# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 899929' #TrackingRef '13705_web_deposit_cif_file_0_XiaoPingShen_1346742789.[Mn(salen)]3[Cr(salen)(CN)2]3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H92 Cr3 Mn3 N18 O16' _chemical_formula_weight 2146.76 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.039(5) _cell_length_b 20.336(6) _cell_length_c 16.729(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.988(5) _cell_angle_gamma 90.00 _cell_volume 5453(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2210 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38691 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10517 _reflns_number_gt 7368 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0400P)^2^+0.5500P] 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 10517 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.02279(17) 0.62021(15) 0.65014(16) 0.0411(7) Uani 1 1 d . . . C2 C 1.00392(18) 0.58019(15) 0.71346(18) 0.0468(7) Uani 1 1 d . . . H2 H 1.0227 0.5909 0.7650 0.056 Uiso 1 1 calc R . . C3 C 0.95704(18) 0.52415(15) 0.70010(18) 0.0443(7) Uani 1 1 d . . . H3 H 0.9453 0.4965 0.7425 0.053 Uiso 1 1 calc R . . C4 C 0.92715(18) 0.50889(14) 0.62280(18) 0.0447(7) Uani 1 1 d . . . H4 H 0.8943 0.4717 0.6144 0.054 Uiso 1 1 calc R . . C5 C 0.94591(17) 0.54852(13) 0.55890(17) 0.0378(6) Uani 1 1 d . . . H5 H 0.9269 0.5379 0.5074 0.045 Uiso 1 1 calc R . . C6 C 0.99447(18) 0.60535(14) 0.57326(17) 0.0423(7) Uani 1 1 d . . . C7 C 1.02236(18) 0.64447(14) 0.50491(17) 0.0413(7) Uani 1 1 d . . . H7 H 1.0138 0.6261 0.4544 0.050 Uiso 1 1 calc R . . C8 C 1.07691(18) 0.74145(14) 0.43630(17) 0.0425(7) Uani 1 1 d . . . H8A H 1.0468 0.7248 0.3892 0.051 Uiso 1 1 calc R . . H8B H 1.1361 0.7379 0.4270 0.051 Uiso 1 1 calc R . . C9 C 1.05446(18) 0.81442(14) 0.44807(17) 0.0421(7) Uani 1 1 d . . . H9A H 1.0798 0.8427 0.4090 0.050 Uiso 1 1 calc R . . H9B H 0.9947 0.8217 0.4475 0.050 Uiso 1 1 calc R . . C10 C 1.12459(17) 0.87815(15) 0.54018(16) 0.0404(7) Uani 1 1 d . . . H10 H 1.1264 0.9075 0.4976 0.049 Uiso 1 1 calc R . . C11 C 1.15814(17) 0.89883(14) 0.61861(17) 0.0406(7) Uani 1 1 d . . . C12 C 1.20429(17) 0.95614(14) 0.61874(16) 0.0384(7) Uani 1 1 d . . . H12 H 1.2101 0.9793 0.5713 0.046 Uiso 1 1 calc R . . C13 C 1.24204(16) 0.97935(15) 0.68883(17) 0.0405(7) Uani 1 1 d . . . H13 H 1.2727 1.0181 0.6881 0.049 Uiso 1 1 calc R . . C14 C 1.23466(17) 0.94553(13) 0.75993(16) 0.0374(6) Uani 1 1 d . . . H14 H 1.2600 0.9614 0.8069 0.045 Uiso 1 1 calc R . . C15 C 1.18830(17) 0.88670(15) 0.76026(16) 0.0399(7) Uani 1 1 d . . . H15 H 1.1835 0.8633 0.8076 0.048 Uiso 1 1 calc R . . C16 C 1.14965(17) 0.86346(14) 0.68986(16) 0.0386(6) Uani 1 1 d . . . C17 C 0.69308(17) 0.84647(14) 0.71164(16) 0.0387(7) Uani 1 1 d . . . C18 C 0.67257(18) 0.91050(15) 0.73326(19) 0.0448(7) Uani 1 1 d . . . H18 H 0.6851 0.9455 0.6999 0.054 Uiso 1 1 calc R . . C19 C 0.63317(17) 0.92210(15) 0.80522(17) 0.0416(7) Uani 1 1 d . . . H19 H 0.6207 0.9649 0.8204 0.050 Uiso 1 1 calc R . . C20 C 0.61283(17) 0.86995(14) 0.85357(16) 0.0398(7) Uani 1 1 d . . . H20 H 0.5852 0.8776 0.9006 0.048 Uiso 1 1 calc R . . C21 C 0.63345(17) 0.80624(15) 0.83227(18) 0.0428(7) Uani 1 1 d . . . H21 H 0.6210 0.7713 0.8657 0.051 Uiso 1 1 calc R . . C22 C 0.67268(17) 0.79479(14) 0.76114(15) 0.0367(6) Uani 1 1 d . . . C23 C 0.69312(15) 0.72603(14) 0.73862(15) 0.0340(6) Uani 1 1 d . . . H23 H 0.6793 0.6943 0.7760 0.041 Uiso 1 1 calc R . . C24 C 0.73761(17) 0.63103(14) 0.66988(16) 0.0391(7) Uani 1 1 d . . . H24A H 0.7951 0.6187 0.6821 0.047 Uiso 1 1 calc R . . H24B H 0.7016 0.6076 0.7055 0.047 Uiso 1 1 calc R . . C25 C 0.71447(19) 0.61698(14) 0.58551(17) 0.0446(7) Uani 1 1 d . . . H25A H 0.6543 0.6167 0.5777 0.054 Uiso 1 1 calc R . . H25B H 0.7358 0.5743 0.5703 0.054 Uiso 1 1 calc R . . C26 C 0.78987(18) 0.64693(16) 0.46766(18) 0.0460(7) Uani 1 1 d . . . H26 H 0.7928 0.6015 0.4621 0.055 Uiso 1 1 calc R . . C27 C 0.82132(18) 0.68722(14) 0.41066(17) 0.0400(7) Uani 1 1 d . . . C28 C 0.86652(18) 0.65808(15) 0.35121(16) 0.0417(7) Uani 1 1 d . . . H28 H 0.8711 0.6125 0.3489 0.050 Uiso 1 1 calc R . . C29 C 0.9054(2) 0.69732(17) 0.29460(18) 0.0505(8) Uani 1 1 d . . . H29 H 0.9345 0.6781 0.2535 0.061 Uiso 1 1 calc R . . C30 C 0.89989(19) 0.76515(16) 0.30059(18) 0.0474(8) Uani 1 1 d . . . H30 H 0.9262 0.7915 0.2637 0.057 Uiso 1 1 calc R . . C31 C 0.85590(17) 0.79402(15) 0.36049(17) 0.0409(7) Uani 1 1 d . . . H31 H 0.8525 0.8396 0.3635 0.049 Uiso 1 1 calc R . . C32 C 0.81666(18) 0.75545(14) 0.41637(16) 0.0402(7) Uani 1 1 d . . . C33 C 0.46694(17) 0.62481(14) 0.63425(16) 0.0394(6) Uani 1 1 d . . . C34 C 0.49244(17) 0.56081(14) 0.62097(18) 0.0422(7) Uani 1 1 d . . . H34 H 0.4825 0.5415 0.5712 0.051 Uiso 1 1 calc R . . C35 C 0.53308(17) 0.52518(14) 0.68239(16) 0.0387(6) Uani 1 1 d . . . H35 H 0.5512 0.4825 0.6732 0.046 Uiso 1 1 calc R . . C36 C 0.54625(17) 0.55361(13) 0.75676(16) 0.0368(6) Uani 1 1 d . . . H36 H 0.5724 0.5296 0.7977 0.044 Uiso 1 1 calc R . . C37 C 0.52073(18) 0.61789(13) 0.77094(17) 0.0407(7) Uani 1 1 d . . . H37 H 0.5305 0.6368 0.8210 0.049 Uiso 1 1 calc R . . C38 C 0.48044(16) 0.65386(15) 0.70991(17) 0.0409(7) Uani 1 1 d . . . C39 C 0.45752(15) 0.72027(13) 0.73663(16) 0.0337(6) Uani 1 1 d . . . H39 H 0.4605 0.7325 0.7902 0.040 Uiso 1 1 calc R . . C40 C 0.41030(17) 0.82864(13) 0.71044(16) 0.0378(6) Uani 1 1 d . . . H40A H 0.4397 0.8392 0.7605 0.045 Uiso 1 1 calc R . . H40B H 0.3508 0.8315 0.7183 0.045 Uiso 1 1 calc R . . C41 C 0.43609(17) 0.87656(14) 0.64365(16) 0.0399(7) Uani 1 1 d . . . H41A H 0.4130 0.9200 0.6518 0.048 Uiso 1 1 calc R . . H41B H 0.4963 0.8799 0.6418 0.048 Uiso 1 1 calc R . . C42 C 0.36373(17) 0.88226(15) 0.51748(17) 0.0426(7) Uani 1 1 d . . . H42 H 0.3598 0.9267 0.5297 0.051 Uiso 1 1 calc R . . C43 C 0.32807(17) 0.85995(13) 0.44143(15) 0.0360(6) Uani 1 1 d . . . C44 C 0.27906(16) 0.90535(14) 0.39836(15) 0.0346(6) Uani 1 1 d . . . H44 H 0.2753 0.9485 0.4163 0.041 Uiso 1 1 calc R . . C45 C 0.23616(16) 0.88648(14) 0.32923(15) 0.0365(6) Uani 1 1 d . . . H45 H 0.2025 0.9167 0.3016 0.044 Uiso 1 1 calc R . . C46 C 0.24304(19) 0.82196(15) 0.30042(17) 0.0441(7) Uani 1 1 d . . . H46 H 0.2149 0.8095 0.2533 0.053 Uiso 1 1 calc R . . C47 C 0.29225(18) 0.77682(15) 0.34302(16) 0.0431(7) Uani 1 1 d . . . H47 H 0.2962 0.7338 0.3246 0.052 Uiso 1 1 calc R . . C48 C 0.33630(16) 0.79561(14) 0.41402(15) 0.0329(6) Uani 1 1 d . . . N1 N 1.05613(15) 0.69949(11) 0.50777(13) 0.0387(6) Uani 1 1 d . . . N2 N 1.09319(14) 0.82191(12) 0.52820(14) 0.0390(5) Uani 1 1 d . . . N3 N 0.72603(14) 0.70422(12) 0.67729(14) 0.0405(6) Uani 1 1 d . . . N4 N 0.75451(14) 0.67372(13) 0.53220(14) 0.0439(6) Uani 1 1 d . . . N5 N 0.43382(13) 0.75917(11) 0.68239(13) 0.0378(5) Uani 1 1 d . . . N6 N 0.39944(13) 0.84543(10) 0.56757(13) 0.0331(5) Uani 1 1 d . . . O1 O 1.06824(12) 0.67466(9) 0.66994(11) 0.0430(5) Uani 1 1 d . . . O2 O 1.10418(11) 0.81078(9) 0.69422(11) 0.0374(4) Uani 1 1 d . . . O3 O 0.72958(11) 0.84345(9) 0.64008(11) 0.0389(5) Uani 1 1 d . . . O4 O 0.77252(11) 0.78383(9) 0.47471(10) 0.0387(5) Uani 1 1 d . . . O5 O 0.43145(11) 0.65738(9) 0.56907(12) 0.0419(5) Uani 1 1 d . . . O6 O 0.38398(11) 0.74957(9) 0.45040(11) 0.0371(4) Uani 1 1 d . . . O7 O 0.8921(2) 0.94544(19) 0.5612(2) 0.0447(10) Uani 0.50 1 d P . . H7D H 0.9078 0.9064 0.5719 0.054 Uiso 0.50 1 d PR . . H7B H 0.9180 0.9597 0.5213 0.054 Uiso 0.50 1 d PR . . O8 O 0.7679(2) 0.03156(19) 0.9524(2) 0.0428(9) Uani 0.50 1 d P . . H8F H 0.7732 0.0707 0.9356 0.051 Uiso 0.50 1 d PR . . H8C H 0.7187 0.0261 0.9686 0.051 Uiso 0.50 1 d PR . . O9 O 0.6734(2) 0.09052(19) 0.0560(2) 0.0440(10) Uani 0.50 1 d P . . H9C H 0.6640 0.0528 0.0358 0.053 Uiso 0.50 1 d PR . . H9D H 0.6329 0.1160 0.0439 0.053 Uiso 0.50 1 d PR . . O10 O 0.3799(2) 0.06254(19) 0.5321(2) 0.0382(9) Uani 0.50 1 d P . . H10D H 0.4065 0.0650 0.4891 0.046 Uiso 0.50 1 d PR . . H10C H 0.3935 0.0947 0.5624 0.046 Uiso 0.50 1 d PR . . N7 N 0.87591(17) 0.76535(13) 0.60723(14) 0.0403(6) Uani 0.50 1 d P . 1 N8 N 0.54056(17) 0.76107(13) 0.54719(15) 0.0425(6) Uani 0.50 1 d P . 1 N9 N 0.21531(16) 0.73585(12) 0.59697(15) 0.0385(6) Uani 0.50 1 d P . 1 C49 C 0.94544(17) 0.76603(13) 0.60802(15) 0.0396(6) Uani 0.50 1 d P . 1 C50 C 0.61287(17) 0.76242(12) 0.55629(15) 0.0403(6) Uani 0.50 1 d P . 1 C51 C 0.28688(16) 0.74486(13) 0.58170(15) 0.0400(6) Uani 0.50 1 d P . 1 Mn1 Mn 1.08045(3) 0.75014(2) 0.60817(3) 0.04021(12) Uani 0.50 1 d P . 1 Cr2 Cr 0.74364(3) 0.76399(2) 0.58220(3) 0.04070(12) Uani 0.50 1 d P . 1 Mn3 Mn 0.41197(3) 0.74978(2) 0.56379(3) 0.04022(12) Uani 0.50 1 d P . 1 C49' C 0.87591(17) 0.76535(13) 0.60723(14) 0.0403(6) Uani 0.50 1 d P . 2 C50' C 0.54056(17) 0.76107(13) 0.54719(15) 0.0425(6) Uani 0.50 1 d P . 2 C51' C 0.21531(16) 0.73585(12) 0.59697(15) 0.0385(6) Uani 0.50 1 d P . 2 N7' N 0.94544(17) 0.76603(13) 0.60802(15) 0.0396(6) Uani 0.50 1 d P . 2 N8' N 0.61287(17) 0.76242(12) 0.55629(15) 0.0403(6) Uani 0.50 1 d P . 2 N9' N 0.28688(16) 0.74486(13) 0.58170(15) 0.0400(6) Uani 0.50 1 d P . 2 Cr1 Cr 1.08045(3) 0.75014(2) 0.60817(3) 0.04021(12) Uani 0.50 1 d P . 2 Mn2 Mn 0.74364(3) 0.76399(2) 0.58220(3) 0.04070(12) Uani 0.50 1 d P . 2 Cr3 Cr 0.41197(3) 0.74978(2) 0.56379(3) 0.04022(12) Uani 0.50 1 d P . 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 C1 0.0348(15) 0.0516(18) 0.0378(15) -0.0125(13) 0.0148(12) -0.0119(13) C2 0.0443(17) 0.0498(18) 0.0452(17) 0.0071(14) -0.0130(14) -0.0098(14) C3 0.0421(16) 0.0484(17) 0.0429(17) 0.0078(13) 0.0080(13) -0.0081(14) C4 0.0450(16) 0.0380(16) 0.0521(18) -0.0099(13) 0.0149(14) -0.0157(13) C5 0.0378(15) 0.0375(15) 0.0388(15) -0.0106(12) 0.0127(12) -0.0038(12) C6 0.0405(16) 0.0389(16) 0.0468(16) 0.0057(13) -0.0099(13) -0.0108(13) C7 0.0445(16) 0.0451(17) 0.0353(15) -0.0115(13) 0.0141(12) -0.0103(14) C8 0.0411(16) 0.0475(18) 0.0378(15) 0.0032(13) -0.0128(12) -0.0140(13) C9 0.0344(15) 0.0398(16) 0.0512(17) 0.0178(13) -0.0102(13) -0.0148(12) C10 0.0424(16) 0.0448(17) 0.0347(14) -0.0108(12) 0.0100(12) -0.0031(13) C11 0.0333(14) 0.0405(16) 0.0474(16) 0.0082(13) -0.0092(12) -0.0098(12) C12 0.0367(15) 0.0416(16) 0.0363(15) 0.0080(12) -0.0067(12) -0.0098(12) C13 0.0267(13) 0.0478(17) 0.0468(17) 0.0036(13) 0.0001(12) -0.0112(13) C14 0.0363(15) 0.0367(15) 0.0383(15) -0.0055(12) -0.0126(12) 0.0109(12) C15 0.0344(14) 0.0547(18) 0.0307(14) 0.0051(13) 0.0026(11) -0.0102(13) C16 0.0385(15) 0.0445(17) 0.0327(14) 0.0035(12) 0.0016(12) -0.0038(13) C17 0.0348(15) 0.0455(17) 0.0347(15) 0.0001(12) -0.0143(12) 0.0118(13) C18 0.0368(16) 0.0427(17) 0.0550(19) 0.0100(14) 0.0013(13) 0.0008(13) C19 0.0389(15) 0.0453(17) 0.0393(15) -0.0067(13) -0.0208(13) 0.0174(13) C20 0.0345(15) 0.0517(18) 0.0326(14) -0.0057(13) -0.0073(11) 0.0104(13) C21 0.0346(15) 0.0444(17) 0.0496(17) 0.0013(14) 0.0051(13) 0.0051(13) C22 0.0345(15) 0.0439(16) 0.0311(14) -0.0121(12) -0.0083(11) 0.0086(12) C23 0.0236(12) 0.0431(15) 0.0346(14) 0.0032(12) -0.0068(11) 0.0169(11) C24 0.0280(14) 0.0476(17) 0.0421(16) 0.0070(13) 0.0066(12) 0.0116(12) C25 0.0453(17) 0.0418(17) 0.0461(17) -0.0123(13) -0.0079(13) 0.0102(14) C26 0.0426(17) 0.0496(18) 0.0452(17) 0.0006(14) -0.0086(13) 0.0057(14) C27 0.0385(15) 0.0417(16) 0.0389(15) 0.0009(12) -0.0116(13) -0.0005(13) C28 0.0477(17) 0.0425(17) 0.0338(15) -0.0037(12) -0.0122(13) 0.0130(14) C29 0.0484(18) 0.060(2) 0.0431(17) -0.0214(15) 0.0065(14) -0.0148(16) C30 0.0407(17) 0.053(2) 0.0478(18) 0.0115(14) -0.0024(14) 0.0029(14) C31 