data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H56 Cr Mn3 N14 O8' _chemical_formula_weight 1318.01 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 14.063(3) _cell_length_b 15.106(3) _cell_length_c 15.981(3) _cell_angle_alpha 76.91(3) _cell_angle_beta 80.10(3) _cell_angle_gamma 66.84(3) _cell_volume 3027.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8316 _cell_measurement_theta_min 1.805 _cell_measurement_theta_max 27.487 _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1354 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8480 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22372 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10619 _reflns_number_gt 8214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'crystalclear' _computing_data_reduction 'crystalclear' _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^)+(0.0831P)^2^+2.2817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10619 _refine_ls_number_parameters 799 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.005 _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 Cr1 Cr 0.0000 0.5000 0.5000 0.0246(2) Uani 1 2 d S . . Cr2 Cr 0.0000 1.0000 0.0000 0.0247(2) Uani 1 2 d S . . Mn1 Mn 0.35515(6) 0.52212(5) 0.51069(4) 0.0328(2) Uani 1 1 d . . . Mn2 Mn -0.02405(5) 0.66308(4) 0.17488(4) 0.02234(17) Uani 1 1 d . . . Mn3 Mn 0.21250(5) 0.14036(4) 0.42488(4) 0.02062(17) Uani 1 1 d . . . O1 O 0.3152(2) 0.6200(2) 0.57738(19) 0.0329(7) Uani 1 1 d . . . O2 O 0.4166(4) 0.5895(3) 0.4196(2) 0.0609(12) Uani 1 1 d . . . O3 O 0.3453(2) 0.1246(2) 0.44809(18) 0.0263(6) Uani 1 1 d . . . O4 O 0.1874(2) 0.05490(19) 0.52474(17) 0.0236(6) Uani 1 1 d . . . O5 O -0.1664(2) 0.6958(2) 0.16561(17) 0.0241(6) Uani 1 1 d . . . O6 O 0.0219(2) 0.5673(2) 0.10483(19) 0.0322(7) Uani 1 1 d . . . O7 O 0.2923(2) 0.0115(2) 0.35423(19) 0.0291(7) Uani 1 1 d . . . H7 H 0.2917 0.0233 0.2946 0.035 Uiso 1 1 calc R . . N1 N 0.2085(3) 0.5495(3) 0.4624(2) 0.0331(9) Uani 1 1 d . . . N2 N -0.0268(3) 0.5446(3) 0.2976(2) 0.0301(8) Uani 1 1 d . . . N3 N 0.1353(3) 0.2739(3) 0.4888(2) 0.0268(8) Uani 1 1 d . . . N4 N -0.0134(3) 0.7868(3) 0.0702(2) 0.0331(9) Uani 1 1 d . . . N5 N 0.1807(3) 0.9429(4) 0.1246(3) 0.0460(11) Uani 1 1 d . . . N6 N -0.1716(3) 1.0752(3) 0.1552(3) 0.0471(11) Uani 1 1 d . . . N7 N 0.3211(3) 0.4311(3) 0.6095(2) 0.0267(8) Uani 1 1 d . . . N8 N 0.4293(3) 0.4009(3) 0.4618(2) 0.0304(8) Uani 1 1 d . . . N9 N -0.0560(3) 0.7510(2) 0.2602(2) 0.0244(8) Uani 1 1 d . . . N10 N 0.1215(3) 0.6391(2) 0.1945(2) 0.0277(8) Uani 1 1 d . . . N11 N 0.2228(3) 0.2274(2) 0.3128(2) 0.0228(7) Uani 1 1 d . . . N12 N 0.0748(3) 0.1671(2) 0.3864(2) 0.0232(7) Uani 1 1 d . . . C1 C 0.1340(4) 0.5328(3) 0.4721(3) 0.0286(10) Uani 1 1 d . . . C2 C -0.0184(3) 0.5246(3) 0.3703(3) 0.0263(9) Uani 1 1 d . . . C3 C 0.0884(3) 0.3540(3) 0.4951(3) 0.0257(9) Uani 1 1 d . . . C4 C -0.0093(3) 0.8628(3) 0.0421(3) 0.0276(10) Uani 1 1 d . . . C5 C 0.1164(4) 0.9623(3) 0.0809(3) 0.0318(10) Uani 1 1 d . . . C6 C -0.1101(4) 1.0476(3) 0.1001(3) 0.0312(10) Uani 1 1 d . . . C7 C 0.2701(3) 0.6229(3) 0.6570(3) 0.0279(10) Uani 1 1 d . . . C8 C 0.2446(3) 0.7071(3) 0.6924(3) 0.0335(11) Uani 1 1 d . . . H8 H 0.2590 0.7600 0.6587 0.040 Uiso 1 1 calc R . . C9 C 0.1994(3) 0.7143(3) 0.7746(3) 0.0342(11) Uani 1 1 d . . . H9 H 0.1856 0.7707 0.7963 0.041 Uiso 1 1 calc R . . C10 C 0.1738(4) 0.6370(4) 0.8263(3) 0.0398(12) Uani 1 1 d . . . H10 H 0.1412 0.6425 0.8817 0.048 Uiso 1 1 calc R . . C11 C 0.1975(4) 0.5531(4) 0.7940(3) 0.0352(11) Uani 1 1 d . . . H11 H 0.1809 0.5016 0.8282 0.042 Uiso 1 1 calc R . . C12 C 0.2459(3) 0.5435(3) 0.7108(3) 0.0293(10) Uani 1 1 d . . . C13 C 0.2738(3) 0.4522(3) 0.6829(3) 0.0280(10) Uani 1 1 d . . . H13 H 0.2561 0.4036 0.7214 0.034 Uiso 1 1 calc R . . C14 C 0.3418(3) 0.3343(3) 0.5886(3) 0.0289(10) Uani 1 1 d . . . H14A H 0.2838 0.3361 0.5622 0.035 Uiso 1 1 calc R . . H14B H 0.3522 0.2850 0.6406 0.035 Uiso 1 1 calc R . . C15 C 0.4401(4) 0.3107(3) 0.5258(3) 0.0363(11) Uani 1 1 d . . . H15A H 0.5012 0.2910 0.5563 0.044 Uiso 1 1 calc R . . H15B H 0.4468 0.2579 0.4974 0.044 Uiso 1 1 calc R . . C16 C 0.4675(3) 0.3962(4) 0.3831(3) 0.0345(11) Uani 1 1 d . . . H16 H 0.4966 0.3350 0.3668 0.041 Uiso 1 1 calc R . . C17 C 0.4681(3) 0.4796(4) 0.3187(3) 0.0328(11) Uani 1 1 d . . . C18 C 0.5010(4) 0.4667(4) 0.2322(3) 0.0457(13) Uani 1 1 d . . . H18 H 0.5209 0.4048 0.2187 0.055 Uiso 1 1 calc R . . C19 C 0.5043(4) 0.5421(4) 0.1682(3) 0.0481(14) Uani 1 1 d . . . H19 H 0.5248 0.5322 0.1114 0.058 Uiso 1 1 calc R . . C20 C 0.4768(4) 0.6334(4) 0.1884(3) 0.0436(13) Uani 1 1 d . . . H20 H 0.4788 0.6854 0.1448 0.052 Uiso 1 1 calc R . . C21 C 0.4462(4) 0.6491(4) 0.2726(3) 0.0461(13) Uani 1 1 d . . . H21 H 0.4283 0.7112 0.2850 0.055 Uiso 1 1 calc R . . C22 C 0.4422(4) 0.5725(4) 0.3389(3) 0.0412(12) Uani 1 1 d . . . C23 C -0.2475(3) 0.7680(3) 0.1945(3) 0.0267(9) Uani 1 1 d . . . C24 C -0.3463(3) 0.7857(3) 0.1715(3) 0.0320(10) Uani 1 1 d . . . H24 H -0.3527 0.7486 0.1351 0.038 Uiso 1 1 calc R . . C25 C -0.4344(4) 0.8575(3) 0.2023(3) 0.0407(12) Uani 1 1 d . . . H25 H -0.4989 0.8676 0.1862 0.049 Uiso 1 1 calc R . . C26 C -0.4279(4) 0.9142(4) 0.2564(4) 0.0450(13) Uani 1 1 d . . . H26 H -0.4873 0.9630 0.2755 0.054 Uiso 1 1 calc R . . C27 C -0.3318(4) 0.8972(3) 0.2816(4) 0.0422(12) Uani 1 1 d . . . H27 H -0.3270 0.9336 0.3194 0.051 Uiso 1 1 calc R . . C28 C -0.2415(3) 0.8255(3) 0.2506(3) 0.0311(10) Uani 1 1 d . . . C29 C -0.1458(4) 0.8116(3) 0.2827(3) 0.0318(10) Uani 1 1 d . . . H29 H -0.1496 0.8493 0.3226 0.038 Uiso 1 1 calc R . . C30 C 0.0344(4) 0.7377(3) 0.3042(3) 0.0324(10) Uani 1 1 d . . . H30A H 0.0428 0.6861 0.3543 0.039 Uiso 1 1 calc R . . H30B H 0.0247 0.7977 0.3230 0.039 Uiso 1 1 calc R . . C31 C 0.1291(4) 0.7108(3) 0.2393(3) 0.0366(11) Uani 1 1 d . . . H31A H 0.1307 0.7685 0.1983 0.044 Uiso 1 1 calc R . . H31B H 0.1922 0.6827 0.2686 0.044 Uiso 1 1 calc R . . C32 C 0.2034(4) 0.5717(3) 0.1671(3) 0.0352(11) Uani 1 1 d . . . H32 H 0.2668 0.5670 0.1815 0.042 Uiso 1 1 calc R . . C33 C 0.2061(4) 0.5041(3) 0.1170(3) 0.0353(11) Uani 1 1 d . . . C34 C 0.3057(4) 0.4359(4) 0.0908(3) 0.0469(14) Uani 1 1 d . . . H34 H 0.3653 0.4368 0.1079 0.056 Uiso 1 1 calc R . . C35 C 0.3147(5) 0.3697(4) 0.0414(3) 0.0603(18) Uani 1 1 d . . . H35 H 0.3799 0.3268 0.0239 0.072 Uiso 1 1 calc R . . C36 C 0.2252(5) 0.3671(5) 0.0173(3) 0.0638(19) Uani 1 1 d . . . H36 H 0.2307 0.3206 -0.0146 0.077 Uiso 1 1 calc R . . C37 C 0.1290(5) 0.4325(4) 0.0402(3) 0.0513(15) Uani 1 1 d . . . H37 H 0.0704 0.4295 0.0234 0.062 Uiso 1 1 calc R . . C38 C 0.1168(4) 0.5040(3) 0.0884(3) 0.0332(11) Uani 1 1 d . . . C39 C 0.4217(3) 0.1379(3) 0.3919(3) 0.0247(9) Uani 1 1 d . . . C40 C 0.5218(3) 0.0994(3) 0.4175(3) 0.0289(10) Uani 1 1 d . . . H40 H 0.5333 0.0644 0.4731 