# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email miguel.clemente@uv.es _publ_contact_author_name 'Miguel Clemente-Leon' loop_ _publ_author_name M.Clemente-Leon E.Coronado M.Lopez-Jorda C.Desplanches S.Asthana H.Wang J.-F.Letard data_120kcor _database_code_depnum_ccdc_archive 'CCDC 807172' #TrackingRef '- C27H26Cl2CrFeMnN4O14_120.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cl2 Cr Fe Mn N4 O14' _chemical_formula_weight 864.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 11.5561(3) _cell_length_b 31.6369(7) _cell_length_c 9.5457(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.984(3) _cell_angle_gamma 90.00 _cell_volume 3279.77(15) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10300 _cell_measurement_theta_min 2.2655 _cell_measurement_theta_max 32.2113 _exptl_crystal_description rombic _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6825 _exptl_absorpt_correction_T_max 0.8520 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26791 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 32.29 _reflns_number_total 10705 _reflns_number_gt 7817 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0228P)^2^+4.8520P] 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 10705 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 C1 C 0.5875(2) 0.06437(8) -0.1026(3) 0.0179(5) Uani 1 1 d . . . C2 C 0.6269(3) 0.04371(10) -0.2095(3) 0.0255(6) Uani 1 1 d . . . H2A H 0.7047 0.0504 -0.2168 0.031 Uiso 1 1 calc R . . C3 C 0.5529(3) 0.01379(10) -0.3034(3) 0.0307(7) Uani 1 1 d . . . H3A H 0.5811 -0.0002 -0.3738 0.037 Uiso 1 1 calc R . . C4 C 0.4373(3) 0.00375(10) -0.2965(3) 0.0286(7) Uani 1 1 d . . . H4 H 0.3858 -0.0161 -0.3642 0.034 Uiso 1 1 calc R . . C5 C 0.3988(3) 0.02274(9) -0.1910(3) 0.0235(6) Uani 1 1 d . . . H5 H 0.3212 0.0152 -0.1844 0.028 Uiso 1 1 calc R . . C6 C 0.4717(2) 0.05314(8) -0.0925(3) 0.0171(5) Uani 1 1 d . . . C7 C 0.4292(2) 0.06971(9) 0.0209(3) 0.0190(5) Uani 1 1 d . . . H7 H 0.3544 0.0588 0.0267 0.023 Uiso 1 1 calc R . . C8 C 0.4345(3) 0.11205(10) 0.2296(3) 0.0270(6) Uani 1 1 d . . . H8A H 0.4746 0.0965 0.3238 0.032 Uiso 1 1 calc R . . H8B H 0.3449 0.1065 0.1962 0.032 Uiso 1 1 calc R . . C9 C 0.4595(3) 0.15901(9) 0.2532(3) 0.0244(6) Uani 1 1 d . . . H9A H 0.4010 0.1751 0.1698 0.029 Uiso 1 1 calc R . . H9B H 0.4482 0.1680 0.3470 0.029 Uiso 1 1 calc R . . C10 C 0.6856(3) 0.16244(10) 0.4092(3) 0.0333(8) Uani 1 1 d . . . H10A H 0.6509 0.1684 0.4887 0.040 Uiso 1 1 calc R . . H10B H 0.7529 0.1829 0.4194 0.040 Uiso 1 1 calc R . . C11 C 0.7365(3) 0.11786(10) 0.4273(3) 0.0316(7) Uani 1 1 d . . . H11A H 0.8171 0.1171 0.5090 0.038 Uiso 1 1 calc R . . H11B H 0.6797 0.0986 0.4538 0.038 Uiso 1 1 calc R . . C12 C 0.8744(2) 0.11097(9) 0.2737(3) 0.0235(6) Uani 1 1 d . . . H12A H 0.8882 0.0909 0.2014 0.028 Uiso 1 1 calc R . . H12B H 0.9396 0.1065 0.3716 0.028 Uiso 1 1 calc R . . C13 C 0.8799(2) 0.15598(9) 0.2218(3) 0.0252(7) Uani 1 1 d . . . H13A H 0.8894 0.1761 0.3045 0.030 Uiso 1 1 calc R . . H13B H 0.9504 0.1595 0.1864 0.030 Uiso 1 1 calc R . . C14 C 0.76459(13) 0.18680(5) -0.01095(17) 0.0151(5) Uani 1 1 d . . . H14 H 0.8415 0.1980 -0.0084 0.018 Uiso 1 1 calc R . . C15 C 0.65702(13) 0.19691(5) -0.13919(17) 0.0141(5) Uani 1 1 d R . . C16 C 0.67565(13) 0.22134(5) -0.25072(17) 0.0170(5) Uani 1 1 d R . . H16 H 0.7551 0.2291 -0.2433 0.020 Uiso 1 1 d R . . C17 C 0.5760(3) 0.23417(8) -0.3733(3) 0.0190(5) Uani 1 1 d . . . H17 H 0.5888 0.2505 -0.4504 0.023 Uiso 1 1 calc R . . C18 C 0.4568(2) 0.22272(9) -0.3815(3) 0.0186(5) Uani 1 1 d . . . H18 H 0.3883 0.2317 -0.4641 0.022 Uiso 1 1 calc R . . C19 C 0.4379(2) 0.19867(9) -0.2716(3) 0.0174(5) Uani 1 1 d . . . H19 H 0.3563 0.1913 -0.2795 0.021 Uiso 1 1 calc R . . C20 C 0.5373(2) 0.18469(8) -0.1470(3) 0.0142(5) Uani 1 1 d . . . C21 C 1.0282(2) 0.26205(8) 0.0377(3) 0.0151(5) Uani 1 1 d . . . C22 C 1.1486(2) 0.23900(8) 0.1291(3) 0.0154(5) Uani 1 1 d . . . C23 C 0.9966(2) 0.12571(8) -0.1759(3) 0.0149(5) Uani 1 1 d . . . C24 C 1.1155(2) 0.12240(9) -0.2164(3) 0.0161(5) Uani 1 1 d . . . C25 C 0.9351(2) -0.00835(8) -0.0484(3) 0.0145(5) Uani 1 1 d . . . C26 C 0.9441(2) 0.01423(8) -0.5416(3) 0.0172(5) Uani 1 1 d . . . N1 N 0.4850(2) 0.09836(7) 0.1156(2) 0.0174(4) Uani 1 1 d . . . N2 N 0.5880(2) 0.16773(7) 0.2608(3) 0.0191(5) Uani 1 1 d . . . H2 H 0.5908 0.1957 0.2319 0.023 Uiso 1 1 calc R . . N3 N 0.7515(2) 0.10356(7) 0.2862(2) 0.0177(5) Uani 1 1 d . . . H3 H 0.7372 0.0746 0.2785 0.021 Uiso 1 1 calc R . . N4 N 0.76355(19) 0.16370(7) 0.0998(3) 0.0169(5) Uani 1 1 d . . . O1 O 0.66373(16) 0.09208(6) -0.0148(2) 0.0196(4) Uani 1 1 d . . . O2 O 0.51197(15) 0.16205(6) -0.0454(2) 0.0167(4) Uani 1 1 d . . . O3 O 0.98187(16) 0.28651(6) 0.1070(2) 0.0197(4) Uani 1 1 d . . . O4 O 0.98644(16) 0.25410(6) -0.0998(2) 0.0191(4) Uani 1 1 d . . . O5 O 1.19130(17) 0.24748(6) 0.2660(2) 0.0214(4) Uani 1 1 d . . . O6 O 1.19162(17) 0.21354(6) 0.0595(2) 0.0227(4) Uani 1 1 d . . . O7 O 0.97173(17) 0.16172(6) -0.1393(2) 0.0206(4) Uani 1 1 d . . . O8 O 0.93557(17) 0.09268(6) -0.1858(2) 0.0199(4) Uani 1 1 d . . . O9 O 1.17533(17) 0.15569(7) -0.2095(2) 0.0223(4) Uani 1 1 d . . . O10 O 1.14022(18) 0.08653(6) -0.2539(2) 0.0226(4) Uani 1 1 d . . . O11 O 0.89996(16) 0.00082(6) -0.1841(2) 0.0175(4) Uani 1 1 d . . . O12 O 0.87864(16) -0.02978(6) 0.0176(2) 0.0200(4) Uani 1 1 d . . . O15 O 0.91165(17) 0.04065(6) -0.4651(2) 0.0227(4) Uani 1 1 d . . . O16 O 0.89636(17) 0.00846(6) -0.6800(2) 0.0230(4) Uani 1 1 d . . . Cl1 Cl 1.21709(7) 0.06514(2) -0.59203(9) 0.02926(16) Uani 1 1 d . . . Cl2 Cl 1.20222(7) 0.15645(2) -0.57438(9) 0.03286(18) Uani 1 1 d . . . Mn1 Mn 1.08863(4) 0.208739(12) -0.16565(4) 0.01313(8) Uani 0.50 1 d P . 1 Cr1 Cr 1.08863(4) 0.208739(12) -0.16565(4) 0.01313(8) Uani 0.50 1 d P . 2 Mn2 Mn 1.01924(4) 0.039827(12) -0.24048(4) 0.01337(8) Uani 0.50 1 d P . 3 Cr2 Cr 1.01924(4) 0.039827(12) -0.24048(4) 0.01337(8) Uani 0.50 1 d P . 4 Fe Fe 0.62475(3) 0.130945(12) 0.10838(4) 0.01373(8) Uani 1 1 d . . . C1S C 1.2791(2) 0.11039(9) -0.4838(3) 0.0208(6) Uani 1 1 d . . . H1S1 H 1.3680 0.1126 -0.4687 0.025 Uiso 1 1 calc R . . H1S2 H 1.2699 0.1078 -0.3848 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0149(11) 0.0176(13) 0.0181(13) -0.0017(10) 0.0018(10) 0.0013(10) C2 0.0205(13) 0.0307(16) 0.0245(15) -0.0091(13) 0.0067(11) 0.0025(12) C3 0.0330(16) 0.0304(17) 0.0242(15) -0.0091(13) 0.0040(13) 0.0070(13) C4 0.0308(16) 0.0211(15) 0.0239(15) -0.0057(12) -0.0033(12) -0.0024(12) C5 0.0203(13) 0.0181(14) 0.0259(15) 0.0008(11) 0.0000(11) -0.0025(11) C6 0.0161(12) 0.0157(12) 0.0169(12) 0.0001(10) 0.0023(10) -0.0001(10) C7 0.0174(12) 0.0177(13) 0.0219(13) 0.0048(11) 0.0068(10) -0.0022(10) C8 0.0342(16) 0.0292(16) 0.0263(15) -0.0018(13) 0.0216(13) -0.0046(13) C9 0.0265(14) 0.0256(15) 0.0249(15) 0.0003(12) 0.0139(12) 0.0042(12) C10 0.0395(18) 0.0324(18) 0.0177(14) -0.0071(13) -0.0035(13) 0.0162(14) C11 0.0427(18) 0.0314(17) 0.0159(14) 0.0016(12) 0.0039(13) 0.0182(14) C12 0.0160(12) 0.0188(14) 0.0286(15) 0.0036(12) -0.0016(11) 0.0008(10) C13 0.0152(12) 0.0205(14) 0.0296(16) 0.0061(12) -0.0057(11) -0.0029(11) C14 0.0115(10) 0.0130(12) 0.0210(13) -0.0037(10) 0.0059(9) -0.0008(9) C15 0.0135(11) 0.0140(12) 0.0152(12) -0.0027(9) 0.0054(9) -0.0008(9) C16 0.0182(12) 0.0169(12) 0.0189(13) -0.0010(10) 0.0099(10) -0.0025(10) C17 0.0262(14) 0.0155(13) 0.0181(13) 0.0007(10) 0.0114(11) -0.0008(11) C18 0.0205(12) 0.0179(13) 0.0153(12) 0.0019(10) 0.0033(10) 0.0035(10) C19 0.0137(11) 0.0196(13) 0.0180(13) -0.0007(10) 0.0041(10) 0.0000(10) C20 0.0150(11) 0.0135(12) 0.0152(12) -0.0032(9) 0.0066(9) 0.0003(9) C21 0.0112(11) 0.0112(11) 0.0225(13) 0.0050(10) 0.0051(10) -0.0008(9) C22 0.0129(11) 0.0117(11) 0.0220(13) 0.0086(10) 0.0067(10) -0.0010(9) C23 0.0155(11) 0.0193(13) 0.0113(11) 0.0005(10) 0.0064(9) 0.0000(10) C24 0.0159(11) 0.0228(14) 0.0113(11) 0.0030(10) 0.0069(9) 0.0031(10) C25 0.0143(11) 0.0112(12) 0.0189(13) -0.0042(10) 0.0068(9) -0.0016(9) C26 0.0156(11) 0.0120(12) 0.0229(13) 0.0075(10) 0.0052(10) -0.0014(9) N1 0.0193(10) 0.0183(11) 0.0164(11) 0.0009(9) 0.0086(9) -0.0016(9) N2 0.0213(11) 0.0152(11) 0.0198(12) 0.0018(9) 0.0056(9) 0.0047(9) N3 0.0200(11) 0.0133(11) 0.0184(11) -0.0001(9) 0.0047(9) 0.0027(8) N4 0.0122(10) 0.0149(11) 0.0201(11) -0.0011(9) 0.0010(8) -0.0010(8) O1 0.0149(8) 0.0239(10) 0.0203(10) -0.0075(8) 0.0062(7) -0.0025(7) O2 0.0112(8) 0.0214(10) 0.0169(9) 0.0029(7) 0.0041(7) -0.0016(7) O3 0.0164(9) 0.0160(9) 0.0265(10) 0.0039(8) 0.0072(8) 0.0064(7) O4 0.0150(8) 0.0155(9) 0.0226(10) 0.0026(8) 0.0008(7) 0.0013(7) O5 0.0178(9) 0.0216(10) 0.0206(10) 0.0080(8) 0.0013(8) 0.0011(8) O6 0.0201(9) 0.0219(10) 0.0303(11) 0.0110(9) 0.0139(8) 0.0096(8) O7 0.0219(9) 0.0231(10) 0.0231(10) -0.0002(8) 0.0159(8) 