0.0327(15) 0.0465(17) 0.0429(16) 0.0115(14) -0.0093(12) -0.0049(13) C32 0.0407(16) 0.0425(16) 0.0371(15) -0.0100(13) -0.0029(12) -0.0108(13) C33 0.0395(16) 0.0387(16) 0.0408(15) 0.0125(13) 0.0149(12) -0.0070(13) C34 0.0373(16) 0.0411(17) 0.0482(17) 0.0063(13) 0.0025(13) -0.0054(13) C35 0.0374(15) 0.0381(15) 0.0416(16) 0.0049(13) 0.0169(12) 0.0075(13) C36 0.0451(16) 0.0310(14) 0.0345(14) 0.0119(11) 0.0046(12) -0.0041(12) C37 0.0485(17) 0.0328(15) 0.0414(16) 0.0136(12) 0.0132(13) -0.0101(13) C38 0.0285(14) 0.0526(18) 0.0421(16) 0.0077(13) 0.0101(12) 0.0133(13) C39 0.0257(13) 0.0342(14) 0.0400(15) 0.0126(11) -0.0143(11) -0.0035(11) C40 0.0357(15) 0.0421(16) 0.0352(15) 0.0065(12) -0.0054(12) 0.0132(12) C41 0.0367(15) 0.0400(16) 0.0421(15) 0.0016(13) -0.0113(12) -0.0015(12) C42 0.0407(16) 0.0425(17) 0.0433(16) -0.0049(13) -0.0168(12) 0.0156(13) C43 0.0395(15) 0.0363(15) 0.0319(14) -0.0025(11) -0.0022(12) -0.0046(12) C44 0.0314(13) 0.0426(16) 0.0300(14) 0.0036(11) 0.0041(11) -0.0097(12) C45 0.0303(14) 0.0474(17) 0.0321(14) -0.0013(12) 0.0053(11) 0.0140(12) C46 0.0488(18) 0.0477(17) 0.0353(15) -0.0016(13) -0.0056(13) -0.0075(14) C47 0.0473(17) 0.0421(17) 0.0395(16) -0.0184(13) -0.0049(13) 0.0104(14) C48 0.0267(13) 0.0430(15) 0.0294(13) -0.0098(11) 0.0071(10) 0.0025(11) N1 0.0429(13) 0.0408(14) 0.0319(12) 0.0046(10) -0.0053(10) -0.0137(11) N2 0.0290(12) 0.0460(14) 0.0423(13) 0.0009(11) 0.0032(10) -0.0150(11) N3 0.0297(12) 0.0529(15) 0.0394(13) 0.0075(11) 0.0082(10) 0.0155(11) N4 0.0301(12) 0.0619(16) 0.0389(13) -0.0017(12) -0.0085(10) 0.0087(11) N5 0.0310(12) 0.0456(14) 0.0363(12) 0.0136(11) -0.0072(9) 0.0121(10) N6 0.0304(11) 0.0318(12) 0.0361(12) 0.0010(9) -0.0125(9) -0.0013(9) O1 0.0453(11) 0.0406(11) 0.0419(11) 0.0011(9) -0.0152(9) -0.0048(9) O2 0.0271(9) 0.0399(11) 0.0443(11) -0.0073(9) -0.0109(8) 0.0043(8) O3 0.0368(10) 0.0381(11) 0.0413(11) 0.0145(8) -0.0063(8) -0.0168(9) O4 0.0332(10) 0.0515(12) 0.0304(10) -0.0012(8) -0.0137(8) 0.0079(9) O5 0.0340(10) 0.0417(11) 0.0496(12) 0.0070(9) -0.0057(9) 0.0028(9) O6 0.0329(10) 0.0349(10) 0.0433(10) -0.0135(8) -0.0029(8) 0.0012(8) O7 0.046(2) 0.048(2) 0.040(2) 0.0190(18) -0.0112(18) -0.0053(18) O8 0.039(2) 0.045(2) 0.045(2) 0.0136(18) 0.0071(17) -0.0033(18) O9 0.045(2) 0.041(2) 0.045(2) 0.0036(18) -0.0176(18) -0.0025(18) O10 0.035(2) 0.051(2) 0.0286(19) -0.0081(16) -0.0069(15) 0.0217(18) N7 0.0441(16) 0.0433(15) 0.0324(13) 0.0144(11) -0.0139(11) -0.0008(12) N8 0.0405(16) 0.0448(16) 0.0417(15) 0.0143(12) -0.0060(12) -0.0012(12) N9 0.0381(14) 0.0349(14) 0.0413(14) -0.0093(11) -0.0149(11) -0.0041(11) C49 0.0382(15) 0.0430(15) 0.0372(14) 0.0169(11) -0.0054(11) -0.0165(12) C50 0.0468(16) 0.0362(14) 0.0374(14) 0.0134(11) -0.0074(12) -0.0012(12) C51 0.0367(15) 0.0443(15) 0.0391(14) -0.0187(12) 0.0015(11) -0.0092(12) Mn1 0.0416(3) 0.0399(3) 0.0386(2) -0.0056(2) -0.00526(19) -0.0035(2) Cr2 0.0397(2) 0.0422(3) 0.0396(3) 0.0143(2) -0.00673(19) -0.0018(2) Mn3 0.0396(3) 0.0374(3) 0.0433(3) 0.0071(2) -0.00432(19) 0.0034(2) C49' 0.0441(16) 0.0433(15) 0.0324(13) 0.0144(11) -0.0139(11) -0.0008(12) C50' 0.0405(16) 0.0448(16) 0.0417(15) 0.0143(12) -0.0060(12) -0.0012(12) C51' 0.0381(14) 0.0349(14) 0.0413(14) -0.0093(11) -0.0149(11) -0.0041(11) N7' 0.0382(15) 0.0430(15) 0.0372(14) 0.0169(11) -0.0054(11) -0.0165(12) N8' 0.0468(16) 0.0362(14) 0.0374(14) 0.0134(11) -0.0074(12) -0.0012(12) N9' 0.0367(15) 0.0443(15) 0.0391(14) -0.0187(12) 0.0015(11) -0.0092(12) Cr1 0.0416(3) 0.0399(3) 0.0386(2) -0.0056(2) -0.00526(19) -0.0035(2) Mn2 0.0397(2) 0.0422(3) 0.0396(3) 0.0143(2) -0.00673(19) -0.0018(2) Cr3 0.0396(3) 0.0374(3) 0.0433(3) 0.0071(2) -0.00432(19) 0.0034(2) _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 C1 O1 1.360(3) . ? C1 C2 1.378(4) . ? C1 C6 1.382(4) . ? C2 C3 1.379(4) . ? C2 H2 0.9300 . ? C3 C4 1.398(4) . ? C3 H3 0.9300 . ? C4 C5 1.380(4) . ? C4 H4 0.9300 . ? C5 C6 1.410(4) . ? C5 H5 0.9300 . ? C6 C7 1.475(4) . ? C7 N1 1.243(3) . ? C7 H7 0.9300 . ? C8 N1 1.515(3) . ? C8 C9 1.541(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N2 1.466(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.263(4) . ? C10 C11 1.462(4) . ? C10 H10 0.9300 . ? C11 C12 1.381(4) . ? C11 C16 1.403(4) . ? C12 C13 1.384(4) . ? C12 H12 0.9300 . ? C13 C14 1.383(4) . ? C13 H13 0.9300 . ? C14 C15 1.409(4) . ? C14 H14 0.9300 . ? C15 C16 1.394(4) . ? C15 H15 0.9300 . ? C16 O2 1.299(3) . ? C17 O3 1.352(3) . ? C17 C22 1.384(4) . ? C17 C18 1.394(4) . ? C18 C19 1.399(4) . ? C18 H18 0.9300 . ? C19 C20 1.380(4) . ? C19 H19 0.9300 . ? C20 C21 1.387(4) . ? C20 H20 0.9300 . ? C21 C22 1.385(4) . ? C21 H21 0.9300 . ? C22 C23 1.488(4) . ? C23 N3 1.251(3) . ? C23 H23 0.9300 . ? C24 C25 1.475(4) . ? C24 N3 1.506(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N4 1.606(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N4 1.352(4) . ? C26 C27 1.367(4) . ? C26 H26 0.9300 . ? C27 C28 1.384(4) . ? C27 C32 1.393(4) . ? C28 C29 1.401(4) . ? C28 H28 0.9300 . ? C29 C30 1.386(4) . ? C29 H29 0.9300 . ? C30 C31 1.377(4) . ? C30 H30 0.9300 . ? C31 C32 1.388(4) . ? C31 H31 0.9300 . ? C32 O4 1.355(3) . ? C33 O5 1.381(3) . ? C33 C34 1.385(4) . ? C33 C38 1.407(4) . ? C34 C35 1.400(4) . ? C34 H34 0.9300 . ? C35 C36 1.382(4) . ? C35 H35 0.9300 . ? C36 C37 1.392(4) . ? C36 H36 0.9300 . ? C37 C38 1.396(4) . ? C37 H37 0.9300 . ? C38 C39 1.473(4) . ? C39 N5 1.253(3) . ? C39 H39 0.9300 . ? C40 N5 1.540(4) . ? C40 C41 1.550(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N6 1.521(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 N6 1.248(3) . ? C42 C43 1.450(4) . ? C42 H42 0.9300 . ? C43 C48 1.394(4) . ? C43 C44 1.396(4) . ? C44 C45 1.379(4) . ? C44 H44 0.9300 . ? C45 C46 1.403(4) . ? C45 H45 0.9300 . ? C46 C47 1.391(4) . ? C46 H46 0.9300 . ? C47 C48 1.413(3) . ? C47 H47 0.9300 . ? C48 O6 1.342(3) . ? N1 Mn1 1.997(2) . ? N2 Mn1 1.995(2) . ? N3 Cr2 2.029(2) . ? N4 Cr2 2.027(3) . ? N5 Mn3 2.012(2) . ? N6 Mn3 1.957(2) . ? O1 Mn1 1.864(2) . ? O2 Mn1 1.9235(18) . ? O3 Cr2 1.901(2) . ? O4 Cr2 1.915(2) . ? O5 Mn3 1.906(2) . ? O6 Mn3 1.9340(19) . ? O7 H7D 0.8501 . ? O7 H7B 0.8500 . ? O8 H8F 0.8500 . ? O8 H8C 0.8500 . ? O9 H9C 0.8500 . ? O9 H9D 0.8500 . ? O10 H10D 0.8501 . ? O10 H10C 0.8501 . ? N7 C49 1.115(4) . ? N7 Cr2 2.148(3) . ? N8 C50 1.165(4) . ? N8 Mn3 2.103(3) . ? N9 C51 1.199(4) . ? N9 Mn1 2.197(3) 1_455 ? C49 Mn1 2.189(3) . ? C50 Cr2 2.127(3) . ? C51 Mn3 2.041(3) . ? Mn1 N9 2.197(3) 1_655 ? 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 O1 C1 C2 115.1(2) . . ? O1 C1 C6 124.1(3) . . ? C2 C1 C6 120.8(3) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.7(3) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C1 C6 C5 120.0(3) . . ? C1 C6 C7 120.3(2) . . ? C5 C6 C7 119.4(3) . . ? N1 C7 C6 126.8(3) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? N1 C8 C9 112.5(2) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C8 97.1(2) . . ? N2 C9 H9A 112.3 . . ? C8 C9 H9A 112.3 . . ? N2 C9 H9B 112.3 . . ? C8 C9 H9B 112.3 . . ? H9A C9 H9B 109.9 . . ? N2 C10 C11 122.4(3) . . ? N2 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C16 119.9(3) . . ? C12 C11 C10 115.1(3) . . ? C16 C11 C10 124.8(3) . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.1(2) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? O2 C16 C15 117.8(2) . . ? O2 C16 C11 122.8(2) . . ? C15 C16 C11 119.4(3) . . ? O3 C17 C22 127.9(3) . . ? O3 C17 C18 112.7(3) . . ? C22 C17 C18 119.4(3) . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.3(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C17 C22 C21 120.7(3) . . ? C17 C22 C23 120.2(2) . . ? C21 C22 C23 119.1(3) . . ? N3 C23 C22 130.1(3) . . ? N3 C23 H23 115.0 . . ? C22 C23 H23 115.0 . . ? C25 C24 N3 104.0(2) . . ? C25 C24 H24A 110.9 . . ? N3 C24 H24A 110.9 . . ? C25 C24 H24B 110.9 . . ? N3 C24 H24B 110.9 . . ? H24A C24 H24B 109.0 . . ? C24 C25 N4 107.5(2) . . ? C24 C25 H25A 110.2 . . ? N4 C25 H25A 110.2 . . ? C24 C25 H25B 110.2 . . ? N4 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? N4 C26 C27 119.4(3) . . ? N4 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C26 C27 C28 117.4(3) . . ? C26 C27 C32 121.8(3) . . ? C28 C27 C32 120.4(3) . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 119.2(3) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 120.3(3) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? O4 C32 C31 120.3(3) . . ? O4 C32 C27 120.3(3) . . ? C31 C32 C27 119.3(3) . . ? O5 C33 C34 116.1(3) . . ? O5 C33 C38 123.7(3) . . ? C34 C33 C38 120.1(3) . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.6(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 119.4(3) . . ? C37 C38 C39 111.9(3) . . ? C33 C38 C39 128.7(2) . . ? N5 C39 C38 115.6(3) . . ? N5 C39 H39 122.2 . . ? C38 C39 H39 122.2 . . ? N5 C40 C41 106.4(2) . . ? N5 C40 H40A 110.4 . . ? C41 C40 H40A 110.4 . . ? N5 C40 H40B 110.4 . . ? C41 C40 H40B 110.4 . . ? H40A C40 H40B 108.6 . . ? N6 C41 C40 103.7(2) . . ? N6 C41 H41A 111.0 . . ? C40 C41 H41A 111.0 . . ? N6 C41 H41B 111.0 . . ? C40 C41 H41B 111.0 . . ? H41A C41 H41B 109.0 . . ? N6 C42 C43 124.0(3) . . ? N6 C42 H42 118.0 . . ? C43 C42 H42 118.0 . . ? C48 C43 C44 120.6(2) . . ? C48 C43 C42 122.9(2) . . ? C44 C43 C42 116.4(2) . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.3(3) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 119.4(2) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C46 C47 C48 120.7(3) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? O6 C48 C43 124.4(2) . . ? O6 C48 C47 116.9(2) . . ? C43 C48 C47 118.7(2) . . ? C7 N1 C8 125.7(2) . . ? C7 N1 Mn1 124.7(2) . . ? C8 N1 Mn1 109.35(16) . . ? C10 N2 C9 113.2(2) . . ? C10 N2 Mn1 127.3(2) . . ? C9 N2 Mn1 119.16(17) . . ? C23 N3 C24 118.3(2) . . ? C23 N3 Cr2 120.3(2) . . ? C24 N3 Cr2 120.43(17) . . ? C26 N4 C25 109.9(2) . . ? C26 N4 Cr2 137.6(2) . . ? C25 N4 Cr2 112.31(17) . . ? C39 N5 C40 115.5(2) . . ? C39 N5 Mn3 133.8(2) . . ? C40 N5 Mn3 110.58(14) . . ? C42 N6 C41 117.8(2) . . ? C42 N6 Mn3 128.32(19) . . ? C41 N6 Mn3 113.80(16) . . ? C1 O1 Mn1 126.93(17) . . ? C16 O2 Mn1 125.69(18) . . ? C17 O3 Cr2 123.52(17) . . ? C32 O4 Cr2 137.41(18) . . ? C33 O5 Mn3 124.86(18) . . ? C48 O6 Mn3 123.55(15) . . ? H7D O7 H7B 109.5 . . ? H8F O8 H8C 109.5 . . ? H9C O9 H9D 109.5 . . ? H10D O10 H10C 109.5 . . ? C49 N7 Cr2 169.4(2) . . ? C50 N8 Mn3 164.1(2) . . ? C51 N9 Mn1 162.0(2) . 1_455 ? N7 C49 Mn1 170.8(2) . . ? N8 C50 Cr2 175.7(2) . . ? N9 C51 Mn3 172.8(2) . . ? O1 Mn1 O2 97.75(9) . . ? O1 Mn1 N2 171.50(9) . . ? O2 Mn1 N2 90.61(9) . . ? O1 Mn1 N1 91.17(9) . . ? O2 Mn1 N1 171.06(9) . . ? N2 Mn1 N1 80.49(10) . . ? O1 Mn1 C49 89.96(9) . . ? O2 Mn1 C49 94.38(9) . . ? N2 Mn1 C49 90.89(9) . . ? N1 Mn1 C49 84.89(10) . . ? O1 Mn1 N9 93.50(9) . 1_655 ? O2 Mn1 N9 88.79(8) . 1_655 ? N2 Mn1 N9 85.15(10) . 1_655 ? N1 Mn1 N9 91.38(9) . 1_655 ? C49 Mn1 N9 174.97(9) . 