# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Marius Andruh' _publ_contact_author_address ; Faculty of Chemistry University of Bucharest Bucharest 020464 ROMANIA ; _publ_contact_author_email MARIUS.ANDRUH@DNT.RO _publ_section_title ; Trinuclear magnetic clusters based on cyanide metal complexes: Synthesis, crystal structures, and magnetic properties of four new [MnII2MIII] complexes (M = Cr, Fe, Co) ; loop_ _publ_author_name 'Marius Andruh' 'Yves Journaux' 'Nathalie Kyritsakas' 'Carmen Paraschiv' 'Louis Ricard' 'Zdirad Zak' data_c1new_a _database_code_depnum_ccdc_archive 'CCDC 294246' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H54 Cr2 Mn3 N27 O8' _chemical_formula_weight 1514.09 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 40.092(8) _cell_length_b 10.399(2) _cell_length_c 17.253(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.43(3) _cell_angle_gamma 90.00 _cell_volume 7187(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4857 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 21.6 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'KUMA KM-4 CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean '0.06 mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every 100 frames' _diffrn_standards_decay_% none _diffrn_reflns_number 29190 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11763 _reflns_number_gt 9452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA Crysalis 168' _computing_cell_refinement 'KUMA Crysalis 168' _computing_data_reduction 'KUMA Crysalis 168' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V5.1' _computing_publication_material SHELXL-97 _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^)+(0.1211P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 11762 _refine_ls_number_parameters 917 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1960 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.003 _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 Mn11 Mn 0.81638(3) -0.14619(13) 0.34672(7) 0.0373(3) Uani 1 1 d . . . O1 O 0.83919(14) -0.0287(6) 0.4431(3) 0.0405(14) Uani 1 1 d . . . N11 N 0.83671(14) -0.0250(7) 0.2461(3) 0.0295(14) Uani 1 1 d . . . N21 N 0.86882(17) -0.2069(7) 0.3228(4) 0.0414(17) Uani 1 1 d . . . N31 N 0.83219(18) -0.3115(8) 0.4259(5) 0.0465(19) Uani 1 1 d . . . N41 N 0.77156(18) -0.1983(7) 0.4198(4) 0.0404(17) Uani 1 1 d . . . N51 N 0.77863(19) 0.0132(8) 0.3195(4) 0.0454(18) Uani 1 1 d . . . C11 C 0.8840(2) 0.0365(9) 0.1717(4) 0.0357(18) Uani 1 1 d . . . H11A' H 0.8682 0.0917 0.1423 0.054 Uiso 1 1 calc R . . H11B' H 0.8947 -0.0227 0.1360 0.054 Uiso 1 1 calc R . . H11C' H 0.9011 0.0898 0.1982 0.054 Uiso 1 1 calc R . . C21 C 0.86612(19) -0.0377(9) 0.2292(4) 0.0344(17) Uani 1 1 d . . . C31 C 0.88590(15) -0.1421(8) 0.2713(4) 0.0279(16) Uani 1 1 d . . . C41 C 0.9181(2) -0.1710(9) 0.2586(6) 0.047(2) Uani 1 1 d . . . H41 H 0.9297 -0.1253 0.2205 0.057 Uiso 1 1 calc R . . C51 C 0.9340(2) -0.2676(10) 0.3015(6) 0.045(2) Uani 1 1 d . . . H51 H 0.9570 -0.2857 0.2967 0.055 Uiso 1 1 calc R . . C61 C 0.9148(2) -0.3359(10) 0.3511(5) 0.050(2) Uani 1 1 d . . . H61 H 0.9238 -0.4098 0.3768 0.061 Uiso 1 1 calc R . . C71 C 0.88296(17) -0.2980(8) 0.3635(4) 0.0272(16) Uani 1 1 d . . . C81 C 0.8601(2) -0.3628(9) 0.4214(5) 0.043(2) Uani 1 1 d . . . C91 C 0.8720(3) -0.4729(11) 0.4659(6) 0.062(3) Uani 1 1 d . . . H91A H 0.8590 -0.4815 0.5126 0.092 Uiso 1 1 calc R . . H91B H 0.8956 -0.4608 0.4811 0.092 Uiso 1 1 calc R . . H91C H 0.8694 -0.5508 0.4343 0.092 Uiso 1 1 calc R . . C101 C 0.8069(2) -0.3596(9) 0.4799(6) 0.048(2) Uani 1 1 d . . . H10A H 0.8179 -0.3869 0.5296 0.058 Uiso 1 1 calc R . . H10B H 0.7948 -0.4343 0.4568 0.058 Uiso 1 1 calc R . . C111 C 0.7832(2) -0.2517(9) 0.4932(6) 0.050(2) Uani 1 1 d . . . H11A H 0.7639 -0.2837 0.5217 0.060 Uiso 1 1 calc R . . H11B H 0.7945 -0.1841 0.5250 0.060 Uiso 1 1 calc R . . C121 C 0.7508(2) -0.0838(9) 0.4247(5) 0.047(2) Uani 1 1 d . . . H12A H 0.7615 -0.0216 0.4615 0.056 Uiso 1 1 calc R . . H12B H 0.7287 -0.1072 0.4439 0.056 Uiso 1 1 calc R . . C131 C 0.7467(2) -0.0243(9) 0.3463(6) 0.052(2) Uani 1 1 d . . . H13A H 0.7361 -0.0867 0.3096 0.063 Uiso 1 1 calc R . . H13B H 0.7320 0.0519 0.3488 0.063 Uiso 1 1 calc R . . C141 C 0.7789(2) 0.0437(10) 0.2338(6) 0.049(2) Uani 1 1 d . . . H14A H 0.7697 -0.0292 0.2029 0.059 Uiso 1 1 calc R . . H14B H 0.7653 0.1211 0.2218 0.059 Uiso 1 1 calc R . . C151 C 0.8141(2) 0.0667(10) 0.2152(6) 0.046(2) Uani 1 1 d . . . H15A H 0.8157 0.0680 0.1581 0.055 Uiso 1 1 calc R . . H15B H 0.8209 0.1526 0.2350 0.055 Uiso 1 1 calc R . . Mn12 Mn 0.65812(3) -0.84141(11) 0.11982(6) 0.0267(3) Uani 1 1 d . . . O2 O 0.61703(12) -0.9201(5) 0.0405(3) 0.0286(12) Uani 1 1 d . . . N12 N 0.62182(16) -0.6811(7) 0.1444(4) 0.0406(17) Uani 1 1 d . . . N22 N 0.62686(15) -0.8981(7) 0.2181(4) 0.0318(15) Uani 1 1 d . . . N32 N 0.67365(16) -1.0396(7) 0.1646(4) 0.0406(17) Uani 1 1 d . . . N42 N 0.69442(17) -0.9284(9) 0.0313(5) 0.054(2) Uani 1 1 d . . . N52 N 0.66907(19) -0.6785(8) 0.0338(4) 0.0462(19) Uani 1 1 d . . . C12 C 0.5784(3) -0.5911(15) 0.2232(8) 0.090(5) Uani 1 1 d . . . H12C' H 0.5822 -0.5713 0.2784 0.135 Uiso 1 1 calc R . . H12D' H 0.5556 -0.6224 0.2139 0.135 Uiso 1 1 calc R . . H12E' H 0.5818 -0.5133 0.1924 0.135 Uiso 1 1 calc R . . C22 C 0.6025(2) -0.6925(9) 0.2000(5) 0.042(2) Uani 1 1 d . . . C32 C 0.60462(18) -0.8124(9) 0.2420(5) 0.0351(19) Uani 1 1 d . . . C42 C 0.5850(2) -0.8426(14) 0.3052(6) 0.059(3) Uani 1 1 d . . . H42 H 0.5691 -0.7831 0.3233 0.071 Uiso 1 1 calc R . . C52 C 0.5895(3) -0.9590(16) 0.3395(5) 0.070(4) Uani 1 1 d . . . H52 H 0.5763 -0.9814 0.3819 0.084 Uiso 1 1 calc R . . C62 C 0.6126(3) -1.0448(13) 0.3147(5) 0.061(3) Uani 1 1 d . . . H62 H 0.6155 -1.1260 0.3392 0.073 Uiso 1 1 calc R . . C72 C 0.6316(2) -1.0092(8) 0.2524(5) 0.038(2) Uani 1 1 d . . . C82 C 0.6570(2) -1.0919(9) 0.2162(6) 0.048(2) Uani 1 1 d . . . C92 C 0.6604(4) -1.2261(10) 0.2451(9) 0.094(5) Uani 1 1 d . . . H92A H 0.6727 -1.2772 0.2081 0.141 Uiso 1 1 calc R . . H92B H 0.6382 -1.2633 0.2508 0.141 Uiso 1 1 calc R . . H92C H 0.6726 -1.2260 0.2956 0.141 Uiso 1 1 calc R . . C102 C 0.6988(3) -1.1024(11) 0.1209(6) 0.062(3) Uani 1 1 d . . . H10C H 0.6881 -1.1679 0.0865 0.075 Uiso 1 1 calc R . . H10D H 0.7148 -1.1470 0.1571 0.075 Uiso 1 1 calc R . . C112 C 0.7172(2) -1.0094(12) 0.0736(6) 0.064(3) Uani 1 1 d . . . H11C H 0.7321 -0.9565 0.1079 0.077 Uiso 1 1 calc R . . H11D H 0.7311 -1.0565 0.0372 0.077 Uiso 1 1 calc R . . C122 C 0.7091(3) -0.8236(15) -0.0111(6) 0.075(4) Uani 1 1 d . . . H12C H 0.7197 -0.8579 -0.0576 0.090 Uiso 1 1 calc R . . H12D H 0.7266 -0.7812 0.0221 0.090 Uiso 1 1 calc R . . C132 C 0.6834(3) -0.7294(12) -0.0348(5) 0.060(3) Uani 1 1 d . . . H13C H 0.6934 -0.6591 -0.0647 0.072 Uiso 1 1 calc R . . H13D H 0.6658 -0.7711 -0.0682 0.072 Uiso 1 1 calc R . . C142 C 0.6379(3) -0.6087(9) 0.0193(6) 0.057(3) Uani 1 1 d . . . H14C H 0.6219 -0.6636 -0.0108 0.069 Uiso 1 1 calc R . . H14D H 0.6421 -0.5307 -0.0116 0.069 Uiso 1 1 calc R . . C152 C 0.6232(3) -0.5710(10) 0.0947(6) 0.060(3) Uani 1 1 d . . . H15C H 0.6371 -0.5031 0.1202 0.072 Uiso 1 1 calc R . . H15D H 0.6004 -0.5361 0.0847 0.072 Uiso 1 1 calc R . . Mn2 Mn 0.47700(3) -0.15461(14) 0.23388(6) 0.0344(3) Uani 1 1 d . . . O3 O 0.46165(17) -0.3084(7) 0.1494(4) 0.0590(19) Uani 1 1 d . A . N14 N 0.43577(14) -0.0312(7) 0.1769(4) 0.0339(15) Uani 1 1 d . A . N24 N 0.42812(15) -0.1987(7) 0.2861(4) 0.0316(15) Uani 1 1 d . A . N34 N 0.48315(19) -0.3162(8) 0.3259(4) 0.046(2) Uani 1 1 d . A . N44 N 0.5351(6) -0.203(3) 0.2649(18) 0.055(8) Uani 0.37 1 d P A 1 N44' N 0.5298(3) -0.2336(15) 0.2201(9) 0.049(3) Uani 