0.0036(8) O8 0.0189(9) 0.0240(10) 0.0215(10) -0.0032(8) 0.0129(8) -0.0038(8) O9 0.0171(9) 0.0317(11) 0.0216(10) -0.0002(9) 0.0111(8) -0.0043(8) O10 0.0267(10) 0.0250(11) 0.0235(10) 0.0052(8) 0.0181(8) 0.0103(8) O11 0.0166(9) 0.0170(9) 0.0159(9) -0.0039(7) 0.0018(7) -0.0032(7) O12 0.0178(9) 0.0208(10) 0.0233(10) -0.0042(8) 0.0094(8) -0.0074(8) O15 0.0194(9) 0.0176(10) 0.0326(11) 0.0107(8) 0.0109(8) 0.0075(8) O16 0.0195(9) 0.0176(10) 0.0238(10) 0.0090(8) -0.0031(8) -0.0027(8) Cl1 0.0339(4) 0.0226(4) 0.0324(4) -0.0036(3) 0.0127(3) -0.0041(3) Cl2 0.0336(4) 0.0232(4) 0.0304(4) 0.0005(3) -0.0038(3) -0.0009(3) Mn1 0.01800(18) 0.01010(18) 0.01299(18) -0.00049(15) 0.00750(15) -0.00076(15) Cr1 0.01800(18) 0.01010(18) 0.01299(18) -0.00049(15) 0.00750(15) -0.00076(15) Mn2 0.01850(19) 0.01031(18) 0.01237(18) -0.00003(15) 0.00664(15) -0.00107(15) Cr2 0.01850(19) 0.01031(18) 0.01237(18) -0.00003(15) 0.00664(15) -0.00107(15) Fe 0.01308(16) 0.01302(17) 0.01394(17) -0.00001(14) 0.00314(13) -0.00054(14) C1S 0.0191(12) 0.0239(14) 0.0193(13) 0.0008(11) 0.0065(10) -0.0024(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.320(3) . ? C1 C2 1.411(4) . ? C1 C6 1.420(4) . ? C2 C3 1.381(4) . ? C2 H2A 0.9500 . ? C3 C4 1.397(5) . ? C3 H3A 0.9500 . ? C4 C5 1.370(4) . ? C4 H4 0.9500 . ? C5 C6 1.406(4) . ? C5 H5 0.9500 . ? C6 C7 1.433(4) . ? C7 N1 1.287(3) . ? C7 H7 0.9500 . ? C8 N1 1.466(4) . ? C8 C9 1.515(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.488(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.488(3) . ? C10 C11 1.515(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.487(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.484(4) . ? C12 C13 1.516(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N4 1.467(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.288(3) . ? C14 C15 1.4513 . ? C14 H14 0.9500 . ? C15 C16 1.3905 . ? C15 C20 1.414(3) . ? C16 C17 1.392(3) . ? C16 H16 0.9300 . ? C17 C18 1.401(4) . ? C17 H17 0.9500 . ? C18 C19 1.373(4) . ? C18 H18 0.9500 . ? C19 C20 1.413(3) . ? C19 H19 0.9500 . ? C20 O2 1.316(3) . ? C21 O3 1.251(3) . ? C21 O4 1.259(3) . ? C21 C22 1.549(3) . ? C22 O6 1.250(3) . ? C22 O5 1.258(3) . ? C23 O8 1.246(3) . ? C23 O7 1.253(3) . ? C23 C24 1.553(3) . ? C24 O9 1.249(3) . ? C24 O10 1.252(3) . ? C25 O12 1.251(3) . ? C25 O11 1.251(3) . ? C25 C25 1.560(5) 3_755 ? C26 O15 1.248(3) . ? C26 O16 1.259(3) . ? C26 C26 1.552(5) 3_754 ? N1 Fe 1.937(2) . ? N2 Fe 2.018(2) . ? N2 H2 0.9300 . ? N3 Fe 2.019(2) . ? N3 H3 0.9300 . ? N4 Fe 1.935(2) . ? O1 Fe 1.8601(19) . ? O2 Fe 1.8746(18) . ? O3 Cr1 2.1037(19) 4_566 ? O3 Mn1 2.1037(19) 4_566 ? O4 Mn1 2.087(2) . ? O5 Cr1 2.069(2) 4_566 ? O5 Mn1 2.069(2) 4_566 ? O6 Mn1 2.076(2) . ? O7 Mn1 2.081(2) . ? O8 Mn2 2.085(2) . ? O9 Mn1 2.070(2) . ? O10 Mn2 2.068(2) . ? O11 Mn2 2.0543(19) . ? O12 Cr2 2.074(2) 3_755 ? O12 Mn2 2.074(2) 3_755 ? O15 Mn2 2.079(2) . ? O16 Cr2 2.090(2) 3_754 ? O16 Mn2 2.090(2) 3_754 ? Cl1 C1S 1.767(3) . ? Cl2 C1S 1.770(3) . ? Mn1 O5 2.069(2) 4_565 ? Mn1 O3 2.1037(19) 4_565 ? Mn2 O12 2.074(2) 3_755 ? Mn2 O16 2.090(2) 3_754 ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 117.1(2) . . ? O1 C1 C6 124.3(2) . . ? C2 C1 C6 118.5(2) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 118.3(3) . . ? C1 C6 C7 122.3(2) . . ? N1 C7 C6 124.7(2) . . ? N1 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N1 C8 C9 107.2(2) . . ? N1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? N2 C9 C8 109.0(2) . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 110.6(2) . . ? N2 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N3 C11 C10 109.9(2) . . ? N3 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N3 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C13 108.8(2) . . ? N3 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N4 C13 C12 106.7(2) . . ? N4 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? N4 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? N4 C14 C15 124.86(11) . . ? N4 C14 H14 117.6 . . ? C15 C14 H14 117.6 . . ? C16 C15 C20 121.10(12) . . ? C16 C15 C14 117.1 . . ? C20 C15 C14 121.65(12) . . ? C15 C16 C17 120.39(13) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 119.1(2) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.8(2) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 121.4(2) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? O2 C20 C19 118.0(2) . . ? O2 C20 C15 124.7(2) . . ? C19 C20 C15 117.3(2) . . ? O3 C21 O4 126.4(2) . . ? O3 C21 C22 117.2(2) . . ? O4 C21 C22 116.4(2) . . ? O6 C22 O5 127.1(2) . . ? O6 C22 C21 116.6(2) . . ? O5 C22 C21 116.3(2) . . ? O8 C23 O7 127.3(2) . . ? O8 C23 C24 116.8(2) . . ? O7 C23 C24 115.9(2) . . ? O9 C24 O10 127.1(2) . . ? O9 C24 C23 116.8(2) . . ? O10 C24 C23 116.1(2) . . ? O12 C25 O11 127.3(2) . . ? O12 C25 C25 116.5(3) . 3_755 ? O11 C25 C25 116.2(3) . 3_755 ? O15 C26 O16 126.8(2) . . ? O15 C26 C26 117.0(3) . 3_754 ? O16 C26 C26 116.2(3) . 3_754 ? C7 N1 C8 119.9(2) . . ? C7 N1 Fe 125.1(2) . . ? C8 N1 Fe 114.66(18) . . ? C9 N2 C10 116.4(3) . . ? C9 N2 Fe 108.07(17) . . ? C10 N2 Fe 110.12(17) . . ? C9 N2 H2 107.3 . . ? C10 N2 H2 107.3 . . ? Fe N2 H2 107.3 . . ? C12 N3 C11 115.9(2) . . ? C12 N3 Fe 107.69(17) . . ? C11 N3 Fe 110.81(17) . . ? C12 N3 H3 107.4 . . ? C11 N3 H3 107.4 . . ? Fe N3 H3 107.4 . . ? C14 N4 C13 118.9(2) . . ? C14 N4 Fe 125.38(15) . . ? C13 N4 Fe 115.16(18) . . ? C1 O1 Fe 125.95(17) . . ? C20 O2 Fe 126.32(16) . . ? C21 O3 Cr1 112.56(16) . 4_566 ? C21 O3 Mn1 112.56(16) . 4_566 ? Cr1 O3 Mn1 0.000(13) 4_566 4_566 ? C21 O4 Mn1 113.34(16) . . ? C22 O5 Cr1 114.02(16) . 4_566 ? C22 O5 Mn1 114.02(16) . 4_566 ? Cr1 O5 Mn1 0.00(3) 4_566 4_566 ? C22 O6 Mn1 113.95(16) . . ? C23 O7 Mn1 113.34(16) . . ? C23 O8 Mn2 113.14(16) . . ? C24 O9 Mn1 113.38(17) . . ? C24 O10 Mn2 113.86(17) . . ? C25 O11 Mn2 113.61(15) . . ? C25 O12 Cr2 112.83(16) . 3_755 ? C25 O12 Mn2 112.83(16) . 3_755 ? Cr2 O12 Mn2 0.00(2) 3_755 3_755 ? C26 O15 Mn2 113.66(16) . . ? C26 O16 Cr2 113.32(17) . 3_754 ? C26 O16 Mn2 113.32(17) . 3_754 ? Cr2 O16 Mn2 0.00(3) 3_754 3_754 ? O5 Mn1 O9 96.29(8) 4_565 . ? O5 Mn1 O6 95.15(8) 4_565 . ? O9 Mn1 O6 97.06(8) . . ? O5 Mn1 O7 169.17(8) 4_565 . ? O9 Mn1 O7 79.86(7) . . ? O6 Mn1 O7 95.37(8) . . ? O5 Mn1 O4 94.54(8) 4_565 . ? O9 Mn1 O4 168.94(8) . . ? O6 Mn1 O4 79.70(7) . . ? O7 Mn1 O4 89.87(7) . . ? O5 Mn1 O3 79.87(7) 4_565 4_565 ? O9 Mn1 O3 90.17(8) . 4_565 ? O6 Mn1 O3 171.66(8) . 4_565 ? O7 Mn1 O3 89.98(7) . 4_565 ? O4 Mn1 O3 93.95(7) . 4_565 ? O11 Mn2 O10 166.87(8) . . ? O11 Mn2 O12 80.60(7) . 3_755 ? O10 Mn2 O12 90.77(8) . 3_755 ? O11 Mn2 O15 93.42(7) . . ? O10 Mn2 O15 96.06(8) . . ? O12 Mn2 O15 171.78(8) 3_755 . ? O11 Mn2 O8 90.35(7) . . ? O10 Mn2 O8 79.84(7) . . ? O12 Mn2 O8 90.93(8) 3_755 . ? O15 Mn2 O8 94.76(8) . . ? O11 Mn2 O16 95.42(8) . 3_754 ? O10 Mn2 O16 95.19(8) . 3_754 ? O12 Mn2 O16 95.04(8) 3_755 3_754 ? O15 Mn2 O16 79.83(7) . 3_754 ? O8 Mn2 O16 172.29(8) . 3_754 ? O1 Fe O2 96.06(8) . . ? O1 Fe N4 86.77(9) . . ? O2 Fe N4 92.88(8) . . ? O1 Fe N1 93.18(9) . . ? O2 Fe N1 86.69(9) . . ? N4 Fe N1 179.55(10) . . ? O1 Fe N2 173.20(9) . . ? O2 Fe N2 90.04(9) . . ? N4 Fe N2 95.94(10) . . ? N1 Fe N2 84.16(10) . . ? O1 Fe N3 89.14(9) . . ? O2 Fe N3 173.66(9) . . ? N4 Fe N3 83.78(9) . . ? N1 Fe N3 96.66(9) . . ? N2 Fe N3 84.97(9) . . ? Cl1 C1S Cl2 110.23(15) . . ? Cl1 C1S H1S1 109.6 . . ? Cl2 C1S H1S1 109.6 . . ? Cl1 C1S H1S2 109.6 . . ? Cl2 C1S H1S2 109.6 . . ? H1S1 C1S H1S2 108.1 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.997 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.091 # Attachment '- C27H26Cl2CrFeMnN4O14_300.cif' data_corabs300 _database_code_depnum_ccdc_archive 'CCDC 807173' #TrackingRef '- C27H26Cl2CrFeMnN4O14_300.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cl2 Cr Fe Mn N4 O14' _chemical_formula_weight 864.