1_655 ? O3 Cr2 O4 109.63(8) . . ? O3 Cr2 N4 173.29(9) . . ? O4 Cr2 N4 77.07(9) . . ? O3 Cr2 N3 95.03(9) . . ? O4 Cr2 N3 155.07(9) . . ? N4 Cr2 N3 78.31(10) . . ? O3 Cr2 C50 89.03(9) . . ? O4 Cr2 C50 94.63(9) . . ? N4 Cr2 C50 90.04(10) . . ? N3 Cr2 C50 89.30(9) . . ? O3 Cr2 N7 91.35(9) . . ? O4 Cr2 N7 84.89(9) . . ? N4 Cr2 N7 89.64(10) . . ? N3 Cr2 N7 91.05(9) . . ? C50 Cr2 N7 179.47(11) . . ? O5 Mn3 O6 94.33(8) . . ? O5 Mn3 N6 174.36(8) . . ? O6 Mn3 N6 90.76(8) . . ? O5 Mn3 N5 91.44(9) . . ? O6 Mn3 N5 173.72(8) . . ? N6 Mn3 N5 83.59(9) . . ? O5 Mn3 C51 96.05(10) . . ? O6 Mn3 C51 87.02(9) . . ? N6 Mn3 C51 86.64(10) . . ? N5 Mn3 C51 89.91(10) . . ? O5 Mn3 N8 87.35(9) . . ? O6 Mn3 N8 93.79(9) . . ? N6 Mn3 N8 89.89(10) . . ? N5 Mn3 N8 88.95(10) . . ? C51 Mn3 N8 176.44(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.1(3) . . . . ? C6 C1 C2 C3 0.8(5) . . . . ? C1 C2 C3 C4 -1.5(5) . . . . ? C2 C3 C4 C5 1.7(5) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? O1 C1 C6 C5 -178.4(3) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? O1 C1 C6 C7 8.4(5) . . . . ? C2 C1 C6 C7 -173.5(3) . . . . ? C4 C5 C6 C1 0.4(4) . . . . ? C4 C5 C6 C7 173.7(3) . . . . ? C1 C6 C7 N1 -16.4(5) . . . . ? C5 C6 C7 N1 170.4(3) . . . . ? N1 C8 C9 N2 48.1(3) . . . . ? N2 C10 C11 C12 168.1(3) . . . . ? N2 C10 C11 C16 -8.8(5) . . . . ? C16 C11 C12 C13 -0.4(4) . . . . ? C10 C11 C12 C13 -177.4(3) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 -0.7(4) . . . . ? C14 C15 C16 O2 -176.6(2) . . . . ? C14 C15 C16 C11 0.7(4) . . . . ? C12 C11 C16 O2 177.0(3) . . . . ? C10 C11 C16 O2 -6.2(5) . . . . ? C12 C11 C16 C15 -0.1(4) . . . . ? C10 C11 C16 C15 176.6(3) . . . . ? O3 C17 C18 C19 179.1(2) . . . . ? C22 C17 C18 C19 1.2(4) . . . . ? C17 C18 C19 C20 -1.7(4) . . . . ? C18 C19 C20 C21 1.9(4) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? O3 C17 C22 C21 -178.5(2) . . . . ? C18 C17 C22 C21 -1.0(4) . . . . ? O3 C17 C22 C23 1.8(4) . . . . ? C18 C17 C22 C23 179.3(2) . . . . ? C20 C21 C22 C17 1.3(4) . . . . ? C20 C21 C22 C23 -179.0(2) . . . . ? C17 C22 C23 N3 -2.3(4) . . . . ? C21 C22 C23 N3 178.0(3) . . . . ? N3 C24 C25 N4 42.3(3) . . . . ? N4 C26 C27 C28 171.7(2) . . . . ? N4 C26 C27 C32 -1.2(4) . . . . ? C26 C27 C28 C29 -175.4(3) . . . . ? C32 C27 C28 C29 -2.3(4) . . . . ? C27 C28 C29 C30 1.9(4) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C29 C30 C31 C32 0.4(4) . . . . ? C30 C31 C32 O4 -179.2(2) . . . . ? C30 C31 C32 C27 -0.8(4) . . . . ? C26 C27 C32 O4 -7.2(4) . . . . ? C28 C27 C32 O4 -179.9(2) . . . . ? C26 C27 C32 C31 174.5(3) . . . . ? C28 C27 C32 C31 1.8(4) . . . . ? O5 C33 C34 C35 176.6(2) . . . . ? C38 C33 C34 C35 -1.1(4) . . . . ? C33 C34 C35 C36 1.2(4) . . . . ? C34 C35 C36 C37 -1.1(4) . . . . ? C35 C36 C37 C38 0.9(4) . . . . ? C36 C37 C38 C33 -0.7(4) . . . . ? C36 C37 C38 C39 179.3(2) . . . . ? O5 C33 C38 C37 -176.7(3) . . . . ? C34 C33 C38 C37 0.9(4) . . . . ? O5 C33 C38 C39 3.3(4) . . . . ? C34 C33 C38 C39 -179.2(3) . . . . ? C37 C38 C39 N5 168.6(2) . . . . ? C33 C38 C39 N5 -11.3(4) . . . . ? N5 C40 C41 N6 48.9(3) . . . . ? N6 C42 C43 C48 -5.4(5) . . . . ? N6 C42 C43 C44 170.1(3) . . . . ? C48 C43 C44 C45 1.9(4) . . . . ? C42 C43 C44 C45 -173.7(3) . . . . ? C43 C44 C45 C46 -1.6(4) . . . . ? C44 C45 C46 C47 1.2(4) . . . . ? C45 C46 C47 C48 -1.1(5) . . . . ? C44 C43 C48 O6 177.9(3) . . . . ? C42 C43 C48 O6 -6.7(4) . . . . ? C44 C43 C48 C47 -1.7(4) . . . . ? C42 C43 C48 C47 173.6(3) . . . . ? C46 C47 C48 O6 -178.4(3) . . . . ? C46 C47 C48 C43 1.3(4) . . . . ? C6 C7 N1 C8 -173.9(3) . . . . ? C6 C7 N1 Mn1 -0.7(5) . . . . ? C9 C8 N1 C7 136.6(3) . . . . ? C9 C8 N1 Mn1 -37.6(3) . . . . ? C11 C10 N2 C9 173.1(3) . . . . ? C11 C10 N2 Mn1 0.5(4) . . . . ? C8 C9 N2 C10 145.3(2) . . . . ? C8 C9 N2 Mn1 -41.5(3) . . . . ? C22 C23 N3 C24 -178.7(2) . . . . ? C22 C23 N3 Cr2 -9.6(4) . . . . ? C25 C24 N3 C23 138.4(3) . . . . ? C25 C24 N3 Cr2 -30.6(3) . . . . ? C27 C26 N4 C25 174.4(2) . . . . ? C27 C26 N4 Cr2 -9.6(4) . . . . ? C24 C25 N4 C26 135.7(2) . . . . ? C24 C25 N4 Cr2 -41.4(2) . . . . ? C38 C39 N5 C40 -179.7(2) . . . . ? C38 C39 N5 Mn3 4.9(4) . . . . ? C41 C40 N5 C39 145.7(2) . . . . ? C41 C40 N5 Mn3 -37.8(2) . . . . ? C43 C42 N6 C41 178.1(3) . . . . ? C43 C42 N6 Mn3 -4.3(5) . . . . ? C40 C41 N6 C42 136.5(3) . . . . ? C40 C41 N6 Mn3 -41.4(2) . . . . ? C2 C1 O1 Mn1 -161.8(2) . . . . ? C6 C1 O1 Mn1 16.4(4) . . . . ? C15 C16 O2 Mn1 -154.4(2) . . . . ? C11 C16 O2 Mn1 28.4(4) . . . . ? C22 C17 O3 Cr2 11.6(3) . . . . ? C18 C17 O3 Cr2 -166.02(18) . . . . ? C31 C32 O4 Cr2 -150.8(2) . . . . ? C27 C32 O4 Cr2 30.9(4) . . . . ? C34 C33 O5 Mn3 -166.50(19) . . . . ? C38 C33 O5 Mn3 11.1(4) . . . . ? C43 C48 O6 Mn3 26.5(4) . . . . ? C47 C48 O6 Mn3 -153.8(2) . . . . ? Cr2 N7 C49 Mn1 -86.0(19) . . . . ? Mn3 N8 C50 Cr2 -12(4) . . . . ? Mn1 N9 C51 Mn3 171.0(11) 1_455 . . . ? C1 O1 Mn1 O2 154.3(2) . . . . ? C1 O1 Mn1 N2 -35.9(7) . . . . ? C1 O1 Mn1 N1 -25.0(2) . . . . ? C1 O1 Mn1 C49 59.9(2) . . . . ? C1 O1 Mn1 N9 -116.5(2) . . . 1_655 ? C16 O2 Mn1 O1 150.6(2) . . . . ? C16 O2 Mn1 N2 -27.9(2) . . . . ? C16 O2 Mn1 N1 -34.0(7) . . . . ? C16 O2 Mn1 C49 -118.9(2) . . . . ? C16 O2 Mn1 N9 57.2(2) . . . 1_655 ? C10 N2 Mn1 O1 -156.3(5) . . . . ? C9 N2 Mn1 O1 31.6(7) . . . . ? C10 N2 Mn1 O2 13.6(3) . . . . ? C9 N2 Mn1 O2 -158.5(2) . . . . ? C10 N2 Mn1 N1 -167.3(3) . . . . ? C9 N2 Mn1 N1 20.5(2) . . . . ? C10 N2 Mn1 C49 108.0(3) . . . . ? C9 N2 Mn1 C49 -64.1(2) . . . . ? C10 N2 Mn1 N9 -75.1(3) . . . 1_655 ? C9 N2 Mn1 N9 112.8(2) . . . 1_655 ? C7 N1 Mn1 O1 17.3(3) . . . . ? C8 N1 Mn1 O1 -168.48(18) . . . . ? C7 N1 Mn1 O2 -158.2(5) . . . . ? C8 N1 Mn1 O2 16.0(7) . . . . ? C7 N1 Mn1 N2 -164.3(3) . . . . ? C8 N1 Mn1 N2 9.90(18) . . . . ? C7 N1 Mn1 C49 -72.5(3) . . . . ? C8 N1 Mn1 C49 101.67(18) . . . . ? C7 N1 Mn1 N9 110.9(3) . . . 1_655 ? C8 N1 Mn1 N9 -74.95(19) . . . 1_655 ? N7 C49 Mn1 O1 -37.5(15) . . . . ? N7 C49 Mn1 O2 -135.2(15) . . . . ? N7 C49 Mn1 N2 134.1(15) . . . . ? N7 C49 Mn1 N1 53.7(15) . . . . ? N7 C49 Mn1 N9 95.9(17) . . . 1_655 ? C17 O3 Cr2 O4 166.13(17) . . . . ? C17 O3 Cr2 N4 -10.5(8) . . . . ? C17 O3 Cr2 N3 -17.65(19) . . . . ? C17 O3 Cr2 C50 71.56(19) . . . . ? C17 O3 Cr2 N7 -108.82(19) . . . . ? C32 O4 Cr2 O3 150.7(2) . . . . ? C32 O4 Cr2 N4 -29.7(2) . . . . ? C32 O4 Cr2 N3 -20.4(4) . . . . ? C32 O4 Cr2 C50 -118.7(2) . . . . ? C32 O4 Cr2 N7 61.1(2) . . . . ? C26 N4 Cr2 O3 -164.5(6) . . . . ? C25 N4 Cr2 O3 11.4(8) . . . . ? C26 N4 Cr2 O4 18.8(3) . . . . ? C25 N4 Cr2 O4 -165.27(17) . . . . ? C26 N4 Cr2 N3 -157.2(3) . . . . ? C25 N4 Cr2 N3 18.74(16) . . . . ? C26 N4 Cr2 C50 113.5(3) . . . . ? C25 N4 Cr2 C50 -70.53(17) . . . . ? C26 N4 Cr2 N7 -66.1(3) . . . . ? C25 N4 Cr2 N7 109.89(17) . . . . ? C23 N3 Cr2 O3 16.7(2) . . . . ? C24 N3 Cr2 O3 -174.49(19) . . . . ? C23 N3 Cr2 O4 -171.80(19) . . . . ? C24 N3 Cr2 O4 -2.9(3) . . . . ? C23 N3 Cr2 N4 -162.5(2) . . . . ? C24 N3 Cr2 N4 6.36(19) . . . . ? C23 N3 Cr2 C50 -72.3(2) . . . . ? C24 N3 Cr2 C50 96.5(2) . . . . ? C23 N3 Cr2 N7 108.1(2) . . . . ? C24 N3 Cr2 N7 -83.1(2) . . . . ? N8 C50 Cr2 O3 -65(3) . . . . ? N8 C50 Cr2 O4 -175(3) . . . . ? N8 C50 Cr2 N4 108(3) . . . . ? N8 C50 Cr2 N3 30(3) . . . . ? N8 C50 Cr2 N7 160(32) . . . . ? C49 N7 Cr2 O3 -121.8(13) . . . . ? C49 N7 Cr2 O4 -12.2(13) . . . . ? C49 N7 Cr2 N4 64.8(13) . . . . ? C49 N7 Cr2 N3 143.1(13) . . . . ? C49 N7 Cr2 C50 13(12) . . . . ? C33 O5 Mn3 O6 169.8(2) . . . . ? C33 O5 Mn3 N6 15.4(11) . . . . ? C33 O5 Mn3 N5 -12.7(2) . . . . ? C33 O5 Mn3 C51 -102.8(2) . . . . ? C33 O5 Mn3 N8 76.2(2) . . . . ? C48 O6 Mn3 O5 155.68(19) . . . . ? C48 O6 Mn3 N6 -26.8(2) . . . . ? C48 O6 Mn3 N5 -1.0(9) . . . . ? C48 O6 Mn3 C51 59.8(2) . . . . ? C48 O6 Mn3 N8 -116.7(2) . . . . ? C42 N6 Mn3 O5 171.3(9) . . . . ? C41 N6 Mn3 O5 -11.1(11) . . . . ? C42 N6 Mn3 O6 16.8(3) . . . . ? C41 N6 Mn3 O6 -165.55(18) . . . . ? C42 N6 Mn3 N5 -160.4(3) . . . . ? C41 N6 Mn3 N5 17.20(18) . . . . ? C42 N6 Mn3 C51 -70.1(3) . . . . ? C41 N6 Mn3 C51 107.48(19) . . . . ? C42 N6 Mn3 N8 110.6(3) . . . . ? C41 N6 Mn3 N8 -71.76(19) . . . . ? C39 N5 Mn3 O5 5.1(3) . . . . ? C40 N5 Mn3 O5 -170.45(17) . . . . ? C39 N5 Mn3 O6 161.8(7) . . . . ? C40 N5 Mn3 O6 -13.7(9) . . . . ? C39 N5 Mn3 N6 -172.3(3) . . . . ? C40 N5 Mn3 N6 12.22(17) . . . . ? C39 N5 Mn3 C51 101.1(3) . . . . ? C40 N5 Mn3 C51 -74.41(18) . . . . ? C39 N5 Mn3 N8 -82.3(3) . . . . ? C40 N5 Mn3 N8 102.23(18) . . . . ? N9 C51 Mn3 O5 29.3(17) . . . . ? N9 C51 Mn3 O6 123.4(17) . . . . ? N9 C51 Mn3 N6 -145.7(17) . . . . ? N9 C51 Mn3 N5 -62.1(17) . . . . ? N9 C51 Mn3 N8 -133.3(18) . . . . ? C50 N8 Mn3 O5 -68.7(9) . . . . ? C50 N8 Mn3 O6 -162.9(9) . . . . ? C50 N8 Mn3 N6 106.4(9) . . . . ? C50 N8 Mn3 N5 22.8(9) . . . . ? C50 N8 Mn3 C51 94.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.204 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.054 data_2 _database_code_depnum_ccdc_archive 'CCDC 899930' #TrackingRef '13706_web_deposit_cif_file_1_XiaoPingShen_1346742789.[Mn(salpn)]3[Cr(salen)(CN)2] .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C105 H90 Cr3 Mn3 N18 O12, 4(H2 O)' _chemical_formula_sum 'C105 H98 Cr3 Mn3 N18 O16' _chemical_formula_weight 2188.83 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.946(3) _cell_length_b 20.452(2) _cell_length_c 16.900(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.377(3) _cell_angle_gamma 90.00 _cell_volume 5507.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3719 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 23.18 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2258 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD' _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 40608 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10695 _reflns_number_gt 7870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.99P] 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 10695 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.47649(19) 0.12001(16) 0.85157(18) 0.0379(7) Uani 1 1 d . B . C2 C 0.4949(2) 0.07799(17) 0.7904(2) 0.0442(8) Uani 1 1 d . . . H2 H 0.4758 0.0870 0.7388 0.053 Uiso 1 1 calc R . . C3 C 0.5428(2) 0.02179(17) 0.8072(2) 0.0437(8) Uani 1 1 d . . . H3 H 0.5551 -0.0069 0.7665 0.052 Uiso 1 1 calc R . . C4 C 0.5717(2) 0.00887(16) 0.8833(2) 0.0431(8) Uani 1 1 d . . . H4 H 0.6073 -0.0264 0.8939 0.052 Uiso 1 1 calc R . . C5 C 0.5472(2) 0.04901(16) 0.9439(2) 0.0405(8) Uani 1 1 d . . . H5 H 0.5602 0.0373 0.9961 0.049 Uiso 1 1 calc R . . C6 C 0.5033(2) 0.10659(15) 0.92794(19) 0.0379(7) Uani 1 1 d . . . C7 C 0.4805(2) 0.14779(16) 0.99583(18) 0.0379(7) Uani 1 1 d . . . H7 H 0.4968 0.1329 1.0461 0.045 Uiso 1 1 calc R . . C8 C 0.4202(2) 0.24026(17) 1.0621(2) 0.0416(8) Uani 1 1 d . . . H8C H 0.4460 0.2226 1.1098 0.050 Uiso 0.50 1 d PR A 2 H8 H 0.3588 0.2392 1.0630 0.050 Uiso 1 1 d R . . C9 C 0.4420(2) 0.31235(16) 1.0514(2) 0.0393(8) Uani 1 1 d . B . H9A H 0.4123 0.3399 1.0877 0.047 Uiso 1 1 calc R . . H9B H 0.5019 0.3199 1.0589 0.047 Uiso 1 1 calc R . . C10 C 0.3767(2) 0.37691(16) 0.95579(18) 0.0355(7) Uani 1 1 d . B . H10 H 0.3705 0.4051 0.9984 0.043 Uiso 1 1 calc R . . C11 C 0.34171(19) 0.39877(16) 0.87510(19) 0.0364(7) Uani 1 1 d . . . C12 C 0.2943(2) 0.45561(16) 0.8735(2) 0.0382(7) Uani 1 1 d . . . H12 H 0.2885 0.4795 0.9197 0.046 Uiso 1 1 calc R . . C13 C 0.25525(18) 0.47712(16) 0.8030(2) 0.0386(7) Uani 1 1 d . . . H13 H 0.2226 0.5148 0.8026 0.046 Uiso 1 1 calc R . . C14 C 0.2648(2) 0.44257(14) 0.73329(18) 0.0351(7) Uani 1 1 d . . . H14 H 0.2398 0.4578 0.6861 0.042 Uiso 1 1 calc R . . C15 C 0.31158(19) 0.38525(17) 0.73387(18) 0.0371(7) Uani 1 1 d . . . H15 H 0.3171 0.3618 0.6872 0.044 Uiso 1 1 calc R . . C16 C 0.3502(2) 0.36278(16) 0.80399(18) 0.0362(7) Uani 1 1 d . B . C17 C 0.4508(4) 0.2190(3) 1.1465(4) 0.0399(15) Uani 0.50 1 d P B 1 H17A H 0.4376 0.1738 1.1542 0.060 Uiso 0.50 1 calc PR B 1 H17B H 0.4233 0.2451 1.1849 0.060 Uiso 0.50 1 calc PR B 1 H17C H 0.5104 0.2252 1.1525 0.060 Uiso 0.50 1 calc PR B 1 C18 C 0.1602(2) 0.28840(16) 1.0894(2) 0.0392(7) Uani 1 1 d . D . C19 C 0.1980(2) 0.26723(17) 