0.63 1 d P A 2 N54 N 0.50015(16) -0.0360(9) 0.1356(4) 0.0425(17) Uani 1 1 d . A . C14 C 0.37688(19) 0.0335(9) 0.1679(5) 0.041(2) Uani 1 1 d . A . H14E H 0.3834 0.0837 0.1229 0.061 Uiso 1 1 calc R . . H14F H 0.3695 0.0918 0.2084 0.061 Uiso 1 1 calc R . . H14G H 0.3586 -0.0247 0.1524 0.061 Uiso 1 1 calc R . . C24 C 0.40562(18) -0.0419(9) 0.1979(4) 0.0340(17) Uani 1 1 d . . . C34 C 0.40078(17) -0.1387(8) 0.2604(4) 0.0289(16) Uani 1 1 d . A . C44 C 0.37000(17) -0.1671(9) 0.2885(5) 0.0366(19) Uani 1 1 d . . . H44 H 0.3504 -0.1236 0.2698 0.044 Uiso 1 1 calc R A . C54 C 0.3686(2) -0.2627(9) 0.3457(5) 0.038(2) Uani 1 1 d . A . H54 H 0.3479 -0.2824 0.3679 0.045 Uiso 1 1 calc R . . C64 C 0.3960(2) -0.3257(8) 0.3690(4) 0.0377(19) Uani 1 1 d . . . H64 H 0.3949 -0.3939 0.4054 0.045 Uiso 1 1 calc R A . C74 C 0.42554(18) -0.2917(7) 0.3402(4) 0.0276(16) Uani 1 1 d . A . C84 C 0.4586(2) -0.3566(9) 0.3606(5) 0.042(2) Uani 1 1 d . . . C94 C 0.4590(3) -0.4566(11) 0.4216(6) 0.060(3) Uani 1 1 d . A . H94A H 0.4428 -0.5240 0.4071 0.090 Uiso 1 1 calc R . . H94B H 0.4531 -0.4179 0.4710 0.090 Uiso 1 1 calc R . . H94C H 0.4814 -0.4943 0.4272 0.090 Uiso 1 1 calc R . . C104 C 0.5175(2) -0.3668(10) 0.3377(7) 0.061(3) Uani 1 1 d . . . H10E H 0.5186 -0.4571 0.3198 0.073 Uiso 1 1 calc R A . H10F H 0.5246 -0.3635 0.3933 0.073 Uiso 1 1 calc R . . C114 C 0.5396(3) -0.2823(18) 0.2906(8) 0.081(5) Uani 1 1 d . A . H11E H 0.5593 -0.2646 0.3256 0.097 Uiso 1 1 calc R B 1 H11F H 0.5477 -0.3397 0.2496 0.097 Uiso 1 1 calc R B 1 C124 C 0.55009(19) -0.1566(13) 0.1796(6) 0.058(3) Uani 1 1 d . . . H12E H 0.5748 -0.1538 0.1840 0.070 Uiso 1 1 calc R A 1 H12F H 0.5435 -0.2201 0.1390 0.070 Uiso 1 1 calc R A 1 C134 C 0.5378(4) -0.035(2) 0.1579(14) 0.047(5) Uani 0.46 1 d P A 1 H13E H 0.5502 -0.0032 0.1133 0.056 Uiso 0.46 1 calc PR A 1 H13F H 0.5419 0.0256 0.2015 0.056 Uiso 0.46 1 calc PR A 1 C13' C 0.5292(4) -0.100(2) 0.1044(10) 0.050(5) Uani 0.54 1 d P A 2 H13G H 0.5429 -0.0385 0.0759 0.060 Uiso 0.54 1 calc PR A 2 H13H H 0.5221 -0.1707 0.0688 0.060 Uiso 0.54 1 calc PR A 2 C144 C 0.4849(5) 0.070(3) 0.1282(12) 0.057(7) Uani 0.44 1 d P A 1 H14H H 0.4933 0.1164 0.0829 0.068 Uiso 0.44 1 calc PR A 1 H14I H 0.4900 0.1233 0.1748 0.068 Uiso 0.44 1 calc PR A 1 C14' C 0.4738(4) -0.005(2) 0.0776(9) 0.053(5) Uani 0.56 1 d P A 2 H14J H 0.4661 -0.0847 0.0507 0.063 Uiso 0.56 1 calc PR A 2 H14K H 0.4824 0.0544 0.0384 0.063 Uiso 0.56 1 calc PR A 2 C154 C 0.4455(2) 0.0558(10) 0.1172(5) 0.047(2) Uani 1 1 d . . . H15E H 0.4344 0.1403 0.1229 0.057 Uiso 1 1 calc R A 1 H15F H 0.4393 0.0207 0.0653 0.057 Uiso 1 1 calc R A 1 Cr2 Cr 0.5000 0.04059(16) 0.5000 0.0226(3) Uani 1 2 d S . . C15 C 0.49389(16) 0.0217(8) 0.3824(4) 0.0265(16) Uani 1 1 d . . . N15 N 0.49057(15) -0.0049(7) 0.3171(3) 0.0307(15) Uani 1 1 d . A . C25 C 0.53495(19) 0.1818(9) 0.4863(4) 0.0326(18) Uani 1 1 d . . . N25 N 0.5535(2) 0.2623(9) 0.4741(4) 0.051(2) Uani 1 1 d . A . C35 C 0.53670(17) -0.0960(8) 0.4921(4) 0.0269(17) Uani 1 1 d . . . N35 N 0.55755(15) -0.1714(7) 0.4851(4) 0.0353(16) Uani 1 1 d . A . Cr3 Cr 0.5000 -0.57654(18) 0.0000 0.0307(4) Uani 1 2 d S . . C16 C 0.49058(18) -0.5831(10) 0.1171(6) 0.046(2) Uani 1 1 d . . . N16 N 0.4859(2) -0.5750(10) 0.1800(5) 0.059(2) Uani 1 1 d . . . C26 C 0.5367(2) -0.7090(9) 0.0249(6) 0.048(2) Uani 1 1 d . . . N26 N 0.5578(2) -0.7826(9) 0.0381(6) 0.072(3) Uani 1 1 d . . . C36 C 0.53530(18) -0.4322(8) 0.0177(4) 0.0298(17) Uani 1 1 d . . . N36 N 0.55424(18) -0.3544(8) 0.0223(5) 0.0479(19) Uani 1 1 d . . . Cr1 Cr 0.75091(2) -0.53772(11) 0.23698(6) 0.0198(2) Uani 1 1 d . . . C13 C 0.7809(2) -0.3785(8) 0.2495(5) 0.038(2) Uani 1 1 d . . . N13 N 0.79580(18) -0.2863(7) 0.2587(4) 0.0433(18) Uani 1 1 d . . . C23 C 0.71762(16) -0.6867(7) 0.2189(4) 0.0236(15) Uani 1 1 d . . . N23 N 0.69832(16) -0.7566(7) 0.1991(4) 0.0368(16) Uani 1 1 d . . . C33 C 0.72291(16) -0.4513(7) 0.3208(4) 0.0243(15) Uani 1 1 d . . . N33 N 0.71108(17) -0.4005(7) 0.3690(4) 0.0363(16) Uani 1 1 d . . . C43 C 0.72435(17) -0.4562(7) 0.1455(4) 0.0260(15) Uani 1 1 d . . . N43 N 0.70859(16) -0.4204(7) 0.0918(4) 0.0338(15) Uani 1 1 d . . . C53 C 0.77570(16) -0.6344(8) 0.3260(4) 0.0267(16) Uani 1 1 d . . . N53 N 0.78850(15) -0.6889(7) 0.3776(4) 0.0324(15) Uani 1 1 d . . . C63 C 0.78256(17) -0.6098(7) 0.1571(4) 0.0239(15) Uani 1 1 d . . . N63 N 0.80065(16) -0.6459(8) 0.1128(4) 0.0383(16) Uani 1 1 d . . . OW1 O 0.82390(12) 0.1992(5) 0.5071(3) 0.0313(12) Uani 1 1 d D . . HW1A H 0.8140 0.1754 0.5503 0.047 Uiso 1 1 d RD . . HW1B H 0.8203 0.2824 0.4967 0.047 Uiso 1 1 d RD . . OW2 O 0.66363(12) -0.3093(5) -0.0198(3) 0.0341(13) Uani 1 1 d D . . HW2A H 0.6798 -0.3407 0.0211 0.051 Uiso 1 1 d RD . . HW2B H 0.6745 -0.2480 -0.0466 0.051 Uiso 1 1 d RD . . OW3 O 0.88953(14) 0.1817(6) 0.5741(3) 0.0414(14) Uani 1 1 d D . . HW3A H 0.9053 0.2265 0.5619 0.062 Uiso 1 1 d RD . . HW3B H 0.8783 0.2402 0.5663 0.062 Uiso 1 1 d RD . . OW4 O 0.61043(15) -1.1783(6) 0.0294(6) 0.076(3) Uani 1 1 d D . . HW4A H 0.6132 -1.1055 0.0554 0.113 Uiso 1 1 d RD . . HW4B H 0.5941 -1.2339 0.0145 0.113 Uiso 1 1 d RD . . OW5 O 0.8891(3) -0.0863(13) 0.5476(6) 0.075(3) Uani 0.78 1 d P C 1 OW5' O 0.8780(10) -0.175(3) 0.5460(16) 0.064(11) Uani 0.22 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn11 0.0360(6) 0.0338(7) 0.0423(7) -0.0037(6) 0.0048(5) -0.0075(6) O1 0.049(3) 0.032(3) 0.040(3) -0.002(3) 0.001(2) -0.015(3) N11 0.026(3) 0.033(4) 0.029(3) 0.001(3) -0.007(2) 0.005(3) N21 0.043(4) 0.036(4) 0.044(4) 0.007(3) -0.001(3) 0.000(3) N31 0.042(4) 0.032(4) 0.066(5) -0.007(4) 0.007(4) -0.002(3) N41 0.053(4) 0.027(4) 0.042(4) -0.005(3) 0.008(3) -0.011(3) N51 0.052(4) 0.042(5) 0.041(4) -0.003(3) -0.009(3) -0.004(4) C11 0.042(4) 0.034(5) 0.032(4) 0.009(4) -0.001(3) -0.008(4) C21 0.040(4) 0.029(4) 0.034(4) -0.008(4) -0.003(3) -0.003(4) C31 0.020(3) 0.038(5) 0.025(3) -0.001(3) -0.004(3) -0.008(3) C41 0.044(4) 0.041(6) 0.056(6) 0.007(5) -0.003(4) -0.007(4) C51 0.030(4) 0.052(6) 0.054(6) -0.006(5) 0.000(4) 0.003(4) C61 0.054(5) 0.047(6) 0.049(5) 0.004(5) -0.019(4) 0.013(5) C71 0.030(3) 0.028(4) 0.023(4) 0.004(3) -0.009(3) -0.002(3) C81 0.046(5) 0.042(6) 0.042(5) -0.004(4) -0.003(4) -0.001(4) C91 0.082(7) 0.045(6) 0.058(6) 0.009(5) 0.007(5) 0.007(6) C101 0.055(5) 0.037(6) 0.054(6) 0.007(5) 0.006(4) 0.004(4) C111 0.061(5) 0.027(5) 0.065(6) -0.021(5) 0.030(5) -0.005(4) C121 0.058(5) 0.035(5) 0.049(5) -0.013(4) 0.018(4) -0.002(4) C131 0.058(5) 0.027(5) 0.075(7) -0.006(5) 0.023(5) 0.002(4) C141 0.052(5) 0.037(5) 0.059(6) -0.013(5) -0.001(4) -0.006(4) C151 0.039(4) 0.045(6) 0.052(6) -0.006(4) -0.015(4) 0.000(4) Mn12 0.0277(5) 0.0265(6) 0.0255(6) 0.0007(5) -0.0039(4) -0.0080(5) O2 0.028(2) 0.028(3) 0.030(3) -0.002(2) -0.007(2) -0.006(2) N12 0.037(3) 0.034(4) 0.049(4) -0.008(4) -0.016(3) -0.003(3) N22 0.028(3) 0.035(4) 0.033(4) 0.002(3) 0.000(3) -0.007(3) N32 0.039(3) 0.028(4) 0.053(4) -0.020(4) -0.024(3) 0.004(3) N42 0.030(3) 0.084(7) 0.048(5) -0.031(5) 0.005(3) 0.000(4) N52 0.064(5) 0.040(5) 0.034(4) 0.000(3) -0.001(3) -0.022(4) C12 0.085(8) 0.102(12) 0.082(9) -0.033(8) -0.005(7) 0.050(8) C22 0.039(4) 0.041(6) 0.045(5) -0.019(4) -0.009(4) 0.011(4) C32 0.025(3) 0.050(6) 0.030(4) -0.006(4) -0.009(3) 0.003(3) C42 0.031(4) 0.105(10) 0.041(5) -0.029(7) 0.009(4) 0.000(5) C52 0.063(7) 0.119(11) 0.026(5) -0.003(7) -0.004(5) -0.048(8) C62 0.086(7) 0.067(7) 0.027(5) 0.003(5) -0.019(5) -0.027(7) C72 0.038(4) 0.033(5) 0.041(5) 0.005(4) -0.010(4) -0.015(4) C82 0.045(5) 0.031(5) 0.065(6) 0.008(5) -0.025(5) -0.003(4) C92 0.136(12) 0.020(6) 0.124(12) 0.016(7) -0.017(10) 0.022(7) C102 0.055(6) 0.065(8) 0.063(7) -0.037(6) -0.041(5) 0.024(5) C112 0.027(4) 