# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sylvie Ferlay Maxim' _publ_contact_author_email 'maxim catalin@yahoo.com' loop_ _publ_author_name S.F.Maxim M.W.Hosseini data_cms27 _database_code_depnum_ccdc_archive 'CCDC 804356' #TrackingRef 'CCDC-804356.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 Fe Mn N2 O19' _chemical_formula_weight 651.18 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' Fe Fe 0.3463 0.8444 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0124(2) _cell_length_b 19.4857(4) _cell_length_c 14.4710(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.089(1) _cell_angle_gamma 90.00 _cell_volume 2526.96(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8476 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 30.06 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.94 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21357 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7379 _reflns_number_gt 6055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The hydrogen atoms of the water molecules were located on a fourrier map and refined with restraints(O-H = 0.82A and H-H = 1.54A). ; _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^)+(0.0475P)^2^+1.6129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7379 _refine_ls_number_parameters 401 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.971 _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 C1 C -0.50787(16) 0.08055(8) 0.33343(10) 0.0184(3) Uani 1 1 d . . . C2 C -0.5057(2) 0.18458(10) 0.42796(13) 0.0351(4) Uani 1 1 d . . . H2A H -0.6013 0.2055 0.4320 0.053 Uiso 1 1 calc R . . H2B H -0.4300 0.2194 0.4315 0.053 Uiso 1 1 calc R . . H2C H -0.4846 0.1528 0.4784 0.053 Uiso 1 1 calc R . . C3 C -0.5116(2) -0.02644(10) 0.24424(13) 0.0341(4) Uani 1 1 d . . . H3A H -0.5191 -0.0467 0.3040 0.051 Uiso 1 1 calc R . . H3B H -0.4222 -0.0422 0.2204 0.051 Uiso 1 1 calc R . . H3C H -0.5968 -0.0394 0.2023 0.051 Uiso 1 1 calc R . . C4 C -0.63331(17) 0.03129(9) 0.46408(11) 0.0230(3) Uani 1 1 d . . . H4 H -0.7218 0.0523 0.4400 0.028 Uiso 1 1 calc R . . C5 C -0.50460(17) 0.03896(8) 0.41997(10) 0.0195(3) Uani 1 1 d . . . C6 C -0.37138(18) 0.00803(9) 0.45550(11) 0.0240(3) Uani 1 1 d . . . H6 H -0.2858 0.0136 0.4256 0.029 Uiso 1 1 calc R . . C8 C -0.5046(2) 0.08609(9) 0.16533(11) 0.0261(3) Uani 1 1 d . . . H8A H -0.5561 0.0598 0.1148 0.031 Uiso 1 1 calc R . . H8B H -0.4022 0.0926 0.1522 0.031 Uiso 1 1 calc R . . N1 N -0.50681(15) 0.04814(7) 0.25324(9) 0.0220(3) Uani 1 1 d . . . N2 N -0.50742(15) 0.14796(7) 0.33956(9) 0.0223(3) Uani 1 1 d . . . C7 C -0.5134(2) 0.19215(10) 0.25700(13) 0.0340(4) Uani 1 1 d . . . H20A H -0.4135 0.2075 0.2482 0.041 Uiso 1 1 calc R . . H20B H -0.5736 0.2323 0.2663 0.041 Uiso 1 1 calc R . . C9 C -0.5788(2) 0.15445(11) 0.17185(13) 0.0333(4) Uani 1 1 d . . . H21A H -0.6850 0.1479 0.1745 0.040 Uiso 1 1 calc R . . H21B H -0.5655 0.1814 0.1170 0.040 Uiso 1 1 calc R . . C10 C -0.07848(15) -0.08369(7) 0.73089(10) 0.0149(3) Uani 1 1 d . . . C11 C 0.08569(15) -0.08652(7) 0.77501(10) 0.0151(3) Uani 