.077 Uiso 1 1 calc R . . C34 C 0.6699(2) 0.28535(13) 0.37505(15) 0.0590(7) Uani 1 1 d . . . H52 H 0.6371 0.2429 0.3846 0.071 Uiso 1 1 calc R . . C35 C 0.66267(15) 0.35119(11) 0.32075(12) 0.0384(5) Uani 1 1 d . . . C36 C 0.60473(15) 0.36148(12) 0.27312(12) 0.0399(5) Uani 1 1 d . . . C37 C 0.54383(17) 0.30028(12) 0.27771(12) 0.0436(5) Uani 1 1 d . . . C38 C 0.5791(2) 0.24519(15) 0.25583(15) 0.0583(7) Uani 1 1 d . . . H56 H 0.6405 0.2449 0.2416 0.070 Uiso 1 1 calc R . . C39 C 0.5234(2) 0.19023(16) 0.25500(16) 0.0677(8) Uani 1 1 d . . . H57 H 0.5478 0.1534 0.2404 0.081 Uiso 1 1 calc R . . C40 C 0.4332(2) 0.19024(15) 0.27559(15) 0.0653(9) Uani 1 1 d . . . H58 H 0.3958 0.1543 0.2739 0.078 Uiso 1 1 calc R . . C41 C 0.3981(2) 0.24355(17) 0.29875(18) 0.0727(9) Uani 1 1 d . . . H59 H 0.3367 0.2430 0.3137 0.087 Uiso 1 1 calc R . . C42 C 0.45293(19) 0.29862(15) 0.30022(17) 0.0625(8) Uani 1 1 d . . . H60 H 0.4282 0.3343 0.3164 0.075 Uiso 1 1 calc R . . C43 C 0.60313(16) 0.42424(12) 0.21761(12) 0.0402(5) Uani 1 1 d . . . C44 C 0.54220(19) 0.43661(14) 0.16923(14) 0.0570(7) Uani 1 1 d . . . H62 H 0.4942 0.4065 0.1718 0.068 Uiso 1 1 calc R . . C45 C 0.56664(18) 0.49942(14) 0.11939(14) 0.0536(7) Uani 1 1 d . . . H63 H 0.5390 0.5205 0.0812 0.064 Uiso 1 1 calc R . . C46 C 0.64325(15) 0.52789(11) 0.13604(11) 0.0372(5) Uani 1 1 d . . . C1 C 0.60585(16) 0.60695(12) 0.30647(11) 0.0399(5) Uani 1 1 d . . . C14 C 0.3975(3) 0.5998(2) 0.2525(2) 0.0918(12) Uani 1 1 d . . . H66 H 0.3830 0.5676 0.2967 0.110 Uiso 1 1 calc R . . C13 C 0.3616(4) 0.5883(3) 0.2005(3) 0.136(2) Uani 1 1 d . . . H67 H 0.3240 0.5484 0.2095 0.163 Uiso 1 1 calc R . . C12 C 0.3813(4) 0.6353(4) 0.1362(3) 0.162(3) Uani 1 1 d . . . H68 H 0.3566 0.6285 0.1008 0.195 Uiso 1 1 calc R . . C11 C 0.4390(4) 0.6941(3) 0.1235(2) 0.134(2) Uani 1 1 d . . . H69 H 0.4530 0.7271 0.0796 0.161 Uiso 1 1 calc R . . C10 C 0.4751(2) 0.7026(2) 0.17727(16) 0.0791(10) Uani 1 1 d . . . C9 C 0.5410(2) 0.7622(2) 0.16683(14) 0.0750(10) Uani 1 1 d . . . C3 C 0.62878(17) 0.80762(14) 0.23329(14) 0.0499(6) Uani 1 1 d . . . C8 C 0.6749(2) 0.86493(16) 0.18031(17) 0.0676(8) Uani 1 1 d . . . H73 H 0.6698 0.8718 0.1350 0.081 Uiso 1 1 calc R . . C7 C 0.7277(2) 0.91082(17) 0.1960(2) 0.0802(11) Uani 1 1 d . . . H74 H 0.7583 0.9491 0.1610 0.096 Uiso 1 1 calc R . . C6 C 0.7361(2) 0.90138(17) 0.2620(2) 0.0789(11) Uani 1 1 d . . . H75 H 0.7717 0.9337 0.2714 0.095 Uiso 1 1 calc R . . C5 C 0.69229(19) 0.84410(15) 0.31595(19) 0.0636(8) Uani 1 1 d . . . H76 H 0.6989 0.8378 0.3609 0.076 Uiso 1 1 calc R . . C4 C 0.63861(16) 0.79656(13) 0.30140(14) 0.0462(6) Uani 1 1 d . . . C2 C 0.40520(18) 0.75202(14) 0.31821(14) 0.0524(6) Uani 1 1 d . . . C15 C 0.58863(19) 0.71292(14) 0.41669(13) 0.0505(6) Uani 1 1 d . . . C16 C 0.52167(19) 0.65275(14) 0.45358(13) 0.0491(6) Uani 1 1 d . . . C17 C 0.5062(3) 0.62437(17) 0.52424(15) 0.0707(9) Uani 1 1 d . . . H81 H 0.5386 0.6421 0.5498 0.085 Uiso 1 1 calc R . . C18 C 0.4433(3) 0.57043(18) 0.55640(16) 0.0758(10) Uani 1 1 d . . . H82 H 0.4328 0.5508 0.6039 0.091 Uiso 1 1 calc R . . C19 C 0.3964(2) 0.54582(17) 0.51780(17) 0.0742(10) Uani 1 1 d . . . H83 H 0.3527 0.5094 0.5388 0.089 Uiso 1 1 calc R . . C20 C 0.41384(19) 0.57551(15) 0.44611(16) 0.0593(7) Uani 1 1 d . . . H84 H 0.3820 0.5580 0.4200 0.071 Uiso 1 1 calc R . . C85 C 0.12177(14) -0.07068(11) 0.38236(11) 0.0343(4) Uani 1 1 d . . . C86 C 0.12450(15) -0.10904(12) 0.45321(11) 0.0401(5) Uani 1 1 d . . . H86 H 0.0755 -0.1283 0.4870 0.048 Uiso 1 1 calc R . . C87 C 0.21085(16) -0.11195(12) 0.46156(11) 0.0413(5) Uani 1 1 d . . . H87 H 0.2327 -0.1336 0.5024 0.050 Uiso 1 1 calc R . . C88 C 0.26369(14) -0.07574(11) 0.39639(10) 0.0344(4) Uani 1 1 d . . . C89 C 0.35665(14) -0.06609(11) 0.38525(11) 0.0350(5) Uani 1 1 d . . . C90 C 0.40403(15) -0.08872(13) 0.44616(11) 0.0401(5) Uani 1 1 d . . . C91 C 0.38836(18) -0.05428(16) 0.49417(14) 0.0549(7) Uani 1 1 d . . . H91 H 0.3469 -0.0182 0.4890 0.066 Uiso 1 1 calc R . . C92 C 0.4338(2) -0.0731(2) 0.54971(15) 0.0707(9) Uani 1 1 d . . . H92 H 0.4221 -0.0504 0.5822 0.085 Uiso 1 1 calc R . . C93 C 0.4964(2) -0.12566(19) 0.55692(15) 0.0720(10) Uani 1 1 d . . . H93 H 0.5279 -0.1376 0.5937 0.086 Uiso 1 1 calc R . . C94 C 0.5122(2) -0.16000(18) 0.51032(16) 0.0699(9) Uani 1 1 d . . . H94 H 0.5545 -0.1955 0.5154 0.084 Uiso 1 1 calc R . . C95 C 0.46577(19) -0.14272(15) 0.45518(14) 0.0548(7) Uani 1 1 d . . . H95 H 0.4761 -0.1674 0.4242 0.066 Uiso 1 1 calc R . . C96 C 0.40733(14) -0.03457(12) 0.32061(11) 0.0351(5) Uani 1 1 d . . . C97 C 0.50308(15) -0.02758(13) 0.30708(12) 0.0426(5) Uani 1 1 d . . . H97 H 0.5416 -0.0414 0.3395 0.051 Uiso 1 1 calc R . . C98 C 0.52735(15) 0.00245(13) 0.23931(12) 0.0428(5) Uani 1 1 d . . . H98 H 0.5858 0.0120 0.2160 0.051 Uiso 1 1 calc R . . C99 C 0.44706(14) 0.01718(11) 0.20932(11) 0.0341(4) Uani 1 1 d . . . C100 C 0.44514(14) 0.05215(11) 0.14005(11) 0.0348(4) Uani 1 1 d . . . C101 C 0.53344(14) 0.07429(13) 0.09392(11) 0.0382(5) Uani 1 1 d . . . C102 C 0.5750(2) 0.02962(17) 0.06090(17) 0.0652(8) Uani 1 1 d . . . H102 H 0.5472 -0.0138 0.0659 0.078 Uiso 1 1 calc R . . C103 C 0.6582(2) 0.0495(2) 0.0202(2) 0.0822(11) Uani 1 1 d . . . H103 H 0.6856 0.0191 -0.0018 0.099 Uiso 1 1 calc R . . C104 C 0.7001(2) 0.1125(2) 0.01208(16) 0.0714(9) Uani 1 1 d . . . H104 H 0.7562 0.1248 -0.0148 0.086 Uiso 1 1 calc R . . C105 C 0.6594(2) 0.15761(19) 0.04349(16) 0.0714(9) Uani 1 1 d . . . H105 H 0.6872 0.2014 0.0373 0.086 Uiso 1 1 calc R . . C106 C 0.57637(19) 0.13839(16) 0.08477(15) 0.0593(7) Uani 1 1 d . . . H106 H 0.5495 0.1692 0.1065 0.071 Uiso 1 1 calc R . . C107 C 0.36669(14) 0.06798(11) 0.11102(10) 0.0341(4) Uani 1 1 d . . . C108 C 0.36416(16) 0.10617(12) 0.04056(11) 0.0403(5) Uani 1 1 d . . . H108 H 0.4134 0.1245 0.0068 0.048 Uiso 1 1 calc R . . C109 C 0.27741(16) 0.11075(12) 0.03200(11) 0.0402(5) Uani 1 1 d . . . H109 H 0.2557 0.1334 -0.0088 0.048 Uiso 1 1 calc R . . C110 C 0.22448(14) 0.07453(11) 0.09706(10) 0.0326(4) Uani 1 1 d . . . C111 C 0.13102(14) 0.06719(11) 0.10905(11) 0.0341(4) Uani 1 1 d . . . C112 C 0.09375(18) 0.06463(14) -0.00229(13) 0.0499(6) Uani 1 1 d . . . H112 H 0.1355 0.0292 -0.0012 0.060 Uiso 1 1 calc R . . C113 C 0.0437(2) 0.08719(17) -0.05568(13) 0.0606(7) Uani 1 1 d . . . H113 H 0.0523 0.0669 -0.0901 0.073 Uiso 1 1 calc R . . C114 C -0.01835(19) 0.13933(16) -0.05777(13) 0.0599(8) Uani 1 1 d . . . H114 H -0.0524 0.1537 -0.0931 0.072 Uiso 1 1 calc R . . C115 C -0.03009(19) 0.17022(16) -0.00772(14) 0.0576(7) Uani 1 1 d . . . H115 H -0.0720 0.2056 -0.0093 0.069 Uiso 1 1 calc R . . C116 C 0.02033(17) 0.14897(14) 0.04521(13) 0.0468(6) Uani 1 1 d . . . H116 H 0.0131 0.1712 0.0782 0.056 Uiso 1 1 calc R . . C117 C 0.08157(15) 0.09475(12) 0.04936(11) 0.0390(5) Uani 1 1 d . . . C118 C 0.08061(14) 0.03606(11) 0.17364(11) 0.0324(4) Uani 1 1 d . . . C119 C -0.01551(15) 0.03211(12) 0.18788(12) 0.0390(5) Uani 1 1 d . . . H119 H -0.0544 0.0478 0.1559 0.047 Uiso 1 1 calc R . . C120 C -0.03904(14) 0.00173(12) 0.25565(11) 0.0382(5) Uani 1 1 d . . . H120 H -0.0973 -0.0061 0.2794 0.046 Uiso 1 1 calc R . . C121 C 0.04158(14) -0.01652(11) 0.28499(11) 0.0320(4) Uani 1 1 d . . . C122 C 0.04324(14) -0.05286(11) 0.35393(11) 0.0331(4) Uani 1 1 d . . . C123 C -0.04467(14) -0.07215(12) 0.40141(11) 0.0357(5) Uani 1 1 d . . . C124 C -0.07549(19) -0.03033(16) 0.44154(16) 0.0592(7) Uani 1 1 d . . . H124 H -0.0421 0.0099 0.4386 0.071 Uiso 1 1 calc R . . C125 C -0.1562(2) -0.04894(19) 0.48589(18) 0.0742(9) Uani 1 1 d . . . H125 H -0.1763 -0.0212 0.5129 0.089 Uiso 1 1 calc R . . C126 C -0.20611(19) -0.10725(18) 0.49033(15) 0.0643(8) Uani 1 1 d . . . H126 H -0.2606 -0.1186 0.5196 0.077 Uiso 1 1 calc R . . C127 C -0.17648(18) -0.14916(16) 0.45186(14) 0.0582(7) Uani 1 1 d . . . H127 H -0.2101 -0.1895 0.4556 0.070 Uiso 1 1 calc R . . C128 C -0.09596(17) -0.13141(14) 0.40720(13) 0.0467(6) Uani 1 1 d . . . H128 H -0.0764 -0.1599 0.3808 0.056 Uiso 1 1 calc R . . C129 C 0.2970(3) -0.11847(18) 0.16956(18) 0.0859(12) Uani 1 1 d . . . H12A H 0.2654 -0.0917 0.1332 0.129 Uiso 1 1 calc R . . H12B H 0.2952 -0.1684 0.1741 0.129 Uiso 1 1 calc R . . H12C H 0.3582 -0.1011 0.1594 0.129 Uiso 1 1 calc R . . C130 C 0.1923(3) 0.11853(18) 0.31874(17) 0.0766(10) Uani 1 1 d . . . H13A H 0.1306 0.1031 0.3259 0.115 Uiso 1 1 calc R . . H13B H 0.1957 0.1686 0.3134 0.115 Uiso 1 1 calc R . . H13C H 0.2197 0.0913 0.3574 0.115 Uiso 1 1 calc R . . C131 C 0.7918(4) 0.6309(4) 0.4487(3) 0.158(2) Uani 1 1 d . . . H13D H 0.8254 0.6730 0.4183 0.237 Uiso 1 1 calc R . . H13E H 0.7456 0.6196 0.4267 0.237 Uiso 1 1 calc R . . H13F H 0.8311 0.5914 0.4602 0.237 Uiso 1 1 calc R . . C132 C 0.6561(5) 0.3671(3) 0.0436(3) 0.177(3) Uani 1 1 d . . . H13G H 0.6763 0.3596 0.0866 0.265 Uiso 1 1 calc R . . H13H H 0.6189 0.3268 0.0471 0.265 Uiso 1 1 calc R . . H13I H 0.6221 0.4099 0.0322 0.265 Uiso 1 1 calc R . . C133 C 0.1448(4) 0.5587(3) 0.1646(3) 0.146(2) Uani 1 1 d . . . H13J H 0.1633 0.5536 0.2077 0.219 Uiso 1 1 calc R . . H13K H 0.0854 0.5381 0.1724 0.219 Uiso 1 1 calc R . . H13L H 0.1449 0.6087 0.1379 0.219 Uiso 1 1 calc R . . C134 C 0.1873(4) 0.5156(3) 0.3803(3) 0.158(2) Uani 1 1 d . . . H13M H 0.1695 0.5236 0.4230 0.236 Uiso 1 1 calc R . . H13N H 0.1433 0.4850 0.3741 0.236 Uiso 1 1 calc R . . H13O H 0.1922 0.5607 0.3436 0.236 Uiso 1 1 calc R . . 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 Cr1 0.03473(19) 0.03516(19) 0.03307(19) -0.00665(15) -0.00398(15) 0.00277(15) Cr2 0.0365(2) 0.03288(19) 0.03478(19) -0.00886(15) -0.00443(15) 0.00429(14) Mn1 0.02988(17) 0.02435(16) 0.02998(17) -0.00661(13) -0.00535(13) -0.00062(12) Mn2 0.02548(16) 0.02859(17) 0.02580(16) -0.00415(13) -0.00326(12) 0.00030(12) O1 0.1042(18) 0.0781(15) 0.0666(14) -0.0259(12) -0.0386(13) -0.0060(13) O2 0.164(3) 0.157(3) 0.0377(13) 0.0159(15) -0.0157(15) -0.066(2) O3 0.147(3) 0.0984(19) 0.0395(12) 0.0058(12) -0.0008(14) -0.0126(18) O4 0.0924(17) 0.0842(16) 0.0861(16) -0.0304(13) -0.0501(14) 0.0016(13) O5 0.0494(10) 0.0378(8) 0.0518(10) -0.0152(8) -0.0088(8) 0.0048(7) O6 0.0459(9) 0.0377(8) 0.0513(10) -0.0170(8) -0.0102(8) 0.0037(7) O7 0.096(2) 0.125(2) 0.103(2) -0.0350(19) -0.0264(17) 0.0085(18) O8 0.099(2) 0.135(3) 0.088(2) -0.0099(18) -0.0263(17) 0.0156(19) O9 0.159(3) 0.0836(19) 0.110(2) -0.0348(18) -0.015(2) -0.0115(19) O10 0.102(2) 0.109(2) 0.151(3) -0.020(2) -0.013(2) -0.0206(19) N9 0.0357(9) 0.0280(8) 0.0368(9) -0.0071(7) -0.0091(8) -0.0008(7) N10 0.0342(9) 0.0285(8) 0.0341(9) -0.0090(7) -0.0063(7) -0.0008(7) N7 0.0381(10) 0.0275(8) 0.0375(9) -0.0087(7) -0.0093(8) -0.0005(7) N8 0.0341(9) 0.0279(8) 0.0350(9) -0.0068(7) -0.0063(7) -0.0007(7) N1 0.0480(12) 0.0393(10) 0.0436(11) -0.0105(9) 0.0010(9) 0.0052(9) N2 0.0632(17) 0.0645(16) 0.103(2) -0.0098(15) -0.0113(15) 0.0256(14) N3 0.0495(12) 0.0502(12) 0.0373(11) -0.0047(9) -0.0020(9) -0.0020(10) N4 0.0412(11) 0.0380(10) 0.0439(11) -0.0105(8) -0.0094(9) 0.0038(8) N5 0.0422(11) 0.0371(10) 0.0413(11) -0.0053(8) 0.0024(9) 0.0070(8) N6 0.0650(15) 0.0718(16) 0.0531(14) -0.0179(12) -0.0162(12) -0.0110(12) N11 0.0430(11) 0.0396(10) 0.0435(11) -0.0132(9) -0.0001(9) 0.0040(9) N12 0.0659(16) 0.0567(14) 0.0840(18) -0.0281(13) -0.0189(14) 0.0260(13) N13 0.0414(11) 0.0410(10) 0.0494(12) -0.0152(9) -0.0097(9) 0.0050(9) N14 0.0530(12) 0.0401(11) 0.0403(11) -0.0079(9) 0.0029(9) 0.0025(9) N16 0.0564(13) 0.0509(12) 0.0496(12) -0.0221(10) -0.0145(10) 0.0100(10) N15 0.0437(11) 0.0391(10) 0.0416(11) -0.0098(9) 0.0002(9) 0.0093(9) N17 0.0287(9) 0.0301(8) 0.0274(8) -0.0058(7) -0.0033(7) -0.0005(7) N18 0.0284(9) 0.0336(9) 0.0287(9) -0.0041(7) -0.0023(7) -0.0012(7) N19 0.0282(9) 0.0352(9) 0.0298(9) -0.0054(7) -0.0040(7) 0.0003(7) N20 0.0307(9) 0.0301(9) 0.0299(9) -0.0057(7) -0.0038(7) 0.0007(7) C67 0.0378(13) 0.0419(13) 0.0756(19) -0.0207(13) -0.0023(12) 0.0005(10) C72 0.0493(17) 0.0600(18) 0.112(3) -0.0342(18) -0.0189(17) 0.0011(14) C71 0.0500(18) 0.0573(19) 0.160(4) -0.035(2) -0.003(2) -0.0132(15) C70 0.066(2) 0.0551(19) 0.133(4) -0.018(2) 0.029(2) -0.0162(17) C69 0.072(2) 0.0512(17) 0.083(2) -0.0126(16) 0.0243(18) -0.0047(15) C68 0.0482(15) 0.0402(13) 0.0614(16) -0.0147(12) 0.0069(12) 0.0045(11) C79 0.080(2) 0.0585(16) 0.0363(14) -0.0105(12) -0.0018(13) 0.0124(15) C80 0.0691(18) 0.0599(16) 0.0433(14) -0.0240(12) -0.0143(13) 0.0222(14) C81 0.096(3) 0.101(3) 0.0545(18) -0.0382(18) -0.0285(18) 0.036(2) C82 0.089(3) 0.135(4) 0.094(3) -0.070(3) -0.047(2) 0.035(3) C83 0.087(3) 0.117(3) 0.107(3) -0.060(3) -0.041(2) 0.003(2) C84 0.067(2) 0.077(2) 0.084(2) -0.0381(18) -0.0215(17) -0.0032(16) C66 0.0498(14) 0.0420(13) 0.0457(13) -0.0148(11) -0.0118(11) 0.0081(11) C73 0.0580(16) 0.0528(15) 0.0544(15) -0.0214(13) -0.0213(13) 0.0126(12) C74 0.0595(16) 0.0501(14) 0.0405(13) -0.0149(11) -0.0120(12) 0.0186(12) C75 0.089(2) 0.071(2) 0.0430(15) -0.0143(14) -0.0132(15) 0.0181(17) C76 0.089(2) 0.072(2) 0.0452(16) -0.0075(15) 0.0014(16) 0.0242(18) C77 0.0621(19) 0.0530(17) 0.0667(19) 0.0002(14) 0.0189(15) 0.0085(14) C78 0.0507(15) 0.0464(14) 0.0563(16) -0.0074(12) 0.0060(12) 0.0025(12) C65 0.0390(12) 0.0366(11) 0.0377(12) -0.0098(9) -0.0004(9) 0.0018(10) C47 0.0441(13) 0.0340(11) 0.0382(12) -0.0059(9) -0.0123(10) -0.0006(9) C48 0.0593(16) 0.0464(14) 0.0452(14) 0.0005(11) -0.0216(12) -0.0140(12) C53 0.0704(19) 0.0697(19) 0.0567(17) -0.0198(14) -0.0244(15) 0.0025(15) C52 0.100(3) 0.098(3) 0.0564(19) -0.0261(18) -0.0275(18) -0.002(2) C51 0.135(4) 0.094(3) 0.063(2) 0.008(2) -0.051(2) -0.019(3) C50 0.149(4) 0.0558(19) 0.077(2) 0.0081(17) -0.057(3) -0.006(2) C49 0.101(3) 0.0529(17) 0.071(2) -0.0045(15) -0.0429(19) -0.0037(17) C54 0.0435(12) 0.0336(11) 0.0367(11) -0.0055(9) -0.0100(10) -0.0014(9) C55 0.0667(17) 0.0420(13) 0.0462(14) 0.0004(11) -0.0190(13) -0.0128(12) C56 0.0596(16) 0.0363(12) 0.0479(14) -0.0015(10) -0.0149(12) -0.0141(11) C57 0.0386(12) 0.0289(10) 0.0399(12) -0.0089(9) -0.0055(9) -0.0037(9) C58 0.0393(12) 0.0316(11) 0.0419(12) -0.0106(9) -0.0070(10) -0.0043(9) C59 0.0476(13) 0.0335(11) 0.0385(12) -0.0081(9) -0.0103(10) -0.0082(10) C60 0.0491(14) 0.0418(13) 0.0539(15) -0.0166(11) -0.0063(12) -0.0046(11) C61 0.0759(19) 0.0412(13) 0.0553(16) -0.0205(12) -0.0105(14) -0.0087(13) C62 0.077(2) 0.0467(14) 0.0478(15) -0.0119(12) -0.0166(14) -0.0247(14) C63 0.0482(15) 0.0648(18) 0.0636(17) -0.0126(14) -0.0173(13) -0.0150(13) C64 0.0466(14) 0.0457(14) 0.0647(17) -0.0146(12) -0.0115(12) -0.0023(11) C21 0.0422(12) 0.0351(11) 0.0412(12) -0.0118(10) -0.0099(10) -0.0035(9) C22 0.0655(17) 0.0492(14) 0.0518(15) -0.0111(12) -0.0231(13) -0.0157(13) C23 0.0666(17) 0.0492(14) 0.0457(14) -0.0081(11) -0.0251(13) -0.0103(13) C24 0.0429(12) 0.0342(11) 0.0375(11) -0.0101(9) -0.0113(10) 0.0018(9) C25 0.0417(12) 