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 12.096(5) _cell_length_b 32.135(5) _cell_length_c 9.467(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 111.981(5) _cell_angle_gamma 90.000(5) _cell_volume 3412(2) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 11797 _cell_measurement_theta_min 2.3160 _cell_measurement_theta_max 32.2326 _exptl_crystal_description rombic _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_T_max 0.8679 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 300(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 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0267 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44282 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 32.32 _reflns_number_total 11352 _reflns_number_gt 5903 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0672P)^2^+3.2669P] 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 11352 _refine_ls_number_parameters 489 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1812 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.051 _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 Fe Fe 0.38894(5) 0.127429(19) 0.94279(7) 0.04978(17) Uani 1 1 d . D . Mn1 Mn 0.92115(5) 0.208522(17) 0.21655(6) 0.03786(15) Uani 0.50 1 d P A 1 Cr1 Cr 0.92115(5) 0.208522(17) 0.21655(6) 0.03786(15) Uani 0.50 1 d P A 2 Mn2 Mn 0.98717(6) 0.040953(18) 0.24251(7) 0.04032(16) Uani 0.50 1 d P A 3 Cr2 Cr 0.98717(6) 0.040953(18) 0.24251(7) 0.04032(16) Uani 0.50 1 d P A 4 O1 O 0.3583(3) 0.08030(13) 1.0415(4) 0.0796(11) Uani 1 1 d . . . O2 O 0.4866(3) 0.16185(11) 1.1032(4) 0.0641(9) Uani 1 1 d . . . O3 O 0.8185(2) 0.25063(9) 0.2809(3) 0.0473(6) Uani 1 1 d . . . O4 O 0.8202(3) 0.21458(9) -0.0136(3) 0.0522(7) Uani 1 1 d . . . O5 O 1.0224(2) 0.21289(8) 0.4498(3) 0.0457(6) Uani 1 1 d . . . O6 O 1.0188(2) 0.25436(8) 0.1572(3) 0.0444(6) Uani 1 1 d . . . O7 O 0.8378(2) 0.15420(9) 0.2451(3) 0.0489(7) Uani 1 1 d . . . O8 O 0.8677(2) 0.08533(8) 0.2622(3) 0.0480(7) Uani 1 1 d . . . O9 O 1.0357(3) 0.16420(9) 0.1872(3) 0.0491(7) Uani 1 1 d . . . O10 O 1.0648(2) 0.09495(9) 0.2022(3) 0.0484(7) Uani 1 1 d . . . O11 O 1.0874(3) 0.04056(9) 0.4758(3) 0.0529(7) Uani 1 1 d . . . O12 O 0.9061(3) -0.00824(9) 0.3119(3) 0.0511(7) Uani 1 1 d . . . O15 O 1.1020(2) 0.00235(9) 0.1881(3) 0.0492(7) Uani 1 1 d . . . O16 O 0.8869(2) 0.03157(9) 0.0130(3) 0.0480(7) Uani 1 1 d . . . N1 N 0.5409(3) 0.09736(13) 0.9420(5) 0.0598(10) Uani 1 1 d . D . N2 N 0.4298(4) 0.16264(14) 0.7741(5) 0.0767(13) Uani 1 1 d . . . H2N H 0.4050 0.1895 0.7688 0.092 Uiso 1 1 calc R B 1 N3 N 0.2467(4) 0.10715(12) 0.7365(5) 0.0613(10) Uani 1 1 d . . . H3N H 0.2581 0.0799 0.7199 0.074 Uiso 1 1 calc R C 1 N4 N 0.2422(3) 0.15952(12) 0.9544(4) 0.0562(9) Uani 1 1 d . . . C1 C 0.4294(4) 0.05082(17) 1.1242(5) 0.0636(13) Uani 1 1 d . . . C2 C 0.3901(5) 0.02528(19) 1.2160(6) 0.0797(16) Uani 1 1 d . . . H2 H 0.3130 0.0285 1.2134 0.096 Uiso 1 1 calc R . . C3 C 0.4618(7) -0.00401(19) 1.3082(6) 0.090(2) Uani 1 1 d . . . H3 H 0.4341 -0.0199 1.3701 0.108 Uiso 1 1 calc R . . C4 C 0.5781(7) -0.01067(18) 1.3116(7) 0.0858(18) Uani 1 1 d . . . H4 H 0.6278 -0.0304 1.3764 0.103 Uiso 1 1 calc R . . C5 C 0.6162(5) 0.01268(16) 1.2169(6) 0.0732(15) Uani 1 1 d . . . H5 H 0.6918 0.0079 1.2161 0.088 Uiso 1 1 calc R . . C6 C 0.5443(4) 0.04332(15) 1.1220(5) 0.0562(11) Uani 1 1 d . . . C7 C 0.5911(4) 0.06635(16) 1.0266(5) 0.0578(11) Uani 1 1 d . . . H7 H 0.6646 0.0580 1.0262 0.069 Uiso 1 1 calc R . . C8 C 0.6022(6) 0.1167(2) 0.8510(8) 0.0875(18) Uani 1 1 d . . . H8A H 0.6876 0.1165 0.9079 0.105 Uiso 1 1 calc R D . H8B H 0.5860 0.1009 0.7580 0.105 Uiso 1 1 calc R . . C9 C 0.5608(6) 0.1596(2) 0.8136(8) 0.097(2) Uani 1 1 d . D . H9A H 0.5799 0.1691 0.7283 0.117 Uiso 1 1 calc R . . H9B H 0.6017 0.1774 0.9001 0.117 Uiso 1 1 calc R . . C10A C 0.3731(14) 0.1400(7) 0.6203(11) 0.080(5) Uani 0.58(3) 1 d P D 1 H10A H 0.4146 0.1142 0.6207 0.096 Uiso 0.58(3) 1 calc PR D 1 H10B H 0.3756 0.1573 0.5377 0.096 Uiso 0.58(3) 1 calc PR D 1 C11A C 0.2373(18) 0.1311(8) 0.602(3) 0.071(4) Uani 0.58(3) 1 d P D 1 H11A H 0.1949 0.1569 0.5977 0.085 Uiso 0.58(3) 1 calc PR D 1 H11B H 0.1958 0.1153 0.5099 0.085 Uiso 0.58(3) 1 calc PR D 1 C10B C 0.322(3) 0.1665(11) 0.629(2) 0.117(13) Uani 0.42(3) 1 d P D 2 H10C H 0.2621 0.1844 0.6415 0.140 Uiso 0.42(3) 1 calc PR D 2 H10D H 0.3432 0.1766 0.5458 0.140 Uiso 0.42(3) 1 calc PR D 2 C11B C 0.284(4) 0.1232(13) 0.608(4) 0.109(13) Uani 0.42(3) 1 d P D 2 H11C H 0.3493 0.1061 0.6038 0.131 Uiso 0.42(3) 1 calc PR D 2 H11D H 0.2180 0.1203 0.5114 0.131 Uiso 0.42(3) 1 calc PR D 2 C12 C 0.1334(5) 0.1113(2) 0.7634(9) 0.104(2) Uani 1 1 d . D . H12A H 0.0665 0.1091 0.6669 0.125 Uiso 1 1 calc R . . H12B H 0.1276 0.0886 0.8279 0.125 Uiso 1 1 calc R . . C13 C 0.1263(4) 0.15044(19) 0.8346(7) 0.0833(18) Uani 1 1 d . D . H13A H 0.0655 0.1489 0.8782 0.100 Uiso 1 1 calc R . . H13B H 0.1048 0.1725 0.7592 0.100 Uiso 1 1 calc R . . C14 C 0.2428(4) 0.18337(13) 1.0637(5) 0.0504(10) Uani 1 1 d . D . H14 H 0.1695 0.1925 1.0624 0.061 Uiso 1 1 calc R . . C15 C 0.3470(4) 0.19704(12) 1.1869(5) 0.0457(9) Uani 1 1 d . . . C16 C 0.3316(5) 0.22248(15) 1.2987(6) 0.0618(12) Uani 1 1 d . D . H16 H 0.2549 0.2293 1.2916 0.074 Uiso 1 1 calc R . . C17 C 0.4274(6) 0.23743(17) 1.4177(7) 0.0783(16) Uani 1 1 d . . . H17 H 0.4155 0.2539 1.4916 0.094 Uiso 1 1 calc R D . C18 C 0.5418(5) 0.22831(16) 1.4290(6) 0.0672(13) Uani 1 1 d . D . H18 H 0.6064 0.2393 1.5088 0.081 Uiso 1 1 calc R . . C19 C 0.5610(4) 0.20304(15) 1.3232(5) 0.0572(11) Uani 1 1 d . . . H19 H 0.6386 0.1971 1.3321 0.069 Uiso 1 1 calc R D . C20 C 0.4648(4) 0.18610(13) 1.2018(4) 0.0465(9) Uani 1 1 d . D . C21 C 0.8601(3) 0.25978(11) 0.4179(4) 0.0378(8) Uani 1 1 d . . . C22 C 0.9775(3) 0.23741(11) 0.5178(4) 0.0368(8) Uani 1 1 d . . . C23 C 0.8942(3) 0.12163(12) 0.2401(4) 0.0375(8) Uani 1 1 d . A . C24 C 1.0088(3) 0.12762(12) 0.2063(4) 0.0379(8) Uani 1 1 d . A . C25 C 1.0530(3) 0.01392(11) 0.5489(5) 0.0415(9) Uani 1 1 d . . . C26 C 0.9371(3) 0.00853(12) -0.0504(4) 0.0390(8) Uani 1 1 d . . . C1S C 0.7300(6) 0.1124(2) 0.5009(8) 0.104(2) Uani 1 1 d D . . H1S1 H 0.6447 0.1142 0.4757 0.125 Uiso 0.667(4) 1 calc PR E 1 H1S2 H 0.7444 0.1120 0.4067 0.125 Uiso 0.667(4) 1 calc PR E 1 H1S3 H 0.7713 0.0872 0.4918 0.125 Uiso 0.333(4) 1 d PR E 2 H1S4 H 0.7284 0.1306 0.4185 0.125 Uiso 0.333(4) 1 d PR E 2 Cl1S Cl 0.8036(4) 0.15659(9) 0.6149(4) 0.0916(10) Uani 0.667(4) 1 d PD E 1 Cl2S Cl 0.7847(3) 0.06812(8) 0.6022(3) 0.0989(10) Uani 0.667(4) 1 d PD E 1 Cl3S Cl 0.5878(6) 0.09886(16) 0.4664(5) 0.103(2) Uani 0.333(4) 1 d PD E 2 Cl4S Cl 0.8154(10) 0.1346(6) 0.6606(16) 0.265(9) Uani 0.333(4) 1 d PD E 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 Fe 0.0384(3) 0.0579(4) 0.0481(3) -0.0041(3) 0.0106(2) 0.0039(3) Mn1 0.0465(3) 0.0344(3) 0.0358(3) 0.0007(2) 0.0189(2) -0.0004(2) Cr1 0.0465(3) 0.0344(3) 0.0358(3) 0.0007(2) 0.0189(2) -0.0004(2) Mn2 0.0508(4) 0.0343(3) 0.0398(3) -0.0047(2) 0.0215(3) -0.0016(3) Cr2 0.0508(4) 0.0343(3) 0.0398(3) -0.0047(2) 0.0215(3) -0.0016(3) O1 0.0461(18) 0.102(3) 0.094(3) 0.033(2) 0.0306(19) 0.0078(18) O2 0.0361(15) 0.091(2) 0.0596(19) -0.0227(17) 0.0112(14) 0.0030(15) O3 0.0432(15) 0.0538(16) 0.0378(14) 0.0125(12) 0.0072(12) 0.0087(12) O4 0.0486(16) 0.0602(18) 0.0523(16) -0.0169(14) 0.0240(14) -0.0241(14) O5 0.0443(15) 0.0410(15) 0.0492(15) 0.0038(12) 0.0146(12) 0.0138(11) O6 0.0454(15) 0.0386(14) 0.0391(14) -0.0035(11) 0.0043(12) -0.0076(11) O7 0.0482(16) 0.0534(17) 0.0572(17) 0.0035(13) 0.0337(14) 0.0058(13) O8 0.0542(17) 0.0490(16) 0.0534(16) -0.0065(13) 0.0345(14) -0.0140(13) O9 0.0541(17) 0.0472(16) 0.0599(17) -0.0015(13) 0.0374(14) -0.0074(13) O10 0.0523(16) 0.0522(17) 0.0542(16) -0.0001(13) 0.0355(14) 0.0006(13) O11 0.0555(17) 0.0422(16) 0.0633(18) -0.0162(14) 0.0249(15) -0.0184(13) O12 0.0504(17) 0.0453(16) 0.0487(17) -0.0156(13) 0.0082(13) -0.0078(13) O15 0.0473(16) 0.0543(17) 0.0418(15) -0.0008(13) 0.0119(13) 0.0048(13) O16 0.0418(15) 0.0538(17) 0.0489(16) 0.0039(13) 0.0175(13) 0.0131(12) N1 0.053(2) 0.071(3) 0.062(2) -0.012(2) 0.0291(19) -0.0061(19) N2 0.079(3) 0.072(3) 0.064(3) 0.013(2) 0.010(2) -0.016(2) N3 0.063(2) 0.042(2) 0.063(2) -0.0121(18) 0.0049(19) -0.0007(17) N4 0.0371(18) 0.062(2) 0.058(2) -0.0097(18) 0.0037(16) 0.0076(16) C1 0.048(3) 0.086(4) 0.049(3) -0.001(2) 0.009(2) -0.014(2) C2 0.065(3) 0.100(4) 0.070(3) 0.009(3) 0.021(3) -0.016(3) C3 0.124(6) 0.075(4) 0.056(3) 0.010(3) 0.018(4) -0.022(4) C4 0.107(5) 0.062(3) 0.068(4) 0.001(3) 0.010(4) -0.002(3) C5 0.065(3) 0.066(3) 0.070(3) -0.010(3) 0.004(3) 0.009(3) C6 0.045(2) 0.064(3) 0.050(2) -0.011(2) 0.0059(19) -0.002(2) C7 0.045(2) 0.069(3) 0.057(3) -0.018(2) 0.016(2) 0.002(2) C8 0.090(4) 0.105(5) 0.088(4) -0.005(4) 0.057(4) -0.012(4) C9 0.109(5) 0.098(5) 0.105(5) -0.005(4) 0.063(4) -0.017(4) C10A 0.108(10) 0.083(11) 0.035(5) 0.002(5) 0.011(5) -0.004(8) C11A 0.071(10) 0.070(9) 0.044(6) -0.002(6) -0.010(7) 0.000(7) C10B 0.15(2) 0.091(19) 0.069(10) 0.008(10) -0.005(11) -0.049(17) C11B 0.12(3) 0.09(2) 0.071(13) 0.006(12) -0.02(2) -0.021(19) C12 0.045(3) 0.088(4) 0.145(6) -0.058(4) -0.005(3) -0.001(3) C13 0.041(3) 0.096(4) 0.083(4) -0.023(3) -0.011(2) 0.009(3) C14 0.039(2) 0.053(2) 0.058(3) 0.009(2) 0.0168(19) 0.0095(18) C15 0.047(2) 0.044(2) 0.051(2) 0.0071(18) 0.0244(19) -0.0002(17) C16 0.069(3) 0.056(3) 0.071(3) -0.008(2) 0.038(3) -0.003(2) C17 0.091(4) 0.069(3) 0.082(4) -0.026(3) 0.040(3) -0.011(3) C18 0.073(3) 0.064(3) 0.058(3) -0.013(2) 0.017(3) -0.022(3) C19 0.045(2) 0.069(3) 0.053(3) 0.000(2) 0.013(2) -0.007(2) C20 0.043(2) 0.057(3) 0.039(2) 0.0032(18) 0.0151(17) -0.0022(18) C21 0.0352(18) 0.0373(19) 