1 1 d . . . C12 C -0.00092(18) 0.09994(8) 0.58229(11) 0.0197(3) Uani 1 1 d . . . C13 C -0.12611(17) 0.14007(8) 0.62530(11) 0.0195(3) Uani 1 1 d . . . C14 C 0.01680(19) 0.10395(8) 0.94796(11) 0.0225(3) Uani 1 1 d . . . C15 C 0.15530(17) 0.13427(8) 0.90709(11) 0.0196(3) Uani 1 1 d . . . Fe Fe 0.00530(2) 0.052289(10) 0.765089(14) 0.01408(6) Uani 1 1 d . . . Mn Mn -0.00274(2) -0.230401(11) 0.736043(16) 0.01573(6) Uani 1 1 d . . . O1 O -0.13795(11) -0.02454(5) 0.72985(8) 0.0184(2) Uani 1 1 d . . . O2 O 0.14323(11) -0.02852(5) 0.79834(8) 0.0176(2) Uani 1 1 d . . . O3 O 0.14718(12) -0.14289(5) 0.78474(8) 0.0211(2) Uani 1 1 d . . . O4 O -0.13856(11) -0.13733(5) 0.70151(8) 0.0184(2) Uani 1 1 d . . . O5 O -0.17200(14) -0.30276(6) 0.68375(8) 0.0249(2) Uani 1 1 d D . . O6 O 0.16259(15) -0.30405(7) 0.78435(9) 0.0304(3) Uani 1 1 d D . . O7 O -0.08019(14) -0.23253(6) 0.87092(8) 0.0222(2) Uani 1 1 d D . . O8 O 0.07267(17) -0.22363(7) 0.59914(9) 0.0338(3) Uani 1 1 d D . . O10 O -0.06286(13) 0.06402(6) 0.89181(8) 0.0204(2) Uani 1 1 d . . . O11 O 0.16492(12) 0.11660(6) 0.82227(8) 0.0202(2) Uani 1 1 d . . . O12 O -0.13932(12) 0.12394(6) 0.71085(7) 0.0195(2) Uani 1 1 d . . . O13 O 0.07585(13) 0.06061(6) 0.64030(8) 0.0212(2) Uani 1 1 d . . . O14 O -0.00803(18) 0.11812(8) 1.02701(9) 0.0420(4) Uani 1 1 d . . . O15 O 0.24241(14) 0.17133(6) 0.95447(9) 0.0293(3) Uani 1 1 d . . . O16 O 0.01721(15) 0.10842(7) 0.50045(9) 0.0311(3) Uani 1 1 d . . . O17 O -0.19916(15) 0.18286(7) 0.57951(9) 0.0316(3) Uani 1 1 d . . . O1W O 0.72381(14) 0.00903(7) 0.00964(9) 0.0282(3) Uani 1 1 d D . . O2W O -0.06905(17) -0.37122(8) 0.54114(10) 0.0409(4) Uani 1 1 d D . . O3W O 0.3032(2) -0.25550(12) 0.94386(14) 0.0580(5) Uani 1 1 d D . . H1W H -0.065(3) -0.1943(10) 0.9077(16) 0.053(7) Uiso 1 1 d D . . H2W H -0.150(2) -0.2548(11) 0.8848(17) 0.044(7) Uiso 1 1 d D . . H3W H 0.066(3) -0.1828(9) 0.5670(16) 0.047(7) Uiso 1 1 d D . . H4W H 0.138(2) -0.2484(11) 0.5820(16) 0.037(6) Uiso 1 1 d D . . H5W H -0.222(2) -0.3256(12) 0.7175(15) 0.046(7) Uiso 1 1 d D . . H6W H -0.148(3) -0.3287(12) 0.6336(14) 0.055(8) Uiso 1 1 d D . . H7W H 0.213(3) -0.2942(14) 0.8349(14) 0.056(8) Uiso 1 1 d D . . H8W H 0.219(3) -0.3300(12) 0.7476(16) 0.057(8) Uiso 1 1 d D . . H9W H 0.0341(19) -0.3741(15) 0.544(2) 0.071(9) Uiso 1 1 d D . . H10W H -0.106(3) -0.4086(10) 0.5233(18) 0.051(8) Uiso 1 1 d D . . H11W H 0.295(4) -0.2169(11) 0.958(3) 0.105(15) Uiso 1 1 d D . . H12W H 0.357(5) -0.286(2) 0.986(3) 0.18(2) Uiso 1 1 d D . . H14W H 0.796(2) 0.0189(14) -0.0298(16) 0.056(8) Uiso 1 1 d D . . H13W H 0.760(3) 0.0198(12) 0.0618(12) 0.042(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0156(6) 0.0219(7) 0.0176(7) 0.0024(5) 0.0014(5) 0.0016(5) C2 0.0481(11) 0.0289(9) 0.0280(9) -0.0081(7) 0.0021(8) 0.0002(8) C3 0.0472(11) 0.0247(9) 0.0316(9) -0.0052(7) 0.0102(8) -0.0008(7) C4 0.0179(7) 0.0302(8) 0.0208(7) 0.0054(6) 0.0011(6) 0.0057(6) C5 0.0211(7) 0.0220(7) 0.0155(7) 0.0019(5) 0.0014(5) 0.0024(6) C6 0.0198(7) 0.0320(8) 0.0208(7) 0.0058(6) 0.0050(6) 0.0042(6) C8 0.0283(8) 0.0348(9) 