0.096(10) 0.069(7) -0.039(7) -0.009(4) 0.011(5) C122 0.051(6) 0.129(12) 0.045(6) -0.026(7) 0.016(5) -0.035(7) C132 0.063(6) 0.088(9) 0.030(5) -0.005(5) 0.007(4) -0.027(6) C142 0.082(7) 0.036(6) 0.050(6) 0.020(4) -0.036(5) -0.028(5) C152 0.067(6) 0.044(6) 0.066(7) -0.005(5) -0.032(5) 0.002(5) Mn2 0.0248(5) 0.0508(8) 0.0277(6) -0.0099(6) 0.0013(4) -0.0026(6) O3 0.069(4) 0.058(5) 0.050(4) -0.024(3) 0.006(3) -0.011(4) N14 0.029(3) 0.042(4) 0.031(3) -0.001(3) -0.002(3) 0.000(3) N24 0.029(3) 0.035(4) 0.031(3) -0.006(3) -0.003(3) 0.002(3) N34 0.052(4) 0.041(5) 0.043(4) -0.015(4) -0.020(4) 0.013(4) N44 0.039(12) 0.08(2) 0.051(17) -0.042(16) -0.023(11) 0.013(12) N44' 0.031(6) 0.060(10) 0.056(9) 0.018(8) -0.010(6) 0.009(6) N54 0.035(3) 0.058(5) 0.035(4) 0.003(4) 0.008(3) 0.003(4) C14 0.033(4) 0.044(5) 0.045(5) 0.000(4) -0.003(3) -0.004(4) C24 0.037(4) 0.035(5) 0.030(4) -0.005(4) -0.002(3) -0.009(4) C34 0.029(3) 0.029(4) 0.029(4) -0.003(3) -0.002(3) -0.008(3) C44 0.023(3) 0.047(6) 0.038(4) -0.012(4) -0.005(3) 0.003(4) C54 0.037(4) 0.049(6) 0.029(4) -0.011(4) 0.016(3) -0.016(4) C64 0.061(5) 0.025(5) 0.028(4) -0.009(3) 0.015(4) -0.014(4) C74 0.038(4) 0.022(4) 0.023(4) -0.003(3) -0.008(3) -0.005(3) C84 0.066(6) 0.034(5) 0.023(4) -0.010(4) -0.011(4) 0.007(4) C94 0.076(7) 0.056(7) 0.047(6) -0.001(5) -0.011(5) 0.006(6) C104 0.043(5) 0.043(6) 0.094(8) -0.028(6) -0.031(5) 0.019(4) C114 0.043(6) 0.139(15) 0.062(8) 0.032(9) 0.011(5) 0.045(8) C124 0.026(4) 0.092(9) 0.057(6) -0.010(6) 0.000(4) -0.008(5) C134 0.032(9) 0.048(13) 0.062(14) 0.018(12) 0.020(9) 0.002(9) C13' 0.024(7) 0.089(16) 0.037(9) 0.012(9) 0.010(6) 0.025(8) C144 0.048(12) 0.09(2) 0.034(11) 0.022(12) 0.023(9) -0.030(13) C14' 0.046(9) 0.081(15) 0.031(8) 0.008(9) 0.004(7) 0.038(9) C154 0.048(5) 0.050(6) 0.044(5) 0.007(5) 0.003(4) -0.002(5) Cr2 0.0224(7) 0.0259(9) 0.0196(8) 0.000 0.0003(6) 0.000 C15 0.019(3) 0.030(4) 0.031(4) -0.005(3) 0.007(3) -0.001(3) N15 0.030(3) 0.042(4) 0.020(3) 0.000(3) -0.002(2) 0.001(3) C25 0.043(4) 0.039(5) 0.017(3) -0.005(3) 0.005(3) -0.007(4) N25 0.063(5) 0.066(6) 0.024(4) -0.003(4) 0.000(3) -0.025(5) C35 0.025(3) 0.040(5) 0.015(3) 0.010(3) 0.000(3) 0.002(3) N35 0.030(3) 0.041(4) 0.035(4) 0.000(3) 0.004(3) 0.003(3) Cr3 0.0206(7) 0.0344(11) 0.0366(10) 0.000 -0.0062(7) 0.000 C16 0.018(3) 0.053(6) 0.065(6) -0.011(5) 0.001(4) -0.005(4) N16 0.062(5) 0.084(7) 0.032(4) 0.007(4) 0.013(4) -0.005(5) C26 0.042(5) 0.031(5) 0.070(7) -0.014(5) -0.024(4) 0.003(4) N26 0.062(5) 0.048(6) 0.101(7) -0.029(5) -0.047(5) 0.023(5) C36 0.031(4) 0.036(5) 0.023(4) 0.004(3) 0.001(3) -0.001(4) N36 0.042(4) 0.033(4) 0.068(5) 0.006(4) -0.001(4) -0.011(4) Cr1 0.0187(5) 0.0186(6) 0.0221(5) -0.0008(5) 0.0012(4) -0.0003(4) C13 0.035(4) 0.035(5) 0.045(5) -0.015(4) 0.022(4) -0.007(4) N13 0.047(4) 0.033(4) 0.050(4) -0.011(4) 0.013(3) -0.016(4) C23 0.024(3) 0.023(4) 0.024(4) -0.007(3) 0.002(3) -0.002(3) N23 0.031(3) 0.041(4) 0.038(4) -0.002(3) -0.004(3) -0.013(3) C33 0.024(3) 0.020(4) 0.028(4) 0.004(3) -0.002(3) -0.001(3) N33 0.043(4) 0.035(4) 0.031(4) -0.005(3) 0.008(3) 0.011(3) C43 0.032(3) 0.019(4) 0.027(4) 0.006(3) -0.001(3) -0.004(3) N43 0.039(3) 0.029(4) 0.034(4) -0.004(3) -0.002(3) 0.005(3) C53 0.020(3) 0.031(4) 0.029(4) -0.009(3) 0.000(3) 0.002(3) N53 0.030(3) 0.039(4) 0.028(3) -0.003(3) -0.003(3) 0.006(3) C63 0.026(3) 0.026(4) 0.020(3) -0.002(3) -0.002(3) 0.004(3) N63 0.038(3) 0.045(4) 0.033(3) 0.006(4) 0.010(3) 0.007(3) OW1 0.032(3) 0.029(3) 0.033(3) 0.016(2) 0.008(2) 0.004(2) OW2 0.035(3) 0.030(3) 0.037(3) 0.014(2) -0.001(2) -0.006(2) OW3 0.049(3) 0.033(4) 0.041(3) 0.000(3) -0.002(3) -0.009(3) OW4 0.036(3) 0.027(4) 0.166(8) -0.021(4) 0.028(4) -0.017(3) OW5 0.064(6) 0.077(9) 0.084(8) 0.004(7) -0.007(5) 0.033(6) OW5' 0.13(3) 0.035(19) 0.032(15) -0.011(14) 0.030(17) -0.03(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 Mn11 O1 2.229(6) . ? Mn11 N13 2.237(7) . ? Mn11 N21 2.250(7) . ? Mn11 N31 2.269(8) . ? Mn11 N51 2.280(8) . ? Mn11 N41 2.303(7) . ? Mn11 N11 2.320(7) . ? N11 C21 1.234(10) . ? N11 C151 1.404(11) . ? N21 C71 1.295(10) . ? N21 C31 1.327(10) . ? N31 C81 1.246(11) . ? N31 C101 1.493(12) . ? N41 C111 1.441(13) . ? N41 C121 1.457(12) . ? N51 C131 1.432(12) . ? N51 C141 1.514(12) . ? C11 C21 1.468(11) . ? C21 C31 1.513(12) . ? C31 C41 1.350(11) . ? C41 C51 1.387(13) . ? C51 C61 1.372(14) . ? C61 C71 1.363(12) . ? C71 C81 1.540(12) . ? C81 C91 1.448(14) . ? C101 C111 1.496(12) . ? C121 C131 1.490(14) . ? C141 C151 1.479(13) . ? Mn12 N22 2.230(7) . ? Mn12 N23 2.249(6) . ? Mn12 O2 2.250(5) . ? Mn12 N12 2.265(7) . ? Mn12 N32 2.279(8) . ? Mn12 N52 2.307(7) . ? Mn12 N42 2.336(7) . ? N12 C22 1.263(12) . ? N12 C152 1.433(13) . ? N22 C72 1.308(10) . ? N22 C32 1.338(10) . ? N32 C82 1.259(13) . ? N32 C102 1.441(13) . ? N42 C112 1.421(14) . ? N42 C122 1.451(15) . ? N52 C132 1.437(12) . ? N52 C142 1.457(13) . ? C12 C22 1.496(13) . ? C22 C32 1.442(13) . ? C32 C42 1.405(13) . ? C42 C52 1.356(18) . ? C52 C62 1.367(17) . ? C62 C72 1.396(13) . ? C72 C82 1.489(14) . ? C82 C92 1.486(14) . ? C102 C112 1.480(16) . ? C122 C132 1.468(18) . ? C142 C152 1.503(15) . ? Mn2 N15 2.172(7) . ? Mn2 O3 2.233(6) . ? Mn2 N24 2.239(6) . ? Mn2 N14 2.282(6) . ? Mn2 N44' 2.293(12) . ? Mn2 N34 2.318(8) . ? Mn2 N54 2.323(8) . ? Mn2 N44 2.42(2) . ? N14 C24 1.282(10) . ? N14 C154 1.437(11) . ? N24 C34 1.322(9) . ? N24 C74 1.351(10) . ? N34 C84 1.247(12) . ? N34 C104 1.479(10) . ? N44 C114 0.95(3) . ? N44 C124 1.68(4) . ? N44' C124 1.356(17) . ? N44' C114 1.360(17) . ? N54 C144 1.27(3) . ? N54 C14' 1.459(16) . ? N54 C13' 1.465(16) . ? N54 C134 1.54(2) . ? C14 C24 1.470(12) . ? C24 C34 1.493(11) . ? C34 C44 1.377(10) . ? C44 C54 1.404(12) . ? C54 C64 1.327(12) . ? C64 C74 1.350(11) . ? C74 C84 1.515(11) . ? C84 C94 1.479(14) . ? C104 C114 1.510(18) . ? C124 C134 1.40(2) . ? C124 C13' 1.622(18) . ? C144 C154 1.59(2) . ? C14' C154 1.492(17) . ? Cr2 C15 2.043(7) 2_656 ? Cr2 C15 2.043(7) . ? Cr2 C25 2.051(8) 2_656 ? Cr2 C25 2.051(8) . ? Cr2 C35 2.054(8) 2_656 ? Cr2 C35 2.054(8) . ? C15 N15 1.162(9) . ? C25 N25 1.146(11) . ? C35 N35 1.156(10) . ? Cr3 C26 2.049(9) 2_655 ? Cr3 C26 2.049(9) . ? Cr3 C16 2.073(11) . ? Cr3 C16 2.073(10) 2_655 ? Cr3 C36 2.076(8) . ? Cr3 C36 2.076(8) 2_655 ? C16 N16 1.111(11) . ? C26 N26 1.154(12) . ? C36 N36 1.110(10) . ? Cr1 C43 2.050(7) . ? Cr1 C13 2.053(8) . ? Cr1 C63 2.054(7) . ? Cr1 C53 2.057(8) . ? Cr1 C23 2.060(7) . ? Cr1 C33 2.073(8) . ? C13 N13 1.137(10) . ? C23 N23 1.105(9) . ? C33 N33 1.109(10) . ? C43 N43 1.161(9) . ? C53 N53 1.156(9) . ? C63 N63 1.140(9) . ? 