0.0344(11) 0.0379(12) -0.0073(9) -0.0111(10) 0.0031(9) C26 0.0494(14) 0.0380(12) 0.0423(13) -0.0075(10) -0.0156(11) 0.0022(10) C27 0.0600(18) 0.087(2) 0.0497(16) -0.0147(15) -0.0155(14) 0.0218(16) C28 0.068(2) 0.117(3) 0.067(2) -0.016(2) -0.0259(17) 0.033(2) C29 0.095(3) 0.087(2) 0.0497(17) -0.0091(16) -0.0298(17) 0.028(2) C30 0.078(2) 0.087(2) 0.0453(16) 0.0031(15) -0.0062(15) 0.0126(18) C31 0.0530(17) 0.076(2) 0.0532(16) -0.0018(14) -0.0094(13) 0.0049(14) C32 0.0442(13) 0.0306(11) 0.0396(12) -0.0045(9) -0.0108(10) -0.0006(9) C33 0.084(2) 0.0347(13) 0.0660(18) 0.0060(12) -0.0393(16) -0.0091(13) C34 0.0739(19) 0.0327(12) 0.0631(17) 0.0027(12) -0.0297(15) -0.0139(12) C35 0.0392(12) 0.0299(10) 0.0415(12) -0.0051(9) -0.0071(10) -0.0052(9) C36 0.0386(12) 0.0341(11) 0.0441(12) -0.0083(10) -0.0079(10) -0.0058(9) C37 0.0472(14) 0.0350(12) 0.0432(13) -0.0014(10) -0.0159(11) -0.0102(10) C38 0.0611(17) 0.0518(15) 0.0633(17) -0.0230(13) -0.0035(14) -0.0129(13) C39 0.087(2) 0.0522(16) 0.0670(19) -0.0224(14) -0.0126(17) -0.0205(15) C40 0.079(2) 0.0504(16) 0.0629(18) -0.0014(13) -0.0363(16) -0.0236(15) C41 0.0478(16) 0.0632(19) 0.097(2) -0.0068(17) -0.0253(16) -0.0136(14) C42 0.0474(15) 0.0491(15) 0.086(2) -0.0140(14) -0.0152(14) -0.0051(12) C43 0.0402(12) 0.0348(11) 0.0438(12) -0.0085(10) -0.0110(10) -0.0049(9) C44 0.0546(16) 0.0494(14) 0.0626(17) -0.0046(12) -0.0270(13) -0.0148(12) C45 0.0551(16) 0.0486(14) 0.0532(15) -0.0032(12) -0.0273(13) -0.0087(12) C46 0.0405(12) 0.0325(11) 0.0369(11) -0.0072(9) -0.0112(9) 0.0003(9) C1 0.0416(12) 0.0387(12) 0.0346(11) -0.0088(9) 0.0011(9) 0.0001(10) C14 0.092(3) 0.100(3) 0.088(3) -0.030(2) -0.026(2) -0.030(2) C13 0.150(5) 0.159(5) 0.112(4) -0.047(4) -0.047(3) -0.060(4) C12 0.166(5) 0.230(7) 0.103(4) -0.053(4) -0.054(4) -0.078(5) C11 0.136(4) 0.201(6) 0.061(2) -0.027(3) -0.034(3) -0.053(4) C10 0.083(2) 0.107(3) 0.0448(16) -0.0177(17) -0.0167(16) -0.016(2) C9 0.085(2) 0.091(2) 0.0338(14) -0.0009(14) -0.0063(14) -0.0177(19) C3 0.0422(13) 0.0426(13) 0.0534(15) -0.0046(11) 0.0013(11) 0.0010(11) C8 0.0576(18) 0.0540(17) 0.0690(19) -0.0002(14) 0.0111(15) -0.0034(14) C7 0.0566(19) 0.0521(18) 0.107(3) -0.0029(18) 0.0098(19) -0.0131(15) C6 0.0445(16) 0.0524(17) 0.134(3) -0.024(2) -0.0122(19) -0.0088(13) C5 0.0499(16) 0.0515(16) 0.092(2) -0.0232(16) -0.0210(15) 0.0027(13) C4 0.0365(12) 0.0379(12) 0.0607(16) -0.0118(11) -0.0080(11) 0.0035(10) C2 0.0440(14) 0.0465(14) 0.0545(15) -0.0013(12) -0.0077(12) 0.0081(11) C15 0.0598(16) 0.0499(14) 0.0448(14) -0.0175(11) -0.0147(12) 0.0093(12) C16 0.0609(16) 0.0462(14) 0.0393(13) -0.0137(11) -0.0080(11) 0.0155(12) C17 0.099(3) 0.0650(19) 0.0397(15) -0.0104(13) -0.0028(15) 0.0121(18) C18 0.097(3) 0.070(2) 0.0431(16) -0.0052(15) 0.0109(16) 0.0168(19) C19 0.0634(19) 0.0555(18) 0.071(2) 0.0063(15) 0.0248(16) 0.0054(15) C20 0.0485(15) 0.0506(15) 0.0631(17) -0.0056(13) 0.0069(13) 0.0031(12) C85 0.0332(11) 0.0336(11) 0.0318(10) -0.0064(9) -0.0022(8) -0.0024(8) C86 0.0372(12) 0.0452(12) 0.0286(11) -0.0021(9) 0.0005(9) -0.0053(10) C87 0.0425(13) 0.0421(12) 0.0306(11) -0.0008(9) -0.0053(9) -0.0025(10) C88 0.0357(11) 0.0345(11) 0.0287(10) -0.0042(8) -0.0069(9) 0.0022(9) C89 0.0345(11) 0.0359(11) 0.0318(11) -0.0069(9) -0.0069(9) 0.0015(9) C90 0.0343(11) 0.0497(13) 0.0312(11) -0.0058(10) -0.0070(9) -0.0028(10) C91 0.0473(15) 0.0728(18) 0.0494(15) -0.0253(13) -0.0101(12) 0.0006(13) C92 0.070(2) 0.105(3) 0.0432(15) -0.0313(16) -0.0088(14) -0.0178(18) C93 0.0644(19) 0.098(2) 0.0405(15) 0.0012(15) -0.0234(14) -0.0155(18) C94 0.0649(19) 0.071(2) 0.0626(19) 0.0009(15) -0.0302(16) 0.0085(15) C95 0.0585(16) 0.0571(16) 0.0461(14) -0.0096(12) -0.0188(12) 0.0113(13) C96 0.0309(11) 0.0383(11) 0.0341(11) -0.0087(9) -0.0070(9) 0.0024(9) C97 0.0306(11) 0.0540(14) 0.0401(12) -0.0102(11) -0.0088(9) 0.0011(10) C98 0.0272(11) 0.0551(14) 0.0411(12) -0.0099(11) -0.0046(9) -0.0005(10) C99 0.0280(10) 0.0366(11) 0.0347(11) -0.0089(9) -0.0025(8) -0.0017(8) C100 0.0302(11) 0.0363(11) 0.0347(11) -0.0094(9) -0.0007(9) -0.0021(9) C101 0.0298(11) 0.0462(12) 0.0331(11) -0.0069(9) -0.0026(9) -0.0021(9) C102 0.0523(16) 0.0584(17) 0.081(2) -0.0313(16) 0.0199(15) -0.0078(13) C103 0.062(2) 0.086(2) 0.095(3) -0.045(2) 0.0309(18) -0.0051(18) C104 0.0406(15) 0.101(3) 0.0624(19) -0.0243(18) 0.0166(13) -0.0167(16) C105 0.0618(19) 0.078(2) 0.0670(19) -0.0208(17) 0.0108(15) -0.0355(16) C106 0.0562(16) 0.0606(17) 0.0602(17) -0.0273(14) 0.0122(13) -0.0157(13) C107 0.0343(11) 0.0333(10) 0.0295(10) -0.0057(8) -0.0002(8) -0.0017(8) C108 0.0388(12) 0.0426(12) 0.0302(11) -0.0026(9) 0.0010(9) -0.0052(10) C109 0.0440(13) 0.0409(12) 0.0281(10) -0.0013(9) -0.0060(9) -0.0016(10) C110 0.0361(11) 0.0295(10) 0.0289(10) -0.0051(8) -0.0055(8) -0.0003(8) C111 0.0372(11) 0.0330(10) 0.0310(10) -0.0077(9) -0.0097(9) 0.0022(9) C112 0.0541(15) 0.0542(15) 0.0411(13) -0.0141(11) -0.0104(11) -0.0030(12) C113 0.076(2) 0.0696(18) 0.0366(13) -0.0156(13) -0.0141(13) -0.0137(15) C114 0.0584(17) 0.0723(18) 0.0396(14) 0.0010(13) -0.0231(12) -0.0106(14) C115 0.0500(15) 0.0600(16) 0.0512(15) 0.0015(13) -0.0192(12) 0.0037(12) C116 0.0493(14) 0.0476(13) 0.0402(13) -0.0077(11) -0.0135(11) 0.0047(11) C117 0.0376(12) 0.0440(12) 0.0301(11) -0.0040(9) -0.0078(9) -0.0060(10) C118 0.0297(10) 0.0323(10) 0.0349(11) -0.0094(9) -0.0080(8) 0.0005(8) C119 0.0330(11) 0.0430(12) 0.0390(12) -0.0084(10) -0.0114(9) 0.0012(9) C120 0.0273(10) 0.0438(12) 0.0407(12) -0.0110(10) -0.0039(9) -0.0016(9) C121 0.0294(10) 0.0316(10) 0.0345(11) -0.0104(8) -0.0046(8) -0.0013(8) C122 0.0298(10) 0.0338(10) 0.0336(11) -0.0096(9) -0.0024(8) -0.0021(8) C123 0.0293(10) 0.0406(12) 0.0327(11) -0.0073(9) -0.0028(9) -0.0018(9) C124 0.0508(16) 0.0579(16) 0.0712(19) -0.0346(15) 0.0151(14) -0.0112(13) C125 0.0593(19) 0.083(2) 0.080(2) -0.0419(19) 0.0247(16) -0.0041(16) C126 0.0385(14) 0.084(2) 0.0562(17) -0.0138(16) 0.0131(12) -0.0099(14) C127 0.0481(15) 0.0654(17) 0.0514(15) -0.0095(13) 0.0011(12) -0.0239(13) C128 0.0456(14) 0.0491(14) 0.0434(13) -0.0162(11) 0.0029(11) -0.0116(11) C129 0.127(3) 0.0564(19) 0.073(2) -0.0327(17) 0.018(2) -0.0106(19) C130 0.097(3) 0.0644(19) 0.075(2) -0.0412(17) 0.0085(19) -0.0057(18) C131 0.111(4) 0.195(6) 0.197(7) -0.116(6) 0.001(4) 0.019(4) C132 0.208(7) 0.132(5) 0.164(6) -0.049(4) 0.045(5) 0.049(5) C133 0.171(6) 0.170(5) 0.129(4) -0.081(4) -0.056(4) 0.059(4) C134 0.146(5) 0.147(5) 0.184(6) -0.055(5) -0.043(5) 0.030(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 Cr1 N3 1.963(2) . ? Cr1 N4 1.968(2) . ? Cr1 N6 2.068(2) . ? Cr1 C2 2.075(3) . ? Cr1 N5 2.093(2) . ? Cr1 C1 2.105(2) . ? Cr2 N13 1.970(2) . ? Cr2 N14 1.970(2) . ? Cr2 C66 2.081(2) . ? Cr2 N16 2.083(2) . ? Cr2 N15 2.093(2) . ? Cr2 C65 2.112(2) . ? Mn1 N9 2.0054(17) . ? Mn1 N7 2.0099(18) . ? Mn1 N10 2.0205(17) . ? Mn1 N8 2.0238(17) . ? Mn1 N1 2.314(2) . ? Mn1 N11 2.326(2) . ? Mn2 N20 2.0098(17) . ? Mn2 N18 2.0101(17) . ? Mn2 N19 2.0124(17) . ? Mn2 N17 2.0135(17) . ? Mn2 O6 2.2565(16) . ? Mn2 O5 2.2762(17) . ? O1 C15 1.251(3) . ? O2 C9 1.221(4) . ? O3 C79 1.229(3) . ? O4 C73 1.250(3) . ? O5 C129 1.415(4) . ? O5 H135 0.76(3) . ? O6 C130 1.410(3) . ? O6 H136 0.78(3) . ? O7 C131 1.383(6) . ? O7 H7 0.8200 . ? O8 C132 1.367(6) . ? O8 H8 0.8200 . ? O9 C133 1.429(6) . ? O9 H9 0.8200 . ? O10 C134 1.398(6) . ? O10 H10 0.8200 . ? N9 C43 1.380(3) . ? N9 C46 1.380(3) . ? N10 C54 1.376(3) . ? N10 C57 1.378(3) . ? N7 C21 1.378(3) . ? N7 C24 1.378(3) . ? N8 C32 1.373(3) . ? N8 C35 1.374(3) . ? N1 C1 1.142(3) . ? N2 C2 1.146(4) . ? N3 C9 1.339(4) . ? N3 C3 1.407(3) . ? N4 C15 1.326(3) . ? N4 C4 1.414(3) . ? N5 C20 1.334(3) . ? N5 C16 1.355(3) . ? N6 C14 1.345(4) . ? N6 C10 1.345(4) . ? N11 C65 1.141(3) . ? N12 C66 1.141(3) . ? N13 C73 1.324(3) . ? N13 C67 1.418(3) . ? N14 C79 1.343(4) . ? N14 C68 1.404(4) . ? N16 C84 1.338(4) . ? N16 C80 1.349(3) . ? N15 C78 1.332(3) . ? N15 C74 1.353(3) . ? N17 C121 1.378(3) . ? N17 C118 1.381(3) . ? N18 C85 1.381(3) . ? N18 C88 1.382(3) . ? N19 C96 1.375(3) . ? N19 C99 1.380(3) . ? N20 C110 1.383(3) . ? N20 C107 1.385(3) . ? C67 C72 1.401(4) . ? C67 C68 1.402(4) . ? C72 C71 1.388(5) . ? C72 H2 0.9300 . ? C71 C70 1.362(6) . ? C71 H3 0.9300 . ? C70 C69 1.367(6) . ? C70 H4 0.9300 . ? C69 C68 1.402(4) . ? C69 H5 0.9300 . ? C79 C80 1.496(4) . ? C80 C81 1.386(4) . ? C81 C82 1.390(6) . ? C81 H9A 0.9300 . ? C82 C83 1.355(6) . ? C82 H10A 0.9300 . ? C83 C84 1.384(5) . ? C83 H11 0.9300 . ? C84 H12 0.9300 . ? C73 C74 1.493(4) . ? C74 C75 1.380(4) . ? C75 C76 1.370(5) . ? C75 H16 0.9300 . ? C76 C77 1.355(5) . ? C76 H17 0.9300 . ? C77 C78 1.405(4) . ? C77 H18 0.9300 . ? C78 H19 0.9300 . ? C47 C54 1.396(3) . ? C47 C46 1.398(3) . ? C47 C48 1.494(3) . ? C48 C49 1.345(4) . ? C48 C53 1.422(4) . ? C53 C52 1.384(4) . ? C53 H23 0.9300 . ? C52 C51 1.385(5) . ? C52 H24 0.9300 . ? C51 C50 1.310(6) . ? C51 H25 0.9300 . ? C50 C49 1.400(4) . ? C50 H26 0.9300 . ? C49 H27 0.9300 . ? C54 C55 1.438(3) . ? C55 C56 1.340(4) . ? C55 H29 0.9300 . ? C56 C57 1.434(3) . ? C56 H30 0.9300 . ? C57 C58 1.391(3) . ? C58 C21 1.401(3) . ? C58 C59 1.501(3) . ? C59 C64 1.384(4) . ? C59 C60 1.385(3) . ? C60 C61 1.388(3) . ? C60 H34 0.9300 . ? C61 C62 1.362(4) . ? C61 H35 0.9300 . ? C62 C63 1.376(4) . ? C62 H36 0.9300 . ? C63 C64 1.380(4) . ? C63 H37 0.9300 . ? C64 H38 0.9300 . ? C21 C22 1.427(3) . ? C22 C23 1.347(4) . ? C22 H40 0.9300 . ? C23 C24 1.431(3) . ? C23 H41 0.9300 . ? C24 C25 1.396(3) . ? C25 C32 1.399(3) . ? C25 C26 1.496(3) . ? C26 C31 1.366(4) . ? C26 C27 1.387(4) . ? C27 C28 1.384(4) . ? C27 H45 0.9300 . ? C28 C29 1.365(5) . ? C28 H46 0.9300 . ? C29 C30 1.346(5) . ? C29 H47 0.9300 . ? C30 C31 1.392(4) . ? C30 H48 0.9300 . ? C31 H49 0.9300 . ? C32 C33 1.426(3) . ? C33 C34 1.342(4) . ? C33 H51 0.9300 . ? C34 C35 1.431(3) . ? C34 H52 0.9300 . ? C35 C36 1.390(3) . ? C36 C43 1.393(3) . ? C36 C37 1.503(3) . ? C37 C42 1.378(4) . ? C37 C38 1.386(4) . ? C38 C39 1.394(4) . ? C38 H56 0.9300 . ? C39 C40 1.364(5) . ? C39 H57 0.9300 . ? C40 C41 1.369(5) . ? C40 H58 0.9300 . ? C41 C42 1.393(4) . ? C41 H59 0.9300 . ? C42 H60 0.9300 . ? C43 C44 1.431(3) . ? C44 C45 1.344(4) . ? C44 H62 0.9300 . ? C45 C46 1.435(3) . ? C45 H63 0.9300 . ? C14 C13 1.376(5) . ? C14 H66 0.9300 . ? C13 C12 1.350(7) . ? C13 H67 0.9300 . ? C12 C11 1.395(7) . ? C12 H68 0.9300 . ? C11 C10 1.387(5) . ? C11 H69 0.9300 . ? C10 C9 1.494(5) . ? C3 C8 1.400(4) . ? C3 C4 1.404(4) . ? C8 C7 1.370(5) . ? C8 H73 0.9300 . ? C7 C6 1.363(5) . ? C7 H74 0.9300 . ? C6 C5 1.395(5) . ? C6 H75 0.9300 . ? C5 C4 1.390(4) . ? C5 H76 0.9300 . ? C15 C16 1.493(4) . ? C16 C17 1.384(4) . ? C17 C18 1.363(5) . ? C17 H81 0.9300 . ? C18 C19 1.360(5) . ? C18 H82 0.9300 . ? C19 C20 1.406(4) . ? C19 H83 0.9300 . ? C20 H84 0.9300 . ? C85 C122 1.394(3) . ? C85 C86 1.433(3) . ? C86 C87 1.339(3) . ? C86 H86 0.9300 . ? C87 C88 1.434(3) . ? C87 H87 0.9300 . ? C88 C89 1.393(3) . ? C89 C96 1.398(3) . ? C89 C90 1.494(3) . ? C90 C91 1.385(4) . ? C90 C95 1.387(4) . ? C91 C92 1.383(4) . ? C91 H91 0.9300 . ? C92 C93 1.376(5) . ? C92 H92 0.9300 . ? C93 C94 1.358(5) . ? C93 H93 0.9300 . ? C94 C95 1.386(4) . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? C96 C97 1.430(3) . ? C97 C98 1.341(3) . ? C97 H97 0.9300 . ? C98 C99 1.431(3) . ? C98 H98 0.9300 . ? C99 C100 1.391(3) . ? C100 C107 1.396(3) . ? C100 C101 1.501(3) . ? C101 C106 1.377(3) . ? C101 C102 1.382(4) . ? C102 C103 1.389(4) . ? C102 H102 0.9300 . ? C103 C104 1.355(5) . ? C103 H103 0.9300 . ? C104 C105 1.363(5) . ? C104 H104 0.9300 . ? C105 C106 1.390(4) . ? C105 H105 0.9300 . ? C106 H106 0.9300 . ? C107 C108 1.425(3) . ? C108 C109 1.346(3) . ? C108 H108 0.9300 . ? C109 C110 1.433(3) . ? C109 H109 0.9300 . ? C110 C111 1.396(3) . ? C111 C118 1.394(3) . ? C111 C117 1.496(3) . ? C112 C117 1.391(3) . ? C112 C113 1.392(4) . ? C112 H112 0.9300 . ? C113 C114 1.373(4) . ? C113 H113 0.9300 . ? C114 C115 1.371(4) . ? C114 H114 0.9300 . ? C115 C116 1.387(3) . ? C115 H115 0.9300 . ? C116 C117 1.391(3) . ? C116 H116 0.9300 . ? C118 C119 1.434(3) . ? C119 C120 1.340(3) . ? C119 H119 0.9300 . ? C120 C121 1.433(3) . ? C120 H120 0.9300 . ? C121 C122 1.389(3) . ? C122 C123 1.504(3) . ? C123 C128 1.379(3) . ? C123 C124 1.394(3) . ? C124 C125 1.389(4) . ? C124 H124 0.9300 . ? C125 C126 1.360(5) . ? C125 H125 0.9300 . ? C126 C127 1.365(4) . ? C126 H126 0.9300 . ? C127 C128 1.389(4) . ? C127 H127 0.9300 . ? C128 H128 0.9300 . ? C129 H12A 0.9600 . ? C129 H12B 0.9600 . ? C129 H12C 0.9600 . ? C130 H13A 0.9600 . ? C130 H13B 0.9600 . ? C130 H13C 0.9600 . ? C131 H13D 0.9600 . ? C131 H13E 0.9600 . ? C131 H13F 0.9600 . ? C132 H13G 0.9600 . ? C132 H13H 0.9600 . ? C132 H13I 0.9600 . ? C133 H13J 0.9600 . ? C133 H13K 0.9600 . ? C133 H13L 0.9600 . ? C134 H13M 0.9600 . ? C134 H13N 0.9600 . ? C134 H13O 0.9600 . ? 