1.1610(2) 0.0420(8) Uani 1 1 d . . . H19 H 0.1918 0.2241 1.1771 0.050 Uiso 1 1 calc R . . C20 C 0.2450(2) 0.31056(17) 1.20821(18) 0.0385(7) Uani 1 1 d . . . H20 H 0.2693 0.2965 1.2562 0.046 Uiso 1 1 calc R . . C21 C 0.2555(2) 0.37428(17) 1.18396(19) 0.0396(7) Uani 1 1 d . . . H21 H 0.2873 0.4029 1.2157 0.047 Uiso 1 1 calc R . . C22 C 0.21918(19) 0.39641(16) 1.11244(18) 0.0360(7) Uani 1 1 d . . . H22 H 0.2266 0.4395 1.0965 0.043 Uiso 1 1 calc R . . C23 C 0.17144(17) 0.35303(16) 1.06497(18) 0.0325(7) Uani 1 1 d . . . C24 C 0.13934(19) 0.38077(17) 0.98603(18) 0.0358(7) Uani 1 1 d . D . H24 H 0.1480 0.4249 0.9762 0.043 Uiso 1 1 calc R . . C25 C 0.0749(2) 0.38272(16) 0.86068(19) 0.0413(8) Uani 1 1 d . D . H25A H 0.1061 0.4231 0.8558 0.050 Uiso 1 1 calc R . . H25B H 0.0154 0.3924 0.8597 0.050 Uiso 1 1 calc R . . C26 C 0.0961(2) 0.33376(18) 0.7949(2) 0.0472(8) Uani 1 1 d . . . H26A H 0.0707 0.3456 0.7445 0.057 Uiso 0.50 1 d PR C 1 H26 H 0.1575 0.3339 0.7946 0.057 Uiso 1 1 d R . . C27 C 0.0342(2) 0.22440(17) 0.7721(2) 0.0402(8) Uani 1 1 d . . . H27 H 0.0190 0.2394 0.7216 0.048 Uiso 1 1 calc R D . C28 C 0.0111(2) 0.15928(18) 0.7884(2) 0.0459(8) Uani 1 1 d . D . C29 C -0.0231(2) 0.12104(17) 0.7261(2) 0.0438(8) Uani 1 1 d . . . H29 H -0.0326 0.1399 0.6765 0.053 Uiso 1 1 calc R D . C30 C -0.0426(2) 0.05696(18) 0.7369(2) 0.0462(8) Uani 1 1 d . D . H30 H -0.0649 0.0313 0.6957 0.055 Uiso 1 1 calc R . . C31 C -0.0275(2) 0.03202(17) 0.8118(2) 0.0401(8) Uani 1 1 d . . . H31 H -0.0416 -0.0116 0.8195 0.048 Uiso 1 1 calc R D . C32 C 0.0051(2) 0.06389(16) 0.8742(2) 0.0402(8) Uani 1 1 d . D . H32 H 0.0141 0.0435 0.9230 0.048 Uiso 1 1 calc R . . C33 C 0.0254(2) 0.12993(15) 0.86282(19) 0.0375(7) Uani 1 1 d . . . C34 C 0.0731(5) 0.3641(4) 0.7126(4) 0.0478(17) Uani 0.50 1 d P D 2 H34A H 0.0732 0.3289 0.6749 0.072 Uiso 0.50 1 d PR D 2 H34B H 0.1109 0.3977 0.6967 0.072 Uiso 0.50 1 d PR D 2 H34C H 0.0174 0.3817 0.7147 0.072 Uiso 0.50 1 d PR D 2 C35 C -0.1838(2) 0.33424(16) 0.77947(19) 0.0376(7) Uani 1 1 d . F . C36 C -0.1544(2) 0.39272(15) 0.74903(19) 0.0388(7) Uani 1 1 d . . . H36 H -0.1648 0.4321 0.7744 0.047 Uiso 1 1 calc R . . C37 C -0.1092(2) 0.39192(16) 0.68030(18) 0.0392(7) Uani 1 1 d . . . H37 H -0.0905 0.4310 0.6592 0.047 Uiso 1 1 calc R . . C38 C -0.0921(2) 0.33383(16) 0.6433(2) 0.0389(8) Uani 1 1 d . . . H38 H -0.0607 0.3337 0.5981 0.047 Uiso 1 1 calc R . . C39 C -0.12146(18) 0.27529(15) 0.67350(18) 0.0312(6) Uani 1 1 d . . . H39 H -0.1102 0.2361 0.6481 0.037 Uiso 1 1 calc R . . C40 C -0.1682(2) 0.27516(16) 0.74225(18) 0.0355(7) Uani 1 1 d . . . C41 C -0.1924(2) 0.20810(16) 0.77210(19) 0.0364(7) Uani 1 1 d . F . H41 H -0.1817 0.1719 0.7407 0.044 Uiso 1 1 calc R . . C42 C -0.2452(2) 0.12900(16) 0.85460(19) 0.0411(8) Uani 1 1 d . F . H42A H -0.2119 0.0992 0.8242 0.049 Uiso 1 1 calc R . . H42B H -0.3043 0.1193 0.8448 0.049 Uiso 1 1 calc R . . C43 C -0.2206(2) 0.12576(16) 0.94326(18) 0.0383(7) Uani 1 1 d . . . H43A H -0.2467 0.0883 0.9659 0.046 Uiso 0.50 1 d PR E 2 H43B H -0.1601 0.1214 0.9501 0.046 Uiso 1 1 d R . . C44 C -0.28692(19) 0.18312(16) 1.05029(18) 0.0351(7) Uani 1 1 d . . . H44 H -0.2961 0.1420 1.0719 0.042 Uiso 1 1 calc R F . C45 C -0.3177(2) 0.23995(17) 1.0945(2) 0.0397(8) Uani 1 1 d . F . C46 C -0.3626(2) 0.22735(18) 1.16256(18) 0.0424(8) Uani 1 1 d . . . H46 H -0.3745 0.1845 1.1765 0.051 Uiso 1 1 calc R F . C47 C -0.3895(2) 0.27850(18) 1.2090(2) 0.0436(8) Uani 1 1 d . F . H47 H -0.4200 0.2700 1.2536 0.052 Uiso 1 1 calc R . . C48 C -0.37054(18) 0.34285(17) 1.18858(18) 0.0358(7) Uani 1 1 d . . . H48 H -0.3881 0.3774 1.2196 0.043 Uiso 1 1 calc R F . C49 C -0.32475(19) 0.35497(16) 1.12088(18) 0.0347(7) Uani 1 1 d . F . H49 H -0.3119 0.3978 1.1072 0.042 Uiso 1 1 calc R . . C50 C -0.2984(2) 0.30346(16) 1.07402(18) 0.0389(8) Uani 1 1 d . . . C51 C -0.2537(5) 0.0674(3) 0.9795(4) 0.0436(16) Uani 0.50 1 d P F 1 H51B H -0.3138 0.0703 0.9798 0.065 Uiso 0.50 1 calc PR F 1 H51C H -0.2313 0.0637 1.0328 0.065 Uiso 0.50 1 calc PR F 1 H51A H -0.2381 0.0297 0.9497 0.065 Uiso 0.50 1 calc PR F 1 N1 N 0.44081(16) 0.20154(13) 0.99184(14) 0.0338(6) Uani 1 1 d . . . N2 N 0.41316(16) 0.32367(13) 0.96890(15) 0.0354(6) Uani 1 1 d . . . N3 N 0.10144(16) 0.34697(13) 0.93288(15) 0.0336(6) Uani 1 1 d . . . N4 N 0.07430(17) 0.26698(13) 0.81841(16) 0.0385(6) Uani 1 1 d . . . N5 N -0.22578(17) 0.19901(13) 0.83609(15) 0.0369(6) Uani 1 1 d . . . N6 N -0.24832(16) 0.18497(14) 0.98421(15) 0.0383(6) Uani 1 1 d . . . O1 O 0.43450(13) 0.16873(10) 0.82651(12) 0.0332(5) Uani 1 1 d . . . O2 O 0.39412(13) 0.31112(10) 0.79905(13) 0.0357(5) Uani 1 1 d . . . O3 O 0.11582(13) 0.24542(10) 1.05170(13) 0.0349(5) Uani 1 1 d . . . O4 O 0.05200(15) 0.15579(12) 0.92460(14) 0.0451(6) Uani 1 1 d . . . O5 O -0.22726(14) 0.34019(11) 0.84154(13) 0.0395(5) Uani 1 1 d . . . O6 O -0.26201(15) 0.32268(11) 1.01471(13) 0.0416(5) Uani 1 1 d . . . O7 O 0.2096(4) 0.1006(3) 0.9954(3) 0.0422(14) Uani 0.40 1 d P . . H7D H 0.2550 0.1036 0.9710 0.051 Uiso 0.40 1 d PR . . H7B H 0.1681 0.1054 0.9627 0.063 Uiso 0.40 1 d PR . . O8 O 0.3309(3) 0.5006(3) 0.3036(3) 0.0403(13) Uani 0.40 1 d P . . H8A H 0.2855 0.5206 0.2911 0.060 Uiso 0.40 1 d PR . . H8B H 0.3696 0.5283 0.3137 0.060 Uiso 0.40 1 d PR . . O9 O 0.1024(4) 0.5323(3) 0.9996(4) 0.0461(14) Uani 0.40 1 d P . . H9C H 0.1248 0.5591 0.9684 0.069 Uiso 0.40 1 d PR . . H9E H 0.0546 0.5466 1.0119 0.069 Uiso 0.40 1 d PR . . O10 O 0.4170(4) 0.5534(3) 0.1651(3) 0.0459(15) Uani 0.40 1 d P . . H10B H 0.4640 0.5547 0.1433 0.069 Uiso 0.40 1 d PR . . H10C H 0.3797 0.5391 0.1321 0.069 Uiso 0.40 1 d PR . . O11 O 0.5745(4) 0.4228(3) 0.9667(3) 0.0444(14) Uani 0.40 1 d P . . H11B H 0.6272 0.4255 0.9756 0.067 Uiso 0.40 1 d PR . . H11C H 0.5595 0.4495 0.9302 0.067 Uiso 0.40 1 d PR . . Mn1 Mn 0.42061(3) 0.25103(3) 0.89024(3) 0.03604(14) Uani 0.50 1 d P . 1 Cr2 Cr 0.09033(3) 0.24923(2) 0.93560(3) 0.03639(14) Uani 0.50 1 d P . 1 Mn3 Mn -0.24252(3) 0.26675(3) 0.91960(3) 0.03649(14) Uani 0.50 1 d P . 1 N7 N 0.28598(18) 0.23688(14) 0.90336(18) 0.0358(6) Uani 0.50 1 d P . 1 N8 N -0.10887(19) 0.26340(14) 0.94435(18) 0.0374(7) Uani 0.50 1 d P . 1 N9 N -0.37425(18) 0.26454(14) 0.89081(18) 0.0376(7) Uani 0.50 1 d P . 1 C52 C 0.2159(2) 0.23964(15) 0.90894(17) 0.0389(7) Uani 0.50 1 d P . 1 C53 C -0.03510(19) 0.26012(14) 0.95356(18) 0.0363(6) Uani 0.50 1 d P . 1 C54 C -0.45040(19) 0.26298(14) 0.88791(17) 0.0363(6) Uani 0.50 1 d P . 1 Cr1 Cr 0.42061(3) 0.25103(3) 0.89024(3) 0.03604(14) Uani 0.50 1 d P . 2 Mn2 Mn 0.09033(3) 0.24923(2) 0.93560(3) 0.03639(14) Uani 0.50 1 d P . 2 Cr3 Cr -0.24252(3) 0.26675(3) 0.91960(3) 0.03649(14) Uani 0.50 1 d P . 2 C52' C 0.28598(18) 0.23688(14) 0.90336(18) 0.0358(6) Uani 0.50 1 d P . 2 C53' C -0.10887(19) 0.26340(14) 0.94435(18) 0.0374(7) Uani 0.50 1 d P . 2 C54' C -0.37425(18) 0.26454(14) 0.89081(18) 0.0376(7) Uani 0.50 1 d P . 2 N7' N 0.2159(2) 0.23964(15) 0.90894(17) 0.0389(7) Uani 0.50 1 d P . 2 N8' N -0.03510(19) 0.26012(14) 0.95356(18) 0.0363(6) Uani 0.50 1 d P . 2 N9' N -0.45040(19) 0.26298(14) 0.88791(17) 0.0363(6) Uani 0.50 1 d P . 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 C1 0.0288(17) 0.0501(19) 0.0358(17) 0.0103(14) 0.0153(13) 0.0124(14) C2 0.042(2) 0.0448(19) 0.0441(19) -0.0030(15) -0.0161(15) 0.0076(15) C3 0.041(2) 0.0438(19) 0.0467(19) -0.0050(15) 0.0077(15) 0.0069(15) C4 0.0400(19) 0.0363(17) 0.054(2) 0.0130(15) 0.0123(16) 0.0208(14) C5 0.0414(19) 0.0386(18) 0.0427(18) 0.0112(14) 0.0166(15) 0.0080(14) C6 0.0402(19) 0.0325(16) 0.0402(18) -0.0018(13) -0.0083(14) 0.0079(13) C7 0.0419(19) 0.0465(19) 0.0262(15) 0.0099(13) 0.0112(13) 0.0008(15) C8 0.0388(19) 0.049(2) 0.0363(18) -0.0022(14) -0.0110(14) 0.0148(15) C9 0.0282(17) 0.0424(18) 0.0466(19) -0.0083(14) -0.0094(14) 0.0168(13) C10 0.0379(18) 0.0401(18) 0.0291(15) 0.0097(13) 0.0097(13) 0.0008(14) C11 0.0260(16) 0.0406(17) 0.0414(18) -0.0052(14) -0.0107(13) 0.0064(13) C12 0.0355(18) 0.0373(17) 0.0416(18) -0.0053(14) -0.0027(14) 0.0077(13) C13 0.0194(15) 0.0439(18) 0.052(2) 0.0024(15) -0.0021(14) 0.0108(13) C14 0.0368(18) 0.0314(15) 0.0360(16) 0.0049(13) -0.0136(13) -0.0104(13) C15 0.0263(16) 0.057(2) 0.0276(15) -0.0042(14) 0.0025(12) 0.0099(14) C16 0.0313(17) 0.0472(19) 0.0299(16) -0.0015(13) -0.0012(13) 0.0080(14) C17 0.034(4) 0.049(4) 0.036(3) -0.001(3) -0.011(3) -0.016(3) C18 0.0354(18) 0.0416(18) 0.0401(18) -0.0079(14) -0.0050(14) 0.0009(14) C19 0.0334(18) 0.0455(19) 0.0456(19) 0.0060(15) -0.0152(15) -0.0150(14) C20 0.0339(18) 0.053(2) 0.0282(16) 0.0026(14) -0.0106(13) -0.0082(14) C21 0.0320(17) 0.048(2) 0.0378(17) 0.0002(14) -0.0042(13) -0.0084(14) C22 0.0322(17) 0.0421(18) 0.0330(16) 0.0012(13) -0.0062(13) -0.0159(13) C23 0.0145(14) 0.0474(18) 0.0352(16) -0.0036(13) -0.0056(12) -0.0141(12) C24 0.0239(15) 0.0504(19) 0.0332(16) -0.0023(14) 0.0017(12) -0.0108(13) C25 0.044(2) 0.0357(17) 0.0439(19) 0.0084(14) -0.0077(15) -0.0081(14) C26 0.046(2) 0.054(2) 0.0408(19) -0.0021(16) -0.0111(16) -0.0065(16) C27 0.0325(18) 0.050(2) 0.0367(17) -0.0019(15) -0.0162(14) -0.0007(14) C28 0.045(2) 0.050(2) 0.0423(19) 0.0055(15) -0.0038(16) -0.0110(16) C29 0.043(2) 0.046(2) 0.0417(19) 0.0062(15) -0.0066(15) 0.0077(15) C30 0.039(2) 0.052(2) 0.046(2) -0.0079(16) -0.0041(16) -0.0085(16) C31 0.0340(18) 0.0395(18) 0.0460(19) -0.0049(14) -0.0065(15) 0.0063(14) C32 0.0374(18) 0.0414(18) 0.0413(18) 0.0055(14) -0.0059(15) 0.0054(14) C33 0.0405(19) 0.0359(17) 0.0368(17) -0.0124(13) 0.0093(14) 0.0067(14) C34 0.053(4) 0.053(4) 0.036(4) -0.006(3) -0.018(3) 0.003(3) C35 0.0288(16) 0.0424(18) 0.0422(18) -0.0090(14) 0.0075(14) -0.0074(13) C36 0.046(2) 0.0296(16) 0.0413(18) -0.0109(13) 0.0052(15) 0.0053(14) C37 0.049(2) 0.0344(16) 0.0353(17) -0.0043(13) 0.0137(15) 0.0071(14) C38 0.0296(17) 0.0470(19) 0.0411(18) -0.0155(14) 0.0147(14) -0.0101(14) C39 0.0231(15) 0.0339(16) 0.0352(16) -0.0082(13) -0.0145(12) 0.0051(12) C40 0.0319(17) 0.0398(17) 0.0339(16) -0.0097(13) -0.0106(13) -0.0057(13) C41 0.0317(17) 0.0417(18) 0.0351(17) -0.0030(13) -0.0096(14) 0.0031(13) C42 0.0364(18) 0.0453(19) 0.0397(18) 0.0013(14) -0.0189(14) -0.0168(14) C43 0.0409(19) 0.0433(18) 0.0298(16) 0.0030(13) -0.0077(13) -0.0042(14) C44 0.0298(16) 0.0402(17) 0.0351(16) 0.0011(13) -0.0027(13) 0.0042(13) C45 0.0279(17) 0.047(2) 0.0440(19) -0.0102(15) -0.0009(14) -0.0121(14) C46 0.043(2) 0.055(2) 0.0282(16) 0.0020(14) -0.0069(14) 0.0068(16) C47 0.046(2) 0.049(2) 0.0351(17) 0.0099(15) -0.0015(15) -0.0018(16) C48 0.0200(15) 0.0500(19) 0.0373(17) 0.0104(14) -0.0003(12) -0.0034(13) C49 0.0302(16) 0.0401(17) 0.0337(16) -0.0050(13) -0.0004(13) 0.0016(13) C50 0.052(2) 0.0359(17) 0.0277(16) -0.0165(13) -0.0097(14) 0.0021(15) C51 0.046(4) 0.049(4) 0.035(3) 0.010(3) -0.002(3) -0.002(3) N1 0.0260(13) 0.0453(15) 0.0294(13) 0.0008(11) -0.0093(10) 0.0002(11) N2 0.0256(14) 0.0430(16) 0.0372(14) -0.0059(12) -0.0042(11) -0.0084(11) N3 0.0263(13) 0.0379(14) 0.0354(14) 0.0005(11) -0.0136(11) 0.0050(10) N4 0.0384(15) 0.0403(15) 0.0357(14) -0.0158(12) -0.0123(12) 0.0037(12) N5 0.0341(15) 0.0428(16) 0.0331(14) -0.0055(11) -0.0053(11) -0.0008(12) N6 0.0286(14) 0.0501(16) 0.0354(15) -0.0005(12) -0.0079(11) 0.0039(12) O1 0.0301(11) 0.0388(12) 0.0294(11) -0.0010(9) -0.0132(9) -0.0040(9) O2 0.0293(11) 0.0381(12) 0.0390(12) -0.0030(9) -0.0084(9) -0.0026(9) O3 0.0290(11) 0.0338(11) 0.0411(12) 0.0130(9) -0.0058(9) -0.0024(9) O4 0.0424(14) 0.0471(14) 0.0451(13) -0.0137(11) -0.0077(11) 0.0048(11) O5 0.0350(12) 0.0424(13) 