0.035 Uiso 1 1 calc R . . C41 C 0.6048(4) 0.1117(3) 0.3626(3) 0.0349(11) Uani 1 1 d . . . H41 H 0.6708 0.0854 0.3819 0.042 Uiso 1 1 calc R . . C42 C 0.5905(4) 0.1634(4) 0.2785(3) 0.0389(12) Uani 1 1 d . . . H42 H 0.6466 0.1708 0.2415 0.047 Uiso 1 1 calc R . . C43 C 0.4930(4) 0.2029(3) 0.2509(3) 0.0346(11) Uani 1 1 d . . . H43 H 0.4832 0.2374 0.1950 0.042 Uiso 1 1 calc R . . C44 C 0.4068(3) 0.1917(3) 0.3065(3) 0.0273(9) Uani 1 1 d . . . C45 C 0.3064(3) 0.2375(3) 0.2733(3) 0.0280(10) Uani 1 1 d . . . H45 H 0.3019 0.2772 0.2192 0.034 Uiso 1 1 calc R . . C46 C 0.1232(3) 0.2818(3) 0.2736(3) 0.0308(10) Uani 1 1 d . . . H46A H 0.1355 0.3003 0.2117 0.037 Uiso 1 1 calc R . . H46B H 0.0839 0.3405 0.2979 0.037 Uiso 1 1 calc R . . C47 C 0.0643(3) 0.2123(3) 0.2942(3) 0.0298(10) Uani 1 1 d . . . H47A H -0.0083 0.2479 0.2844 0.036 Uiso 1 1 calc R . . H47B H 0.0938 0.1625 0.2580 0.036 Uiso 1 1 calc R . . C48 C -0.0028(3) 0.1551(3) 0.4354(3) 0.0267(9) Uani 1 1 d . . . H48 H -0.0661 0.1782 0.4120 0.032 Uiso 1 1 calc R . . C49 C 0.0016(3) 0.1080(3) 0.5250(3) 0.0247(9) Uani 1 1 d . . . C50 C -0.0931(4) 0.1093(4) 0.5714(3) 0.0338(11) Uani 1 1 d . . . H50 H -0.1544 0.1421 0.5448 0.041 Uiso 1 1 calc R . . C51 C -0.0963(4) 0.0618(4) 0.6568(3) 0.0353(11) Uani 1 1 d . . . H51 H -0.1593 0.0651 0.6884 0.042 Uiso 1 1 calc R . . C52 C -0.0032(4) 0.0095(3) 0.6937(3) 0.0299(10) Uani 1 1 d . . . H52 H -0.0043 -0.0243 0.7501 0.036 Uiso 1 1 calc R . . C53 C 0.0913(3) 0.0062(3) 0.6488(3) 0.0247(9) Uani 1 1 d . . . H53 H 0.1524 -0.0299 0.6750 0.030 Uiso 1 1 calc R . . C54 C 0.0952(3) 0.0573(3) 0.5637(3) 0.0228(9) Uani 1 1 d . . . C55 C 0.3431(4) -0.0861(3) 0.3962(3) 0.0347(11) Uani 1 1 d . . . H55A H 0.4159 -0.0993 0.3951 0.052 Uiso 1 1 calc R . . H55B H 0.3341 -0.1307 0.3668 0.052 Uiso 1 1 calc R . . H55C H 0.3137 -0.0942 0.4549 0.052 Uiso 1 1 calc R . . N13 N 0.4376(6) 0.6501(7) 0.9353(5) 0.109(2) Uani 1 1 d U . . C56 C 0.3577(5) 0.6846(5) 0.9698(4) 0.0585(16) Uani 1 1 d . . . C57 C 0.2644(7) 0.7319(6) 1.0096(6) 0.111(3) Uani 1 1 d . . . H57A H 0.2364 0.7981 0.9796 0.166 Uiso 1 1 calc R . . H57B H 0.2724 0.7321 1.0680 0.166 Uiso 1 1 calc R . . H57C H 0.2179 0.6993 1.0095 0.166 Uiso 1 1 calc R . . N14 N 0.4863(11) 0.8398(6) 1.0172(8) 0.236(8) Uani 1 1 d . . . C58 C 0.4307(8) 0.8973(5) 0.9802(6) 0.112(4) Uani 1 1 d D . . C59 C 0.3440(5) 0.9684(5) 0.9378(4) 0.077(2) Uani 1 1 d D . . H59A H 0.3171 0.9370 0.9070 0.116 Uiso 1 1 d R . . H59B H 0.3653 1.0166 0.8981 0.116 Uiso 1 1 d R . . H59C H 0.2910 0.9993 0.9799 0.116 Uiso 1 1 d R . . O8 O 0.3030(3) 0.0113(4) 0.1895(2) 0.0466(13) Uani 0.831(7) 1 d PU A 1 C60 C 0.3337(8) 0.0812(7) 0.1229(6) 0.088(3) Uani 0.831(7) 1 d PU A 1 O8' O 0.2510(13) 0.1677(12) 0.1108(10) 0.023(4) Uani 0.169(7) 1 d PU A 2 C60' C 0.1648(19) 0.1901(17) 0.0606(15) 0.025(6) Uani 0.169(7) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0348(6) 0.0169(5) 0.0212(5) -0.0020(4) -0.0056(4) -0.0081(4) Cr2 0.0267(5) 0.0303(5) 0.0184(5) -0.0027(4) 0.0015(4) -0.0142(4) Mn1 0.0495(5) 0.0354(4) 0.0266(4) -0.0077(3) 0.0036(3) -0.0310(4) Mn2 0.0255(4) 0.0212(3) 0.0209(3) -0.0041(3) -0.0018(3) -0.0092(3) Mn3 0.0200(3) 0.0216(3) 0.0206(3) -0.0035(3) -0.0011(2) -0.0084(3) O1 0.050(2) 0.0344(17) 0.0271(16) -0.0077(14) 0.0010(14) -0.0291(16) O2 0.117(4) 0.072(3) 0.0303(19) -0.0159(18) 0.018(2) -0.081(3) O3 0.0243(16) 0.0296(15) 0.0262(15) -0.0058(13) -0.0030(12) -0.0104(13) O4 0.0220(15) 0.0214(14) 0.0242(15) -0.0020(12) -0.0008(12) -0.0062(12) O5 0.0267(16) 0.0245(14) 0.0235(15) -0.0079(12) -0.0003(12) -0.0109(13) O6 0.0349(18) 0.0321(16) 0.0277(16) -0.0123(14) -0.0056(13) -0.0055(14) O7 0.0336(17) 0.0289(16) 0.0244(15) -0.0095(13) 0.0006(13) -0.0098(14) N1 0.038(2) 0.027(2) 0.035(2) -0.0009(17) -0.0107(18) -0.0133(18) N2 0.042(2) 0.0265(19) 0.027(2) -0.0022(16) -0.0086(17) -0.0174(18) N3 0.034(2) 0.0227(19) 0.0249(19) -0.0056(16) -0.0052(15) -0.0100(17) N4 0.035(2) 0.036(2) 0.029(2) 0.0026(18) -0.0015(16) -0.0177(18) N5 0.037(2) 0.074(3) 0.026(2) -0.007(2) -0.0011(19) -0.021(2) N6 0.047(3) 0.067(3) 0.036(2) -0.024(2) 0.012(2) -0.029(2) N7 0.029(2) 0.0260(18) 0.029(2) -0.0047(16) -0.0001(15) -0.0159(16) N8 0.027(2) 0.037(2) 0.029(2) -0.0031(17) -0.0056(16) -0.0142(17) N9 0.029(2) 0.0193(17) 0.0257(19) -0.0028(15) -0.0020(15) -0.0112(16) N10 0.028(2) 0.0230(18) 0.030(2) -0.0004(16) -0.0041(16) -0.0093(16) N11 0.0209(18) 0.0275(18) 0.0224(18) -0.0034(15) -0.0031(14) -0.0116(15) N12 0.0250(19) 0.0220(17) 0.0202(17) -0.0041(15) -0.0019(14) -0.0061(15) C1 0.044(3) 0.018(2) 0.022(2) -0.0027(18) -0.012(2) -0.006(2) C2 0.034(2) 0.018(2) 0.029(3) -0.0019(18) -0.0061(19) -0.0119(19) C3 0.035(2) 0.026(2) 0.021(2) -0.0008(18) -0.0042(18) -0.016(2) C4 0.025(2) 0.037(3) 0.017(2) 0.000(2) 0.0008(17) -0.011(2) C5 0.030(3) 0.039(3) 0.024(2) -0.005(2) 0.007(2) -0.014(2) C6 0.039(3) 0.037(2) 0.025(2) -0.006(2) -0.003(2) -0.021(2) C7 0.030(2) 0.028(2) 0.030(2) -0.0041(19) -0.0062(19) -0.015(2) C8 0.035(3) 0.030(2) 0.041(3) -0.008(2) -0.007(2) -0.015(2) C9 0.029(2) 0.034(2) 0.044(3) -0.016(2) -0.009(2) -0.008(2) C10 0.044(3) 0.047(3) 0.031(3) -0.016(2) -0.002(2) -0.015(2) C11 0.036(3) 0.041(3) 0.031(2) -0.006(2) -0.003(2) -0.017(2) C12 0.035(3) 0.030(2) 0.026(2) -0.0019(19) -0.0075(19) -0.016(2) C13 0.031(2) 0.029(2) 0.024(2) 0.0028(19) -0.0059(18) -0.014(2) C14 0.034(3) 0.024(2) 0.031(2) -0.0036(19) -0.0049(19) -0.014(2) C15 0.038(3) 0.035(3) 0.036(3) -0.008(2) -0.008(2) -0.011(2) C16 0.029(2) 0.043(3) 0.029(2) -0.009(2) -0.0062(19) -0.009(2) C17 0.025(2) 0.049(3) 0.026(2) -0.009(2) -0.0013(18) -0.015(2) C18 0.045(3) 0.052(3) 0.035(3) -0.009(3) -0.002(2) -0.013(3) C19 0.056(3) 0.065(4) 0.025(3) -0.009(3) -0.002(2) -0.025(3) C20 0.049(3) 0.065(4) 0.027(3) -0.001(2) -0.003(2) -0.036(3) C21 0.064(4) 0.059(3) 0.035(3) -0.007(3) 0.004(2) -0.047(3) C22 0.047(3) 0.064(3) 0.032(3) -0.012(2) 0.002(2) -0.041(3) C23 0.031(2) 0.023(2) 0.027(2) -0.0022(18) 0.0038(18) -0.0138(19) C24 0.030(2) 0.032(2) 0.037(3) -0.007(2) -0.002(2) -0.015(2) C25 0.027(3) 0.034(3) 0.057(3) -0.004(2) 0.001(2) -0.011(2) C26 0.030(3) 0.030(2) 0.068(4) -0.016(3) 0.012(2) -0.007(2) C27 0.041(3) 0.032(2) 0.057(3) -0.021(2) 0.014(2) -0.017(2) C28 0.033(2) 0.020(2) 0.037(3) -0.0053(19) 0.004(2) -0.0089(19) C29 0.041(3) 0.025(2) 0.037(3) -0.010(2) -0.001(2) -0.019(2) C30 0.040(3) 0.029(2) 0.035(3) -0.006(2) -0.009(2) -0.018(2) C31 0.036(3) 0.033(2) 0.047(3) -0.001(2) -0.014(2) -0.018(2) C32 0.030(3) 0.032(2) 0.040(3) 0.006(2) -0.004(2) -0.013(2) C33 0.034(3) 0.029(2) 0.028(2) 0.002(2) 0.006(2) -0.004(2) C34 0.036(3) 0.042(3) 0.040(3) 0.006(3) 0.007(2) -0.002(2) C35 0.066(4) 0.046(3) 0.029(3) -0.008(3) 0.013(3) 0.016(3) C36 0.075(4) 0.058(4) 0.032(3) -0.022(3) -0.013(3) 0.014(3) C37 0.060(4) 0.045(3) 