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 N3 Cr1 N4 81.50(9) . . ? N3 Cr1 N6 80.30(10) . . ? N4 Cr1 N6 161.81(9) . . ? N3 Cr1 C2 91.29(10) . . ? N4 Cr1 C2 92.27(10) . . ? N6 Cr1 C2 88.46(11) . . ? N3 Cr1 N5 161.66(9) . . ? N4 Cr1 N5 80.18(8) . . ? N6 Cr1 N5 118.01(9) . . ? C2 Cr1 N5 88.47(9) . . ? N3 Cr1 C1 94.75(9) . . ? N4 Cr1 C1 95.01(9) . . ? N6 Cr1 C1 86.20(10) . . ? C2 Cr1 C1 171.16(10) . . ? N5 Cr1 C1 87.82(8) . . ? N13 Cr2 N14 81.45(9) . . ? N13 Cr2 C66 93.01(9) . . ? N14 Cr2 C66 92.69(9) . . ? N13 Cr2 N16 161.24(9) . . ? N14 Cr2 N16 79.98(9) . . ? C66 Cr2 N16 85.20(9) . . ? N13 Cr2 N15 80.13(9) . . ? N14 Cr2 N15 161.55(9) . . ? C66 Cr2 N15 87.29(9) . . ? N16 Cr2 N15 118.36(9) . . ? N13 Cr2 C65 93.36(9) . . ? N14 Cr2 C65 95.25(9) . . ? C66 Cr2 C65 170.48(10) . . ? N16 Cr2 C65 91.00(9) . . ? N15 Cr2 C65 86.85(8) . . ? N9 Mn1 N7 179.16(7) . . ? N9 Mn1 N10 89.39(7) . . ? N7 Mn1 N10 90.54(7) . . ? N9 Mn1 N8 90.17(7) . . ? N7 Mn1 N8 89.90(7) . . ? N10 Mn1 N8 179.55(7) . . ? N9 Mn1 N1 90.72(8) . . ? N7 Mn1 N1 88.44(8) . . ? N10 Mn1 N1 84.85(7) . . ? N8 Mn1 N1 95.07(7) . . ? N9 Mn1 N11 92.36(7) . . ? N7 Mn1 N11 88.47(7) . . ? N10 Mn1 N11 96.06(7) . . ? N8 Mn1 N11 84.03(7) . . ? N1 Mn1 N11 176.79(7) . . ? N20 Mn2 N18 179.71(7) . . ? N20 Mn2 N19 90.65(7) . . ? N18 Mn2 N19 89.63(7) . . ? N20 Mn2 N17 89.57(7) . . ? N18 Mn2 N17 90.15(7) . . ? N19 Mn2 N17 179.22(7) . . ? N20 Mn2 O6 87.71(7) . . ? N18 Mn2 O6 92.22(7) . . ? N19 Mn2 O6 90.10(7) . . ? N17 Mn2 O6 89.15(7) . . ? N20 Mn2 O5 90.86(7) . . ? N18 Mn2 O5 89.21(7) . . ? N19 Mn2 O5 88.44(7) . . ? N17 Mn2 O5 92.31(7) . . ? O6 Mn2 O5 177.95(6) . . ? C129 O5 Mn2 122.87(17) . . ? C129 O5 H135 110(2) . . ? Mn2 O5 H135 105(2) . . ? C130 O6 Mn2 122.41(17) . . ? C130 O6 H136 108(2) . . ? Mn2 O6 H136 106(2) . . ? C131 O7 H7 109.5 . . ? C132 O8 H8 109.5 . . ? C133 O9 H9 109.5 . . ? C134 O10 H10 109.5 . . ? C43 N9 C46 106.49(17) . . ? C43 N9 Mn1 126.35(14) . . ? C46 N9 Mn1 127.02(14) . . ? C54 N10 C57 106.51(17) . . ? C54 N10 Mn1 127.41(14) . . ? C57 N10 Mn1 126.08(14) . . ? C21 N7 C24 106.35(18) . . ? C21 N7 Mn1 126.49(14) . . ? C24 N7 Mn1 126.82(14) . . ? C32 N8 C35 106.16(17) . . ? C32 N8 Mn1 126.35(14) . . ? C35 N8 Mn1 126.26(14) . . ? C1 N1 Mn1 158.61(18) . . ? C9 N3 C3 125.5(2) . . ? C9 N3 Cr1 118.7(2) . . ? C3 N3 Cr1 115.15(17) . . ? C15 N4 C4 126.4(2) . . ? C15 N4 Cr1 118.90(17) . . ? C4 N4 Cr1 114.69(16) . . ? C20 N5 C16 118.6(2) . . ? C20 N5 Cr1 130.2(2) . . ? C16 N5 Cr1 111.14(16) . . ? C14 N6 C10 119.3(3) . . ? C14 N6 Cr1 129.0(2) . . ? C10 N6 Cr1 111.7(2) . . ? C65 N11 Mn1 159.33(18) . . ? C73 N13 C67 126.5(2) . . ? C73 N13 Cr2 118.95(18) . . ? C67 N13 Cr2 114.49(17) . . ? C79 N14 C68 125.2(2) . . ? C79 N14 Cr2 119.1(2) . . ? C68 N14 Cr2 115.09(17) . . ? C84 N16 C80 118.7(3) . . ? C84 N16 Cr2 129.1(2) . . ? C80 N16 Cr2 111.83(18) . . ? C78 N15 C74 118.7(2) . . ? C78 N15 Cr2 130.3(2) . . ? C74 N15 Cr2 111.00(17) . . ? C121 N17 C118 106.32(16) . . ? C121 N17 Mn2 126.16(13) . . ? C118 N17 Mn2 127.43(14) . . ? C85 N18 C88 105.67(17) . . ? C85 N18 Mn2 127.19(14) . . ? C88 N18 Mn2 127.13(14) . . ? C96 N19 C99 106.43(17) . . ? C96 N19 Mn2 127.50(14) . . ? C99 N19 Mn2 126.06(14) . . ? C110 N20 C107 105.66(16) . . ? C110 N20 Mn2 127.53(14) . . ? C107 N20 Mn2 126.79(14) . . ? C72 C67 C68 119.6(3) . . ? C72 C67 N13 125.8(3) . . ? C68 C67 N13 114.5(2) . . ? C71 C72 C67 118.5(4) . . ? C71 C72 H2 120.7 . . ? C67 C72 H2 120.7 . . ? C70 C71 C72 121.7(3) . . ? C70 C71 H3 119.1 . . ? C72 C71 H3 119.1 . . ? C71 C70 C69 120.7(3) . . ? C71 C70 H4 119.6 . . ? C69 C70 H4 119.6 . . ? C70 C69 C68 119.6(4) . . ? C70 C69 H5 120.2 . . ? C68 C69 H5 120.2 . . ? C69 C68 C67 119.8(3) . . ? C69 C68 N14 125.8(3) . . ? C67 C68 N14 114.4(2) . . ? O3 C79 N14 128.8(3) . . ? O3 C79 C80 119.6(3) . . ? N14 C79 C80 111.6(2) . . ? N16 C80 C81 121.6(3) . . ? N16 C80 C79 117.2(2) . . ? C81 C80 C79 121.1(3) . . ? C80 C81 C82 118.6(3) . . ? C80 C81 H9A 120.7 . . ? C82 C81 H9A 120.7 . . ? C83 C82 C81 119.6(3) . . ? C83 C82 H10A 120.2 . . ? C81 C82 H10A 120.2 . . ? C82 C83 C84 119.3(4) . . ? C82 C83 H11 120.4 . . ? C84 C83 H11 120.4 . . ? N16 C84 C83 122.1(4) . . ? N16 C84 H12 118.9 . . ? C83 C84 H12 118.9 . . ? N12 C66 Cr2 175.4(2) . . ? O4 C73 N13 127.7(3) . . ? O4 C73 C74 120.1(3) . . ? N13 C73 C74 112.2(2) . . ? N15 C74 C75 121.4(3) . . ? N15 C74 C73 117.3(2) . . ? C75 C74 C73 121.3(3) . . ? C76 C75 C74 119.9(3) . . ? C76 C75 H16 120.1 . . ? C74 C75 H16 120.1 . . ? C77 C76 C75 119.0(3) . . ? C77 C76 H17 120.5 . . ? C75 C76 H17 120.5 . . ? C76 C77 C78 119.5(3) . . ? C76 C77 H18 120.3 . . ? C78 C77 H18 120.3 . . ? N15 C78 C77 121.5(3) . . ? N15 C78 H19 119.3 . . ? C77 C78 H19 119.3 . . ? N11 C65 Cr2 177.1(2) . . ? C54 C47 C46 122.6(2) . . ? C54 C47 C48 120.3(2) . . ? C46 C47 C48 117.1(2) . . ? C49 C48 C53 117.7(3) . . ? C49 C48 C47 124.2(3) . . ? C53 C48 C47 118.0(2) . . ? C52 C53 C48 120.5(3) . . ? C52 C53 H23 119.7 . . ? C48 C53 H23 119.7 . . ? C53 C52 C51 118.8(3) . . ? C53 C52 H24 120.6 . . ? C51 C52 H24 120.6 . . ? C50 C51 C52 120.5(3) . . ? C50 C51 H25 119.7 . . ? C52 C51 H25 119.7 . . ? C51 C50 C49 121.8(3) . . ? C51 C50 H26 119.1 . . ? C49 C50 H26 119.1 . . ? C48 C49 C50 120.6(3) . . ? C48 C49 H27 119.7 . . ? C50 C49 H27 119.7 . . ? N10 C54 C47 126.1(2) . . ? N10 C54 C55 109.05(19) . . ? C47 C54 C55 124.8(2) . . ? C56 C55 C54 107.5(2) . . ? C56 C55 H29 126.2 . . ? C54 C55 H29 126.3 . . ? C55 C56 C57 107.6(2) . . ? C55 C56 H30 126.2 . . ? C57 C56 H30 126.2 . . ? N10 C57 C58 126.24(19) . . ? N10 C57 C56 109.19(19) . . ? C58 C57 C56 124.5(2) . . ? C57 C58 C21 124.3(2) . . ? C57 C58 C59 119.15(19) . . ? C21 C58 C59 116.53(19) . . ? C64 C59 C60 118.2(2) . . ? C64 C59 C58 121.7(2) . . ? C60 C59 C58 120.0(2) . . ? C59 C60 C61 120.2(3) . . ? C59 C60 H34 119.9 . . ? C61 C60 H34 119.9 . . ? C62 C61 C60 121.0(3) . . ? C62 C61 H35 119.5 . . ? C60 C61 H35 119.5 . . ? C61 C62 C63 119.3(2) . . ? C61 C62 H36 120.4 . . ? C63 C62 H36 120.4 . . ? C62 C63 C64 120.3(3) . . ? C62 C63 H37 119.9 . . ? C64 C63 H37 119.9 . . ? C63 C64 C59 121.0(3) . . ? C63 C64 H38 119.5 . . ? C59 C64 H38 119.5 . . ? N7 C21 C58 125.8(2) . . ? N7 C21 C22 109.4(2) . . ? C58 C21 C22 124.8(2) . . ? C23 C22 C21 107.5(2) . . ? C23 C22 H40 126.2 . . ? C21 C22 H40 126.2 . . ? C22 C23 C24 107.4(2) . . ? C22 C23 H41 126.3 . . ? C24 C23 H41 126.3 . . ? N7 C24 C25 126.3(2) . . ? N7 C24 C23 109.29(19) . . ? C25 C24 C23 124.4(2) . . ? C24 C25 C32 123.4(2) . . ? C24 C25 C26 117.5(2) . . ? C32 C25 C26 119.1(2) . . ? C31 C26 C27 117.5(2) . . ? C31 C26 C25 123.1(2) . . ? C27 C26 C25 119.5(2) . . ? C28 C27 C26 121.1(3) . . ? C28 C27 H45 119.5 . . ? C26 C27 H45 119.5 . . ? C29 C28 C27 119.7(3) . . ? C29 C28 H46 120.1 . . ? C27 C28 H46 120.1 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H47 119.9 . . ? C28 C29 H47 119.9 . . ? C29 C30 C31 120.0(3) . . ? C29 C30 H48 120.0 . . ? C31 C30 H48 120.0 . . ? C26 C31 C30 121.3(3) . . ? C26 C31 H49 119.3 . . ? C30 C31 H49 119.3 . . ? N8 C32 C25 126.13(19) . . ? N8 C32 C33 109.6(2) . . ? C25 C32 C33 124.3(2) . . ? C34 C33 C32 107.6(2) . . ? C34 C33 H51 126.2 . . ? C32 C33 H51 126.2 . . ? C33 C34 C35 107.2(2) . . ? C33 C34 H52 126.4 . . ? C35 C34 H52 126.4 . . ? N8 C35 C36 125.75(19) . . ? N8 C35 C34 109.5(2) . . ? C36 C35 C34 124.8(2) . . ? C35 C36 C43 124.0(2) . . ? C35 C36 C37 119.1(2) . . ? C43 C36 C37 116.7(2) . . ? C42 C37 C38 118.6(2) . . ? C42 C37 C36 122.1(2) . . ? C38 C37 C36 119.2(2) . . ? C37 C38 C39 120.6(3) . . ? C37 C38 H56 119.7 . . ? C39 C38 H56 119.7 . . ? C40 C39 C38 120.2(3) . . ? C40 C39 H57 119.9 . . ? C38 C39 H57 119.9 . . ? C39 C40 C41 119.6(3) . . ? C39 C40 H58 120.2 . . ? C41 C40 H58 120.2 . . ? C40 C41 C42 120.9(3) . . ? C40 C41 H59 119.6 . . ? C42 C41 H59 119.6 . . ? C37 C42 C41 120.1(3) . . ? C37 C42 H60 120.0 . . ? C41 C42 H60 120.0 . . ? N9 C43 C36 126.0(2) . . ? N9 C43 C44 109.0(2) . . ? C36 C43 C44 124.8(2) . . ? C45 C44 C43 107.9(2) . . ? C45 C44 H62 126.1 . . ? C43 C44 H62 126.1 . . ? C44 C45 C46 107.4(2) . . ? C44 C45 H63 126.3 . . ? C46 C45 H63 126.3 . . ? N9 C46 C47 126.8(2) . . ? N9 C46 C45 109.14(19) . . ? C47 C46 C45 124.1(2) . . ? N1 C1 Cr1 174.5(2) . . ? N6 C14 C13 121.9(4) . . ? N6 C14 H66 119.0 . . ? C13 C14 H66 119.0 . . ? C12 C13 C14 119.5(4) . . ? C12 C13 H67 120.3 . . ? C14 C13 H67 120.3 . . ? C13 C12 C11 119.5(4) . . ? C13 C12 H68 120.3 . . ? C11 C12 H68 120.3 . . ? C10 C11 C12 119.0(4) . . ? C10 C11 H69 120.5 . . ? C12 C11 H69 120.5 . . ? N6 C10 C11 120.8(4) . . ? N6 C10 C9 117.2(3) . . ? C11 C10 C9 121.9(3) . . ? O2 C9 N3 128.7(3) . . ? O2 C9 C10 119.9(3) . . ? N3 C9 C10 111.5(2) . . ? C8 C3 C4 120.1(3) . . ? C8 C3 N3 125.6(3) . . ? C4 C3 N3 114.3(2) . . ? C7 C8 C3 119.2(3) . . ? C7 C8 H73 120.4 . . ? C3 C8 H73 120.4 . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H74 119.4 . . ? C8 C7 H74 119.4 . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H75 119.4 . . ? C5 C6 H75 119.4 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H76 120.6 . . ? C6 C5 H76 120.6 . . ? C5 C4 C3 119.6(3) . . ? C5 C4 N4 126.1(3) . . ? C3 C4 N4 114.3(2) . . ? N2 C2 Cr1 176.5(3) . . ? O1 C15 N4 127.9(3) . . ? O1 C15 C16 119.6(2) . . ? N4 C15 C16 112.5(2) . . ? N5 C16 C17 121.5(3) . . ? N5 C16 C15 117.0(2) . . ? C17 C16 C15 121.5(3) . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H81 120.0 . . ? C16 C17 H81 120.0 . . ? C19 C18 C17 118.8(3) . . ? C19 C18 H82 120.6 . . ? C17 C18 H82 120.6 . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H83 120.0 . . ? C20 C19 H83 120.0 . . ? N5 C20 C19 121.2(3) . . ? N5 C20 H84 119.4 . . ? C19 C20 H84 119.4 . . ? N18 C85 C122 125.47(19) . . ? N18 C85 C86 109.95(18) . . ? C122 C85 C86 124.5(2) . . ? C87 C86 C85 107.05(19) . . ? C87 C86 H86 126.5 . . ? C85 C86 H86 126.5 . . ? C86 C87 C88 107.98(19) . . ? C86 C87 H87 126.0 . . ? C88 C87 H87 126.0 . . ? N18 C88 C89 126.11(19) . . ? N18 C88 C87 109.31(19) . . ? C89 C88 C87 124.58(19) . . ? C88 C89 C96 123.57(19) . . ? C88 C89 C90 117.91(19) . . ? C96 C89 C90 118.50(19) . . ? C91 C90 C95 118.6(2) . . ? C91 C90 C89 119.9(2) . . ? C95 C90 C89 121.4(2) . . ? C92 C91 C90 120.6(3) . . ? C92 C91 H91 119.7 . . ? C90 C91 H91 119.7 . . ? C93 C92 C91 120.0(3) . . ? C93 C92 H92 120.0 . . ? C91 C92 H92 120.0 . . ? C94 C93 C92 120.0(3) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.6(3) . . ? C93 C94 H94 119.7 . . ? C95 C94 H94 119.7 . . ? C94 C95 C90 120.1(3) . . ? C94 C95 H95 119.9 . . ? C90 C95 H95 119.9 . . ? N19 C96 C89 125.89(19) . . ? N19 C96 C97 109.22(19) . . ? C89 C96 C97 124.9(2) . . ? C98 C97 C96 107.7(2) . . ? C98 C97 H97 126.2 . . ? C96 C97 H97 126.2 . . ? C97 C98 C99 107.5(2) . . ? C97 C98 H98 126.2 . . ? C99 C98 H98 126.2 . . ? N19 C99 C100 126.61(19) . . ? N19 C99 C98 109.09(18) . . ? C100 C99 C98 124.28(19) . . ? C99 C100 C107 124.28(19) . . ? C99 C100 C101 117.48(19) . . ? C107 C100 C101 118.25(19) . . ? C106 C101 C102 118.3(2) . . ? C106 C101 C100 121.2(2) . . ? C102 C101 C100 120.5(2) . . ? C101 C102 C103 120.0(3) . . ? C101 C102 H102 120.0 . . ? C103 C102 H102 120.0 . . ? C104 C103 C102 121.1(3) . . ? C104 C103 H103 119.4 . . ? C102 C103 H103 119.4 . . ? C103 C104 C105 119.5(3) . . ? C103 C104 H104 120.2 . . ? C105 C104 H104 120.2 . . ? C104 C105 C106 120.2(3) . . ? C104 C105 H105 119.9 . . ? C106 C105 H105 119.9 . . ? C101 C106 C105 120.9(3) . . ? C101 C106 H106 119.6 . . ? C105 C106 H106 119.6 . . ? N20 C107 C100 125.53(19) . . ? N20 C107 C108 109.93(18) . . ? C100 C107 C108 124.5(2) . . ? C109 C108 C107 107.33(19) . . ? C109 C108 H108 126.3 . . ? C107 C108 H108 126.3 . . ? C108 C109 C110 107.68(19) . . ? C108 C109 H109 126.2 . . ? C110 C109 H109 126.2 . . ? N20 C110 C111 125.68(18) . . ? N20 C110 C109 109.37(18) . . ? C111 C110 C109 124.93(19) . . ? C118 C111 C110 123.87(19) . . ? C118 C111 C117 117.77(19) . . ? C110 C111 C117 118.36(19) . . ? C117 C112 C113 120.3(3) . . ? C117 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C114 C113 C112 120.3(3) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 120.0(2) . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 120.3(3) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C117 120.6(3) . . ? C115 C116 H116 119.7 . . ? C117 C116 H116 119.7 . . ? C112 C117 C116 118.4(2) . . ? C112 C117 C111 120.3(2) . . ? C116 C117 C111 121.2(2) . . ? N17 C118 C111 125.85(19) . . ? N17 C118 C119 109.22(18) . . ? C111 C118 C119 124.92(19) . . ? C120 C119 C118 107.48(19) . . ? C120 C119 H119 126.3 . . ? C118 C119 H119 126.3 . . ? C119 C120 C121 107.75(19) . . ? C119 C120 H120 126.1 . . ? C121 C120 H120 126.1 . . ? N17 C121 C122 126.77(18) . . ? N17 C121 C120 109.18(18) . . ? C122 C121 C120 124.02(19) . . ? C121 C122 C85 123.93(19) . . ? C121 C122 C123 118.30(18) . . ? C85 C122 C123 117.74(18) . . ? C128 C123 C124 118.4(2) . . ? C128 C123 C122 121.5(2) . . ? C124 C123 C122 120.1(2) . . ? C125 C124 C123 119.8(3) . . ? C125 C124 H124 120.1 . . ? C123 C124 H124 120.1 . . ? C126 C125 C124 120.8(3) . . ? C126 C125 H125 119.6 . . ? C124 C125 H125 119.6 . . ? C125 C126 C127 120.1(3) . . ? C125 C126 H126 119.9 . . ? C127 C126 H126 119.9 . . ? C126 C127 C128 119.9(3) . . ? C126 C127 H127 120.1 . . ? C128 C127 H127 120.1 . . ? C123 C128 C127 120.9(2) . . ? C123 C128 H128 119.5 . . ? C127 C128 H128 119.5 . . ? O5 C129 H12A 109.5 . . ? O5 C129 H12B 109.5 . . ? H12A C129 H12B 109.5 . . ? O5 C129 H12C 109.5 . . ? H12A C129 H12C 109.5 . . ? H12B C129 H12C 109.5 . . ? O6 C130 H13A 109.5 . . ? O6 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? O6 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? O7 C131 H13D 109.5 . . ? O7 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? O7 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? O8 C132 H13G 109.5 . . ? O8 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? O8 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? O9 C133 H13J 109.5 . . ? O9 C133 H13K 109.5 . . ? H13J C133 H13K 109.5 . . ? O9 C133 H13L 109.5 . . ? H13J C133 H13L 109.5 . . ? H13K C133 H13L 109.5 . . ? O10 C134 H13M 109.5 . . ? O10 C134 H13N 109.5 . . ? H13M C134 H13N 109.5 . . ? O10 C134 H13O 109.5 . . ? H13M C134 H13O 109.5 . . ? H13N C134 H13O 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.663 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.056 data_dp2 _database_code_depnum_ccdc_archive 'CCDC 696720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C134 H108 Co2 Mn2 N20 O12' _chemical_formula_weight 2418.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0132(18) _cell_length_b 13.8829(19) _cell_length_c 19.838(3) _cell_angle_alpha 72.979(2) _cell_angle_beta 73.582(2) _cell_angle_gamma 70.255(2) _cell_volume 2914.