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 Mn11 N13 172.6(3) . . ? O1 Mn11 N21 86.2(3) . . ? N13 Mn11 N21 90.7(3) . . ? O1 Mn11 N31 82.6(3) . . ? N13 Mn11 N31 90.0(3) . . ? N21 Mn11 N31 70.0(3) . . ? O1 Mn11 N51 90.2(3) . . ? N13 Mn11 N51 96.4(3) . . ? N21 Mn11 N51 141.6(3) . . ? N31 Mn11 N51 147.2(3) . . ? O1 Mn11 N41 91.4(2) . . ? N13 Mn11 N41 86.8(3) . . ? N21 Mn11 N41 142.3(3) . . ? N31 Mn11 N41 72.3(3) . . ? N51 Mn11 N41 76.0(3) . . ? O1 Mn11 N11 96.6(2) . . ? N13 Mn11 N11 88.7(2) . . ? N21 Mn11 N11 69.8(2) . . ? N31 Mn11 N11 139.8(2) . . ? N51 Mn11 N11 72.7(3) . . ? N41 Mn11 N11 147.6(2) . . ? C21 N11 C151 126.1(8) . . ? C21 N11 Mn11 119.3(6) . . ? C151 N11 Mn11 114.3(5) . . ? C71 N21 C31 120.5(7) . . ? C71 N21 Mn11 119.8(6) . . ? C31 N21 Mn11 119.5(5) . . ? C81 N31 C101 122.1(8) . . ? C81 N31 Mn11 121.1(7) . . ? C101 N31 Mn11 116.8(5) . . ? C111 N41 C121 115.3(7) . . ? C111 N41 Mn11 110.0(5) . . ? C121 N41 Mn11 107.4(5) . . ? C131 N51 C141 114.7(7) . . ? C131 N51 Mn11 109.3(6) . . ? C141 N51 Mn11 108.7(6) . . ? N11 C21 C11 127.2(8) . . ? N11 C21 C31 116.7(7) . . ? C11 C21 C31 116.1(7) . . ? N21 C31 C41 121.3(8) . . ? N21 C31 C21 114.3(6) . . ? C41 C31 C21 124.5(7) . . ? C31 C41 C51 119.7(9) . . ? C61 C51 C41 116.8(8) . . ? C71 C61 C51 120.0(9) . . ? N21 C71 C61 121.3(8) . . ? N21 C71 C81 114.4(7) . . ? C61 C71 C81 124.2(8) . . ? N31 C81 C91 125.6(9) . . ? N31 C81 C71 114.4(8) . . ? C91 C81 C71 119.9(8) . . ? N31 C101 C111 107.3(8) . . ? N41 C111 C101 109.8(7) . . ? N41 C121 C131 109.2(7) . . ? N51 C131 C121 109.9(8) . . ? C151 C141 N51 107.1(7) . . ? N11 C151 C141 114.4(8) . . ? N22 Mn12 N23 93.0(2) . . ? N22 Mn12 O2 86.9(2) . . ? N23 Mn12 O2 178.1(3) . . ? N22 Mn12 N12 70.5(3) . . ? N23 Mn12 N12 92.7(2) . . ? O2 Mn12 N12 85.5(2) . . ? N22 Mn12 N32 70.0(3) . . ? N23 Mn12 N32 88.3(2) . . ? O2 Mn12 N32 93.4(2) . . ? N12 Mn12 N32 140.4(3) . . ? N22 Mn12 N52 144.3(3) . . ? N23 Mn12 N52 87.2(3) . . ? O2 Mn12 N52 91.7(2) . . ? N12 Mn12 N52 73.8(3) . . ? N32 Mn12 N52 145.7(3) . . ? N22 Mn12 N42 141.3(3) . . ? N23 Mn12 N42 95.7(3) . . ? O2 Mn12 N42 85.5(2) . . ? N12 Mn12 N42 146.2(3) . . ? N32 Mn12 N42 72.7(3) . . ? N52 Mn12 N42 73.9(3) . . ? C22 N12 C152 124.8(8) . . ? C22 N12 Mn12 119.5(6) . . ? C152 N12 Mn12 115.8(7) . . ? C72 N22 C32 122.4(7) . . ? C72 N22 Mn12 120.1(6) . . ? C32 N22 Mn12 117.5(5) . . ? C82 N32 C102 125.4(9) . . ? C82 N32 Mn12 119.0(6) . . ? C102 N32 Mn12 114.8(7) . . ? C112 N42 C122 116.1(8) . . ? C112 N42 Mn12 107.3(6) . . ? C122 N42 Mn12 108.4(7) . . ? C132 N52 C142 114.3(8) . . ? C132 N52 Mn12 110.6(7) . . ? C142 N52 Mn12 106.9(5) . . ? N12 C22 C32 116.0(8) . . ? N12 C22 C12 124.0(10) . . ? C32 C22 C12 120.0(10) . . ? N22 C32 C42 119.4(9) . . ? N22 C32 C22 116.5(7) . . ? C42 C32 C22 124.0(9) . . ? C52 C42 C32 118.1(10) . . ? C42 C52 C62 121.6(10) . . ? C52 C62 C72 117.9(11) . . ? N22 C72 C62 120.6(9) . . ? N22 C72 C82 114.2(8) . . ? C62 C72 C82 125.2(9) . . ? N32 C82 C92 126.7(11) . . ? N32 C82 C72 116.1(8) . . ? C92 C82 C72 117.2(11) . . ? N32 C102 C112 111.6(9) . . ? N42 C112 C102 110.4(8) . . ? N42 C122 C132 110.3(8) . . ? N52 C132 C122 108.5(8) . . ? N52 C142 C152 110.3(7) . . ? N12 C152 C142 109.6(9) . . ? N15 Mn2 O3 178.5(2) . . ? N15 Mn2 N24 94.6(2) . . ? O3 Mn2 N24 83.9(2) . . ? N15 Mn2 N14 92.2(2) . . ? O3 Mn2 N14 87.0(3) . . ? N24 Mn2 N14 70.0(2) . . ? N15 Mn2 N44' 96.8(5) . . ? O3 Mn2 N44' 84.6(5) . . ? N24 Mn2 N44' 142.8(4) . . ? N14 Mn2 N44' 144.3(4) . . ? N15 Mn2 N34 92.9(2) . . ? O3 Mn2 N34 86.9(3) . . ? N24 Mn2 N34 69.2(3) . . ? N14 Mn2 N34 139.2(3) . . ? N44' Mn2 N34 74.9(4) . . ? N15 Mn2 N54 90.3(3) . . ? O3 Mn2 N54 90.6(3) . . ? N24 Mn2 N54 141.9(2) . . ? N14 Mn2 N54 72.0(2) . . ? N44' Mn2 N54 73.5(4) . . ? N34 Mn2 N54 148.3(3) . . ? N15 Mn2 N44 77.9(6) . . ? O3 Mn2 N44 103.4(6) . . ? N24 Mn2 N44 136.0(9) . . ? N14 Mn2 N44 152.1(9) . . ? N44' Mn2 N44 20.7(6) . . ? N34 Mn2 N44 68.0(9) . . ? N54 Mn2 N44 82.0(9) . . ? C24 N14 C154 123.0(7) . . ? C24 N14 Mn2 120.2(6) . . ? C154 N14 Mn2 116.7(5) . . ? C34 N24 C74 118.9(6) . . ? C34 N24 Mn2 119.7(5) . . ? C74 N24 Mn2 121.2(5) . . ? C84 N34 C104 124.3(9) . . ? C84 N34 Mn2 120.7(6) . . ? C104 N34 Mn2 115.0(7) . . ? C114 N44 C124 126(2) . . ? C114 N44 Mn2 116(2) . . ? C124 N44 Mn2 97.1(15) . . ? C124 N44' C114 121.7(13) . . ? C124 N44' Mn2 114.7(9) . . ? C114 N44' Mn2 105.9(10) . . ? C144 N54 C14' 53.6(13) . . ? C144 N54 C13' 138.6(13) . . ? C14' N54 C13' 114.4(10) . . ? C144 N54 C134 118.9(15) . . ? C14' N54 C134 147.4(12) . . ? C13' N54 C134 46.3(11) . . ? C144 N54 Mn2 109.2(9) . . ? C14' N54 Mn2 108.5(8) . . ? C13' N54 Mn2 112.0(9) . . ? C134 N54 Mn2 103.8(8) . . ? N14 C24 C14 126.0(8) . . ? N14 C24 C34 114.6(7) . . ? C14 C24 C34 119.3(7) . . ? N24 C34 C44 121.5(8) . . ? N24 C34 C24 115.4(6) . . ? C44 C34 C24 123.0(7) . . ? C34 C44 C54 117.6(7) . . ? C64 C54 C44 120.4(7) . . ? C54 C64 C74 119.2(8) . . ? C64 C74 N24 122.4(7) . . ? C64 C74 C84 124.7(8) . . ? N24 C74 C84 112.8(7) . . ? N34 C84 C94 126.4(9) . . ? N34 C84 C74 116.0(8) . . ? C94 C84 C74 117.5(9) . . ? N34 C104 C114 106.5(9) . . ? N44 C114 N44' 38.5(15) . . ? N44 C114 C104 131(2) . . ? N44' C114 C104 122.9(12) . . ? N44' C124 C134 117.3(11) . . ? N44' C124 C13' 109.0(10) . . ? C134 C124 C13' 45.4(12) . . ? N44' C124 N44 30.3(9) . . ? C134 C124 N44 110.8(15) . . ? C13' C124 N44 127.6(11) . . ? C124 C134 N54 113.0(15) . . ? N54 C13' C124 105.3(11) . . ? N54 C144 C154 113.9(17) . . ? N54 C14' C154 108.8(11) . . ? N14 C154 C14' 107.1(10) . . ? N14 C154 C144 105.7(10) . . ? C14' C154 C144 47.4(12) . . ? C15 Cr2 C15 169.0(5) 2_656 . ? C15 Cr2 C25 90.5(3) 2_656 2_656 ? C15 Cr2 C25 97.4(3) . 2_656 ? C15 Cr2 C25 97.4(3) 2_656 . ? C15 Cr2 C25 90.5(3) . . ? C25 Cr2 C25 88.5(5) 2_656 . ? C15 Cr2 C35 85.6(3) 2_656 2_656 ? C15 Cr2 C35 86.8(3) . 2_656 ? C25 Cr2 C35 89.6(3) 2_656 2_656 ? C25 Cr2 C35 176.4(3) . 2_656 ? C15 Cr2 C35 86.8(3) 2_656 . ? C15 Cr2 C35 85.6(3) . . ? C25 Cr2 C35 176.4(3) 2_656 . ? C25 Cr2 C35 89.6(3) . . ? C35 Cr2 C35 92.5(4) 2_656 . ? N15 C15 Cr2 171.7(7) . . ? C15 N15 Mn2 145.8(6) . . ? N25 C25 Cr2 175.6(7) . . ? N35 C35 Cr2 177.6(6) . . ? C26 Cr3 C26 95.5(5) 2_655 . ? C26 Cr3 C16 91.3(4) 2_655 . ? C26 Cr3 C16 86.1(4) . . ? C26 Cr3 C16 86.1(4) 2_655 2_655 ? C26 Cr3 C16 91.3(4) . 2_655 ? C16 Cr3 C16 176.2(6) . 2_655 ? C26 Cr3 C36 175.0(3) 2_655 . ? C26 Cr3 C36 88.6(3) . . ? C16 Cr3 C36 91.8(3) . . ? C16 Cr3 C36 90.9(3) 2_655 . ? C26 Cr3 C36 88.6(3) 2_655 2_655 ? C26 Cr3 C36 175.0(3) . 2_655 ? C16 Cr3 C36 90.9(3) . 2_655 ? C16 Cr3 C36 91.8(3) 2_655 2_655 ? C36 Cr3 C36 87.4(4) . 2_655 ? N16 C16 Cr3 173.7(10) . . ? N26 C26 Cr3 178.8(11) . . ? N36 C36 Cr3 175.7(7) . . ? C43 Cr1 C13 91.8(3) . . ? C43 Cr1 C63 87.1(3) . . ? C13 Cr1 C63 89.4(3) . . ? C43 Cr1 C53 175.1(3) . . ? C13 Cr1 C53 93.0(3) . . ? C63 Cr1 C53 91.7(3) . . ? C43 Cr1 C23 83.3(3) . . ? C13 Cr1 C23 174.7(3) . . ? C63 Cr1 C23 92.2(3) . . ? C53 Cr1 C23 92.0(3) . . ? C43 Cr1 C33 94.5(3) . . ? C13 Cr1 C33 84.8(3) . . ? C63 Cr1 C33 174.0(3) . . ? C53 Cr1 C33 87.1(3) . . ? C23 Cr1 C33 93.8(3) . . ? N13 C13 Cr1 175.4(7) . . ? C13 N13 Mn11 145.1(7) . . ? N23 C23 Cr1 169.1(7) . . ? C23 N23 Mn12 157.0(7) . . ? N33 C33 Cr1 172.5(7) . . ? N43 C43 Cr1 174.2(7) . . ? N53 C53 Cr1 177.4(6) . . ? N63 C63 Cr1 177.7(7) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 3.594 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.109 data_jmp110m _database_code_depnum_ccdc_archive 'CCDC 294247' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H42 Cr Mn2 N13 O5 S,1.5(O2)' _chemical_formula_sum 'C37 H42 Cr Mn2 N13 O8 S' _chemical_formula_weight 990.78 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7483(2) _cell_length_b 11.5277(3) _cell_length_c 11.6016(3) _cell_angle_alpha 68.5041(11) _cell_angle_beta 86.9896(11) _cell_angle_gamma 78.3951(12) _cell_volume 1187.93(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8668 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 30.80 _exptl_crystal_description quadratic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 1.385 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 509 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8618 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_process_details sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58977 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.80 _reflns_number_total 7400 _reflns_number_gt 6108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.8915P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7400 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1778 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.002 _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 