# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cms273 _database_code_depnum_ccdc_archive 'CCDC 888661' #TrackingRef 'crystal2_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H80 Fe3 N12 O40 S2' _chemical_formula_weight 1817.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7415(11) _cell_length_b 15.2796(9) _cell_length_c 15.5035(16) _cell_angle_alpha 112.633(9) _cell_angle_beta 92.380(7) _cell_angle_gamma 94.048(9) _cell_volume 1901.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 157 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 21.5 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 942 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.56080 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area-detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21959 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_unetI/netI 0.0717 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 20.25 _reflns_number_total 7400 _reflns_number_gt 5493 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material Platon _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. Because of the pour thermal parameters of the solvent molecules several restraints DFIX, DANG, OMIT, SADI, DELU, SIMU were employed Lines of res file: SADI 0.001 O1M C1M O12M C12M DELU O1M C1M DELU O12M C12M SIMU 0.01 0.02 1.7 O1M C1M SIMU 0.01 0.02 1.7 O12M C12M AFIX 6 O4W 5 0.225333 0.196029 0.902693 11.00000 0.07294 0.10067 = 0.08725 0.01246 -0.00350 -0.01005 H4WA 2 0.276882 0.150327 0.867835 11.00000 -1.50000 H4WB 2 0.288850 0.242145 0.941441 11.00000 -1.50000 AFIX 0 417_ALERT_2_A Short Inter D-H..H-D H1M .. H4WA .. 1.78 Ang. 417_ALERT_2_B Short Inter D-H..H-D H4WA .. H12M .. 1.91 Ang. 420_ALERT_2_B D-H Without Acceptor >O1M - >H1M ... ? 420_ALERT_2_B D-H Without Acceptor O4W - H4WA ... ? These alerts are generated because there is a large amount of disorder in the structure (MeOH over two positions 0.52 and 0.48). Short contacts between disordered fragments are to be expected. b) Many hydrogen atom thermal parameters were refined creating a varied range 306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) ....... O2W 306_ALERT_2_B Isolated Oxygen Atom (H-atoms Missing ?) ....... O3W The hydrogen atoms of the water molecules O2w and O3w were not located on a fourrier map, but were included in the molecular formula ; _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^)+(0.0395P)^2^+5.3893P] 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 7400 _refine_ls_number_parameters 539 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 C1M C 0.5069(13) 0.0048(10) 0.8758(10) 0.053(4) Uani 0.52 1 d PDU A 1 H1MA H 0.5953 0.0012 0.8403 0.080 Uiso 0.52 1 calc PR A 1 H1MB H 0.4716 -0.0578 0.8716 0.080 Uiso 0.52 1 calc PR A 1 H1MC H 0.5341 0.0455 0.9402 0.080 Uiso 0.52 1 calc PR A 1 O1M O 0.3779(9) 0.0457(7) 0.8363(5) 0.0281(19) Uani 0.52 1 d PDU A 1 H1M H 0.4151 0.0745 0.8060 0.042 Uiso 0.52 1 calc PR A 1 C12M C 0.560(3) 0.0390(18) 0.890(2) 0.174(11) Uani 0.48 1 d PDU B 2 H12A H 0.5381 -0.0217 0.8946 0.261 Uiso 0.48 1 calc PR B 2 H12B H 0.5625 0.0886 0.9519 0.261 Uiso 0.48 1 calc PR B 2 H12C H 0.6573 0.0410 0.8648 0.261 Uiso 0.48 1 calc PR B 2 O12M O 0.433(3) 0.0534(15) 0.8264(19) 0.177(11) Uani 0.48 1 d PDU B 2 H12M H 0.3506 0.0274 0.8319 0.266 Uiso 0.48 1 calc PR B 2 O4W O 0.2254(6) 0.1960(5) 0.9027(5) 0.0962(19) Uani 1 1 d G . . H4WA H 0.2772 0.1503 0.8682 0.144 Uiso 1 1 d G . . H4WB H 0.2887 0.2423 0.9414 0.144 Uiso 1 1 d G . . C1 C 0.1808(5) 0.1782(3) 1.1032(3) 0.0221(10) Uani 1 1 d . . . C2 C 0.0312(5) 0.2026(3) 1.0647(3) 0.0191(9) Uani 1 1 d . . . C3 C 0.2830(5) 0.4362(3) 1.0294(3) 0.0221(10) Uani 1 1 d . . . C4 C 0.1746(5) 0.5081(3) 1.0882(3) 0.0196(9) Uani 1 1 d . . . C5 C 0.1541(5) 0.4179(3) 1.3612(3) 0.0203(9) Uani 1 1 d . . . C6 C 0.3160(5) 0.4672(3) 1.3594(3) 0.0208(10) Uani 1 1 d . . . Fe1 Fe 0.19938(7) 0.37732(4) 1.17197(4) 0.01731(16) Uani 1 1 d . . . Fe2 Fe 0.0000 0.0000 1.0000 0.0267(2) Uani 1 2 d S . . O1 O 0.1984(4) 0.0932(2) 1.0823(2) 0.0299(8) Uani 1 1 d . . . O2 O -0.0666(3) 0.1356(2) 1.0158(2) 0.0233(7) Uani 1 1 d . . . O1W O 0.0989(4) -0.0175(2) 0.8743(2) 0.0385(9) Uani 1 1 d . . . O3 O 0.2736(3) 0.2495(2) 1.1553(2) 0.0213(7) Uani 1 1 d . . . O4 O 0.0203(3) 0.2900(2) 1.0874(2) 0.0205(7) Uani 1 1 d . . . O5 O 0.0787(3) 0.3794(2) 1.2810(2) 0.0220(7) Uani 1 1 d . . . O6 O 0.3600(3) 0.4495(2) 1.2770(2) 0.0212(7) Uani 1 1 d . . . O7 O 0.1102(4) 0.4177(2) 1.4354(2) 0.0291(8) Uani 1 1 d . . . O8 O 0.3893(4) 0.5184(2) 1.4338(2) 0.0280(7) Uani 1 1 d . . . O9 O 0.3195(3) 0.3773(2) 1.0663(2) 0.0240(7) Uani 1 1 d . . . O10 O 0.1264(3) 0.4908(2) 1.1579(2) 0.0221(7) Uani 1 1 d . . . O11 O 0.3249(4) 0.4379(2) 0.9570(2) 0.0346(8) Uani 1 1 d . . . O12 O 0.1444(4) 0.5738(2) 1.0666(2) 0.0294(8) Uani 1 1 d . . . C22 C 0.5877(5) 0.2549(4) 0.6936(3) 0.0311(12) Uani 1 1 d . . . C23 C 0.5215(6) 0.3147(4) 0.7837(4) 0.0460(16) Uani 1 1 d . . . H23A H 0.4593 0.2741 0.8055 0.069 Uiso 1 1 calc R . . H23B H 0.4593 0.3593 0.7728 0.069 Uiso 1 1 calc R . . H23C H 0.6037 0.3486 0.8302 0.069 Uiso 1 1 calc R . . C24 C 0.5589(6) 0.1566(4) 0.6576(3) 0.0342(12) Uani 1 1 d . . . H24 H 0.4959 0.1275 0.6877 0.041 Uiso 1 1 calc R . . C25 C 0.6785(6) 0.2973(3) 0.6477(3) 0.0341(12) Uani 1 1 d . . . H25 H 0.6987 0.3632 0.6726 0.041 Uiso 1 1 calc R . . C26 C 0.7410(6) 0.2438(3) 0.5647(3) 0.0282(11) Uani 1 1 d . . . H26 H 0.7997 0.2733 0.5330 0.034 Uiso 1 1 calc R . . C27 C 0.6245(5) 0.1017(3) 0.5764(3) 0.0286(11) Uani 1 1 d . . . H27 H 0.6083 0.0356 0.5533 0.034 Uiso 1 1 calc R . . C28 C 0.7137(5) 0.1452(3) 0.5302(3) 0.0192(9) Uani 1 1 d . . . O13 O 0.9233(4) 0.1280(3) 0.4125(3) 0.0426(10) Uani 1 1 d . . . O14 O 0.6628(4) 0.0639(3) 0.3511(2) 0.0468(11) Uani 1 1 d . . . O15 O 0.8089(5) -0.0140(3) 0.4290(3) 0.0466(10) Uani 1 1 d . . . S1 S 0.78482(13) 0.07534(8) 0.42270(8) 0.0224(3) Uani 1 1 d . . . C7 C 0.3019(5) 0.2734(3) 0.4885(3) 0.0163(9) Uani 1 1 d . . . C8 C 0.0128(5) 0.2252(3) 0.7374(3) 0.0181(9) Uani 1 1 d . . . C9 C 0.2690(4) 0.5473(3) 0.7914(3) 0.0181(9) Uani 1 1 d . . . C10 C 0.1391(5) 0.3856(3) 0.7600(3) 0.0186(9) Uani 1 1 d . . . H10 H 0.1048 0.4097 0.8200 0.022 Uiso 1 1 calc R . . C11 C 0.1042(4) 0.2892(3) 0.7030(3) 0.0155(9) Uani 1 1 d . . . C12 C 0.1577(5) 0.2536(3) 0.6140(3) 0.0185(9) Uani 1 1 d . . . H12 H 0.1369 0.1893 0.5759 0.022 Uiso 1 1 calc R . . C13 C 0.2425(5) 0.3141(3) 0.5818(3) 0.0182(9) Uani 1 1 d . . . C14 C 0.2775(5) 0.4108(3) 0.6383(3) 0.0179(9) Uani 1 1 d . . . H14 H 0.3347 0.4506 0.6164 0.021 Uiso 1 1 calc R . . C15 C 0.2252(5) 0.4464(3) 0.7276(3) 0.0176(9) Uani 1 1 d . . . C16 C 0.3323(5) 0.6783(3) 0.9277(3) 0.0233(10) Uani 1 1 d . . . H16A H 0.4315 0.6933 0.9630 0.028 Uiso 1 1 calc R . . H16B H 0.2549 0.7092 0.9691 0.028 Uiso 1 1 calc R . . C17 C 0.3367(5) 0.7080(3) 0.8437(3) 0.0246(10) Uani 1 1 d . . . H17A H 0.2656 0.7554 0.8486 0.030 Uiso 1 1 calc R . . H17B H 0.4394 0.7332 0.8385 0.030 Uiso 1 1 calc R . . C18 C 0.3264(5) 0.1676(3) 0.3383(3) 0.0255(10) Uani 1 1 d . . . H18A H 0.2616 0.1628 0.2840 0.031 Uiso 1 1 calc R . . H18B H 0.3709 0.1077 0.3249 0.031 Uiso 1 1 calc R . . C19 C 0.4539(5) 0.2522(3) 0.3657(3) 0.0203(9) Uani 1 1 d . . . H19A H 0.5559 0.2304 0.3628 0.024 Uiso 1 1 calc R . . H19B H 0.4441 0.2873 0.3256 0.024 Uiso 1 1 calc R . . C20 C -0.0959(6) 0.0873(3) 0.7458(3) 0.0296(11) Uani 1 1 d . . . H20A H -0.0397 0.0481 0.7700 0.036 Uiso 1 1 calc R . . H20B H -0.1828 0.0487 0.7045 0.036 Uiso 1 1 calc R . . C21 C -0.1480(5) 0.1733(3) 0.8253(3) 0.0254(10) Uani 1 1 d . . . H21A H -0.2589 0.1738 0.8212 0.030 Uiso 1 1 calc R . . H21B H -0.1143 0.1742 0.8861 0.030 Uiso 1 1 calc R . . N1 N 0.2894(4) 0.6178(2) 0.7633(3) 0.0210(8) Uani 1 1 d . . . H1 H 0.2769 0.6122 0.7060 0.025 Uiso 1 1 calc R . . N2 N 0.2924(4) 0.5747(3) 0.8821(2) 0.0228(8) Uani 1 1 d . . . H2 H 0.2855 0.5371 0.9114 0.027 Uiso 1 1 calc R . . N3 N 0.0043(4) 0.1317(2) 0.6973(3) 0.0240(8) Uani 1 1 d . . . H3 H 0.0514 0.1005 0.6488 0.029 Uiso 1 1 calc R . . N4 N -0.0706(4) 0.2541(3) 0.8087(3) 0.0208(8) Uani 1 1 d . . . H4 H -0.0798 0.3130 0.8422 0.025 