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8718 _exptl_absorpt_correction_T_max 0.9003 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15668 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11244 _reflns_number_gt 6981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1458P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11244 _refine_ls_number_parameters 796 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2383 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 9.102 _refine_ls_shift/su_mean 0.084 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 Mn1 Mn 0.5000 0.0000 0.5000 0.0346(2) Uani 1 2 d S . . Mn2 Mn 0.0000 0.5000 0.0000 0.0375(2) Uani 1 2 d S . . Co1 Co 0.20357(6) 0.18058(5) 0.31390(3) 0.0541(2) Uani 1 1 d . . . O1 O 0.2096(6) -0.0990(4) 0.2937(3) 0.1157(18) Uani 1 1 d . . . O2 O 0.4402(5) 0.3337(4) 0.1871(3) 0.1179(18) Uani 1 1 d . . . O3 O 0.0218(3) 0.5009(3) 0.10986(17) 0.0532(8) Uani 1 1 d D . . O4 O 0.2777(14) 0.7125(8) 0.3750(5) 0.258(6) Uani 1 1 d D . . O5 O 0.8633(18) 0.3946(13) 0.4999(8) 0.54(2) Uani 1 1 d D . . O6 O 0.7034(16) 0.3587(15) 0.3702(14) 1.04(5) Uani 1 1 d D . . N1 N 0.0306(5) 0.3182(4) 0.2102(3) 0.0816(15) Uani 1 1 d . . . N2 N 0.3441(3) 0.0640(3) 0.4379(2) 0.0532(10) Uani 1 1 d . . . N3 N 0.2450(4) 0.0604(3) 0.2755(2) 0.0570(10) Uani 1 1 d . . . N4 N 0.3389(4) 0.2080(3) 0.2429(2) 0.0541(10) Uani 1 1 d . . . N5 N 0.1972(4) 0.3139(4) 0.3342(3) 0.0734(13) Uani 1 1 d . . . N6 N 0.0679(4) 0.1194(4) 0.3748(2) 0.0633(12) Uani 1 1 d . . . N7 N 0.5321(3) -0.1435(3) 0.48288(18) 0.0405(8) Uani 1 1 d . . . N8 N 0.6061(3) 0.0396(2) 0.40362(17) 0.0382(8) Uani 1 1 d . . . N9 N -0.1342(3) 0.4322(3) 0.05126(18) 0.0423(8) Uani 1 1 d . . . N10 N 0.1196(3) 0.3582(3) 0.00659(18) 0.0415(8) Uani 1 1 d . . . C1 C 0.0924(5) 0.2662(4) 0.2489(3) 0.0580(12) Uani 1 1 d . . . C2 C 0.2932(4) 0.1066(4) 0.3918(2) 0.0485(11) Uani 1 1 d . . . C3 C 0.3431(5) 0.0544(4) 0.2157(3) 0.0610(13) Uani 1 1 d . . . C4 C 0.3944(4) 0.1361(4) 0.1982(3) 0.0557(12) Uani 1 1 d . . . C5 C 0.4918(5) 0.1413(4) 0.1385(3) 0.0660(14) Uani 1 1 d . . . H3 H 0.5280 0.1952 0.1266 0.079 Uiso 1 1 calc R . . C6 C 0.5322(5) 0.0670(5) 0.0987(3) 0.0715(15) Uani 1 1 d . . . C7 C 0.4797(6) -0.0113(6) 0.1145(4) 0.092(2) Uani 1 1 d . . . H5 H 0.5066 -0.0592 0.0851 0.111 Uiso 1 1 calc R . . C8 C 0.3864(6) -0.0215(5) 0.1740(4) 0.0810(18) Uani 1 1 d . . . H6 H 0.3534 -0.0775 0.1858 0.097 Uiso 1 1 calc R . . C9 C 0.6356(6) 0.0710(7) 0.0333(4) 0.112(3) Uani 1 1 d . . . H7A H 0.6950 0.0039 0.0367 0.169 Uiso 1 1 calc R . . H7B H 0.6720 0.1236 0.0319 0.169 Uiso 1 1 calc R . . H7C H 0.6051 0.0879 -0.0097 0.169 Uiso 1 1 calc R . . C10 C 0.3626(5) 0.2992(4) 0.2320(3) 0.0699(15) Uani 1 1 d . . . C11 C 0.2799(6) 0.3592(4) 0.2847(3) 0.0751(16) Uani 1 1 d . . . C12 C 0.2844(8) 0.4579(6) 0.2837(5) 0.122(3) Uani 1 1 d . . . H19 H 0.3404 0.4885 0.2491 0.147 Uiso 1 1 calc R . . C13 C 0.2052(12) 0.5084(9) 0.3343(8) 0.182(5) Uani 1 1 d . . . H18 H 0.2054 0.5755 0.3339 0.218 Uiso 1 1 calc R . . C14 C 0.1254(10) 0.4628(10) 0.3856(7) 0.176(5) Uani 1 1 d . . . H17 H 0.0735 0.4967 0.4216 0.211 Uiso 1 1 calc R . . C15 C 0.1227(8) 0.3636(7) 0.3836(5) 0.122(3) Uani 1 1 d . . . H16 H 0.0669 0.3324 0.4179 0.147 Uiso 1 1 calc R . . C16 C 0.1858(6) -0.0104(5) 0.3064(3) 0.0743(16) Uani 1 1 d . . . C17 C 0.0805(5) 0.0271(5) 0.3602(3) 0.0713(17) Uani 1 1 d . . . C18 C -0.0063(7) -0.0276(7) 0.3925(4) 0.111(3) Uani 1 1 d . . . H12 H 0.0035 -0.0915 0.3823 0.133 Uiso 1 1 calc R . . C19 C -0.1083(8) 0.0160(9) 0.4407(5) 0.123(4) Uani 1 1 d . . . H13 H -0.1689 -0.0175 0.4619 0.148 Uiso 1 1 calc R . . C20 C -0.1178(6) 0.1059(9) 0.4560(4) 0.114(3) Uani 1 1 d . . . H14 H -0.1836 0.1334 0.4897 0.137 Uiso 1 1 calc R . . C21 C -0.0281(5) 0.1608(6) 0.4214(3) 0.089(2) Uani 1 1 d . . . H15 H -0.0367 0.2247 0.4313 0.107 Uiso 1 1 calc R . . C22 C 0.4895(4) -0.2245(3) 0.5291(2) 0.0474(10) Uani 1 1 d . . . C23 C 0.5308(7) -0.3101(4) 0.4962(3) 0.101(3) Uani 1 1 d . . . H23 H 0.5142 -0.3746 0.5160 0.121 Uiso 1 1 calc R . . C24 C 0.5971(8) -0.2835(5) 0.4325(4) 0.119(3) Uani 1 1 d . . . H24 H 0.6357 -0.3260 0.3994 0.143 Uiso 1 1 calc R . . C25 C 0.6000(5) -0.1798(4) 0.4230(3) 0.0585(13) Uani 1 1 d . . . C26 C 0.6622(4) -0.1240(3) 0.3613(2) 0.0481(10) Uani 1 1 d . . . C27 C 0.7261(5) -0.1786(4) 0.3007(3) 0.0562(12) Uani 1 1 d . . . C28 C 0.8285(6) -0.2618(4) 0.3063(3) 0.093(2) Uani 1 1 d . . . H28 H 0.8615 -0.2825 0.3471 0.111 Uiso 1 1 calc R . . C29 C 0.8823(7) -0.3150(4) 0.2501(4) 0.104(3) Uani 1 1 d . . . H29 H 0.9513 -0.3712 0.2540 0.124 Uiso 1 1 calc R . . C30 C 0.8356(7) -0.2862(5) 0.1904(4) 0.088(2) Uani 1 1 d . . . H30 H 0.8722 -0.3221 0.1534 0.106 Uiso 1 1 calc R . . C31 C 0.7359(6) -0.2049(6) 0.1848(3) 0.0819(18) Uani 1 1 d . . . H31 H 0.7040 -0.1848 0.1436 0.098 Uiso 1 1 calc R . . C32 C 0.6800(5) -0.1510(5) 0.2394(3) 0.0722(15) Uani 1 1 d . . . H32 H 0.6107 -0.0955 0.2346 0.087 Uiso 1 1 calc R . . C33 C 0.6623(4) -0.0210(3) 0.3535(2) 0.0438(10) Uani 1 1 d . . . C34 C 0.7212(6) 0.0382(4) 0.2905(3) 0.0782(18) Uani 1 1 d . . . H34 H 0.7653 0.0152 0.2486 0.094 Uiso 1 1 calc R . . C35 C 0.7015(7) 0.1323(5) 0.3026(3) 0.103(3) Uani 1 1 d . . . H35 H 0.7312 0.1865 0.2709 0.124 Uiso 1 1 calc R . . C36 C 0.6268(4) 0.1361(3) 0.3726(2) 0.0502(11) Uani 1 1 d . . . C37 C 0.5863(4) 0.2216(3) 0.4033(2) 0.0478(11) Uani 1 1 d . . . C38 C 0.6165(5) 0.3215(4) 0.3611(3) 0.0683(15) Uani 1 1 d D . . C39 C 0.5206(9) 0.4145(7) 0.3541(5) 0.166(5) Uani 1 1 d D . . H39 H 0.4428 0.4118 0.3783 0.199 Uiso 1 1 calc R . . C40 C 0.5383(10) 0.5112(8) 0.3119(6) 0.188(6) Uani 1 1 d D . . H40 H 0.4743 0.5718 0.3075 0.225 Uiso 1 1 calc R . . C41 C 0.6516(10) 0.5113(9) 0.2784(5) 0.173(6) Uani 1 1 d D . . H41 H 0.6670 0.5737 0.2502 0.208 Uiso 1 1 calc R . . C42 C 0.7361(11) 0.4309(7) 0.2839(4) 0.138(4) Uani 1 1 d D . . H42 H 0.8145 0.4331 0.2609 0.166 Uiso 1 1 calc R . . C43 C 0.7136(13) 0.3370(8) 0.3249(4) 0.311(15) Uani 1 1 d D . . H43 H 0.7801 0.2782 0.3251 0.373 Uiso 1 1 calc R . . C44 C -0.2544(4) 0.4819(3) 0.0692(2) 0.0438(10) Uani 1 1 d . . . C45 C -0.3190(4) 0.4049(4) 0.1085(2) 0.0518(11) Uani 1 1 d . . . H45 H -0.4015 0.4186 0.1277 0.062 Uiso 1 1 calc R . . C46 C -0.2389(4) 0.3110(4) 0.1124(2) 0.0525(11) Uani 1 1 d . . . H46 H -0.2554 0.2469 0.1342 0.063 Uiso 1 1 calc R . . C47 C -0.1226(4) 0.3265(3) 0.0767(2) 0.0446(10) Uani 1 1 d . . . C48 C -0.0161(4) 0.2464(3) 0.0710(2) 0.0435(10) Uani 1 1 d . . . C49 C -0.0208(4) 0.1352(4) 0.1003(2) 0.0484(10) Uani 1 1 d . . . C50 C -0.0721(5) 0.0907(4) 0.0688(3) 0.0673(14) Uani 1 1 d . . . H50 H -0.1071 0.1309 0.0296 0.081 Uiso 1 1 calc R . . C51 C -0.0731(6) -0.0149(5) 0.0941(4) 0.0806(17) Uani 1 1 d . . . H51 H -0.1100 -0.0441 0.0729 0.097 Uiso 1 1 calc R . . C52 C -0.0192(5) -0.0731(5) 0.1501(4) 0.0806(18) Uani 1 1 d . . . H52 H -0.0174 -0.1435 0.1664 0.097 Uiso 1 1 calc R . . C53 C 0.0311(6) -0.0318(5) 0.1821(3) 0.0813(17) Uani 1 1 d . . . H53 H 0.0677 -0.0731 0.2205 0.098 Uiso 1 1 calc R . . C54 C 0.0287(5) 0.0718(4) 0.1584(3) 0.0694(14) Uani 1 1 d . . . H54 H 0.0618 0.1004 0.1824 0.083 Uiso 1 1 calc R . . C55 C 0.0980(4) 0.2624(3) 0.0392(2) 0.0429(10) Uani 1 1 d . . . C56 C 0.2090(4) 0.1808(4) 0.0358(3) 0.0526(11) Uani 1 1 d . . . H56 H 0.2180 0.1094 0.0539 0.063 Uiso 1 1 calc R . . C57 C 0.2972(4) 0.2265(4) 0.0015(3) 0.0509(11) Uani 1 1 d . . . H57 H 0.3792 0.1920 -0.0089 0.061 Uiso 1 1 calc R . . C58 C 0.2450(4) 0.3365(3) -0.0164(2) 0.0435(10) Uani 1 1 d . . . C59 C 0.3080(4) 0.4105(4) -0.0526(2) 0.0458(10) Uani 1 1 d . . . C60 C 0.4426(4) 0.3707(3) -0.0748(3) 0.0500(11) Uani 1 1 d . . . C61 C 0.4965(4) 0.3255(4) -0.1339(3) 0.0659(14) Uani 1 1 d . . . H61 H 0.4485 0.3183 -0.1606 0.079 Uiso 1 1 calc R . . C62 C 0.6212(5) 0.2908(5) -0.1537(3) 0.0784(17) Uani 1 1 d . . . H62 H 0.6567 0.2602 -0.1934 0.094 Uiso 1 1 calc R . . C63 C 0.6923(5) 0.3018(5) -0.1144(4) 0.0789(18) Uani 1 1 d . . . H63 H 0.7760 0.2797 -0.1278 0.095 Uiso 1 1 calc R . . C64 C 0.6409(5) 0.3440(5) -0.0572(4) 0.0810(18) Uani 1 1 d . . . H64 H 0.6896 0.3497 -0.0303 0.097 Uiso 1 1 calc R . . C65 C 0.5160(4) 0.3801(4) -0.0363(3) 0.0663(14) Uani 1 1 d . . . H65 H 0.4823 0.4106 0.0035 0.080 Uiso 1 1 calc R . . C66 C 0.1230(6) 0.5208(6) 0.1195(3) 0.095(2) Uani 1 1 d . . . H66A H 0.1948 0.4682 0.1046 0.142 Uiso 1 1 calc R . . H66B H 0.1143 0.5191 0.1694 0.142 Uiso 1 1 calc R . . H66C H 0.1289 0.5887 0.0912 0.142 Uiso 1 1 calc R . . C67 C 0.7362(13) 0.4572(16) 0.348(2) 0.45(3) Uani 1 1 d D . . H67A H 0.7462 0.4736 0.3898 0.681 Uiso 1 1 calc R . . H67B H 0.6733 0.5125 0.3281 0.681 Uiso 1 1 calc RD . . H67C H 0.8105 0.4504 0.3133 0.681 Uiso 1 1 calc R . . H3A H 0.011(4) 0.4449(19) 0.135(2) 0.047(14) Uiso 1 1 d D . . H4A H 0.286(3) 0.736(3) 0.4055(15) 0.017(9) Uiso 1 1 d D . . H5A H 0.87(2) 0.391(5) 0.458(3) 0.43(13) Uiso 1 1 d D . . H6A H 0.699(2) 0.340(2) 0.4141(13) 0.000(6) Uiso 1 1 d D . . H4B H 0.334(10) 0.655(12) 0.369(10) 0.44(16) Uiso 1 1 d D . . H5B H 0.886(3) 0.340(2) 0.5271(16) 0.002(7) Uiso 1 1 d 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 Mn1 0.0353(5) 0.0376(5) 0.0277(4) -0.0007(3) -0.0054(3) -0.0122(4) Mn2 0.0314(4) 0.0454(5) 0.0313(5) -0.0016(4) -0.0036(3) -0.0131(4) Co1 0.0525(4) 0.0588(4) 0.0464(4) 0.0040(3) -0.0162(3) -0.0180(3) O1 0.176(5) 0.081(3) 0.110(4) -0.002(3) -0.038(4) -0.071(3) O2 0.118(4) 0.109(4) 0.134(4) -0.036(3) 0.032(3) -0.080(3) O3 0.0565(19) 0.063(2) 0.0399(17) -0.0029(16) -0.0141(15) -0.0193(17) O4 0.495(19) 0.130(7) 0.132(7) -0.027(5) -0.021(9) -0.105(9) O5 0.71(4) 0.71(4) 0.40(2) -0.45(3) 0.41(2) -0.61(3) O6 0.65(5) 0.52(4) 2.00(15) -0.04(6) -1.00(8) 0.17(3) N1 0.090(3) 0.082(3) 0.058(3) 0.009(2) -0.034(3) -0.011(3) N2 0.045(2) 0.069(3) 0.043(2) 0.0014(19) -0.0165(17) -0.0167(18) N3 0.057(2) 0.057(2) 0.056(2) 0.0048(19) -0.024(2) -0.020(2) N4 0.056(2) 0.054(2) 0.054(2) -0.0004(19) -0.0138(19) -0.0242(19) N5 0.068(3) 0.077(3) 0.072(3) -0.021(3) -0.007(2) -0.017(2) N6 0.046(2) 0.089(3) 0.041(2) 0.016(2) -0.0192(18) -0.020(2) N7 0.0428(19) 0.0393(18) 0.0348(18) -0.0040(15) -0.0027(15) -0.0136(15) N8 0.0408(18) 0.0397(18) 0.0324(18) -0.0030(14) -0.0064(14) -0.0140(15) N9 0.0334(18) 0.052(2) 0.0373(19) -0.0016(16) -0.0036(14) -0.0166(16) N10 0.0356(18) 0.048(2) 0.0373(19) -0.0033(15) -0.0059(14) -0.0138(15) C1 0.058(3) 0.058(3) 0.051(3) 0.003(2) -0.014(2) -0.018(2) C2 0.040(2) 0.056(3) 0.046(3) -0.001(2) -0.008(2) -0.019(2) C3 0.057(3) 0.065(3) 0.056(3) -0.008(3) -0.018(2) -0.010(3) C4 0.053(3) 0.057(3) 0.050(3) -0.003(2) -0.016(2) -0.010(2) C5 0.060(3) 0.073(3) 0.060(3) -0.005(3) -0.018(3) -0.017(3) C6 0.067(3) 0.082(4) 0.064(4) -0.029(3) -0.017(3) -0.004(3) C7 0.091(5) 0.106(5) 0.079(5) -0.047(4) -0.021(4) 0.000(4) C8 0.097(5) 0.065(4) 0.092(5) -0.022(3) -0.041(4) -0.014(3) C9 0.088(5) 0.153(7) 0.084(5) -0.050(5) 0.006(4) -0.017(5) C10 0.063(3) 0.070(3) 0.081(4) -0.021(3) -0.001(3) -0.031(3) C11 0.086(4) 0.062(3) 0.086(4) -0.013(3) -0.016(3) -0.036(3) C12 0.134(7) 0.098(5) 0.149(8) -0.050(5) 0.001(6) -0.055(5) C13 0.197(11) 0.141(9) 0.234(14) -0.123(10) 0.036(10) -0.076(8) C14 0.174(10) 0.172(10) 0.201(12) -0.133(10) 0.057(9) -0.069(9) C15 0.123(6) 0.120(6) 0.125(7) -0.073(6) 0.025(5) -0.036(5) C16 0.095(4) 0.066(4) 0.073(4) 0.010(3) -0.030(3) -0.047(3) C17 0.070(4) 0.087(4) 0.061(3) 0.025(3) -0.035(3) -0.043(3) C18 0.116(6) 0.156(7) 0.083(5) 0.042(5) -0.049(5) -0.099(6) C19 0.090(6) 0.195(10) 0.087(6) 0.047(6) -0.041(5) -0.092(7) C20 0.053(4) 0.191(9) 0.059(4) 0.030(5) -0.013(3) -0.034(5) C21 0.049(3) 0.132(6) 0.062(4) 0.005(4) -0.010(3) -0.017(3) C22 0.056(3) 0.041(2) 0.040(2) -0.0023(19) -0.004(2) -0.017(2) C23 0.160(6) 0.056(3) 0.068(4) -0.024(3) 0.046(4) -0.054(4) C24 0.196(8) 0.062(4) 0.079(4) -0.042(3) 0.064(5) -0.065(4) C25 0.077(3) 0.045(2) 0.044(3) -0.013(2) 0.008(2) -0.019(2) C26 0.053(3) 0.046(2) 0.036(2) -0.0071(19) 0.0007(19) -0.012(2) C27 0.070(3) 0.048(3) 0.044(3) -0.011(2) 0.009(2) -0.024(2) C28 0.110(5) 0.062(3) 0.055(3) -0.006(3) 0.001(3) 0.020(3) C29 0.129(6) 0.050(3) 0.082(5) -0.023(3) 0.020(4) 0.012(4) C30 0.121(6) 0.072(4) 0.074(4) -0.036(3) 0.025(4) -0.048(4) C31 0.094(5) 0.103(5) 0.062(4) -0.044(3) 0.009(3) -0.043(4) C32 0.072(4) 0.084(4) 0.066(4) -0.030(3) -0.001(3) -0.027(3) C33 0.044(2) 0.043(2) 0.036(2) -0.0053(18) -0.0027(18) -0.0103(19) C34 0.114(5) 0.067(3) 0.045(3) -0.015(3) 0.028(3) -0.048(3) C35 0.162(7) 0.065(4) 0.064(4) -0.024(3) 0.053(4) -0.063(4) C36 0.066(3) 0.045(2) 0.037(2) -0.0078(19) 0.003(2) -0.024(2) C37 0.053(3) 0.050(2) 0.037(2) 0.0019(19) -0.0034(19) -0.024(2) C38 0.083(4) 0.048(3) 0.061(3) -0.012(2) 0.018(3) -0.029(3) C39 0.136(8) 0.110(7) 0.223(12) 0.042(7) -0.041(8) -0.061(6) C40 0.141(9) 0.132(9) 0.251(15) 0.053(9) -0.059(9) -0.055(7) C41 0.121(9) 0.166(11) 0.187(11) 0.060(9) -0.021(8) -0.076(8) C42 0.160(10) 0.091(6) 0.101(6) 0.018(5) 0.041(6) -0.045(7) C43 0.55(3) 0.157(10) 0.184(12) -0.106(10) 0.241(17) -0.242(17) C44 0.039(2) 0.054(3) 0.036(2) -0.0034(19) -0.0050(18) -0.018(2) C45 0.038(2) 0.064(3) 0.048(3) -0.002(2) -0.0018(19) -0.022(2) C46 0.050(3) 0.059(3) 0.043(3) 0.003(2) -0.001(2) -0.027(2) C47 0.045(2) 0.055(3) 0.035(2) -0.0028(19) -0.0039(18) -0.025(2) C48 0.047(2) 0.046(2) 0.038(2) -0.0052(18) -0.0098(19) -0.016(2) C49 0.045(2) 0.051(3) 0.049(3) -0.007(2) -0.005(2) -0.019(2) C50 0.076(4) 0.066(3) 0.064(3) -0.012(3) -0.012(3) -0.029(3) C51 0.087(4) 0.076(4) 0.094(5) -0.028(4) -0.015(4) -0.037(3) C52 0.072(4) 0.059(3) 0.099(5) -0.014(3) 0.007(3) -0.026(3) C53 0.096(4) 0.067(4) 0.074(4) 0.012(3) -0.022(3) -0.033(3) C54 0.084(4) 0.064(3) 0.063(3) 0.003(3) -0.020(3) -0.035(3) C55 0.043(2) 0.046(2) 0.037(2) -0.0033(18) -0.0085(18) -0.0145(19) C56 0.045(3) 0.051(3) 0.057(3) -0.008(2) -0.006(2) -0.013(2) C57 0.036(2) 0.051(3) 0.059(3) -0.011(2) -0.004(2) -0.010(2) C58 0.038(2) 0.053(2) 0.038(2) -0.0071(19) -0.0049(18) -0.0139(19) C59 0.035(2) 0.063(3) 0.038(2) -0.009(2) -0.0040(18) -0.017(2) C60 0.035(2) 0.048(2) 0.060(3) -0.007(2) -0.003(2) -0.0134(19) C61 0.054(3) 0.093(4) 0.051(3) -0.019(3) -0.002(2) -0.026(3) C62 0.061(3) 0.089(4) 0.075(4) -0.031(3) 0.023(3) -0.027(3) C63 0.035(3) 0.083(4) 0.104(5) -0.022(4) 0.008(3) -0.014(3) C64 0.045(3) 0.101(5) 0.107(5) -0.034(4) -0.015(3) -0.023(3) C65 0.047(3) 0.080(4) 0.075(4) -0.030(3) -0.011(3) -0.012(3) C66 0.085(4) 0.158(7) 0.069(4) -0.033(4) -0.009(3) -0.065(4) C67 0.131(11) 0.28(2) 1.03(7) -0.44(4) 0.14(2) -0.102(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N7 2.009(3) . ? Mn1 N7 2.009(3) 2_656 ? Mn1 N8 2.016(3) . ? Mn1 N8 2.016(3) 2_656 ? Mn1 N2 2.314(4) . ? Mn1 N2 2.314(4) 2_656 ? Mn2 N10 2.001(3) . ? Mn2 N10 2.001(3) 2_565 ? Mn2 N9 2.014(3) 2_565 ? Mn2 N9 2.014(3) . ? Mn2 O3 2.271(3) 2_565 ? Mn2 O3 2.271(3) . ? Co1 N3 1.892(4) . ? Co1 N4 1.893(4) . ? Co1 C1 1.965(5) . ? Co1 C2 1.966(5) . ? Co1 N5 1.979(5) . ? Co1 N6 2.014(4) . ? O1 C16 1.250(7) . ? O2 C10 1.214(6) . ? O3 C66 1.407(6) . ? O3 H3A 0.821(10) . ? O4 H4B 0.86(3) . ? O4 H4A 0.812(10) . ? O4 H4B 0.86(3) . ? O5 H5B 0.800(10) . ? O5 H5A 0.823(13) . ? O5 H5A 0.823(13) . ? O5 H5B 0.800(10) . ? O6 H6A 0.824(10) . ? O6 C67 1.461(18) . ? O6 H6A 0.824(10) . ? N1 C1 1.139(6) . ? N2 C2 1.148(5) . ? N3 C16 1.311(6) . ? N3 C3 1.415(6) . ? N4 C10 1.335(6) . ? N4 C4 1.400(6) . ? N5 C15 1.311(8) . ? N5 C11 1.362(7) . ? N6 C21 1.333(7) . ? N6 C17 1.344(7) . ? N7 C25 1.362(6) . ? N7 C22 1.374(5) . ? N8 C33 1.372(5) . ? N8 C36 1.375(5) . ? N9 C44 1.367(5) . ? N9 C47 1.377(5) . ? N10 C55 1.374(5) . ? N10 C58 1.398(5) . ? C3 C4 1.382(7) . ? C3 C8 1.401(8) . ? C4 C5 1.414(7) . ? C5 C6 1.357(8) . ? C5 H3 0.9300 . ? C6 C7 1.353(9) . ? C6 C9 1.524(9) . ? C7 C8 1.389(9) . ? C7 H5 0.9300 . ? C8 H6 0.9300 . ? C9 H7A 0.9600 . ? C9 H7B 0.9600 . ? C9 H7C 0.9600 . ? C10 C11 1.462(8) . ? C11 C12 1.383(9) . ? C12 C13 1.353(13) . ? C12 H19 0.9300 . ? C13 C14 1.355(14) . ? C13 H18 0.9300 . ? C14 C15 1.401(12) . ? C14 H17 0.9300 . ? C15 H16 0.9300 . ? C16 C17 1.459(9) . ? C17 C18 1.395(8) . ? C18 C19 1.400(13) . ? C18 H12 0.9300 . ? C19 C20 1.330(12) . ? C19 H13 0.9300 . ? C20 C21 1.430(10) . ? C20 H14 0.9300 . ? C21 H15 0.9300 . ? C22 C37 1.395(6) 2_656 ? C22 C23 1.398(7) . ? C23 C24 1.313(8) . ? C23 H23 0.9300 . ? C24 C25 1.408(7) . ? C24 H24 0.9300 . ? C25 C26 1.405(6) . ? C26 C33 1.393(6) . ? C26 C27 1.492(6) . ? C27 C32 1.378(7) . ? C27 C28 1.380(7) . ? C28 C29 1.399(9) . ? C28 H28 0.9300 . ? C29 C30 1.351(10) . ? C29 H29 0.9300 . ? C30 C31 1.345(9) . ? C30 H30 0.9300 . ? C31 C32 1.381(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.425(6) . ? C34 C35 1.328(7) . ? C34 H34 0.9300 . ? C35 C36 1.430(7) . ? C35 H35 0.9300 . ? C36 C37 1.373(6) . ? C37 C22 1.395(6) 2_656 ? C37 C38 1.498(6) . ? C38 C43 1.236(11) . ? C38 C39 1.412(9) . ? C39 C40 1.408(11) . ? C39 H39 0.9300 . ? C40 C41 1.335(11) . ? C40 H40 0.9300 . ? C41 C42 1.230(11) . ? C41 H41 0.9300 . ? C42 C43 1.388(10) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C59 1.392(6) 2_565 ? C44 C45 1.443(6) . ? C45 C46 1.329(6) . ? C45 H45 0.9300 . ? C46 C47 1.434(6) . ? C46 H46 0.9300 . ? C47 C48 1.385(6) . ? C48 C55 1.400(6) . ? C48 C49 1.497(6) . ? C49 C50 1.362(7) . ? C49 C54 1.377(7) . ? C50 C51 1.406(8) . ? C50 H50 0.9300 . ? C51 C52 1.354(9) . ? C51 H51 0.9300 . ? C52 C53 1.327(9) . ? C52 H52 0.9300 . ? C53 C54 1.370(7) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.427(6) . ? C56 C57 1.335(6) . ? C56 H56 0.9300 . ? C57 C58 1.420(6) . ? C57 H57 0.9300 . ? C58 C59 1.389(6) . ? C59 C44 1.392(6) 2_565 ? C59 C60 1.500(6) . ? C60 C65 1.376(7) . ? C60 C61 1.384(7) . ? C61 C62 1.387(7) . ? C61 H61 0.9300 . ? C62 C63 1.376(9) . ? C62 H62 0.9300 . ? C63 C64 1.327(9) . ? C63 H63 0.9300 . ? C64 C65 1.390(7) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Mn1 N7 180.00(18) . 