0.0155(7) 0.0019(6) 0.0031(6) -0.0028(7) N1 0.0266(7) 0.0233(7) 0.0162(6) 0.0011(5) 0.0032(5) -0.0012(5) N2 0.0252(6) 0.0221(6) 0.0195(6) 0.0012(5) 0.0026(5) 0.0019(5) C7 0.0487(11) 0.0231(9) 0.0323(9) 0.0092(7) 0.0138(8) 0.0082(7) C9 0.0292(9) 0.0472(11) 0.0245(8) 0.0146(8) 0.0074(7) 0.0126(8) C10 0.0134(6) 0.0157(6) 0.0156(6) 0.0014(5) 0.0021(5) -0.0004(5) C11 0.0136(6) 0.0151(6) 0.0167(6) 0.0007(5) 0.0020(5) -0.0004(5) C12 0.0238(7) 0.0170(7) 0.0194(7) 0.0016(5) 0.0071(6) 0.0034(5) C13 0.0223(7) 0.0174(7) 0.0195(7) 0.0009(5) 0.0052(6) 0.0038(5) C14 0.0297(8) 0.0172(7) 0.0216(7) -0.0031(6) 0.0084(6) -0.0058(6) C15 0.0248(7) 0.0146(6) 0.0195(7) 0.0007(5) 0.0035(6) -0.0033(5) Fe 0.01649(10) 0.01172(10) 0.01421(10) 0.00044(7) 0.00248(7) 0.00067(7) Mn 0.01813(11) 0.01233(11) 0.01726(11) -0.00045(8) 0.00439(8) -0.00009(8) O1 0.0151(5) 0.0152(5) 0.0242(5) -0.0007(4) -0.0015(4) 0.0018(4) O2 0.0157(5) 0.0140(5) 0.0224(5) 0.0005(4) -0.0016(4) -0.0006(4) O3 0.0162(5) 0.0144(5) 0.0321(6) 0.0000(4) -0.0005(4) 0.0018(4) O4 0.0170(5) 0.0150(5) 0.0227(5) -0.0011(4) 0.0002(4) -0.0020(4) O5 0.0294(6) 0.0235(6) 0.0230(6) -0.0038(5) 0.0087(5) -0.0104(5) O6 0.0333(7) 0.0320(7) 0.0254(6) -0.0048(5) 0.0009(5) 0.0165(5) O7 0.0273(6) 0.0209(6) 0.0195(5) -0.0027(4) 0.0081(5) -0.0051(4) O8 0.0511(8) 0.0244(6) 0.0303(7) 0.0078(5) 0.0248(6) 0.0105(6) O10 0.0244(5) 0.0196(5) 0.0181(5) -0.0021(4) 0.0072(4) -0.0058(4) O11 0.0245(5) 0.0189(5) 0.0181(5) -0.0013(4) 0.0063(4) -0.0063(4) O12 0.0233(5) 0.0182(5) 0.0178(5) 0.0020(4) 0.0066(4) 0.0070(4) O13 0.0237(5) 0.0222(5) 0.0186(5) 0.0033(4) 0.0068(4) 0.0081(4) O14 0.0581(9) 0.0458(8) 0.0257(6) -0.0180(6) 0.0219(6) -0.0268(7) O15 0.0360(7) 0.0269(6) 0.0248(6) -0.0042(5) 0.0027(5) -0.0142(5) O16 0.0409(7) 0.0343(7) 0.0202(6) 0.0075(5) 0.0126(5) 0.0142(6) O17 0.0370(7) 0.0343(7) 0.0247(6) 0.0105(5) 0.0083(5) 0.0195(5) O1W 0.0247(6) 0.0356(7) 0.0240(6) 0.0005(5) 0.0008(5) -0.0038(5) O2W 0.0432(8) 0.0496(9) 0.0321(7) -0.0181(7) 0.0150(6) -0.0194(7) O3W 0.0574(11) 0.0661(13) 0.0462(10) -0.0141(10) -0.0145(8) 0.0002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.316(2) . ? C1 N1 1.322(2) . ? C1 C5 1.489(2) . ? C2 N2 1.463(2) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N1 1.459(2) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.390(2) . ? C4 C6 1.390(2) 3_456 ? C4 H4 0.9300 . ? C5 C6 1.392(2) . ? C6 C4 1.390(2) 3_456 ? C6 H6 0.9300 . ? C8 N1 1.474(2) . ? C8 C9 1.498(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N2 C7 1.469(2) . ? C7 C9 1.500(3) . ? C7 H20A 0.9700 . ? C7 H20B 0.9700 . ? C9 H21A 0.9700 . ? C9 H21B 0.9700 . ? C10 O4 1.2319(17) . ? C10 O1 1.2704(17) . ? C10 C11 1.549(2) . ? C11 O3 1.2316(17) . ? C11 O2 1.2739(17) . ? C12 O16 1.2238(19) . ? C12 O13 1.2835(19) . ? C12 C13 1.556(2) . ? C13 O17 1.2146(19) . ? C13 O12 1.2949(18) . ? C14 O14 1.220(2) . ? C14 O10 1.2874(19) . ? C14 C15 1.554(2) . ? C15 O15 1.2222(19) . ? C15 O11 1.2866(18) . ? Fe O13 1.9838(11) . ? Fe O1 2.0071(11) . ? Fe O10 2.0077(11) . ? Fe O12 2.0117(11) . ? Fe O11 2.0179(11) . ? Fe O2 2.0321(10) . ? Mn O6 2.1325(12) . ? Mn O7 2.1418(11) . ? Mn O5 2.1547(12) . ? Mn O8 2.1656(12) . ? Mn O4 2.2152(11) . ? Mn O3 2.2424(11) . ? O5 H5W 0.827(17) . ? O5 H6W 0.929(16) . ? O6 H7W 0.841(17) . ? O6 H8W 0.925(16) . ? O7 H1W 0.918(16) . ? O7 H2W 0.808(17) . ? O8 H3W 0.920(16) . ? O8 H4W 0.819(17) . ? O1W H14W 0.928(16) . ? O1W H13W 0.818(17) . ? O2W H9W 0.928(17) . ? O2W H10W 0.831(17) . ? O3W H11W 0.783(19) . ? O3W H12W 0.949(19) . ? 