0.041(2) 0.0119(15) 0.0144(16) 0.0040(14) C22 0.0346(18) 0.0322(18) 0.041(2) 0.0055(15) 0.0107(15) 0.0040(14) C23 0.0387(18) 0.045(2) 0.0317(17) -0.0047(15) 0.0169(15) -0.0068(16) C24 0.0424(19) 0.046(2) 0.0309(16) -0.0016(15) 0.0202(15) -0.0044(16) C25 0.039(2) 0.034(2) 0.050(2) -0.0130(17) 0.0157(17) -0.0021(15) C26 0.0381(19) 0.0380(19) 0.040(2) 0.0010(16) 0.0129(16) 0.0024(15) C1S 0.111(6) 0.119(6) 0.107(5) 0.002(4) 0.070(5) -0.003(4) Cl1S 0.0847(19) 0.0818(16) 0.0827(17) -0.0047(13) 0.0018(14) -0.0009(13) Cl2S 0.122(2) 0.0750(16) 0.109(2) 0.0176(13) 0.0547(17) 0.0080(14) Cl3S 0.153(5) 0.095(4) 0.068(3) -0.018(2) 0.048(3) -0.043(3) Cl4S 0.095(7) 0.47(3) 0.217(14) -0.030(15) 0.047(8) -0.091(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Fe O1 1.888(4) . ? Fe O2 1.892(3) . ? Fe N1 2.079(4) . ? Fe N4 2.091(4) . ? Fe N2 2.161(4) . ? Fe N3 2.164(4) . ? Mn1 O4 2.070(3) . ? Mn1 O3 2.076(3) . ? Mn1 O9 2.077(3) . ? Mn1 O7 2.083(3) . ? Mn1 O5 2.091(3) . ? Mn1 O6 2.092(3) . ? Mn2 O15 2.066(3) . ? Mn2 O10 2.075(3) . ? Mn2 O16 2.076(3) . ? Mn2 O11 2.084(3) . ? Mn2 O8 2.088(3) . ? Mn2 O12 2.091(3) . ? O1 C1 1.321(6) . ? O2 C20 1.316(5) . ? O3 C21 1.238(4) . ? O4 C21 1.252(4) 4_565 ? O5 C22 1.261(4) . ? O6 C22 1.252(4) 4_565 ? O7 C23 1.259(4) . ? O8 C23 1.248(4) . ? O9 C24 1.251(4) . ? O10 C24 1.258(4) . ? O11 C25 1.265(5) . ? O12 C25 1.235(5) 3_756 ? O15 C26 1.259(4) 3_755 ? O16 C26 1.245(4) . ? N1 C7 1.280(6) . ? N1 C8 1.469(6) . ? N2 C9 1.488(8) . ? N2 C10B 1.50(2) . ? N2 C10A 1.540(14) . ? N2 H2N 0.9100 . ? N3 C11A 1.46(3) . ? N3 C12 1.490(8) . ? N3 C11B 1.54(5) . ? N3 H3N 0.9100 . ? N4 C14 1.285(6) . ? N4 C13 1.465(6) . ? C1 C2 1.401(7) . ? C1 C6 1.419(7) . ? C2 C3 1.354(8) . ? C2 H2 0.9300 . ? C3 C4 1.411(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(8) . ? C4 H4 0.9300 . ? C5 C6 1.396(7) . ? C5 H5 0.9300 . ? C6 C7 1.438(7) . ? C7 H7 0.9300 . ? C8 C9 1.464(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10A C11A 1.61(3) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C10B C11B 1.46(5) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12 C13 1.445(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.429(6) . ? C14 H14 0.9300 . ? C15 C16 1.404(6) . ? C15 C20 1.422(6) . ? C16 C17 1.366(7) . ? C16 H16 0.9300 . ? C17 C18 1.378(8) . ? C17 H17 0.9300 . ? C18 C19 1.375(7) . ? C18 H18 0.9300 . ? C19 C20 1.404(6) . ? C19 H19 0.9300 . ? C21 O4 1.252(4) 4_566 ? C21 C22 1.556(5) . ? C22 O6 1.252(4) 4_566 ? C23 C24 1.547(5) . ? C25 O12 1.235(5) 3_756 ? C25 C25 1.554(7) 3_756 ? C26 O15 1.259(4) 3_755 ? C26 C26 1.561(7) 3_755 ? C1S Cl4S 1.642(12) . ? C1S Cl3S 1.684(8) . ? C1S Cl2S 1.704(7) . ? C1S Cl1S 1.805(8) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? C1S H1S4 0.9700 . ? Cl2S H1S3 1.1699 . ? 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 Fe O2 104.53(18) . . ? O1 Fe N1 88.06(16) . . ? O2 Fe N1 89.28(14) . . ? O1 Fe N4 92.41(16) . . ? O2 Fe N4 87.52(14) . . ? N1 Fe N4 176.78(15) . . ? O1 Fe N2 158.09(19) . . ? O2 Fe N2 92.32(17) . . ? N1 Fe N2 78.09(18) . . ? N4 Fe N2 102.37(18) . . ? O1 Fe N3 88.16(17) . . ? O2 Fe N3 161.20(15) . . ? N1 Fe N3 105.22(16) . . ? N4 Fe N3 77.99(15) . . ? N2 Fe N3 79.36(17) . . ? O4 Mn1 O3 93.76(11) . . ? O4 Mn1 O9 94.81(12) . . ? O3 Mn1 O9 171.27(11) . . ? O4 Mn1 O7 95.27(11) . . ? O3 Mn1 O7 97.84(11) . . ? O9 Mn1 O7 79.76(11) . . ? O4 Mn1 O5 170.75(11) . . ? O3 Mn1 O5 79.90(10) . . ? O9 Mn1 O5 91.77(11) . . ? O7 Mn1 O5 92.28(11) . . ? O4 Mn1 O6 79.69(10) . . ? O3 Mn1 O6 94.57(11) . . ? O9 Mn1 O6 88.56(11) . . ? O7 Mn1 O6 166.89(11) . . ? O5 Mn1 O6 94.02(11) . . ? O15 Mn2 O10 93.63(11) . . ? O15 Mn2 O16 80.55(11) . . ? O10 Mn2 O16 93.23(12) . . ? O15 Mn2 O11 94.69(11) . . ? O10 Mn2 O11 94.36(11) . . ? O16 Mn2 O11 171.28(11) . . ? O15 Mn2 O8 170.00(11) . . ? O10 Mn2 O8 79.71(10) . . ? O16 Mn2 O8 92.31(11) . . ? O11 Mn2 O8 93.26(11) . . ? O15 Mn2 O12 93.59(12) . . ? O10 Mn2 O12 170.87(11) . . ? O16 Mn2 O12 93.46(11) . . ? O11 Mn2 O12 79.48(11) . . ? O8 Mn2 O12 93.82(11) . . ? C1 O1 Fe 131.6(3) . . ? C20 O2 Fe 133.2(3) . . ? C21 O3 Mn1 114.1(2) . . ? C21 O4 Mn1 114.7(2) 4_565 . ? C22 O5 Mn1 112.8(2) . . ? C22 O6 Mn1 112.9(2) 4_565 . ? C23 O7 Mn1 113.4(2) . . ? C23 O8 Mn2 113.2(2) . . ? C24 O9 Mn1 113.7(2) . . ? C24 O10 Mn2 114.0(2) . . ? C25 O11 Mn2 113.8(2) . . ? C25 O12 Mn2 113.6(2) 3_756 . ? C26 O15 Mn2 113.4(2) 3_755 . ? C26 O16 Mn2 113.1(2) . . ? C7 N1 C8 118.0(4) . . ? C7 N1 Fe 125.0(3) . . ? C8 N1 Fe 116.5(4) . . ? C9 N2 C10B 135.4(16) . . ? C9 N2 C10A 105.2(8) . . ? C10B N2 C10A 41.2(13) . . ? C9 N2 Fe 107.2(4) . . ? C10B N2 Fe 111.1(9) . . ? C10A N2 Fe 107.9(6) . . ? C9 N2 H2N 112.1 . . ? C10B N2 H2N 73.5 . . ? C10A N2 H2N 112.1 . . ? Fe N2 H2N 112.1 . . ? C11A N3 C12 109.1(9) . . ? C11A N3 C11B 23.1(15) . . ? C12 N3 C11B 132.0(16) . . ? C11A N3 Fe 113.9(10) . . ? C12 N3 Fe 106.9(3) . . ? C11B N3 Fe 104.0(13) . . ? C11A N3 H3N 108.9 . . ? C12 N3 H3N 108.9 . . ? C11B N3 H3N 94.4 . . ? Fe N3 H3N 108.9 . . ? C14 N4 C13 117.2(4) . . ? C14 N4 Fe 125.9(3) . . ? C13 N4 Fe 116.5(3) . . ? O1 C1 C2 119.4(5) . . ? O1 C1 C6 122.5(4) . . ? C2 C1 C6 118.1(5) . . ? C3 C2 C1 121.5(6) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 120.8(6) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.5(6) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 121.7(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 119.2(5) . . ? C5 C6 C7 118.1(5) . . ? C1 C6 C7 122.7(4) . . ? N1 C7 C6 126.0(4) . . ? N1 C7 H7 117.0 . . ? C6 C7 H7 117.0 . . ? C9 C8 N1 109.7(5) . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? N1 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 N2 111.0(5) . . ? C8 C9 H9A 109.4 . . ? N2 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? N2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N2 C10A C11A 105.2(13) . . ? N2 C10A H10A 110.7 . . ? C11A C10A H10A 110.7 . . ? N2 C10A H10B 110.7 . . ? C11A C10A H10B 110.7 . . ? H10A C10A H10B 108.8 . . ? N3 C11A C10A 104.9(13) . . ? N3 C11A H11A 110.8 . . ? C10A C11A H11A 110.8 . . ? N3 C11A H11B 110.8 . . ? C10A C11A H11B 110.8 . . ? H11A C11A H11B 108.8 . . ? C11B C10B N2 100(3) . . ? C11B C10B H10C 111.8 . . ? N2 C10B H10C 111.8 . . ? C11B C10B H10D 111.8 . . ? N2 C10B H10D 111.8 . . ? H10C C10B H10D 109.6 . . ? C10B C11B N3 112(4) . . ? C10B C11B H11C 109.1 . . ? N3 C11B H11C 109.1 . . ? C10B C11B H11D 109.1 . . ? N3 C11B H11D 109.1 . . ? H11C C11B H11D 107.8 . . ? C13 C12 N3 112.1(5) . . ? C13 C12 H12A 109.2 . . ? N3 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? N3 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 N4 109.2(4) . . ? C12 C13 H13A 109.8 . . ? N4 C13 H13A 109.8 . . ? C12 C13 H13B 109.8 . . ? N4 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 125.3(4) . . ? N4 C14 H14 117.3 . . ? C15 C14 H14 117.3 . . ? C16 C15 C20 118.7(4) . . ? C16 C15 C14 118.0(4) . . ? C20 C15 C14 123.3(4) . . ? C17 C16 C15 121.0(5) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.4(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O2 C20 C19 119.0(4) . . ? O2 C20 C15 122.4(4) . . ? C19 C20 C15 118.6(4) . . ? O3 C21 O4 127.9(3) . 4_566 ? O3 C21 C22 116.6(3) . . ? O4 C21 C22 115.5(3) 4_566 . ? O6 C22 O5 126.3(3) 4_566 . ? O6 C22 C21 117.1(3) 4_566 . ? O5 C22 C21 116.6(3) . . ? O8 C23 O7 126.5(3) . . ? O8 C23 C24 117.2(3) . . ? O7 C23 C24 116.3(3) . . ? O9 C24 O10 127.4(3) . . ? O9 C24 C23 116.7(3) . . ? O10 C24 C23 115.9(3) . . ? O12 C25 O11 127.0(3) 3_756 . ? O12 C25 C25 117.5(5) 3_756 3_756 ? O11 C25 C25 115.5(4) . 3_756 ? O16 C26 O15 127.0(3) . 3_755 ? O16 C26 C26 117.0(4) . 3_755 ? O15 C26 C26 116.0(4) 3_755 3_755 ? Cl4S C1S Cl3S 122.4(6) . . ? Cl4S C1S Cl2S 82.4(8) . . ? Cl3S C1S Cl2S 92.7(4) . . ? Cl4S C1S Cl1S 26.7(7) . . ? Cl3S C1S Cl1S 123.9(4) . . ? Cl2S C1S Cl1S 108.7(4) . . ? Cl4S C1S H1S1 116.4 . . ? Cl3S C1S H1S1 18.5 . . ? Cl2S C1S H1S1 110.0 . . ? Cl1S C1S H1S1 110.0 . . ? Cl4S C1S H1S2 125.7 . . ? Cl3S C1S H1S2 109.9 . . ? Cl2S C1S H1S2 110.0 . . ? Cl1S C1S H1S2 110.0 . . ? H1S1 C1S H1S2 108.3 . . ? Cl4S C1S H1S3 106.1 . . ? Cl3S C1S H1S3 106.9 . . ? Cl2S C1S H1S3 41.5 . . ? Cl1S C1S H1S3 123.6 . . ? H1S1 C1S H1S3 124.3 . . ? H1S2 C1S H1S3 68.5 . . ? Cl4S C1S H1S4 107.1 . . ? Cl3S C1S H1S4 106.8 . . ? Cl2S C1S H1S4 147.5 . . ? Cl1S C1S H1S4 82.1 . . ? H1S1 C1S H1S4 93.8 . . ? H1S2 C1S H1S4 39.2 . . ? H1S3 C1S H1S4 106.7 . . ? C1S Cl2S H1S3 33.3 . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.461 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.076 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 813345' #TrackingRef 'C27H26Cl2CrFeMnN4O14_250.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cl2 Cr Fe Mn N4 O14' _chemical_formula_weight 864.