0.73563(4) 0.73104(3) 0.74450(3) 0.02412(12) Uani 1 1 d . . . Cr1 Cr 0.5000 0.5000 0.5000 0.02083(13) Uani 1 2 d S . . N1 N 0.5824(2) 0.7563(2) 0.88540(19) 0.0272(4) Uani 1 1 d . . . C1 C 0.5779(3) 0.6586(3) 0.9923(2) 0.0312(5) Uani 1 1 d . . . C2 C 0.4851(3) 0.6745(3) 1.0842(3) 0.0413(6) Uani 1 1 d . . . H2 H 0.4797 0.6054 1.1595 0.050 Uiso 1 1 calc R . . C3 C 0.4019(3) 0.7927(4) 1.0631(3) 0.0478(8) Uani 1 1 d . . . H3 H 0.3388 0.8050 1.1247 0.057 Uiso 1 1 calc R . . C4 C 0.4091(3) 0.8937(3) 0.9528(3) 0.0412(6) Uani 1 1 d . . . H4 H 0.3528 0.9754 0.9382 0.049 Uiso 1 1 calc R . . C5 C 0.5019(3) 0.8713(3) 0.8642(2) 0.0291(5) Uani 1 1 d . . . C6 C 0.5237(3) 0.9710(2) 0.7423(2) 0.0290(5) Uani 1 1 d . . . C7 C 0.4299(3) 1.0992(3) 0.7051(3) 0.0425(6) Uani 1 1 d . . . H7A H 0.4483 1.1422 0.7599 0.064 Uiso 1 1 calc R . . H7B H 0.3319 1.0895 0.7118 0.064 Uiso 1 1 calc R . . H7C H 0.4482 1.1499 0.6194 0.064 Uiso 1 1 calc R . . N2 N 0.6246(2) 0.93656(19) 0.67898(19) 0.0271(4) Uani 1 1 d . . . C8 C 0.6655(3) 1.0221(2) 0.5597(3) 0.0345(5) Uani 1 1 d . . . H8A H 0.6600 1.1078 0.5622 0.041 Uiso 1 1 calc R . . H8B H 0.6013 1.0295 0.4929 0.041 Uiso 1 1 calc R . . C9 C 0.8139(3) 0.9684(3) 0.5346(3) 0.0401(6) Uani 1 1 d . . . H9A H 0.8376 1.0144 0.4480 0.048 Uiso 1 1 calc R . . H9B H 0.8806 0.9778 0.5906 0.048 Uiso 1 1 calc R . . O1 O 0.8224(2) 0.83578(18) 0.55599(19) 0.0358(4) Uani 1 1 d . . . C10 C 0.9580(3) 0.7718(3) 0.5352(3) 0.0483(8) Uani 1 1 d . . . H10A H 1.0309 0.7859 0.5822 0.058 Uiso 1 1 calc R . . H10B H 0.9797 0.8042 0.4460 0.058 Uiso 1 1 calc R . . C11 C 0.9535(3) 0.6316(3) 0.5792(3) 0.0446(7) Uani 1 1 d . . . H11A H 0.8807 0.6173 0.5323 0.053 Uiso 1 1 calc R . . H11B H 1.0452 0.5821 0.5676 0.053 Uiso 1 1 calc R . . O2 O 0.9209(2) 0.59408(18) 0.70899(19) 0.0352(4) Uani 1 1 d . . . C12 C 0.9007(3) 0.4653(3) 0.7645(3) 0.0377(6) Uani 1 1 d . . . H12A H 0.9870 0.4057 0.7588 0.045 Uiso 1 1 calc R . . H12B H 0.8233 0.4527 0.7212 0.045 Uiso 1 1 calc R . . C13 C 0.8652(3) 0.4415(3) 0.8999(3) 0.0405(6) Uani 1 1 d . . . H13A H 0.8343 0.3591 0.9377 0.049 Uiso 1 1 calc R . . H13B H 0.9492 0.4378 0.9465 0.049 Uiso 1 1 calc R . . N3 N 0.7533(3) 0.5446(2) 0.9060(2) 0.0330(4) Uani 1 1 d . . . C14 C 0.6820(3) 0.5394(3) 1.0028(2) 0.0339(5) Uani 1 1 d . . . C15 C 0.6987(4) 0.4288(3) 1.1233(3) 0.0486(8) Uani 1 1 d . . . H15A H 0.7541 0.3535 1.1111 0.073 Uiso 1 1 calc R . . H15B H 0.6062 0.4123 1.1538 0.073 Uiso 1 1 calc R . . H15C H 0.7468 0.4484 1.1841 0.073 Uiso 1 1 calc R . . N4 N 0.5948(2) 0.6644(2) 0.64546(19) 0.0281(4) Uani 1 1 d . . . C16 C 0.5543(2) 0.6069(2) 0.5957(2) 0.0240(4) Uani 1 1 d . . . C17 C 0.3424(3) 0.6509(2) 0.4028(2) 0.0273(4) Uani 1 1 d . . . N5 N 0.2525(3) 0.7325(2) 0.3496(2) 0.0381(5) Uani 1 1 d . . . C18 C 0.6480(2) 0.5687(2) 0.3710(2) 0.0265(4) Uani 1 1 d . . . N6 N 0.7295(2) 0.6091(2) 0.3000(2) 0.0362(5) Uani 1 1 d . . . N7 N 0.9015(5) 0.7920(4) 0.8259(4) 0.02412(12) Uani 0.50 1 d P . . C19 C 0.9908(6) 0.8327(5) 0.8246(5) 0.0333(10) Uani 0.50 1 d P . . S1 S 1.12558(17) 0.89817(16) 0.8133(2) 0.0586(5) Uani 0.50 1 d P . . O5 O 0.8838(4) 0.7752(3) 0.8567(3) 0.02412(12) Uani 0.50 1 d P . . O6 O 0.1928(3) 0.2021(3) 0.9183(2) 0.0551(6) Uani 1 1 d . . . O7 O 0.9575(7) 0.1416(5) 0.8421(8) 0.106(3) Uani 0.50 1 d P . . 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 0.02624(19) 0.02284(18) 0.02377(19) -0.00955(13) 0.00100(13) -0.00394(13) Cr1 0.0223(2) 0.0204(2) 0.0203(2) -0.00902(18) -0.00102(17) -0.00179(17) N1 0.0288(9) 0.0320(10) 0.0231(9) -0.0120(8) 0.0007(7) -0.0073(8) C1 0.0334(12) 0.0383(13) 0.0223(10) -0.0086(9) -0.0020(9) -0.0114(10) C2 0.0358(13) 0.0632(19) 0.0227(11) -0.0105(12) 0.0011(10) -0.0150(13) C3 0.0314(13) 0.081(2) 0.0293(13) -0.0222(15) 0.0049(10) -0.0054(14) C4 0.0306(12) 0.0586(18) 0.0337(13) -0.0222(13) 0.0001(10) 0.0029(12) C5 0.0256(10) 0.0375(12) 0.0267(11) -0.0163(10) -0.0012(8) -0.0024(9) C6 0.0299(11) 0.0269(11) 0.0321(12) -0.0146(9) -0.0020(9) -0.0015(9) C7 0.0424(15) 0.0306(13) 0.0494(17) -0.0156(12) 0.0028(12) 0.0057(11) N2 0.0295(9) 0.0242(9) 0.0281(10) -0.0101(7) 0.0002(8) -0.0048(7) C8 0.0375(13) 0.0237(11) 0.0369(13) -0.0048(9) 0.0029(10) -0.0065(9) C9 0.0366(13) 0.0314(13) 0.0464(16) -0.0058(11) 0.0111(12) -0.0120(11) O1 0.0317(9) 0.0318(9) 0.0394(10) -0.0103(8) 0.0124(8) -0.0043(7) C10 0.0360(14) 0.0515(18) 0.0501(18) -0.0154(14) 0.0194(13) -0.0031(13) C11 0.0387(15) 0.0462(16) 0.0469(16) -0.0226(13) 0.0107(12) 0.0043(12) O2 0.0340(9) 0.0313(9) 0.0402(10) -0.0160(8) 0.0012(8) -0.0008(7) C12 0.0362(13) 0.0261(11) 0.0512(16) -0.0184(11) -0.0072(12) 0.0036(10) C13 0.0472(15) 0.0240(11) 0.0449(15) -0.0092(10) -0.0124(12) 0.0021(10) N3 0.0398(12) 0.0255(9) 0.0302(10) -0.0059(8) -0.0067(9) -0.0047(8) C14 0.0455(14) 0.0299(12) 0.0251(11) -0.0048(9) -0.0080(10) -0.0124(10) C15 0.077(2) 0.0360(14) 0.0284(13) -0.0028(11) -0.0050(14) -0.0178(15) N4 0.0311(10) 0.0274(9) 0.0274(9) -0.0120(8) -0.0004(8) -0.0053(8) C16 0.0242(10) 0.0238(10) 0.0231(10) -0.0088(8) 0.0008(8) -0.0024(8) C17 0.0297(11) 0.0263(10) 0.0267(11) -0.0111(9) 0.0011(8) -0.0043(9) N5 0.0360(11) 0.0343(11) 0.0369(12) -0.0092(9) -0.0030(9) 0.0025(9) C18 0.0267(10) 0.0245(10) 0.0269(10) -0.0100(8) -0.0021(8) 0.0000(8) N6 0.0319(11) 0.0390(12) 0.0343(11) -0.0116(9) 0.0057(9) -0.0040(9) N7 0.02624(19) 0.02284(18) 0.02377(19) -0.00955(13) 0.00100(13) -0.00394(13) C19 0.036(3) 0.028(2) 0.033(2) -0.0084(19) -0.007(2) -0.0016(19) S1 0.0334(7) 0.0357(7) 0.1031(16) -0.0174(9) -0.0151(8) -0.0098(6) O5 0.02624(19) 0.02284(18) 0.02377(19) -0.00955(13) 0.00100(13) -0.00394(13) O6 0.0571(15) 0.0555(14) 0.0452(13) -0.0086(11) 0.0055(11) -0.0142(12) O7 0.087(4) 0.035(2) 0.158(7) 0.028(3) -0.099(5) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N1 2.215(2) . ? Mn1 O5 2.240(4) . ? Mn1 N4 2.243(2) . ? Mn1 N3 2.257(2) . ? Mn1 N2 2.258(2) . ? Mn1 N7 2.259(5) . ? Mn1 O2 2.2750(19) . ? Mn1 O1 2.2886(19) . ? Cr1 C18 2.077(2) . ? Cr1 C18 2.077(2) 2_666 ? Cr1 C17 2.080(2) 2_666 ? Cr1 C17 2.080(2) . ? Cr1 C16 2.087(2) . ? Cr1 C16 2.087(2) 2_666 ? N1 C5 1.340(3) . ? N1 C1 1.342(3) . ? C1 C2 1.401(4) . ? C1 C14 1.504(4) . ? C2 C3 1.380(5) . ? C2 H2 0.9500 . ? C3 C4 1.390(5) . ? C3 H3 0.9500 . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? C5 C6 1.497(4) . ? C6 N2 1.283(3) . ? C6 C7 1.495(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N2 C8 1.465(3) . ? C8 C9 1.513(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O1 1.442(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O1 C10 1.433(3) . ? C10 C11 1.516(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.444(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O2 C12 1.435(3) . ? C12 C13 1.525(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.462(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N3 C14 1.278(4) . ? C14 C15 1.497(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? N4 C16 1.157(3) . ? C17 N5 1.155(3) . ? C18 N6 1.151(3) . ? N7 C19 1.066(7) . ? C19 O5 1.312(7) . ? C19 S1 1.619(6) . ? 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 Mn1 O5 84.04(10) . . ? N1 Mn1 N4 95.90(8) . . ? O5 Mn1 N4 173.72(11) . . ? N1 Mn1 N3 71.16(8) . . ? O5 Mn1 N3 84.73(11) . . ? N4 Mn1 N3 89.30(8) . . ? N1 Mn1 N2 71.42(8) . . ? O5 Mn1 N2 89.02(11) . . ? N4 Mn1 N2 96.92(8) . . ? N3 Mn1 N2 142.49(8) . . ? N1 Mn1 N7 92.27(12) . . ? O5 Mn1 N7 9.91(12) . . ? N4 Mn1 N7 171.80(12) . . ? N3 Mn1 N7 92.61(12) . . ? N2 Mn1 N7 86.40(13) . . ? N1 Mn1 O2 143.55(8) . . ? O5 Mn1 O2 87.11(11) . . ? N4 Mn1 O2 89.27(7) . . ? N3 Mn1 O2 72.86(8) . . ? N2 Mn1 O2 143.79(8) . . ? N7 Mn1 O2 83.68(12) . . ? N1 Mn1 O1 143.34(8) . . ? O5 Mn1 O1 95.75(10) . . ? N4 Mn1 O1 88.06(8) . . ? N3 Mn1 O1 145.47(8) . . ? N2 Mn1 O1 71.92(7) . . ? N7 Mn1 O1 85.85(12) . . ? O2 Mn1 O1 72.69(7) . . ? C18 Cr1 C18 180.00(9) . 