Uiso 1 1 calc R . . N5 N 0.4224(4) 0.3104(2) 0.4629(2) 0.0196(8) Uani 1 1 d . . . H5 H 0.4763 0.3621 0.4982 0.024 Uiso 1 1 calc R . . N6 N 0.2404(2) 0.19252(14) 0.42136(13) 0.0228(8) Uani 1 1 d . . . H6 H 0.1603 0.1593 0.4265 0.027 Uiso 1 1 calc R . . O2W O 0.7862(2) 0.38407(14) 0.41377(13) 0.0280(7) Uani 1 1 d R . . O3W O 0.0639(2) -0.19318(14) 0.73797(13) 0.0408(9) Uani 1 1 d 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 C1M 0.034(6) 0.067(10) 0.045(7) 0.007(7) -0.001(5) 0.013(6) O1M 0.028(3) 0.040(5) 0.008(3) 0.002(3) -0.003(3) -0.012(3) C12M 0.34(3) 0.076(14) 0.15(2) 0.085(14) 0.05(2) 0.075(17) O12M 0.32(3) 0.077(13) 0.151(18) 0.044(11) 0.032(19) 0.108(16) O4W 0.073(4) 0.102(5) 0.088(5) 0.013(4) -0.003(3) -0.010(3) C1 0.024(2) 0.021(2) 0.020(2) 0.0064(19) -0.0003(19) 0.0027(18) C2 0.022(2) 0.021(2) 0.015(2) 0.0084(18) -0.0001(18) 0.0040(17) C3 0.019(2) 0.022(2) 0.022(2) 0.0052(19) 0.0015(19) 0.0036(17) C4 0.019(2) 0.019(2) 0.017(2) 0.0022(18) -0.0010(18) 0.0030(17) C5 0.021(2) 0.017(2) 0.021(2) 0.0044(18) 0.0008(19) 0.0062(17) C6 0.021(2) 0.016(2) 0.024(2) 0.0066(18) -0.0021(19) 0.0037(17) Fe1 0.0163(3) 0.0162(3) 0.0177(3) 0.0044(2) 0.0015(2) 0.0027(2) Fe2 0.0359(6) 0.0172(5) 0.0231(5) 0.0050(4) -0.0056(4) -0.0022(4) O1 0.0311(18) 0.0190(17) 0.036(2) 0.0077(14) -0.0085(15) 0.0043(13) O2 0.0243(17) 0.0207(16) 0.0221(16) 0.0065(13) -0.0065(13) -0.0008(12) O1W 0.049(2) 0.037(2) 0.030(2) 0.0137(16) 0.0020(17) -0.0020(16) O3 0.0187(16) 0.0169(15) 0.0261(17) 0.0065(13) -0.0045(13) 0.0017(12) O4 0.0216(16) 0.0186(16) 0.0194(16) 0.0054(12) -0.0036(13) 0.0044(12) O5 0.0182(15) 0.0263(17) 0.0172(15) 0.0041(13) 0.0031(12) -0.0008(12) O6 0.0174(15) 0.0215(16) 0.0212(16) 0.0052(13) -0.0003(13) -0.0006(12) O7 0.0281(18) 0.039(2) 0.0188(17) 0.0097(15) 0.0046(14) -0.0002(14) O8 0.0277(18) 0.0272(17) 0.0233(17) 0.0060(14) -0.0049(14) -0.0080(13) O9 0.0241(17) 0.0268(17) 0.0262(17) 0.0139(14) 0.0085(13) 0.0118(13) O10 0.0239(16) 0.0206(16) 0.0208(16) 0.0055(13) 0.0045(13) 0.0077(12) O11 0.045(2) 0.040(2) 0.0266(19) 0.0181(16) 0.0165(16) 0.0189(16) O12 0.041(2) 0.0232(17) 0.0271(18) 0.0114(14) 0.0057(15) 0.0129(14) C22 0.016(2) 0.045(3) 0.026(3) 0.006(2) -0.001(2) 0.009(2) C23 0.034(3) 0.069(4) 0.025(3) 0.005(3) 0.004(2) 0.021(3) C24 0.025(3) 0.046(3) 0.026(3) 0.010(2) 0.002(2) -0.008(2) C25 0.049(3) 0.022(2) 0.027(3) 0.004(2) -0.001(2) 0.016(2) C26 0.036(3) 0.024(2) 0.026(3) 0.012(2) -0.001(2) 0.005(2) C27 0.025(2) 0.028(3) 0.027(3) 0.006(2) 0.000(2) -0.0064(19) C28 0.015(2) 0.022(2) 0.018(2) 0.0040(18) 0.0007(17) 0.0056(16) O13 0.032(2) 0.046(2) 0.040(2) 0.0074(18) 0.0143(17) -0.0098(16) O14 0.043(2) 0.060(3) 0.0250(19) 0.0017(18) -0.0037(17) 0.0185(19) O15 0.065(3) 0.030(2) 0.055(3) 0.0199(18) 0.037(2) 0.0258(18) S1 0.0225(6) 0.0206(6) 0.0218(6) 0.0052(4) 0.0044(5) 0.0029(4) C7 0.016(2) 0.016(2) 0.015(2) 0.0032(17) 0.0002(17) 0.0022(16) C8 0.017(2) 0.020(2) 0.017(2) 0.0068(17) -0.0011(17) 0.0052(17) C9 0.011(2) 0.021(2) 0.021(2) 0.0064(18) 0.0055(17) 0.0033(16) C10 0.016(2) 0.020(2) 0.017(2) 0.0036(17) 0.0013(17) 0.0044(16) C11 0.0103(19) 0.020(2) 0.017(2) 0.0070(17) 0.0011(16) 0.0037(15) C12 0.017(2) 0.020(2) 0.016(2) 0.0032(17) 0.0005(17) 0.0041(16) C13 0.017(2) 0.022(2) 0.015(2) 0.0061(17) 0.0023(17) 0.0042(17) C14 0.017(2) 0.019(2) 0.017(2) 0.0059(17) 0.0015(17) -0.0001(16) C15 0.015(2) 0.018(2) 0.016(2) 0.0028(17) -0.0013(17) 0.0044(16) C16 0.024(2) 0.021(2) 0.019(2) 0.0005(18) 0.0015(19) 0.0059(18) C17 0.020(2) 0.017(2) 0.030(3) 0.0017(19) 0.0035(19) 0.0009(17) C18 0.028(3) 0.022(2) 0.018(2) -0.0015(18) 0.0088(19) -0.0024(18) C19 0.022(2) 0.022(2) 0.016(2) 0.0065(18) 0.0081(18) 0.0035(17) C20 0.038(3) 0.025(2) 0.033(3) 0.016(2) 0.011(2) 0.010(2) C21 0.029(3) 0.029(2) 0.026(2) 0.019(2) 0.009(2) 0.0032(19) N1 0.023(2) 0.0201(19) 0.0166(18) 0.0031(15) 0.0010(15) 0.0022(15) N2 0.030(2) 0.0193(19) 0.0163(19) 0.0041(15) 0.0023(16) 0.0036(15) N3 0.031(2) 0.0182(19) 0.024(2) 0.0089(16) 0.0094(17) 0.0052(15) N4 0.026(2) 0.0185(18) 0.0208(19) 0.0094(15) 0.0087(16) 0.0064(15) N5 0.0179(19) 0.0214(19) 0.0144(18) 0.0024(15) 0.0009(15) -0.0040(14) N6 0.025(2) 0.0187(19) 0.0181(19) 0.0005(15) 0.0062(16) -0.0051(15) O2W 0.0296(18) 0.0299(18) 0.0212(17) 0.0078(14) 0.0016(14) -0.0053(14) O3W 0.056(2) 0.036(2) 0.0261(19) 0.0076(16) 0.0081(17) -0.0025(17) _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 C1M O1M 1.5406(15) . ? C1M H1MA 0.9600 . ? C1M H1MB 0.9600 . ? C1M H1MC 0.9600 . ? O1M H1M 0.8200 . ? C12M O12M 1.5405(10) . ? C12M H12A 0.9600 . ? C12M H12B 0.9600 . ? C12M H12C 0.9600 . ? O12M H12M 0.8200 . ? O4W H4WA 0.8700 . ? O4W H4WB 0.8700 . ? C1 O1 1.235(5) . ? C1 O3 1.281(5) . ? C1 C2 1.543(6) . ? C2 O4 1.255(5) . ? C2 O2 1.256(5) . ? C3 O11 1.204(6) . ? C3 O9 1.289(5) . ? C3 C4 1.544(6) . ? C4 O12 1.216(5) . ? C4 O10 1.288(5) . ? C5 O7 1.228(5) . ? C5 O5 1.281(5) . ? C5 C6 1.563(6) . ? C6 O8 1.235(5) . ? C6 O6 1.281(5) . ? Fe1 O10 1.973(3) . ? Fe1 O9 1.982(3) . ? Fe1 O6 2.012(3) . ? Fe1 O5 2.020(3) . ? Fe1 O3 2.027(3) . ? Fe1 O4 2.034(3) . ? Fe2 O1W 2.095(4) . ? Fe2 O1W 2.095(4) 2_557 ? Fe2 O2 2.117(3) 2_557 ? Fe2 O2 2.117(3) . ? Fe2 O1 2.175(3) . ? Fe2 O1 2.175(3) 2_557 ? C22 C25 1.373(8) . ? C22 C24 1.386(7) . ? C22 C23 1.511(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.390(7) . ? C24 H24 0.9300 . ? C25 C26 1.390(7) . ? C25 H25 0.9300 . ? C26 C28 1.390(6) . ? C26 H26 0.9300 . ? C27 C28 1.379(7) . ? C27 H27 0.9300 . ? C28 S1 1.765(4) . ? O13 S1 1.454(4) . ? O14 S1 1.458(4) . ? O15 S1 1.434(4) . ? C7 N5 1.308(6) . ? C7 N6 1.330(4) . ? C7 C13 1.471(6) . ? C8 N4 1.298(6) . ? C8 N3 1.317(5) . ? C8 C11 1.484(6) . ? C9 N2 1.307(5) . ? C9 N1 1.312(6) . ? C9 C15 1.488(6) . ? C10 C11 1.399(6) . ? C10 C15 1.405(6) . ? C10 H10 0.9300 . ? C11 C12 1.389(6) . ? C12 C13 1.394(6) . ? C12 H12 0.9300 . ? C13 C14 1.401(6) . ? C14 C15 1.390(6) . ? C14 H14 0.9300 . ? C16 N2 1.473(5) . ? C16 C17 1.536(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.476(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.454(5) . ? C18 C19 1.559(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.474(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.468(6) . ? C20 C21 1.529(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.480(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? 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 O12M C12M H12A 109.5 . . ? O12M C12M H12B 109.5 . . ? H12A C12M H12B 109.5 . . ? O12M C12M H12C 109.5 . . ? H12A C12M H12C 109.5 . . ? H12B C12M H12C 109.5 . . ? C12M O12M H12M 109.5 . . ? H4WA O4W H4WB 109.5 . . ? O1 C1 O3 126.6(4) . . ? O1 C1 C2 117.5(4) . . ? O3 C1 C2 115.8(4) . . ? O4 C2 O2 126.7(4) . . ? O4 C2 C1 114.7(4) . . ? O2 C2 C1 118.6(4) . . ? O11 C3 O9 126.1(4) . . ? O11 C3 C4 121.2(4) . . ? O9 C3 C4 112.7(4) . . ? O12 C4 O10 126.8(4) . . ? O12 C4 C3 119.3(4) . . ? O10 C4 C3 113.8(4) . . ? O7 C5 O5 125.8(4) . . ? O7 C5 C6 120.0(4) . . ? O5 C5 C6 114.2(4) . . ? O8 C6 O6 125.9(4) . . ? O8 C6 C5 119.8(4) . . ? O6 C6 C5 114.4(4) . . ? O10 Fe1 O9 80.92(12) . . ? O10 Fe1 O6 95.77(12) . . ? O9 Fe1 O6 98.01(13) . . ? O10 Fe1 O5 98.64(13) . . ? O9 Fe1 O5 179.08(13) . . ? O6 Fe1 O5 81.22(12) . . ? O10 Fe1 O3 167.42(13) . . ? O9 Fe1 O3 88.96(13) . . ? O6 Fe1 O3 93.01(12) . . ? O5 Fe1 O3 91.58(13) . . ? O10 Fe1 O4 92.65(12) . . ? O9 Fe1 O4 94.09(13) . . ? O6 Fe1 O4 166.21(13) . . ? O5 Fe1 O4 86.73(12) . . ? O3 Fe1 O4 80.57(11) . . ? O1W Fe2 O1W 180.000(1) . 2_557 ? O1W Fe2 O2 88.10(13) . 2_557 ? O1W Fe2 O2 91.90(13) 2_557 2_557 ? O1W Fe2 O2 91.90(13) . . ? O1W Fe2 O2 88.10(13) 2_557 . ? O2 Fe2 O2 180.000(1) 2_557 . ? O1W Fe2 O1 91.61(14) . . ? O1W Fe2 O1 88.39(14) 2_557 . ? O2 Fe2 O1 101.52(11) 2_557 . ? O2 Fe2 O1 78.48(11) . . ? O1W Fe2 O1 88.39(14) . 2_557 ? O1W Fe2 O1 91.61(14) 2_557 2_557 ? O2 Fe2 O1 78.48(11) 2_557 2_557 ? O2 Fe2 O1 101.52(11) . 2_557 ? O1 Fe2 O1 180.000(1) . 