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 11.9215(15) _cell_length_b 31.910(3) _cell_length_c 9.4841(11) _cell_angle_alpha 90.00 _cell_angle_beta 111.535(13) _cell_angle_gamma 90.00 _cell_volume 3356.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 5082 _cell_measurement_theta_min 2.9938 _cell_measurement_theta_max 32.5852 _exptl_crystal_description Prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7744 _exptl_absorpt_correction_T_max 0.8998 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Sapphire3' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean 16.0267 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43973 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.1168 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 32.66 _reflns_number_total 11354 _reflns_number_gt 4665 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11354 _refine_ls_number_parameters 489 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1372 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.865 _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 N1 N 0.5355(3) 0.09760(11) 0.9239(4) 0.0679(9) Uani 1 1 d . C . N2 N 0.4282(3) 0.16417(11) 0.7614(4) 0.0782(11) Uani 1 1 d . . . H2A H 0.4020 0.1915 0.7540 0.094 Uiso 1 1 calc R A 1 N3 N 0.2497(3) 0.10641(10) 0.7262(4) 0.0619(9) Uani 1 1 d . . . H3A H 0.2614 0.0786 0.7103 0.074 Uiso 1 1 calc R B 1 N4 N 0.2433(3) 0.16125(10) 0.9373(4) 0.0585(8) Uani 1 1 d . . . C1 C 0.4250(4) 0.05586(15) 1.1167(5) 0.0693(12) Uani 1 1 d . C . C2 C 0.3851(4) 0.03197(17) 1.2150(5) 0.0864(15) Uani 1 1 d . . . H2 H 0.3080 0.0369 1.2170 0.104 Uiso 1 1 calc R . . C3 C 0.4548(6) 0.00264(18) 1.3046(6) 0.1009(18) Uani 1 1 d . . . H3 H 0.4262 -0.0127 1.3693 0.121 Uiso 1 1 calc R . . C4 C 0.5715(6) -0.00595(17) 1.3043(6) 0.0948(16) Uani 1 1 d . . . H4 H 0.6203 -0.0266 1.3684 0.114 Uiso 1 1 calc R . . C5 C 0.6113(4) 0.01617(15) 1.2099(5) 0.0766(13) Uani 1 1 d . . . H5 H 0.6884 0.0106 1.2086 0.092 Uiso 1 1 calc R . . C6 C 0.5402(4) 0.04699(13) 1.1146(5) 0.0606(10) Uani 1 1 d . . . C7 C 0.5864(4) 0.06726(14) 1.0122(5) 0.0670(11) Uani 1 1 d . . . H7 H 0.6600 0.0574 1.0098 0.080 Uiso 1 1 calc R . . C8 C 0.5968(5) 0.11496(18) 0.8281(6) 0.1007(18) Uani 1 1 d . . . H8A H 0.5758 0.0986 0.7344 0.121 Uiso 1 1 calc R C . H8B H 0.6844 0.1136 0.8816 0.121 Uiso 1 1 calc R . . C9 C 0.5580(5) 0.15994(16) 0.7913(6) 0.0923(16) Uani 1 1 d . C . H9A H 0.6041 0.1780 0.8765 0.111 Uiso 1 1 calc R . . H9B H 0.5745 0.1689 0.7020 0.111 Uiso 1 1 calc R . . C10A C 0.3744(16) 0.1386(7) 0.6062(13) 0.075(5) Uani 0.44(2) 1 d P C 1 H10A H 0.4195 0.1127 0.6093 0.090 Uiso 0.44(2) 1 calc PR C 1 H10B H 0.3722 0.1555 0.5190 0.090 Uiso 0.44(2) 1 calc PR C 1 C11A C 0.241(3) 0.1293(10) 0.605(2) 0.070(6) Uani 0.44(2) 1 d P C 1 H11A H 0.1999 0.1558 0.6059 0.084 Uiso 0.44(2) 1 calc PR C 1 H11B H 0.1941 0.1140 0.5120 0.084 Uiso 0.44(2) 1 calc PR C 1 C10B C 0.3228(16) 0.1656(6) 0.6190(11) 0.096(6) Uani 0.56(2) 1 d P C 2 H10C H 0.3461 0.1771 0.5378 0.116 Uiso 0.56(2) 1 calc PR C 2 H10D H 0.2605 0.1838 0.6309 0.116 Uiso 0.56(2) 1 calc PR C 2 C11B C 0.276(3) 0.1227(9) 0.580(2) 0.100(8) Uani 0.56(2) 1 d P C 2 H11C H 0.3349 0.1047 0.5604 0.120 Uiso 0.56(2) 1 calc PR C 2 H11D H 0.2011 0.1228 0.4898 0.120 Uiso 0.56(2) 1 calc PR C 2 C12 C 0.1348(4) 0.11236(14) 0.7497(6) 0.0916(17) Uani 1 1 d . C . H12A H 0.0679 0.1100 0.6518 0.110 Uiso 1 1 calc R . . H12B H 0.1259 0.0899 0.8154 0.110 Uiso 1 1 calc R . . C13 C 0.1269(4) 0.15203(15) 0.8163(5) 0.0869(15) Uani 1 1 d . C . H13A H 0.0631 0.1511 0.8583 0.104 Uiso 1 1 calc R . . H13B H 0.1070 0.1741 0.7390 0.104 Uiso 1 1 calc R . . C14 C 0.2435(3) 0.18423(11) 1.0453(4) 0.0499(9) Uani 1 1 d . C . H14 H 0.1685 0.1940 1.0433 0.060 Uiso 1 1 calc R . . C15 C 0.3486(3) 0.19678(11) 1.1711(4) 0.0471(9) Uani 1 1 d . . . C16 C 0.3327(4) 0.22147(12) 1.2816(5) 0.0594(10) Uani 1 1 d . C . H16 H 0.2540 0.2282 1.2743 0.071 Uiso 1 1 calc R . . C17 C 0.4278(4) 0.23627(13) 1.4007(5) 0.0748(13) Uani 1 1 d . . . H17 H 0.4147 0.2531 1.4746 0.090 Uiso 1 1 calc R C . C18 C 0.5447(4) 0.22643(12) 1.4129(5) 0.0634(11) Uani 1 1 d . C . H18 H 0.6109 0.2364 1.4956 0.076 Uiso 1 1 calc R . . C19 C 0.5629(3) 0.20215(12) 1.3037(4) 0.0557(10) Uani 1 1 d . . . H19 H 0.6422 0.1965 1.3109 0.067 Uiso 1 1 calc R C . C20 C 0.4661(3) 0.18557(12) 1.1815(4) 0.0481(9) Uani 1 1 d . C . C21 C -0.0208(3) 0.26258(9) 1.0007(4) 0.0332(7) Uani 1 1 d . . . C22 C -0.1388(3) 0.24014(9) 0.9030(4) 0.0332(7) Uani 1 1 d . . . C23 C -0.1074(3) 0.12226(10) 1.2328(3) 0.0355(7) Uani 1 1 d . . . C24 C 0.0095(3) 0.12682(10) 1.1970(3) 0.0359(7) Uani 1 1 d . . . C25 C -0.0540(3) -0.01404(10) 1.4536(4) 0.0408(8) Uani 1 1 d . . . C26 C 0.0630(3) -0.00846(10) 1.0496(4) 0.0366(7) Uani 1 1 d . . . O1 O 0.3533(3) 0.08446(11) 1.0305(4) 0.0874(10) Uani 1 1 d . . . O2 O 0.4891(2) 0.16227(9) 1.0829(3) 0.0625(7) Uani 1 1 d . . . O3 O 0.02444(19) 0.28673(6) 0.9325(2) 0.0419(5) Uani 1 1 d . . . O4 O 0.02054(19) 0.25423(6) 1.1391(2) 0.0408(5) Uani 1 1 d . . . O5 O -0.18114(19) 0.24890(7) 0.7669(2) 0.0425(5) Uani 1 1 d . . . O6 O -0.1800(2) 0.21447(7) 0.9716(3) 0.0460(6) Uani 1 1 d . . . O7 O -0.1640(2) 0.15493(7) 1.2326(2) 0.0439(6) Uani 1 1 d . . . O8 O -0.1339(2) 0.08603(7) 1.2589(3) 0.0455(6) Uani 1 1 d . . . O9 O 0.0364(2) 0.16304(7) 1.1726(3) 0.0449(6) Uani 1 1 d . . . O10 O 0.0661(2) 0.09426(7) 1.1978(3) 0.0444(6) Uani 1 1 d . . . O11 O -0.0967(2) -0.00812(7) 1.3135(3) 0.0470(6) Uani 1 1 d . . . O12 O -0.0871(2) -0.04062(7) 1.5267(3) 0.0490(6) Uani 1 1 d . . . O13 O 0.10070(19) 0.00174(7) 1.1857(2) 0.0444(5) Uani 1 1 d . . . O14 O 0.1151(2) -0.03092(7) 0.9860(2) 0.0444(6) Uani 1 1 d . . . C1S C -0.2704(5) 0.11178(15) 1.4958(6) 0.0853(14) Uani 1 1 d D . . H1S1 H -0.3572 0.1136 1.4744 0.102 Uiso 0.778(3) 1 calc PR D 1 H1S2 H -0.2586 0.1106 1.3989 0.102 Uiso 0.778(3) 1 calc PR D 1 H1S3 H -0.2315 0.0873 1.4737 0.102 Uiso 0.222(3) 1 d PR D 2 H1S4 H -0.2714 0.1330 1.4221 0.102 Uiso 0.222(3) 1 d PR D 2 Cl1S Cl -0.21345(16) 0.06790(5) 1.59814(19) 0.0867(6) Uani 0.778(3) 1 d PD D 1 Cl2S Cl -0.19567(18) 0.15701(5) 1.6007(2) 0.0793(6) Uani 0.778(3) 1 d PD D 1 Cl3S Cl -0.4169(7) 0.0982(2) 1.4589(7) 0.117(3) Uani 0.222(3) 1 d PD D 2 Cl4S Cl -0.1827(14) 0.1300(8) 1.6603(18) 0.335(14) Uani 0.222(3) 1 d PD D 2 Fe Fe 0.38769(4) 0.128544(16) 0.92454(6) 0.05096(16) Uani 1 1 d . C . Mn1 Mn -0.01444(5) 0.040621(15) 1.24209(5) 0.03788(14) Uani 0.50 1 d P . 1 Cr1 Cr -0.01444(5) 0.040621(15) 1.24209(5) 0.03788(14) Uani 0.50 1 d P . 1 Mn2 Mn -0.07841(4) 0.208616(14) 1.20078(5) 0.03470(13) Uani 0.50 1 d P . . Cr2 Cr -0.07841(4) 0.208616(14) 1.20078(5) 0.03470(13) 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 N1 0.069(2) 0.064(2) 0.079(3) -0.009(2) 0.036(2) -0.0091(19) N2 0.076(3) 0.077(3) 0.066(2) 0.0183(19) 0.008(2) -0.025(2) N3 0.066(2) 0.0407(18) 0.067(2) -0.0122(16) 0.0103(18) -0.0036(16) N4 0.0356(17) 0.061(2) 0.065(2) -0.0140(17) 0.0018(15) 0.0050(15) C1 0.047(2) 0.093(3) 0.059(3) 0.005(2) 0.009(2) -0.015(2) C2 0.063(3) 0.125(4) 0.064(3) 0.023(3) 0.014(2) -0.013(3) C3 0.111(5) 0.102(4) 0.073(4) 0.016(3) 0.014(3) -0.031(4) C4 0.100(4) 0.085(4) 0.074(4) 0.009(3) 0.002(3) 0.004(3) C5 0.065(3) 0.083(3) 0.067(3) -0.007(3) 0.007(2) 0.000(3) C6 0.052(2) 0.066(3) 0.058(3) -0.012(2) 0.013(2) -0.006(2) C7 0.053(3) 0.071(3) 0.073(3) -0.025(2) 0.018(2) -0.008(2) C8 0.115(4) 0.125(5) 0.091(4) -0.016(3) 0.072(4) -0.010(4) C9 0.108(4) 0.084(4) 0.107(4) -0.015(3) 0.065(4) -0.031(3) C10A 0.086(10) 0.078(11) 0.052(7) -0.005(7) 0.013(6) -0.021(8) C11A 0.083(12) 0.094(11) 0.024(9) -0.023(8) 0.008(7) -0.026(9) C10B 0.123(11) 0.089(11) 0.053(6) 0.009(6) 0.003(6) -0.036(9) C11B 0.16(2) 0.114(15) 0.038(6) -0.025(7) 0.043(9) -0.061(14) C12 0.039(2) 0.067(3) 0.143(5) -0.047(3) 0.002(3) -0.005(2) C13 0.047(3) 0.087(3) 0.096(4) -0.020(3) -0.010(2) 0.008(2) C14 0.0376(19) 0.049(2) 0.063(3) 0.0039(19) 0.0182(18) 0.0055(17) C15 0.042(2) 0.048(2) 0.056(2) 0.0087(17) 0.0222(18) -0.0006(16) C16 0.054(2) 0.057(2) 0.073(3) -0.001(2) 0.030(2) 0.002(2) C17 0.078(3) 0.064(3) 0.089(3) -0.031(2) 0.039(3) -0.011(2) C18 0.065(3) 0.058(3) 0.062(3) -0.012(2) 0.017(2) -0.014(2) C19 0.039(2) 0.068(3) 0.059(2) 0.002(2) 0.0166(18) -0.0073(18) C20 0.042(2) 0.058(2) 0.043(2) 0.0036(18) 0.0142(17) -0.0020(17) C21 0.0313(16) 0.0272(15) 0.0392(19) -0.0091(14) 0.0107(15) 0.0005(13) C22 0.0307(16) 0.0318(17) 0.0360(19) -0.0098(14) 0.0108(15) -0.0017(13) C23 0.0377(17) 0.0421(19) 0.0303(17) -0.0020(14) 0.0165(14) -0.0055(15) C24 0.0394(17) 0.0404(19) 0.0321(17) -0.0010(14) 0.0181(14) -0.0023(15) C25 0.0387(19) 0.0327(18) 0.050(2) -0.0116(15) 0.0151(17) -0.0026(15) C26 0.0379(18) 0.0336(17) 0.0394(19) 0.0011(14) 0.0155(15) -0.0007(14) O1 0.0493(18) 