0.032(3) -0.021(2) -0.015(3) 0.009(3) C38 0.038(3) 0.032(2) 0.019(2) 0.0011(19) -0.0017(19) -0.005(2) C39 0.025(2) 0.020(2) 0.032(2) -0.0102(18) -0.0004(18) -0.0092(18) C40 0.025(2) 0.025(2) 0.039(3) -0.007(2) -0.0056(19) -0.0094(19) C41 0.026(2) 0.029(2) 0.054(3) -0.016(2) -0.002(2) -0.012(2) C42 0.030(3) 0.043(3) 0.055(3) -0.023(3) 0.009(2) -0.022(2) C43 0.033(3) 0.038(3) 0.038(3) -0.011(2) 0.004(2) -0.019(2) C44 0.022(2) 0.029(2) 0.034(2) -0.009(2) 0.0010(18) -0.0132(19) C45 0.037(3) 0.029(2) 0.021(2) -0.0031(18) -0.0003(18) -0.018(2) C46 0.031(2) 0.033(2) 0.026(2) 0.002(2) -0.0057(19) -0.012(2) C47 0.029(2) 0.038(3) 0.022(2) -0.003(2) -0.0052(18) -0.012(2) C48 0.027(2) 0.030(2) 0.027(2) -0.0089(19) -0.0043(18) -0.012(2) C49 0.025(2) 0.028(2) 0.025(2) -0.0073(18) -0.0022(17) -0.0118(19) C50 0.029(2) 0.053(3) 0.027(2) -0.013(2) 0.0063(18) -0.023(2) C51 0.039(3) 0.052(3) 0.028(2) -0.013(2) 0.007(2) -0.032(2) C52 0.042(3) 0.035(2) 0.022(2) -0.0044(19) 0.0012(19) -0.026(2) C53 0.031(2) 0.020(2) 0.024(2) -0.0086(18) 0.0005(18) -0.0099(19) C54 0.027(2) 0.021(2) 0.025(2) -0.0122(18) 0.0068(17) -0.0130(18) C55 0.033(3) 0.031(2) 0.039(3) -0.013(2) -0.002(2) -0.008(2) N13 0.094(5) 0.159(6) 0.094(5) -0.051(5) 0.013(4) -0.059(5) C56 0.047(4) 0.065(4) 0.060(4) -0.027(3) 0.003(3) -0.013(3) C57 0.102(7) 0.079(5) 0.093(6) 0.023(5) 0.029(5) -0.007(5) N14 0.350(17) 0.077(6) 0.241(13) -0.073(7) -0.210(13) 0.062(8) C58 0.169(9) 0.047(4) 0.114(7) -0.032(4) -0.095(7) 0.011(5) C59 0.067(4) 0.109(6) 0.067(4) -0.011(4) 0.020(3) -0.058(4) O8 0.043(2) 0.088(3) 0.025(2) -0.021(2) 0.0005(17) -0.036(2) C60 0.115(6) 0.088(5) 0.076(5) -0.025(4) 0.006(5) -0.055(5) O8' 0.030(7) 0.034(7) 0.014(6) -0.005(5) -0.012(5) -0.017(6) C60' 0.029(9) 0.024(8) 0.020(8) 0.000(7) -0.002(7) -0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C2 2.064(4) . ? Cr1 C2 2.065(4) 2_566 ? Cr1 C3 2.075(4) . ? Cr1 C3 2.075(4) 2_566 ? Cr1 C1 2.083(5) . ? Cr1 C1 2.083(5) 2_566 ? Cr2 C6 2.065(5) 2_575 ? Cr2 C6 2.065(5) . ? Cr2 C4 2.078(5) . ? Cr2 C4 2.078(5) 2_575 ? Cr2 C5 2.083(5) . ? Cr2 C5 2.083(5) 2_575 ? Mn1 O2 1.867(3) . ? Mn1 O1 1.868(3) . ? Mn1 N7 1.973(3) . ? Mn1 N8 1.979(4) . ? Mn1 N1 2.180(4) . ? Mn2 O6 1.874(3) . ? Mn2 O5 1.888(3) . ? Mn2 N9 1.991(4) . ? Mn2 N10 2.001(4) . ? Mn2 N4 2.243(4) . ? Mn2 N2 2.343(4) . ? Mn3 O3 1.879(3) . ? Mn3 O4 1.889(3) . ? Mn3 N11 1.988(3) . ? Mn3 N12 1.994(3) . ? Mn3 N3 2.263(4) . ? Mn3 O7 2.272(3) . ? O1 C7 1.323(5) . ? O2 C22 1.333(6) . ? O3 C39 1.325(5) . ? O4 C54 1.329(5) . ? O5 C23 1.332(5) . ? O6 C38 1.324(5) . ? O7 C55 1.423(5) . ? O7 H7 0.9300 . ? N1 C1 1.150(6) . ? N2 C2 1.147(5) . ? N3 C3 1.146(5) . ? N4 C4 1.155(6) . ? N5 C5 1.142(6) . ? N6 C6 1.148(6) . ? N7 C13 1.286(6) . ? N7 C14 1.478(5) . ? N8 C16 1.286(6) . ? N8 C15 1.479(6) . ? N9 C29 1.283(6) . ? N9 C30 1.482(5) . ? N10 C32 1.289(6) . ? N10 C31 1.473(6) . ? N11 C45 1.284(5) . ? N11 C46 1.481(5) . ? N12 C48 1.278(5) . ? N12 C47 1.483(5) . ? C7 C8 1.402(6) . ? C7 C12 1.429(6) . ? C8 C9 1.365(7) . ? C8 H8 0.9300 . ? C9 C10 1.403(7) . ? C9 H9 0.9300 . ? C10 C11 1.376(7) . ? C10 H10 0.9300 . ? C11 C12 1.396(6) . ? C11 H11 0.9300 . ? C12 C13 1.431(6) . ? C13 H13 0.9300 . ? C14 C15 1.530(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.437(7) . ? C16 H16 0.9300 . ? C17 C22 1.403(7) . ? C17 C18 1.411(7) . ? C18 C19 1.358(7) . ? C18 H18 0.9300 . ? C19 C20 1.377(8) . ? C19 H19 0.9300 . ? C20 C21 1.385(7) . ? C20 H20 0.9300 . ? C21 C22 1.393(7) . ? C21 H21 0.9300 . ? C23 C24 1.405(6) . ? C23 C28 1.416(6) . ? C24 C25 1.389(7) . ? C24 H24 0.9300 . ? C25 C26 1.383(7) . ? C25 H25 0.9300 . ? C26 C27 1.388(7) . ? C26 H26 0.9300 . ? C27 C28 1.405(6) . ? C27 H27 0.9300 . ? C28 C29 1.442(6) . ? C29 H29 0.9300 . ? C30 C31 1.518(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.420(7) . ? C32 H32 0.9300 . ? C33 C38 1.409(7) . ? C33 C34 1.434(7) . ? C34 C35 1.366(8) . ? C34 H34 0.9300 . ? C35 C36 1.396(9) . ? C35 H35 0.9300 . ? C36 C37 1.372(8) . ? C36 H36 0.9300 . ? C37 C38 1.404(7) . ? C37 H37 0.9300 . ? C39 C40 1.391(6) . ? C39 C44 1.424(6) . ? C40 C41 1.382(6) . ? C40 H40 0.9300 . ? C41 C42 1.397(7) . ? C41 H41 0.9300 . ? C42 C43 1.369(7) . ? C42 H42 0.9300 . ? C43 C44 1.418(6) . ? C43 H43 0.9300 . ? C44 C45 1.442(6) . ? C45 H45 0.9300 . ? C46 C47 1.526(6) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.447(6) . ? C48 H48 0.9300 . ? C49 C50 1.404(6) . ? C49 C54 1.406(6) . ? C50 C51 1.393(6) . ? C50 H50 0.9300 . ? C51 C52 1.387(6) . ? C51 H51 0.9300 . ? C52 C53 1.386(6) . ? C52 H52 0.9300 . ? C53 C54 1.406(6) . ? C53 H53 0.9300 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? N13 C56 1.138(9) . ? C56 C57 1.349(9) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? N14 C58 1.053(9) . ? C58 C59 1.423(7) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? O8 C60 1.458(10) . ? O8' C60' 1.45(3) . ? 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 C2 Cr1 C2 179.999(1) . 2_566 ? C2 Cr1 C3 89.76(16) . . ? C2 Cr1 C3 90.24(16) 2_566 . ? C2 Cr1 C3 90.24(16) . 2_566 ? C2 Cr1 C3 89.76(16) 2_566 2_566 ? C3 Cr1 C3 180.0(3) . 2_566 ? C2 Cr1 C1 91.01(16) . . ? C2 Cr1 C1 88.99(16) 2_566 . ? C3 Cr1 C1 90.19(16) . . ? C3 Cr1 C1 89.81(16) 2_566 . ? C2 Cr1 C1 88.99(16) . 2_566 ? C2 Cr1 C1 91.01(16) 2_566 2_566 ? C3 Cr1 C1 89.81(16) . 2_566 ? C3 Cr1 C1 90.19(16) 2_566 2_566 ? C1 Cr1 C1 179.999(1) . 2_566 ? C6 Cr2 C6 179.998(1) 2_575 . ? C6 Cr2 C4 92.09(17) 2_575 . ? C6 Cr2 C4 87.92(17) . . ? C6 Cr2 C4 87.91(17) 2_575 2_575 ? C6 Cr2 C4 92.08(17) . 2_575 ? C4 Cr2 C4 180.0 . 2_575 ? C6 Cr2 C5 90.58(17) 2_575 . ? C6 Cr2 C5 89.42(17) . . ? C4 Cr2 C5 90.00(17) . . ? C4 Cr2 C5 90.00(17) 2_575 . ? C6 Cr2 C5 89.42(17) 2_575 2_575 ? C6 Cr2 C5 90.58(17) . 2_575 ? C4 Cr2 C5 90.00(17) . 2_575 ? C4 Cr2 C5 90.00(17) 2_575 2_575 ? C5 Cr2 C5 180.0 . 