2_557 ? C1 O1 Fe2 112.4(3) . . ? C2 O2 Fe2 112.9(3) . . ? C1 O3 Fe1 113.7(3) . . ? C2 O4 Fe1 115.2(2) . . ? C5 O5 Fe1 114.6(3) . . ? C6 O6 Fe1 114.8(3) . . ? C3 O9 Fe1 115.7(3) . . ? C4 O10 Fe1 115.8(3) . . ? C25 C22 C24 119.7(5) . . ? C25 C22 C23 120.4(5) . . ? C24 C22 C23 120.0(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 C27 119.7(5) . . ? C22 C24 H24 120.1 . . ? C27 C24 H24 120.1 . . ? C22 C25 C26 121.5(5) . . ? C22 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C28 118.3(5) . . ? C25 C26 H26 120.8 . . ? C28 C26 H26 120.8 . . ? C28 C27 C24 120.0(4) . . ? C28 C27 H27 120.0 . . ? C24 C27 H27 120.0 . . ? C27 C28 C26 120.7(4) . . ? C27 C28 S1 119.7(3) . . ? C26 C28 S1 119.5(4) . . ? O15 S1 O13 114.7(2) . . ? O15 S1 O14 111.2(3) . . ? O13 S1 O14 112.1(3) . . ? O15 S1 C28 105.5(2) . . ? O13 S1 C28 107.1(2) . . ? O14 S1 C28 105.5(2) . . ? N5 C7 N6 112.4(3) . . ? N5 C7 C13 124.4(4) . . ? N6 C7 C13 123.1(4) . . ? N4 C8 N3 111.9(4) . . ? N4 C8 C11 124.6(4) . . ? N3 C8 C11 123.5(4) . . ? N2 C9 N1 112.9(4) . . ? N2 C9 C15 122.9(4) . . ? N1 C9 C15 124.3(4) . . ? C11 C10 C15 120.7(4) . . ? C11 C10 H10 119.6 . . ? C15 C10 H10 119.6 . . ? C12 C11 C10 119.2(4) . . ? C12 C11 C8 120.3(4) . . ? C10 C11 C8 120.6(4) . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 121.1(4) . . ? C12 C13 C7 118.6(4) . . ? C14 C13 C7 120.2(4) . . ? C15 C14 C13 118.9(4) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C10 120.0(4) . . ? C14 C15 C9 120.0(4) . . ? C10 C15 C9 119.8(4) . . ? N2 C16 C17 102.4(3) . . ? N2 C16 H16A 111.3 . . ? C17 C16 H16A 111.3 . . ? N2 C16 H16B 111.3 . . ? C17 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? N1 C17 C16 102.9(3) . . ? N1 C17 H17A 111.2 . . ? C16 C17 H17A 111.2 . . ? N1 C17 H17B 111.2 . . ? C16 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? N6 C18 C19 103.0(3) . . ? N6 C18 H18A 111.2 . . ? C19 C18 H18A 111.2 . . ? N6 C18 H18B 111.2 . . ? C19 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? N5 C19 C18 102.0(3) . . ? N5 C19 H19A 111.4 . . ? C18 C19 H19A 111.4 . . ? N5 C19 H19B 111.4 . . ? C18 C19 H19B 111.4 . . ? H19A C19 H19B 109.2 . . ? N3 C20 C21 102.8(4) . . ? N3 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? N3 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? N4 C21 C20 102.2(4) . . ? N4 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? N4 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C9 N1 C17 110.6(4) . . ? C9 N1 H1 124.7 . . ? C17 N1 H1 124.7 . . ? C9 N2 C16 111.2(4) . . ? C9 N2 H2 124.4 . . ? C16 N2 H2 124.4 . . ? C8 N3 C20 111.4(4) . . ? C8 N3 H3 124.3 . . ? C20 N3 H3 124.3 . . ? C8 N4 C21 111.7(4) . . ? C8 N4 H4 124.1 . . ? C21 N4 H4 124.1 . . ? C7 N5 C19 111.4(3) . . ? C7 N5 H5 124.3 . . ? C19 N5 H5 124.3 . . ? C7 N6 C18 111.1(3) . . ? C7 N6 H6 124.4 . . ? C18 N6 H6 124.4 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.25 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.058 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.094 data_cms277 _database_code_depnum_ccdc_archive 'CCDC 888662' #TrackingRef 'crystal3_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H80 Co Fe2 N12 O40 S2' _chemical_formula_weight 1820.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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' Co Co 0.3050 0.6296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.2886 0.5448 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0826 0.0763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8522(9) _cell_length_b 15.2760(8) _cell_length_c 15.5174(12) _cell_angle_alpha 112.9760(10) _cell_angle_beta 92.716(7) _cell_angle_gamma 94.762(8) _cell_volume 1917.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 173 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 21.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 943 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.56080 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type area-detector _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16113 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0851 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 20.00 _reflns_number_total 7115 _reflns_number_gt 4600 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'Denzo and Scalepak' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material Platon _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. Because of the pour thermal parameters of the solvent molecules several restraints DFIX, DANG, OMIT, SADI, DELU, SIMU were employed Lines of res file: SADI 0.001 O1M C1M O12M C12M DELU O1M C1M DELU O12M C12M SIMU 0.01 0.02 1.7 O1M C1M SIMU 0.01 0.02 1.7 O12M C12M AFIX 6 O4W 6 0.247401 0.176537 0.897770 11.00000 0.17827 0.14903 = 0.20001 0.04803 0.03847 -0.01893 H4WA 2 0.309970 0.143075 0.858912 11.00000 -1.50000 H4WB 2 0.280304 0.236434 0.916990 11.00000 -1.50000 AFIX 0 The hydrogen atoms of the water molecules were located on a fourrier map and refined with restraints DFIX and DANG (O-H = 0.82A and H-H = 1.54A) 417_ALERT_2_B Short Inter D-H..H-D H1M .. H4WA .. 1.80 Ang. 420_ALERT_2_B D-H Without Acceptor O4W - H4WA ... ? These alerts are generated because there is a large amount of disorder in the structure (MeOH over two positions 0.52 and 0.48) ; _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^+3.2517P] 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 7115 _refine_ls_number_parameters 569 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1334 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.181 _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 C1M C 0.492(3) -0.002(2) 0.877(2) 0.176(11) Uani 0.52 1 d PDU A 1 H1MA H 0.5814 -0.0100 0.8436 0.263 Uiso 0.52 1 calc PR A 1 H1MB H 0.4452 -0.0632 0.8712 0.263 Uiso 0.52 1 calc PR A 1 H1MC H 0.5189 0.0377 0.9422 0.263 Uiso 0.52 1 calc PR A 1 O1M O 0.379(2) 0.0460(16) 0.8357(14) 0.149(7) Uani 0.52 1 d PDU A 1 H1M H 0.4061 0.0452 0.7857 0.223 Uiso 0.52 1 calc PR A 1 C12M C 0.565(3) 0.040(2) 0.8882(19) 0.138(8) Uani 0.48 1 d PDU B 2 H12A H 0.5349 -0.0252 0.8800 0.207 Uiso 0.48 1 calc PR B 2 H12B H 0.5407 0.0824 0.9489 0.207 Uiso 0.48 1 calc PR B 2 H12C H 0.6723 0.0482 0.8836 0.207 Uiso 0.48 1 calc PR B 2 O12M O 0.479(2) 0.0612(12) 0.8113(12) 0.110(5) Uani 0.48 1 d PDU B 2 H12M H 0.4664 0.1181 0.8316 0.165 Uiso 0.48 1 calc PR B 2 O4W O 0.2474(13) 0.1765(8) 0.8978(9) 0.184(4) Uani 1 1 d G . . H4WA H 0.3100 0.1431 0.8589 0.276 Uiso 1 1 d G . . H4WB H 0.2803 0.2364 0.9170 0.276 Uiso 1 1 d G . . C1 C 0.1743(6) 0.1760(4) 0.1046(4) 0.0379(13) Uani 1 1 d . . . C2 C 0.0298(6) 0.1992(4) 0.0635(4) 0.0371(13) Uani 1 1 d . . . C3 C 0.2807(6) 0.4315(4) 0.0281(4) 0.0401(14) Uani 1 1 d . . . C4 C 0.1740(6) 0.5046(4) 0.0861(4) 0.0389(13) Uani 1 1 d . . . C5 C 0.1521(6) 0.4198(4) 0.3601(4) 0.0408(14) Uani 1 1 d . . . C6 C 0.3133(6) 0.4665(4) 0.3571(4) 0.0400(13) Uani 1 1 d . . . Fe Fe 0.19490(9) 0.37548(5) 0.17066(6) 0.0356(2) Uani 1 1 d . . . Co Co 0.0000 0.0000 0.0000 0.0490(3) Uani 1 2 d S . . O1 O 0.1885(5) 0.0905(3) 0.0859(3) 0.0525(11) Uani 1 1 d . . . O2 O -0.0665(4) 0.1324(3) 0.0138(3) 0.0477(10) Uani 1 1 d . . . O1W O -0.1028(7) 0.0127(4) 0.1192(4) 0.0784(15) Uani 1 1 d D . . O3 O 0.2661(4) 0.2466(3) 0.1564(3) 0.0414(9) Uani 1 1 d . . . O4 O 0.0173(4) 0.2870(3) 0.0856(3) 0.0402(9) Uani 1 1 d . . . O5 O 0.0762(4) 0.3817(3) 0.2792(3) 0.0455(10) Uani 1 1 d . . . O6 O 0.3547(4) 0.4477(3) 0.2752(3) 0.0407(9) Uani 1 1 d . . . O7 O 0.1091(5) 0.4203(3) 0.4330(3) 0.0608(12) Uani 1 1 d . . . O8 O 0.3865(5) 0.5175(3) 0.4316(3) 0.0544(11) Uani 1 1 d . . . O9 O 0.3110(4) 0.3714(3) 0.0638(3) 0.0444(10) Uani 1 1 d . . . O10 O 0.1246(4) 0.4885(3) 0.1550(3) 0.0434(10) Uani 1 1 d . . . O11 O 0.3238(6) 0.4326(3) -0.0439(3) 0.0639(13) Uani 1 1 d . . . O12 O 0.1477(5) 0.5709(3) 0.0648(3) 0.0542(11) Uani 1 1 d . . . H1W H -0.191(5) -0.020(5) 0.115(6) 0.11(3) Uiso 1 1 d D . . H2W H -0.086(11) 0.070(3) 0.154(7) 0.20(6) Uiso 1 1 d D . . C22 C 0.5958(7) 0.2547(5) 0.6865(5) 0.0578(18) Uani 1 1 d . . . C23 C 0.5279(9) 0.3137(6) 0.7766(5) 0.091(3) Uani 1 1 d . . . H23A H 0.4664 0.2719 0.7971 0.136 Uiso 1 1 calc R . . H23B H 0.4661 0.3575 0.7652 0.136 Uiso 1 1 calc R . . H23C H 0.6084 0.3489 0.8244 0.136 Uiso 1 1 calc R . . C24 C 0.5656(8) 0.1566(6) 0.6480(5) 0.074(2) Uani 1 1 d . . . H24 H 0.4999 0.1269 0.6758 0.088 Uiso 1 1 calc R . . C25 C 0.6895(9) 