0.120(3) 0.089(2) 0.042(2) 0.0209(16) 0.0007(17) O2 0.0327(13) 0.091(2) 0.0563(16) -0.0185(15) 0.0081(12) 0.0027(13) O3 0.0387(13) 0.0387(13) 0.0471(14) -0.0052(10) 0.0142(11) -0.0118(10) O4 0.0384(12) 0.0372(12) 0.0386(13) -0.0054(10) 0.0046(10) -0.0055(10) O5 0.0385(12) 0.0435(13) 0.0389(13) -0.0114(10) 0.0065(10) -0.0058(10) O6 0.0439(13) 0.0483(14) 0.0484(14) -0.0131(11) 0.0199(12) -0.0169(11) O7 0.0440(13) 0.0467(14) 0.0515(14) 0.0044(11) 0.0300(12) 0.0048(11) O8 0.0531(14) 0.0439(14) 0.0508(14) -0.0039(11) 0.0326(12) -0.0103(11) O9 0.0482(14) 0.0416(13) 0.0579(15) -0.0002(11) 0.0348(12) -0.0056(11) O10 0.0464(14) 0.0420(13) 0.0562(15) 0.0019(11) 0.0324(12) 0.0031(11) O11 0.0468(14) 0.0385(13) 0.0457(15) -0.0137(11) 0.0050(12) -0.0047(11) O12 0.0533(15) 0.0383(13) 0.0563(15) -0.0177(11) 0.0213(12) -0.0172(11) O13 0.0447(13) 0.0459(13) 0.0369(13) -0.0017(11) 0.0082(11) 0.0055(11) O14 0.0420(13) 0.0469(13) 0.0446(14) 0.0006(11) 0.0163(11) 0.0098(11) C1S 0.083(4) 0.101(4) 0.085(4) -0.006(3) 0.047(3) -0.002(3) Cl1S 0.1064(13) 0.0623(10) 0.0982(13) 0.0132(8) 0.0457(10) 0.0072(9) Cl2S 0.0759(11) 0.0692(10) 0.0714(11) -0.0042(8) 0.0018(8) -0.0015(8) Cl3S 0.184(8) 0.099(5) 0.079(4) -0.023(3) 0.062(5) -0.049(5) Cl4S 0.181(15) 0.58(4) 0.26(2) -0.02(2) 0.103(15) -0.14(2) Fe 0.0389(3) 0.0566(3) 0.0533(3) -0.0015(3) 0.0122(2) 0.0004(3) Mn1 0.0498(3) 0.0304(3) 0.0364(3) -0.0037(2) 0.0193(2) -0.0005(2) Cr1 0.0498(3) 0.0304(3) 0.0364(3) -0.0037(2) 0.0193(2) -0.0005(2) Mn2 0.0419(3) 0.0309(3) 0.0338(3) 0.0004(2) 0.0168(2) -0.0002(2) Cr2 0.0419(3) 0.0309(3) 0.0338(3) 0.0004(2) 0.0168(2) -0.0002(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 N1 C7 1.278(5) . ? N1 C8 1.468(5) . ? N1 Fe 2.022(4) . ? N2 C10B 1.469(11) . ? N2 C9 1.474(6) . ? N2 C10A 1.598(15) . ? N2 Fe 2.113(3) . ? N2 H2A 0.9200 . ? N3 C11A 1.34(3) . ? N3 C12 1.478(5) . ? N3 C11B 1.61(2) . ? N3 Fe 2.115(3) . ? N3 H3A 0.9200 . ? N4 C14 1.259(4) . ? N4 C13 1.470(5) . ? N4 Fe 2.054(3) . ? C1 O1 1.311(5) . ? C1 C6 1.409(6) . ? C1 C2 1.415(6) . ? C2 C3 1.331(7) . ? C2 H2 0.9400 . ? C3 C4 1.419(7) . ? C3 H3 0.9400 . ? C4 C5 1.355(6) . ? C4 H4 0.9400 . ? C5 C6 1.393(6) . ? C5 H5 0.9400 . ? C6 C7 1.435(6) . ? C7 H7 0.9400 . ? C8 C9 1.509(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10A C11A 1.61(4) . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C10B C11B 1.48(3) . ? C10B H10C 0.9800 . ? C10B H10D 0.9800 . ? C11B H11C 0.9800 . ? C11B H11D 0.9800 . ? C12 C13 1.434(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.434(5) . ? C14 H14 0.9400 . ? C15 C16 1.379(5) . ? C15 C20 1.414(5) . ? C16 C17 1.358(6) . ? C16 H16 0.9400 . ? C17 C18 1.392(6) . ? C17 H17 0.9400 . ? C18 C19 1.373(5) . ? C18 H18 0.9400 . ? C19 C20 1.404(5) . ? C19 H19 0.9400 . ? C20 O2 1.301(4) . ? C21 O3 1.249(4) . ? C21 O4 1.250(3) . ? C21 C22 1.547(4) . ? C22 O5 1.233(3) . ? C22 O6 1.253(4) . ? C23 O7 1.241(3) . ? C23 O8 1.247(3) . ? C23 C24 1.558(4) . ? C24 O10 1.238(3) . ? C24 O9 1.243(3) . ? C25 O12 1.248(4) . ? C25 O11 1.250(4) . ? C25 C25 1.551(6) 3_558 ? C26 O14 1.240(3) . ? C26 O13 1.245(4) . ? C26 C26 1.548(6) 3_557 ? O1 Fe 1.860(3) . ? O2 Fe 1.882(3) . ? O3 Cr2 2.092(2) 4_565 ? O3 Mn2 2.092(2) 4_565 ? O4 Mn2 2.088(2) . ? O5 Cr2 2.073(2) 4_565 ? O5 Mn2 2.073(2) 4_565 ? O6 Mn2 2.072(2) . ? O7 Mn2 2.072(2) . ? O8 Mn1 2.079(2) . ? O9 Mn2 2.080(2) . ? O10 Mn1 2.080(2) . ? O11 Mn1 2.081(2) . ? O12 Cr1 2.080(2) 3_558 ? O12 Mn1 2.080(2) 3_558 ? O13 Mn1 2.061(2) . ? O14 Cr1 2.076(2) 3_557 ? O14 Mn1 2.076(2) 3_557 ? C1S Cl4S 1.634(13) . ? C1S Cl1S 1.697(5) . ? C1S Cl3S 1.705(8) . ? C1S Cl2S 1.794(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9700 . ? C1S H1S4 0.9700 . ? Cl1S H1S3 1.2793 . ? Cl2S H1S4 1.7746 . ? Mn1 O14 2.076(2) 3_557 ? Mn1 O12 2.080(2) 3_558 ? Mn2 O5 2.073(2) 4_566 ? Mn2 O3 2.092(2) 4_566 ? 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 C7 N1 C8 117.8(4) . . ? C7 N1 Fe 124.9(3) . . ? C8 N1 Fe 116.8(3) . . ? C10B N2 C9 131.5(9) . . ? C10B N2 C10A 41.5(6) . . ? C9 N2 C10A 99.7(8) . . ? C10B N2 Fe 110.0(5) . . ? C9 N2 Fe 108.4(3) . . ? C10A N2 Fe 106.1(6) . . ? C10B N2 H2A 75.4 . . ? C9 N2 H2A 113.8 . . ? C10A N2 H2A 113.8 . . ? Fe N2 H2A 113.8 . . ? C11A N3 C12 106.2(12) . . ? C11A N3 C11B 20.0(18) . . ? C12 N3 C11B 124.6(11) . . ? C11A N3 Fe 111.9(12) . . ? C12 N3 Fe 106.5(3) . . ? C11B N3 Fe 109.0(9) . . ? C11A N3 H3A 110.7 . . ? C12 N3 H3A 110.7 . . ? C11B N3 H3A 94.6 . . ? Fe N3 H3A 110.7 . . ? C14 N4 C13 118.1(3) . . ? C14 N4 Fe 126.4(3) . . ? C13 N4 Fe 115.1(3) . . ? O1 C1 C6 123.2(4) . . ? O1 C1 C2 119.0(4) . . ? C6 C1 C2 117.8(4) . . ? C3 C2 C1 121.2(5) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 118.9(5) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.2(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 119.8(4) . . ? C5 C6 C7 117.6(4) . . ? C1 C6 C7 122.5(4) . . ? N1 C7 C6 125.2(4) . . ? N1 C7 H7 117.4 . . ? C6 C7 H7 117.4 . . ? N1 C8 C9 108.8(4) . . ? N1 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? N1 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? N2 C9 C8 110.0(4) . . ? N2 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? N2 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N2 C10A C11A 99.4(14) . . ? N2 C10A H10A 111.9 . . ? C11A C10A H10A 111.9 . . ? N2 C10A H10B 111.9 . . ? C11A C10A H10B 111.9 . . ? H10A C10A H10B 109.6 . . ? N3 C11A C10A 109.3(19) . . ? N3 C11A H11A 109.8 . . ? C10A C11A H11A 109.8 . . ? N3 C11A H11B 109.8 . . ? C10A C11A H11B 109.8 . . ? H11A C11A H11B 108.3 . . ? N2 C10B C11B 108.7(17) . . ? N2 C10B H10C 110.0 . . ? C11B C10B H10C 110.0 . . ? N2 C10B H10D 110.0 . . ? C11B C10B H10D 110.0 . . ? H10C C10B H10D 108.3 . . ? C10B C11B N3 105.0(14) . . ? C10B C11B H11C 110.8 . . ? N3 C11B H11C 110.8 . . ? C10B C11B H11D 110.8 . . ? N3 C11B H11D 110.8 . . ? H11C C11B H11D 108.8 . . ? C13 C12 N3 113.2(4) . . ? C13 C12 H12A 108.9 . . ? N3 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? N3 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 N4 109.0(4) . . ? C12 C13 H13A 109.9 . . ? N4 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? N4 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 125.4(3) . . ? N4 C14 H14 117.3 . . ? C15 C14 H14 117.3 . . ? C16 C15 C20 120.0(4) . . ? C16 C15 C14 118.0(3) . . ? C20 C15 C14 121.9(3) . . ? C17 C16 C15 121.7(4) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 119.7(4) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 121.7(4) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? O2 C20 C19 118.8(3) . . ? O2 C20 C15 124.1(3) . . ? C19 C20 C15 117.1(3) . . ? O3 C21 O4 126.6(3) . . ? O3 C21 C22 116.5(3) . . ? O4 C21 C22 116.9(3) . . ? O5 C22 O6 127.2(3) . . ? O5 C22 C21 117.1(3) . . ? O6 C22 C21 115.8(3) . . ? O7 C23 O8 127.0(3) . . ? O7 C23 C24 116.8(3) . . ? O8 C23 C24 116.2(3) . . ? O10 C24 O9 127.2(3) . . ? O10 C24 C23 116.7(3) . . ? O9 C24 C23 116.1(3) . . ? O12 C25 O11 127.2(3) . . ? O12 C25 C25 116.3(4) . 3_558 ? O11 C25 C25 116.4(4) . 3_558 ? O14 C26 O13 127.0(3) . . ? O14 C26 C26 117.0(4) . 3_557 ? O13 C26 C26 116.0(3) . 3_557 ? C1 O1 Fe 129.8(3) . . ? C20 O2 Fe 131.1(2) . . ? C21 O3 Cr2 112.93(19) . 4_565 ? C21 O3 Mn2 112.93(19) . 4_565 ? Cr2 O3 Mn2 0.00(3) 4_565 4_565 ? C21 O4 Mn2 113.40(19) . . ? C22 O5 Cr2 113.89(19) . 4_565 ? C22 O5 Mn2 113.89(19) . 4_565 ? Cr2 O5 Mn2 0.00(3) 4_565 4_565 ? C22 O6 Mn2 114.47(19) . . ? C23 O7 Mn2 113.47(19) . . ? C23 O8 Mn1 113.6(2) . . ? C24 O9 Mn2 113.54(19) . . ? C24 O10 Mn1 113.6(2) . . ? C25 O11 Mn1 113.7(2) . . ? C25 O12 Cr1 113.9(2) . 3_558 ? C25 O12 Mn1 113.9(2) . 3_558 ? Cr1 O12 Mn1 0.000(15) 3_558 3_558 ? C26 O13 Mn1 113.9(2) . . ? C26 O14 Cr1 113.1(2) . 3_557 ? C26 O14 Mn1 113.1(2) . 3_557 ? Cr1 O14 Mn1 0.00(4) 3_557 3_557 ? Cl4S C1S Cl1S 76.5(10) . . ? Cl4S C1S Cl3S 122.3(6) . . ? Cl1S C1S Cl3S 94.2(4) . . ? Cl4S C1S Cl2S 33.9(9) . . ? Cl1S C1S Cl2S 109.5(3) . . ? Cl3S C1S Cl2S 125.5(3) . . ? Cl4S C1S H1S1 115.7 . . ? Cl1S C1S H1S1 109.8 . . ? Cl3S C1S H1S1 18.1 . . ? Cl2S C1S H1S1 109.8 . . ? Cl4S C1S H1S2 130.3 . . ? Cl1S C1S H1S2 109.8 . . ? Cl3S C1S H1S2 106.7 . . ? Cl2S C1S H1S2 109.8 . . ? H1S1 C1S H1S2 108.2 . . ? Cl4S C1S H1S3 107.7 . . ? Cl1S C1S H1S3 48.4 . . ? Cl3S C1S H1S3 106.6 . . ? Cl2S C1S H1S3 126.0 . . ? H1S1 C1S H1S3 123.8 . . ? H1S2 C1S H1S3 61.3 . . ? Cl4S C1S H1S4 105.9 . . ? Cl1S C1S H1S4 152.2 . . ? Cl3S C1S H1S4 106.8 . . ? Cl2S C1S H1S4 73.1 . . ? H1S1 C1S H1S4 94.4 . . ? H1S2 C1S H1S4 47.2 . . ? H1S3 C1S H1S4 106.6 . . ? C1S Cl1S H1S3 34.6 . . ? C1S Cl2S H1S4 31.5 . . ? O1 Fe O2 101.87(14) . . ? O1 Fe N1 89.87(14) . . ? O2 Fe N1 88.63(12) . . ? O1 Fe N4 89.81(14) . . ? O2 Fe N4 88.25(11) . . ? N1 Fe N4 176.73(14) . . ? O1 Fe N2 163.18(16) . . ? O2 Fe N2 91.38(13) . . ? N1 Fe N2 80.04(16) . . ? N4 Fe N2 101.02(15) . . ? O1 Fe N3 88.52(14) . . ? O2 Fe N3 164.35(12) . . ? N1 Fe N3 103.21(14) . . ? N4 Fe N3 80.03(13) . . ? N2 Fe N3 80.84(14) . . ? O13 Mn1 O14 79.93(8) . 