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 N2 C1 N1 122.38(14) . . ? N2 C1 C5 119.12(14) . . ? N1 C1 C5 118.47(14) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 119.40(14) . 3_456 ? C5 C4 H4 120.3 . . ? C6 C4 H4 120.3 3_456 . ? C4 C5 C6 120.85(14) . . ? C4 C5 C1 120.10(14) . . ? C6 C5 C1 119.04(13) . . ? C4 C6 C5 119.75(14) 3_456 . ? C4 C6 H6 120.1 3_456 . ? C5 C6 H6 120.1 . . ? N1 C8 C9 110.17(13) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C1 N1 C3 123.45(14) . . ? C1 N1 C8 121.34(14) . . ? C3 N1 C8 115.19(14) . . ? C1 N2 C2 123.03(14) . . ? C1 N2 C7 122.03(14) . . ? C2 N2 C7 114.91(15) . . ? N2 C7 C9 111.00(16) . . ? N2 C7 H20A 109.4 . . ? C9 C7 H20A 109.4 . . ? N2 C7 H20B 109.4 . . ? C9 C7 H20B 109.4 . . ? H20A C7 H20B 108.0 . . ? C8 C9 C7 110.36(15) . . ? C8 C9 H21A 109.6 . . ? C7 C9 H21A 109.6 . . ? C8 C9 H21B 109.6 . . ? C7 C9 H21B 109.6 . . ? H21A C9 H21B 108.1 . . ? O4 C10 O1 126.60(13) . . ? O4 C10 C11 118.53(12) . . ? O1 C10 C11 114.86(12) . . ? O3 C11 O2 126.54(13) . . ? O3 C11 C10 118.51(12) . . ? O2 C11 C10 114.95(12) . . ? O16 C12 O13 126.55(14) . . ? O16 C12 C13 119.75(14) . . ? O13 C12 C13 113.70(13) . . ? O17 C13 O12 126.06(14) . . ? O17 C13 C12 120.06(13) . . ? O12 C13 C12 113.86(13) . . ? O14 C14 O10 125.67(15) . . ? O14 C14 C15 120.36(15) . . ? O10 C14 C15 113.97(13) . . ? O15 C15 O11 126.09(14) . . ? O15 C15 C14 120.36(14) . . ? O11 C15 C14 113.55(13) . . ? O13 Fe O1 95.12(5) . . ? O13 Fe O10 168.75(5) . . ? O1 Fe O10 93.79(4) . . ? O13 Fe O12 81.09(4) . . ? O1 Fe O12 92.63(5) . . ? O10 Fe O12 91.66(4) . . ? O13 Fe O11 92.24(5) . . ? O1 Fe O11 168.17(5) . . ? O10 Fe O11 80.13(4) . . ? O12 Fe O11 97.65(5) . . ? O13 Fe O2 91.82(4) . . ? O1 Fe O2 80.97(4) . . ? O10 Fe O2 96.35(5) . . ? O12 Fe O2 170.03(4) . . ? O11 Fe O2 89.57(4) . . ? O6 Mn O7 88.41(5) . . ? O6 Mn O5 96.82(6) . . ? O7 Mn O5 91.16(5) . . ? O6 Mn O8 93.71(5) . . ? O7 Mn O8 177.52(5) . . ? O5 Mn O8 89.87(5) . . ? O6 Mn O4 167.18(5) . . ? O7 Mn O4 89.76(4) . . ? O5 Mn O4 95.90(4) . . ? O8 Mn O4 87.90(5) . . ? O6 Mn O3 91.83(5) . . ? O7 Mn O3 88.40(4) . . ? O5 Mn O3 171.32(5) . . ? O8 Mn O3 90.23(5) . . ? O4 Mn O3 75.43(4) . . ? C10 O1 Fe 114.49(9) . . ? C11 O2 Fe 113.77(9) . . ? C11 O3 Mn 113.17(9) . . ? C10 O4 Mn 113.87(9) . . ? Mn O5 H5W 123.5(17) . . ? Mn O5 H6W 114.4(16) . . ? H5W O5 H6W 111(2) . . ? Mn O6 H7W 115.0(18) . . ? Mn O6 H8W 126.0(17) . . ? H7W O6 H8W 110(2) . . ? Mn O7 H1W 118.1(16) . . ? Mn O7 H2W 125.1(18) . . ? H1W O7 H2W 111(2) . . ? Mn O8 H3W 120.2(15) . . ? Mn O8 H4W 123.1(17) . . ? H3W O8 H4W 112(2) . . ? C14 O10 Fe 116.18(9) . . ? C15 O11 Fe 116.11(9) . . ? C13 O12 Fe 114.83(9) . . ? C12 O13 Fe 116.20(9) . . ? H14W O1W H13W 106(2) . . ? H9W O2W H10W 109(2) . . ? H11W O3W H12W 120(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.504 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.059 # Attachment 'CCDC-804357.cif' data_e1933a _database_code_depnum_ccdc_archive 'CCDC 804357' #TrackingRef 'CCDC-804357.