0.2966(5) 0.6437(5) 0.066(2) Uani 1 1 d . . . H25 H 0.7128 0.3627 0.6701 0.079 Uiso 1 1 calc R . . C26 C 0.7506(8) 0.2437(4) 0.5625(5) 0.0552(17) Uani 1 1 d . . . H26 H 0.8116 0.2743 0.5331 0.066 Uiso 1 1 calc R . . C27 C 0.6315(7) 0.1018(5) 0.5686(5) 0.064(2) Uani 1 1 d . . . H27 H 0.6146 0.0354 0.5452 0.076 Uiso 1 1 calc R . . C28 C 0.7220(6) 0.1455(4) 0.5242(4) 0.0435(14) Uani 1 1 d . . . O13 O 0.9436(6) 0.1183(4) 0.4187(4) 0.111(2) Uani 1 1 d . . . O14 O 0.6952(8) 0.0754(5) 0.3451(4) 0.129(3) Uani 1 1 d . . . O15 O 0.7962(7) -0.0187(4) 0.4166(5) 0.111(2) Uani 1 1 d . . . S1 S 0.79718(18) 0.07525(11) 0.41897(12) 0.0509(4) Uani 1 1 d . . . C7 C 0.3025(6) 0.2743(4) 0.4913(4) 0.0339(12) Uani 1 1 d . . . C8 C 0.0155(6) 0.2274(4) 0.7377(4) 0.0335(12) Uani 1 1 d . . . C9 C 0.2724(6) 0.5485(4) 0.7947(4) 0.0336(12) Uani 1 1 d . . . C10 C 0.1404(6) 0.3880(4) 0.7621(4) 0.0329(12) Uani 1 1 d . . . H10 H 0.1043 0.4127 0.8213 0.039 Uiso 1 1 calc R . . C11 C 0.1065(6) 0.2913(4) 0.7046(4) 0.0326(12) Uani 1 1 d . . . C12 C 0.1583(6) 0.2552(4) 0.6164(4) 0.0321(12) Uani 1 1 d . . . H12 H 0.1354 0.1906 0.5779 0.039 Uiso 1 1 calc R . . C13 C 0.2451(6) 0.3152(4) 0.5846(4) 0.0324(12) Uani 1 1 d . . . C14 C 0.2791(6) 0.4115(4) 0.6416(4) 0.0355(12) Uani 1 1 d . . . H14 H 0.3357 0.4517 0.6201 0.043 Uiso 1 1 calc R . . C15 C 0.2286(6) 0.4479(4) 0.7309(4) 0.0322(12) Uani 1 1 d . . . C16 C 0.3381(7) 0.6795(4) 0.9324(4) 0.0424(14) Uani 1 1 d . . . H16A H 0.4360 0.6949 0.9688 0.051 Uiso 1 1 calc R . . H16B H 0.2614 0.7098 0.9733 0.051 Uiso 1 1 calc R . . C17 C 0.3440(7) 0.7096(4) 0.8494(4) 0.0460(15) Uani 1 1 d . . . H17A H 0.2756 0.7575 0.8546 0.055 Uiso 1 1 calc R . . H17B H 0.4463 0.7344 0.8448 0.055 Uiso 1 1 calc R . . C18 C 0.3277(7) 0.1698(4) 0.3416(4) 0.0517(16) Uani 1 1 d . . . H18A H 0.2638 0.1649 0.2870 0.062 Uiso 1 1 calc R . . H18B H 0.3708 0.1099 0.3279 0.062 Uiso 1 1 calc R . . C19 C 0.4509(7) 0.2528(4) 0.3700(4) 0.0439(14) Uani 1 1 d . . . H19A H 0.5512 0.2313 0.3679 0.053 Uiso 1 1 calc R . . H19B H 0.4426 0.2875 0.3296 0.053 Uiso 1 1 calc R . . C20 C -0.0931(8) 0.0907(4) 0.7459(5) 0.0552(17) Uani 1 1 d . . . H20A H -0.0379 0.0521 0.7707 0.066 Uiso 1 1 calc R . . H20B H -0.1797 0.0512 0.7043 0.066 Uiso 1 1 calc R . . C21 C -0.1430(7) 0.1770(4) 0.8247(4) 0.0467(15) Uani 1 1 d . . . H21A H -0.2525 0.1775 0.8194 0.056 Uiso 1 1 calc R . . H21B H -0.1111 0.1782 0.8859 0.056 Uiso 1 1 calc R . . N1 N 0.2939(5) 0.6193(3) 0.7685(3) 0.0395(11) Uani 1 1 d . . . H1 H 0.2807 0.6141 0.7114 0.047 Uiso 1 1 calc R . . N2 N 0.2977(5) 0.5759(3) 0.8858(3) 0.0437(12) Uani 1 1 d . . . H2 H 0.2914 0.5378 0.9145 0.052 Uiso 1 1 calc R . . N3 N 0.0054(5) 0.1343(3) 0.6976(3) 0.0445(12) Uani 1 1 d . . . H3 H 0.0508 0.1028 0.6490 0.053 Uiso 1 1 calc R . . N4 N -0.0646(5) 0.2571(3) 0.8096(3) 0.0401(11) Uani 1 1 d . . . H4 H -0.0707 0.3163 0.8438 0.048 Uiso 1 1 calc R . . N5 N 0.4210(5) 0.3118(3) 0.4662(3) 0.0382(11) Uani 1 1 d . . . H5 H 0.4748 0.3643 0.5016 0.046 Uiso 1 1 calc R . . N6 N 0.2424(5) 0.1941(3) 0.4244(3) 0.0431(12) Uani 1 1 d . . . H6 H 0.1629 0.1601 0.4287 0.052 Uiso 1 1 calc R . . O2W O -0.2146(6) 0.3858(3) 0.4098(3) 0.0575(12) Uani 1 1 d D . . O3W O -0.0715(8) 0.1919(4) 0.2590(4) 0.0884(18) Uani 1 1 d D . . H3W H -0.133(8) 0.171(5) 0.293(5) 0.12(3) Uiso 1 1 d D . . H4W H -0.032(11) 0.247(3) 0.274(6) 0.14(5) Uiso 1 1 d D . . H5W H -0.122(3) 0.388(4) 0.410(4) 0.07(2) Uiso 1 1 d D . . H6W H -0.258(6) 0.428(3) 0.457(3) 0.06(2) 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 C1M 0.13(2) 0.20(2) 0.17(2) 0.045(17) -0.010(16) 0.003(16) O1M 0.129(15) 0.169(17) 0.132(15) 0.051(12) 0.000(12) -0.015(12) C12M 0.140(18) 0.125(16) 0.171(19) 0.079(14) 0.015(15) 0.029(14) O12M 0.105(12) 0.090(10) 0.139(13) 0.051(9) 0.002(10) 0.010(9) O4W 0.178(9) 0.149(8) 0.200(12) 0.048(8) 0.038(8) -0.019(7) C1 0.043(3) 0.040(3) 0.031(3) 0.015(3) -0.001(3) 0.008(3) C2 0.041(3) 0.036(3) 0.033(3) 0.013(3) -0.002(3) 0.001(3) C3 0.046(3) 0.035(3) 0.034(3) 0.006(3) 0.007(3) 0.009(3) C4 0.041(3) 0.034(3) 0.036(3) 0.009(3) -0.006(3) 0.005(2) C5 0.040(3) 0.036(3) 0.038(4) 0.005(3) 0.005(3) 0.001(2) C6 0.041(3) 0.033(3) 0.044(4) 0.014(3) -0.003(3) 0.001(2) Fe 0.0352(4) 0.0338(4) 0.0341(5) 0.0097(4) 0.0021(4) 0.0034(3) Co 0.0607(8) 0.0337(6) 0.0466(8) 0.0131(6) -0.0119(6) -0.0045(5) O1 0.058(3) 0.034(2) 0.059(3) 0.015(2) -0.019(2) 0.0038(19) O2 0.048(2) 0.043(2) 0.047(3) 0.017(2) -0.016(2) -0.0030(19) O1W 0.096(4) 0.065(4) 0.068(4) 0.025(3) 0.012(3) -0.015(3) O3 0.038(2) 0.035(2) 0.047(3) 0.0152(19) -0.0109(19) 0.0022(17) O4 0.039(2) 0.035(2) 0.042(2) 0.0117(18) -0.0091(19) 0.0065(17) O5 0.038(2) 0.057(3) 0.033(2) 0.011(2) 0.0035(19) -0.0078(19) O6 0.035(2) 0.042(2) 0.038(2) 0.0106(19) 0.0008(18) -0.0037(16) O7 0.054(3) 0.083(3) 0.038(3) 0.019(2) 0.006(2) -0.009(2) O8 0.060(3) 0.055(3) 0.039(3) 0.015(2) -0.015(2) -0.019(2) O9 0.047(2) 0.046(2) 0.047(3) 0.021(2) 0.017(2) 0.0205(19) O10 0.050(2) 0.041(2) 0.039(2) 0.0124(19) 0.012(2) 0.0159(18) O11 0.091(4) 0.066(3) 0.050(3) 0.033(2) 0.034(3) 0.032(3) O12 0.073(3) 0.045(2) 0.049(3) 0.021(2) 0.007(2) 0.021(2) C22 0.038(4) 0.078(5) 0.046(4) 0.012(4) -0.007(3) 0.018(3) C23 0.063(5) 0.127(7) 0.060(5) 0.006(5) 0.002(4) 0.043(5) C24 0.056(4) 0.096(6) 0.057(5) 0.021(5) 0.011(4) -0.017(4) C25 0.095(6) 0.045(4) 0.051(5) 0.008(4) 0.002(4) 0.028(4) C26 0.071(4) 0.041(4) 0.056(4) 0.022(3) 0.001(4) 0.008(3) C27 0.058(4) 0.052(4) 0.061(5) 0.007(4) 0.010(4) -0.023(3) C28 0.037(3) 0.045(4) 0.043(4) 0.013(3) -0.004(3) 0.001(3) O13 0.077(4) 0.116(5) 0.083(4) -0.014(3) 0.042(3) -0.045(3) O14 0.139(6) 0.175(7) 0.048(4) 0.004(4) -0.011(4) 0.088(5) O15 0.145(5) 0.059(3) 0.146(6) 0.043(4) 0.096(5) 0.045(3) S1 0.0487(9) 0.0440(9) 0.0523(11) 0.0107(8) 0.0088(8) 0.0041(7) C7 0.033(3) 0.031(3) 0.034(3) 0.009(3) 0.004(2) 0.004(2) C8 0.033(3) 0.036(3) 0.035(3) 0.017(3) 0.004(3) 0.007(2) C9 0.028(3) 0.035(3) 0.033(3) 0.007(3) 0.008(2) 0.007(2) C10 0.032(3) 0.038(3) 0.027(3) 0.011(2) 0.004(2) 0.005(2) C11 0.026(3) 0.036(3) 0.037(3) 0.015(3) 0.002(2) 0.003(2) C12 0.033(3) 0.032(3) 0.026(3) 0.006(2) 0.004(2) 0.001(2) C13 0.034(3) 0.036(3) 0.027(3) 0.011(2) 0.005(2) 0.007(2) C14 0.034(3) 0.038(3) 0.037(3) 0.017(3) 0.004(3) 0.001(2) C15 0.033(3) 0.033(3) 0.030(3) 0.009(2) 0.005(2) 0.010(2) C16 0.041(3) 0.032(3) 0.038(3) -0.004(3) -0.001(3) 0.006(2) C17 0.044(3) 0.036(3) 0.049(4) 0.008(3) 0.007(3) 0.000(3) C18 0.057(4) 0.050(4) 0.037(4) 0.006(3) 0.013(3) -0.005(3) C19 0.047(3) 0.051(4) 0.029(3) 0.010(3) 0.012(3) 0.006(3) C20 0.070(4) 0.041(4) 0.063(5) 0.029(3) 0.017(4) 0.005(3) C21 0.056(4) 0.050(4) 0.044(4) 0.028(3) 0.014(3) 0.005(3) N1 0.046(3) 0.032(3) 0.036(3) 0.010(2) 0.005(2) 0.002(2) N2 0.057(3) 0.037(3) 0.031(3) 0.008(2) 0.003(2) 0.002(2) N3 0.058(3) 0.033(3) 0.041(3) 0.012(2) 0.016(3) 0.006(2) N4 0.050(3) 0.035(3) 0.038(3) 0.015(2) 0.015(2) 0.008(2) N5 0.036(3) 0.040(3) 0.029(3) 0.004(2) 0.004(2) -0.006(2) N6 0.045(3) 0.040(3) 0.033(3) 0.005(2) 0.012(2) -0.009(2) O2W 0.059(3) 0.061(3) 0.039(3) 0.008(2) 0.008(2) -0.008(2) O3W 0.127(5) 0.065(4) 0.062(4) 0.015(3) 0.022(4) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1M O1M 1.5410(16) . ? C1M H1MA 0.9600 . ? C1M H1MB 0.9600 . ? C1M H1MC 0.9600 . ? O1M H1M 0.8200 . ? C12M O12M 1.5407(11) . ? C12M H12A 0.9600 . ? C12M H12B 0.9600 . ? C12M H12C 0.9600 . ? O12M H12M 0.8200 . ? O4W H4WA 0.8773 . ? O4W H4WB 0.8634 . ? C1 O1 1.241(6) . ? C1 O3 1.260(6) . ? C1 C2 1.531(8) . ? C2 O2 1.242(6) . ? C2 O4 1.265(6) . ? C3 O11 1.205(6) . ? C3 O9 1.282(6) . ? C3 C4 1.555(7) . ? C4 O12 1.218(6) . ? C4 O10 1.276(6) . ? C5 O7 1.208(6) . ? C5 O5 1.285(7) . ? C5 C6 1.553(8) . ? C6 O8 1.226(7) . ? C6 O6 1.268(6) . ? Fe O9 1.976(4) . ? Fe O10 1.979(4) . ? Fe O6 1.994(4) . ? Fe O5 2.002(4) . ? Fe O4 2.024(4) . ? Fe O3 2.049(4) . ? Co O1W 2.048(5) . ? Co O1W 2.048(5) 2 ? Co O2 2.088(4) 2 ? Co O2 2.088(4) . ? Co O1 2.107(4) 2 ? Co O1 2.107(4) . ? O1W H1W 0.876(12) . ? O1W H2W 0.82(2) . ? C22 C25 1.354(9) . ? C22 C24 1.375(10) . ? C22 C23 1.522(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.380(9) . ? C24 H24 0.9300 . ? C25 C26 