3_557 ? O13 Mn1 O8 168.50(9) . . ? O14 Mn1 O8 91.94(9) 3_557 . ? O13 Mn1 O10 92.42(9) . . ? O14 Mn1 O10 92.59(9) 3_557 . ? O8 Mn1 O10 79.75(8) . . ? O13 Mn1 O12 95.05(9) . 3_558 ? O14 Mn1 O12 171.42(9) 3_557 3_558 ? O8 Mn1 O12 93.96(9) . 3_558 ? O10 Mn1 O12 94.58(9) . 3_558 ? O13 Mn1 O11 94.18(9) . . ? O14 Mn1 O11 93.82(9) 3_557 . ? O8 Mn1 O11 94.47(8) . . ? O10 Mn1 O11 171.51(9) . . ? O12 Mn1 O11 79.53(9) 3_558 . ? O7 Mn2 O6 95.61(9) . . ? O7 Mn2 O5 96.85(8) . 4_566 ? O6 Mn2 O5 94.36(9) . 4_566 ? O7 Mn2 O9 79.81(8) . . ? O6 Mn2 O9 94.98(9) . . ? O5 Mn2 O9 170.34(9) 4_566 . ? O7 Mn2 O4 167.51(9) . . ? O6 Mn2 O4 79.39(8) . . ? O5 Mn2 O4 94.96(9) 4_566 . ? O9 Mn2 O4 89.17(8) . . ? O7 Mn2 O3 92.05(9) . 4_566 ? O6 Mn2 O3 170.77(8) . 4_566 ? O5 Mn2 O3 79.58(8) 4_566 4_566 ? O9 Mn2 O3 91.43(9) . 4_566 ? O4 Mn2 O3 94.10(8) . 4_566 ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.645 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.071 data_shelxl _database_code_depnum_ccdc_archive 'CCDC 813714' #TrackingRef 'C27H26Cl2CrFeMnN4O14_90.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 Cl2 Cr Fe Mn N4 O14' _chemical_formula_weight 864.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 11.5602(4) _cell_length_b 31.6268(12) _cell_length_c 9.5237(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.199(4) _cell_angle_gamma 90.00 _cell_volume 3267.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 6961 _cell_measurement_theta_min 2.9819 _cell_measurement_theta_max 32.4716 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7693 _exptl_absorpt_correction_T_max 0.8973 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Single source at offset), Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0267 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29715 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1263 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 32.55 _reflns_number_total 10846 _reflns_number_gt 6039 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10846 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 0.9635(3) 0.18452(10) 1.1493(4) 0.0176(7) Uani 1 1 d . . . C2 C 1.0632(3) 0.19870(10) 1.2733(4) 0.0203(7) Uani 1 1 d . . . H2 H 1.1449 0.1914 1.2811 0.024 Uiso 1 1 calc R . . C3 C 1.0439(3) 0.22317(10) 1.3842(4) 0.0230(7) Uani 1 1 d . . . H3 H 1.1121 0.2323 1.4675 0.028 Uiso 1 1 calc R . . C4 C 0.9243(3) 0.23442(10) 1.3735(4) 0.0237(8) Uani 1 1 d . . . H4 H 0.9111 0.2511 1.4497 0.028 Uiso 1 1 calc R . . C5 C 0.8263(3) 0.22138(10) 1.2529(4) 0.0216(7) Uani 1 1 d . . . H5 H 0.7452 0.2292 1.2464 0.026 Uiso 1 1 calc R . . C6 C 0.8424(3) 0.19678(10) 1.1392(4) 0.0176(7) Uani 1 1 d . . . C7 C 0.7369(3) 0.18649(10) 1.0121(4) 0.0211(7) Uani 1 1 d . . . H7 H 0.6599 0.1977 1.0090 0.025 Uiso 1 1 calc R . . C8 C 0.6217(3) 0.15526(11) 0.7783(4) 0.0305(9) Uani 1 1 d . . . H8A H 0.6124 0.1753 0.6952 0.037 Uiso 1 1 calc R . . H8B H 0.5507 0.1589 0.8127 0.037 Uiso 1 1 calc R . . C9 C 0.6269(3) 0.11110(11) 0.7277(4) 0.0281(8) Uani 1 1 d . . . H9A H 0.5611 0.1065 0.6297 0.034 Uiso 1 1 calc R . . H9B H 0.6136 0.0911 0.8006 0.034 Uiso 1 1 calc R . . C10 C 0.7648(4) 0.11814(12) 0.5735(4) 0.0386(10) Uani 1 1 d . . . H10A H 0.6838 0.1177 0.4916 0.046 Uiso 1 1 calc R . . H10B H 0.8207 0.0987 0.5460 0.046 Uiso 1 1 calc R . . C11 C 0.8168(4) 0.16227(12) 0.5919(4) 0.0368(10) Uani 1 1 d . . . H11A H 0.8520 0.1680 0.5126 0.044 Uiso 1 1 calc R . . H11B H 0.7498 0.1829 0.5808 0.044 Uiso 1 1 calc R . . C12 C 1.0430(3) 0.15904(11) 0.7489(4) 0.0294(9) Uani 1 1 d . . . H12A H 1.1016 0.1752 0.8323 0.035 Uiso 1 1 calc R . . H12B H 1.0540 0.1679 0.6546 0.035 Uiso 1 1 calc R . . C13 C 1.0674(4) 0.11221(12) 0.7735(5) 0.0337(9) Uani 1 1 d . . . H13A H 1.0277 0.0966 0.6789 0.040 Uiso 1 1 calc R . . H13B H 1.1572 0.1067 0.8080 0.040 Uiso 1 1 calc R . . C14 C 1.0727(3) 0.06946(11) 0.9816(4) 0.0251(8) Uani 1 1 d . . . H14 H 1.1474 0.0584 0.9760 0.030 Uiso 1 1 calc R . . C15 C 1.0293(3) 0.05292(11) 1.0952(4) 0.0234(7) Uani 1 1 d . . . C16 C 1.1015(3) 0.02246(11) 1.1936(4) 0.0281(8) Uani 1 1 d . . . H16 H 1.1793 0.0151 1.1876 0.034 Uiso 1 1 calc R . . C17 C 1.0628(4) 0.00305(12) 1.2984(4) 0.0328(9) Uani 1 1 d . . . H17 H 1.1138 -0.0171 1.3656 0.039 Uiso 1 1 calc R . . C18 C 0.9463(4) 0.01352(12) 1.3047(5) 0.0367(10) Uani 1 1 d . . . H18 H 0.9175 -0.0005 1.3746 0.044 Uiso 1 1 calc R . . C19 C 0.8737(3) 0.04362(12) 1.2116(4) 0.0310(9) Uani 1 1 d . . . H19 H 0.7962 0.0507 1.2192 0.037 Uiso 1 1 calc R . . C20 C 0.9133(3) 0.06426(10) 1.1044(4) 0.0227(7) Uani 1 1 d . . . C21 C 0.3528(3) 0.23913(9) 0.8746(4) 0.0155(7) Uani 1 1 d . . . C22 C 0.4734(3) 0.26213(9) 0.9684(4) 0.0169(7) Uani 1 1 d . . . C23 C 0.3854(3) 0.12246(10) 1.2191(3) 0.0168(7) Uani 1 1 d . . . C24 C 0.5045(3) 0.12594(9) 1.1789(3) 0.0150(6) Uani 1 1 d . . . C25 C 0.4443(3) -0.01421(10) 1.4577(4) 0.0195(7) Uani 1 1 d . . . C26 C 0.5644(3) -0.00821(9) 1.0491(4) 0.0161(7) Uani 1 1 d . . . N1 N 0.7376(2) 0.16335(9) 0.9018(3) 0.0217(6) Uani 1 1 d . . . N2 N 0.7499(3) 0.10341(8) 0.7143(3) 0.0231(6) Uani 1 1 d . . . H2A H 0.7639 0.0744 0.7213 0.028 Uiso 1 1 calc R . . N3 N 0.9140(3) 0.16766(9) 0.7408(3) 0.0232(6) Uani 1 1 d . . . H3A H 0.9110 0.1956 0.7697 0.028 Uiso 1 1 calc R . . N4 N 1.0165(3) 0.09832(9) 0.8870(3) 0.0241(7) Uani 1 1 d . . . O1 O 0.98919(19) 0.16179(7) 1.0481(3) 0.0224(5) Uani 1 1 d . . . O2 O 0.8380(2) 0.09228(7) 1.0176(3) 0.0263(6) Uani 1 1 d . . . O3 O 0.3101(2) 0.24761(7) 0.7382(3) 0.0219(5) Uani 1 1 d . . . O4 O 0.3104(2) 0.21366(7) 0.9447(3) 0.0229(5) Uani 1 1 d . . . O5 O 0.51966(19) 0.28649(6) 0.8988(3) 0.0207(5) Uani 1 1 d . . . O6 O 0.51531(19) 0.25414(6) 1.1056(3) 0.0196(5) Uani 1 1 d . . . O7 O 0.3264(2) 0.15563(7) 1.2132(3) 0.0216(5) Uani 1 1 d . . . O8 O 0.3600(2) 0.08642(7) 1.2543(3) 0.0232(5) Uani 1 1 d . . . O9 O 0.5307(2) 0.16186(7) 1.1438(3) 0.0208(5) Uani 1 1 d . . . O10 O 0.5651(2) 0.09288(7) 1.1872(3) 0.0196(5) Uani 1 1 d . . . O11 O 0.3968(2) -0.00865(7) 1.3188(3) 0.0240(5) Uani 1 1 d . . . O12 O 0.4116(2) -0.04050(7) 1.5335(3) 0.0237(5) Uani 1 1 d . . . O13 O 0.60069(19) 0.00071(7) 1.1851(3) 0.0193(5) Uani 1 1 d . . . O14 O 0.62119(19) -0.02979(7) 0.9836(3) 0.0210(5) Uani 1 1 d . . . C1S C 0.2217(3) 0.11086(10) 1.4850(4) 0.0242(8) Uani 1 1 d . . . H1S1 H 0.1328 0.1129 1.4697 0.029 Uiso 1 1 calc R . . H1S2 H 0.2307 0.1085 1.3856 0.029 Uiso 1 1 calc R . . Cl1 Cl 0.29834(9) 0.15688(3) 1.57698(11) 0.0339(2) Uani 1 1 d . . . Cl2 Cl 0.28436(9) 0.06567(3) 1.59248(11) 0.0314(2) Uani 1 1 d . . . Fe Fe 0.87702(4) 0.130678(15) 0.89347(6) 0.01886(12) Uani 1 1 d . . . Mn1 Mn 0.41338(5) 0.208694(14) 1.17050(6) 0.01459(11) Uani 0.50 1 d P . 1 Cr1 Cr 0.41338(5) 0.208694(14) 1.17050(6) 0.01459(11) Uani 0.50 1 d P . 2 Mn2 Mn 0.48110(5) 0.039915(15) 1.24054(6) 0.01531(11) Uani 0.50 1 d P . 3 Cr2 Cr 0.48110(5) 0.039915(15) 1.24054(6) 0.01531(11) Uani 0.50 1 d P . 4 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 0.0184(16) 0.0200(17) 0.0160(16) 0.0020(14) 0.0078(14) -0.0011(13) C2 0.0130(15) 0.0249(18) 0.0225(18) -0.0013(15) 0.0055(14) -0.0009(13) C3 0.0223(17) 0.0216(18) 0.0239(19) -0.0014(15) 0.0066(15) -0.0072(14) C4 0.0273(19) 0.0186(18) 0.029(2) -0.0052(16) 0.0140(17) -0.0011(15) C5 0.0196(16) 0.0202(18) 0.028(2) 0.0056(15) 0.0119(16) 0.0063(14) C6 0.0146(15) 0.0193(17) 0.0194(17) 0.0045(14) 0.0067(14) -0.0016(13) C7 0.0175(16) 0.0209(18) 0.0262(19) 0.0019(15) 0.0091(15) 0.0005(14) C8 0.0180(17) 0.033(2) 0.032(2) -0.0047(18) -0.0023(16) 0.0022(16) C9 0.0156(16) 0.0227(19) 0.039(2) -0.0078(17) 0.0013(16) -0.0025(14) C10 0.045(2) 0.044(3) 0.020(2) -0.0042(19) 0.0043(18) -0.021(2) C11 0.036(2) 0.046(3) 0.022(2) 0.0099(19) 0.0013(18) -0.0133(19) C12 0.032(2) 0.029(2) 0.034(2) -0.0040(17) 0.0197(18) -0.0067(16) C13 0.037(2) 0.040(2) 0.035(2) -0.0014(19) 0.025(2) 0.0023(18) C14 0.0189(17) 0.027(2) 0.028(2) -0.0056(17) 0.0061(16) 0.0014(15) C15 0.0217(17) 0.0225(18) 0.0240(19) -0.0011(15) 0.0053(15) -0.0013(14) C16 0.0216(18) 0.025(2) 0.031(2) -0.0031(17) 0.0010(16) -0.0005(15) C17 0.034(2) 0.028(2) 0.028(2) 0.0035(17) 0.0000(18) 0.0027(17) C18 0.037(2) 0.040(2) 0.031(2) 0.010(2) 0.0084(19) -0.0070(19) C19 0.0208(18) 0.040(2) 0.031(2) 0.0069(19) 0.0080(17) -0.0022(17) C20 0.0186(17) 0.0232(19) 0.0216(19) 0.0010(15) 0.0011(15) -0.0029(14) C21 0.0113(14) 0.0133(16) 0.0214(18) -0.0083(14) 0.0051(14) 0.0009(12) C22 0.0123(14) 0.0135(16) 0.0263(19) -0.0046(14) 0.0085(14) 0.0024(12) C23 0.0146(14) 0.0250(19) 0.0114(15) -0.0012(13) 