2_575 ? O2 Mn1 O1 93.25(15) . . ? O2 Mn1 N7 167.73(18) . . ? O1 Mn1 N7 91.54(14) . . ? O2 Mn1 N8 89.73(16) . . ? O1 Mn1 N8 163.82(15) . . ? N7 Mn1 N8 82.62(15) . . ? O2 Mn1 N1 101.84(17) . . ? O1 Mn1 N1 101.41(15) . . ? N7 Mn1 N1 88.26(14) . . ? N8 Mn1 N1 93.52(15) . . ? O6 Mn2 O5 94.64(13) . . ? O6 Mn2 N9 171.42(13) . . ? O5 Mn2 N9 91.97(14) . . ? O6 Mn2 N10 91.99(15) . . ? O5 Mn2 N10 173.34(14) . . ? N9 Mn2 N10 81.37(15) . . ? O6 Mn2 N4 96.59(14) . . ? O5 Mn2 N4 93.38(13) . . ? N9 Mn2 N4 88.46(14) . . ? N10 Mn2 N4 86.46(14) . . ? O6 Mn2 N2 90.37(13) . . ? O5 Mn2 N2 91.17(13) . . ? N9 Mn2 N2 84.03(13) . . ? N10 Mn2 N2 88.17(14) . . ? N4 Mn2 N2 171.35(14) . . ? O3 Mn3 O4 96.14(12) . . ? O3 Mn3 N11 91.76(13) . . ? O4 Mn3 N11 171.60(13) . . ? O3 Mn3 N12 172.91(13) . . ? O4 Mn3 N12 90.93(13) . . ? N11 Mn3 N12 81.15(13) . . ? O3 Mn3 N3 92.30(13) . . ? O4 Mn3 N3 93.34(13) . . ? N11 Mn3 N3 89.19(14) . . ? N12 Mn3 N3 87.89(14) . . ? O3 Mn3 O7 87.17(12) . . ? O4 Mn3 O7 89.76(12) . . ? N11 Mn3 O7 87.76(13) . . ? N12 Mn3 O7 92.25(13) . . ? N3 Mn3 O7 176.89(11) . . ? C7 O1 Mn1 130.2(3) . . ? C22 O2 Mn1 126.8(3) . . ? C39 O3 Mn3 127.5(3) . . ? C54 O4 Mn3 126.6(3) . . ? C23 O5 Mn2 128.3(3) . . ? C38 O6 Mn2 129.6(3) . . ? C55 O7 Mn3 123.6(3) . . ? C55 O7 H7 118.2 . . ? Mn3 O7 H7 118.2 . . ? C1 N1 Mn1 147.6(3) . . ? C2 N2 Mn2 143.6(3) . . ? C3 N3 Mn3 158.4(3) . . ? C4 N4 Mn2 155.7(4) . . ? C13 N7 C14 119.9(4) . . ? C13 N7 Mn1 126.4(3) . . ? C14 N7 Mn1 113.2(3) . . ? C16 N8 C15 120.5(4) . . ? C16 N8 Mn1 126.0(3) . . ? C15 N8 Mn1 113.5(3) . . ? C29 N9 C30 119.1(4) . . ? C29 N9 Mn2 126.5(3) . . ? C30 N9 Mn2 114.3(3) . . ? C32 N10 C31 121.2(4) . . ? C32 N10 Mn2 125.0(3) . . ? C31 N10 Mn2 113.7(3) . . ? C45 N11 C46 119.8(4) . . ? C45 N11 Mn3 125.7(3) . . ? C46 N11 Mn3 114.5(3) . . ? C48 N12 C47 120.5(4) . . ? C48 N12 Mn3 125.3(3) . . ? C47 N12 Mn3 113.9(3) . . ? N1 C1 Cr1 175.5(4) . . ? N2 C2 Cr1 174.6(4) . . ? N3 C3 Cr1 176.8(4) . . ? N4 C4 Cr2 176.1(4) . . ? N5 C5 Cr2 178.8(4) . . ? N6 C6 Cr2 179.2(4) . . ? O1 C7 C8 119.4(4) . . ? O1 C7 C12 123.5(4) . . ? C8 C7 C12 117.1(4) . . ? C9 C8 C7 122.3(4) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C8 C9 C10 120.3(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.1(5) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 119.8(4) . . ? C11 C12 C13 118.5(4) . . ? C7 C12 C13 121.7(4) . . ? N7 C13 C12 126.0(4) . . ? N7 C13 H13 117.0 . . ? C12 C13 H13 117.0 . . ? N7 C14 C15 106.8(3) . . ? N7 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? N7 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? N8 C15 C14 106.7(4) . . ? N8 C15 H15A 110.4 . . ? C14 C15 H15A 110.4 . . ? N8 C15 H15B 110.4 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? N8 C16 C17 124.1(5) . . ? N8 C16 H16 118.0 . . ? C17 C16 H16 118.0 . . ? C22 C17 C18 118.6(5) . . ? C22 C17 C16 122.6(4) . . ? C18 C17 C16 118.8(5) . . ? C19 C18 C17 121.9(5) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 119.1(5) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C19 C20 C21 121.0(5) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 120.6(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? O2 C22 C21 118.8(5) . . ? O2 C22 C17 122.4(4) . . ? C21 C22 C17 118.8(5) . . ? O5 C23 C24 118.3(4) . . ? O5 C23 C28 124.0(4) . . ? C24 C23 C28 117.6(4) . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 121.2(5) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.1(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 120.7(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C23 120.4(4) . . ? C27 C28 C29 116.4(4) . . ? C23 C28 C29 123.1(4) . . ? N9 C29 C28 124.9(4) . . ? N9 C29 H29 117.6 . . ? C28 C29 H29 117.6 . . ? N9 C30 C31 106.9(4) . . ? N9 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? N9 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? N10 C31 C30 107.3(4) . . ? N10 C31 H31A 110.3 . . ? C30 C31 H31A 110.3 . . ? N10 C31 H31B 110.3 . . ? C30 C31 H31B 110.3 . . ? H31A C31 H31B 108.5 . . ? N10 C32 C33 126.1(4) . . ? N10 C32 H32 116.9 . . ? C33 C32 H32 116.9 . . ? C38 C33 C32 123.4(4) . . ? C38 C33 C34 118.7(5) . . ? C32 C33 C34 117.8(5) . . ? C35 C34 C33 121.2(6) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 119.3(5) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 120.6(6) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 121.7(6) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? O6 C38 C37 118.3(5) . . ? O6 C38 C33 123.5(4) . . ? C37 C38 C33 118.2(5) . . ? O3 C39 C40 118.9(4) . . ? O3 C39 C44 123.5(4) . . ? C40 C39 C44 117.6(4) . . ? C41 C40 C39 121.9(4) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 120.5(4) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.4(4) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 120.8(4) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C43 C44 C39 119.8(4) . . ? C43 C44 C45 117.4(4) . . ? C39 C44 C45 122.9(4) . . ? N11 C45 C44 124.8(4) . . ? N11 C45 H45 117.6 . . ? C44 C45 H45 117.6 . . ? N11 C46 C47 105.9(3) . . ? N11 C46 H46A 110.5 . . ? C47 C46 H46A 110.5 . . ? N11 C46 H46B 110.5 . . ? C47 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? N12 C47 C46 106.4(3) . . ? N12 C47 H47A 110.4 . . ? C46 C47 H47A 110.4 . . ? N12 C47 H47B 110.4 . . ? C46 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? N12 C48 C49 124.2(4) . . ? N12 C48 H48 117.9 . . ? C49 C48 H48 117.9 . . ? C50 C49 C54 120.3(4) . . ? C50 C49 C48 116.5(4) . . ? C54 C49 C48 123.0(4) . . ? C51 C50 C49 120.8(4) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C52 C51 C50 118.5(4) . . ? C52 C51 H51 120.8 . . ? C50 C51 H51 120.8 . . ? C53 C52 C51 121.7(4) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C52 C53 C54 120.4(4) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? O4 C54 C49 123.8(4) . . ? O4 C54 C53 118.0(4) . . ? C49 C54 C53 118.2(4) . . ? O7 C55 H55A 109.5 . . ? O7 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O7 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N13 C56 C57 175.6(9) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N14 C58 C59 170.8(16) . . ? C58 C59 H59A 109.4 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C7 -175.7(4) . . . . ? N7 Mn1 O1 C7 -7.0(4) . . . . ? N8 Mn1 O1 C7 -75.4(6) . . . . ? N1 Mn1 O1 C7 81.5(4) . . . . ? O1 Mn1 O2 C22 -163.4(5) . . . . ? N7 Mn1 O2 C22 83.8(9) . . . . ? N8 Mn1 O2 C22 32.5(5) . . . . ? N1 Mn1 O2 C22 -61.0(5) . . . . ? O4 Mn3 O3 C39 155.5(3) . . . . ? N11 Mn3 O3 C39 -21.6(3) . . . . ? N12 Mn3 O3 C39 -19.4(13) . . . . ? N3 Mn3 O3 C39 -110.9(3) . . . . ? O7 Mn3 O3 C39 66.1(3) . . . . ? O3 Mn3 O4 C54 154.8(3) . . . . ? N11 Mn3 O4 C54 -45.2(11) . . . . ? N12 Mn3 O4 C54 -25.8(3) . . . . ? N3 Mn3 O4 C54 62.2(3) . . . . ? O7 Mn3 O4 C54 -118.0(3) . . . . ? O6 Mn2 O5 C23 -173.3(3) . . . . ? N9 Mn2 O5 C23 12.2(3) . . . . ? N10 Mn2 O5 C23 12.1(12) . . . . ? N4 Mn2 O5 C23 -76.4(3) . . . . ? N2 Mn2 O5 C23 96.3(3) . . . . ? O5 Mn2 O6 C38 -172.4(3) . . . . ? N9 Mn2 O6 C38 -32.1(11) . . . . ? N10 Mn2 O6 C38 7.0(4) . . . . ? N4 Mn2 O6 C38 93.7(4) . . . . ? N2 Mn2 O6 C38 -81.2(4) . . . . ? O3 Mn3 O7 C55 68.6(3) . . . . ? O4 Mn3 O7 C55 -27.6(3) . . . . ? N11 Mn3 O7 C55 160.5(3) . . . . ? N12 Mn3 O7 C55 -118.5(3) . . . . ? N3 Mn3 O7 C55 149(2) . . . . ? O2 Mn1 N1 C1 172.6(7) . . . . ? O1 Mn1 N1 C1 -91.6(7) . . . . ? N7 Mn1 N1 C1 -0.4(7) . . . . ? N8 Mn1 N1 C1 82.1(7) . . . . ? O6 Mn2 N2 C2 151.3(6) . . . . ? O5 Mn2 N2 C2 -114.1(6) . . . . ? N9 Mn2 N2 C2 -22.2(6) . . . . ? N10 Mn2 N2 C2 59.3(6) . . . . ? N4 Mn2 N2 C2 7.6(13) . . . . ? O3 Mn3 N3 C3 117.4(9) . . . . ? O4 Mn3 N3 C3 -146.3(9) . . . . ? N11 Mn3 N3 C3 25.7(9) . . . . ? N12 Mn3 N3 C3 -55.5(9) . . . . ? O7 Mn3 N3 C3 37(3) . . . . ? O6 Mn2 N4 C4 -162.4(9) . . . . ? O5 Mn2 N4 C4 102.5(9) . . . . ? N9 Mn2 