1.370(9) . ? C25 H25 0.9300 . ? C26 C28 1.377(8) . ? C26 H26 0.9300 . ? C27 C28 1.373(8) . ? C27 H27 0.9300 . ? C28 S1 1.764(6) . ? O13 S1 1.405(5) . ? O14 S1 1.426(6) . ? O15 S1 1.421(5) . ? C7 N5 1.301(6) . ? C7 N6 1.307(7) . ? C7 C13 1.470(7) . ? C8 N4 1.298(6) . ? C8 N3 1.304(6) . ? C8 C11 1.472(7) . ? C9 N1 1.298(6) . ? C9 N2 1.310(7) . ? C9 C15 1.473(7) . ? C10 C15 1.393(7) . ? C10 C11 1.393(7) . ? C10 H10 0.9300 . ? C11 C12 1.380(7) . ? C12 C13 1.395(7) . ? C12 H12 0.9300 . ? C13 C14 1.387(7) . ? C14 C15 1.388(7) . ? C14 H14 0.9300 . ? C16 N2 1.464(7) . ? C16 C17 1.528(8) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.473(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.458(6) . ? C18 C19 1.510(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.462(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.456(7) . ? C20 C21 1.523(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.460(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? O2W H5W 0.82(2) . ? O2W H6W 0.898(14) . ? O3W H3W 0.896(14) . ? O3W H4W 0.82(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 O12M C12M H12A 109.5 . . ? O12M C12M H12B 109.5 . . ? H12A C12M H12B 109.5 . . ? O12M C12M H12C 109.5 . . ? H12A C12M H12C 109.5 . . ? H12B C12M H12C 109.5 . . ? C12M O12M H12M 109.5 . . ? H4WA O4W H4WB 108.5 . . ? O1 C1 O3 126.3(5) . . ? O1 C1 C2 117.6(5) . . ? O3 C1 C2 116.0(5) . . ? O2 C2 O4 125.1(5) . . ? O2 C2 C1 118.9(5) . . ? O4 C2 C1 116.0(5) . . ? O11 C3 O9 125.8(5) . . ? O11 C3 C4 121.0(5) . . ? O9 C3 C4 113.1(5) . . ? O12 C4 O10 126.2(5) . . ? O12 C4 C3 119.7(5) . . ? O10 C4 C3 114.0(5) . . ? O7 C5 O5 126.0(5) . . ? O7 C5 C6 120.9(6) . . ? O5 C5 C6 113.1(5) . . ? O8 C6 O6 126.6(5) . . ? O8 C6 C5 118.6(5) . . ? O6 C6 C5 114.8(5) . . ? O9 Fe O10 81.48(15) . . ? O9 Fe O6 98.85(16) . . ? O10 Fe O6 96.38(16) . . ? O9 Fe O5 179.05(16) . . ? O10 Fe O5 97.58(16) . . ? O6 Fe O5 81.08(15) . . ? O9 Fe O4 92.89(16) . . ? O10 Fe O4 92.50(16) . . ? O6 Fe O4 166.20(15) . . ? O5 Fe O4 87.30(16) . . ? O9 Fe O3 88.72(15) . . ? O10 Fe O3 167.84(16) . . ? O6 Fe O3 92.22(15) . . ? O5 Fe O3 92.23(16) . . ? O4 Fe O3 80.75(14) . . ? O1W Co O1W 180.0(3) . 2 ? O1W Co O2 90.9(2) . 2 ? O1W Co O2 89.1(2) 2 2 ? O1W Co O2 89.1(2) . . ? O1W Co O2 90.9(2) 2 . ? O2 Co O2 180.0(3) 2 . ? O1W Co O1 91.4(2) . 2 ? O1W Co O1 88.6(2) 2 2 ? O2 Co O1 80.32(15) 2 2 ? O2 Co O1 99.68(15) . 2 ? O1W Co O1 88.6(2) . . ? O1W Co O1 91.4(2) 2 . ? O2 Co O1 99.68(15) 2 . ? O2 Co O1 80.32(15) . . ? O1 Co O1 180.0(2) 2 . ? C1 O1 Co 111.7(4) . . ? C2 O2 Co 111.5(4) . . ? Co O1W H1W 120(6) . . ? Co O1W H2W 105(8) . . ? H1W O1W H2W 121(6) . . ? C1 O3 Fe 113.3(3) . . ? C2 O4 Fe 113.9(3) . . ? C5 O5 Fe 115.1(3) . . ? C6 O6 Fe 115.1(3) . . ? C3 O9 Fe 115.5(3) . . ? C4 O10 Fe 115.3(3) . . ? C25 C22 C24 118.6(6) . . ? C25 C22 C23 121.2(7) . . ? C24 C22 C23 120.2(7) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 C27 120.9(6) . . ? C22 C24 H24 119.6 . . ? C27 C24 H24 119.5 . . ? C22 C25 C26 121.5(7) . . ? C22 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C28 120.2(6) . . ? C25 C26 H26 119.9 . . ? C28 C26 H26 119.9 . . ? C28 C27 C24 119.8(6) . . ? C28 C27 H27 120.1 . . ? C24 C27 H27 120.1 . . ? C27 C28 C26 119.0(6) . . ? C27 C28 S1 119.6(5) . . ? C26 C28 S1 121.4(5) . . ? O13 S1 O15 113.3(4) . . ? O13 S1 O14 112.0(5) . . ? O15 S1 O14 110.4(5) . . ? O13 S1 C28 107.9(3) . . ? O15 S1 C28 107.2(3) . . ? O14 S1 C28 105.5(3) . . ? N5 C7 N6 112.0(5) . . ? N5 C7 C13 124.3(5) . . ? N6 C7 C13 123.7(5) . . ? N4 C8 N3 112.4(4) . . ? N4 C8 C11 123.9(5) . . ? N3 C8 C11 123.7(5) . . ? N1 C9 N2 112.3(5) . . ? N1 C9 C15 125.1(5) . . ? N2 C9 C15 122.6(5) . . ? C15 C10 C11 120.0(5) . . ? C15 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0(5) . . ? C12 C11 C8 119.8(5) . . ? C10 C11 C8 120.3(5) . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.1(5) . . ? C14 C13 C7 120.9(4) . . ? C12 C13 C7 119.0(5) . . ? C15 C14 C13 120.0(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C10 119.9(5) . . ? C14 C15 C9 120.6(5) . . ? C10 C15 C9 119.5(4) . . ? N2 C16 C17 102.4(4) . . ? N2 C16 H16A 111.3 . . ? C17 C16 H16A 111.3 . . ? N2 C16 H16B 111.3 . . ? C17 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? N1 C17 C16 102.6(4) . . ? N1 C17 H17A 111.3 . . ? C16 C17 H17A 111.3 . . ? N1 C17 H17B 111.3 . . ? C16 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? N6 C18 C19 102.9(4) . . ? N6 C18 H18A 111.2 . . ? C19 C18 H18A 111.2 . . ? N6 C18 H18B 111.2 . . ? C19 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? N5 C19 C18 102.9(4) . . ? N5 C19 H19A 111.2 . . ? C18 C19 H19A 111.2 . . ? N5 C19 H19B 111.2 . . ? C18 C19 H19B 111.2 . . ? H19A C19 H19B 109.1 . . ? N3 C20 C21 102.9(4) . . ? N3 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? N3 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? N4 C21 C20 102.4(4) . . ? N4 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? N4 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C9 N1 C17 111.2(5) . . ? C9 N1 H1 124.4 . . ? C17 N1 H1 124.4 . . ? C9 N2 C16 111.4(5) . . ? C9 N2 H2 124.3 . . ? C16 N2 H2 124.3 . . ? C8 N3 C20 111.0(4) . . ? C8 N3 H3 124.5 . . ? C20 N3 H3 124.5 . . ? C8 N4 C21 111.3(4) . . ? C8 N4 H4 124.3 . . ? C21 N4 H4 124.3 . . ? C7 N5 C19 111.1(5) . . ? C7 N5 H5 124.5 . . ? C19 N5 H5 124.5 . . ? C7 N6 C18 111.2(4) . . ? C7 N6 H6 124.4 . . ? C18 N6 H6 124.4 . . ? H5W O2W H6W 121(5) . . ? H3W O3W H4W 126(6) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.514 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.078 data_e2343 _database_code_depnum_ccdc_archive 'CCDC 888663' #TrackingRef 'crystal4_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H80 Cr2 Mn N12 O40 S2' _chemical_formula_weight 1808.40 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7134(2) _cell_length_b 15.3318(3) _cell_length_c 15.4825(4) _cell_angle_alpha 112.4810(10) _cell_angle_beta 92.5320(10) _cell_angle_gamma 94.8230(10) _cell_volume 1897.84(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 32517 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 937 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.85 _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 28808 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0157 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6367 _reflns_number_gt 5788 _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 'Diamond 3' _computing_publication_material Platon _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. Because of the pour thermal parameters of the solvent molecules several restraints DFIX, DANG, OMIT, SADI, DELU, SIMU were employed Lines of res file: SADI 0.001 O1M C1M O12M C12M DELU O1M C1M DELU O12M C12M SIMU 0.01 0.02 1.7 O1M C1M SIMU 0.01 0.02 1.7 O12M C12M AFIX 6 O4W 6 0.227686 0.191691 0.905257 11.00000 0.07593 0.08991 = 0.09392 0.01292 0.00354 -0.01361 H4WA 2 0.291363 0.152454 0.873861 11.00000 -1.50000 H4WB 2 0.279247 0.245558 0.940545 11.00000 -1.50000 AFIX 0 The hydrogen atoms of the water molecules were located on a fourrier map and refined with restraints DFIX and DANG (O-H = 0.82A and H-H = 1.54A) 029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.950 A full set of data was collected, however the very high angle data was poor and was omitted A full set of data was collected, however the very high angle data was dominated by noise and was omitted. PLAT420_ALERT_2_B D-H Without Acceptor O4W - H4WA ... ? isolated water molecule ; _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^+3.2517P] 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 6367 _refine_ls_number_parameters 569 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.135 _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 C1M C 0.5045(17) 0.0027(12) 0.8720(13) 0.127(7) Uani 0.52 1 d PDU A 1 H1MA H 0.5644 -0.0344 0.8234 0.190 Uiso 0.52 1 calc PR A 1 H1MB H 0.4518 -0.0375 0.8986 0.190 Uiso 0.52 1 calc PR A 1 H1MC H 0.5716 0.0519 0.9200 0.190 Uiso 0.52 1 calc PR A 1 O1M O 0.3850(9) 0.0478(7) 0.8305(6) 0.049(2) Uani 0.52 1 d PDU A 1 H1M H 0.4057 0.0420 0.7775 0.074 Uiso 0.52 1 calc PR A 1 C12M C 