0.0053(12) -0.0043(13) C24 0.0142(14) 0.0186(17) 0.0117(16) -0.0019(13) 0.0039(12) -0.0015(13) C25 0.0149(15) 0.0159(18) 0.027(2) -0.0087(15) 0.0060(15) 0.0033(13) C26 0.0169(15) 0.0092(15) 0.0223(18) 0.0041(13) 0.0067(14) -0.0009(12) N1 0.0146(13) 0.0253(16) 0.0228(16) 0.0021(13) 0.0033(12) 0.0020(12) N2 0.0250(15) 0.0158(15) 0.0299(17) -0.0012(13) 0.0112(14) -0.0030(12) N3 0.0234(15) 0.0202(15) 0.0248(17) -0.0010(13) 0.0068(13) -0.0049(12) N4 0.0235(15) 0.0271(17) 0.0239(17) -0.0002(14) 0.0112(14) -0.0007(13) O1 0.0138(11) 0.0310(14) 0.0229(13) -0.0058(11) 0.0067(10) 0.0001(10) O2 0.0184(12) 0.0330(14) 0.0277(14) 0.0080(12) 0.0081(11) 0.0018(11) O3 0.0168(11) 0.0209(13) 0.0229(14) -0.0078(11) 0.0003(10) -0.0011(10) O4 0.0203(12) 0.0216(13) 0.0308(14) -0.0128(11) 0.0137(11) -0.0110(10) O5 0.0150(11) 0.0171(12) 0.0306(14) -0.0052(11) 0.0087(10) -0.0050(9) O6 0.0139(11) 0.0161(12) 0.0250(14) -0.0047(10) 0.0018(10) -0.0015(9) O7 0.0160(11) 0.0287(13) 0.0232(13) 0.0003(11) 0.0109(10) 0.0050(10) O8 0.0246(12) 0.0286(14) 0.0226(13) -0.0053(11) 0.0160(11) -0.0094(10) O9 0.0202(12) 0.0234(13) 0.0241(13) -0.0006(10) 0.0144(11) -0.0033(10) O10 0.0182(11) 0.0222(12) 0.0224(13) 0.0024(10) 0.0122(10) 0.0034(10) O11 0.0201(12) 0.0185(13) 0.0255(14) -0.0100(11) -0.0023(11) 0.0021(10) O12 0.0226(12) 0.0174(12) 0.0340(15) -0.0124(11) 0.0133(11) -0.0067(10) O13 0.0179(12) 0.0185(12) 0.0197(13) 0.0033(10) 0.0043(10) 0.0029(9) O14 0.0177(12) 0.0232(13) 0.0241(13) 0.0048(11) 0.0099(10) 0.0066(10) C1S 0.0203(17) 0.030(2) 0.0231(19) -0.0025(16) 0.0082(15) 0.0013(15) Cl1 0.0328(5) 0.0284(5) 0.0319(5) -0.0012(4) 0.0003(4) -0.0012(4) Cl2 0.0346(5) 0.0269(5) 0.0343(5) 0.0027(4) 0.0141(4) 0.0045(4) Fe 0.0150(2) 0.0211(3) 0.0199(3) 0.0008(2) 0.0053(2) -0.0008(2) Mn1 0.0178(2) 0.0114(2) 0.0165(3) 0.0007(2) 0.0084(2) 0.00094(19) Cr1 0.0178(2) 0.0114(2) 0.0165(3) 0.0007(2) 0.0084(2) 0.00094(19) Mn2 0.0202(3) 0.0118(2) 0.0153(3) 0.0002(2) 0.0078(2) 0.0013(2) Cr2 0.0202(3) 0.0118(2) 0.0153(3) 0.0002(2) 0.0078(2) 0.0013(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 1.316(3) . ? C1 C2 1.409(5) . ? C1 C6 1.423(4) . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? C3 C4 1.396(4) . ? C3 H3 0.9500 . ? C4 C5 1.370(5) . ? C4 H4 0.9500 . ? C5 C6 1.398(4) . ? C5 H5 0.9500 . ? C6 C7 1.428(5) . ? C7 N1 1.282(4) . ? C7 H7 0.9500 . ? C8 N1 1.468(4) . ? C8 C9 1.486(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.491(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.484(4) . ? C10 C11 1.506(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.484(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.491(4) . ? C12 C13 1.511(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N4 1.465(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.289(4) . ? C14 C15 1.439(5) . ? C14 H14 0.9500 . ? C15 C16 1.401(5) . ? C15 C20 1.420(4) . ? C16 C17 1.372(5) . ? C16 H16 0.9500 . ? C17 C18 1.409(5) . ? C17 H17 0.9500 . ? C18 C19 1.372(5) . ? C18 H18 0.9500 . ? C19 C20 1.414(5) . ? C19 H19 0.9500 . ? C20 O2 1.315(4) . ? C21 O3 1.249(4) . ? C21 O4 1.249(4) . ? C21 C22 1.553(4) . ? C22 O5 1.251(4) . ? C22 O6 1.253(4) . ? C23 O7 1.242(3) . ? C23 O8 1.251(3) . ? C23 C24 1.555(4) . ? C24 O10 1.246(3) . ? C24 O9 1.251(3) . ? C25 O12 1.242(4) . ? C25 O11 1.257(4) . ? C25 C25 1.550(6) 3_658 ? C26 O13 1.248(4) . ? C26 O14 1.253(3) . ? C26 C26 1.549(6) 3_657 ? N1 Fe 1.939(3) . ? N2 Fe 2.021(3) . ? N2 H2A 0.9300 . ? N3 Fe 2.023(3) . ? N3 H3A 0.9300 . ? N4 Fe 1.929(3) . ? O1 Fe 1.871(2) . ? O2 Fe 1.856(2) . ? O3 Cr1 2.069(2) 4_565 ? O3 Mn1 2.069(2) 4_565 ? O4 Mn1 2.073(3) . ? O5 Cr1 2.101(2) 4_565 ? O5 Mn1 2.101(2) 4_565 ? O6 Mn1 2.083(2) . ? O7 Mn1 2.068(2) . ? O8 Mn2 2.065(2) . ? O9 Mn1 2.082(2) . ? O10 Mn2 2.085(2) . ? O11 Mn2 2.089(2) . ? O12 Cr2 2.080(3) 3_658 ? O12 Mn2 2.080(3) 3_658 ? O13 Mn2 2.057(2) . ? O14 Cr2 2.077(2) 3_657 ? O14 Mn2 2.077(2) 3_657 ? C1S Cl2 1.762(3) . ? C1S Cl1 1.770(3) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? Mn1 O3 2.069(2) 4_566 ? Mn1 O5 2.101(2) 4_566 ? Mn2 O14 2.077(2) 3_657 ? Mn2 O12 2.080(3) 3_658 ? 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 117.5(3) . . ? O1 C1 C6 124.4(3) . . ? C2 C1 C6 118.1(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.4(3) . . ? C5 C6 C7 118.7(3) . . ? C1 C6 C7 121.8(3) . . ? N1 C7 C6 125.4(3) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? N1 C8 C9 107.2(3) . . ? N1 C8 H8A 110.3 . . ? C9 C8 H8A 110.3 . . ? N1 C8 H8B 110.3 . . ? C9 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? C8 C9 N2 109.1(3) . . ? C8 C9 H9A 109.9 . . ? N2 C9 H9A 109.9 . . ? C8 C9 H9B 109.9 . . ? N2 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 C11 110.6(3) . . ? N2 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N3 C11 C10 111.0(3) . . ? N3 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N3 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N3 C12 C13 108.5(3) . . ? N3 C12 H12A 110.0 . . ? C13 C12 H12A 110.0 . . ? N3 C12 H12B 110.0 . . ? C13 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N4 C13 C12 107.9(3) . . ? N4 C13 H13A 110.1 . . ? C12 C13 H13A 110.1 . . ? N4 C13 H13B 110.1 . . ? C12 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N4 C14 C15 124.1(3) . . ? N4 C14 H14 117.9 . . ? C15 C14 H14 117.9 . . ? C16 C15 C20 119.3(3) . . ? C16 C15 C14 118.1(3) . . ? C20 C15 C14 122.4(3) . . ? C17 C16 C15 121.7(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 118.9(4) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 121.0(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? O2 C20 C19 117.1(3) . . ? O2 C20 C15 124.4(3) . . ? C19 C20 C15 118.4(3) . . ? O3 C21 O4 127.4(3) . . ? O3 C21 C22 116.9(3) . . ? O4 C21 C22 115.7(3) . . ? O5 C22 O6 126.5(3) . . ? O5 C22 C21 116.5(3) . . ? O6 C22 C21 116.9(3) . . ? O7 C23 O8 127.3(3) . . ? O7 C23 C24 116.6(3) . . ? O8 C23 C24 116.1(3) . . ? O10 C24 O9 126.6(3) . . ? O10 C24 C23 116.8(3) . . ? O9 C24 C23 116.5(3) . . ? O12 C25 O11 126.5(3) . . ? O12 C25 C25 116.8(4) . 3_658 ? O11 C25 C25 116.6(4) . 3_658 ? O13 C26 O14 126.4(3) . . ? O13 C26 C26 117.3(3) . 3_657 ? O14 C26 C26 116.2(4) . 3_657 ? C7 N1 C8 119.6(3) . . ? C7 N1 Fe 125.3(2) . . ? C8 N1 Fe 114.6(2) . . ? C10 N2 C9 116.0(3) . . ? C10 N2 Fe 110.6(2) . . ? C9 N2 Fe 107.2(2) . . ? C10 N2 H2A 107.6 . . ? C9 N2 H2A 107.6 . . ? Fe N2 H2A 107.6 . . ? C11 N3 C12 116.2(3) . . ? C11 N3 Fe 110.0(2) . . ? C12 N3 Fe 108.3(2) . . ? C11 N3 H3A 107.3 . . ? C12 N3 H3A 107.3 . . ? Fe N3 H3A 107.3 . . ? C14 N4 C13 119.6(3) . . ? C14 N4 Fe 125.3(2) . . ? C13 N4 Fe 114.7(2) . . ? C1 O1 Fe 126.4(2) . . ? C20 O2 Fe 126.0(2) . . ? C21 O3 Cr1 113.8(2) . 4_565 ? C21 O3 Mn1 113.8(2) . 4_565 ? Cr1 O3 Mn1 0.00(3) 4_565 4_565 ? C21 O4 Mn1 114.4(2) . . ? C22 O5 Cr1 112.9(2) . 4_565 ? C22 O5 Mn1 112.9(2) . 4_565 ? Cr1 O5 Mn1 0.00(3) 4_565 4_565 ? C22 O6 Mn1 113.2(2) . . ? C23 O7 Mn1 113.44(18) . . ? C23 O8 Mn2 113.92(18) . . ? C24 O9 Mn1 112.68(17) . . ? C24 O10 Mn2 112.99(18) . . ? C25 O11 Mn2 113.0(2) . . ? C25 O12 Cr2 113.7(2) . 3_658 ? C25 O12 Mn2 113.7(2) . 3_658 ? Cr2 O12 Mn2 0.000(17) 3_658 3_658 ? C26 O13 Mn2 112.82(19) . . ? C26 O14 Cr2 112.7(2) . 3_657 ? C26 O14 Mn2 112.7(2) . 3_657 ? Cr2 O14 Mn2 0.00(4) 3_657 3_657 ? Cl2 C1S Cl1 110.1(2) . . ? Cl2 C1S H1S1 109.6 . . ? Cl1 C1S H1S1 109.6 . . ? Cl2 C1S H1S2 109.6 . . ? Cl1 C1S H1S2 109.6 . . ? H1S1 C1S H1S2 108.1 . . ? O2 Fe O1 95.60(11) . . ? O2 Fe N4 93.61(11) . . ? O1 Fe N4 86.80(11) . . ? O2 Fe N1 86.23(11) . . ? O1 Fe N1 92.72(11) . . ? N4 Fe N1 179.48(14) . . ? O2 Fe N2 89.58(11) . . ? O1 Fe N2 173.48(11) . . ? N4 Fe N2 96.84(12) . . ? N1 Fe N2 83.66(12) . . ? O2 Fe N3 173.79(11) . . ? O1 Fe N3 90.03(11) . . ? N4 Fe N3 84.10(11) . . ? N1 Fe N3 96.12(11) . . ? N2 Fe N3 84.98(11) . . ? O7 Mn1 O3 96.24(8) . 4_566 ? O7 Mn1 O4 96.97(9) . . ? O3 Mn1 O4 94.93(9) 4_566 . ? O7 Mn1 O9 80.10(8) . . ? O3 Mn1 O9 169.48(9) 4_566 . ? O4 Mn1 O9 95.30(9) . . ? O7 Mn1 O6 169.03(8) . . ? O3 Mn1 O6 94.46(8) 4_566 . ? O4 Mn1 O6 79.70(9) . . ? O9 Mn1 O6 89.76(8) . . ? O7 Mn1 O5 90.32(9) . 4_566 ? O3 Mn1 O5 79.83(9) 4_566 4_566 ? O4 Mn1 O5 171.47(8) . 4_566 ? O9 Mn1 O5 90.28(9) . 4_566 ? O6 Mn1 O5 93.91(9) . 4_566 ? O13 Mn2 O8 167.33(9) . . ? O13 Mn2 O14 80.66(9) . 3_657 ? O8 Mn2 O14 90.98(9) . 3_657 ? O13 Mn2 O12 93.30(9) . 3_658 ? O8 Mn2 O12 95.92(9) . 3_658 ? O14 Mn2 O12 171.54(9) 3_657 3_658 ? O13 Mn2 O10 90.62(8) . . ? O8 Mn2 O10 79.99(8) . . ? O14 Mn2 O10 91.22(9) 3_657 . ? O12 Mn2 O10 94.77(9) 3_658 . ? O13 Mn2 O11 94.93(8) . . ? O8 Mn2 O11 95.24(8) . . ? O14 Mn2 O11 94.77(9) 3_657 . ? O12 Mn2 O11 79.77(9) 3_658 . ? O10 Mn2 O11 172.41(9) . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.059 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.108