N4 C4 10.6(9) . . . . ? N10 Mn2 N4 C4 -70.8(9) . . . . ? N2 Mn2 N4 C4 -19.1(16) . . . . ? O2 Mn1 N7 C13 122.0(7) . . . . ? O1 Mn1 N7 C13 9.0(4) . . . . ? N8 Mn1 N7 C13 173.9(4) . . . . ? N1 Mn1 N7 C13 -92.4(4) . . . . ? O2 Mn1 N7 C14 -66.3(8) . . . . ? O1 Mn1 N7 C14 -179.3(3) . . . . ? N8 Mn1 N7 C14 -14.5(3) . . . . ? N1 Mn1 N7 C14 79.3(3) . . . . ? O2 Mn1 N8 C16 -20.7(4) . . . . ? O1 Mn1 N8 C16 -121.5(5) . . . . ? N7 Mn1 N8 C16 168.9(4) . . . . ? N1 Mn1 N8 C16 81.1(4) . . . . ? O2 Mn1 N8 C15 158.3(3) . . . . ? O1 Mn1 N8 C15 57.5(6) . . . . ? N7 Mn1 N8 C15 -12.1(3) . . . . ? N1 Mn1 N8 C15 -99.9(3) . . . . ? O6 Mn2 N9 C29 -148.1(8) . . . . ? O5 Mn2 N9 C29 -7.7(3) . . . . ? N10 Mn2 N9 C29 172.3(4) . . . . ? N4 Mn2 N9 C29 85.7(3) . . . . ? N2 Mn2 N9 C29 -98.6(3) . . . . ? O6 Mn2 N9 C30 27.7(10) . . . . ? O5 Mn2 N9 C30 168.1(3) . . . . ? N10 Mn2 N9 C30 -11.9(3) . . . . ? N4 Mn2 N9 C30 -98.6(3) . . . . ? N2 Mn2 N9 C30 77.1(3) . . . . ? O6 Mn2 N10 C32 -4.6(3) . . . . ? O5 Mn2 N10 C32 170.1(9) . . . . ? N9 Mn2 N10 C32 170.0(4) . . . . ? N4 Mn2 N10 C32 -101.1(4) . . . . ? N2 Mn2 N10 C32 85.7(3) . . . . ? O6 Mn2 N10 C31 171.4(3) . . . . ? O5 Mn2 N10 C31 -13.9(12) . . . . ? N9 Mn2 N10 C31 -14.0(3) . . . . ? N4 Mn2 N10 C31 75.0(3) . . . . ? N2 Mn2 N10 C31 -98.3(3) . . . . ? O3 Mn3 N11 C45 15.0(4) . . . . ? O4 Mn3 N11 C45 -145.1(8) . . . . ? N12 Mn3 N11 C45 -164.8(4) . . . . ? N3 Mn3 N11 C45 107.2(4) . . . . ? O7 Mn3 N11 C45 -72.1(4) . . . . ? O3 Mn3 N11 C46 -166.4(3) . . . . ? O4 Mn3 N11 C46 33.5(11) . . . . ? N12 Mn3 N11 C46 13.8(3) . . . . ? N3 Mn3 N11 C46 -74.2(3) . . . . ? O7 Mn3 N11 C46 106.4(3) . . . . ? O3 Mn3 N12 C48 -163.2(10) . . . . ? O4 Mn3 N12 C48 21.8(4) . . . . ? N11 Mn3 N12 C48 -161.0(4) . . . . ? N3 Mn3 N12 C48 -71.5(4) . . . . ? O7 Mn3 N12 C48 111.6(4) . . . . ? O3 Mn3 N12 C47 11.3(13) . . . . ? O4 Mn3 N12 C47 -163.7(3) . . . . ? N11 Mn3 N12 C47 13.5(3) . . . . ? N3 Mn3 N12 C47 103.0(3) . . . . ? O7 Mn3 N12 C47 -73.9(3) . . . . ? Mn1 N1 C1 Cr1 28(5) . . . . ? C2 Cr1 C1 N1 -178(100) . . . . ? C2 Cr1 C1 N1 2(5) 2_566 . . . ? C3 Cr1 C1 N1 -88(5) . . . . ? C3 Cr1 C1 N1 92(5) 2_566 . . . ? C1 Cr1 C1 N1 7(42) 2_566 . . . ? Mn2 N2 C2 Cr1 -4(5) . . . . ? C2 Cr1 C2 N2 47(25) 2_566 . . . ? C3 Cr1 C2 N2 -134(4) . . . . ? C3 Cr1 C2 N2 46(4) 2_566 . . . ? C1 Cr1 C2 N2 -44(4) . . . . ? C1 Cr1 C2 N2 136(4) 2_566 . . . ? Mn3 N3 C3 Cr1 18(8) . . . . ? C2 Cr1 C3 N3 -17(7) . . . . ? C2 Cr1 C3 N3 163(7) 2_566 . . . ? C3 Cr1 C3 N3 110(25) 2_566 . . . ? C1 Cr1 C3 N3 -108(7) . . . . ? C1 Cr1 C3 N3 72(7) 2_566 . . . ? Mn2 N4 C4 Cr2 13(6) . . . . ? C6 Cr2 C4 N4 127(6) 2_575 . . . ? C6 Cr2 C4 N4 -53(6) . . . . ? C4 Cr2 C4 N4 -137(23) 2_575 . . . ? C5 Cr2 C4 N4 36(6) . . . . ? C5 Cr2 C4 N4 -144(6) 2_575 . . . ? C6 Cr2 C5 N5 74(23) 2_575 . . . ? C6 Cr2 C5 N5 -106(23) . . . . ? C4 Cr2 C5 N5 166(23) . . . . ? C4 Cr2 C5 N5 -14(23) 2_575 . . . ? C5 Cr2 C5 N5 -34(21) 2_575 . . . ? C6 Cr2 C6 N6 25(32) 2_575 . . . ? C4 Cr2 C6 N6 -155(34) . . . . ? C4 Cr2 C6 N6 25(34) 2_575 . . . ? C5 Cr2 C6 N6 115(34) . . . . ? C5 Cr2 C6 N6 -65(34) 2_575 . . . ? Mn1 O1 C7 C8 -178.0(3) . . . . ? Mn1 O1 C7 C12 2.7(6) . . . . ? O1 C7 C8 C9 -179.0(4) . . . . ? C12 C7 C8 C9 0.4(6) . . . . ? C7 C8 C9 C10 -1.9(7) . . . . ? C8 C9 C10 C11 1.8(7) . . . . ? C9 C10 C11 C12 -0.3(7) . . . . ? C10 C11 C12 C7 -1.1(7) . . . . ? C10 C11 C12 C13 176.5(4) . . . . ? O1 C7 C12 C11 -179.5(4) . . . . ? C8 C7 C12 C11 1.1(6) . . . . ? O1 C7 C12 C13 2.9(7) . . . . ? C8 C7 C12 C13 -176.4(4) . . . . ? C14 N7 C13 C12 -178.0(4) . . . . ? Mn1 N7 C13 C12 -6.9(6) . . . . ? C11 C12 C13 N7 -178.0(4) . . . . ? C7 C12 C13 N7 -0.5(7) . . . . ? C13 N7 C14 C15 -151.4(4) . . . . ? Mn1 N7 C14 C15 36.4(4) . . . . ? C16 N8 C15 C14 -146.6(4) . . . . ? Mn1 N8 C15 C14 34.3(4) . . . . ? N7 C14 C15 N8 -44.1(5) . . . . ? C15 N8 C16 C17 -174.6(4) . . . . ? Mn1 N8 C16 C17 4.3(6) . . . . ? N8 C16 C17 C22 10.6(7) . . . . ? N8 C16 C17 C18 -172.5(4) . . . . ? C22 C17 C18 C19 -2.5(7) . . . . ? C16 C17 C18 C19 -179.5(5) . . . . ? C17 C18 C19 C20 1.3(8) . . . . ? C18 C19 C20 C21 0.1(8) . . . . ? C19 C20 C21 C22 -0.3(8) . . . . ? Mn1 O2 C22 C21 153.7(4) . . . . ? Mn1 O2 C22 C17 -28.2(7) . . . . ? C20 C21 C22 O2 177.2(5) . . . . ? C20 C21 C22 C17 -1.0(8) . . . . ? C18 C17 C22 O2 -175.9(5) . . . . ? C16 C17 C22 O2 1.0(7) . . . . ? C18 C17 C22 C21 2.3(7) . . . . ? C16 C17 C22 C21 179.1(4) . . . . ? Mn2 O5 C23 C24 172.8(3) . . . . ? Mn2 O5 C23 C28 -10.5(5) . . . . ? O5 C23 C24 C25 177.5(4) . . . . ? C28 C23 C24 C25 0.5(6) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C24 C25 C26 C27 -1.4(7) . . . . ? C25 C26 C27 C28 2.0(7) . . . . ? C26 C27 C28 C23 -1.3(7) . . . . ? C26 C27 C28 C29 -178.3(4) . . . . ? O5 C23 C28 C27 -176.8(4) . . . . ? C24 C23 C28 C27 0.1(6) . . . . ? O5 C23 C28 C29 0.0(6) . . . . ? C24 C23 C28 C29 176.8(4) . . . . ? C30 N9 C29 C28 -174.4(4) . . . . ? Mn2 N9 C29 C28 1.2(6) . . . . ? C27 C28 C29 N9 -178.5(4) . . . . ? C23 C28 C29 N9 4.6(7) . . . . ? C29 N9 C30 C31 -150.1(4) . . . . ? Mn2 N9 C30 C31 33.8(4) . . . . ? C32 N10 C31 C30 -148.2(4) . . . . ? Mn2 N10 C31 C30 35.7(4) . . . . ? N9 C30 C31 N10 -43.1(4) . . . . ? C31 N10 C32 C33 -174.4(4) . . . . ? Mn2 N10 C32 C33 1.4(6) . . . . ? N10 C32 C33 C38 1.8(7) . . . . ? N10 C32 C33 C34 178.4(4) . . . . ? C38 C33 C34 C35 -2.1(7) . . . . ? C32 C33 C34 C35 -178.9(4) . . . . ? C33 C34 C35 C36 -1.3(8) . . . . ? C34 C35 C36 C37 2.4(8) . . . . ? C35 C36 C37 C38 -0.1(9) . . . . ? Mn2 O6 C38 C37 173.5(3) . . . . ? Mn2 O6 C38 C33 -6.1(6) . . . . ? C36 C37 C38 O6 177.1(5) . . . . ? C36 C37 C38 C33 -3.3(7) . . . . ? C32 C33 C38 O6 0.5(7) . . . . ? C34 C33 C38 O6 -176.1(4) . . . . ? C32 C33 C38 C37 -179.2(4) . . . . ? C34 C33 C38 C37 4.3(6) . . . . ? Mn3 O3 C39 C40 -163.8(3) . . . . ? Mn3 O3 C39 C44 17.7(6) . . . . ? O3 C39 C40 C41 -179.1(4) . . . . ? C44 C39 C40 C41 -0.4(6) . . . . ? C39 C40 C41 C42 -0.4(7) . . . . ? C40 C41 C42 C43 0.8(7) . . . . ? C41 C42 C43 C44 -0.2(7) . . . . ? C42 C43 C44 C39 -0.7(7) . . . . ? C42 C43 C44 C45 178.5(4) . . . . ? O3 C39 C44 C43 179.5(4) . . . . ? C40 C39 C44 C43 1.0(6) . . . . ? O3 C39 C44 C45 0.3(7) . . . . ? C40 C39 C44 C45 -178.2(4) . . . . ? C46 N11 C45 C44 177.3(4) . . . . ? Mn3 N11 C45 C44 -4.2(6) . . . . ? C43 C44 C45 N11 173.9(4) . . . . ? C39 C44 C45 N11 -6.9(7) . . . . ? C45 N11 C46 C47 142.2(4) . . . . ? Mn3 N11 C46 C47 -36.5(4) . . . . ? C48 N12 C47 C46 138.5(4) . . . . ? Mn3 N12 C47 C46 -36.3(4) . . . . ? N11 C46 C47 N12 44.8(5) . . . . ? C47 N12 C48 C49 177.3(4) . . . . ? Mn3 N12 C48 C49 -8.6(6) . . . . ? N12 C48 C49 C50 174.3(4) . . . . ? N12 C48 C49 C54 -10.0(7) . . . . ? C54 C49 C50 C51 1.1(7) . . . . ? C48 C49 C50 C51 176.9(4) . . . . ? C49 C50 C51 C52 -3.0(7) . . . . ? C50 C51 C52 C53 2.2(7) . . . . ? C51 C52 C53 C54 0.5(6) . . . . ? Mn3 O4 C54 C49 16.8(6) . . . . ? Mn3 O4 C54 C53 -163.1(3) . . . . ? C50 C49 C54 O4 -178.2(4) . . . . ? C48 C49 C54 O4 6.3(6) . . . . ? C50 C49 C54 C53 1.6(6) . . . . ? C48 C49 C54 C53 -173.9(4) . . . . ? C52 C53 C54 O4 177.4(4) . . . . ? C52 C53 C54 C49 -2.