2_666 ? C18 Cr1 C17 88.19(9) . 2_666 ? C18 Cr1 C17 91.81(9) 2_666 2_666 ? C18 Cr1 C17 91.81(9) . . ? C18 Cr1 C17 88.19(9) 2_666 . ? C17 Cr1 C17 179.999(2) 2_666 . ? C18 Cr1 C16 87.25(9) . . ? C18 Cr1 C16 92.75(9) 2_666 . ? C17 Cr1 C16 89.47(9) 2_666 . ? C17 Cr1 C16 90.53(9) . . ? C18 Cr1 C16 92.75(9) . 2_666 ? C18 Cr1 C16 87.25(9) 2_666 2_666 ? C17 Cr1 C16 90.53(9) 2_666 2_666 ? C17 Cr1 C16 89.46(9) . 2_666 ? C16 Cr1 C16 179.999(1) . 2_666 ? C5 N1 C1 121.7(2) . . ? C5 N1 Mn1 118.80(16) . . ? C1 N1 Mn1 119.38(17) . . ? N1 C1 C2 120.0(3) . . ? N1 C1 C14 114.2(2) . . ? C2 C1 C14 125.7(3) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.8(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 117.8(3) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 114.9(2) . . ? C4 C5 C6 124.1(2) . . ? N2 C6 C7 125.9(2) . . ? N2 C6 C5 115.2(2) . . ? C7 C6 C5 118.9(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 N2 C8 123.2(2) . . ? C6 N2 Mn1 119.29(17) . . ? C8 N2 Mn1 117.34(16) . . ? N2 C8 C9 108.5(2) . . ? N2 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N2 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O1 C9 C8 107.7(2) . . ? O1 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O1 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C10 O1 C9 114.0(2) . . ? C10 O1 Mn1 112.83(18) . . ? C9 O1 Mn1 111.72(16) . . ? O1 C10 C11 106.8(2) . . ? O1 C10 H10A 110.4 . . ? C11 C10 H10A 110.4 . . ? O1 C10 H10B 110.4 . . ? C11 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? O2 C11 C10 106.0(2) . . ? O2 C11 H11A 110.5 . . ? C10 C11 H11A 110.5 . . ? O2 C11 H11B 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? C12 O2 C11 113.9(2) . . ? C12 O2 Mn1 110.85(16) . . ? C11 O2 Mn1 111.89(16) . . ? O2 C12 C13 107.4(2) . . ? O2 C12 H12A 110.2 . . ? C13 C12 H12A 110.2 . . ? O2 C12 H12B 110.2 . . ? C13 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? N3 C13 C12 108.9(2) . . ? N3 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? N3 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C14 N3 C13 123.6(2) . . ? C14 N3 Mn1 119.65(19) . . ? C13 N3 Mn1 115.96(18) . . ? N3 C14 C15 125.6(3) . . ? N3 C14 C1 115.2(2) . . ? C15 C14 C1 119.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 N4 Mn1 161.81(19) . . ? N4 C16 Cr1 174.7(2) . . ? N5 C17 Cr1 178.2(2) . . ? N6 C18 Cr1 178.6(2) . . ? C19 N7 Mn1 156.0(4) . . ? N7 C19 S1 176.4(5) . . ? O5 C19 S1 169.0(5) . . ? C19 O5 Mn1 131.5(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.80 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.750 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.175 data_mnfe _database_code_depnum_ccdc_archive 'CCDC 294248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MnLFe(CN)6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H49 Fe Mn2 N13 O7.50 S' _chemical_formula_weight 993.68 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' S S 0.1246 0.1234 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.478(5) _cell_length_b 13.805(5) _cell_length_c 17.086(5) _cell_angle_alpha 90.00 _cell_angle_beta 125.900(5) _cell_angle_gamma 90.00 _cell_volume 4486(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour brownish _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(10) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 11202 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6540 _reflns_number_gt 5414 _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^)+(0.0593P)^2^+5.1622P] 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 6540 _refine_ls_number_parameters 297 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.156 _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 Fe1 Fe 0.2500 0.2500 1.0000 0.01732(10) Uani 1 2 d S . . Mn1 Mn 0.151330(15) 0.35230(2) 0.646616(19) 0.01581(9) Uani 1 1 d . . . O1 O 0.15642(8) 0.50086(10) 0.70966(10) 0.0233(3) Uani 1 1 d . . . O2 O 0.04875(8) 0.37124(11) 0.63019(11) 0.0258(3) Uani 1 1 d . . . N1 N 0.08790(9) 0.21524(13) 0.58113(13) 0.0235(3) Uani 1 1 d . . . N2 N 0.20614(9) 0.25512(11) 0.60769(11) 0.0176(3) Uani 1 1 d . . . N3 N 0.24809(9) 0.42747(12) 0.67940(11) 0.0196(3) Uani 1 1 d . . . N4 N 0.20527(10) 0.29330(13) 0.79389(12) 0.0252(4) Uani 1 1 d . . . N5 N 0.34374(11) 0.07406(14) 1.03364(14) 0.0298(4) Uani 1 1 d . . . N6 N 0.38136(13) 0.37956(17) 1.08777(17) 0.0434(5) Uani 1 1 d . . . O3 O 0.09295(7) 0.42401(10) 0.50210(10) 0.0227(3) Uani 1 1 d . . . C1 C 0.10735(13) 0.15180(15) 0.54739(17) 0.0275(4) Uani 1 1 d . . . C2 C 0.17835(11) 0.16872(14) 0.56850(14) 0.0216(4) Uani 1 1 d . . . C3 C 0.21474(13) 0.10123(15) 0.55257(15) 0.0281(4) Uani 1 1 d . . . H3 H 0.1947 0.0401 0.5241 0.034 Uiso 1 1 calc R . . C4 C 0.28119(13) 0.12630(17) 0.57958(16) 0.0301(5) Uani 1 1 d . . . H4 H 0.3075 0.0814 0.5706 0.036 Uiso 1 1 calc R . . C5 C 0.30946(11) 0.21621(16) 0.61952(15) 0.0256(4) Uani 1 1 d . . . H5 H 0.3548 0.2339 0.6375 0.031 Uiso 1 1 calc R . . C6 C 0.26975(10) 0.28022(14) 0.63265(13) 0.0186(3) Uani 1 1 d . . . C7 C 0.29306(10) 0.38024(15) 0.67528(14) 0.0208(4) Uani 1 1 d . . . C8 C 0.26169(12) 0.52456(15) 0.72079(16) 0.0263(4) Uani 1 1 d . . . H8A H 0.2839 0.5649 0.6976 0.032 Uiso 1 1 calc R . . H8B H 0.2943 0.5208 0.7921 0.032 Uiso 1 1 calc R . . C9 C 0.19276(12) 0.56986(15) 0.69067(15) 0.0259(4) Uani 1 1 d . . . H9A H 0.2018 0.6301 0.7278 0.031 Uiso 1 1 calc R . . H9B H 0.1639 0.5862 0.6210 0.031 Uiso 1 1 calc R . . C10 C 0.08738(12) 0.53145(16) 0.67780(16) 0.0295(5) Uani 1 1 d . . . H10A H 0.0593 0.5510 0.6090 0.035 Uiso 1 1 calc R . . H10B H 0.0907 0.5874 0.7165 0.035 Uiso 1 1 calc R . . C11 C 0.05351(12) 0.44689(17) 0.69091(16) 0.0299(5) Uani 1 1 d . . . H11A H 0.0823 0.4258 0.7593 0.036 Uiso 1 1 calc R . . H11B H 0.0061 0.4647 0.6719 0.036 Uiso 1 1 calc R . . C12 C 0.02263(13) 0.28042(18) 0.63811(19) 0.0336(5) Uani 1 1 d . . . H12A H -0.0249 0.2888 0.6226 0.040 Uiso 1 1 calc R . . H12B H 0.0543 0.2546 0.7046 0.040 Uiso 1 1 calc R . . C13 C 0.01989(13) 0.21184(19) 0.56654(19) 0.0353(5) Uani 1 1 d . . . H13A H 0.0101 0.1451 0.5769 0.042 Uiso 1 1 calc R . . H13B H -0.0181 0.2315 0.4997 0.042 Uiso 1 1 calc R . . C14 C 0.06568(18) 0.0647(2) 0.4893(3) 0.0609(10) Uani 1 1 d . . . H14A H 0.0858 0.0065 0.5297 0.091 Uiso 1 1 calc R . . H14B H 0.0673 0.0583 0.4335 0.091 Uiso 1 1 calc R . . H14C H 0.0168 0.0723 0.4669 0.091 Uiso 1 1 calc R . . C15 C 0.36443(12) 0.4153(2) 0.71000(19) 0.0375(5) Uani 1 1 d . . . H15A H 0.3700 0.4830 0.7307 0.056 Uiso 1 1 calc R . . H15B H 0.3699 0.4106 0.6575 0.056 Uiso 1 1 calc R . . H15C H 0.4003 0.3754 0.7646 0.056 Uiso 1 1 calc R . . C16 C 0.22352(11) 0.27525(14) 0.87119(14) 0.0207(4) Uani 1 1 d . . . C17 C 0.30821(11) 0.13924(14) 1.01958(14) 0.0218(4) Uani 1 1 d . . . C18 C 0.33197(12) 0.33219(15) 1.05509(15) 0.0265(4) Uani 1 1 d . . . S1 S 0.51877(6) 0.24543(9) 0.84372(7) 0.0259(2) Uani 0.50 1 d PD . 1 C19 C 0.5000 0.2166(3) 0.7500 0.0445(7) Uani 1 2 d SD . 1 N7 N 0.4777(3) 0.2009(4) 0.6633(3) 0.0445(7) Uani 0.50 1 d PD . 1 O4 O -0.0103(3) -0.0383(4) 0.2760(4) 0.103(3) Uani 0.50 1 d P . 1 O5 O 0.1376(4) -0.1534(8) 0.6062(6) 0.058(2) Uani 0.25 1 d P . . 