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H28 Cr Mn N2 O19' _chemical_formula_weight 647.33 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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0030(2) _cell_length_b 19.3913(5) _cell_length_c 14.5081(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.087(1) _cell_angle_gamma 90.00 _cell_volume 2518.54(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7956 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15487 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4875 _reflns_number_gt 4126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The hydrogen atoms of the water molecules were located on a fourrier map and refined with restraints(O-H = 0.82A and H-H = 1.54A). ; _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^)+(0.1533P)^2^+0.7392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4875 _refine_ls_number_parameters 399 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2217 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.187 _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 C1 C 0.4936(5) 0.0798(2) 0.3325(3) 0.0393(9) Uani 1 1 d . . . C2 C 0.4988(6) 0.1847(3) 0.4267(3) 0.0555(12) Uani 1 1 d . . . H2A H 0.4982 0.2335 0.4152 0.083 Uiso 1 1 calc R . . H2B H 0.5880 0.1726 0.4656 0.083 Uiso 1 1 calc R . . H2C H 0.4129 0.1725 0.4572 0.083 Uiso 1 1 calc R . . C3 C 0.4872(6) -0.0280(3) 0.2446(3) 0.0544(13) Uani 1 1 d . . . H3A H 0.4894 -0.0407 0.1808 0.082 Uiso 1 1 calc R . . H3B H 0.3968 -0.0448 0.2663 0.082 Uiso 1 1 calc R . . H3C H 0.5717 -0.0478 0.2811 0.082 Uiso 1 1 calc R . . C4 C 0.3667(5) 0.0314(2) 0.4640(3) 0.0425(10) Uani 1 1 d . . . H4 H 0.2784 0.0525 0.4397 0.051 Uiso 1 1 calc R . . C5 C 0.4968(5) 0.0380(2) 0.4192(3) 0.0402(9) Uani 1 1 d . . . C6 C 0.6284(5) 0.0070(2) 0.4553(3) 0.0424(10) Uani 1 1 d . . . H6 H 0.7140 0.0119 0.4252 0.051 Uiso 1 1 calc R . . C7 C 0.4888(6) 0.1911(3) 0.2557(4) 0.0566(13) Uani 1 1 d . . . H20A H 0.5888 0.2063 0.2465 0.068 Uiso 1 1 calc R . . H20B H 0.4288 0.2317 0.2645 0.068 Uiso 1 1 calc R . . C8 C 0.4948(5) 0.0841(3) 0.1653(3) 0.0475(11) Uani 1 1 d . . . H8A H 0.4422 0.0579 0.1151 0.057 Uiso 1 1 calc R . . H8B H 0.5972 0.0902 0.1518 0.057 Uiso 1 1 calc R . . C9 C 0.4227(6) 0.1525(3) 0.1717(3) 0.0576(13) Uani 1 1 d . . . H21A H 0.3164 0.1464 0.1748 0.069 Uiso 1 1 calc R . . H21B H 0.4357 0.1792 0.1166 0.069 Uiso 1 1 calc R . . C10 C 0.9211(4) 0.9204(2) 0.7297(3) 0.0347(9) Uani 1 1 d . . . C11 C 1.0842(4) 0.9171(2) 0.7768(3) 0.0360(9) Uani 1 1 d . . . C12 C 0.9995(5) 1.0986(2) 0.5847(3) 0.0390(9) Uani 1 1 d . . . C13 C 0.8778(4) 1.1411(2) 0.6286(3) 0.0382(9) Uani 1 1 d . . . C14 C 