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.685 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.094 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29.50 H28.25 Cl3 Cr0.50 Mn1.50 N6 O7.75' _chemical_formula_weight 805.59 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.771(8) _cell_length_b 11.199(2) _cell_length_c 19.971(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.58(3) _cell_angle_gamma 90.00 _cell_volume 7620(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8736 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.02 _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3278 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8404 _exptl_absorpt_correction_T_max 0.9479 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26724 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6633 _reflns_number_gt 5237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1116P)^2^+33.3216P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00122(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6633 _refine_ls_number_parameters 475 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2301 _refine_ls_wR_factor_gt 0.2137 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.092 _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 O7 O -0.0017(11) 0.469(2) 0.2178(14) 0.172(11) Uani 0.35 1 d PDU . . C1 C 0.00642(17) 0.8927(5) 0.0901(3) 0.0420(13) Uani 1 1 d . . . C2 C 0.03343(19) 1.1305(6) 0.0750(4) 0.0484(15) Uani 1 1 d . . . C3 C 0.05015(18) 0.9304(5) -0.0041(3) 0.0445(14) Uani 1 1 d . . . C4 C 0.07720(16) 0.7302(5) 0.3416(3) 0.0408(13) Uani 1 1 d . . . C5 C 0.10088(19) 0.6300(6) 0.3694(4) 0.0577(17) Uani 1 1 d . . . H5A H 0.0901 0.5546 0.3540 0.069 Uiso 1 1 calc R . . C6 C 0.13944(19) 0.6395(7) 0.4187(4) 0.0613(18) Uani 1 1 d . . . H6 H 0.1547 0.5709 0.4352 0.074 Uiso 1 1 calc R . . C7 C 0.15606(17) 0.7500(7) 0.4442(4) 0.0551(17) Uani 1 1 d . . . C8 C 0.13377(16) 0.8511(6) 0.4189(3) 0.0451(14) Uani 1 1 d . . . H8 H 0.1450 0.9253 0.4364 0.054 Uiso 1 1 calc R . . C9 C 0.09439(16) 0.8444(5) 0.3670(3) 0.0388(12) Uani 1 1 d . . . C10 C 0.07401(16) 0.9551(5) 0.3406(3) 0.0402(12) Uani 1 1 d . . . H10 H 0.0878 1.0252 0.3600 0.048 Uiso 1 1 calc R . . C11 C 0.0199(2) 1.0838(6) 0.2640(5) 0.079(2) Uani 1 1 d U . . H11 H 0.0223 1.0846 0.2171 0.095 Uiso 1 1 calc R . . C12 C 0.0435(4) 1.1893(11) 0.2980(8) 0.050(3) Uani 0.50 1 d PU . . H12A H 0.0275 1.2595 0.2804 0.075 Uiso 0.50 1 calc PR . . H12B H 0.0651 1.1936 0.2850 0.075 Uiso 0.50 1 calc PR . . H12C H 0.0533 1.1843 0.3510 0.075 Uiso 0.50 1 calc PR . . C13 C 0.1647(2) 0.6952(7) 0.2518(4) 0.0623(18) Uani 1 1 d . . . C14 C 0.1932(2) 0.7603(7) 0.3088(4) 0.0653(19) Uani 1 1 d . . . H14 H 0.2164 0.7229 0.3405 0.078 Uiso 1 1 calc R . . C15 C 0.1876(2) 0.8809(7) 0.3194(4) 0.0640(18) Uani 1 1 d . . . H15 H 0.2071 0.9233 0.3578 0.077 Uiso 1 1 calc R . . C16 C 0.1529(2) 0.9376(6) 0.2723(4) 0.0593(18) Uani 1 1 d . . . C17 C 0.1242(2) 0.8748(6) 0.2148(4) 0.0560(17) Uani 1 1 d . . . H17 H 0.1010 0.9128 0.1834 0.067 Uiso 1 1 calc R . . C18 C 0.1299(2) 0.7538(6) 0.2037(4) 0.0574(17) Uani 1 1 d . . . C19 C 0.0988(2) 0.6919(6) 0.1423(4) 0.0589(18) Uani 1 1 d . . . H19 H 0.0758 0.7344 0.1162 0.071 Uiso 1 1 calc R . . C20 C 0.0648(2) 0.5278(7) 0.0602(5) 0.074(2) Uani 1 1 d . . . H20 H 0.0516 0.4822 0.0848 0.089 Uiso 1 1 calc R . . C21 C 0.0350(2) 0.6087(8) 0.0071(6) 0.093(3) Uani 1 1 d . . . H21A H 0.0228 0.6538 0.0324 0.139 Uiso 1 1 calc R . . H21B H 0.0154 0.5625 -0.0318 0.139 Uiso 1 1 calc R . . H21C H 0.0473 0.6622 -0.0139 0.139 Uiso 1 1 calc R . . C22 C 0.0794(2) 0.4398(7) 0.0228(5) 0.069(2) Uani 1 1 d . . . H22A H 0.0865 0.4802 -0.0126 0.082 Uiso 1 1 calc R . . H22B H 0.0590 0.3823 -0.0040 0.082 Uiso 1 1 calc R . . C23 C 0.12032(17) 0.2654(6) 0.0724(4) 0.0511(15) Uani 1 1 d . . . H23 H 0.1008 0.2241 0.0336 0.061 Uiso 1 1 calc R . . C24 C 0.15478(17) 0.1992(5) 0.1200(3) 0.0442(13) Uani 1 1 d . . . C25 C 0.15695(19) 0.0779(6) 0.1044(4) 0.0521(15) Uani 1 1 d . . . H25 H 0.1356 0.0414 0.0664 0.063 Uiso 1 1 calc R . . C26 C 0.18963(19) 0.0133(5) 0.1436(4) 0.0499(15) Uani 1 1 d . . . C27 C 0.2225(2) 0.0671(6) 0.1989(4) 0.0563(16) Uani 1 1 d . . . H27 H 0.2453 0.0227 0.2239 0.068 Uiso 1 1 calc R . . C28 C 0.22168(19) 0.1850(5) 0.2168(4) 0.0513(15) Uani 1 1 d . . . H28 H 0.2437 0.2195 0.2544 0.062 Uiso 1 1 calc R . . C29 C 0.18732(17) 0.2550(5) 0.1779(3) 0.0433(13) Uani 1 1 d . . . C30 C 0.20733(19) 0.5538(6) 0.0947(4) 0.0584(17) Uani 1 1 d . . . H30A H 0.2250 0.6168 0.1217 0.088 Uiso 1 1 calc R . . H30B H 0.2044 0.5529 0.0445 0.088 Uiso 1 1 calc R . . H30C H 0.2177 0.4786 0.1180 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.20575(4) 0.76087(19) 0.50586(10) 0.0677(5) Uani 1 1 d . . . Cl2 Cl 0.14546(7) 1.08639(16) 0.28613(13) 0.0759(6) Uani 1 1 d . . . Cl3 Cl 0.19106(6) -0.13772(15) 0.12418(12) 0.0737(6) Uani 1 1 d . . . Cr1 Cr 0.0000 1.0000 0.0000 0.0368(3) Uani 1 2 d S . . Mn1 Mn 0.0000 0.83127(10) 0.2500 0.0330(3) Uani 1 2 d S . . Mn2 Mn 0.14649(3) 0.47817(8) 0.16462(6) 0.0499(3) Uani 1 1 d . . . N1 N 0.00857(15) 0.8422(4) 0.1426(3) 0.0467(12) Uani 1 1 d . . . N2 N 0.05152(19) 1.2026(5) 0.1181(3) 0.0638(15) Uani 1 1 d . . . N3 N 0.07729(16) 0.8915(5) -0.0096(3) 0.0549(13) Uani 1 1 d . . . N4 N 0.03763(14) 0.9650(4) 0.2915(3) 0.0423(11) Uani 1 1 d U . . N5 N 0.09988(15) 0.5858(5) 0.1205(3) 0.0575(14) Uani 1 1 d . . . N6 N 0.11433(14) 0.3770(4) 0.0792(3) 0.0515(13) Uani 1 1 d . . . O1 O 0.04005(11) 0.7158(3) 0.2925(2) 0.0452(10) Uani 1 1 d . . . O2 O 0.17145(16) 0.5773(4) 0.2461(3) 0.0713(14) Uani 1 1 d . . . O3 O 0.18809(13) 0.3680(4) 0.1981(3) 0.0546(11) Uani 1 1 d . . . O4 O 0.1095(2) 0.3742(5) 0.2160(4) 0.0938(19) Uani 1 1 d . . . H4A H 0.0858 0.3552 0.1892 0.113 Uiso 1 1 d R . . H4B H 0.1202 0.3562 0.2618 0.113 Uiso 1 1 d R . . O5 O 0.17039(12) 0.5732(4) 0.0946(3) 0.0610(13) Uani 1 1 d . . . H5 H 0.1544 0.6312 0.0622 0.073 Uiso 1 1 calc R . . O6 O 0.12247(16) 0.6952(5) 0.9761(3) 0.0756(15) Uani 1 1 d D . . O9 O 0.1953(5) 0.440(2) 0.3820(11) 0.094(5) Uani 0.33 1 d PU A 1 O8 O 0.0405(3) 0.5195(10) 0.1996(7) 0.064(3) Uani 0.40 1 d PDU . . O9A O 0.1523(5) 0.3440(13) 0.3662(9) 0.076(4) Uani 0.37 1 d PU B 2 O9B O 0.2109(5) 0.3610(18) 0.3792(8) 0.113(8) Uani 0.30 1 d PU C 3 H7A H 0.0000 0.5118 0.2500 0.169 Uiso 0.70 2 d SPRD . . H6A H 0.1315 0.7233 0.9502 0.169 Uiso 1 1 d RD . . H8A H 0.0189 0.4912 0.1830 0.169 Uiso 0.40 1 d PRD . . 