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 Fe1 0.0254(2) 0.01444(18) 0.01191(17) 0.00183(12) 0.01080(16) 0.00383(14) Mn1 0.01729(15) 0.01748(15) 0.01286(14) 0.00048(9) 0.00895(12) 0.00088(10) O1 0.0264(7) 0.0215(7) 0.0216(7) -0.0002(5) 0.0138(6) 0.0046(6) O2 0.0250(7) 0.0322(8) 0.0258(7) 0.0005(6) 0.0181(7) 0.0014(6) N1 0.0247(9) 0.0242(8) 0.0232(8) -0.0011(7) 0.0149(7) -0.0053(7) N2 0.0213(8) 0.0181(7) 0.0140(7) 0.0013(5) 0.0107(7) 0.0014(6) N3 0.0215(8) 0.0196(7) 0.0160(7) -0.0020(6) 0.0101(6) -0.0025(6) N4 0.0312(9) 0.0268(9) 0.0172(8) 0.0031(6) 0.0140(7) 0.0049(7) N5 0.0420(11) 0.0252(9) 0.0291(9) 0.0046(7) 0.0246(9) 0.0087(8) N6 0.0408(13) 0.0353(11) 0.0379(12) 0.0005(9) 0.0139(10) -0.0068(10) O3 0.0232(7) 0.0243(7) 0.0162(6) 0.0032(5) 0.0091(6) -0.0015(6) C1 0.0343(12) 0.0227(10) 0.0284(11) -0.0054(8) 0.0200(10) -0.0087(8) C2 0.0296(10) 0.0194(8) 0.0169(8) 0.0005(7) 0.0143(8) -0.0001(7) C3 0.0439(13) 0.0209(9) 0.0231(10) -0.0006(8) 0.0217(10) 0.0040(9) C4 0.0425(13) 0.0289(10) 0.0252(10) 0.0051(8) 0.0234(10) 0.0151(9) C5 0.0256(10) 0.0320(11) 0.0223(10) 0.0057(8) 0.0157(9) 0.0092(8) C6 0.0198(9) 0.0215(9) 0.0152(8) 0.0034(7) 0.0105(7) 0.0036(7) C7 0.0199(9) 0.0246(9) 0.0165(8) 0.0023(7) 0.0098(8) -0.0009(7) C8 0.0288(11) 0.0224(9) 0.0241(10) -0.0075(8) 0.0135(9) -0.0067(8) C9 0.0360(11) 0.0187(9) 0.0220(9) -0.0032(7) 0.0165(9) -0.0014(8) C10 0.0285(11) 0.0312(11) 0.0264(10) -0.0017(8) 0.0147(9) 0.0102(9) C11 0.0282(11) 0.0413(13) 0.0245(10) 0.0010(9) 0.0178(9) 0.0102(9) C12 0.0301(11) 0.0411(13) 0.0409(13) 0.0012(10) 0.0271(11) -0.0047(10) C13 0.0284(11) 0.0414(13) 0.0401(13) -0.0104(11) 0.0223(11) -0.0140(10) C14 0.0597(19) 0.0483(17) 0.090(3) -0.0430(17) 0.052(2) -0.0321(15) C15 0.0244(11) 0.0477(14) 0.0410(13) -0.0085(11) 0.0195(11) -0.0098(10) C16 0.0275(10) 0.0184(8) 0.0165(8) 0.0020(7) 0.0129(8) 0.0049(7) C17 0.0325(11) 0.0193(8) 0.0164(8) 0.0022(7) 0.0159(8) 0.0031(8) C18 0.0312(11) 0.0222(9) 0.0186(9) 0.0035(7) 0.0104(9) 0.0030(8) S1 0.0265(5) 0.0306(6) 0.0178(5) -0.0021(4) 0.0115(4) 0.0003(4) C19 0.0367(16) 0.0370(15) 0.066(2) 0.000 0.0338(18) 0.000 N7 0.0367(16) 0.0370(15) 0.066(2) 0.000 0.0338(18) 0.000 O4 0.048(3) 0.088(3) 0.076(5) -0.047(3) -0.018(3) 0.041(3) O5 0.030(4) 0.102(8) 0.036(4) -0.018(4) 0.016(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C16 1.936(2) 7_557 ? Fe1 C16 1.936(2) . ? Fe1 C18 1.937(2) 7_557 ? Fe1 C18 1.937(2) . ? Fe1 C17 1.945(2) 7_557 ? Fe1 C17 1.945(2) . ? Mn1 N4 2.2050(18) . ? Mn1 N2 2.2139(16) . ? Mn1 O3 2.2331(15) . ? Mn1 N3 2.2492(17) . ? Mn1 N1 2.2573(19) . ? Mn1 O2 2.2703(16) . ? Mn1 O1 2.2868(16) . ? O1 C9 1.437(3) . ? O1 C10 1.438(3) . ? O2 C11 1.430(3) . ? O2 C12 1.437(3) . ? N1 C1 1.272(3) . ? N1 C13 1.465(3) . ? N2 C2 1.336(3) . ? N2 C6 1.336(2) . ? N3 C7 1.277(3) . ? N3 C8 1.461(3) . ? N4 C16 1.152(3) . ? N5 C17 1.152(3) . ? N6 C18 1.151(3) . ? C1 C14 1.500(3) . ? C1 C2 1.503(3) . ? C2 C3 1.395(3) . ? C3 C4 1.386(3) . ? C4 C5 1.384(3) . ? C5 C6 1.395(3) . ? C6 C7 1.506(3) . ? C7 C15 1.493(3) . ? C8 C9 1.516(3) . ? C10 C11 1.501(3) . ? C12 C13 1.518(3) . ? S1 N7 0.641(5) 2_656 ? S1 C19 1.4453(16) . ? C19 N7 1.268(4) 2_656 ? C19 N7 1.268(4) . ? C19 S1 1.4454(16) 2_656 ? N7 S1 0.641(5) 2_656 ? O4 O4 1.236(13) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Fe1 C16 180.0 7_557 . ? C16 Fe1 C18 90.70(9) 7_557 7_557 ? C16 Fe1 C18 89.30(9) . 7_557 ? C16 Fe1 C18 89.30(9) 7_557 . ? C16 Fe1 C18 90.70(9) . . ? C18 Fe1 C18 180.0 7_557 . ? C16 Fe1 C17 93.56(8) 7_557 7_557 ? C16 Fe1 C17 86.45(8) . 7_557 ? C18 Fe1 C17 88.82(9) 7_557 7_557 ? C18 Fe1 C17 91.19(9) . 7_557 ? C16 Fe1 C17 86.45(8) 7_557 . ? C16 Fe1 C17 93.55(8) . . ? C18 Fe1 C17 91.18(9) 7_557 . ? C18 Fe1 C17 88.81(9) . . ? C17 Fe1 C17 179.997(1) 7_557 . ? N4 Mn1 N2 94.18(6) . . ? N4 Mn1 O3 174.29(6) . . ? N2 Mn1 O3 91.40(6) . . ? N4 Mn1 N3 93.77(7) . . ? N2 Mn1 N3 70.99(6) . . ? O3 Mn1 N3 86.92(6) . . ? N4 Mn1 N1 91.52(7) . . ? N2 Mn1 N1 70.97(6) . . ? O3 Mn1 N1 91.42(6) . . ? N3 Mn1 N1 141.87(6) . . ? N4 Mn1 O2 92.38(6) . . ? N2 Mn1 O2 142.55(6) . . ? O3 Mn1 O2 83.88(5) . . ? N3 Mn1 O2 145.18(6) . . ? N1 Mn1 O2 72.03(6) . . ? N4 Mn1 O1 87.55(6) . . ? N2 Mn1 O1 143.69(6) . . ? O3 Mn1 O1 87.24(6) . . ? N3 Mn1 O1 72.70(6) . . ? N1 Mn1 O1 145.31(6) . . ? O2 Mn1 O1 73.36(6) . . ? C9 O1 C10 113.99(16) . . ? C9 O1 Mn1 111.23(11) . . ? C10 O1 Mn1 110.43(12) . . ? C11 O2 C12 115.16(17) . . ? C11 O2 Mn1 111.64(12) . . ? C12 O2 Mn1 111.61(13) . . ? C1 N1 C13 123.10(19) . . ? C1 N1 Mn1 119.61(14) . . ? C13 N1 Mn1 116.59(14) . . ? C2 N2 C6 121.16(17) . . ? C2 N2 Mn1 119.51(13) . . ? C6 N2 Mn1 119.00(13) . . ? C7 N3 C8 122.81(18) . . ? C7 N3 Mn1 119.83(14) . . ? C8 N3 Mn1 116.49(13) . . ? C16 N4 Mn1 165.27(16) . . ? N1 C1 C14 125.7(2) . . ? N1 C1 C2 115.27(18) . . ? C14 C1 C2 119.0(2) . . ? N2 C2 C3 121.3(2) . . ? N2 C2 C1 113.96(17) . . ? C3 C2 C1 124.72(19) . . ? C4 C3 C2 117.8(2) . . ? C5 C4 C3 120.57(19) . . ? C4 C5 C6 118.4(2) . . ? N2 C6 C5 120.78(19) . . ? N2 C6 C7 114.40(16) . . ? C5 C6 C7 124.82(18) . . ? N3 C7 C15 125.7(2) . . ? N3 C7 C6 114.64(17) . . ? C15 C7 C6 119.62(18) . . ? N3 C8 C9 109.11(17) . . ? O1 C9 C8 107.86(16) . . ? O1 C10 C11 107.06(17) . . ? O2 C11 C10 106.40(16) . . ? O2 C12 C13 106.69(18) . . ? N1 C13 C12 108.41(18) . . ? N4 C16 Fe1 176.65(18) . . ? N5 C17 Fe1 178.28(18) . . ? N6 C18 Fe1 178.7(2) . . ? N7 S1 C19 61.2(4) 2_656 . ? N7 C19 N7 160.3(6) 2_656 . ? N7 C19 S1 26.3(2) 2_656 . ? N7 C19 S1 172.2(4) . . ? N7 C19 S1 172.2(4) 2_656 2_656 ? N7 C19 S1 26.3(2) . 2_656 ? S1 C19 S1 148.1(3) . 2_656 ? S1 N7 C19 92.5(5) 2_656 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.827 _refine_diff_density_min -1.623 _refine_diff_density_rms 0.079 data_mnco _database_code_depnum_ccdc_archive 'CCDC 294249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common MnLCo(CN)6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H49 Co Mn2 N13 O7.50 S' _chemical_formula_weight 996.76 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.460(5) _cell_length_b 13.766(5) _cell_length_c 17.047(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 125.998(5) _cell_angle_gamma 90.000(5) _cell_volume 4454(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 10792 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6473 _reflns_number_gt 5340 _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^)+(0.0577P)^2^+5.0934P] 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 6473 _refine_ls_number_parameters 297 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 1.0000 0.01530(10) Uani 1 2 d S . . Mn1 Mn 0.151772(15) 0.35128(2) 0.64772(2) 0.01448(9) Uani 1 1 d . . . O1 O 0.15694(8) 0.49992(10) 0.71133(11) 0.0213(3) Uani 1 1 d . . . O2 O 0.04908(8) 0.37002(11) 0.63090(11) 0.0238(3) Uani 1 1 d . . . N1 N 0.08781(10) 0.21400(13) 0.58098(13) 0.0218(4) Uani 1 1 d . . . N2 N 0.20631(9) 0.25447(11) 0.60789(12) 0.0163(3) Uani 1 1 d . . . N3 N 0.24874(9) 0.42654(12) 0.68121(12) 0.0182(3) Uani 1 1 d . . . N4 N 0.20595(10) 0.29172(13) 0.79581(13) 0.0236(4) Uani 1 1 d . . . N5 N 0.34131(11) 0.07586(14) 1.03015(14) 0.0275(4) Uani 1 1 d . . . N6 N 0.37984(12) 0.37776(16) 1.08692(17) 0.0378(5) Uani 1 1 d . . . O3 O 0.09384(8) 0.42541(10) 0.50343(10) 0.0216(3) Uani 1 1 d . . . C1 C 0.10705(13) 0.15088(15) 0.54640(17) 0.0252(5) Uani 1 1 d . . . C2 C 0.17818(12) 0.16795(14) 0.56760(14) 0.0199(4) Uani 1 1 d . . . C3 C 0.21433(13) 0.10051(15) 0.55107(16) 0.0260(5) Uani 1 1 d . . . H3 H 0.1940 0.0394 0.5220 0.031 Uiso 1 1 calc R . . C4 C 0.28084(13) 0.12546(17) 0.57833(16) 0.0274(5) Uani 1 1 d . . . H4 H 0.3071 0.0805 0.5691 0.033 Uiso 1 1 calc R . . C5 C 0.30952(12) 0.21570(17) 0.61914(15) 0.0240(4) Uani 1 1 d . . . H5 H 0.3549 0.2334 0.6372 0.029 Uiso 1 1 calc R . . C6 C 0.27007(11) 0.27946(14) 0.63286(14) 0.0176(4) Uani 1 1 d . . . C7 C 0.29355(11) 0.37956(15) 0.67618(14) 0.0191(4) Uani 1 1 d . . . C8 C 0.26266(12) 0.52366(15) 0.72324(16) 0.0247(4) Uani 1 1 d . . . H8A H 0.2851 0.5642 0.7004 0.030 Uiso 1 1 