0.555(3) 0.0322(13) 0.8858(15) 0.144(7) Uani 0.48 1 d PDU B 2 H12A H 0.5195 -0.0306 0.8809 0.216 Uiso 0.48 1 calc PR B 2 H12B H 0.5540 0.0762 0.9496 0.216 Uiso 0.48 1 calc PR B 2 H12C H 0.6587 0.0332 0.8671 0.216 Uiso 0.48 1 calc PR B 2 O12M O 0.4484(19) 0.0609(10) 0.8214(10) 0.108(5) Uani 0.48 1 d PDU B 2 H12M H 0.4043 0.0130 0.7796 0.162 Uiso 0.48 1 calc PR B 2 O4W O 0.2277(5) 0.1917(3) 0.9053(3) 0.0949(13) Uani 1 1 d G . . H4WA H 0.2914 0.1525 0.8739 0.142 Uiso 1 1 d G . . H4WB H 0.2792 0.2456 0.9405 0.142 Uiso 1 1 d G . . C1 C 0.1769(4) 0.1810(2) 0.1085(2) 0.0261(6) Uani 1 1 d . . . C2 C 0.0315(4) 0.2044(2) 0.06480(19) 0.0246(6) Uani 1 1 d . . . C3 C 0.2776(3) 0.4339(2) 0.0328(2) 0.0257(6) Uani 1 1 d . . . C4 C 0.1709(3) 0.50601(19) 0.09238(19) 0.0245(6) Uani 1 1 d . . . C5 C 0.1536(3) 0.4180(2) 0.3598(2) 0.0244(6) Uani 1 1 d . . . C6 C 0.3146(3) 0.46699(19) 0.3560(2) 0.0239(6) Uani 1 1 d . . . Cr1 Cr 0.19401(5) 0.37532(3) 0.17256(3) 0.02021(13) Uani 1 1 d . . . Mn1 Mn 0.0000 0.0000 0.0000 0.0433(2) Uani 1 2 d S . . O1 O 0.1957(3) 0.09670(15) 0.08905(16) 0.0379(6) Uani 1 1 d . . . O2 O -0.0656(3) 0.13818(15) 0.01568(14) 0.0327(5) Uani 1 1 d . . . O1W O -0.1098(4) 0.0170(2) 0.1264(2) 0.0609(8) Uani 1 1 d D . . O3 O 0.2659(2) 0.25221(13) 0.16313(13) 0.0252(4) Uani 1 1 d . . . O4 O 0.0220(2) 0.29142(14) 0.08462(13) 0.0256(4) Uani 1 1 d . . . O5 O 0.0761(2) 0.37807(14) 0.27926(13) 0.0262(4) Uani 1 1 d . . . O6 O 0.3548(2) 0.45042(14) 0.27326(14) 0.0254(4) Uani 1 1 d . . . O7 O 0.1102(3) 0.41922(16) 0.43393(14) 0.0348(5) Uani 1 1 d . . . O8 O 0.3903(3) 0.51677(16) 0.42960(15) 0.0343(5) Uani 1 1 d . . . O9 O 0.3111(2) 0.37333(14) 0.06761(14) 0.0265(4) Uani 1 1 d . . . O10 O 0.1242(2) 0.48932(14) 0.16240(14) 0.0260(4) Uani 1 1 d . . . O11 O 0.3211(3) 0.43620(16) -0.03989(15) 0.0383(6) Uani 1 1 d . . . O12 O 0.1419(3) 0.57256(15) 0.07167(15) 0.0334(5) Uani 1 1 d . . . H1W H -0.187(4) -0.016(3) 0.129(4) 0.09(2) Uiso 1 1 d D . . H2W H -0.097(7) 0.0738(11) 0.160(4) 0.13(3) Uiso 1 1 d D . . C22 C 0.5894(4) 0.2564(3) 0.6938(2) 0.0378(8) Uani 1 1 d . . . C23 C 0.5244(5) 0.3158(3) 0.7841(3) 0.0533(11) Uani 1 1 d . . . H23A H 0.4620 0.2751 0.8060 0.080 Uiso 1 1 calc R . . H23B H 0.4623 0.3599 0.7731 0.080 Uiso 1 1 calc R . . H23C H 0.6078 0.3501 0.8306 0.080 Uiso 1 1 calc R . . C24 C 0.5591(4) 0.1585(3) 0.6562(2) 0.0441(9) Uani 1 1 d . . . H24 H 0.4942 0.1291 0.6854 0.053 Uiso 1 1 calc R . . C25 C 0.6834(4) 0.2987(2) 0.6478(2) 0.0399(8) Uani 1 1 d . . . H25 H 0.7052 0.3644 0.6724 0.048 Uiso 1 1 calc R . . C26 C 0.7457(4) 0.2451(2) 0.5660(2) 0.0353(7) Uani 1 1 d . . . H26 H 0.8075 0.2746 0.5353 0.042 Uiso 1 1 calc R . . C27 C 0.6240(4) 0.1034(2) 0.5756(2) 0.0373(8) Uani 1 1 d . . . H27 H 0.6059 0.0376 0.5525 0.045 Uiso 1 1 calc R . . C28 C 0.7154(4) 0.1471(2) 0.5302(2) 0.0274(6) Uani 1 1 d . . . O13 O 0.9273(3) 0.1278(2) 0.41501(19) 0.0589(8) Uani 1 1 d . . . O14 O 0.6671(4) 0.0674(2) 0.35174(18) 0.0639(9) Uani 1 1 d . . . O15 O 0.8055(4) -0.01343(18) 0.4279(2) 0.0583(8) Uani 1 1 d . . . S1 S 0.78744(9) 0.07685(5) 0.42344(5) 0.02951(19) Uani 1 1 d . . . C7 C 0.3040(3) 0.27383(19) 0.48966(19) 0.0222(6) Uani 1 1 d . . . C8 C 0.0142(3) 0.2240(2) 0.73678(19) 0.0231(6) Uani 1 1 d . . . C9 C 0.2702(3) 0.5445(2) 0.79335(19) 0.0224(6) Uani 1 1 d . . . C10 C 0.1403(3) 0.3837(2) 0.76127(19) 0.0229(6) Uani 1 1 d . . . H10 H 0.1052 0.4072 0.8209 0.027 Uiso 1 1 calc R . . C11 C 0.1063(3) 0.2882(2) 0.70380(19) 0.0224(6) Uani 1 1 d . . . C12 C 0.1592(3) 0.2530(2) 0.61499(19) 0.0238(6) Uani 1 1 d . . . H12 H 0.1376 0.1889 0.5769 0.029 Uiso 1 1 calc R . . C13 C 0.2447(3) 0.3137(2) 0.58304(19) 0.0232(6) Uani 1 1 d . . . C14 C 0.2785(3) 0.4095(2) 0.64008(19) 0.0231(6) Uani 1 1 d . . . H14 H 0.3352 0.4502 0.6185 0.028 Uiso 1 1 calc R . . C15 C 0.2270(3) 0.44414(19) 0.72959(19) 0.0224(6) Uani 1 1 d . . . C16 C 0.3336(4) 0.6741(2) 0.9298(2) 0.0277(6) Uani 1 1 d . . . H16A H 0.4329 0.6894 0.9660 0.033 Uiso 1 1 calc R . . H16B H 0.2556 0.7041 0.9706 0.033 Uiso 1 1 calc R . . C17 C 0.3398(4) 0.7046(2) 0.8460(2) 0.0285(7) Uani 1 1 d . . . H17A H 0.2691 0.7516 0.8506 0.034 Uiso 1 1 calc R . . H17B H 0.4434 0.7303 0.8417 0.034 Uiso 1 1 calc R . . C18 C 0.3298(4) 0.1698(2) 0.3400(2) 0.0303(7) Uani 1 1 d . . . H18A H 0.2649 0.1647 0.2853 0.036 Uiso 1 1 calc R . . H18B H 0.3743 0.1106 0.3269 0.036 Uiso 1 1 calc R . . C19 C 0.4560(4) 0.2538(2) 0.36764(19) 0.0277(6) Uani 1 1 d . . . H19A H 0.5583 0.2328 0.3651 0.033 Uiso 1 1 calc R . . H19B H 0.4463 0.2887 0.3274 0.033 Uiso 1 1 calc R . . C20 C -0.0960(4) 0.0865(2) 0.7449(2) 0.0379(8) Uani 1 1 d . . . H20A H -0.0405 0.0481 0.7701 0.046 Uiso 1 1 calc R . . H20B H -0.1831 0.0473 0.7029 0.046 Uiso 1 1 calc R . . C21 C -0.1490(4) 0.1723(2) 0.8236(2) 0.0319(7) Uani 1 1 d . . . H21A H -0.2604 0.1719 0.8181 0.038 Uiso 1 1 calc R . . H21B H -0.1164 0.1737 0.8849 0.038 Uiso 1 1 calc R . . N1 N 0.2916(3) 0.61504(16) 0.76552(17) 0.0252(5) Uani 1 1 d . . . H1 H 0.2793 0.6097 0.7082 0.030 Uiso 1 1 calc R . . N2 N 0.2932(3) 0.57162(17) 0.88423(16) 0.0274(5) Uani 1 1 d . . . H2 H 0.2855 0.5339 0.9134 0.033 Uiso 1 1 calc R . . N3 N 0.0057(3) 0.13097(17) 0.69709(18) 0.0306(6) Uani 1 1 d . . . H3 H 0.0537 0.1002 0.6492 0.037 Uiso 1 1 calc R . . N4 N -0.0710(3) 0.25256(17) 0.80767(17) 0.0264(5) Uani 1 1 d . . . H4 H -0.0800 0.3111 0.8408 0.032 Uiso 1 1 calc R . . N5 N 0.4250(3) 0.31140(17) 0.46462(16) 0.0257(5) Uani 1 1 d . . . H5 H 0.4797 0.3632 0.5002 0.031 Uiso 1 1 calc R . . N6 N 0.2423(3) 0.19376(17) 0.42306(16) 0.0279(6) Uani 1 1 d . . . H6 H 0.1615 0.1600 0.4277 0.033 Uiso 1 1 calc R . . O2W O -0.2171(3) 0.38809(17) 0.41302(15) 0.0347(5) Uani 1 1 d D . . O3W O -0.0717(4) 0.1937(2) 0.26231(19) 0.0537(7) Uani 1 1 d D . . H3W H -0.094(5) 0.184(3) 0.3092(18) 0.063(14) Uiso 1 1 d D . . H4W H -0.045(6) 0.2481(12) 0.267(3) 0.070(15) Uiso 1 1 d D . . H5W H -0.1226(5) 0.398(3) 0.416(3) 0.051(13) Uiso 1 1 d D . . H6W H -0.259(4) 0.425(2) 0.457(2) 0.062(14) 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 C1M 0.055(7) 0.202(15) 0.077(8) 0.002(10) -0.021(6) 0.033(9) O1M 0.043(4) 0.062(5) 0.028(3) 0.004(3) -0.002(3) -0.007(3) C12M 0.243(19) 0.082(9) 0.152(15) 0.081(10) 0.065(12) 0.059(11) O12M 0.136(12) 0.055(6) 0.111(9) 0.007(6) -0.029(8) 0.040(8) O4W 0.076(3) 0.090(3) 0.094(3) 0.013(2) 0.004(2) -0.014(2) C1 0.0313(18) 0.0237(15) 0.0216(14) 0.0075(12) -0.0006(12) 0.0021(12) C2 0.0285(17) 0.0268(15) 0.0173(13) 0.0075(12) 0.0013(11) 0.0008(12) C3 0.0243(16) 0.0264(15) 0.0242(15) 0.0075(12) 0.0016(12) 0.0025(12) C4 0.0265(16) 0.0207(14) 0.0218(14) 0.0035(11) -0.0014(11) 0.0023(11) C5 0.0240(16) 0.0223(14) 0.0247(15) 0.0064(12) 0.0013(12) 0.0034(11) C6 0.0243(16) 0.0197(13) 0.0259(15) 0.0074(12) -0.0007(12) 0.0014(11) Cr1 0.0198(3) 0.0192(2) 0.0199(2) 0.00542(18) 0.00217(17) 0.00279(17) Mn1 0.0706(6) 0.0229(4) 0.0282(4) 0.0048(3) -0.0064(3) -0.0097(3) O1 0.0512(16) 0.0211(11) 0.0370(12) 0.0075(9) -0.0097(11) 0.0056(10) O2 0.0362(13) 0.0293(11) 0.0264(11) 0.0072(9) -0.0086(9) -0.0060(9) O1W 0.085(2) 0.0476(18) 0.0434(16) 0.0157(14) 0.0068(15) -0.0217(16) O3 0.0251(11) 0.0222(10) 0.0261(10) 0.0075(8) -0.0029(8) 0.0029(8) O4 0.0251(12) 0.0254(11) 0.0241(10) 0.0073(8) -0.0015(8) 0.0035(8) O5 0.0217(11) 0.0301(11) 0.0225(10) 0.0067(8) 0.0011(8) -0.0024(8) O6 0.0217(11) 0.0248(10) 0.0269(11) 0.0075(8) 0.0020(8) -0.0004(8) O7 0.0339(13) 0.0448(13) 0.0230(11) 0.0113(10) 0.0027(9) -0.0020(10) O8 0.0328(13) 0.0361(12) 0.0280(11) 0.0095(10) -0.0070(9) -0.0090(10) O9 0.0274(12) 0.0260(10) 0.0281(11) 0.0105(9) 0.0091(8) 0.0100(8) O10 0.0294(12) 0.0234(10) 0.0251(10) 0.0074(8) 0.0074(8) 0.0090(8) O11 0.0501(16) 0.0416(13) 0.0297(12) 0.0175(10) 0.0160(10) 0.0163(11) O12 0.0444(14) 0.0252(11) 0.0321(11) 0.0113(9) 0.0036(10) 0.0108(9) C22 0.0259(19) 0.050(2) 0.0287(16) 0.0041(15) -0.0053(13) 0.0136(15) C23 0.039(2) 0.075(3) 0.0339(19) 0.0049(19) 0.0010(16) 0.024(2) C24 0.033(2) 0.057(2) 0.0320(18) 0.0076(16) 0.0050(14) -0.0072(16) C25 0.053(2) 0.0288(17) 0.0346(18) 0.0067(14) -0.0025(15) 0.0166(15) C26 0.044(2) 0.0290(16) 0.0341(17) 0.0137(14) 0.0015(14) 0.0056(14) C27 