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 O7 0.168(13) 0.130(12) 0.195(15) 0.021(9) 0.055(10) -0.006(9) C1 0.049(3) 0.037(3) 0.039(3) -0.008(3) 0.019(3) 0.007(2) C2 0.058(4) 0.048(3) 0.049(4) 0.004(3) 0.032(3) 0.004(3) C3 0.055(4) 0.043(3) 0.037(3) 0.007(3) 0.022(3) 0.003(3) C4 0.044(3) 0.043(3) 0.030(3) 0.001(2) 0.011(2) 0.003(3) C5 0.057(4) 0.046(4) 0.058(4) 0.002(3) 0.012(3) 0.012(3) C6 0.044(4) 0.067(4) 0.061(4) 0.007(4) 0.011(3) 0.020(3) C7 0.037(3) 0.081(5) 0.046(4) 0.003(3) 0.016(3) 0.005(3) C8 0.039(3) 0.056(4) 0.039(3) 0.000(3) 0.016(3) -0.001(3) C9 0.038(3) 0.045(3) 0.034(3) 0.006(2) 0.016(2) 0.003(2) C10 0.039(3) 0.044(3) 0.038(3) 0.000(3) 0.017(2) -0.004(2) C11 0.062(4) 0.043(3) 0.096(5) 0.009(3) 0.001(3) -0.002(3) C12 0.053(6) 0.041(5) 0.053(6) 0.006(5) 0.021(5) 0.004(5) C13 0.077(5) 0.059(4) 0.055(4) 0.003(3) 0.033(4) 0.016(4) C14 0.080(5) 0.060(4) 0.050(4) 0.000(3) 0.023(4) 0.017(4) C15 0.078(5) 0.062(4) 0.058(4) 0.000(4) 0.035(4) 0.008(4) C16 0.082(5) 0.047(4) 0.066(5) 0.008(3) 0.049(4) 0.012(4) C17 0.065(4) 0.047(4) 0.070(5) 0.019(3) 0.041(4) 0.014(3) C18 0.065(4) 0.052(4) 0.065(4) 0.012(3) 0.037(4) 0.017(3) C19 0.053(4) 0.056(4) 0.070(5) 0.017(4) 0.028(4) 0.014(3) C20 0.056(4) 0.058(4) 0.093(6) 0.005(4) 0.017(4) 0.003(3) C21 0.063(5) 0.063(5) 0.133(9) 0.013(5) 0.024(5) 0.003(4) C22 0.046(4) 0.069(5) 0.072(5) 0.009(4) 0.008(3) 0.005(3) C23 0.043(3) 0.051(4) 0.055(4) 0.011(3) 0.017(3) -0.007(3) C24 0.045(3) 0.041(3) 0.048(4) 0.007(3) 0.020(3) -0.001(3) C25 0.060(4) 0.046(3) 0.050(4) 0.003(3) 0.023(3) -0.010(3) C26 0.058(4) 0.034(3) 0.053(4) 0.002(3) 0.020(3) 0.000(3) C27 0.069(4) 0.044(4) 0.053(4) 0.010(3) 0.023(3) 0.013(3) C28 0.059(4) 0.038(3) 0.044(4) 0.004(3) 0.011(3) 0.006(3) C29 0.050(3) 0.039(3) 0.041(3) 0.007(3) 0.020(3) 0.002(3) C30 0.058(4) 0.053(4) 0.063(4) -0.003(3) 0.025(3) -0.002(3) Cl1 0.0376(8) 0.0969(14) 0.0556(10) 0.0039(10) 0.0079(7) 0.0092(8) Cl2 0.1042(15) 0.0464(10) 0.0979(16) 0.0077(9) 0.0632(13) 0.0103(9) Cl3 0.0880(13) 0.0392(9) 0.0791(14) -0.0003(8) 0.0221(11) 0.0025(8) Cr1 0.0458(7) 0.0397(7) 0.0283(7) 0.0021(5) 0.0191(5) 0.0069(5) Mn1 0.0364(6) 0.0315(6) 0.0272(6) 0.000 0.0103(5) 0.000 Mn2 0.0515(6) 0.0446(6) 0.0509(6) 0.0089(4) 0.0195(5) 0.0097(4) N1 0.063(3) 0.047(3) 0.038(3) 0.006(2) 0.028(2) 0.009(2) N2 0.087(4) 0.058(3) 0.052(4) -0.015(3) 0.036(3) -0.013(3) N3 0.053(3) 0.059(3) 0.057(3) 0.008(3) 0.028(3) 0.013(3) N4 0.044(3) 0.034(2) 0.045(3) 0.004(2) 0.015(2) 0.0005(19) N5 0.050(3) 0.048(3) 0.075(4) 0.009(3) 0.027(3) 0.007(2) N6 0.042(3) 0.042(3) 0.066(4) 0.013(3) 0.019(3) 0.003(2) O1 0.046(2) 0.035(2) 0.040(2) 0.0042(17) 0.0060(18) 0.0030(17) O2 0.087(3) 0.054(3) 0.057(3) 0.000(2) 0.016(3) 0.027(3) O3 0.062(3) 0.040(2) 0.051(3) 0.003(2) 0.014(2) 0.011(2) O4 0.135(5) 0.074(4) 0.074(4) 0.008(3) 0.047(4) -0.010(4) O5 0.042(2) 0.064(3) 0.077(3) 0.025(3) 0.026(2) 0.004(2) O6 0.078(3) 0.080(3) 0.071(4) 0.024(3) 0.034(3) 0.023(3) O9 0.089(9) 0.112(9) 0.087(9) 0.012(7) 0.046(7) 0.020(7) O8 0.058(6) 0.059(6) 0.073(7) -0.010(5) 0.027(5) 0.003(5) O9A 0.090(8) 0.073(7) 0.067(7) 0.001(6) 0.038(6) 0.006(6) O9B 0.122(11) 0.101(10) 0.107(11) 0.004(8) 0.042(8) 0.025(8) _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 O7 O7 1.24(5) 2 ? O7 H7A 0.7816 . ? O7 H8A 1.2711 . ? C1 N1 1.163(7) . ? C1 Cr1 2.089(6) . ? C2 N2 1.163(8) . ? C2 Cr1 2.083(7) . ? C3 N3 1.162(7) . ? C3 Cr1 2.082(6) . ? C4 O1 1.330(7) . ? C4 C5 1.393(8) . ? C4 C9 1.424(8) . ? C5 C6 1.365(9) . ? C5 H5A 0.9300 . ? C6 C7 1.383(10) . ? C6 H6 0.9300 . ? C7 C8 1.370(9) . ? C7 Cl1 1.748(6) . ? C8 C9 1.400(8) . ? C8 H8 0.9300 . ? C9 C10 1.435(8) . ? C10 N4 1.303(7) . ? C10 H10 0.9300 . ? C11 C11 1.359(14) 2 ? C11 C12 1.459(14) . ? C11 N4 1.483(8) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O2 1.359(8) . ? C13 C14 1.389(11) . ? C13 C18 1.410(10) . ? C14 C15 1.397(10) . ? C14 H14 0.9300 . ? C15 C16 1.394(10) . ? C15 H15 0.9300 . ? C16 C17 1.383(10) . ? C16 Cl2 1.732(7) . ? C17 C18 1.405(9) . ? C17 H17 0.9300 . ? C18 C19 1.455(10) . ? C19 N5 1.272(9) . ? C19 H19 0.9300 . ? C20 C21 1.477(11) . ? C20 C22 1.480(12) . ? C20 N5 1.500(9) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N6 1.489(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N6 1.287(8) . ? C23 C24 1.442(8) . ? C23 H23 0.9300 . ? C24 C25 1.404(9) . ? C24 C29 1.418(8) . ? C25 C26 1.351(9) . ? C25 H25 0.9300 . ? C26 C27 1.393(9) . ? C26 Cl3 1.741(6) . ? C27 C28 1.372(9) . ? C27 H27 0.9300 . ? C28 C29 1.425(8) . ? C28 H28 0.9300 . ? C29 O3 1.325(7) . ? C30 O5 1.411(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Cr1 C3 2.082(6) 5_575 ? Cr1 C2 2.083(7) 5_575 ? Cr1 C1 2.089(6) 5_575 ? Mn1 O1 1.890(4) . ? Mn1 O1 1.890(4) 2 ? Mn1 N4 1.983(5) 2 ? Mn1 N4 1.983(5) . ? Mn1 N1 2.306(5) 2 ? Mn1 N1 2.306(5) . ? Mn2 O2 1.856(5) . ? Mn2 O3 1.879(4) . ? Mn2 N6 1.970(6) . ? Mn2 N5 1.997(5) . ? Mn2 O5 2.235(4) . ? Mn2 O4 2.365(6) . ? O4 H4A 0.8500 . ? O4 H4B 0.8498 . ? O5 H5 0.9300 . ? O6 H6A 0.7974 . ? O8 H8A 0.8017 . ? 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 O7 O7 H7A 37.8 2 . ? O7 O7 H8A 139.0 2 . ? H7A O7 H8A 118.5 . . ? N1 C1 Cr1 173.4(5) . . ? N2 C2 Cr1 178.1(6) . . ? N3 C3 Cr1 177.1(5) . . ? O1 C4 C5 119.2(5) . . ? O1 C4 C9 123.1(5) . . ? C5 C4 C9 117.8(5) . . ? C6 C5 C4 121.8(6) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 119.6(6) . . ? C8 C7 Cl1 120.3(5) . . ? C6 C7 Cl1 120.0(5) . . ? C7 C8 C9 121.1(6) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C4 119.2(5) . . ? C8 C9 C10 117.1(5) . . ? C4 C9 C10 123.7(5) . . ? N4 C10 C9 125.1(5) . . ? N4 C10 H10 117.5 . . ? C9 C10 H10 117.5 . . ? C11 C11 C12 122.4(7) 2 . ? C11 C11 N4 113.2(4) 2 . ? C12 C11 N4 117.9(7) . . ? C11 C11 H11 98.5 2 . ? C12 C11 H11 98.5 . . ? N4 C11 H11 98.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C14 118.1(6) . . ? O2 C13 C18 123.3(7) . . ? C14 C13 C18 118.6(7) . . ? C13 C14 C15 121.2(7) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.1(6) . . ? C17 C16 Cl2 119.9(5) . . ? C15 C16 Cl2 120.0(6) . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C13 120.2(7) . . ? C17 C18 C19 118.0(6) . . ? C13 C18 C19 121.8(6) . . ? N5 C19 C18 126.9(6) . . ? N5 C19 H19 116.6 . . ? C18 C19 H19 116.6 . . ? C21 C20 C22 112.4(8) . . ? C21 C20 N5 116.5(7) . . ? C22 C20 N5 107.4(6) . . ? C21 C20 H20 106.6 . . ? C22 C20 H20 106.6 . . ? N5 C20 H20 106.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 N6 109.6(7) . . ? C20 C22 H22A 109.7 . . ? N6 C22 H22A 109.7 . . ? C20 C22 H22B 109.7 . . ? N6 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? N6 C23 C24 125.5(6) . . ? N6 C23 H23 117.3 . . ? C24 C23 H23 117.3 . . ? C25 C24 C29 119.6(5) . . ? C25 C24 C23 118.3(6) . . ? C29 C24 C23 121.9(6) . . ? C26 C25 C24 121.0(6) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 120.5(6) . . ? C25 C26 Cl3 119.9(5) . . ? C27 C26 Cl3 119.6(5) . . ? C28 C27 C26 120.6(6) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.4(6) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? O3 C29 C24 124.5(5) . . ? O3 C29 C28 117.7(5) . . ? C24 C29 C28 117.8(5) . . ? O5 C30 H30A 109.5 . . ? O5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C3 Cr1 C3 180.00(14) . 