calc R . . H8B H 0.2952 0.5196 0.7948 0.030 Uiso 1 1 calc R . . C9 C 0.19342(13) 0.56912(15) 0.69258(16) 0.0240(4) Uani 1 1 d . . . H9A H 0.2024 0.6295 0.7298 0.029 Uiso 1 1 calc R . . H9B H 0.1646 0.5855 0.6227 0.029 Uiso 1 1 calc R . . C10 C 0.08778(12) 0.53081(16) 0.67880(17) 0.0274(5) Uani 1 1 d . . . H10A H 0.0598 0.5503 0.6098 0.033 Uiso 1 1 calc R . . H10B H 0.0910 0.5870 0.7175 0.033 Uiso 1 1 calc R . . C11 C 0.05363(12) 0.44583(17) 0.69175(17) 0.0277(5) Uani 1 1 d . . . H11A H 0.0824 0.4246 0.7603 0.033 Uiso 1 1 calc R . . H11B H 0.0061 0.4637 0.6724 0.033 Uiso 1 1 calc R . . C12 C 0.02253(13) 0.27896(19) 0.63834(19) 0.0313(5) Uani 1 1 d . . . H12A H -0.0251 0.2876 0.6223 0.038 Uiso 1 1 calc R . . H12B H 0.0540 0.2528 0.7050 0.038 Uiso 1 1 calc R . . C13 C 0.02001(13) 0.21041(19) 0.5667(2) 0.0332(5) Uani 1 1 d . . . H13A H 0.0104 0.1434 0.5771 0.040 Uiso 1 1 calc R . . H13B H -0.0182 0.2300 0.4996 0.040 Uiso 1 1 calc R . . C14 C 0.06501(18) 0.0643(2) 0.4870(3) 0.0566(10) Uani 1 1 d . . . H14A H 0.0859 0.0052 0.5260 0.085 Uiso 1 1 calc R . . H14B H 0.0652 0.0600 0.4298 0.085 Uiso 1 1 calc R . . H14C H 0.0164 0.0709 0.4663 0.085 Uiso 1 1 calc R . . C15 C 0.36501(13) 0.4153(2) 0.7108(2) 0.0352(6) Uani 1 1 d . . . H15A H 0.3711 0.4823 0.7339 0.053 Uiso 1 1 calc R . . H15B H 0.3696 0.4131 0.6572 0.053 Uiso 1 1 calc R . . H15C H 0.4011 0.3739 0.7638 0.053 Uiso 1 1 calc R . . C16 C 0.22431(11) 0.27405(14) 0.87369(14) 0.0190(4) Uani 1 1 d . . . C17 C 0.30623(12) 0.14112(14) 1.01700(14) 0.0197(4) Uani 1 1 d . . . C18 C 0.33048(12) 0.33036(15) 1.05398(15) 0.0232(4) Uani 1 1 d . . . S1 S 0.51870(6) 0.24371(9) 0.84373(8) 0.0242(2) Uani 0.50 1 d PD . 1 C19 C 0.5000 0.2148(3) 0.7500 0.0436(8) Uani 1 2 d SD . 1 N7 N 0.4770(3) 0.1997(4) 0.6628(3) 0.0436(8) Uani 0.50 1 d PD . 1 O4 O -0.0086(3) -0.0367(4) 0.2725(4) 0.089(3) Uani 0.50 1 d P . 1 O5 O 0.1374(4) -0.1547(8) 0.6060(6) 0.054(2) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0214(2) 0.01229(17) 0.01074(17) 0.00146(12) 0.00867(15) 0.00269(13) Mn1 0.01526(16) 0.01550(15) 0.01234(15) 0.00020(10) 0.00792(12) 0.00043(10) O1 0.0233(8) 0.0190(7) 0.0210(7) 0.0005(5) 0.0126(6) 0.0045(6) O2 0.0225(8) 0.0291(8) 0.0248(8) -0.0002(6) 0.0166(7) 0.0003(6) N1 0.0211(9) 0.0231(8) 0.0211(9) -0.0007(7) 0.0124(7) -0.0054(7) N2 0.0193(8) 0.0163(7) 0.0130(7) 0.0017(5) 0.0093(7) 0.0021(6) N3 0.0194(8) 0.0177(8) 0.0149(7) -0.0011(6) 0.0086(7) -0.0022(6) N4 0.0299(10) 0.0228(9) 0.0178(8) 0.0033(6) 0.0139(8) 0.0042(7) N5 0.0377(11) 0.0230(9) 0.0269(10) 0.0043(7) 0.0219(9) 0.0082(8) N6 0.0341(12) 0.0312(11) 0.0342(12) 0.0000(9) 0.0123(10) -0.0057(9) O3 0.0207(7) 0.0226(7) 0.0166(7) 0.0028(5) 0.0083(6) -0.0016(6) C1 0.0305(12) 0.0217(10) 0.0263(11) -0.0053(8) 0.0182(10) -0.0084(8) C2 0.0272(11) 0.0169(8) 0.0159(9) 0.0013(7) 0.0128(8) 0.0001(8) C3 0.0391(13) 0.0182(9) 0.0225(10) 0.0003(8) 0.0192(10) 0.0044(9) C4 0.0381(13) 0.0259(10) 0.0237(10) 0.0045(8) 0.0213(10) 0.0139(9) C5 0.0227(10) 0.0305(11) 0.0217(10) 0.0057(8) 0.0147(9) 0.0084(8) C6 0.0186(9) 0.0197(9) 0.0143(8) 0.0037(7) 0.0096(8) 0.0040(7) C7 0.0174(9) 0.0229(9) 0.0149(9) 0.0019(7) 0.0084(8) -0.0011(7) C8 0.0267(11) 0.0206(9) 0.0236(10) -0.0066(8) 0.0129(9) -0.0059(8) C9 0.0327(12) 0.0168(9) 0.0207(10) -0.0025(7) 0.0146(9) -0.0019(8) C10 0.0260(11) 0.0278(11) 0.0261(11) -0.0020(8) 0.0141(9) 0.0087(9) C11 0.0263(11) 0.0358(12) 0.0245(11) 0.0007(9) 0.0169(9) 0.0092(9) C12 0.0269(12) 0.0381(13) 0.0391(13) 0.0004(10) 0.0251(11) -0.0047(10) C13 0.0263(12) 0.0357(13) 0.0408(14) -0.0094(10) 0.0216(11) -0.0128(10) C14 0.0541(19) 0.0464(17) 0.083(2) -0.0426(17) 0.048(2) -0.0324(15) C15 0.0231(12) 0.0435(14) 0.0406(14) -0.0082(11) 0.0196(11) -0.0100(10) C16 0.0246(10) 0.0147(8) 0.0171(9) 0.0012(7) 0.0120(8) 0.0037(7) C17 0.0284(11) 0.0179(9) 0.0149(9) 0.0021(7) 0.0138(8) 0.0027(8) C18 0.0277(11) 0.0186(9) 0.0167(9) 0.0026(7) 0.0095(9) 0.0036(8) S1 0.0238(6) 0.0287(6) 0.0169(5) -0.0027(4) 0.0101(4) 0.0005(4) C19 0.0343(17) 0.0359(16) 0.066(2) 0.000 0.0325(18) 0.000 N7 0.0343(17) 0.0359(16) 0.066(2) 0.000 0.0325(18) 0.000 O4 0.042(3) 0.072(3) 0.068(5) -0.040(3) -0.016(3) 0.034(3) O5 0.029(4) 0.097(7) 0.029(4) -0.012(4) 0.013(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C16 1.893(2) 7_557 ? Co1 C16 1.893(2) . ? Co1 C18 1.896(2) 7_557 ? Co1 C18 1.896(2) . ? Co1 C17 1.903(2) . ? Co1 C17 1.903(2) 7_557 ? Mn1 N4 2.2110(19) . ? Mn1 N2 2.2125(17) . ? Mn1 O3 2.2381(15) . ? Mn1 N3 2.2467(18) . ? Mn1 N1 2.2606(19) . ? Mn1 O2 2.2674(16) . ? Mn1 O1 2.2854(16) . ? O1 C10 1.436(3) . ? O1 C9 1.437(3) . ? O2 C11 1.430(3) . ? O2 C12 1.438(3) . ? N1 C1 1.272(3) . ? N1 C13 1.462(3) . ? N2 C6 1.337(3) . ? N2 C2 1.339(3) . ? N3 C7 1.279(3) . ? N3 C8 1.460(3) . ? N4 C16 1.155(3) . ? N5 C17 1.148(3) . ? N6 C18 1.148(3) . ? C1 C14 1.498(3) . ? C1 C2 1.504(3) . ? C2 C3 1.393(3) . ? C3 C4 1.384(4) . ? C4 C5 1.389(3) . ? C5 C6 1.391(3) . ? C6 C7 1.507(3) . ? C7 C15 1.496(3) . ? C8 C9 1.519(3) . ? C10 C11 1.506(3) . ? C12 C13 1.517(4) . ? S1 N7 0.634(5) 2_656 ? S1 C19 1.4420(16) . ? C19 N7 1.266(4) . ? C19 N7 1.266(4) 2_656 ? C19 S1 1.4420(16) 2_656 ? N7 S1 0.634(5) 2_656 ? O4 O4 1.056(13) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Co1 C16 180.0 7_557 . ? C16 Co1 C18 90.60(9) 7_557 7_557 ? C16 Co1 C18 89.40(9) . 7_557 ? C16 Co1 C18 89.40(9) 7_557 . ? C16 Co1 C18 90.60(9) . . ? C18 Co1 C18 180.00(12) 7_557 . ? C16 Co1 C17 87.72(8) 7_557 . ? C16 Co1 C17 92.28(8) . . ? C18 Co1 C17 91.02(9) 7_557 . ? C18 Co1 C17 88.98(9) . . ? C16 Co1 C17 92.28(8) 7_557 7_557 ? C16 Co1 C17 87.72(8) . 7_557 ? C18 Co1 C17 88.98(9) 7_557 7_557 ? C18 Co1 C17 91.02(9) . 7_557 ? C17 Co1 C17 180.00(14) . 7_557 ? N4 Mn1 N2 94.53(7) . . ? N4 Mn1 O3 173.79(6) . . ? N2 Mn1 O3 91.40(6) . . ? N4 Mn1 N3 93.68(7) . . ? N2 Mn1 N3 70.97(7) . . ? O3 Mn1 N3 86.51(6) . . ? N4 Mn1 N1 91.76(7) . . ? N2 Mn1 N1 71.00(7) . . ? O3 Mn1 N1 91.91(6) . . ? N3 Mn1 N1 141.88(7) . . ? N4 Mn1 O2 92.39(7) . . ? N2 Mn1 O2 142.45(6) . . ? O3 Mn1 O2 84.00(6) . . ? N3 Mn1 O2 145.24(6) . . ? N1 Mn1 O2 71.93(6) . . ? N4 Mn1 O1 87.46(6) . . ? N2 Mn1 O1 143.70(6) . . ? O3 Mn1 O1 86.67(6) . . ? N3 Mn1 O1 72.73(6) . . ? N1 Mn1 O1 145.25(6) . . ? O2 Mn1 O1 73.39(6) . . ? C10 O1 C9 113.78(16) . . ? C10 O1 Mn1 110.43(12) . . ? C9 O1 Mn1 111.13(12) . . ? C11 O2 C12 115.06(17) . . ? C11 O2 Mn1 111.74(13) . . ? C12 O2 Mn1 111.88(13) . . ? C1 N1 C13 123.2(2) . . ? C1 N1 Mn1 119.53(15) . . ? C13 N1 Mn1 116.58(15) . . ? C6 N2 C2 120.92(18) . . ? C6 N2 Mn1 119.20(13) . . ? C2 N2 Mn1 119.58(14) . . ? C7 N3 C8 122.68(18) . . ? C7 N3 Mn1 119.94(14) . . ? C8 N3 Mn1 116.62(14) . . ? C16 N4 Mn1 164.97(17) . . ? N1 C1 C14 125.8(2) . . ? N1 C1 C2 115.31(19) . . ? C14 C1 C2 118.9(2) . . ? N2 C2 C3 121.4(2) . . ? N2 C2 C1 113.89(18) . . ? C3 C2 C1 124.66(19) . . ? C4 C3 C2 117.8(2) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 118.3(2) . . ? N2 C6 C5 120.95(19) . . ? N2 C6 C7 114.18(17) . . ? C5 C6 C7 124.86(19) . . ? N3 C7 C15 125.6(2) . . ? N3 C7 C6 114.65(18) . . ? C15 C7 C6 119.74(19) . . ? N3 C8 C9 108.84(18) . . ? O1 C9 C8 107.87(17) . . ? O1 C10 C11 106.92(17) . . ? O2 C11 C10 106.25(18) . . ? O2 C12 C13 106.57(19) . . ? N1 C13 C12 108.74(19) . . ? N4 C16 Co1 176.56(19) . . ? N5 C17 Co1 177.99(18) . . ? N6 C18 Co1 178.9(2) . . ? N7 S1 C19 61.2(4) 2_656 . ? N7 C19 N7 161.1(7) . 2_656 ? N7 C19 S1 171.5(4) . . ? N7 C19 S1 26.1(2) 2_656 . ? N7 C19 S1 26.1(2) . 2_656 ? N7 C19 S1 171.5(4) 2_656 2_656 ? S1 C19 S1 148.0(3) . 2_656 ? S1 N7 C19 92.7(5) 2_656 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.898 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.085