0.0412(12) -0.0078(10) 0.0029(10) 0.0046(10) O6 0.0459(14) 0.0460(13) 0.0318(12) -0.0063(10) -0.0112(10) 0.0032(11) O7 0.048(4) 0.051(3) 0.027(3) -0.021(2) -0.014(2) 0.002(3) O8 0.025(3) 0.046(3) 0.048(3) 0.017(3) -0.013(2) -0.008(2) O9 0.037(3) 0.043(3) 0.058(4) -0.007(3) -0.005(3) -0.005(3) O10 0.047(4) 0.054(4) 0.036(3) -0.017(3) -0.011(3) 0.005(3) O11 0.043(3) 0.049(3) 0.039(3) -0.012(3) -0.023(3) 0.001(3) Mn1 0.0244(3) 0.0434(3) 0.0404(3) -0.0004(2) 0.0025(2) 0.0150(2) Cr2 0.0373(3) 0.0369(3) 0.0345(3) -0.0053(2) -0.0051(2) 0.0132(2) Mn3 0.0255(3) 0.0485(3) 0.0360(3) -0.0091(2) 0.0072(2) -0.0146(2) N7 0.0276(16) 0.0352(16) 0.0433(17) 0.0019(12) -0.0154(13) -0.0031(11) N8 0.0349(17) 0.0347(16) 0.0421(17) -0.0003(12) -0.0054(13) -0.0016(12) N9 0.0280(16) 0.0427(17) 0.0415(16) -0.0203(13) -0.0073(13) 0.0092(12) C52 0.0370(18) 0.0435(17) 0.0356(16) -0.0195(13) -0.0065(13) 0.0060(13) C53 0.0342(17) 0.0331(15) 0.0411(16) 0.0033(12) -0.0058(13) 0.0036(12) C54 0.0337(17) 0.0410(16) 0.0338(15) -0.0072(12) -0.0050(12) 0.0003(12) Cr1 0.0244(3) 0.0434(3) 0.0404(3) -0.0004(2) 0.0025(2) 0.0150(2) Mn2 0.0373(3) 0.0369(3) 0.0345(3) -0.0053(2) -0.0051(2) 0.0132(2) Cr3 0.0255(3) 0.0485(3) 0.0360(3) -0.0091(2) 0.0072(2) -0.0146(2) C52' 0.0276(16) 0.0352(16) 0.0433(17) 0.0019(12) -0.0154(13) -0.0031(11) C53' 0.0349(17) 0.0347(16) 0.0421(17) -0.0003(12) -0.0054(13) -0.0016(12) C54' 0.0280(16) 0.0427(17) 0.0415(16) -0.0203(13) -0.0073(13) 0.0092(12) N7' 0.0370(18) 0.0435(17) 0.0356(16) -0.0195(13) -0.0065(13) 0.0060(13) N8' 0.0342(17) 0.0331(15) 0.0411(16) 0.0033(12) -0.0058(13) 0.0036(12) N9' 0.0337(17) 0.0410(16) 0.0338(15) -0.0072(12) -0.0050(12) 0.0003(12) _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 C1 O1 1.264(4) . ? C1 C6 1.370(4) . ? C1 C2 1.385(5) . ? C2 C3 1.402(5) . ? C2 H2 0.9300 . ? C3 C4 1.375(5) . ? C3 H3 0.9300 . ? C4 C5 1.381(5) . ? C4 H4 0.9300 . ? C5 C6 1.390(4) . ? C5 H5 0.9300 . ? C6 C7 1.481(4) . ? C7 N1 1.269(4) . ? C7 H7 0.9300 . ? C8 N1 1.476(4) . ? C8 C9 1.527(5) . ? C8 C17 1.549(7) . ? C8 H8C 0.9601 . ? C8 H8 0.9801 . ? C9 N2 1.469(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.250(4) . ? C10 C11 1.519(4) . ? C10 H10 0.9300 . ? C11 C12 1.386(4) . ? C11 C16 1.421(4) . ? C12 C13 1.392(5) . ? C12 H12 0.9300 . ? C13 C14 1.387(4) . ? C13 H13 0.9300 . ? C14 C15 1.389(4) . ? C14 H14 0.9300 . ? C15 C16 1.391(4) . ? C15 H15 0.9300 . ? C16 O2 1.272(4) . ? C17 H8C 0.6249 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O3 1.282(4) . ? C18 C23 1.398(5) . ? C18 C19 1.398(5) . ? C19 C20 1.390(4) . ? C19 H19 0.9300 . ? C20 C21 1.379(5) . ? C20 H20 0.9300 . ? C21 C22 1.394(4) . ? C21 H21 0.9300 . ? C22 C23 1.400(4) . ? C22 H22 0.9300 . ? C23 C24 1.519(4) . ? C24 N3 1.267(4) . ? C24 H24 0.9300 . ? C25 N3 1.470(4) . ? C25 C26 1.544(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N4 1.468(5) . ? C26 C34 1.554(7) . ? C26 H26A 0.9599 . ? C26 H26 0.9800 . ? C27 N4 1.319(4) . ? C27 C28 1.412(5) . ? C27 H27 0.9300 . ? C28 C29 1.403(5) . ? C28 C33 1.404(5) . ? C29 C30 1.361(5) . ? C29 H29 0.9300 . ? C30 C31 1.377(5) . ? C30 H30 0.9300 . ? C31 C32 1.327(5) . ? C31 H31 0.9300 . ? C32 C33 1.404(5) . ? C32 H32 0.9300 . ? C33 O4 1.230(4) . ? C34 H26A 0.6607 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 O5 1.287(4) . ? C35 C40 1.389(4) . ? C35 C36 1.391(5) . ? C36 C37 1.392(4) . ? C36 H36 0.9300 . ? C37 C38 1.375(4) . ? C37 H37 0.9300 . ? C38 C39 1.391(4) . ? C38 H38 0.9300 . ? C39 C40 1.406(4) . ? C39 H39 0.9300 . ? C40 C41 1.517(5) . ? C41 N5 1.239(4) . ? C41 H41 0.9300 . ? C42 N5 1.501(4) . ? C42 C43 1.535(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C51 1.451(7) . ? C43 N6 1.472(4) . ? C43 H43A 0.9598 . ? C43 H43B 0.9699 . ? C44 N6 1.298(4) . ? C44 C45 1.477(4) . ? C44 H44 0.9300 . ? C45 C50 1.382(5) . ? C45 C46 1.404(5) . ? C46 C47 1.386(5) . ? C46 H46 0.9300 . ? C47 C48 1.397(5) . ? C47 H47 0.9300 . ? C48 C49 1.405(4) . ? C48 H48 0.9300 . ? C49 C50 1.393(4) . ? C49 H49 0.9300 . ? C50 O6 1.243(4) . ? C51 H43A 0.4991 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C51 H51A 0.9600 . ? N1 Mn1 2.008(3) . ? N2 Mn1 2.000(3) . ? N3 Cr2 2.008(3) . ? N4 Cr2 2.019(3) . ? N5 Mn3 2.003(3) . ? N6 Mn3 2.002(3) . ? O1 Mn1 2.015(2) . ? O2 Mn1 2.003(2) . ? O3 Cr2 1.989(2) . ? O4 Cr2 2.013(2) . ? O5 Mn3 2.020(2) . ? O6 Mn3 2.008(2) . ? O7 H7D 0.8500 . ? O7 H7B 0.8501 . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? O9 H9C 0.8500 . ? O9 H9E 0.8499 . ? O10 H10B 0.8500 . ? O10 H10C 0.8501 . ? O11 H11B 0.8501 . ? O11 H11C 0.8501 . ? Mn1 C54 2.073(3) 1_655 ? Mn1 N7 2.187(3) . ? Cr2 C53 2.048(3) . ? Cr2 C52 2.079(3) . ? Mn3 N9 2.137(3) . ? Mn3 N8 2.156(3) . ? N7 C52 1.127(4) . ? N8 C53 1.182(4) . ? N9 C54 1.214(4) . ? C54 Mn1 2.073(3) 1_455 ? 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 O1 C1 C6 127.9(3) . . ? O1 C1 C2 111.4(3) . . ? C6 C1 C2 120.7(3) . . ? C1 C2 C3 119.3(3) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 121.1(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C7 122.6(3) . . ? C5 C6 C7 118.0(3) . . ? N1 C7 C6 126.1(3) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? N1 C8 C9 111.3(3) . . ? N1 C8 C17 121.2(4) . . ? C9 C8 C17 108.4(3) . . ? N1 C8 H8C 111.8 . . ? C9 C8 H8C 111.8 . . ? N1 C8 H8 104.8 . . ? C9 C8 H8 104.8 . . ? C17 C8 H8 104.8 . . ? H8C C8 H8 111.8 . . ? N2 C9 C8 101.6(3) . . ? N2 C9 H9A 111.5 . . ? C8 C9 H9A 111.5 . . ? N2 C9 H9B 111.5 . . ? C8 C9 H9B 111.5 . . ? H9A C9 H9B 109.3 . . ? N2 C10 C11 124.5(3) . . ? N2 C10 H10 117.8 . . ? C11 C10 H10 117.8 . . ? C12 C11 C16 119.3(3) . . ? C12 C11 C10 116.4(3) . . ? C16 C11 C10 124.2(3) . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? O2 C16 C15 116.4(3) . . ? O2 C16 C11 123.9(3) . . ? C15 C16 C11 119.7(3) . . ? C8 C17 H17A 109.5 . . ? H8C C17 H17A 103.2 . . ? C8 C17 H17B 109.5 . . ? H8C C17 H17B 124.6 . . ? C8 C17 H17C 109.5 . . ? H8C C17 H17C 99.8 . . ? O3 C18 C23 125.2(3) . . ? O3 C18 C19 115.3(3) . . ? C23 C18 C19 119.5(3) . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C18 C23 C22 120.2(3) . . ? C18 C23 C24 124.7(3) . . ? C22 C23 C24 115.0(3) . . ? N3 C24 C23 123.5(3) . . ? N3 C24 H24 118.2 . . ? C23 C24 H24 118.2 . . ? N3 C25 C26 102.2(3) . . ? N3 C25 H25A 111.3 . . ? C26 C25 H25A 111.3 . . ? N3 C25 H25B 111.3 . . ? C26 C25 H25B 111.3 . . ? H25A C25 H25B 109.2 . . ? N4 C26 C25 110.3(3) . . ? N4 C26 C34 124.3(4) . . ? C25 C26 C34 109.6(4) . . ? N4 C26 H26A 112.3 . . ? C25 C26 H26A 112.3 . . ? N4 C26 H26 104.6 . . ? C25 C26 H26 104.5 . . ? C34 C26 H26 101.1 . . ? H26A C26 H26 112.3 . . ? N4 C27 C28 129.2(3) . . ? N4 C27 H27 115.4 . . ? C28 C27 H27 115.4 . . ? C29 C28 C33 118.5(3) . . ? C29 C28 C27 118.4(3) . . ? C33 C28 C27 123.0(3) . . ? C30 C29 C28 121.4(3) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C31 116.6(3) . . ? C29 C30 H30 121.7 . . ? C31 C30 H30 121.7 . . ? C32 C31 C30 126.6(3) . . ? C32 C31 H31 116.7 . . ? C30 C31 H31 116.7 . . ? C31 C32 C33 116.7(3) . . ? C31 C32 H32 121.7 . . ? C33 C32 H32 121.7 . . ? O4 C33 C28 127.9(3) . . ? O4 C33 C32 111.8(3) . . ? C28 C33 C32 120.3(3) . . ? C26 C34 H34A 106.7 . . ? H26A C34 H34A 96.6 . . ? C26 C34 H34B 114.1 . . ? H26A C34 H34B 134.0 . . ? H34A C34 H34B 109.5 . . ? C26 C34 H34C 107.5 . . ? H26A C34 H34C 95.8 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O5 C35 C40 124.3(3) . . ? O5 C35 C36 114.9(3) . . ? C40 C35 C36 120.7(3) . . ? C35 C36 C37 119.5(3) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.2(3) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C35 C40 C39 118.9(3) . . ? C35 C40 C41 125.7(3) . . ? C39 C40 C41 115.3(3) . . ? N5 C41 C40 123.4(3) . . ? N5 C41 H41 118.3 . . ? C40 C41 H41 118.3 . . ? N5 C42 C43 101.4(2) . . ? N5 C42 H42A 111.5 . . ? C43 C42 H42A 111.5 . . ? N5 C42 H42B 111.5 . . ? C43 C42 H42B 111.5 . . ? H42A C42 H42B 109.3 . . ? C51 C43 N6 110.9(4) . . ? C51 C43 C42 111.3(4) . . ? N6 C43 C42 110.7(3) . . ? N6 C43 H43A 109.0 . . ? C42 C43 H43A 109.0 . . ? C51 C43 H43B 104.6 . . ? N6 C43 H43B 109.6 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.0 . . ? N6 C44 C45 126.3(3) . . ? N6 C44 H44 116.9 . . ? C45 C44 H44 116.9 . . ? C50 C45 C46 120.3(3) . . ? C50 C45 C44 122.1(3) . . ? C46 C45 C44 117.5(3) . . ? C47 C46 C45 120.4(3) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 119.7(3) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C47 C48 C49 119.5(3) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 120.6(3) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? O6 C50 C45 128.0(3) . . ? O6 C50 C49 112.4(3) . . ? C45 C50 C49 119.5(3) . . ? C43 C51 H51B 109.5 . . ? H43A C51 H51B 101.1 . . ? C43 C51 H51C 109.5 . . ? H43A C51 H51C 114.7 . . ? C43 C51 H51A 109.5 . . ? H43A C51 H51A 112.3 . . ? C7 N1 C8 123.3(3) . . ? C7 N1 Mn1 123.0(2) . . ? C8 N1 Mn1 112.6(2) . . ? C10 N2 C9 115.5(3) . . ? C10 N2 Mn1 124.7(2) . . ? C9 N2 Mn1 119.3(2) . . ? C24 N3 C25 115.4(3) . . ? C24 N3 Cr2 124.5(2) . . ? C25 N3 Cr2 119.5(2) . . ? C27 N4 C26 124.6(3) . . ? C27 N4 Cr2 120.1(2) . . ? C26 N4 Cr2 114.2(2) . . ? C41 N5 C42 115.2(3) . . ? C41 N5 Mn3 125.9(2) . . ? C42 N5 Mn3 118.6(2) . . ? C44 N6 C43 122.9(3) . . ? C44 N6 Mn3 121.9(2) . . ? C43 N6 Mn3 114.2(2) . . ? C1 O1 Mn1 123.2(2) . . ? C16 O2 Mn1 123.9(2) . . ? C18 O3 Cr2 123.3(2) . . ? C33 O4 Cr2 125.4(2) . . ? C35 O5 Mn3 123.1(2) . . ? C50 O6 Mn3 124.0(2) . . ? H7D O7 H7B 109.5 . . ? H8A O8 H8B 109.5 . . ? H9C O9 H9E 109.5 . . ? H10B O10 H10C 109.5 . . ? H11B O11 H11C 109.5 . . ? N2 Mn1 O2 92.25(10) . . ? N2 Mn1 N1 79.51(11) . . ? O2 Mn1 N1 171.45(10) . . ? N2 Mn1 O1 170.49(10) . . ? O2 Mn1 O1 97.22(9) . . ? N1 Mn1 O1 91.07(10) . . ? N2 Mn1 C54 90.65(11) . 1_655 ? O2 Mn1 C54 95.21(10) . 1_655 ? N1 Mn1 C54 87.22(11) . 1_655 ? O1 Mn1 C54 87.55(10) . 1_655 ? N2 Mn1 N7 86.86(11) . . ? O2 Mn1 N7 89.00(10) . . ? N1 Mn1 N7 88.28(11) . . ? O1 Mn1 N7 94.23(10) . . ? C54 Mn1 N7 175.19(11) 1_655 . ? O3 Cr2 N3 92.69(9) . . ? O3 Cr2 O4 95.90(9) . . ? N3 Cr2 O4 165.96(10) . . ? O3 Cr2 N4 170.78(10) . . ? N3 Cr2 N4 78.83(10) . . ? O4 Cr2 N4 93.12(10) . . ? O3 Cr2 C53 91.08(11) . . ? N3 Cr2 C53 89.01(11) . . ? O4 Cr2 C53 79.76(11) . . ? N4 Cr2 C53 92.36(12) . . ? O3 Cr2 C52 92.92(10) . . ? N3 Cr2 C52 90.13(11) . . ? O4 Cr2 C52 100.48(11) . . ? N4 Cr2 C52 83.59(12) . . ? C53 Cr2 C52 175.94(12) . . ? N6 Mn3 N5 79.45(11) . . ? N6 Mn3 O6 91.56(10) . . ? N5 Mn3 O6 170.98(11) . . ? N6 Mn3 O5 170.71(10) . . ? N5 Mn3 O5 91.77(10) . . ? O6 Mn3 O5 97.24(9) . . ? N6 Mn3 N9 92.25(12) . . ? N5 Mn3 N9 89.05(11) . . ? O6 Mn3 N9 90.63(10) . . ? O5 Mn3 N9 90.63(11) . . ? N6 Mn3 N8 86.29(11) . . ? N5 Mn3 N8 87.43(11) . . ? O6 Mn3 N8 92.72(11) . . ? O5 Mn3 N8 90.31(10) . . ? N9 Mn3 N8 176.38(11) . . ? C52 N7 Mn1 169.5(3) . . ? C53 N8 Mn3 176.1(3) . . ? C54 N9 Mn3 169.2(3) . . ? N7 C52 Cr2 171.9(3) . . ? N8 C53 Cr2 163.6(3) . . ? N9 C54 Mn1 173.7(3) . 1_455 ? 