2_656 ? N7 Mn1 N8 90.16(13) . . ? N7 Mn1 N8 89.84(13) 2_656 . ? N7 Mn1 N8 89.84(13) . 2_656 ? N7 Mn1 N8 90.16(13) 2_656 2_656 ? N8 Mn1 N8 180.000(1) . 2_656 ? N7 Mn1 N2 90.27(14) . . ? N7 Mn1 N2 89.73(14) 2_656 . ? N8 Mn1 N2 85.51(13) . . ? N8 Mn1 N2 94.49(13) 2_656 . ? N7 Mn1 N2 89.73(14) . 2_656 ? N7 Mn1 N2 90.27(14) 2_656 2_656 ? N8 Mn1 N2 94.49(13) . 2_656 ? N8 Mn1 N2 85.51(13) 2_656 2_656 ? N2 Mn1 N2 180.00(15) . 2_656 ? N10 Mn2 N10 180.00(18) . 2_565 ? N10 Mn2 N9 90.24(13) . 2_565 ? N10 Mn2 N9 89.76(13) 2_565 2_565 ? N10 Mn2 N9 89.76(13) . . ? N10 Mn2 N9 90.24(13) 2_565 . ? N9 Mn2 N9 180.0 2_565 . ? N10 Mn2 O3 91.37(13) . 2_565 ? N10 Mn2 O3 88.63(13) 2_565 2_565 ? N9 Mn2 O3 87.76(13) 2_565 2_565 ? N9 Mn2 O3 92.24(13) . 2_565 ? N10 Mn2 O3 88.63(13) . . ? N10 Mn2 O3 91.37(13) 2_565 . ? N9 Mn2 O3 92.24(13) 2_565 . ? N9 Mn2 O3 87.76(13) . . ? O3 Mn2 O3 180.0 2_565 . ? N3 Co1 N4 82.76(18) . . ? N3 Co1 C1 93.74(19) . . ? N4 Co1 C1 91.79(18) . . ? N3 Co1 C2 93.81(18) . . ? N4 Co1 C2 95.65(17) . . ? C1 Co1 C2 170.0(2) . . ? N3 Co1 N5 164.86(19) . . ? N4 Co1 N5 82.10(19) . . ? C1 Co1 N5 86.5(2) . . ? C2 Co1 N5 87.9(2) . . ? N3 Co1 N6 81.2(2) . . ? N4 Co1 N6 163.8(2) . . ? C1 Co1 N6 86.85(17) . . ? C2 Co1 N6 87.85(16) . . ? N5 Co1 N6 113.9(2) . . ? C66 O3 Mn2 122.3(3) . . ? C66 O3 H3A 112(3) . . ? Mn2 O3 H3A 104(3) . . ? H4B O4 H4A 112(3) . . ? H4B O4 H4B 0(10) . . ? H4A O4 H4B 112(3) . . ? H5B O5 H5A 116(3) . . ? H5B O5 H5A 116(3) . . ? H5A O5 H5A 0(10) . . ? H5B O5 H5B 0(4) . . ? H5A O5 H5B 116(3) . . ? H5A O5 H5B 116(3) . . ? H6A O6 C67 106(4) . . ? H6A O6 H6A 0(5) . . ? C67 O6 H6A 106(4) . . ? C2 N2 Mn1 159.5(3) . . ? C16 N3 C3 125.8(5) . . ? C16 N3 Co1 119.2(4) . . ? C3 N3 Co1 114.9(3) . . ? C10 N4 C4 125.0(4) . . ? C10 N4 Co1 118.9(4) . . ? C4 N4 Co1 115.3(3) . . ? C15 N5 C11 119.2(6) . . ? C15 N5 Co1 129.5(5) . . ? C11 N5 Co1 111.2(4) . . ? C21 N6 C17 120.6(5) . . ? C21 N6 Co1 128.6(5) . . ? C17 N6 Co1 110.7(4) . . ? C25 N7 C22 106.2(4) . . ? C25 N7 Mn1 126.9(3) . . ? C22 N7 Mn1 126.9(3) . . ? C33 N8 C36 106.6(3) . . ? C33 N8 Mn1 126.6(3) . . ? C36 N8 Mn1 126.5(3) . . ? C44 N9 C47 106.3(3) . . ? C44 N9 Mn2 127.0(3) . . ? C47 N9 Mn2 126.7(3) . . ? C55 N10 C58 105.3(3) . . ? C55 N10 Mn2 127.9(3) . . ? C58 N10 Mn2 126.7(3) . . ? N1 C1 Co1 177.5(5) . . ? N2 C2 Co1 179.0(4) . . ? C4 C3 C8 120.0(5) . . ? C4 C3 N3 113.2(5) . . ? C8 C3 N3 126.7(5) . . ? C3 C4 N4 113.7(4) . . ? C3 C4 C5 119.3(5) . . ? N4 C4 C5 127.0(5) . . ? C6 C5 C4 119.6(6) . . ? C6 C5 H3 120.2 . . ? C4 C5 H3 120.2 . . ? C7 C6 C5 121.1(6) . . ? C7 C6 C9 117.7(6) . . ? C5 C6 C9 121.2(6) . . ? C6 C7 C8 121.3(6) . . ? C6 C7 H5 119.4 . . ? C8 C7 H5 119.4 . . ? C7 C8 C3 118.6(6) . . ? C7 C8 H6 120.7 . . ? C3 C8 H6 120.7 . . ? C6 C9 H7A 109.5 . . ? C6 C9 H7B 109.5 . . ? H7A C9 H7B 109.5 . . ? C6 C9 H7C 109.4 . . ? H7A C9 H7C 109.5 . . ? H7B C9 H7C 109.5 . . ? O2 C10 N4 129.0(6) . . ? O2 C10 C11 120.5(5) . . ? N4 C10 C11 110.4(5) . . ? N5 C11 C12 121.6(7) . . ? N5 C11 C10 116.9(5) . . ? C12 C11 C10 121.5(6) . . ? C13 C12 C11 118.1(9) . . ? C13 C12 H19 120.9 . . ? C11 C12 H19 121.0 . . ? C12 C13 C14 121.0(9) . . ? C12 C13 H18 119.5 . . ? C14 C13 H18 119.5 . . ? C13 C14 C15 118.8(9) . . ? C13 C14 H17 120.6 . . ? C15 C14 H17 120.6 . . ? N5 C15 C14 121.3(8) . . ? N5 C15 H16 119.4 . . ? C14 C15 H16 119.4 . . ? O1 C16 N3 127.7(7) . . ? O1 C16 C17 121.1(6) . . ? N3 C16 C17 111.2(6) . . ? N6 C17 C18 121.5(7) . . ? N6 C17 C16 116.9(5) . . ? C18 C17 C16 121.6(7) . . ? C19 C18 C17 118.4(9) . . ? C19 C18 H12 120.8 . . ? C17 C18 H12 120.8 . . ? C20 C19 C18 119.3(7) . . ? C20 C19 H13 120.4 . . ? C18 C19 H13 120.3 . . ? C19 C20 C21 120.9(8) . . ? C19 C20 H14 119.5 . . ? C21 C20 H14 119.6 . . ? N6 C21 C20 119.2(8) . . ? N6 C21 H15 120.4 . . ? C20 C21 H15 120.4 . . ? N7 C22 C37 126.1(4) . 2_656 ? N7 C22 C23 108.9(4) . . ? C37 C22 C23 125.0(4) 2_656 . ? C24 C23 C22 108.0(5) . . ? C24 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? C23 C24 C25 108.3(5) . . ? C23 C24 H24 125.8 . . ? C25 C24 H24 125.8 . . ? N7 C25 C26 126.4(4) . . ? N7 C25 C24 108.6(4) . . ? C26 C25 C24 125.0(5) . . ? C33 C26 C25 123.5(4) . . ? C33 C26 C27 119.6(4) . . ? C25 C26 C27 116.8(4) . . ? C32 C27 C28 118.2(5) . . ? C32 C27 C26 120.7(5) . . ? C28 C27 C26 121.0(5) . . ? C27 C28 C29 119.5(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 121.1(6) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 119.4(6) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C32 121.1(7) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 120.7(6) . . ? C27 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? N8 C33 C26 126.3(4) . . ? N8 C33 C34 109.3(4) . . ? C26 C33 C34 124.4(4) . . ? C35 C34 C33 107.4(5) . . ? C35 C34 H34 126.3 . . ? C33 C34 H34 126.3 . . ? C34 C35 C36 108.3(5) . . ? C34 C35 H35 125.9 . . ? C36 C35 H35 125.9 . . ? N8 C36 C37 126.6(4) . . ? N8 C36 C35 108.4(4) . . ? C37 C36 C35 125.0(4) . . ? C36 C37 C22 123.9(4) . 2_656 ? C36 C37 C38 119.4(4) . . ? C22 C37 C38 116.5(4) 2_656 . ? C43 C38 C39 111.3(8) . . ? C43 C38 C37 130.5(7) . . ? C39 C38 C37 118.0(5) . . ? C40 C39 C38 122.5(9) . . ? C40 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C41 C40 C39 116.6(10) . . ? C41 C40 H40 121.7 . . ? C39 C40 H40 121.7 . . ? C42 C41 C40 121.7(11) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C43 119.5(11) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.4 . . ? C38 C43 C42 128.4(12) . . ? C38 C43 H43 115.8 . . ? C42 C43 H43 115.8 . . ? N9 C44 C59 126.1(4) . 2_565 ? N9 C44 C45 109.3(4) . . ? C59 C44 C45 124.5(4) 2_565 . ? C46 C45 C44 107.4(4) . . ? C46 C45 H45 126.3 . . ? C44 C45 H45 126.3 . . ? C45 C46 C47 107.6(4) . . ? C45 C46 H46 126.2 . . ? C47 C46 H46 126.2 . . ? N9 C47 C48 126.4(4) . . ? N9 C47 C46 109.3(4) . . ? C48 C47 C46 124.3(4) . . ? C47 C48 C55 124.0(4) . . ? C47 C48 C49 119.1(4) . . ? C55 C48 C49 116.9(4) . . ? C50 C49 C54 116.6(5) . . ? C50 C49 C48 120.8(4) . . ? C54 C49 C48 122.6(4) . . ? C49 C50 C51 121.4(5) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C52 C51 C50 118.6(6) . . ? C52 C51 H51 120.7 . . ? C50 C51 H51 120.7 . . ? C53 C52 C51 121.4(6) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 119.7(6) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C49 122.3(6) . . ? C53 C54 H54 118.8 . . ? C49 C54 H54 118.8 . . ? N10 C55 C48 125.2(4) . . ? N10 C55 C56 110.2(4) . . ? C48 C55 C56 124.6(4) . . ? C57 C56 C55 107.0(4) . . ? C57 C56 H56 126.5 . . ? C55 C56 H56 126.5 . . ? C56 C57 C58 108.5(4) . . ? C56 C57 H57 125.7 . . ? C58 C57 H57 125.8 . . ? C59 C58 N10 125.5(4) . . ? C59 C58 C57 125.5(4) . . ? N10 C58 C57 108.9(4) . . ? C58 C59 C44 124.3(4) . 2_565 ? C58 C59 C60 117.2(4) . . ? C44 C59 C60 118.4(4) 2_565 . ? C65 C60 C61 118.3(4) . . ? C65 C60 C59 119.8(4) . . ? C61 C60 C59 121.9(4) . . ? C60 C61 C62 120.7(5) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.7 . . ? C63 C62 C61 119.7(6) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.1 . . ? C64 C63 C62 119.8(5) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C65 121.8(6) . . ? C63 C64 H64 119.1 . . ? C65 C64 H64 119.1 . . ? C60 C65 C64 119.8(5) . . ? C60 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? O3 C66 H66A 109.4 . . ? O3 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O3 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O6 C67 H67A 108.9 . . ? O6 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? O6 C67 H67C 110.0 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.870 _refine_diff_density_min -0.931 _refine_diff_density_rms 0.084 data_1 _database_code_depnum_ccdc_archive 'CCDC 898330' #TrackingRef 'Cobpb, 4-ClTPP 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H40 Cl4 Co Mn N10 O3, 3(C H4 O)' _chemical_formula_sum 'C68 H52 Cl4 Co Mn N10 O6' _chemical_formula_weight 1360.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.9553(14) _cell_length_b 17.9118(16) _cell_length_c 24.897(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.081(5) _cell_angle_gamma 90.00 _cell_volume 7026.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2315 _cell_measurement_theta_min 2.213 _cell_measurement_theta_max 25.876 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8803 _exptl_absorpt_correction_T_max 0.9460 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56446 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12340 _reflns_number_gt 8487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1184P)^2^+0.9637P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12340 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.77373(3) 1.01711(3) 0.55216(2) 0.07320(19) Uani 1 1 d . . . Mn1 Mn 0.85868(3) 0.75068(2) 0.628403(16) 0.04672(15) Uani 1 1 d . . . Cl1 Cl 1.27189(9) 1.01609(8) 0.86726(5) 0.1177(5) Uani 1 1 d . . . O1 O 0.9949(2) 1.1220(2) 0.5919(2) 0.1517(16) Uani 1 1 d . . . O2 O 0.5946(3) 1.0103(2) 0.64660(19) 0.1329(14) Uani 1 1 d . . . O3 O 0.87752(19) 0.64274(14) 0.67932(10) 0.0845(8) Uani 1 1 d . . . H3 H 0.8907 0.6439 0.7125 0.127 Uiso 1 1 d R . . O4 O 0.4385(5) 0.8614(5) 0.2886(3) 0.241(3) Uani 1 1 d . . . H4 H 0.4567 0.9017 0.3010 0.362 Uiso 1 1 calc R . . O5 O 0.6544(9) 0.2475(8) 0.4108(7) 0.407(8) Uani 1 1 d . . . H5 H 0.6515 0.2087 0.4279 0.610 Uiso 1 1 calc R . . O6 O 0.1682(9) 0.1366(8) 0.6163(8) 0.450(10) Uani 1 1 d . . . H6 H 0.1234 0.1371 0.6285 0.675 Uiso 1 1 calc R . . N1 N 0.6887(2) 1.1657(2) 0.5164(3) 0.140(2) Uani 1 1 d . . . N2 N 0.84194(16) 0.86042(16) 0.58314(11) 0.0578(6) Uani 1 1 d . . . N3 N 0.8663(2) 1.06460(18) 0.59512(19) 0.0894(10) Uani 1 1 d . . . N4 N 0.7251(2) 1.01998(18) 0.61583(18) 0.0909(10) Uani 1 1 d . . . N5 N 0.8436(2) 1.03180(19) 0.49440(19) 0.0865(10) Uani 1 1 d . . . N6 N 0.66754(19) 0.96589(18) 0.52249(17) 0.0806(10) Uani 1 1 d . . . N7 N 0.86167(16) 0.80672(14) 0.69863(9) 0.0531(6) Uani 1 1 d . . . N8 N 0.98597(16) 0.75876(14) 0.63608(10) 0.0536(6) Uani 1 1 d . . . N9 N 0.85674(15) 0.69013(13) 0.56016(9) 0.0497(6) Uani 1 1 d . . . N10 N 0.73190(16) 0.73887(14) 0.62226(10) 0.0513(6) Uani 1 1 d . . . C1 C 0.7212(2) 1.1116(2) 0.5313(2) 0.0957(15) Uani 1 1 d . . . C2 C 0.8198(2) 0.9199(2) 0.57099(15) 0.0609(8) Uani 1 1 d . . . C3 C 0.8569(3) 1.0720(2) 0.6494(3) 0.1007(15) Uani 1 1 d . . . C4 C 0.7785(4) 1.0498(3) 0.6620(2) 0.1011(14) Uani 1 1 d . . . C5 C 0.7588(4) 1.0542(3) 0.7154(3) 0.1246(18) Uani 1 1 d . . . H47 H 0.7063 1.0398 0.7236 0.150 Uiso 1 1 calc R . . C6 C 0.8243(6) 1.0820(4) 0.7557(3) 0.139(2) Uani 1 1 d . . . H48 H 0.8145 1.0858 0.7914 0.166 Uiso 1 1 calc R . . C7 C 0.8981(6) 1.1026(4) 0.7441(3) 0.140(2) Uani 1 1 d . . . H49 H 0.9384 1.1208 0.7721 0.168 Uiso 1 1 calc R . . C8 C 0.9198(4) 1.0985(3) 0.6915(3) 0.1262(19) Uani 1 1 d . . . H50 H 0.9732 1.1127 0.6847 0.151 Uiso 1 1 calc R . . C9 C 0.9302(3) 1.0879(2) 0.5699(3) 0.0983(14) Uani 1 1 d . . . C10 C 0.9165(2) 1.0698(2) 0.5131(3) 0.0927(14) Uani 1 1 d . . . C11 C 0.9731(3) 1.0908(3) 0.4778(3) 0.1062(17) Uani 1 1 d . . . H54 H 1.0218 1.1179 0.4908 0.127 Uiso 1 1 calc R . . C12 C 0.9565(4) 1.0718(4) 0.4257(3) 0.122(2) Uani 1 1 d . . . H55 H 0.9947 1.0837 0.4024 0.147 Uiso 1 1 calc R . . C13 C 0.8851(4) 1.0358(4) 0.4067(3) 0.132(2) Uani 1 1 d . . . H56 H 0.8729 1.0238 0.3700 0.159 Uiso 1 1 calc R . . C14 C 0.8278(3) 1.0156(3) 0.4421(3) 0.1141(17) Uani 1 1 d . . . H57 H 0.7780 0.9904 0.4282 0.137 Uiso 1 1 calc R . . C15 C 0.6436(3) 1.0014(3) 0.6113(3) 0.0954(14) Uani 1 1 d . . . C16 C 0.6143(2) 0.9635(2) 0.5600(2) 0.0894(14) Uani 1 1 d . . . C17 C 0.5382(3) 0.9248(3) 0.5492(3) 0.1150(18) Uani 1 1 d . . . H61 H 0.5013 0.9232 0.5747 0.138 Uiso 1 1 calc R . . C18 C 0.5186(3) 0.8892(3) 0.5003(3) 0.124(2) Uani 1 1 d . . . H62 H 0.4678 0.8630 0.4929 0.148 Uiso 1 1 calc R . . C19 C 0.5705(4) 0.8906(3) 0.4622(3) 0.1221(19) Uani 1 1 d . . . H63 H 0.5567 0.8667 0.4288 0.147 Uiso 1 1 calc R . . C20 C 0.6462(3) 0.9301(3) 0.4762(2) 0.1006(14) Uani 1 1 d . . . H64 H 0.6838 0.9313 0.4513 0.121 Uiso 1 1 calc R . . C21 C 0.7930(2) 0.82359(19) 0.72379(12) 0.0613(8) Uani 1 1 d . . . C22 C 0.8217(3) 0.8711(2) 0.76933(15) 0.0767(10) Uani 1 1 d . . . H2 H 0.7886 0.8895 0.7939 0.092 Uiso 1 1 calc R . . C23 C 0.9033(3) 0.8841(2) 0.77044(14) 0.0771(11) Uani 1 1 d . . . H3A H 0.9373 0.9147 0.7951 0.092 Uiso 1 1 calc R . . C24 C 0.9299(2) 0.84320(19) 0.72720(12) 0.0588(8) Uani 1 1 d . . . C25 C 1.0145(2) 0.83846(19) 0.71782(12) 0.0598(8) Uani 1 1 d . . . C26 C 1.0791(2) 0.8825(2) 0.75420(13) 0.0625(8) Uani 1 1 d . . . C27 C 1.0822(3) 0.9579(3) 0.75049(17) 0.0873(12) Uani 1 1 d . . . H26 H 1.0436 0.9823 0.7245 0.105 Uiso 1 1 calc R . . C28 C 1.1425(3) 0.9999(3) 0.7849(2) 0.0959(14) Uani 1 1 d . . . H25 H 1.1441 1.0516 0.7817 0.115 Uiso 1 1 calc R . . C29 C 1.1983(3) 0.9642(3) 0.82315(15) 0.0802(11) Uani 1 1 d . . . C30 C 1.1990(3) 0.8885(3) 0.82672(17) 0.0979(14) Uani 1 1 d . . . H23 H 1.2393 0.8642 0.8518 0.117 Uiso 1 1 calc R . . C31 C 1.1390(3) 0.8482(2) 0.79265(16) 0.0907(13) Uani 1 1 d . . . H22 H 1.1388 0.7964 0.7956 0.109 Uiso 1 1 calc R . . C32 C 1.03992(19) 0.79631(19) 0.67613(12) 0.0567(8) Uani 1 1 d . . . C33 C 1.1254(2) 0.7861(2) 0.66825(15) 0.0735(10) Uani 1 1 d . . . H7 H 1.1733 0.8057 0.6897 0.088 Uiso 1 1 calc R . . C34 C 1.1243(2) 0.7425(2) 0.62386(15) 0.0743(10) Uani 1 1 d . . . H8 H 1.1715 0.7258 0.6097 0.089 Uiso 1 1 calc R . . C35 C 1.0381(2) 0.72687(19) 0.60261(13) 0.0589(8) Uani 1 1 d . . . C36 C 1.0100(2) 0.68828(18) 0.55478(12) 0.0565(8) Uani 1 1 d . . . C37 C 1.0741(2) 0.66334(19) 0.52049(13) 0.0584(8) Uani 1 1 d . . . C38 C 1.1188(2) 0.7144(2) 0.49571(15) 0.0719(9) Uani 1 1 d . . . H32 H 1.1108 0.7650 0.5016 0.086 Uiso 1 1 calc R . . C39 C 1.1758(2) 0.6925(2) 0.46196(16) 0.0765(10) Uani 1 1 d . . . H31 H 1.2059 0.7280 0.4456 0.092 Uiso 1 1 calc R . . C40 C 1.1868(2) 0.6189(2) 0.45323(14) 0.0679(9) Uani 1 1 d . . . C41 C 1.1436(2) 0.5651(2) 0.47800(15) 0.0754(10) Uani 1 1 d . . . H29 H 1.1518 0.5146 0.4718 0.091 Uiso 1 1 calc R . . C42 C 1.0885(2) 0.5878(2) 0.51197(14) 0.0670(9) Uani 1 1 d . . . H28 H 1.0603 0.5522 0.5296 0.080 Uiso 1 1 calc R . . C43 C 0.92497(19) 0.67303(17) 0.53510(12) 0.0528(7) Uani 1 1 d . . . C44 C 0.8950(2) 0.6373(2) 0.48412(12) 0.0619(8) Uani 1 1 d . . . H12 H 0.9283 0.6210 0.4590 0.074 Uiso 1 1 calc R . . C45 C 0.8107(2) 0.6315(2) 0.47927(13) 0.0618(8) Uani 1 1 d . . . H13 H 0.7749 0.6100 0.4503 0.074 Uiso 1 1 calc R . . C46 C 0.7856(2) 0.66410(17) 0.52638(11) 0.0530(7) Uani 1 1 d . . . C47 C 0.70171(19) 0.66832(17) 0.53625(11) 0.0528(7) Uani 1 1 d . . . C48 C 0.63655(19) 0.62723(18) 0.49797(11) 0.0526(7) Uani 1 1 d . . . C49 C 0.6399(2) 0.55071(19) 0.49496(14) 0.0647(9) Uani 1 1 d . . . H34 H 0.6828 0.5257 0.5176 0.078 Uiso 1 1 calc R . . C50 C 0.5823(2) 0.5092(2) 0.45973(15) 0.0675(9) Uani 1 1 d . . . H35 H 0.5867 0.4575 0.4584 0.081 Uiso 1 1 calc R . . C51 C 0.5187(2) 0.5458(2) 0.42695(12) 0.0613(8) Uani 1 1 d . . . C52 C 0.5107(3) 0.6222(2) 0.42919(15) 0.0801(11) Uani 1 1 d . . . H37 H 0.4661 0.6464 0.4075 0.096 Uiso 1 1 calc R . . C53 C 0.5703(2) 0.6622(2) 0.46421(15) 0.0752(10) Uani 1 1 d . . . H38 H 0.5659 0.7140 0.4652 0.090 Uiso 1 1 calc R . . C54 C 0.67752(19) 0.70219(17) 0.58178(12) 0.0519(7) Uani 1 1 d . . . C55 C 0.5933(2) 0.70361(19) 0.59424(13) 0.0615(8) Uani 1 1 d . . . H17 H 0.5453 0.6832 0.5733 0.074 Uiso 1 1 calc R . . C56 C 0.5959(2) 0.73955(19) 0.64128(14) 0.0645(9) Uani 1 1 d . . . H18 H 0.5499 0.7485 0.6592 0.077 Uiso 1 1 calc R . . C57 C 0.6817(2) 0.76205(18) 0.65950(13) 0.0564(8) Uani 1 1 d . . . C58 C 0.7102(2) 0.80101(19) 0.70784(13) 0.0598(8) Uani 1 1 d . . . C59 C 0.6455(2) 0.8212(2) 0.74286(14) 0.0681(9) Uani 1 1 d . . . C60 C 0.5886(3) 0.8771(3) 0.72884(19) 0.0941(13) Uani 1 1 d . . . H44 H 0.5904 0.9032 0.6968 0.113 Uiso 1 1 calc R . . C61 C 0.5283(4) 0.8966(3) 0.7604(2) 0.1147(17) Uani 1 1 d . . . H43 H 0.4892 0.9343 0.7496 0.138 Uiso 1 1 calc R . . C62 C 0.5276(3) 0.8594(4) 0.8070(2) 0.1034(16) Uani 1 1 d . . . C63 C 0.5805(3) 0.8030(4) 0.82343(17) 0.1028(16) Uani 1 1 d . . . H41 H 0.5766 0.7770 0.8553 0.123 Uiso 1 1 calc R . . C64 C 0.6427(3) 0.7840(3) 0.79096(15) 0.0848(12) Uani 1 1 d . . . H40 H 0.6817 0.7463 0.8021 0.102 Uiso 1 1 calc R . . C65 C 0.8799(6) 0.5692(3) 0.6609(3) 0.176(3) Uani 1 1 d . . . H67A H 0.9322 0.5609 0.6473 0.265 Uiso 1 1 calc R . . H67B H 0.8330 0.5609 0.6322 0.265 Uiso 1 1 calc R . . H67C H 0.8761 0.5355 0.6903 0.265 Uiso 1 1 calc R . . C66 C 0.6295(8) 0.3083(7) 0.4410(7) 0.330(11) Uani 1 1 d . . . H69A H 0.6060 0.2898 0.4717 0.494 Uiso 1 1 calc R . . H69B H 0.5875 0.3375 0.4183 0.494 Uiso 1 1 calc R . . H69C H 0.6780 0.3389 0.4537 0.494 Uiso 1 1 calc R . . C67 C 0.4250(9) 0.8113(8) 0.3335(5) 0.281(7) Uani 1 1 d . . . H68A H 0.4405 0.8367 0.3676 0.422 Uiso 1 1 calc R . . H68B H 0.4595 0.7674 0.3329 0.422 Uiso 1 1 calc R . . H68C H 0.3663 0.7971 0.3293 0.422 Uiso 1 1 calc R . . C68 C 0.1726(12) 0.1997(10) 0.5835(11) 0.432(15) Uani 1 1 d . . . H70A H 0.1520 0.2425 0.6007 0.648 Uiso 1 1 calc R . . H70B H 0.1384 0.1918 0.5487 0.648 Uiso 1 1 calc R . . H70C H 0.2305 0.2080 0.5789 0.648 Uiso 1 1 calc R . . Cl2 Cl 1.25637(8) 0.59105(7) 0.40980(5) 0.1005(4) Uani 1 1 d . . . Cl3 Cl 0.44472(7) 0.49396(6) 0.38311(4) 0.0828(3) Uani 1 1 d . . . Cl4 Cl 0.45291(11) 0.88570(16) 0.84826(8) 0.1923(10) 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 0.0511(3) 0.0508(3) 0.1175(4) 0.0187(3) 0.0123(3) -0.0013(2) Mn1 0.0536(3) 0.0462(3) 0.0407(2) -0.00440(19) 0.00860(19) -0.0014(2) Cl1 0.1125(9) 0.1273(11) 0.1030(8) -0.0327(7) -0.0153(7) -0.0393(8) O1 0.083(2) 0.125(3) 0.245(5) -0.035(3) 0.018(3) -0.039(2) O2 0.121(3) 0.121(3) 0.176(4) 0.036(3) 0.083(3) 0.023(2) O3 0.128(2) 0.0553(15) 0.0662(14) 0.0079(12) 0.0036(14) 0.0001(15) O4 0.315(9) 0.217(7) 0.161(5) -0.020(5) -0.058(5) 0.042(6) O5 0.319(14) 0.318(15) 0.54(2) -0.018(14) -0.070(14) 0.056(11) O6 0.347(15) 0.229(11) 0.74(3) 0.055(15) -0.024(16) -0.048(11) N1 0.075(2) 0.067(2) 0.270(6) 0.052(3) 0.003(3) -0.003(2) N2 0.0564(15) 0.0545(17) 0.0640(16) 0.0067(13) 0.0136(12) -0.0040(13) N3 0.068(2) 0.0572(19) 0.141(3) 0.002(2) 0.011(2) 0.0040(16) N4 0.079(2) 0.062(2) 0.134(3) 0.006(2) 0.023(2) 0.0130(17) N5 0.0614(19) 0.072(2) 0.126(3) 0.033(2) 0.014(2) 0.0023(16) N6 0.0535(17) 0.0564(18) 0.128(3) 0.0231(19) 0.0041(19) -0.0062(14) N7 0.0592(15) 0.0558(15) 0.0453(13) -0.0067(11) 0.0113(12) -0.0074(12) N8 0.0559(15) 0.0561(15) 0.0473(13) -0.0075(12) 0.0036(11) 0.0036(12) N9 0.0548(14) 0.0501(14) 0.0441(12) -0.0077(11) 0.0077(11) 0.0003(11) N10 0.0585(15) 0.0502(14) 0.0477(13) -0.0049(11) 0.0163(12) -0.0049(12) C1 0.057(2) 0.058(2) 0.170(5) 0.027(3) 0.012(2) -0.0048(19) C2 0.0476(17) 0.054(2) 0.082(2) 0.0114(18) 0.0131(15) -0.0065(15) C3 0.094(3) 0.064(3) 0.138(5) -0.009(3) 0.000(3) 0.016(2) C4 0.109(4) 0.069(3) 0.123(4) -0.002(3) 0.015(3) 0.027(3) C5 0.139(5) 0.095(4) 0.140(5) 0.004(4) 0.023(4) 0.030(4) C6 0.171(7) 0.106(5) 0.130(5) -0.011(4) -0.005(5) 0.035(5) C7 0.154(7) 0.110(5) 0.144(6) -0.023(4) -0.013(5) 0.023(5) C8 0.128(5) 0.092(4) 0.148(5) -0.025(4) -0.011(4) 0.015(3) C9 0.066(3) 0.066(3) 0.163(5) -0.001(3) 0.018(3) -0.005(2) C10 0.058(2) 0.061(2) 0.162(5) 0.028(3) 0.026(3) 0.0015(19) C11 0.063(3) 0.082(3) 0.178(5) 0.038(4) 0.035(3) -0.002(2) C12 0.082(4) 0.120(5) 0.170(6) 0.069(5) 0.034(4) 0.004(3) C13 0.111(4) 0.153(5) 0.137(5) 0.056(4) 0.030(4) 0.004(4) C14 0.085(3) 0.125(4) 0.133(5) 0.040(4) 0.017(3) -0.018(3) C15 0.078(3) 0.072(3) 0.141(4) 0.029(3) 0.035(3) 0.011(2) C16 0.051(2) 0.063(2) 0.156(4) 0.039(3) 0.023(3) 0.0021(18) C17 0.074(3) 0.081(3) 0.194(6) 0.037(4) 0.032(3) -0.003(3) C18 0.065(3) 0.080(3) 0.218(7) 0.030(4) -0.004(4) -0.011(3) C19 0.086(4) 0.092(4) 0.178(6) 0.012(4) -0.010(4) -0.018(3) C20 0.070(3) 0.085(3) 0.146(5) 0.018(3) 0.012(3) -0.010(2) C21 0.075(2) 0.063(2) 0.0493(17) -0.0120(15) 0.0208(16) -0.0105(17) C22 0.086(3) 0.085(3) 0.065(2) -0.0249(19) 0.0306(19) -0.015(2) C23 0.088(3) 0.087(3) 0.059(2) -0.0269(19) 0.0196(19) -0.019(2) C24 0.066(2) 0.062(2) 0.0489(16) -0.0100(15) 0.0108(15) -0.0069(16) C25 0.066(2) 0.061(2) 0.0503(17) -0.0087(15) 0.0020(15) -0.0043(16) C26 0.065(2) 0.071(2) 0.0503(17) -0.0127(16) 0.0039(15) -0.0067(17) C27 0.088(3) 0.079(3) 0.086(3) -0.009(2) -0.013(2) -0.004(2) C28 0.102(3) 0.070(3) 0.107(3) -0.011(2) -0.009(3) -0.017(2) C29 0.082(3) 0.087(3) 0.067(2) -0.019(2) -0.003(2) -0.017(2) C30 0.107(3) 0.099(3) 0.074(3) -0.005(2) -0.028(2) -0.009(3) C31 0.113(3) 0.075(3) 0.073(2) -0.004(2) -0.018(2) -0.010(2) C32 0.0552(18) 0.061(2) 0.0516(17) -0.0054(15) 0.0021(14) -0.0001(15) C33 0.056(2) 0.089(3) 0.069(2) -0.019(2) -0.0080(16) 0.0017(19) C34 0.055(2) 0.094(3) 0.071(2) -0.021(2) 0.0009(17) 0.0101(18) C35 0.0562(18) 0.065(2) 0.0546(18) -0.0062(16) 0.0060(15) 0.0089(16) C36 0.0595(19) 0.0553(18) 0.0549(17) -0.0063(15) 0.0096(14) 0.0057(15) C37 0.0546(18) 0.063(2) 0.0576(18) -0.0081(16) 0.0081(15) 0.0059(16) C38 0.073(2) 0.061(2) 0.085(2) -0.0132(19) 0.0219(19) -0.0008(18) C39 0.075(2) 0.072(2) 0.086(3) -0.007(2) 0.028(2) -0.0061(19) C40 0.061(2) 0.080(3) 0.064(2) 0.0003(19) 0.0143(16) 0.0204(18) C41 0.084(2) 0.066(2) 0.080(2) 0.0003(19) 0.024(2) 0.027(2) C42 0.072(2) 0.063(2) 0.068(2) -0.0001(17) 0.0183(17) 0.0121(17) C43 0.0566(18) 0.0549(18) 0.0474(16) -0.0043(14) 0.0100(14) 0.0042(14) C44 0.067(2) 0.072(2) 0.0480(17) -0.0121(16) 0.0116(15) 0.0032(17) C45 0.065(2) 0.071(2) 0.0497(17) -0.0120(16) 0.0103(15) -0.0034(17) C46 0.0598(18) 0.0564(18) 0.0430(15) -0.0041(14) 0.0085(14) -0.0003(15) C47 0.0595(18) 0.0527(17) 0.0464(16) -0.0003(14) 0.0085(14) -0.0024(14) C48 0.0562(17) 0.0583(19) 0.0434(15) -0.0016(14) 0.0083(13) -0.0019(15) C49 0.064(2) 0.056(2) 0.069(2) 0.0013(17) -0.0028(16) 0.0033(16) C50 0.071(2) 0.055(2) 0.073(2) -0.0020(17) 0.0013(18) -0.0015(17) C51 0.073(2) 0.064(2) 0.0466(17) -0.0001(15) 0.0093(15) -0.0166(17) C52 0.089(3) 0.066(2) 0.075(2) 0.0079(19) -0.019(2) -0.002(2) C53 0.084(2) 0.056(2) 0.078(2) -0.0013(18) -0.012(2) -0.0014(18) C54 0.0545(17) 0.0499(17) 0.0518(17) -0.0020(14) 0.0103(14) -0.0009(14) C55 0.0571(19) 0.067(2) 0.0606(19) -0.0057(17) 0.0088(15) -0.0046(16) C56 0.062(2) 0.072(2) 0.065(2) -0.0101(17) 0.0247(16) -0.0056(17) C57 0.0626(19) 0.0581(19) 0.0515(17) -0.0033(15) 0.0186(15) -0.0061(15) C58 0.070(2) 0.0591(19) 0.0547(18) -0.0072(15) 0.0248(16) -0.0101(16) C59 0.078(2) 0.070(2) 0.061(2) -0.0161(18) 0.0249(18) -0.0197(19) C60 0.112(3) 0.090(3) 0.092(3) -0.004(2) 0.054(3) 0.007(3) C61 0.121(4) 0.119(4) 0.117(4) -0.015(3) 0.060(3) 0.015(3) C62 0.093(3) 0.139(5) 0.088(3) -0.036(3) 0.046(3) -0.022(3) C63 0.108(4) 0.146(5) 0.061(2) -0.012(3) 0.035(2) -0.036(4) C64 0.091(3) 0.105(3) 0.062(2) -0.007(2) 0.026(2) -0.018(2) C65 0.317(11) 0.086(4) 0.125(5) 0.015(4) 0.029(6) 0.020(5) C66 0.228(12) 0.156(9) 0.54(3) -0.056(12) -0.138(14) 0.101(9) C67 0.341(18) 0.245(14) 0.226(12) -0.003(11) -0.050(12) 0.095(12) C68 0.34(2) 0.201(16) 0.72(4) 0.08(2) 0.00(2) -0.070(16) Cl2 0.1009(8) 0.1172(9) 0.0935(7) 0.0104(6) 0.0464(6) 0.0435(7) Cl3 0.0997(7) 0.0832(7) 0.0591(5) 0.0004(4) -0.0076(5) -0.0314(5) Cl4 0.1339(13) 0.328(3) 0.1381(13) -0.0844(16) 0.0920(11) -0.0257(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N4 1.872(4) . ? Co1 N3 1.885(4) . ? Co1 C2 1.920(4) . ? Co1 C1 1.924(4) . ? Co1 N6 1.965(3) . ? Co1 N5 1.972(4) . ? Mn1 N7 2.010(2) . ? Mn1 N9 2.012(2) . ? Mn1 N8 2.015(3) . ? Mn1 N10 2.016(3) . ? Mn1 N2 2.260(3) . ? Mn1 O3 2.305(2) . ? Cl1 C29 1.744(4) . ? O1 C9 1.250(6) . ? O2 C15 1.274(6) . ? O3 C65 1.397(6) . ? O3 H3 0.8200 . ? O4 C67 1.476(14) . ? O4 H4 0.8200 . ? O5 C66 1.416(16) . ? O5 H5 0.8200 . ? O6 C68 1.401(19) . ? O6 H6 0.8200 . ? N1 C1 1.133(5) . ? N2 C2 1.147(4) . ? N3 C9 1.344(6) . ? N3 C3 1.389(7) . ? N4 C15 1.330(6) . ? N4 C4 1.422(7) . ? N5 C14 1.320(7) . ? N5 C10 1.364(6) . ? N6 C20 1.314(6) . ? N6 C16 1.359(6) . ? N7 C24 1.369(4) . ? N7 C21 1.379(4) . ? N8 C32 1.385(4) . ? N8 C35 1.390(4) . ? N9 C43 1.372(4) . ? N9 C46 1.383(4) . ? N10 C57 1.381(4) . ? N10 C54 1.387(4) . ? C3 C4 1.394(7) . ? C3 C8 1.414(7) . ? C4 C5 1.417(7) . ? C5 C6 1.419(9) . ? C5 H47 0.9300 . ? C6 C7 1.309(9) . ? C6 H48 0.9300 . ? C7 C8 1.407(9) . ? C7 H49 0.9300 . ? C8 H50 0.9300 . ? C9 C10 1.435(7) . ? C10 C11 1.408(7) . ? C11 C12 1.326(8) . ? C11 H54 0.9300 . ? C12 C13 1.328(8) . ? C12 H55 0.9300 . ? C13 C14 1.414(7) . ? C13 H56 0.9300 . ? C14 H57 0.9300 . ? C15 C16 1.458(7) . ? C16 C17 1.387(7) . ? C17 C18 1.367(8) . ? C17 H61 0.9300 . ? C18 C19 1.354(8) . ? C18 H62 0.9300 . ? C19 C20 1.395(7) . ? C19 H63 0.9300 . ? C20 H64 0.9300 . ? C21 C58 1.379(5) . ? C21 C22 1.433(5) . ? C22 C23 1.318(5) . ? C22 H2 0.9300 . ? C23 C24 1.422(5) . ? C23 H3A 0.9300 . ? C24 C25 1.409(5) . ? C25 C32 1.394(4) . ? C25 C26 1.486(4) . ? C26 C27 1.356(6) . ? C26 C31 1.385(5) . ? C27 C28 1.402(6) . ? C27 H26 0.9300 . ? C28 C29 1.357(6) . ? C28 H25 0.9300 . ? C29 C30 1.359(6) . ? C30 C31 1.379(6) . ? C30 H23 0.9300 . ? C31 H22 0.9300 . ? C32 C33 1.420(5) . ? C33 C34 1.350(5) . ? C33 H7 0.9300 . ? C34 C35 1.421(5) . ? C34 H8 0.9300 . ? C35 C36 1.389(4) . ? C36 C43 1.394(4) . ? C36 C37 1.501(4) . ? C37 C38 1.364(5) . ? C37 C42 1.393(5) . ? C38 C39 1.388(5) . ? C38 H32 0.9300 . ? C39 C40 1.352(5) . ? C39 H31 0.9300 . ? C40 C41 1.386(5) . ? C40 Cl2 1.740(3) . ? C41 C42 1.375(5) . ? C41 H29 0.9300 . ? C42 H28 0.9300 . ? C43 C44 1.435(4) . ? C44 C45 1.335(5) . ? C44 H12 0.9300 . ? C45 C46 1.424(4) . ? C45 H13 0.9300 . ? C46 C47 1.400(4) . ? C47 C54 1.393(4) . ? C47 C48 1.489(4) . ? C48 C49 1.374(5) . ? C48 C53 1.392(5) . ? C49 C50 1.383(5) . ? C49 H34 0.9300 . ? C50 C51 1.365(5) . ? C50 H35 0.9300 . ? C51 C52 1.376(5) . ? C51 Cl3 1.744(3) . ? C52 C53 1.384(5) . ? C52 H37 0.9300 . ? C53 H38 0.9300 . ? C54 C55 1.427(4) . ? C55 C56 1.331(5) . ? C55 H17 0.9300 . ? C56 C57 1.432(5) . ? C56 H18 0.9300 . ? C57 C58 1.403(4) . ? C58 C59 1.497(5) . ? C59 C60 1.359(6) . ? C59 C64 1.378(5) . ? C60 C61 1.380(6) . ? C60 H44 0.9300 . ? C61 C62 1.341(8) . ? C61 H43 0.9300 . ? C62 C63 1.337(7) . ? C62 Cl4 1.756(4) . ? C63 C64 1.417(6) . ? C63 H41 0.9300 . ? C64 H40 0.9300 . ? C65 H67A 0.9600 . ? C65 H67B 0.9600 . ? C65 H67C 0.9600 . ? C66 H69A 0.9600 . ? C66 H69B 0.9600 . ? C66 H69C 0.9600 . ? C67 H68A 0.9600 . ? C67 H68B 0.9600 . ? C67 H68C 0.9600 . ? C68 H70A 0.9600 . ? C68 H70B 0.9600 . ? C68 H70C 0.9600 . ? 