0.036(2) 0.0332(17) 0.0341(17) 0.0057(14) 0.0014(14) -0.0084(14) C28 0.0238(17) 0.0281(15) 0.0266(15) 0.0070(12) -0.0024(12) 0.0027(12) O13 0.0499(17) 0.0613(18) 0.0468(15) 0.0036(13) 0.0192(13) -0.0183(13) O14 0.064(2) 0.076(2) 0.0326(14) -0.0029(13) -0.0087(13) 0.0284(16) O15 0.078(2) 0.0380(14) 0.0698(19) 0.0249(13) 0.0440(16) 0.0276(14) S1 0.0297(4) 0.0265(4) 0.0288(4) 0.0067(3) 0.0039(3) 0.0026(3) C7 0.0216(16) 0.0228(14) 0.0212(14) 0.0072(11) 0.0014(11) 0.0041(11) C8 0.0228(16) 0.0243(14) 0.0227(14) 0.0094(11) 0.0008(11) 0.0050(11) C9 0.0145(15) 0.0257(14) 0.0244(14) 0.0061(12) 0.0050(11) 0.0042(11) C10 0.0206(16) 0.0264(14) 0.0200(13) 0.0065(11) 0.0025(11) 0.0057(11) C11 0.0185(15) 0.0266(14) 0.0228(14) 0.0099(12) 0.0017(11) 0.0047(11) C12 0.0237(16) 0.0217(14) 0.0223(14) 0.0047(11) 0.0001(11) 0.0021(11) C13 0.0217(16) 0.0259(14) 0.0201(13) 0.0066(11) 0.0018(11) 0.0033(11) C14 0.0207(16) 0.0247(14) 0.0229(14) 0.0083(11) 0.0020(11) 0.0026(11) C15 0.0202(16) 0.0224(14) 0.0223(14) 0.0057(11) 0.0011(11) 0.0046(11) C16 0.0231(17) 0.0272(15) 0.0251(15) 0.0015(12) 0.0005(12) 0.0055(12) C17 0.0256(17) 0.0226(14) 0.0306(16) 0.0030(12) 0.0051(12) 0.0006(12) C18 0.0335(18) 0.0307(16) 0.0200(14) 0.0026(12) 0.0059(12) 0.0004(13) C19 0.0293(17) 0.0306(16) 0.0203(14) 0.0064(12) 0.0063(12) 0.0021(12) C20 0.047(2) 0.0284(16) 0.0455(19) 0.0212(15) 0.0130(16) 0.0057(14) C21 0.0361(19) 0.0329(17) 0.0319(16) 0.0179(14) 0.0076(13) 0.0037(13) N1 0.0267(14) 0.0220(12) 0.0230(12) 0.0046(10) 0.0027(10) 0.0018(10) N2 0.0319(15) 0.0261(13) 0.0216(12) 0.0064(10) 0.0030(10) 0.0027(10) N3 0.0390(16) 0.0231(13) 0.0300(13) 0.0089(11) 0.0127(11) 0.0061(11) N4 0.0317(15) 0.0240(12) 0.0255(12) 0.0108(10) 0.0089(10) 0.0056(10) N5 0.0266(14) 0.0251(12) 0.0190(12) 0.0026(10) 0.0034(10) -0.0031(10) N6 0.0286(14) 0.0257(13) 0.0221(12) 0.0022(10) 0.0067(10) -0.0039(10) O2W 0.0332(15) 0.0391(13) 0.0259(12) 0.0073(10) 0.0028(10) -0.0033(11) O3W 0.080(2) 0.0415(16) 0.0371(15) 0.0137(12) 0.0136(14) -0.0047(14) _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 C1M O1M 1.5424(16) . ? C1M H1MA 0.9600 . ? C1M H1MB 0.9600 . ? C1M H1MC 0.9600 . ? O1M H1M 0.8200 . ? C12M O12M 1.5417(11) . ? C12M H12A 0.9600 . ? C12M H12B 0.9600 . ? C12M H12C 0.9600 . ? O12M H12M 0.8200 . ? O4W H4WA 0.8731 . ? O4W H4WB 0.8679 . ? C1 O1 1.237(4) . ? C1 O3 1.266(3) . ? C1 C2 1.543(4) . ? C2 O2 1.238(4) . ? C2 O4 1.260(4) . ? C3 O11 1.215(4) . ? C3 O9 1.285(4) . ? C3 C4 1.551(4) . ? C4 O12 1.223(4) . ? C4 O10 1.281(3) . ? C5 O7 1.218(4) . ? C5 O5 1.288(3) . ? C5 C6 1.549(4) . ? C6 O8 1.225(4) . ? C6 O6 1.278(3) . ? Cr1 O9 1.948(2) . ? Cr1 O10 1.957(2) . ? Cr1 O6 1.970(2) . ? Cr1 O5 1.972(2) . ? Cr1 O4 1.977(2) . ? Cr1 O3 1.993(2) . ? Mn1 O1W 2.152(3) 2 ? Mn1 O1W 2.152(3) . ? Mn1 O2 2.167(2) . ? Mn1 O2 2.167(2) 2 ? Mn1 O1 2.193(2) . ? Mn1 O1 2.193(2) 2 ? O1W H1W 0.8202(7) . ? O1W H2W 0.8201(12) . ? C22 C24 1.383(5) . ? C22 C25 1.383(5) . ? C22 C23 1.513(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.388(5) . ? C24 H24 0.9300 . ? C25 C26 1.384(5) . ? C25 H25 0.9300 . ? C26 C28 1.384(4) . ? C26 H26 0.9300 . ? C27 C28 1.378(4) . ? C27 H27 0.9300 . ? C28 S1 1.769(3) . ? O13 S1 1.430(3) . ? O14 S1 1.450(3) . ? O15 S1 1.434(3) . ? C7 N5 1.303(4) . ? C7 N6 1.316(4) . ? C7 C13 1.474(4) . ? C8 N4 1.306(4) . ? C8 N3 1.313(4) . ? C8 C11 1.470(4) . ? C9 N2 1.306(4) . ? C9 N1 1.311(4) . ? C9 C15 1.481(4) . ? C10 C11 1.390(4) . ? C10 C15 1.390(4) . ? C10 H10 0.9300 . ? C11 C12 1.388(4) . ? C12 C13 1.391(4) . ? C12 H12 0.9300 . ? C13 C14 1.392(4) . ? C14 C15 1.392(4) . ? C14 H14 0.9300 . ? C16 N2 1.459(4) . ? C16 C17 1.540(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.471(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.464(4) . ? C18 C19 1.532(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.473(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.463(4) . ? C20 C21 1.534(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.464(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? O2W H5W 0.8201(12) . ? O2W H6W 0.8202(8) . ? O3W H3W 0.8202(8) . ? O3W H4W 0.8201(12) . ? 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 O12M C12M H12A 109.5 . . ? O12M C12M H12B 109.5 . . ? H12A C12M H12B 109.5 . . ? O12M C12M H12C 109.5 . . ? H12A C12M H12C 109.5 . . ? H12B C12M H12C 109.5 . . ? C12M O12M H12M 109.5 . . ? H4WA O4W H4WB 109.5 . . ? O1 C1 O3 126.1(3) . . ? O1 C1 C2 118.6(3) . . ? O3 C1 C2 115.3(2) . . ? O2 C2 O4 125.9(3) . . ? O2 C2 C1 118.6(3) . . ? O4 C2 C1 115.5(2) . . ? O11 C3 O9 125.3(3) . . ? O11 C3 C4 121.4(3) . . ? O9 C3 C4 113.3(2) . . ? O12 C4 O10 126.2(3) . . ? O12 C4 C3 119.8(3) . . ? O10 C4 C3 114.0(2) . . ? O7 C5 O5 125.7(3) . . ? O7 C5 C6 120.8(3) . . ? O5 C5 C6 113.6(2) . . ? O8 C6 O6 126.3(3) . . ? O8 C6 C5 119.0(3) . . ? O6 C6 C5 114.7(2) . . ? O9 Cr1 O10 82.80(8) . . ? O9 Cr1 O6 97.04(9) . . ? O10 Cr1 O6 92.27(9) . . ? O9 Cr1 O5 179.66(9) . . ? O10 Cr1 O5 97.03(9) . . ? O6 Cr1 O5 82.67(8) . . ? O9 Cr1 O4 90.48(9) . . ? O10 Cr1 O4 92.70(9) . . ? O6 Cr1 O4 171.45(8) . . ? O5 Cr1 O4 89.82(8) . . ? O9 Cr1 O3 90.37(8) . . ? O10 Cr1 O3 171.83(8) . . ? O6 Cr1 O3 93.01(8) . . ? O5 Cr1 O3 89.82(9) . . ? O4 Cr1 O3 82.85(8) . . ? O1W Mn1 O1W 180.0(2) 2 . ? O1W Mn1 O2 92.57(11) 2 . ? O1W Mn1 O2 87.43(11) . . ? O1W Mn1 O2 87.43(11) 2 2 ? O1W Mn1 O2 92.57(11) . 2 ? O2 Mn1 O2 180.00(15) . 2 ? O1W Mn1 O1 92.42(11) 2 . ? O1W Mn1 O1 87.58(11) . . ? O2 Mn1 O1 77.49(8) . . ? O2 Mn1 O1 102.51(8) 2 . ? O1W Mn1 O1 87.58(11) 2 2 ? O1W Mn1 O1 92.42(11) . 2 ? O2 Mn1 O1 102.51(8) . 2 ? O2 Mn1 O1 77.49(8) 2 2 ? O1 Mn1 O1 180.0(2) . 2 ? C1 O1 Mn1 112.2(2) . . ? C2 O2 Mn1 113.0(2) . . ? Mn1 O1W H1W 125(4) . . ? Mn1 O1W H2W 107(4) . . ? H1W O1W H2W 120(5) . . ? C1 O3 Cr1 112.85(19) . . ? C2 O4 Cr1 113.42(19) . . ? C5 O5 Cr1 114.26(18) . . ? C6 O6 Cr1 114.20(18) . . ? C3 O9 Cr1 114.63(18) . . ? C4 O10 Cr1 114.43(18) . . ? C24 C22 C25 118.3(3) . . ? C24 C22 C23 121.0(4) . . ? C25 C22 C23 120.7(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 C27 121.2(3) . . ? C22 C24 H24 119.4 . . ? C27 C24 H24 119.4 . . ? C26 C25 C22 121.3(3) . . ? C26 C25 H25 119.4 . . ? C22 C25 H25 119.4 . . ? C25 C26 C28 119.4(3) . . ? C25 C26 H26 120.3 . . ? C28 C26 H26 120.3 . . ? C28 C27 C24 119.5(3) . . ? C28 C27 H27 120.3 . . ? C24 C27 H27 120.3 . . ? C27 C28 C26 120.3(3) . . ? C27 C28 S1 119.2(2) . . ? C26 C28 S1 120.5(2) . . ? O13 S1 O15 114.80(19) . . ? O13 S1 O14 112.2(2) . . ? O15 S1 O14 110.7(2) . . ? O13 S1 C28 107.02(15) . . ? O15 S1 C28 106.65(15) . . ? O14 S1 C28 104.67(15) . . ? N5 C7 N6 112.5(2) . . ? N5 C7 C13 124.4(3) . . ? N6 C7 C13 123.1(3) . . ? N4 C8 N3 112.1(3) . . ? N4 C8 C11 124.1(3) . . ? N3 C8 C11 123.8(3) . . ? N2 C9 N1 112.9(3) . . ? N2 C9 C15 122.8(3) . . ? N1 C9 C15 124.3(3) . . ? C11 C10 C15 120.0(3) . . ? C11 C10 H10 120.0 . . ? C15 C10 H10 120.0 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 C8 120.2(2) . . ? C12 C11 C8 119.7(3) . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 C7 118.8(3) . . ? C14 C13 C7 120.9(3) . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C10 C15 C14 120.2(3) . . ? C10 C15 C9 119.5(2) . . ? C14 C15 C9 120.2(3) . . ? N2 C16 C17 102.6(2) . . ? N2 C16 H16A 111.2 . . ? C17 C16 H16A 111.2 . . ? N2 C16 H16B 111.2 . . ? C17 C16 H16B 111.2 . . ? H16A C16 H16B 109.2 . . ? N1 C17 C16 102.6(2) . . ? N1 C17 H17A 111.2 . . ? C16 C17 H17A 111.2 . . ? N1 C17 H17B 111.2 . . ? C16 C17 H17B 111.2 . . ? H17A C17 H17B 109.2 . . ? N6 C18 C19 103.1(2) . . ? N6 C18 H18A 111.1 . . ? C19 C18 H18A 111.1 . . ? N6 C18 H18B 111.1 . . ? C19 C18 H18B 111.1 . . ? H18A C18 H18B 109.1 . . ? N5 C19 C18 102.3(2) . . ? N5 C19 H19A 111.3 . . ? C18 C19 H19A 111.3 . . ? N5 C19 H19B 111.3 . . ? C18 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? N3 C20 C21 102.7(2) . . ? N3 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? N3 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.1 . . ? N4 C21 C20 102.5(2) . . ? N4 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? N4 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C9 N1 C17 110.5(2) . . ? C9 N1 H1 124.7 . . ? C17 N1 H1 124.7 . . ? C9 N2 C16 111.3(2) . . ? C9 N2 H2 124.4 . . ? C16 N2 H2 124.4 . . ? C8 N3 C20 111.2(2) . . ? C8 N3 H3 124.4 . . ? C20 N3 H3 124.4 . . ? C8 N4 C21 111.5(2) . . ? C8 N4 H4 124.3 . . ? C21 N4 H4 124.3 . . ? C7 N5 C19 111.3(2) . . ? C7 N5 H5 124.3 . . ? C19 N5 H5 124.3 . . ? C7 N6 C18 110.8(2) . . ? C7 N6 H6 124.6 . . ? C18 N6 H6 124.6 . . ? H5W O2W H6W 115(4) . . ? H3W O3W H4W 119(4) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.563 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.065 data_e2345 _database_code_depnum_ccdc_archive 'CCDC 888664' #TrackingRef 'crystal5_rev2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H80 Cr2 Fe N12 O40 S2' _chemical_formula_weight 1809.31 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7301(2) _cell_length_b 15.2924(4) _cell_length_c 15.4365(4) _cell_angle_alpha 112.5550(10) _cell_angle_beta 92.7400(10) _cell_angle_gamma 94.8370(10) _cell_volume 1889.22(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30656 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 0.