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 C1 C2 C3 178.7(3) . . . . ? C6 C1 C2 C3 -1.1(5) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C2 C3 C4 C5 5.3(5) . . . . ? C3 C4 C5 C6 -8.6(5) . . . . ? O1 C1 C6 C5 178.2(3) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? O1 C1 C6 C7 4.3(6) . . . . ? C2 C1 C6 C7 -176.0(3) . . . . ? C4 C5 C6 C1 6.9(5) . . . . ? C4 C5 C6 C7 -178.8(3) . . . . ? C1 C6 C7 N1 -6.1(6) . . . . ? C5 C6 C7 N1 179.9(3) . . . . ? N1 C8 C9 N2 41.7(3) . . . . ? C17 C8 C9 N2 177.4(4) . . . . ? N2 C10 C11 C12 172.4(3) . . . . ? N2 C10 C11 C16 -3.5(5) . . . . ? C16 C11 C12 C13 0.2(5) . . . . ? C10 C11 C12 C13 -175.9(3) . . . . ? C11 C12 C13 C14 -1.3(5) . . . . ? C12 C13 C14 C15 1.8(5) . . . . ? C13 C14 C15 C16 -1.1(5) . . . . ? C14 C15 C16 O2 -177.8(3) . . . . ? C14 C15 C16 C11 -0.1(5) . . . . ? C12 C11 C16 O2 178.1(3) . . . . ? C10 C11 C16 O2 -6.2(5) . . . . ? C12 C11 C16 C15 0.5(5) . . . . ? C10 C11 C16 C15 176.2(3) . . . . ? O3 C18 C19 C20 -177.5(3) . . . . ? C23 C18 C19 C20 1.3(5) . . . . ? C18 C19 C20 C21 -1.0(5) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? C20 C21 C22 C23 0.0(5) . . . . ? O3 C18 C23 C22 177.8(3) . . . . ? C19 C18 C23 C22 -0.9(5) . . . . ? O3 C18 C23 C24 -6.1(5) . . . . ? C19 C18 C23 C24 175.3(3) . . . . ? C21 C22 C23 C18 0.2(5) . . . . ? C21 C22 C23 C24 -176.3(3) . . . . ? C18 C23 C24 N3 -2.6(5) . . . . ? C22 C23 C24 N3 173.7(3) . . . . ? N3 C25 C26 N4 40.4(3) . . . . ? N3 C25 C26 C34 -179.2(4) . . . . ? N4 C27 C28 C29 -172.8(3) . . . . ? N4 C27 C28 C33 3.2(6) . . . . ? C33 C28 C29 C30 0.3(5) . . . . ? C27 C28 C29 C30 176.5(3) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C29 C30 C31 C32 -1.0(6) . . . . ? C30 C31 C32 C33 0.8(5) . . . . ? C29 C28 C33 O4 -177.4(3) . . . . ? C27 C28 C33 O4 6.6(6) . . . . ? C29 C28 C33 C32 -0.5(5) . . . . ? C27 C28 C33 C32 -176.5(3) . . . . ? C31 C32 C33 O4 177.3(3) . . . . ? C31 C32 C33 C28 0.0(5) . . . . ? O5 C35 C36 C37 -177.7(3) . . . . ? C40 C35 C36 C37 0.4(5) . . . . ? C35 C36 C37 C38 -1.4(5) . . . . ? C36 C37 C38 C39 1.5(5) . . . . ? C37 C38 C39 C40 -0.5(5) . . . . ? O5 C35 C40 C39 178.4(3) . . . . ? C36 C35 C40 C39 0.6(5) . . . . ? O5 C35 C40 C41 -5.9(5) . . . . ? C36 C35 C40 C41 176.2(3) . . . . ? C38 C39 C40 C35 -0.5(5) . . . . ? C38 C39 C40 C41 -176.6(3) . . . . ? C35 C40 C41 N5 -3.6(5) . . . . ? C39 C40 C41 N5 172.2(3) . . . . ? N5 C42 C43 C51 165.2(4) . . . . ? N5 C42 C43 N6 41.4(3) . . . . ? N6 C44 C45 C50 -8.4(5) . . . . ? N6 C44 C45 C46 176.1(3) . . . . ? C50 C45 C46 C47 1.2(5) . . . . ? C44 C45 C46 C47 176.7(3) . . . . ? C45 C46 C47 C48 -0.9(5) . . . . ? C46 C47 C48 C49 0.3(5) . . . . ? C47 C48 C49 C50 0.2(5) . . . . ? C46 C45 C50 O6 -177.2(3) . . . . ? C44 C45 C50 O6 7.5(6) . . . . ? C46 C45 C50 C49 -0.7(5) . . . . ? C44 C45 C50 C49 -176.0(3) . . . . ? C48 C49 C50 O6 177.0(3) . . . . ? C48 C49 C50 C45 0.0(5) . . . . ? C6 C7 N1 C8 -179.9(3) . . . . ? C6 C7 N1 Mn1 -12.7(5) . . . . ? C9 C8 N1 C7 132.7(3) . . . . ? C17 C8 N1 C7 3.5(6) . . . . ? C9 C8 N1 Mn1 -35.7(3) . . . . ? C17 C8 N1 Mn1 -164.9(3) . . . . ? C11 C10 N2 C9 -180.0(3) . . . . ? C11 C10 N2 Mn1 -8.3(4) . . . . ? C8 C9 N2 C10 139.2(3) . . . . ? C8 C9 N2 Mn1 -33.0(3) . . . . ? C23 C24 N3 C25 179.8(3) . . . . ? C23 C24 N3 Cr2 -8.8(4) . . . . ? C26 C25 N3 C24 138.6(3) . . . . ? C26 C25 N3 Cr2 -33.3(3) . . . . ? C28 C27 N4 C26 179.3(4) . . . . ? C28 C27 N4 Cr2 -12.7(5) . . . . ? C25 C26 N4 C27 134.7(3) . . . . ? C34 C26 N4 C27 1.4(6) . . . . ? C25 C26 N4 Cr2 -33.9(3) . . . . ? C34 C26 N4 Cr2 -167.2(4) . . . . ? C40 C41 N5 C42 179.7(3) . . . . ? C40 C41 N5 Mn3 -7.9(4) . . . . ? C43 C42 N5 C41 139.3(3) . . . . ? C43 C42 N5 Mn3 -33.7(3) . . . . ? C45 C44 N6 C43 -179.2(3) . . . . ? C45 C44 N6 Mn3 -11.7(4) . . . . ? C51 C43 N6 C44 9.1(5) . . . . ? C42 C43 N6 C44 133.2(3) . . . . ? C51 C43 N6 Mn3 -159.3(3) . . . . ? C42 C43 N6 Mn3 -35.2(3) . . . . ? C6 C1 O1 Mn1 15.8(5) . . . . ? C2 C1 O1 Mn1 -163.9(2) . . . . ? C15 C16 O2 Mn1 -156.6(2) . . . . ? C11 C16 O2 Mn1 25.7(4) . . . . ? C23 C18 O3 Cr2 24.5(4) . . . . ? C19 C18 O3 Cr2 -156.8(2) . . . . ? C28 C33 O4 Cr2 -3.9(5) . . . . ? C32 C33 O4 Cr2 178.9(2) . . . . ? C40 C35 O5 Mn3 24.5(4) . . . . ? C36 C35 O5 Mn3 -157.5(2) . . . . ? C45 C50 O6 Mn3 13.7(5) . . . . ? C49 C50 O6 Mn3 -163.0(2) . . . . ? C10 N2 Mn1 O2 19.4(3) . . . . ? C9 N2 Mn1 O2 -169.2(2) . . . . ? C10 N2 Mn1 N1 -158.3(3) . . . . ? C9 N2 Mn1 N1 13.1(2) . . . . ? C10 N2 Mn1 C54 114.6(3) . . . 1_655 ? C9 N2 Mn1 C54 -74.0(2) . . . 1_655 ? C10 N2 Mn1 N7 -69.5(3) . . . . ? C9 N2 Mn1 N7 101.9(2) . . . . ? C16 O2 Mn1 N2 -28.2(3) . . . . ? C16 O2 Mn1 O1 152.7(2) . . . . ? C16 O2 Mn1 C54 -119.1(3) . . . 1_655 ? C16 O2 Mn1 N7 58.6(3) . . . . ? C7 N1 Mn1 N2 -155.5(3) . . . . ? C8 N1 Mn1 N2 12.9(2) . . . . ? C7 N1 Mn1 O1 23.2(3) . . . . ? C8 N1 Mn1 O1 -168.4(2) . . . . ? C7 N1 Mn1 C54 -64.3(3) . . . 1_655 ? C8 N1 Mn1 C54 104.1(2) . . . 1_655 ? C7 N1 Mn1 N7 117.4(3) . . . . ? C8 N1 Mn1 N7 -74.2(2) . . . . ? C1 O1 Mn1 O2 157.2(2) . . . . ? C1 O1 Mn1 N1 -25.0(2) . . . . ? C1 O1 Mn1 C54 62.2(2) . . . 1_655 ? C1 O1 Mn1 N7 -113.3(2) . . . . ? C18 O3 Cr2 N3 -26.8(2) . . . . ? C18 O3 Cr2 O4 164.3(2) . . . . ? C18 O3 Cr2 C53 -115.9(2) . . . . ? C18 O3 Cr2 C52 63.5(3) . . . . ? C24 N3 Cr2 O3 19.2(3) . . . . ? C25 N3 Cr2 O3 -169.7(2) . . . . ? C24 N3 Cr2 O4 147.0(4) . . . . ? C25 N3 Cr2 O4 -41.9(6) . . . . ? C24 N3 Cr2 N4 -157.1(3) . . . . ? C25 N3 Cr2 N4 14.0(2) . . . . ? C24 N3 Cr2 C53 110.3(3) . . . . ? C25 N3 Cr2 C53 -78.6(2) . . . . ? C24 N3 Cr2 C52 -73.7(3) . . . . ? C25 N3 Cr2 C52 97.4(2) . . . . ? C33 O4 Cr2 O3 177.9(3) . . . . ? C33 O4 Cr2 N3 50.5(6) . . . . ? C33 O4 Cr2 N4 -3.9(3) . . . . ? C33 O4 Cr2 C53 87.9(3) . . . . ? C33 O4 Cr2 C52 -88.0(3) . . . . ? C27 N4 Cr2 N3 -157.2(3) . . . . ? C26 N4 Cr2 N3 11.9(2) . . . . ? C27 N4 Cr2 O4 11.1(3) . . . . ? C26 N4 Cr2 O4 -179.7(2) . . . . ? C27 N4 Cr2 C53 -68.7(3) . . . . ? C26 N4 Cr2 C53 100.5(2) . . . . ? C27 N4 Cr2 C52 111.3(3) . . . . ? C26 N4 Cr2 C52 -79.5(2) . . . . ? C44 N6 Mn3 N5 -156.3(3) . . . . ? C43 N6 Mn3 N5 12.2(2) . . . . ? C44 N6 Mn3 O6 23.0(3) . . . . ? C43 N6 Mn3 O6 -168.5(2) . . . . ? C44 N6 Mn3 N9 -67.7(3) . . . . ? C43 N6 Mn3 N9 100.8(2) . . . . ? C44 N6 Mn3 N8 115.6(3) . . . . ? C43 N6 Mn3 N8 -75.9(2) . . . . ? C41 N5 Mn3 N6 -158.2(3) . . . . ? C42 N5 Mn3 N6 13.9(2) . . . . ? C41 N5 Mn3 O5 18.7(3) . . . . ? C42 N5 Mn3 O5 -169.1(2) . . . . ? C41 N5 Mn3 N9 109.3(3) . . . . ? C42 N5 Mn3 N9 -78.5(2) . . . . ? C41 N5 Mn3 N8 -71.5(3) . . . . ? C42 N5 Mn3 N8 100.6(2) . . . . ? C50 O6 Mn3 N6 -24.7(3) . . . . ? C50 O6 Mn3 O5 158.2(3) . . . . ? C50 O6 Mn3 N9 67.5(3) . . . . ? C50 O6 Mn3 N8 -111.1(3) . . . . ? C35 O5 Mn3 N5 -26.7(3) . . . . ? C35 O5 Mn3 O6 153.5(2) . . . . ? C35 O5 Mn3 N9 -115.7(2) . . . . ? C35 O5 Mn3 N8 60.8(3) . . . . ? N2 Mn1 N7 C52 46.6(15) . . . . ? O2 Mn1 N7 C52 -45.7(15) . . . . ? N1 Mn1 N7 C52 126.2(15) . . . . ? O1 Mn1 N7 C52 -142.9(15) . . . . ? N5 Mn3 N9 C54 134.6(14) . . . . ? O6 Mn3 N9 C54 -36.4(14) . . . . ? O5 Mn3 N9 C54 -133.7(14) . . . . ? N3 Cr2 C53 N8 99.3(9) . . . . ? O4 Cr2 C53 N8 -72.3(9) . . . . ? N4 Cr2 C53 N8 20.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.576 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.071 data_3 _database_code_depnum_ccdc_archive 'CCDC 899931' #TrackingRef '16197_web_deposit_cif_file_0_XiaopingShen_1355494041.MnCr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H22 Cr Mn N8 O2' _chemical_formula_weight 633.50 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5129(19) _cell_length_b 21.587(4) _cell_length_c 13.479(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.71(3) _cell_angle_gamma 90.00 _cell_volume 2766.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11523 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7820 _exptl_absorpt_correction_T_max 0.8910 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 Smart Aepex CCD' _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 12178 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 24.71 _reflns_number_total 4677 _reflns_number_gt 4252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.8838P] 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 4677 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5552(2) 0.46507(10) 0.70573(14) 0.0140(4) Uani 1 1 d . . . C2 C 0.7232(2) 0.56421(9) 0.79872(15) 0.0161(4) Uani 1 1 d . . . C3 C 0.6525(2) 0.57244(9) 0.58857(15) 0.0157(4) Uani 1 1 d . . . C4 C 0.47699(19) 0.15662(10) 0.77858(14) 0.0144(4) Uani 1 1 d . . . C5 C 0.3176(2) 0.56009(9) 0.54640(15) 0.0174(4) Uani 1 1 d . . . H5 H 0.3948 0.5558 0.5039 0.021 Uiso 1 1 calc R . . C6 C 0.1838(2) 0.56521(9) 0.50454(16) 0.0220(5) Uani 1 1 d . . . H6 H 0.1694 0.5647 0.4345 0.026 Uiso 1 1 calc R . . C7 C 0.0711(2) 0.57108(10) 0.56635(16) 0.0232(5) Uani 1 1 d . . . H7 H -0.0219 0.5749 0.5393 0.028 Uiso 1 1 calc R . . C8 C 0.0953(2) 0.57138(9) 0.66846(16) 0.0201(5) Uani 1 1 d . . . H8 H 0.0190 0.5749 0.7120 0.024 Uiso 1 1 calc R . . C9 C 0.2321(2) 0.56642(8) 0.70610(15) 0.0147(4) Uani 1 1 d . . . C10 C 0.2708(2) 0.56786(8) 0.81348(15) 0.0151(4) Uani 1 1 d . . . C11 C 0.1759(2) 0.57777(9) 0.88791(15) 0.0187(5) Uani 1 1 d . . . H11 H 0.0784 0.5819 0.8722 0.022 Uiso 1 1 calc R . . C12 C 0.2251(2) 0.58159(10) 0.98581(16) 0.0209(5) Uani 1 1 d . . . H12 H 0.1616 0.5891 1.0375 0.025 Uiso 1 1 calc R . . C13 C 0.3670(2) 0.57432(9) 1.00737(16) 0.0207(5) Uani 1 1 d . . . H13 H 0.4029 0.5771 1.0738 0.025 Uiso 1 1 calc R . . C14 C 0.4554(2) 0.56291(9) 0.93012(15) 0.0177(5) Uani 1 1 d . . . H14 H 0.5526 0.5566 0.9449 0.021 Uiso 1 1 calc R . . C15 C 0.8248(2) 0.27960(9) 0.80058(15) 0.0168(4) Uani 1 1 d . . . C16 C 0.9310(2) 0.27786(9) 0.87572(16) 0.0207(5) Uani 1 1 d . . . H16 H 0.9163 0.2988 0.9366 0.025 Uiso 1 1 calc R . . C17 C 1.0552(2) 0.24666(10) 0.86319(17) 0.0260(5) Uani 1 1 d . . . H17 H 1.1236 0.2458 0.9160 0.031 Uiso 1 1 calc R . . C18 C 1.0827(2) 0.21628(10) 0.77454(19) 0.0292(5) Uani 1 1 d . . . H18 H 1.1678 0.1939 0.7671 0.035 Uiso 1 1 calc R . . C19 C 0.9841(2) 0.21943(10) 0.69826(18) 0.0255(5) Uani 1 1 d . . . H19 H 1.0033 0.2000 0.6369 0.031 Uiso 1 1 calc R . . C20 C 0.8548(2) 0.25077(9) 0.70846(16) 0.0196(5) Uani 1 1 d . . . C21 C 0.7617(2) 0.25482(9) 0.62338(16) 0.0204(5) Uani 1 1 d . . . H21 H 0.7933 0.2371 0.5635 0.024 Uiso 1 1 calc R . . C22 C 0.5563(2) 0.28337(10) 0.52631(15) 0.0210(5) Uani 1 1 d . . . H22A H 0.5901 0.2521 0.4789 0.025 Uiso 1 1 calc R . . H22B H 0.5652 0.3249 0.4960 0.025 Uiso 1 1 calc R . . C23 C 0.4047(2) 0.27071(10) 0.55058(14) 0.0201(5) Uani 1 1 d . . . H23A H 0.3412 0.2844 0.4954 0.024 Uiso 1 1 calc R . . H23B H 0.3901 0.2258 0.5614 0.024 Uiso 1 1 calc R . . C24 C 0.2585(2) 0.33381(9) 0.65109(15) 0.0175(4) Uani 1 1 d . . . H24 H 0.1929 0.3326 0.5965 0.021 Uiso 1 1 calc R . . C25 C 0.2185(2) 0.36703(9) 0.73799(15) 0.0168(4) Uani 1 1 d . . . C26 C 0.0917(2) 0.40059(10) 0.73274(16) 0.0231(5) Uani 1 1 d . . . H26 H 0.0398 0.4024 0.6715 0.028 Uiso 1 1 calc R . . C27 C 0.0411(2) 0.43085(9) 0.81388(17) 0.0249(5) Uani 1 1 d . . . H27 H -0.0430 0.4545 0.8085 0.030 Uiso 1 1 calc R . . C28 C 0.1155(2) 0.42617(9) 0.90419(17) 0.0230(5) Uani 1 1 d . . . H28 H 0.0805 0.4462 0.9611 0.028 Uiso 1 1 calc R . . C29 C 0.2392(2) 0.39284(9) 0.91232(16) 0.0203(5) Uani 1 1 d . . . H29 H 0.2863 0.3893 0.9752 0.024 Uiso 1 1 calc R . . C30 C 0.2966(2) 0.36411(9) 0.82936(15) 0.0161(4) Uani 1 1 d . . . Cr1 Cr 0.53925(3) 0.561080(13) 0.71437(2) 0.01101(10) Uani 1 1 d . . . Mn1 Mn 0.53722(3) 0.309540(13) 0.73894(2) 0.01223(10) Uani 1 1 d . . . N1 N 0.56622(18) 0.41217(8) 0.70085(12) 0.0176(4) Uani 1 1 d . . . N2 N 0.82579(19) 0.56680(8) 0.84585(14) 0.0245(4) Uani 1 1 d . . . N3 N 0.71971(19) 0.58151(9) 0.52083(14) 0.0243(4) Uani 1 1 d . . . N4 N 0.49569(18) 0.20878(8) 0.77362(12) 0.0184(4) Uani 1 1 d . . . N5 N 0.34248(17) 0.56093(7) 0.64504(12) 0.0137(4) Uani 1 1 d . . . N6 N 0.40995(17) 0.56029(7) 0.83490(12) 0.0129(4) Uani 1 1 d . . . N7 N 0.63931(17) 0.28018(7) 0.62050(12) 