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 N4 Co1 N3 84.25(19) . . ? N4 Co1 C2 90.69(14) . . ? N3 Co1 C2 92.02(14) . . ? N4 Co1 C1 89.03(19) . . ? N3 Co1 C1 91.45(17) . . ? C2 Co1 C1 176.47(16) . . ? N4 Co1 N6 83.30(18) . . ? N3 Co1 N6 167.46(19) . . ? C2 Co1 N6 86.69(13) . . ? C1 Co1 N6 89.78(15) . . ? N4 Co1 N5 166.30(17) . . ? N3 Co1 N5 82.56(18) . . ? C2 Co1 N5 93.46(14) . . ? C1 Co1 N5 87.61(18) . . ? N6 Co1 N5 109.96(18) . . ? N7 Mn1 N9 177.30(10) . . ? N7 Mn1 N8 89.80(10) . . ? N9 Mn1 N8 89.98(10) . . ? N7 Mn1 N10 90.24(10) . . ? N9 Mn1 N10 89.88(10) . . ? N8 Mn1 N10 177.82(10) . . ? N7 Mn1 N2 89.09(10) . . ? N9 Mn1 N2 93.61(10) . . ? N8 Mn1 N2 91.31(10) . . ? N10 Mn1 N2 90.87(10) . . ? N7 Mn1 O3 87.55(10) . . ? N9 Mn1 O3 89.75(10) . . ? N8 Mn1 O3 88.06(11) . . ? N10 Mn1 O3 89.77(11) . . ? N2 Mn1 O3 176.59(9) . . ? C65 O3 Mn1 128.1(3) . . ? C65 O3 H3 109.8 . . ? Mn1 O3 H3 121.6 . . ? C67 O4 H4 109.5 . . ? C66 O5 H5 109.5 . . ? C68 O6 H6 109.5 . . ? C2 N2 Mn1 161.0(3) . . ? C9 N3 C3 129.1(5) . . ? C9 N3 Co1 117.4(4) . . ? C3 N3 Co1 113.5(3) . . ? C15 N4 C4 128.0(5) . . ? C15 N4 Co1 116.9(4) . . ? C4 N4 Co1 114.7(3) . . ? C14 N5 C10 117.9(4) . . ? C14 N5 Co1 130.4(3) . . ? C10 N5 Co1 111.6(4) . . ? C20 N6 C16 118.8(4) . . ? C20 N6 Co1 130.2(3) . . ? C16 N6 Co1 110.6(3) . . ? C24 N7 C21 106.4(2) . . ? C24 N7 Mn1 126.7(2) . . ? C21 N7 Mn1 126.4(2) . . ? C32 N8 C35 105.6(3) . . ? C32 N8 Mn1 127.3(2) . . ? C35 N8 Mn1 127.1(2) . . ? C43 N9 C46 106.4(2) . . ? C43 N9 Mn1 126.65(19) . . ? C46 N9 Mn1 126.64(19) . . ? C57 N10 C54 105.6(2) . . ? C57 N10 Mn1 126.8(2) . . ? C54 N10 Mn1 127.58(19) . . ? N1 C1 Co1 176.4(5) . . ? N2 C2 Co1 175.3(3) . . ? N3 C3 C4 115.5(5) . . ? N3 C3 C8 125.4(6) . . ? C4 C3 C8 119.1(6) . . ? C3 C4 C5 122.4(6) . . ? C3 C4 N4 111.7(5) . . ? C5 C4 N4 125.9(6) . . ? C4 C5 C6 115.8(7) . . ? C4 C5 H47 122.1 . . ? C6 C5 H47 122.1 . . ? C7 C6 C5 122.1(8) . . ? C7 C6 H48 119.0 . . ? C5 C6 H48 119.0 . . ? C6 C7 C8 123.5(7) . . ? C6 C7 H49 118.2 . . ? C8 C7 H49 118.2 . . ? C7 C8 C3 117.2(7) . . ? C7 C8 H50 121.4 . . ? C3 C8 H50 121.4 . . ? O1 C9 N3 125.6(6) . . ? O1 C9 C10 121.9(5) . . ? N3 C9 C10 112.4(4) . . ? N5 C10 C11 121.1(6) . . ? N5 C10 C9 116.0(4) . . ? C11 C10 C9 122.9(5) . . ? C12 C11 C10 119.5(5) . . ? C12 C11 H54 120.2 . . ? C10 C11 H54 120.2 . . ? C11 C12 C13 120.0(6) . . ? C11 C12 H55 120.0 . . ? C13 C12 H55 120.0 . . ? C12 C13 C14 120.4(7) . . ? C12 C13 H56 119.8 . . ? C14 C13 H56 119.8 . . ? N5 C14 C13 121.0(6) . . ? N5 C14 H57 119.5 . . ? C13 C14 H57 119.5 . . ? O2 C15 N4 127.5(6) . . ? O2 C15 C16 121.1(5) . . ? N4 C15 C16 111.4(4) . . ? N6 C16 C17 120.4(6) . . ? N6 C16 C15 116.0(4) . . ? C17 C16 C15 123.5(5) . . ? C18 C17 C16 118.4(6) . . ? C18 C17 H61 120.8 . . ? C16 C17 H61 120.8 . . ? C19 C18 C17 122.5(5) . . ? C19 C18 H62 118.8 . . ? C17 C18 H62 118.8 . . ? C18 C19 C20 115.8(6) . . ? C18 C19 H63 122.1 . . ? C20 C19 H63 122.1 . . ? N6 C20 C19 124.1(5) . . ? N6 C20 H64 117.9 . . ? C19 C20 H64 117.9 . . ? C58 C21 N7 126.8(3) . . ? C58 C21 C22 125.1(3) . . ? N7 C21 C22 108.1(3) . . ? C23 C22 C21 108.3(3) . . ? C23 C22 H2 125.9 . . ? C21 C22 H2 125.9 . . ? C22 C23 C24 107.7(3) . . ? C22 C23 H3A 126.2 . . ? C24 C23 H3A 126.2 . . ? N7 C24 C25 126.1(3) . . ? N7 C24 C23 109.4(3) . . ? C25 C24 C23 124.4(3) . . ? C32 C25 C24 123.7(3) . . ? C32 C25 C26 119.1(3) . . ? C24 C25 C26 117.2(3) . . ? C27 C26 C31 117.4(3) . . ? C27 C26 C25 121.1(3) . . ? C31 C26 C25 121.5(3) . . ? C26 C27 C28 121.5(4) . . ? C26 C27 H26 119.3 . . ? C28 C27 H26 119.3 . . ? C29 C28 C27 119.2(4) . . ? C29 C28 H25 120.4 . . ? C27 C28 H25 120.4 . . ? C28 C29 C30 120.9(4) . . ? C28 C29 Cl1 119.5(3) . . ? C30 C29 Cl1 119.5(3) . . ? C29 C30 C31 119.0(4) . . ? C29 C30 H23 120.5 . . ? C31 C30 H23 120.5 . . ? C30 C31 C26 122.0(4) . . ? C30 C31 H22 119.0 . . ? C26 C31 H22 119.0 . . ? N8 C32 C25 125.4(3) . . ? N8 C32 C33 109.8(3) . . ? C25 C32 C33 124.8(3) . . ? C34 C33 C32 107.4(3) . . ? C34 C33 H7 126.3 . . ? C32 C33 H7 126.3 . . ? C33 C34 C35 107.8(3) . . ? C33 C34 H8 126.1 . . ? C35 C34 H8 126.1 . . ? C36 C35 N8 125.1(3) . . ? C36 C35 C34 125.5(3) . . ? N8 C35 C34 109.4(3) . . ? C35 C36 C43 124.3(3) . . ? C35 C36 C37 118.6(3) . . ? C43 C36 C37 117.0(3) . . ? C38 C37 C42 118.1(3) . . ? C38 C37 C36 120.6(3) . . ? C42 C37 C36 121.3(3) . . ? C37 C38 C39 121.6(3) . . ? C37 C38 H32 119.2 . . ? C39 C38 H32 119.2 . . ? C40 C39 C38 119.1(4) . . ? C40 C39 H31 120.4 . . ? C38 C39 H31 120.4 . . ? C39 C40 C41 121.3(3) . . ? C39 C40 Cl2 119.5(3) . . ? C41 C40 Cl2 119.2(3) . . ? C42 C41 C40 118.6(3) . . ? C42 C41 H29 120.7 . . ? C40 C41 H29 120.7 . . ? C41 C42 C37 121.2(4) . . ? C41 C42 H28 119.4 . . ? C37 C42 H28 119.4 . . ? N9 C43 C36 126.4(3) . . ? N9 C43 C44 108.9(3) . . ? C36 C43 C44 124.6(3) . . ? C45 C44 C43 107.8(3) . . ? C45 C44 H12 126.1 . . ? C43 C44 H12 126.1 . . ? C44 C45 C46 107.7(3) . . ? C44 C45 H13 126.1 . . ? C46 C45 H13 126.1 . . ? N9 C46 C47 126.2(3) . . ? N9 C46 C45 109.1(3) . . ? C47 C46 C45 124.6(3) . . ? C54 C47 C46 124.2(3) . . ? C54 C47 C48 118.7(3) . . ? C46 C47 C48 116.8(3) . . ? C49 C48 C53 116.7(3) . . ? C49 C48 C47 119.9(3) . . ? C53 C48 C47 123.4(3) . . ? C48 C49 C50 122.9(3) . . ? C48 C49 H34 118.6 . . ? C50 C49 H34 118.6 . . ? C51 C50 C49 118.5(3) . . ? C51 C50 H35 120.7 . . ? C49 C50 H35 120.7 . . ? C50 C51 C52 121.2(3) . . ? C50 C51 Cl3 119.0(3) . . ? C52 C51 Cl3 119.8(3) . . ? C51 C52 C53 118.8(3) . . ? C51 C52 H37 120.6 . . ? C53 C52 H37 120.6 . . ? C52 C53 C48 121.8(3) . . ? C52 C53 H38 119.1 . . ? C48 C53 H38 119.1 . . ? N10 C54 C47 125.1(3) . . ? N10 C54 C55 109.6(3) . . ? C47 C54 C55 125.2(3) . . ? C56 C55 C54 107.5(3) . . ? C56 C55 H17 126.3 . . ? C54 C55 H17 126.3 . . ? C55 C56 C57 108.1(3) . . ? C55 C56 H18 126.0 . . ? C57 C56 H18 126.0 . . ? N10 C57 C58 125.6(3) . . ? N10 C57 C56 109.2(3) . . ? C58 C57 C56 125.2(3) . . ? C21 C58 C57 124.0(3) . . ? C21 C58 C59 118.6(3) . . ? C57 C58 C59 117.4(3) . . ? C60 C59 C64 117.9(4) . . ? C60 C59 C58 121.5(3) . . ? C64 C59 C58 120.6(4) . . ? C59 C60 C61 122.6(5) . . ? C59 C60 H44 118.7 . . ? C61 C60 H44 118.7 . . ? C62 C61 C60 117.9(5) . . ? C62 C61 H43 121.0 . . ? C60 C61 H43 121.0 . . ? C63 C62 C61 123.3(4) . . ? C63 C62 Cl4 118.6(5) . . ? C61 C62 Cl4 118.1(5) . . ? C62 C63 C64 118.2(4) . . ? C62 C63 H41 120.9 . . ? C64 C63 H41 120.9 . . ? C59 C64 C63 120.1(5) . . ? C59 C64 H40 120.0 . . ? C63 C64 H40 120.0 . . ? O3 C65 H67A 109.5 . . ? O3 C65 H67B 109.5 . . ? H67A C65 H67B 109.5 . . ? O3 C65 H67C 109.5 . . ? H67A C65 H67C 109.5 . . ? H67B C65 H67C 109.5 . . ? O5 C66 H69A 109.5 . . ? O5 C66 H69B 109.5 . . ? H69A C66 H69B 109.5 . . ? O5 C66 H69C 109.5 . . ? H69A C66 H69C 109.5 . . ? H69B C66 H69C 109.5 . . ? O4 C67 H68A 109.5 . . ? O4 C67 H68B 109.5 . . ? H68A C67 H68B 109.5 . . ? O4 C67 H68C 109.5 . . ? H68A C67 H68C 109.5 . . ? H68B C67 H68C 109.5 . . ? O6 C68 H70A 109.5 . . ? O6 C68 H70B 109.5 . . ? H70A C68 H70B 109.5 . . ? O6 C68 H70C 109.5 . . ? H70A C68 H70C 109.5 . . ? H70B C68 H70C 109.5 . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.293 0.750 469 12 ' ' 2 0.750 0.201 0.250 469 12 ' ' _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.638 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.061 data_test _database_code_depnum_ccdc_archive 'CCDC 898331' #TrackingRef 'Crbpb,4-ClTPPMn 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H44 Cl4 Cr Mn N10 O5' _chemical_formula_weight 1293.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.102(4) _cell_length_b 18.120(4) _cell_length_c 24.444(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.438(4) _cell_angle_gamma 90.00 _cell_volume 7035(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1897 _cell_measurement_theta_min 2.321 _cell_measurement_theta_max 25.278 _exptl_crystal_description block _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2644 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9433 _exptl_absorpt_correction_T_max 0.9634 _exptl_absorpt_process_details 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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34452 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.1375 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.01 _reflns_number_total 12257 _reflns_number_gt 4985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0900P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12257 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1894 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 Mn1 Mn 0.85542(6) 0.75185(5) 0.12819(3) 0.0489(3) Uani 1 1 d . . . Cr1 Cr 0.77298(7) 0.48111(6) 0.04344(5) 0.0696(4) Uani 1 1 d . . . Cl1 Cl 0.44291(13) 1.00773(10) -0.11797(7) 0.0857(6) Uani 1 1 d . . . Cl2 Cl 1.26914(14) 0.48531(12) 0.36476(9) 0.1052(7) Uani 1 1 d . . . Cl3 Cl 0.45176(18) 0.6055(2) 0.34431(11) 0.1670(13) Uani 1 1 d . . . Cl4 Cl 1.25555(14) 0.90519(12) -0.08855(8) 0.1052(7) Uani 1 1 d . . . O1 O 0.6008(4) 0.4806(3) 0.1472(3) 0.118(2) Uani 1 1 d . . . O2 O 0.9926(4) 0.3683(3) 0.0845(3) 0.128(2) Uani 1 1 d . . . O3 O 0.8726(3) 0.8570(3) 0.18035(18) 0.0834(14) Uani 1 1 d . . . H3A H 0.8894 0.8597 0.2136 0.100 Uiso 1 1 d R . . O4 O 0.9386(7) 0.8607(7) 0.2923(4) 0.284(7) Uani 1 1 d . . . H4A H 0.9420 0.8316 0.3244 0.341 Uiso 1 1 d R . . H4B H 0.8949 0.8584 0.2682 0.341 Uiso 1 1 d R . . O5 O 0.6390(9) 0.1948(10) 0.9235(9) 0.465(13) Uani 1 1 d . . . H5B H 0.6217 0.1893 0.9537 0.557 Uiso 1 1 d R . . H5A H 0.6536 0.2379 0.9161 0.557 Uiso 1 1 d R . . N1 N 0.8372(3) 0.6464(3) 0.0794(2) 0.0561(14) Uani 1 1 d . . . N2 N 0.6909(5) 0.3321(5) -0.0091(4) 0.155(4) Uani 1 1 d . . . N3 N 0.7261(4) 0.4732(3) 0.1120(3) 0.0772(17) Uani 1 1 d . . . N4 N 0.8687(4) 0.4314(3) 0.0894(3) 0.0809(18) Uani 1 1 d . . . N5 N 0.6585(4) 0.5329(3) 0.0191(3) 0.0766(17) Uani 1 1 d . . . N6 N 0.8526(4) 0.4694(3) -0.0132(3) 0.0782(17) Uani 1 1 d . . . N7 N 0.8582(3) 0.6942(3) 0.19794(18) 0.0537(13) Uani 1 1 d . . . N8 N 0.7299(3) 0.7635(2) 0.12168(18) 0.0495(12) Uani 1 1 d . . . N9 N 0.8535(3) 0.8132(2) 0.05976(18) 0.0497(12) Uani 1 1 d . . . N10 N 0.9804(3) 0.7436(3) 0.13614(18) 0.0522(12) Uani 1 1 d . . . C1 C 0.8187(4) 0.5881(4) 0.0652(3) 0.0621(18) Uani 1 1 d . . . C2 C 0.7190(5) 0.3833(4) 0.0128(4) 0.095(3) Uani 1 1 d . . . C3 C 0.7818(6) 0.4432(4) 0.1588(4) 0.092(2) Uani 1 1 d . . . C4 C 0.8600(7) 0.4226(4) 0.1458(4) 0.088(2) Uani 1 1 d . . . C5 C 0.9249(7) 0.3963(5) 0.1863(5) 0.117(3) Uani 1 1 d . . . H5 H 0.9763 0.3817 0.1773 0.140 Uiso 1 1 calc R . . C6 C 0.9095(9) 0.3930(6) 0.2402(6) 0.131(4) Uani 1 1 d . . . H6 H 0.9521 0.3783 0.2685 0.157 Uiso 1 1 calc R . . C7 C 0.8312(11) 0.4112(6) 0.2521(5) 0.141(4) Uani 1 1 d . . . H7 H 0.8218 0.4061 0.2885 0.169 Uiso 1 1 calc R . . C8 C 0.7658(8) 0.4369(5) 0.2126(5) 0.119(3) Uani 1 1 d . . . H8 H 0.7137 0.4492 0.2218 0.142 Uiso 1 1 calc R . . C9 C 0.9203(5) 0.4284(4) 0.0049(4) 0.083(2) Uani 1 1 d . . . C10 C 0.9774(5) 0.4079(5) -0.0283(5) 0.101(3) Uani 1 1 d . . . H10 H 1.0227 0.3777 -0.0147 0.122 Uiso 1 1 calc R . . C11 C 0.9661(7) 0.4328(6) -0.0817(6) 0.118(3) Uani 1 1 d . . . H11 H 1.0054 0.4213 -0.1044 0.141 Uiso 1 1 calc R . . C12 C 0.8981(6) 0.4739(5) -0.1017(4) 0.107(3) Uani 1 1 d . . . H12 H 0.8897 0.4905 -0.1382 0.128 Uiso 1 1 calc R . . C13 C 0.8406(5) 0.4914(5) -0.0668(5) 0.099(3) Uani 1 1 d . . . H13 H 0.7928 0.5187 -0.0807 0.118 Uiso 1 1 calc R . . C14 C 0.9306(5) 0.4063(4) 0.0639(5) 0.089(2) Uani 1 1 d . . . C15 C 0.6119(5) 0.5326(4) 0.0605(4) 0.080(2) Uani 1 1 d . . . C16 C 0.5379(6) 0.5726(5) 0.0544(5) 0.105(3) Uani 1 1 d . . . H16 H 0.5067 0.5728 0.0832 0.126 Uiso 1 1 calc R . . C17 C 0.5102(6) 0.6104(6) 0.0093(6) 0.124(4) Uani 1 1 d . . . H17 H 0.4601 0.6368 0.0062 0.149 Uiso 1 1 calc R . . C18 C 0.5571(7) 0.6104(5) -0.0341(6) 0.127(4) Uani 1 1 d . . . H18 H 0.5384 0.6363 -0.0666 0.152 Uiso 1 1 calc R . . C19 C 0.6324(5) 0.5708(4) -0.0277(4) 0.090(2) Uani 1 1 d . . . H19 H 0.6646 0.5707 -0.0560 0.108 Uiso 1 1 calc R . . C20 C 0.6464(6) 0.4920(5) 0.1108(4) 0.087(2) Uani 1 1 d . . . C21 C 0.7903(4) 0.6762(4) 0.2226(2) 0.0597(17) Uani 1 1 d . . . C22 C 0.8171(5) 0.6270(4) 0.2693(3) 0.078(2) Uani 1 1 d . . . H22 H 0.7836 0.6064 0.2928 0.093 Uiso 1 1 calc R . . C23 C 0.9002(5) 0.6177(4) 0.2714(3) 0.081(2) Uani 1 1 d . . . H23 H 0.9351 0.5894 0.2973 0.097 Uiso 1 1 calc R . . C24 C 0.9260(4) 0.6582(3) 0.2274(2) 0.0582(17) Uani 1 1 d . . . C25 C 1.0083(4) 0.6636(3) 0.2186(2) 0.0574(16) Uani 1 1 d . . . C26 C 1.0746(4) 0.6197(4) 0.2554(3) 0.0637(18) Uani 1 1 d . . . C27 C 1.0713(4) 0.5444(4) 0.2538(3) 0.0705(19) Uani 1 1 d . . . H27 H 1.0280 0.5211 0.2302 0.085 Uiso 1 1 calc R . . C28 C 1.1319(5) 0.5024(4) 0.2869(3) 0.079(2) Uani 1 1 d . . . H28 H 1.1299 0.4511 0.2853 0.095 Uiso 1 1 calc R . . C29 C 1.1944(5) 0.5376(5) 0.3220(3) 0.073(2) Uani 1 1 d . . . C30 C 1.1981(5) 0.6130(5) 0.3248(3) 0.084(2) Uani 1 1 d . . . H30 H 1.2411 0.6366 0.3485 0.101 Uiso 1 1 calc R . . C31 C 1.1372(5) 0.6525(4) 0.2921(3) 0.080(2) Uani 1 1 d . . . H31 H 1.1381 0.7037 0.2947 0.096 Uiso 1 1 calc R . . C32 C 1.0343(4) 0.7051(3) 0.1769(2) 0.0604(17) Uani 1 1 d . . . C33 C 1.1191(4) 0.7133(4) 0.1673(3) 0.079(2) Uani 1 1 d . . . H33 H 1.1666 0.6921 0.1882 0.094 Uiso 1 1 calc R . . C34 C 1.1184(4) 0.7566(4) 0.1234(3) 0.078(2) Uani 1 1 d . . . H34 H 1.1651 0.7725 0.1088 0.094 Uiso 1 1 calc R . . C35 C 1.0326(4) 0.7742(3) 0.1026(2) 0.0602(17) Uani 1 1 d . . . C36 C 1.0051(4) 0.8134(3) 0.0545(2) 0.0551(16) Uani 1 1 d . . . C37 C 1.0692(4) 0.8369(4) 0.0200(2) 0.0533(15) Uani 1 1 d . . . C38 C 1.1111(4) 0.7868(4) -0.0057(3) 0.073(2) Uani 1 1 d . . . H38 H 1.1004 0.7370 -0.0008 0.088 Uiso 1 1 calc R . . C39 C 1.1693(4) 0.8061(4) -0.0390(3) 0.075(2) Uani 1 1 d . . . H39 H 1.1972 0.7701 -0.0561 0.090 Uiso 1 1 calc R . . C40 C 1.1849(4) 0.8787(5) -0.0460(3) 0.0688(19) Uani 1 1 d . . . C41 C 1.1426(5) 0.9310(4) -0.0208(3) 0.079(2) Uani 1 1 d . . . H41 H 1.1521 0.9808 -0.0264 0.095 Uiso 1 1 calc R . . C42 C 1.0870(4) 0.9105(4) 0.0124(3) 0.0673(18) Uani 1 1 d . . . H42 H 1.0604 0.9465 0.0304 0.081 Uiso 1 1 calc R . . C43 C 0.9215(4) 0.8298(3) 0.0345(2) 0.0517(15) Uani 1 1 d . . . C44 C 0.8921(4) 0.8667(3) -0.0163(2) 0.0634(18) Uani 1 1 d . . . H44 H 0.9251 0.8839 -0.0415 0.076 Uiso 1 1 calc R . . C45 C 0.8081(5) 0.8724(4) -0.0214(2) 0.0689(19) Uani 1 1 d . . . H45 H 0.7727 0.8940 -0.0509 0.083 Uiso 1 1 calc R . . C46 C 0.7828(4) 0.8399(3) 0.0258(2) 0.0511(15) Uani 1 1 d . . . C47 C 0.7006(4) 0.8361(3) 0.0358(2) 0.0515(15) Uani 1 1 d . . . C48 C 0.6356(4) 0.8773(4) -0.0034(2) 0.0494(15) Uani 1 1 d . . . C49 C 0.6383(4) 0.9512(4) -0.0059(3) 0.0646(18) Uani 1 1 d . . . H49 H 0.6816 0.9756 0.0169 0.078 Uiso 1 1 calc R . . C50 C 0.5799(5) 0.9931(4) -0.0405(3) 0.0665(18) Uani 1 1 d . . . H50 H 0.5831 1.0444 -0.0408 0.080 Uiso 1 1 calc R . . C51 C 0.5176(4) 0.9563(4) -0.0743(2) 0.0613(17) Uani 1 1 d . . . C52 C 0.5120(5) 0.8819(4) -0.0729(3) 0.083(2) Uani 1 1 d . . . H52 H 0.4686 0.8574 -0.0955 0.100 Uiso 1 1 calc R . . C53 C 0.5713(5) 0.8430(4) -0.0373(3) 0.081(2) Uani 1 1 d . . . H53 H 0.5675 0.7919 -0.0363 0.097 Uiso 1 1 calc R . . C54 C 0.6770(4) 0.8005(3) 0.0811(2) 0.0509(15) Uani 1 1 d . . . C55 C 0.5936(4) 0.7982(3) 0.0930(3) 0.0599(17) Uani 1 1 d . . . H55 H 0.5463 0.8193 0.0717 0.072 Uiso 1 1 calc R . . C56 C 0.5951(4) 0.7603(3) 0.1405(3) 0.0630(17) Uani 1 1 d . . . H56 H 0.5493 0.7498 0.1579 0.076 Uiso 1 1 calc R . . C57 C 0.6802(4) 0.7391(3) 0.1589(2) 0.0517(15) Uani 1 1 d . . . C58 C 0.7065(4) 0.6990(3) 0.2066(2) 0.0569(16) Uani 1 1 d . . . C59 C 0.6442(4) 0.6766(4) 0.2420(3) 0.0607(17) Uani 1 1 d . . . C60 C 0.6359(5) 0.7133(4) 0.2888(3) 0.079(2) Uani 1 1 d . . . H60 H 0.6710 0.7532 0.2999 0.095 Uiso 1 1 calc R . . C61 C 0.5761(5) 0.6925(6) 0.3204(3) 0.095(3) Uani 1 1 d . . . H61 H 0.5702 0.7186 0.3523 0.114 Uiso 1 1 calc R . . C62 C 0.5266(6) 0.6345(6) 0.3045(4) 0.095(3) Uani 1 1 d . . . C63 C 0.5317(6) 0.5963(5) 0.2582(4) 0.111(3) Uani 1 1 d . . . H63 H 0.4966 0.5563 0.2475 0.133 Uiso 1 1 calc R . . C64 C 0.5918(6) 0.6191(5) 0.2267(3) 0.100(3) Uani 1 1 d . . . H64 H 0.5960 0.5940 0.1941 0.121 Uiso 1 1 calc R . . C65 C 0.8692(11) 0.9293(5) 0.1636(4) 0.212(7) Uani 1 1 d . . . H65A H 0.9176 0.9404 0.1468 0.317 Uiso 1 1 calc R . . H65B H 0.8686 0.9608 0.1951 0.317 Uiso 1 1 calc R . . H65C H 0.8190 0.9372 0.1371 0.317 Uiso 1 1 calc R . . 