1.0218(5) 1.1028(2) 0.9471(3) 0.0418(10) Uani 1 1 d . . . C15 C 1.1551(5) 1.1352(2) 0.9046(3) 0.0394(9) Uani 1 1 d . . . N1 N 0.4928(4) 0.0460(2) 0.2530(2) 0.0431(9) Uani 1 1 d . . . N2 N 0.4949(4) 0.1474(2) 0.3383(2) 0.0425(8) Uani 1 1 d . . . Cr Cr 1.00664(6) 1.05408(4) 0.76565(4) 0.0337(3) Uani 1 1 d . . . Mn Mn 0.99591(6) 0.77241(4) 0.73671(4) 0.0357(3) Uani 1 1 d . . . O1 O 0.8630(3) 0.98000(16) 0.7262(2) 0.0375(7) Uani 1 1 d . . . O2 O 1.1403(3) 0.97482(16) 0.8022(2) 0.0379(7) Uani 1 1 d . . . O3 O 1.1445(3) 0.86015(16) 0.7873(2) 0.0412(7) Uani 1 1 d . . . O4 O 0.8606(3) 0.86633(16) 0.70084(19) 0.0378(7) Uani 1 1 d . . . O5 O 0.8268(4) 0.70013(18) 0.6832(2) 0.0443(8) Uani 1 1 d D . . O6 O 1.1611(4) 0.69847(19) 0.7854(2) 0.0490(8) Uani 1 1 d D . . O7 O 0.9166(4) 0.76966(17) 0.8711(2) 0.0406(7) Uani 1 1 d D . . O8 O 1.0760(4) 0.77958(19) 0.6014(2) 0.0513(9) Uani 1 1 d D . . O10 O 0.9410(3) 1.06183(16) 0.8915(2) 0.0391(7) Uani 1 1 d . . . O11 O 1.1599(3) 1.12054(16) 0.8183(2) 0.0397(7) Uani 1 1 d . . . O12 O 0.8686(3) 1.12696(16) 0.7149(2) 0.0391(7) Uani 1 1 d . . . O13 O 1.0743(3) 1.05784(16) 0.6418(2) 0.0391(7) Uani 1 1 d . . . O14 O 0.9975(4) 1.1159(2) 1.0262(2) 0.0588(10) Uani 1 1 d . . . O15 O 1.2450(4) 1.17190(18) 0.9512(2) 0.0497(8) Uani 1 1 d . . . O16 O 1.0189(4) 1.10727(19) 0.5037(2) 0.0500(8) Uani 1 1 d . . . O17 O 0.8036(4) 1.18346(19) 0.5823(2) 0.0526(9) Uani 1 1 d . . . O1W O 0.7246(4) 0.01026(19) 0.0079(2) 0.0500(8) Uani 1 1 d D . . O2W O 0.9264(5) 0.6319(2) 0.5400(3) 0.0623(10) Uani 1 1 d D . . O3W O 0.3014(5) 0.7423(3) 0.9462(3) 0.0777(13) Uani 1 1 d D . . H1W H 0.933(6) 0.8101(18) 0.909(3) 0.060(16) Uiso 1 1 d D . . H2W H 0.861(7) 0.741(2) 0.891(4) 0.08(2) Uiso 1 1 d D . . H3W H 1.080(7) 0.8191(19) 0.561(3) 0.070(18) Uiso 1 1 d D . . H4W H 1.127(5) 0.7469(18) 0.585(3) 0.040(13) Uiso 1 1 d D . . H5W H 0.770(6) 0.678(3) 0.714(3) 0.07(2) Uiso 1 1 d D . . H6W H 0.862(7) 0.668(3) 0.638(4) 0.10(2) Uiso 1 1 d D . . H7W H 1.196(8) 0.707(4) 0.838(2) 0.10(2) Uiso 1 1 d D . . H8W H 1.212(6) 0.672(3) 0.743(3) 0.069(18) Uiso 1 1 d D . . H9W H 1.034(3) 0.635(5) 0.550(7) 0.16(4) Uiso 1 1 d D . . H10W H 0.893(7) 0.5930(18) 0.528(5) 0.08(2) Uiso 1 1 d D . . H11W H 0.317(8) 0.7807(16) 0.967(5) 0.08(2) Uiso 1 1 d D . . H12W H 0.334(12) 0.699(2) 0.969(6) 0.16(4) Uiso 1 1 d D . . H13W H 0.751(5) 0.023(2) 0.0620(17) 0.032(11) Uiso 1 1 d D . . H14W H 0.803(5) 0.019(3) -0.031(3) 0.079(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0248(19) 0.050(2) 0.0434(19) 0.0024(18) 0.0035(16) 0.0032(17) C2 0.052(3) 0.058(3) 0.057(3) -0.007(2) 0.007(2) -0.001(2) C3 0.055(3) 0.055(3) 0.054(2) -0.002(2) 0.011(2) 0.005(2) C4 0.0265(19) 0.056(3) 0.045(2) 0.0034(19) 0.0060(16) 0.0074(18) C5 0.031(2) 0.050(2) 0.0399(19) -0.0012(17) 0.0044(16) 0.0023(18) C6 0.0279(19) 0.058(3) 0.0422(19) 0.0047(18) 0.0080(16) 0.0053(19) C7 0.060(3) 0.050(3) 0.063(3) 0.011(2) 0.022(2) 0.009(2) C8 0.038(2) 0.062(3) 0.043(2) 0.004(2) 0.0051(18) -0.005(2) C9 0.044(3) 0.078(4) 0.053(2) 0.022(2) 0.013(2) 0.016(3) C10 0.0228(19) 0.044(2) 