5_575 ? C3 Cr1 C2 89.3(2) . 5_575 ? C3 Cr1 C2 90.7(2) 5_575 5_575 ? C3 Cr1 C2 90.7(2) . . ? C3 Cr1 C2 89.3(2) 5_575 . ? C2 Cr1 C2 179.997(1) 5_575 . ? C3 Cr1 C1 92.8(2) . . ? C3 Cr1 C1 87.2(2) 5_575 . ? C2 Cr1 C1 91.4(2) 5_575 . ? C2 Cr1 C1 88.6(2) . . ? C3 Cr1 C1 87.2(2) . 5_575 ? C3 Cr1 C1 92.8(2) 5_575 5_575 ? C2 Cr1 C1 88.6(2) 5_575 5_575 ? C2 Cr1 C1 91.4(2) . 5_575 ? C1 Cr1 C1 179.998(1) . 5_575 ? O1 Mn1 O1 93.6(2) . 2 ? O1 Mn1 N4 174.06(18) . 2 ? O1 Mn1 N4 92.25(18) 2 2 ? O1 Mn1 N4 92.24(18) . . ? O1 Mn1 N4 174.06(18) 2 . ? N4 Mn1 N4 81.9(3) 2 . ? O1 Mn1 N1 91.45(19) . 2 ? O1 Mn1 N1 92.70(18) 2 2 ? N4 Mn1 N1 89.2(2) 2 2 ? N4 Mn1 N1 86.27(19) . 2 ? O1 Mn1 N1 92.70(18) . . ? O1 Mn1 N1 91.44(19) 2 . ? N4 Mn1 N1 86.27(19) 2 . ? N4 Mn1 N1 89.2(2) . . ? N1 Mn1 N1 173.9(3) 2 . ? O2 Mn2 O3 92.9(2) . . ? O2 Mn2 N6 173.3(2) . . ? O3 Mn2 N6 92.2(2) . . ? O2 Mn2 N5 92.5(2) . . ? O3 Mn2 N5 174.6(2) . . ? N6 Mn2 N5 82.5(2) . . ? O2 Mn2 O5 94.3(2) . . ? O3 Mn2 O5 91.93(19) . . ? N6 Mn2 O5 89.8(2) . . ? N5 Mn2 O5 87.3(2) . . ? O2 Mn2 O4 94.9(2) . . ? O3 Mn2 O4 94.7(2) . . ? N6 Mn2 O4 80.4(2) . . ? N5 Mn2 O4 85.1(2) . . ? O5 Mn2 O4 168.4(2) . . ? C1 N1 Mn1 151.7(4) . . ? C10 N4 C11 121.0(5) . . ? C10 N4 Mn1 125.6(4) . . ? C11 N4 Mn1 113.3(4) . . ? C19 N5 C20 122.1(6) . . ? C19 N5 Mn2 124.4(5) . . ? C20 N5 Mn2 113.4(4) . . ? C23 N6 C22 121.2(6) . . ? C23 N6 Mn2 125.3(4) . . ? C22 N6 Mn2 113.3(4) . . ? C4 O1 Mn1 129.2(4) . . ? C13 O2 Mn2 127.7(5) . . ? C29 O3 Mn2 127.9(4) . . ? Mn2 O4 H4A 120.7 . . ? Mn2 O4 H4B 119.3 . . ? H4A O4 H4B 120.0 . . ? C30 O5 Mn2 126.3(4) . . ? C30 O5 H5 116.9 . . ? Mn2 O5 H5 116.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C5 C6 178.6(6) . . . . ? C9 C4 C5 C6 -0.8(10) . . . . ? C4 C5 C6 C7 1.7(12) . . . . ? C5 C6 C7 C8 -1.1(11) . . . . ? C5 C6 C7 Cl1 -178.7(6) . . . . ? C6 C7 C8 C9 -0.4(9) . . . . ? Cl1 C7 C8 C9 177.1(5) . . . . ? C7 C8 C9 C4 1.3(9) . . . . ? C7 C8 C9 C10 -176.6(5) . . . . ? O1 C4 C9 C8 180.0(5) . . . . ? C5 C4 C9 C8 -0.7(8) . . . . ? O1 C4 C9 C10 -2.3(9) . . . . ? C5 C4 C9 C10 177.1(6) . . . . ? C8 C9 C10 N4 178.7(5) . . . . ? C4 C9 C10 N4 0.9(9) . . . . ? O2 C13 C14 C15 -177.9(7) . . . . ? C18 C13 C14 C15 0.8(11) . . . . ? C13 C14 C15 C16 0.2(11) . . . . ? C14 C15 C16 C17 -0.8(10) . . . . ? C14 C15 C16 Cl2 178.9(6) . . . . ? C15 C16 C17 C18 0.2(10) . . . . ? Cl2 C16 C17 C18 -179.5(5) . . . . ? C16 C17 C18 C13 0.9(10) . . . . ? C16 C17 C18 C19 -179.9(6) . . . . ? O2 C13 C18 C17 177.3(6) . . . . ? C14 C13 C18 C17 -1.3(10) . . . . ? O2 C13 C18 C19 -1.9(11) . . . . ? C14 C13 C18 C19 179.4(7) . . . . ? C17 C18 C19 N5 174.5(7) . . . . ? C13 C18 C19 N5 -6.2(11) . . . . ? C21 C20 C22 N6 169.4(6) . . . . ? N5 C20 C22 N6 39.9(8) . . . . ? N6 C23 C24 C25 -179.1(6) . . . . ? N6 C23 C24 C29 -4.0(10) . . . . ? C29 C24 C25 C26 0.0(9) . . . . ? C23 C24 C25 C26 175.2(6) . . . . ? C24 C25 C26 C27 -2.3(10) . . . . ? C24 C25 C26 Cl3 178.6(5) . . . . ? C25 C26 C27 C28 3.0(10) . . . . ? Cl3 C26 C27 C28 -178.0(5) . . . . ? C26 C27 C28 C29 -1.3(10) . . . . ? C25 C24 C29 O3 -178.7(6) . . . . ? C23 C24 C29 O3 6.3(9) . . . . ? C25 C24 C29 C28 1.7(9) . . . . ? C23 C24 C29 C28 -173.3(6) . . . . ? C27 C28 C29 O3 179.3(6) . . . . ? C27 C28 C29 C24 -1.1(9) . . . . ? N3 C3 Cr1 C3 -176(11) . . . 5_575 ? N3 C3 Cr1 C2 47(11) . . . 5_575 ? N3 C3 Cr1 C2 -133(11) . . . . ? N3 C3 Cr1 C1 138(11) . . . . ? N3 C3 Cr1 C1 -42(11) . . . 5_575 ? N2 C2 Cr1 C3 -134(20) . . . . ? N2 C2 Cr1 C3 46(20) . . . 5_575 ? N2 C2 Cr1 C2 -154(19) . . . 5_575 ? N2 C2 Cr1 C1 -41(20) . . . . ? N2 C2 Cr1 C1 139(20) . . . 5_575 ? N1 C1 Cr1 C3 145(5) . . . . ? N1 C1 Cr1 C3 -35(5) . . . 5_575 ? N1 C1 Cr1 C2 -126(5) . . . 5_575 ? N1 C1 Cr1 C2 54(5) . . . . ? N1 C1 Cr1 C1 -61(10) . . . 5_575 ? Cr1 C1 N1 Mn1 1(6) . . . . ? O1 Mn1 N1 C1 -154.6(10) . . . . ? O1 Mn1 N1 C1 111.7(10) 2 . . . ? N4 Mn1 N1 C1 19.6(10) 2 . . . ? N4 Mn1 N1 C1 -62.4(10) . . . . ? N1 Mn1 N1 C1 -21.4(10) 2 . . . ? C9 C10 N4 C11 -176.0(7) . . . . ? C9 C10 N4 Mn1 7.3(8) . . . . ? C11 C11 N4 C10 -157.2(10) 2 . . . ? C12 C11 N4 C10 -4.8(13) . . . . ? C11 C11 N4 Mn1 19.8(13) 2 . . . ? C12 C11 N4 Mn1 172.3(8) . . . . ? O1 Mn1 N4 C10 -10.6(5) . . . . ? O1 Mn1 N4 C10 160.9(16) 2 . . . ? N4 Mn1 N4 C10 170.3(6) 2 . . . ? N1 Mn1 N4 C10 80.7(5) 2 . . . ? N1 Mn1 N4 C10 -103.3(5) . . . . ? O1 Mn1 N4 C11 172.5(5) . . . . ? O1 Mn1 N4 C11 -16(2) 2 . . . ? N4 Mn1 N4 C11 -6.6(5) 2 . . . ? N1 Mn1 N4 C11 -96.2(6) 2 . . . ? N1 Mn1 N4 C11 79.8(6) . . . . ? C18 C19 N5 C20 174.9(7) . . . . ? C18 C19 N5 Mn2 -2.3(10) . . . . ? C21 C20 N5 C19 24.3(12) . . . . ? C22 C20 N5 C19 151.3(7) . . . . ? C21 C20 N5 Mn2 -158.2(7) . . . . ? C22 C20 N5 Mn2 -31.2(8) . . . . ? O2 Mn2 N5 C19 12.8(6) . . . . ? O3 Mn2 N5 C19 -164(2) . . . . ? N6 Mn2 N5 C19 -171.5(6) . . . . ? O5 Mn2 N5 C19 -81.4(6) . . . . ? O4 Mn2 N5 C19 107.5(6) . . . . ? O2 Mn2 N5 C20 -164.6(5) . . . . ? O3 Mn2 N5 C20 19(3) . . . . ? N6 Mn2 N5 C20 11.1(5) . . . . ? O5 Mn2 N5 C20 101.2(5) . . . . ? O4 Mn2 N5 C20 -69.9(5) . . . . ? C24 C23 N6 C22 174.2(6) . . . . ? C24 C23 N6 Mn2 -10.3(9) . . . . ? C20 C22 N6 C23 143.3(7) . . . . ? C20 C22 N6 Mn2 -32.7(7) . . . . ? O2 Mn2 N6 C23 -123.5(18) . . . . ? O3 Mn2 N6 C23 16.8(6) . . . . ? N5 Mn2 N6 C23 -163.9(6) . . . . ? O5 Mn2 N6 C23 108.7(5) . . . . ? O4 Mn2 N6 C23 -77.6(5) . . . . ? O2 Mn2 N6 C22 52(2) . . . . ? O3 Mn2 N6 C22 -167.3(5) . . . . ? N5 Mn2 N6 C22 11.9(5) . . . . ? O5 Mn2 N6 C22 -75.4(5) . . . . ? O4 Mn2 N6 C22 98.3(5) . . . . ? C5 C4 O1 Mn1 175.3(5) . . . . ? C9 C4 O1 Mn1 -5.4(8) . . . . ? O1 Mn1 O1 C4 -169.3(6) 2 . . . ? N4 Mn1 O1 C4 19(2) 2 . . . ? N4 Mn1 O1 C4 9.8(5) . . . . ? N1 Mn1 O1 C4 -76.5(5) 2 . . . ? N1 Mn1 O1 C4 99.1(5) . . . . ? C14 C13 O2 Mn2 -162.4(6) . . . . ? C18 C13 O2 Mn2 18.9(10) . . . . ? O3 Mn2 O2 C13 158.7(6) . . . . ? N6 Mn2 O2 C13 -61(2) . . . . ? N5 Mn2 O2 C13 -21.0(6) . . . . ? O5 Mn2 O2 C13 66.5(6) . . . . ? O4 Mn2 O2 C13 -106.4(6) . . . . ? C24 C29 O3 Mn2 6.9(9) . . . . ? C28 C29 O3 Mn2 -173.5(4) . . . . ? O2 Mn2 O3 C29 160.5(5) . . . . ? N6 Mn2 O3 C29 -15.2(5) . . . . ? N5 Mn2 O3 C29 -23(3) . . . . ? O5 Mn2 O3 C29 -105.1(5) . . . . ? O4 Mn2 O3 C29 65.3(5) . . . . ? O2 Mn2 O5 C30 84.2(5) . . . . ? O3 Mn2 O5 C30 -8.8(5) . . . . ? N6 Mn2 O5 C30 -101.0(5) . . . . ? N5 Mn2 O5 C30 176.5(5) . . . . ? O4 Mn2 O5 C30 -133.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.306 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.104