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 Mn1 0.0551(6) 0.0517(6) 0.0406(5) 0.0057(4) 0.0102(4) 0.0011(4) Cr1 0.0556(7) 0.0555(7) 0.0981(8) -0.0138(6) 0.0138(6) 0.0019(5) Cl1 0.1058(15) 0.0859(13) 0.0583(10) -0.0020(9) -0.0079(10) 0.0355(11) Cl2 0.0990(16) 0.1129(17) 0.0945(14) 0.0245(12) -0.0115(12) 0.0308(13) Cl3 0.123(2) 0.272(4) 0.1251(19) 0.058(2) 0.0770(17) -0.009(2) Cl4 0.1071(17) 0.1253(18) 0.0952(14) -0.0143(13) 0.0517(13) -0.0510(13) O1 0.111(5) 0.114(5) 0.143(5) -0.032(4) 0.065(4) -0.017(4) O2 0.084(4) 0.105(4) 0.186(6) -0.002(4) -0.003(4) 0.036(4) O3 0.118(4) 0.066(3) 0.064(3) -0.009(3) 0.008(3) -0.001(3) O4 0.280(12) 0.333(14) 0.194(8) -0.133(9) -0.091(8) 0.143(10) O5 0.279(16) 0.38(2) 0.66(3) -0.25(2) -0.148(18) -0.038(13) N1 0.055(3) 0.057(4) 0.059(3) -0.006(3) 0.015(3) 0.003(3) N2 0.083(5) 0.089(6) 0.283(11) -0.076(7) 0.003(6) 0.002(4) N3 0.066(4) 0.076(4) 0.095(5) -0.012(4) 0.029(4) -0.005(3) N4 0.057(4) 0.055(4) 0.128(6) -0.009(4) 0.007(4) -0.003(3) N5 0.062(4) 0.060(4) 0.107(5) -0.017(4) 0.010(4) -0.003(3) N6 0.066(4) 0.068(4) 0.099(5) -0.020(4) 0.009(4) -0.002(3) N7 0.056(3) 0.064(3) 0.044(3) 0.010(3) 0.015(3) 0.006(3) N8 0.062(3) 0.044(3) 0.044(3) 0.005(2) 0.014(3) 0.004(2) N9 0.049(3) 0.055(3) 0.045(3) 0.004(2) 0.006(3) -0.006(2) N10 0.056(3) 0.056(3) 0.044(3) 0.010(3) 0.007(2) -0.004(3) C1 0.052(4) 0.071(5) 0.065(4) 0.004(4) 0.017(3) 0.007(4) C2 0.055(5) 0.062(5) 0.167(8) -0.035(5) 0.012(5) -0.007(4) C3 0.089(7) 0.071(6) 0.113(8) 0.002(5) 0.005(6) -0.018(5) C4 0.116(8) 0.059(5) 0.085(6) 0.006(5) 0.007(6) -0.019(5) C5 0.127(9) 0.093(7) 0.122(8) 0.039(6) -0.004(7) -0.010(5) C6 0.135(11) 0.104(8) 0.138(11) 0.023(7) -0.025(9) -0.034(8) C7 0.190(13) 0.127(9) 0.098(8) 0.011(7) 0.003(10) -0.070(10) C8 0.157(10) 0.115(8) 0.082(6) 0.000(6) 0.017(7) -0.041(7) C9 0.055(5) 0.066(5) 0.128(8) -0.020(5) 0.017(5) 0.003(4) C10 0.059(6) 0.094(7) 0.156(9) -0.045(7) 0.032(6) 0.001(4) C11 0.077(7) 0.124(9) 0.156(10) -0.063(8) 0.030(7) -0.012(6) C12 0.088(7) 0.130(8) 0.108(7) -0.039(6) 0.032(6) -0.009(6) C13 0.066(6) 0.108(7) 0.123(8) -0.037(6) 0.017(6) 0.011(5) C14 0.062(6) 0.058(5) 0.144(9) -0.023(5) 0.007(6) -0.001(4) C15 0.061(5) 0.058(5) 0.121(7) -0.031(5) 0.020(5) -0.005(4) C16 0.083(7) 0.087(7) 0.148(9) -0.030(6) 0.028(6) 0.017(5) C17 0.058(6) 0.090(7) 0.217(13) -0.032(8) 0.000(8) 0.018(5) C18 0.083(8) 0.083(7) 0.202(12) -0.011(7) -0.012(8) 0.003(6) C19 0.065(6) 0.076(6) 0.125(7) -0.009(5) 0.003(5) 0.013(4) C20 0.078(7) 0.076(6) 0.115(7) -0.031(5) 0.032(6) -0.011(5) C21 0.068(5) 0.071(5) 0.042(3) 0.005(3) 0.014(3) 0.007(4) C22 0.084(6) 0.099(6) 0.055(4) 0.036(4) 0.026(4) 0.016(4) C23 0.074(5) 0.108(6) 0.065(4) 0.042(4) 0.025(4) 0.028(4) C24 0.071(5) 0.064(4) 0.043(3) 0.011(3) 0.017(3) 0.008(4) C25 0.055(4) 0.063(4) 0.052(4) 0.012(3) 0.003(3) 0.003(3) C26 0.065(5) 0.074(5) 0.052(4) 0.010(4) 0.009(4) -0.006(4) C27 0.067(5) 0.070(5) 0.068(4) 0.007(4) -0.009(4) 0.005(4) C28 0.093(6) 0.068(5) 0.076(5) 0.013(4) 0.012(5) -0.002(4) C29 0.069(5) 0.096(6) 0.052(4) 0.018(4) 0.005(4) 0.012(4) C30 0.090(6) 0.080(6) 0.074(5) 0.005(5) -0.014(4) -0.007(5) C31 0.104(6) 0.061(5) 0.065(4) 0.006(4) -0.018(4) 0.003(4) C32 0.070(5) 0.061(4) 0.051(4) 0.008(3) 0.010(4) -0.007(3) C33 0.051(5) 0.109(6) 0.073(5) 0.031(4) 0.001(4) -0.003(4) C34 0.052(5) 0.113(6) 0.069(4) 0.024(4) 0.010(4) -0.013(4) C35 0.062(5) 0.066(4) 0.051(4) 0.013(3) 0.006(3) -0.009(3) C36 0.061(5) 0.055(4) 0.049(4) 0.014(3) 0.008(3) -0.004(3) C37 0.055(4) 0.055(4) 0.051(4) 0.005(3) 0.012(3) -0.006(3) C38 0.075(5) 0.057(5) 0.091(5) 0.017(4) 0.026(4) -0.009(4) C39 0.072(5) 0.070(5) 0.088(5) -0.005(4) 0.026(4) -0.002(4) C40 0.067(5) 0.080(5) 0.061(4) 0.003(4) 0.017(4) -0.021(4) C41 0.088(6) 0.066(5) 0.088(5) -0.004(4) 0.032(5) -0.031(4) C42 0.071(5) 0.066(5) 0.068(4) -0.005(4) 0.022(4) -0.014(4) C43 0.060(4) 0.053(4) 0.042(3) 0.005(3) 0.008(3) -0.004(3) C44 0.066(5) 0.081(5) 0.046(4) 0.013(3) 0.017(3) 0.000(4) C45 0.079(6) 0.078(5) 0.049(4) 0.016(3) 0.009(4) 0.006(4) C46 0.059(4) 0.052(4) 0.042(3) 0.007(3) 0.005(3) -0.002(3) C47 0.050(4) 0.057(4) 0.048(3) -0.001(3) 0.010(3) 0.001(3) C48 0.058(4) 0.053(4) 0.038(3) 0.003(3) 0.010(3) 0.003(3) C49 0.074(5) 0.060(5) 0.059(4) 0.000(4) 0.006(4) -0.007(4) C50 0.081(5) 0.058(4) 0.060(4) 0.008(4) 0.007(4) 0.009(4) C51 0.075(5) 0.065(5) 0.044(4) -0.004(3) 0.008(3) 0.012(4) C52 0.101(6) 0.065(5) 0.072(5) -0.012(4) -0.022(4) 0.009(4) C53 0.103(6) 0.057(5) 0.073(5) 0.008(4) -0.015(5) 0.005(4) C54 0.056(4) 0.051(4) 0.045(3) 0.006(3) 0.007(3) 0.001(3) C55 0.052(4) 0.068(4) 0.059(4) 0.003(4) 0.005(3) 0.008(3) C56 0.059(5) 0.071(5) 0.062(4) 0.006(4) 0.019(3) 0.003(4) C57 0.057(4) 0.054(4) 0.048(3) 0.006(3) 0.020(3) 0.003(3) C58 0.067(5) 0.054(4) 0.054(4) 0.006(3) 0.021(3) 0.009(3) C59 0.067(5) 0.066(5) 0.054(4) 0.012(4) 0.026(4) 0.010(4) C60 0.084(6) 0.097(6) 0.064(4) 0.002(4) 0.032(4) 0.008(4) C61 0.075(6) 0.159(9) 0.056(5) 0.005(5) 0.023(4) 0.013(6) C62 0.080(6) 0.132(8) 0.080(6) 0.025(6) 0.038(5) 0.013(6) C63 0.118(8) 0.106(7) 0.122(7) 0.008(6) 0.057(6) -0.019(5) C64 0.128(7) 0.090(6) 0.100(6) -0.017(5) 0.065(6) -0.026(6) C65 0.45(2) 0.072(7) 0.116(8) -0.029(7) 0.069(11) -0.043(10) _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 Mn1 N7 1.994(5) . ? Mn1 N10 1.995(5) . ? Mn1 N9 2.005(4) . ? Mn1 N8 2.012(5) . ? Mn1 N1 2.246(6) . ? Mn1 O3 2.283(4) . ? Cr1 N3 1.952(6) . ? Cr1 N4 1.970(6) . ? Cr1 N6 2.046(7) . ? Cr1 C2 2.060(8) . ? Cr1 N5 2.068(6) . ? Cr1 C1 2.110(8) . ? Cl1 C51 1.741(7) . ? Cl2 C29 1.740(7) . ? Cl3 C62 1.750(8) . ? Cl4 C40 1.730(7) . ? O1 C20 1.261(9) . ? O2 C14 1.250(9) . ? O3 C65 1.371(10) . ? O3 H3A 0.8160 . ? O4 H4A 0.9407 . ? O4 H4A 0.9407 . ? O4 H4B 0.8409 . ? O5 H5B 0.8386 . ? O5 H5A 0.8435 . ? N1 C1 1.137(7) . ? N2 C2 1.129(8) . ? N3 C20 1.323(9) . ? N3 C3 1.440(10) . ? N4 C14 1.340(9) . ? N4 C4 1.418(10) . ? N5 C19 1.341(9) . ? N5 C15 1.355(9) . ? N6 C9 1.334(9) . ? N6 C13 1.352(10) . ? N7 C21 1.370(7) . ? N7 C24 1.370(7) . ? N8 C54 1.372(7) . ? N8 C57 1.379(7) . ? N9 C43 1.375(7) . ? N9 C46 1.382(7) . ? N10 C35 1.382(7) . ? N10 C32 1.397(7) . ? C3 C8 1.386(11) . ? C3 C4 1.399(11) . ? C4 C5 1.399(12) . ? C5 C6 1.380(14) . ? C5 H5 0.9300 . ? C6 C7 1.381(14) . ? C6 H6 0.9300 . ? C7 C8 1.387(15) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.373(11) . ? C9 C14 1.479(11) . ? C10 C11 1.365(12) . ? C10 H10 0.9300 . ? C11 C12 1.348(12) . ? C11 H11 0.9300 . ? C12 C13 1.395(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.382(11) . ? C15 C20 1.462(11) . ? C16 C17 1.313(12) . ? C16 H16 0.9300 . ? C17 C18 1.398(13) . ? C17 H17 0.9300 . ? C18 C19 1.396(11) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C21 C58 1.404(8) . ? C21 C22 1.457(8) . ? C22 C23 1.341(9) . ? C22 H22 0.9300 . ? C23 C24 1.420(8) . ? C23 H23 0.9300 . ? C24 C25 1.379(8) . ? C25 C32 1.387(8) . ? C25 C26 1.506(8) . ? C26 C27 1.365(8) . ? C26 C31 1.368(9) . ? C27 C28 1.389(9) . ? C27 H27 0.9300 . ? C28 C29 1.368(9) . ? C28 H28 0.9300 . ? C29 C30 1.369(9) . ? C30 C31 1.363(9) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.431(9) . ? C33 C34 1.327(8) . ? C33 H33 0.9300 . ? C34 C35 1.428(9) . ? C34 H34 0.9300 . ? C35 C36 1.382(8) . ? C36 C43 1.388(8) . ? C36 C37 1.498(8) . ? C37 C38 1.346(8) . ? C37 C42 1.383(8) . ? C38 C39 1.384(9) . ? C38 H38 0.9300 . ? C39 C40 1.355(9) . ? C39 H39 0.9300 . ? C40 C41 1.372(9) . ? C41 C42 1.354(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.423(7) . ? C44 C45 1.340(8) . ? C44 H44 0.9300 . ? C45 C46 1.413(8) . ? C45 H45 0.9300 . ? C46 C47 1.385(8) . ? C47 C54 1.386(7) . ? C47 C48 1.498(8) . ? C48 C49 1.342(8) . ? C48 C53 1.363(8) . ? C49 C50 1.385(8) . ? C49 H49 0.9300 . ? C50 C51 1.366(8) . ? C50 H50 0.9300 . ? C51 C52 1.351(9) . ? C52 C53 1.377(9) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.422(8) . ? C55 C56 1.347(8) . ? C55 H55 0.9300 . ? C56 C57 1.423(8) . ? C56 H56 0.9300 . ? C57 C58 1.380(8) . ? C58 C59 1.488(8) . ? C59 C60 1.347(8) . ? C59 C64 1.353(9) . ? C60 C61 1.382(10) . ? C60 H60 0.9300 . ? C61 C62 1.338(11) . ? C61 H61 0.9300 . ? C62 C63 1.340(11) . ? C63 C64 1.394(10) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Mn1 N10 89.8(2) . . ? N7 Mn1 N9 177.90(19) . . ? N10 Mn1 N9 90.00(19) . . ? N7 Mn1 N8 90.2(2) . . ? N10 Mn1 N8 177.97(18) . . ? N9 Mn1 N8 89.88(19) . . ? N7 Mn1 N1 89.44(19) . . ? N10 Mn1 N1 91.74(18) . . ? N9 Mn1 N1 92.66(18) . . ? N8 Mn1 N1 90.28(18) . . ? N7 Mn1 O3 88.63(18) . . ? N10 Mn1 O3 88.84(18) . . ? N9 Mn1 O3 89.27(17) . . ? N8 Mn1 O3 89.13(17) . . ? N1 Mn1 O3 177.98(18) . . ? N3 Cr1 N4 81.5(3) . . ? N3 Cr1 N6 161.1(3) . . ? N4 Cr1 N6 79.7(3) . . ? N3 Cr1 C2 92.8(3) . . ? N4 Cr1 C2 93.3(3) . . ? N6 Cr1 C2 86.5(3) . . ? N3 Cr1 N5 80.2(3) . . ? N4 Cr1 N5 161.6(3) . . ? N6 Cr1 N5 118.7(3) . . ? C2 Cr1 N5 89.0(3) . . ? N3 Cr1 C1 91.1(2) . . ? N4 Cr1 C1 93.9(2) . . ? N6 Cr1 C1 92.0(2) . . ? C2 Cr1 C1 172.2(3) . . ? N5 Cr1 C1 85.0(2) . . ? C65 O3 Mn1 129.4(5) . . ? C65 O3 H3A 103.3 . . ? Mn1 O3 H3A 126.7 . . ? H4A O4 H4A 0.0 . . ? H4A O4 H4B 119.1 . . ? H4A O4 H4B 119.1 . . ? H5B O5 H5A 116.3 . . ? C1 N1 Mn1 163.4(5) . . ? C20 N3 C3 126.2(8) . . ? C20 N3 Cr1 118.1(6) . . ? C3 N3 Cr1 115.6(6) . . ? C14 N4 C4 127.9(8) . . ? C14 N4 Cr1 117.5(6) . . ? C4 N4 Cr1 114.4(6) . . ? C19 N5 C15 120.4(7) . . ? C19 N5 Cr1 128.1(6) . . ? C15 N5 Cr1 111.0(6) . . ? C9 N6 C13 117.7(8) . . ? C9 N6 Cr1 113.7(6) . . ? C13 N6 Cr1 128.3(6) . . ? C21 N7 C24 106.3(5) . . ? C21 N7 Mn1 126.3(4) . . ? C24 N7 Mn1 127.0(4) . . ? C54 N8 C57 106.0(5) . . ? C54 N8 Mn1 127.2(4) . . ? C57 N8 Mn1 126.8(4) . . ? C43 N9 C46 107.0(5) . . ? C43 N9 Mn1 126.3(4) . . ? C46 N9 Mn1 126.4(4) . . ? C35 N10 C32 104.8(5) . . ? C35 N10 Mn1 127.9(4) . . ? C32 N10 Mn1 127.3(4) . . ? N1 C1 Cr1 173.7(5) . . ? N2 C2 Cr1 173.0(10) . . ? C8 C3 C4 120.5(10) . . ? C8 C3 N3 126.7(10) . . ? C4 C3 N3 112.7(9) . . ? C3 C4 C5 121.7(9) . . ? C3 C4 N4 115.2(9) . . ? C5 C4 N4 123.0(10) . . ? C6 C5 C4 117.3(11) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? C5 C6 C7 120.3(12) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 123.2(12) . . ? C6 C7 H7 118.4 . . ? C8 C7 H7 118.4 . . ? C7 C8 C3 116.8(11) . . ? C7 C8 H8 121.6 . . ? C3 C8 H8 121.6 . . ? N6 C9 C10 123.0(10) . . ? N6 C9 C14 115.4(8) . . ? C10 C9 C14 121.6(9) . . ? C11 C10 C9 118.6(10) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C12 C11 C10 120.1(10) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.0(10) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N6 C13 C12 121.5(8) . . ? N6 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? O2 C14 N4 127.2(10) . . ? O2 C14 C9 119.9(9) . . ? N4 C14 C9 112.9(8) . . ? N5 C15 C16 119.3(9) . . ? N5 C15 C20 116.7(7) . . ? C16 C15 C20 123.9(9) . . ? C17 C16 C15 122.2(10) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C18 119.0(10) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 118.9(11) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? N5 C19 C18 120.2(9) . . ? N5 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? O1 C20 N3 128.2(10) . . ? O1 C20 C15 119.4(9) . . ? N3 C20 C15 112.5(8) . . ? N7 C21 C58 127.3(6) . . ? N7 C21 C22 109.6(6) . . ? C58 C21 C22 123.1(6) . . ? C23 C22 C21 105.8(6) . . ? C23 C22 H22 127.1 . . ? C21 C22 H22 127.1 . . ? C22 C23 C24 108.7(6) . . ? C22 C23 H23 125.7 . . ? C24 C23 H23 125.7 . . ? N7 C24 C25 126.1(5) . . ? N7 C24 C23 109.6(6) . . ? C25 C24 C23 124.1(6) . . ? C24 C25 C32 124.5(6) . . ? C24 C25 C26 118.4(5) . . ? C32 C25 C26 117.1(6) . . ? C27 C26 C31 118.3(6) . . ? C27 C26 C25 119.3(6) . . ? C31 C26 C25 122.4(7) . . ? C26 C27 C28 120.7(7) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 118.9(7) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 121.3(7) . . ? C28 C29 Cl2 119.2(7) . . ? C30 C29 Cl2 119.5(6) . . ? C31 C30 C29 118.2(7) . . ? C31 C30 H30 120.9 . . ? C29 C30 H30 120.9 . . ? C30 C31 C26 122.5(7) . . ? C30 C31 H31 118.7 . . ? C26 C31 H31 118.7 . . ? C25 C32 N10 124.6(6) . . ? C25 C32 C33 126.1(6) . . ? N10 C32 C33 109.2(5) . . ? C34 C33 C32 108.2(6) . . ? C34 C33 H33 125.9 . . ? C32 C33 H33 125.9 . . ? C33 C34 C35 107.4(6) . . ? C33 C34 H34 126.3 . . ? C35 C34 H34 126.3 . . ? C36 C35 N10 124.7(6) . . ? C36 C35 C34 125.0(6) . . ? N10 C35 C34 110.3(5) . . ? C35 C36 C43 124.5(6) . . ? C35 C36 C37 118.1(6) . . ? C43 C36 C37 117.3(5) . . ? C38 C37 C42 117.1(6) . . ? C38 C37 C36 121.1(6) . . ? C42 C37 C36 121.8(6) . . ? C37 C38 C39 123.0(6) . . ? C37 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C40 C39 C38 118.5(7) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C40 C41 119.8(6) . . ? C39 C40 Cl4 120.0(6) . . ? C41 C40 Cl4 120.2(6) . . ? C42 C41 C40 120.4(7) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C37 121.2(7) . . ? C41 C42 H42 119.4 . . ? C37 C42 H42 119.4 . . ? N9 C43 C36 126.4(5) . . ? N9 C43 C44 108.6(5) . . ? C36 C43 C44 125.0(6) . . ? C45 C44 C43 107.6(6) . . ? C45 C44 H44 126.2 . . ? C43 C44 H44 126.2 . . ? C44 C45 C46 108.4(6) . . ? C44 C45 H45 125.8 . . ? C46 C45 H45 125.8 . . ? N9 C46 C47 126.3(5) . . ? N9 C46 C45 108.4(6) . . ? C47 C46 C45 125.2(6) . . ? C46 C47 C54 124.0(5) . . ? C46 C47 C48 116.7(5) . . ? C54 C47 C48 119.2(5) . . ? C49 C48 C53 117.0(6) . . ? C49 C48 C47 120.1(6) . . ? C53 C48 C47 122.9(6) . . ? C48 C49 C50 123.4(6) . . ? C48 C49 H49 118.3 . . ? C50 C49 H49 118.3 . . ? C51 C50 C49 117.4(6) . . ? C51 C50 H50 121.3 . . ? C49 C50 H50 121.3 . . ? C52 C51 C50 121.1(6) . . ? C52 C51 Cl1 120.5(6) . . ? C50 C51 Cl1 118.3(5) . . ? C51 C52 C53 119.0(7) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C48 C53 C52 122.0(7) . . ? C48 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? N8 C54 C47 125.9(6) . . ? N8 C54 C55 109.5(5) . . ? C47 C54 C55 124.7(6) . . ? C56 C55 C54 107.9(5) . . ? C56 C55 H55 126.1 . . ? C54 C55 H55 126.1 . . ? C55 C56 C57 106.9(6) . . ? C55 C56 H56 126.5 . . ? C57 C56 H56 126.5 . . ? N8 C57 C58 126.5(6) . . ? N8 C57 C56 109.8(5) . . ? C58 C57 C56 123.7(6) . . ? C57 C58 C21 122.6(6) . . ? C57 C58 C59 119.6(6) . . ? C21 C58 C59 117.8(5) . . ? C60 C59 C64 118.1(7) . . ? C60 C59 C58 121.9(7) . . ? C64 C59 C58 119.9(6) . . ? C59 C60 C61 120.9(8) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C62 C61 C60 119.2(8) . . ? C62 C61 H61 120.4 . . ? C60 C61 H61 120.4 . . ? C61 C62 C63 122.4(8) . . ? C61 C62 Cl3 120.4(8) . . ? C63 C62 Cl3 117.3(9) . . ? C62 C63 C64 117.2(9) . . ? C62 C63 H63 121.4 . . ? C64 C63 H63 121.4 . . ? C59 C64 C63 122.2(8) . . ? C59 C64 H64 118.9 . . ? C63 C64 H64 118.9 . . ? O3 C65 H65A 109.5 . . ? O3 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? O3 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.173 0.250 646 137 ' ' 2 0.146 0.231 0.603 40 8 ' ' 3 0.354 0.731 0.897 40 8 ' ' 4 0.750 0.315 0.750 646 136 ' ' 5 0.646 0.269 0.103 40 8 ' ' 6 0.854 0.769 0.397 40 7 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.689 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.076