0.0382(17) -0.0011(16) 0.0069(14) 0.0014(17) C11 0.022(2) 0.048(2) 0.0387(17) 0.0007(17) 0.0069(15) 0.0005(17) C12 0.033(2) 0.043(2) 0.043(2) -0.0017(17) 0.0090(17) 0.0055(18) C13 0.0264(19) 0.045(2) 0.044(2) 0.0037(18) 0.0091(16) 0.0026(17) C14 0.039(2) 0.044(2) 0.044(2) -0.0035(18) 0.0103(18) -0.004(2) C15 0.033(2) 0.043(2) 0.042(2) 0.0001(17) 0.0075(16) -0.0006(18) N1 0.036(2) 0.053(3) 0.0406(16) 0.0004(15) 0.0068(15) -0.0033(15) N2 0.0322(18) 0.048(2) 0.0477(18) 0.0017(15) 0.0040(15) 0.0021(16) Cr 0.0243(4) 0.0390(5) 0.0383(5) -0.0009(2) 0.0059(3) 0.0002(2) Mn 0.0271(4) 0.0405(5) 0.0402(5) -0.0005(2) 0.0072(3) 0.0001(2) O1 0.0256(13) 0.0426(16) 0.0440(14) -0.0028(12) 0.0018(11) 0.0007(12) O2 0.0246(13) 0.0422(16) 0.0464(15) -0.0002(12) 0.0008(11) -0.0010(12) O3 0.0270(14) 0.0404(16) 0.0554(16) -0.0002(13) 0.0007(12) 0.0035(13) O4 0.0270(14) 0.0429(16) 0.0434(14) -0.0012(12) 0.0036(11) -0.0031(13) O5 0.0358(17) 0.0534(19) 0.0452(16) -0.0040(14) 0.0114(13) -0.0086(15) O6 0.0403(18) 0.060(2) 0.0461(17) -0.0027(15) 0.0037(14) 0.0150(16) O7 0.0336(17) 0.0465(18) 0.0430(15) -0.0018(13) 0.0095(13) -0.0054(13) O8 0.057(2) 0.050(2) 0.0517(18) 0.0074(15) 0.0270(17) 0.0100(17) O10 0.0333(16) 0.0436(17) 0.0412(14) -0.0014(12) 0.0073(12) -0.0018(12) O11 0.0326(15) 0.0449(17) 0.0426(15) -0.0028(12) 0.0080(12) -0.0053(13) O12 0.0337(16) 0.0438(16) 0.0411(15) 0.0018(12) 0.0092(12) 0.0048(13) O13 0.0288(15) 0.0464(18) 0.0428(15) 0.0022(12) 0.0079(12) 0.0071(12) O14 0.062(2) 0.069(2) 0.0488(17) -0.0149(16) 0.0215(16) -0.0217(19) O15 0.0442(18) 0.057(2) 0.0483(16) -0.0034(14) 0.0054(14) -0.0146(15) O16 0.0492(19) 0.059(2) 0.0435(16) 0.0054(14) 0.0129(14) 0.0134(16) O17 0.0473(19) 0.061(2) 0.0509(16) 0.0087(15) 0.0109(14) 0.0164(16) O1W 0.0364(17) 0.066(2) 0.0477(16) 0.0003(15) 0.0056(14) -0.0038(15) O2W 0.054(2) 0.080(3) 0.0547(19) -0.0138(19) 0.0168(17) -0.017(2) O3W 0.066(3) 0.098(4) 0.065(2) -0.014(2) -0.012(2) 0.003(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 C1 N2 1.313(6) . ? C1 N1 1.327(6) . ? C1 C5 1.494(6) . ? C2 N2 1.471(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 N1 1.439(8) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C6 1.385(6) 3_656 ? C4 C5 1.403(6) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? C6 C4 1.385(6) 3_656 ? C6 H6 0.9300 . ? C7 N2 1.465(6) . ? C7 C9 1.498(8) . ? C7 H20A 0.9700 . ? C7 H20B 0.9700 . ? C8 N1 1.473(6) . ? C8 C9 1.484(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H21A 0.9700 . ? C9 H21B 0.9700 . ? C10 O4 1.233(5) . ? C10 O1 1.268(5) . ? C10 C11 1.553(6) . ? C11 O3 1.233(5) . ? C11 O2 1.267(5) . ? C12 O16 1.218(5) . ? C12 O13 1.283(5) . ? C12 C13 1.560(6) . ? C13 O17 1.215(5) . ? C13 O12 1.293(5) . ? C14 O14 1.218(6) . ? C14 O10 1.299(5) . ? C14 C15 1.540(6) . ? C15 O15 1.226(5) . ? C15 O11 1.289(5) . ? Cr O13 1.958(3) . ? Cr O12 1.972(3) . ? Cr O1 1.976(3) . ? Cr O11 1.981(3) . ? Cr O10 1.983(3) . ? Cr O2 1.989(3) . ? Mn O6 2.131(3) . ? Mn O7 2.147(3) . ? Mn O5 2.153(3) . ? Mn O8 2.167(3) . ? Mn O4 2.222(3) . ? Mn O3 2.239(3) . ? O5 H5W 