0.0165(4) Uani 1 1 d . . . N8 N 0.37591(18) 0.30561(7) 0.64143(12) 0.0158(4) Uani 1 1 d . . . O1 O 0.70623(14) 0.30880(6) 0.81806(10) 0.0162(3) Uani 1 1 d . . . O2 O 0.41771(14) 0.33407(6) 0.84106(9) 0.0160(3) 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 C1 0.0112(10) 0.0175(12) 0.0135(10) 0.0003(8) 0.0009(7) -0.0007(8) C2 0.0156(11) 0.0152(11) 0.0178(10) 0.0006(8) 0.0055(9) 0.0005(8) C3 0.0135(11) 0.0132(10) 0.0203(11) -0.0001(9) -0.0009(9) 0.0025(8) C4 0.0109(10) 0.0167(12) 0.0156(10) -0.0003(8) 0.0001(8) -0.0013(8) C5 0.0185(11) 0.0162(11) 0.0175(11) -0.0019(8) 0.0011(8) 0.0009(8) C6 0.0211(12) 0.0263(12) 0.0183(11) -0.0012(9) -0.0048(9) 0.0014(9) C7 0.0143(11) 0.0282(12) 0.0266(12) -0.0007(10) -0.0058(9) 0.0017(9) C8 0.0127(11) 0.0225(11) 0.0252(11) 0.0003(9) 0.0021(9) 0.0001(8) C9 0.0141(11) 0.0114(10) 0.0185(11) 0.0002(8) -0.0001(8) -0.0009(7) C10 0.0144(11) 0.0108(10) 0.0202(11) 0.0009(8) 0.0007(8) -0.0008(7) C11 0.0131(11) 0.0199(11) 0.0233(11) -0.0003(9) 0.0031(8) -0.0005(8) C12 0.0200(12) 0.0216(11) 0.0217(11) -0.0008(9) 0.0087(9) 0.0000(9) C13 0.0224(12) 0.0234(11) 0.0162(10) -0.0017(9) 0.0007(9) -0.0031(9) C14 0.0146(11) 0.0198(11) 0.0187(11) 0.0016(9) -0.0009(8) -0.0008(8) C15 0.0144(11) 0.0123(10) 0.0240(11) 0.0041(9) 0.0013(8) -0.0009(8) C16 0.0189(12) 0.0207(11) 0.0225(11) 0.0046(9) 0.0008(9) -0.0012(9) C17 0.0171(12) 0.0251(12) 0.0355(13) 0.0089(11) -0.0045(9) -0.0003(9) C18 0.0158(12) 0.0218(12) 0.0502(15) 0.0026(11) 0.0034(10) 0.0035(9) C19 0.0190(12) 0.0203(11) 0.0374(13) -0.0052(10) 0.0060(10) 0.0006(9) C20 0.0179(11) 0.0139(10) 0.0272(11) -0.0008(9) 0.0030(9) 0.0001(8) C21 0.0219(12) 0.0168(10) 0.0228(11) -0.0058(9) 0.0059(9) -0.0018(9) C22 0.0270(12) 0.0234(11) 0.0124(10) -0.0020(9) -0.0012(8) 0.0013(9) C23 0.0256(12) 0.0204(11) 0.0141(10) -0.0044(9) -0.0031(8) -0.0012(9) C24 0.0166(11) 0.0169(10) 0.0188(10) 0.0057(9) -0.0025(8) -0.0025(8) C25 0.0154(11) 0.0135(10) 0.0217(11) 0.0039(9) 0.0030(8) -0.0013(8) C26 0.0186(11) 0.0239(12) 0.0269(12) 0.0080(10) 0.0000(9) 0.0025(9) C27 0.0166(12) 0.0219(12) 0.0366(13) 0.0056(10) 0.0067(10) 0.0054(9) C28 0.0201(12) 0.0194(11) 0.0300(12) -0.0042(10) 0.0092(9) -0.0028(9) C29 0.0160(11) 0.0214(11) 0.0235(11) -0.0047(9) 0.0029(8) -0.0033(9) C30 0.0143(11) 0.0120(10) 0.0221(11) 0.0005(9) 0.0021(8) -0.0037(8) Cr1 0.00959(19) 0.00933(18) 0.01414(18) -0.00009(12) 0.00066(13) 0.00047(11) Mn1 0.01352(18) 0.01029(17) 0.01287(17) -0.00051(12) 0.00004(12) 0.00052(11) N1 0.0193(9) 0.0146(10) 0.0189(9) 0.0018(8) 0.0011(7) 0.0001(7) N2 0.0153(10) 0.0357(12) 0.0225(10) -0.0013(8) 0.0004(8) 0.0007(8) N3 0.0203(10) 0.0281(10) 0.0247(10) 0.0053(8) 0.0043(8) 0.0039(8) N4 0.0210(10) 0.0148(10) 0.0195(9) 0.0018(8) 0.0001(7) 0.0001(7) N5 0.0131(9) 0.0106(8) 0.0174(9) -0.0005(7) 0.0008(7) 0.0004(6) N6 0.0107(9) 0.0118(8) 0.0162(9) 0.0005(7) 0.0008(7) -0.0009(6) N7 0.0196(10) 0.0139(9) 0.0161(9) -0.0011(7) 0.0013(7) -0.0017(7) N8 0.0177(9) 0.0133(8) 0.0162(9) -0.0004(7) -0.0006(7) -0.0020(7) O1 0.0139(7) 0.0172(7) 0.0174(7) -0.0009(6) -0.0008(6) 0.0022(6) O2 0.0143(7) 0.0188(7) 0.0149(7) -0.0010(6) 0.0005(6) 0.0020(6) _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 C1 N1 1.149(3) . ? C1 Cr1 2.082(2) . ? C2 N2 1.150(3) . ? C2 Cr1 2.059(2) . ? C3 N3 1.147(3) . ? C3 Cr1 2.051(2) . ? C4 N4 1.142(3) . ? C4 Cr1 2.071(2) 2_646 ? C5 N5 1.344(3) . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C7 C8 1.389(3) . ? C7 H7 0.9500 . ? C8 C9 1.387(3) . ? C8 H8 0.9500 . ? C9 N5 1.359(3) . ? C9 C10 1.483(3) . ? C10 N6 1.356(3) . ? C10 C11 1.386(3) . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 N6 1.343(3) . ? C14 H14 0.9500 . ? C15 O1 1.320(2) . ? C15 C16 1.409(3) . ? C15 C20 1.425(3) . ? C16 C17 1.375(3) . ? C16 H16 0.9500 . ? C17 C18 1.395(3) . ? C17 H17 0.9500 . ? C18 C19 1.373(3) . ? C18 H18 0.9500 . ? C19 C20 1.414(3) . ? C19 H19 0.9500 . ? C20 C21 1.430(3) . ? C21 N7 1.287(3) . ? C21 H21 0.9500 . ? C22 N7 1.477(3) . ? C22 C23 1.513(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N8 1.471(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N8 1.282(3) . ? C24 C25 1.434(3) . ? C24 H24 0.9500 . ? C25 C26 1.407(3) . ? C25 C30 1.421(3) . ? C26 C27 1.373(3) . ? C26 H26 0.9500 . ? C27 C28 1.394(3) . ? C27 H27 0.9500 . ? C28 C29 1.381(3) . ? C28 H28 0.9500 . ? C29 C30 1.404(3) . ? C29 H29 0.9500 . ? C30 O2 1.327(2) . ? Cr1 N6 2.0669(18) . ? Cr1 N5 2.0671(18) . ? Cr1 C4 2.071(2) 2_656 ? Mn1 O2 1.8871(14) . ? Mn1 O1 1.9027(15) . ? Mn1 N8 1.9923(18) . ? Mn1 N7 1.9966(17) . ? Mn1 N4 2.2621(18) . ? Mn1 N1 2.2927(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 Cr1 178.94(17) . . ? N2 C2 Cr1 179.09(17) . . ? N3 C3 Cr1 176.15(19) . . ? N4 C4 Cr1 175.24(17) . 2_646 ? N5 C5 C6 122.4(2) . . ? N5 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C7 118.9(2) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C8 119.3(2) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 119.2(2) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? N5 C9 C8 121.26(19) . . ? N5 C9 C10 114.78(17) . . ? C8 C9 C10 123.95(19) . . ? N6 C10 C11 121.13(19) . . ? N6 C10 C9 114.68(18) . . ? C11 C10 C9 124.16(19) . . ? C10 C11 C12 119.26(19) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 119.5(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 118.4(2) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? N6 C14 C13 122.85(19) . . ? N6 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? O1 C15 C16 118.85(19) . . ? O1 C15 C20 123.95(18) . . ? C16 C15 C20 117.18(19) . . ? C17 C16 C15 121.7(2) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 121.3(2) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 118.5(2) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 121.9(2) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C15 119.39(19) . . ? C19 C20 C21 118.1(2) . . ? C15 C20 C21 122.46(19) . . ? N7 C21 C20 126.04(19) . . ? N7 C21 H21 117.0 . . ? C20 C21 H21 117.0 . . ? N7 C22 C23 107.13(16) . . ? N7 C22 H22A 110.3 . . ? C23 C22 H22A 110.3 . . ? N7 C22 H22B 110.3 . . ? C23 C22 H22B 110.3 . . ? H22A C22 H22B 108.5 . . ? N8 C23 C22 106.86(16) . . ? N8 C23 H23A 110.4 . . ? C22 C23 H23A 110.4 . . ? N8 C23 H23B 110.4 . . ? C22 C23 H23B 110.4 . . ? H23A C23 H23B 108.6 . . ? N8 C24 C25 124.97(19) . . ? N8 C24 H24 117.5 . . ? C25 C24 H24 117.5 . . ? C26 C25 C30 119.47(19) . . ? C26 C25 C24 117.64(18) . . ? C30 C25 C24 122.77(18) . . ? C27 C26 C25 121.7(2) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 118.7(2) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 121.1(2) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 121.2(2) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? O2 C30 C29 118.58(18) . . ? O2 C30 C25 123.67(18) . . ? C29 C30 C25 117.71(18) . . ? C3 Cr1 C2 89.66(8) . . ? C3 Cr1 N6 172.15(7) . . ? C2 Cr1 N6 94.70(7) . . ? C3 Cr1 N5 96.74(8) . . ? C2 Cr1 N5 173.11(7) . . ? N6 Cr1 N5 78.65(7) . . ? C3 Cr1 C4 87.74(8) . 2_656 ? C2 Cr1 C4 90.30(7) . 2_656 ? N6 Cr1 C4 85.71(7) . 2_656 ? N5 Cr1 C4 87.39(7) . 2_656 ? C3 Cr1 C1 91.82(8) . . ? C2 Cr1 C1 90.08(7) . . ? N6 Cr1 C1 94.69(7) . . ? N5 Cr1 C1 92.27(7) . . ? C4 Cr1 C1 179.42(8) 2_656 . ? O2 Mn1 O1 96.37(6) . . ? O2 Mn1 N8 91.39(6) . . ? O1 Mn1 N8 172.21(6) . . ? O2 Mn1 N7 172.04(6) . . ? O1 Mn1 N7 91.29(6) . . ? N8 Mn1 N7 80.93(7) . . ? O2 Mn1 N4 90.36(6) . . ? O1 Mn1 N4 91.49(6) . . ? N8 Mn1 N4 87.68(6) . . ? N7 Mn1 N4 87.26(7) . . ? O2 Mn1 N1 88.36(6) . . ? O1 Mn1 N1 91.62(6) . . ? N8 Mn1 N1 89.36(6) . . ? N7 Mn1 N1 93.61(6) . . ? N4 Mn1 N1 176.75(6) . . ? C1 N1 Mn1 159.38(15) . . ? C4 N4 Mn1 171.29(16) . . ? C5 N5 C9 118.94(18) . . ? C5 N5 Cr1 125.32(14) . . ? C9 N5 Cr1 115.59(14) . . ? C14 N6 C10 118.86(17) . . ? C14 N6 Cr1 124.65(14) . . ? C10 N6 Cr1 115.57(13) . . ? C21 N7 C22 120.43(17) . . ? C21 N7 Mn1 124.92(14) . . ? C22 N7 Mn1 114.34(13) . . ? C24 N8 C23 120.82(18) . . ? C24 N8 Mn1 124.68(14) . . ? C23 N8 Mn1 114.35(13) . . ? C15 O1 Mn1 128.06(13) . . ? C30 O2 Mn1 126.16(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.282 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.057 data_4 _database_code_depnum_ccdc_archive 'CCDC 899932' #TrackingRef '16202_web_deposit_cif_file_0_XiaopingShen_1355531900.MnCr.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H24 Cr Mn N8 O2' _chemical_formula_weight 647.52 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2635(19) _cell_length_b 21.400(4) _cell_length_c 14.823(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.68(3) _cell_angle_gamma 90.00 _cell_volume 2912.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11943 _cell_measurement_theta_min 2.7690 _cell_measurement_theta_max 28.9877 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex CCD' _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 13829 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5636 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The restraints are generated by the refinement command (delu 0.01 c29a c31a isor 0.01 c29a > c31b simu 0.01 0.02 c29a > c31b ) for treating the disordered carbon atoms. ; _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^)+(0.0774P)^2^+0.9618P] 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 5636 _refine_ls_number_parameters 416 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.016 _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 Mn1 Mn 0.56807(6) 0.81635(2) 0.76825(3) 0.02975(17) Uani 1 1 d . . . Cr1 Cr 0.43614(5) 0.56912(2) 0.76168(3) 0.02588(17) Uani 1 1 d . . . O1 O 0.4137(3) 0.84088(11) 0.83185(15) 0.0355(6) Uani 1 1 d . . . N1 N 0.5096(4) 0.71560(15) 0.7836(2) 0.0505(9) Uani 1 1 d . . . C1 C 0.4777(4) 0.66401(16) 0.7773(2) 0.0340(8) Uani 1 1 d . . . O2 O 0.7121(3) 0.81121(11) 0.87074(15) 0.0360(6) Uani 1 1 d . . . N2 N 0.1369(4) 0.6045(2) 0.6393(3) 0.0702(12) Uani 1 1 d . . . C2 C 0.2427(4) 0.59011(19) 0.6846(3) 0.0425(9) Uani 1 1 d . . . N3 N 0.2975(3) 0.57044(15) 0.9479(2) 0.0414(8) Uani 1 1 d . . . C3 C 0.3454(4) 0.56930(15) 0.8805(2) 0.0313(8) Uani 1 1 d . . . N4 N 0.5513(3) 0.56961(12) 0.65144(19) 0.0291(6) Uani 1 1 d . . . N6 N 0.3812(4) 0.42083(14) 0.7467(2) 0.0402(7) Uani 1 1 d . . . C4 C 0.3987(4) 0.47353(17) 0.7506(2) 0.0323(8) Uani 1 1 d . . . N5 N 0.6468(3) 0.55532(12) 0.82437(19) 0.0287(6) Uani 1 1 d . . . C5 C 0.6856(4) 0.54744(17) 0.9140(2) 0.0376(8) Uani 1 1 d . . . H5 H 0.6124 0.5390 0.9515 0.045 Uiso 1 1 calc R . . C6 C 0.8298(4) 0.55118(17) 0.9536(3) 0.0428(9) Uani 1 1 d . . . H6 H 0.8552 0.5446 1.0172 0.051 Uiso 1 1 calc R . . N7 N 0.4438(4) 0.82319(17) 0.6494(2) 0.0517(9) Uani 1 1 d . . . C7 C 0.9352(4) 0.56457(18) 0.8995(3) 0.0463(10) Uani 1 1 d . . . H7 H 1.0336 0.5701 0.9260 0.056 Uiso 1 1 calc R . . N8 N 0.7129(4) 0.79289(18) 0.6866(2) 0.0537(9) Uani 1 1 d . . . C8 C 0.8973(4) 0.56996(17) 0.8060(3) 0.0398(9) Uani 1 1 d . . . H8 H 0.9695 0.5772 0.7674 0.048 Uiso 1 1 calc R . . C9 C 0.7512(4) 0.56448(14) 0.7702(2) 0.0296(7) Uani 1 1 d . . . C10 C 0.6984(4) 0.56893(14) 0.6728(2) 0.0312(8) Uani 1 1 d . . . C11 C 0.7884(4) 0.57089(17) 0.6048(3) 0.0421(9) Uani 1 1 d . . . H11 H 0.8913 0.5700 0.6201 0.051 Uiso 1 1 calc R . . C12 C 0.7264(4) 0.57415(18) 0.5147(3) 0.0441(9) Uani 1 1 d . . . H12 H 0.7864 0.5755 0.4675 0.053 Uiso 1 1 calc R . . C13 C 0.5777(4) 0.57542(17) 0.4941(2) 0.0416(9) Uani 1 1 d . . . H13 H 0.5331 0.5781 0.4327 0.050 Uiso 1 1 calc R . . C14 C 0.4947(4) 0.57271(16) 0.5638(2) 0.0360(8) Uani 1 1 d . . . H14 H 0.3916 