0.83(2) . ? O5 H6W 0.98(2) . ? O6 H7W 0.81(2) . ? O6 H8W 0.95(2) . ? O7 H1W 0.96(2) . ? O7 H2W 0.82(2) . ? O8 H3W 0.96(2) . ? O8 H4W 0.84(2) . ? O1W H13W 0.83(2) . ? O1W H14W 0.97(2) . ? O2W H9W 0.97(2) . ? O2W H10W 0.82(2) . ? O3W H11W 0.81(2) . ? O3W H12W 0.95(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 N2 C1 N1 123.2(4) . . ? N2 C1 C5 119.3(4) . . ? N1 C1 C5 117.5(4) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 119.2(4) 3_656 . ? C6 C4 H4 120.4 3_656 . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 C1 119.6(4) . . ? C4 C5 C1 119.8(4) . . ? C5 C6 C4 120.2(4) . 3_656 ? C5 C6 H6 119.9 . . ? C4 C6 H6 119.9 3_656 . ? N2 C7 C9 110.7(5) . . ? N2 C7 H20A 109.5 . . ? C9 C7 H20A 109.5 . . ? N2 C7 H20B 109.5 . . ? C9 C7 H20B 109.5 . . ? H20A C7 H20B 108.1 . . ? N1 C8 C9 110.5(4) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C7 111.0(4) . . ? C8 C9 H21A 109.4 . . ? C7 C9 H21A 109.4 . . ? C8 C9 H21B 109.4 . . ? C7 C9 H21B 109.4 . . ? H21A C9 H21B 108.0 . . ? O4 C10 O1 126.6(4) . . ? O4 C10 C11 118.5(3) . . ? O1 C10 C11 114.9(3) . . ? O3 C11 O2 126.8(4) . . ? O3 C11 C10 118.3(3) . . ? O2 C11 C10 114.9(3) . . ? O16 C12 O13 126.1(4) . . ? O16 C12 C13 120.0(4) . . ? O13 C12 C13 113.9(3) . . ? O17 C13 O12 126.2(4) . . ? O17 C13 C12 120.0(4) . . ? O12 C13 C12 113.8(3) . . ? O14 C14 O10 124.6(4) . . ? O14 C14 C15 121.2(4) . . ? O10 C14 C15 114.2(4) . . ? O15 C15 O11 125.2(4) . . ? O15 C15 C14 120.9(4) . . ? O11 C15 C14 113.9(4) . . ? C1 N1 C3 124.2(4) . . ? C1 N1 C8 120.2(4) . . ? C3 N1 C8 115.5(4) . . ? C1 N2 C7 121.8(4) . . ? C1 N2 C2 123.1(4) . . ? C7 N2 C2 115.1(4) . . ? O13 Cr O12 82.90(12) . . ? O13 Cr O1 91.11(13) . . ? O12 Cr O1 92.63(13) . . ? O13 Cr O11 93.32(13) . . ? O12 Cr O11 93.63(14) . . ? O1 Cr O11 172.74(12) . . ? O13 Cr O10 173.48(14) . . ? O12 Cr O10 92.96(13) . . ? O1 Cr O10 94.12(13) . . ? O11 Cr O10 81.89(13) . . ? O13 Cr O2 92.01(12) . . ? O12 Cr O2 173.09(12) . . ? O1 Cr O2 82.77(13) . . ? O11 Cr O2 91.32(12) . . ? O10 Cr O2 92.52(13) . . ? O6 Mn O7 88.27(13) . . ? O6 Mn O5 97.09(15) . . ? O7 Mn O5 91.20(12) . . ? O6 Mn O8 93.19(14) . . ? O7 Mn O8 177.74(14) . . ? O5 Mn O8 90.33(14) . . ? O6 Mn O4 167.12(13) . . ? O7 Mn O4 90.37(12) . . ? O5 Mn O4 95.75(12) . . ? O8 Mn O4 87.82(12) . . ? O6 Mn O3 91.77(13) . . ? O7 Mn O3 88.03(12) . . ? O5 Mn O3 171.08(13) . . ? O8 Mn O3 90.20(14) . . ? O4 Mn O3 75.38(11) . . ? C10 O1 Cr 113.4(2) . . ? C11 O2 Cr 113.2(2) . . ? C11 O3 Mn 113.6(3) . . ? C10 O4 Mn 113.9(2) . . ? Mn O5 H5W 127(4) . . ? Mn O5 H6W 113(4) . . ? H5W O5 H6W 107(4) . . ? Mn O6 H7W 112(5) . . ? Mn O6 H8W 121(3) . . ? H7W O6 H8W 123(5) . . ? Mn O7 H1W 117(3) . . ? Mn O7 H2W 128(4) . . ? H1W O7 H2W 115(5) . . ? Mn O8 H3W 129(3) . . ? Mn O8 H4W 118(3) . . ? H3W O8 H4W 112(4) . . ? C14 O10 Cr 114.6(3) . . ? C15 O11 Cr 115.1(3) . . ? C13 O12 Cr 114.2(3) . . ? C12 O13 Cr 115.0(3) . . ? H13W O1W H14W 110(4) . . ? H9W O2W H10W 116(5) . . ? H11W O3W H12W 131(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.262 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.169