0.5731 0.5491 0.043 Uiso 1 1 calc R . . C15 C 0.3156(4) 0.8478(2) 0.6360(3) 0.0478(10) Uani 1 1 d . A . H15 H 0.2708 0.8514 0.5747 0.057 Uiso 1 1 calc R . . C16 C 0.2348(4) 0.87010(16) 0.7051(3) 0.0374(8) Uani 1 1 d . . . C17 C 0.0978(4) 0.89644(19) 0.6770(3) 0.0491(10) Uani 1 1 d . A . H17 H 0.0642 0.8996 0.6137 0.059 Uiso 1 1 calc R . . C18 C 0.0117(5) 0.9175(2) 0.7376(3) 0.0575(12) Uani 1 1 d . . . H18 H -0.0811 0.9351 0.7173 0.069 Uiso 1 1 calc R A . C19 C 0.0617(4) 0.91293(19) 0.8299(3) 0.0548(11) Uani 1 1 d . A . H19 H 0.0024 0.9279 0.8729 0.066 Uiso 1 1 calc R . . C20 C 0.1953(4) 0.88717(18) 0.8604(3) 0.0441(9) Uani 1 1 d . . . H20 H 0.2261 0.8842 0.9240 0.053 Uiso 1 1 calc R A . C21 C 0.2866(4) 0.86520(15) 0.7995(2) 0.0351(8) Uani 1 1 d . A . C22 C 0.8414(4) 0.78435(15) 0.8781(2) 0.0328(8) Uani 1 1 d . A . C23 C 0.9252(4) 0.78226(17) 0.9648(3) 0.0423(9) Uani 1 1 d . . . H23 H 0.8882 0.8002 1.0157 0.051 Uiso 1 1 calc R . . C24 C 1.0598(4) 0.7545(2) 0.9760(3) 0.0518(11) Uani 1 1 d . . . H24 H 1.1142 0.7532 1.0350 0.062 Uiso 1 1 calc R . . C25 C 1.1187(5) 0.72833(19) 0.9033(3) 0.0519(10) Uani 1 1 d . . . H25 H 1.2108 0.7081 0.9129 0.062 Uiso 1 1 calc R . . C26 C 1.0434(4) 0.73188(17) 0.8187(3) 0.0452(9) Uani 1 1 d . A . H26 H 1.0849 0.7153 0.7686 0.054 Uiso 1 1 calc R . . C27 C 0.9042(4) 0.75982(15) 0.8037(2) 0.0357(8) Uani 1 1 d . . . C28 C 0.8386(5) 0.7682(2) 0.7118(3) 0.0522(11) Uani 1 1 d . A . H28 H 0.8922 0.7543 0.6652 0.063 Uiso 1 1 calc R . . C29A C 0.5182(8) 0.8073(4) 0.5670(5) 0.0581(17) Uani 0.699(8) 1 d PU A 1 H29A H 0.4781 0.8319 0.5119 0.070 Uiso 0.699(8) 1 calc PR A 1 C30A C 0.6731(8) 0.8155(4) 0.5901(5) 0.0570(18) Uani 0.699(8) 1 d PU A 1 H30A H 0.6995 0.8600 0.5853 0.068 Uiso 0.699(8) 1 calc PR A 1 H30B H 0.7259 0.7909 0.5483 0.068 Uiso 0.699(8) 1 calc PR A 1 C31A C 0.5059(8) 0.7334(3) 0.5500(5) 0.066(2) Uani 0.699(8) 1 d PU A 1 H31A H 0.5529 0.7224 0.4967 0.098 Uiso 0.699(8) 1 calc PR A 1 H31B H 0.4031 0.7212 0.5393 0.098 Uiso 0.699(8) 1 calc PR A 1 H31C H 0.5544 0.7113 0.6036 0.098 Uiso 0.699(8) 1 calc PR A 1 C29B C 0.6362(17) 0.7764(9) 0.5910(10) 0.050(3) Uani 0.301(8) 1 d PU A 2 H29B H 0.6769 0.7378 0.5662 0.060 Uiso 0.301(8) 1 calc PR A 2 C30B C 0.484(2) 0.7754(10) 0.5820(13) 0.062(3) Uani 0.301(8) 1 d PU A 2 H30C H 0.4482 0.7334 0.5964 0.074 Uiso 0.301(8) 1 calc PR A 2 H30D H 0.4413 0.7867 0.5192 0.074 Uiso 0.301(8) 1 calc PR A 2 C31B C 0.675(2) 0.8335(9) 0.5429(14) 0.077(4) Uani 0.301(8) 1 d PU A 2 H31D H 0.6359 0.8306 0.4784 0.116 Uiso 0.301(8) 1 calc PR A 2 H31E H 0.7816 0.8374 0.5490 0.116 Uiso 0.301(8) 1 calc PR A 2 H31F H 0.6344 0.8703 0.5698 0.116 Uiso 0.301(8) 1 calc PR 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 Mn1 0.0354(3) 0.0289(3) 0.0260(3) -0.0007(2) 0.0077(2) 0.0042(2) Cr1 0.0246(3) 0.0277(3) 0.0262(3) 0.0001(2) 0.0065(2) -0.0014(2) O1 0.0326(13) 0.0426(14) 0.0329(13) -0.0007(11) 0.0098(10) 0.0039(11) N1 0.070(2) 0.0315(19) 0.052(2) -0.0009(15) 0.0146(18) -0.0005(16) C1 0.038(2) 0.033(2) 0.0337(19) -0.0003(16) 0.0110(15) 0.0009(15) O2 0.0366(14) 0.0435(14) 0.0284(13) -0.0007(11) 0.0061(10) 0.0087(11) N2 0.035(2) 0.123(4) 0.053(2) 0.029(2) 0.0060(18) 0.001(2) C2 0.027(2) 0.065(3) 0.036(2) 0.0071(19) 0.0085(16) -0.0021(17) N3 0.0364(18) 0.056(2) 0.0336(17) 0.0043(14) 0.0102(14) 0.0014(14) C3 0.0307(18) 0.0324(18) 0.0310(19) 0.0006(15) 0.0054(15) 0.0003(14) N4 0.0315(16) 0.0256(14) 0.0315(15) 0.0002(12) 0.0086(12) -0.0023(11) N6 0.0458(19) 0.0333(18) 0.0447(18) -0.0043(14) 0.0180(15) -0.0061(14) C4 0.0303(18) 0.039(2) 0.0301(18) -0.0017(15) 0.0131(14) -0.0032(15) N5 0.0231(14) 0.0302(15) 0.0335(15) 0.0016(12) 0.0059(12) -0.0017(11) C5 0.034(2) 0.047(2) 0.0322(19) 0.0062(16) 0.0043(15) -0.0031(16) C6 0.036(2) 0.052(2) 0.039(2) 0.0049(18) -0.0007(17) -0.0032(17) N7 0.050(2) 0.078(2) 0.0268(17) -0.0055(16) 0.0061(15) 0.0155(18) C7 0.027(2) 0.057(2) 0.054(2) 0.009(2) 0.0001(18) -0.0020(17) N8 0.054(2) 0.078(2) 0.0304(17) -0.0062(17) 0.0100(15) 0.0255(19) C8 0.0277(19) 0.044(2) 0.049(2) 0.0044(18) 0.0104(17) -0.0008(16) C9 0.0270(17) 0.0245(16) 0.0383(19) 0.0059(14) 0.0077(15) 0.0004(13) C10 0.0325(19) 0.0245(16) 0.0387(19) 0.0048(14) 0.0129(15) 0.0022(14) C11 0.038(2) 0.042(2) 0.050(2) 0.0048(18) 0.0190(18) 0.0023(16) C12 0.051(2) 0.050(2) 0.036(2) 0.0098(17) 0.0225(18) 0.0051(18) C13 0.054(3) 0.042(2) 0.0300(19) 0.0036(16) 0.0128(17) -0.0008(18) C14 0.040(2) 0.039(2) 0.0296(19) -0.0007(15) 0.0084(16) -0.0025(16) C15 0.043(2) 0.064(3) 0.035(2) 0.0037(19) 0.0023(17) 0.000(2) C16 0.037(2) 0.0339(19) 0.042(2) 0.0054(16) 0.0089(16) -0.0033(15) C17 0.040(2) 0.050(2) 0.058(3) 0.015(2) 0.007(2) 0.0006(18) C18 0.038(2) 0.055(3) 0.080(3) 0.009(2) 0.010(2) 0.008(2) C19 0.037(2) 0.055(3) 0.077(3) -0.010(2) 0.025(2) 0.0011(19) C20 0.039(2) 0.047(2) 0.049(2) -0.0075(18) 0.0143(18) -0.0041(17) C21 0.036(2) 0.0294(18) 0.041(2) -0.0015(15) 0.0122(16) -0.0052(15) C22 0.0352(19) 0.0294(18) 0.0342(19) 0.0051(15) 0.0066(15) 0.0006(14) C23 0.042(2) 0.047(2) 0.039(2) 0.0100(18) 0.0095(17) 0.0031(17) C24 0.040(2) 0.068(3) 0.046(2) 0.014(2) 0.0010(19) 0.006(2) C25 0.042(2) 0.053(2) 0.060(3) 0.011(2) 0.006(2) 0.0150(19) C26 0.040(2) 0.042(2) 0.056(2) -0.0051(19) 0.0115(18) 0.0053(17) C27 0.038(2) 0.0291(18) 0.040(2) -0.0011(16) 0.0073(16) 0.0031(15) C28 0.050(3) 0.065(3) 0.043(2) -0.015(2) 0.0143(19) 0.018(2) C29A 0.057(3) 0.080(4) 0.040(3) 0.007(3) 0.015(3) 0.009(3) C30A 0.063(4) 0.080(4) 0.032(3) 0.008(3) 0.017(3) 0.014(3) C31A 0.095(5) 0.055(4) 0.049(4) -0.013(3) 0.015(3) -0.011(3) C29B 0.055(5) 0.063(5) 0.036(4) 0.000(5) 0.014(4) 0.004(4) C30B 0.063(6) 0.074(6) 0.049(5) -0.009(5) 0.008(5) 0.010(5) C31B 0.086(7) 0.079(7) 0.065(7) 0.007(6) 0.004(7) -0.016(6) _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 O2 1.886(2) . ? Mn1 O1 1.889(2) . ? Mn1 N7 1.977(3) . ? Mn1 N8 1.987(3) . ? Mn1 N1 2.242(3) . ? Mn1 N6 2.301(3) 2_656 ? Cr1 C2 2.042(4) . ? Cr1 C3 2.050(4) . ? Cr1 N5 2.067(3) . ? Cr1 N4 2.067(3) . ? Cr1 C1 2.074(4) . ? Cr1 C4 2.078(4) . ? O1 C21 1.318(4) . ? N1 C1 1.144(4) . ? O2 C22 1.321(4) . ? N2 C2 1.154(5) . ? N3 C3 1.147(4) . ? N4 C14 1.337(4) . ? N4 C10 1.358(4) . ? N6 C4 1.140(4) . ? N6 Mn1 2.301(3) 2_646 ? N5 C5 1.340(4) . ? N5 C9 1.351(4) . ? C5 C6 1.388(5) . ? C5 H5 0.9500 . ? C6 C7 1.374(6) . ? C6 H6 0.9500 . ? N7 C15 1.290(5) . ? N7 C30B 1.510(19) . ? N7 C29A 1.518(8) . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? N8 C28 1.289(5) . ? N8 C30A 1.508(7) . ? N8 C29B 1.539(15) . ? C8 C9 1.391(5) . ? C8 H8 0.9500 . ? C9 C10 1.465(5) . ? C10 C11 1.391(5) . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.371(5) . ? C12 H12 0.9500 . ? C13 C14 1.369(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.428(5) . ? C15 H15 0.9500 . ? C16 C17 1.400(5) . ? C16 C21 1.421(5) . ? C17 C18 1.356(6) . ? C17 H17 0.9500 . ? C18 C19 1.388(6) . ? C18 H18 0.9500 . ? C19 C20 1.375(6) . ? C19 H19 0.9500 . ? C20 C21 1.398(5) . ? C20 H20 0.9500 . ? C22 C23 1.410(5) . ? C22 C27 1.415(5) . ? C23 C24 1.370(5) . ? C23 H23 0.9500 . ? C24 C25 1.389(6) . ? C24 H24 0.9500 . ? C25 C26 1.353(6) . ? C25 H25 0.9500 . ? C26 C27 1.412(5) . ? C26 H26 0.9500 . ? C27 C28 1.428(5) . ? C28 H28 0.9500 . ? C29A C30A 1.441(10) . ? C29A C31A 1.605(11) . ? C29A H29A 1.0000 . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C29B C30B 1.40(2) . ? C29B C31B 1.48(2) . ? C29B H29B 1.0000 . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 96.61(10) . . ? O2 Mn1 N7 170.73(13) . . ? O1 Mn1 N7 92.00(12) . . ? O2 Mn1 N8 90.78(12) . . ? O1 Mn1 N8 172.52(12) . . ? N7 Mn1 N8 80.55(14) . . ? O2 Mn1 N1 90.97(12) . . ? O1 Mn1 N1 90.43(12) . . ? N7 Mn1 N1 92.39(14) . . ? N8 Mn1 N1 90.61(15) . . ? O2 Mn1 N6 90.16(11) . 2_656 ? O1 Mn1 N6 87.47(11) . 2_656 ? N7 Mn1 N6 86.80(14) . 2_656 ? N8 Mn1 N6 91.36(14) . 2_656 ? N1 Mn1 N6 177.71(13) . 2_656 ? C2 Cr1 C3 92.87(14) . . ? C2 Cr1 N5 171.05(13) . . ? C3 Cr1 N5 94.88(12) . . ? C2 Cr1 N4 93.64(13) . . ? C3 Cr1 N4 173.22(13) . . ? N5 Cr1 N4 78.49(11) . . ? C2 Cr1 C1 89.03(15) . . ? C3 Cr1 C1 89.62(13) . . ? N5 Cr1 C1 86.54(12) . . ? N4 Cr1 C1 88.61(12) . . ? C2 Cr1 C4 92.73(15) . . ? C3 Cr1 C4 89.23(13) . . ? N5 Cr1 C4 91.86(12) . . ? N4 Cr1 C4 92.34(11) . . ? C1 Cr1 C4 177.95(14) . . ? C21 O1 Mn1 128.8(2) . . ? C1 N1 Mn1 169.6(3) . . ? N1 C1 Cr1 175.2(3) . . ? C22 O2 Mn1 128.9(2) . . ? N2 C2 Cr1 176.6(4) . . ? N3 C3 Cr1 178.2(3) . . ? C14 N4 C10 118.6(3) . . ? C14 N4 Cr1 126.3(2) . . ? C10 N4 Cr1 115.1(2) . . ? C4 N6 Mn1 159.5(3) . 2_646 ? N6 C4 Cr1 178.0(3) . . ? C5 N5 C9 119.2(3) . . ? C5 N5 Cr1 125.2(2) . . ? C9 N5 Cr1 114.8(2) . . ? N5 C5 C6 121.9(3) . . ? N5 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C7 C6 C5 118.9(4) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C15 N7 C30B 118.5(8) . . ? C15 N7 C29A 118.4(4) . . ? C30B N7 C29A 30.6(7) . . ? C15 N7 Mn1 125.5(3) . . ? C30B N7 Mn1 112.0(7) . . ? C29A N7 Mn1 115.3(3) . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C28 N8 C30A 120.2(4) . . ? C28 N8 C29B 117.4(7) . . ? C30A N8 C29B 34.5(6) . . ? C28 N8 Mn1 125.8(3) . . ? C30A N8 Mn1 113.4(3) . . ? C29B N8 Mn1 110.6(6) . . ? C7 C8 C9 118.5(3) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N5 C9 C8 121.5(3) . . ? N5 C9 C10 115.1(3) . . ? C8 C9 C10 123.4(3) . . ? N4 C10 C11 120.7(3) . . ? N4 C10 C9 115.0(3) . . ? C11 C10 C9 124.3(3) . . ? C12 C11 C10 119.3(4) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 118.7(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? N4 C14 C13 123.3(4) . . ? N4 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? N7 C15 C16 125.9(4) . . ? N7 C15 H15 117.0 . . ? C16 C15 H15 117.0 . . ? C17 C16 C21 119.8(4) . . ? C17 C16 C15 117.5(4) . . ? C21 C16 C15 122.7(3) . . ? C18 C17 C16 121.7(4) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 118.8(4) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 121.2(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? O1 C21 C20 119.1(3) . . ? O1 C21 C16 123.7(3) . . ? C20 C21 C16 117.2(3) . . ? O2 C22 C23 118.2(3) . . ? O2 C22 C27 124.0(3) . . ? C23 C22 C27 117.7(3) . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.8(4) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 119.2(4) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 121.1(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C22 119.7(3) . . ? C26 C27 C28 117.8(3) . . ? C22 C27 C28 122.1(3) . . ? N8 C28 C27 125.5(4) . . ? N8 C28 H28 117.3 . . ? C27 C28 H28 117.3 . . ? C30A C29A N7 109.1(6) . . ? C30A C29A C31A 101.7(6) . . ? N7 C29A C31A 108.5(6) . . ? C30A C29A H29A 112.3 . . ? N7 C29A H29A 112.3 . . ? C31A C29A H29A 112.3 . . ? C29A C30A N8 107.2(6) . . ? C29A C30A H30A 110.3 . . ? N8 C30A H30A 110.3 . . ? C29A C30A H30B 110.3 . . ? N8 C30A H30B 110.3 . . ? H30A C30A H30B 108.5 . . ? C29A C31A H31A 109.5 . . ? C29A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C29A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C30B C29B C31B 106.0(16) . . ? C30B C29B N8 115.3(12) . . ? C31B C29B N8 98.1(13) . . ? C30B C29B H29B 112.1 . . ? C31B C29B H29B 112.1 . . ? N8 C29B H29B 112.1 . . ? C29B C30B N7 105.0(14) . . ? C29B C30B H30C 110.8 . . ? N7 C30B H30C 110.8 . . ? C29B C30B H30D 110.7 . . ? N7 C30B H30D 110.7 . . ? H30C C30B H30D 108.8 . . ? C29B C31B H31D 109.5 . . ? C29B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C29B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.813 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.072