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.28 _exptl_absorpt_correction_T_max 0.74 _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 24038 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_unetI/netI 0.0172 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 24.50 _reflns_number_total 5972 _reflns_number_gt 5455 _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 'Diamond 3' _computing_publication_material Platon _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. Hydrogen atoms for the water molecules were located directly from difference-Fourier maps and allowed to refine using DFIX and DANG restraints for their bond distance throughout the final convergence process. Lines of res file: SADI 0.001 O1M C1M O12M C12M DELU O1M C1M DELU O12M C12M SIMU 0.01 0.02 1.7 O1M C1M SIMU 0.01 0.02 1.7 O12M C12M AFIX 6 O4W 6 0.231619 0.185388 0.900916 11.00000 0.07069 0.11079 = 0.08827 0.01401 0.00637 -0.01171 H4WA 2 0.299532 0.154725 0.864584 11.00000 -1.50000 H4WB 2 0.277768 0.236564 0.944800 11.00000 -1.50000 AFIX 0 029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.952 A full set of data was collected, however the very high angle data was poor and was omitted A full set of data was collected, however the very high angle data was dominated by noise and was omitted. 420_ALERT_2_B D-H Without Acceptor O4W - H4WA ... ? isolated water molecule ; _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^+3.2517P] 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 5972 _refine_ls_number_parameters 569 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 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 C1M C 0.5182(10) 0.0096(8) 0.8746(7) 0.057(3) Uani 0.52 1 d PDU A 1 H1MA H 0.6060 0.0107 0.8397 0.086 Uiso 0.52 1 calc PR A 1 H1MB H 0.4883 -0.0546 0.8684 0.086 Uiso 0.52 1 calc PR A 1 H1MC H 0.5444 0.0495 0.9398 0.086 Uiso 0.52 1 calc PR A 1 O1M O 0.3835(6) 0.0465(4) 0.8358(4) 0.0507(15) Uani 0.52 1 d PDU A 1 H1M H 0.3806 0.0257 0.7781 0.076 Uiso 0.52 1 calc PR A 1 C12M C 0.548(2) 0.0360(14) 0.8917(11) 0.130(6) Uani 0.48 1 d PDU B 2 H12A H 0.5261 -0.0313 0.8755 0.194 Uiso 0.48 1 calc PR B 2 H12B H 0.5139 0.0701 0.9526 0.194 Uiso 0.48 1 calc PR B 2 H12C H 0.6569 0.0519 0.8929 0.194 Uiso 0.48 1 calc PR B 2 O12M O 0.4623(9) 0.0635(5) 0.8180(5) 0.0664(19) Uani 0.48 1 d PDU B 2 H12M H 0.4297 0.0151 0.7721 0.100 Uiso 0.48 1 calc PR B 2 O4W O 0.2316(4) 0.1854(3) 0.9009(3) 0.0988(12) Uani 1 1 d G . . H4WA H 0.2995 0.1547 0.8646 0.148 Uiso 1 1 d G . . H4WB H 0.2778 0.2366 0.9448 0.148 Uiso 1 1 d G . . C1 C 0.1757(3) 0.17802(18) 0.10764(18) 0.0248(6) Uani 1 1 d . . . C2 C 0.0298(3) 0.20156(18) 0.06362(18) 0.0224(5) Uani 1 1 d . . . C3 C 0.2775(3) 0.43185(18) 0.03163(19) 0.0247(6) Uani 1 1 d . . . C4 C 0.1716(3) 0.50451(17) 0.09168(18) 0.0232(5) Uani 1 1 d . . . C5 C 0.1532(3) 0.41665(17) 0.35959(19) 0.0240(6) Uani 1 1 d . . . C6 C 0.3141(3) 0.46585(17) 0.35570(19) 0.0231(6) Uani 1 1 d . . . Cr1 Cr 0.19334(4) 0.37295(3) 0.17170(3) 0.01929(12) Uani 1 1 d . . . Fe2 Fe 0.0000 0.0000 0.0000 0.03382(16) Uani 1 2 d S . . O1 O 0.1936(2) 0.09375(13) 0.08818(15) 0.0374(5) Uani 1 1 d . . . O2 O -0.0676(2) 0.13527(13) 0.01449(13) 0.0293(4) Uani 1 1 d . . . O1W O -0.1057(3) 0.01410(18) 0.12171(18) 0.0515(6) Uani 1 1 d D . . O3 O 0.26497(19) 0.24977(12) 0.16236(12) 0.0242(4) Uani 1 1 d . . . O4 O 0.02094(19) 0.28902(12) 0.08328(12) 0.0235(4) Uani 1 1 d . . . O5 O 0.07582(19) 0.37582(13) 0.27869(12) 0.0251(4) Uani 1 1 d . . . O6 O 0.35435(19) 0.44873(12) 0.27312(12) 0.0239(4) Uani 1 1 d . . . O7 O 0.1097(2) 0.41833(14) 0.43419(13) 0.0339(5) Uani 1 1 d . . . O8 O 0.3893(2) 0.51654(14) 0.42998(14) 0.0329(4) Uani 1 1 d . . . O9 O 0.3099(2) 0.37045(12) 0.06626(13) 0.0261(4) Uani 1 1 d . . . O10 O 0.1239(2) 0.48749(12) 0.16153(12) 0.0243(4) Uani 1 1 d . . . O11 O 0.3221(2) 0.43475(15) -0.04063(14) 0.0372(5) Uani 1 1 d . . . O12 O 0.1428(2) 0.57121(13) 0.07089(14) 0.0318(4) Uani 1 1 d . . . H1W H -0.176(4) -0.025(3) 0.122(4) 0.104(19) Uiso 1 1 d D . . H2W H -0.093(6) 0.0693(12) 0.160(3) 0.094(18) Uiso 1 1 d D . . C22 C 0.5902(3) 0.2571(2) 0.6923(2) 0.0359(7) Uani 1 1 d . . . C23 C 0.5254(4) 0.3170(3) 0.7825(2) 0.0521(9) Uani 1 1 d . . . H23A H 0.4628 0.2764 0.8045 0.078 Uiso 1 1 calc R . . H23B H 0.4635 0.3611 0.7710 0.078 Uiso 1 1 calc R . . H23C H 0.6086 0.3516 0.8293 0.078 Uiso 1 1 calc R . . C24 C 0.5596(3) 0.1589(2) 0.6549(2) 0.0412(7) Uani 1 1 d . . . H24 H 0.4944 0.1297 0.6842 0.049 Uiso 1 1 calc R . . C25 C 0.6843(4) 0.2987(2) 0.6462(2) 0.0382(7) Uani 1 1 d . . . H25 H 0.7067 0.3647 0.6708 0.046 Uiso 1 1 calc R . . C26 C 0.7463(3) 0.2449(2) 0.5642(2) 0.0331(6) Uani 1 1 d . . . H26 H 0.8079 0.2743 0.5335 0.040 Uiso 1 1 calc R . . C27 C 0.6240(3) 0.1033(2) 0.5747(2) 0.0350(7) Uani 1 1 d . . . H27 H 0.6059 0.0373 0.5520 0.042 Uiso 1 1 calc R . . C28 C 0.7156(3) 0.14661(18) 0.52856(19) 0.0254(6) Uani 1 1 d . . . O13 O 0.9273(3) 0.12612(18) 0.41303(16) 0.0540(6) Uani 1 1 d . . . O14 O 0.6673(3) 0.06561(19) 0.34922(16) 0.0603(7) Uani 1 1 d . . . O15 O 0.8058(3) -0.01465(16) 0.42706(18) 0.0565(7) Uani 1 1 d . . . S1 S 0.78687(7) 0.07535(5) 0.42166(5) 0.02731(16) Uani 1 1 d . . . C7 C 0.3034(3) 0.27397(17) 0.49000(18) 0.0211(5) Uani 1 1 d . . . C8 C 0.0125(3) 0.22450(17) 0.73729(18) 0.0215(5) Uani 1 1 d . . . C9 C 0.2706(3) 0.54605(17) 0.79465(18) 0.0211(5) Uani 1 1 d . . . C10 C 0.1394(3) 0.38500(17) 0.76187(18) 0.0218(5) Uani 1 1 d . . . H10 H 0.1040 0.4088 0.8215 0.026 Uiso 1 1 calc R . . C11 C 0.1050(3) 0.28892(17) 0.70421(18) 0.0206(5) Uani 1 1 d . . . C12 C 0.1580(3) 0.25345(18) 0.61542(18) 0.0229(5) Uani 1 1 d . . . H12 H 0.1363 0.1891 0.5773 0.028 Uiso 1 1 calc R . . C13 C 0.2438(3) 0.31413(18) 0.58327(18) 0.0217(5) Uani 1 1 d . . . C14 C 0.2784(3) 0.41055(18) 0.64099(18) 0.0219(5) Uani 1 1 d . . . H14 H 0.3357 0.4512 0.6197 0.026 Uiso 1 1 calc R . . C15 C 0.2268(3) 0.44537(17) 0.73022(18) 0.0213(5) Uani 1 1 d . . . C16 C 0.3346(3) 0.67597(18) 0.93204(18) 0.0263(6) Uani 1 1 d . . . H16A H 0.4335 0.6915 0.9689 0.032 Uiso 1 1 calc R . . H16B H 0.2563 0.7059 0.9725 0.032 Uiso 1 1 calc R . . C17 C 0.3416(3) 0.70660(18) 0.84825(19) 0.0275(6) Uani 1 1 d . . . H17A H 0.2720 0.7541 0.8529 0.033 Uiso 1 1 calc R . . H17B H 0.4455 0.7319 0.8442 0.033 Uiso 1 1 calc R . . C18 C 0.3300(3) 0.16850(19) 0.34008(19) 0.0288(6) Uani 1 1 d . . . H18A H 0.2657 0.1621 0.2845 0.035 Uiso 1 1 calc R . . H18B H 0.3751 0.1096 0.3283 0.035 Uiso 1 1 calc R . . C19 C 0.4549(3) 0.25324(18) 0.36778(18) 0.0260(6) Uani 1 1 d . . . H19A H 0.5574 0.2328 0.3654 0.031 Uiso 1 1 calc R . . H19B H 0.4443 0.2879 0.3271 0.031 Uiso 1 1 calc R . . C20 C -0.0979(3) 0.0868(2) 0.7448(2) 0.0335(6) Uani 1 1 d . . . H20A H -0.0421 0.0484 0.7701 0.040 Uiso 1 1 calc R . . H20B H -0.1851 0.0473 0.7027 0.040 Uiso 1 1 calc R . . C21 C -0.1503(3) 0.17310(19) 0.8240(2) 0.0290(6) Uani 1 1 d . . . H21A H -0.2614 0.1731 0.8181 0.035 Uiso 1 1 calc R . . H21B H -0.1185 0.1742 0.8855 0.035 Uiso 1 1 calc R . . N1 N 0.2923(2) 0.61685(14) 0.76701(15) 0.0237(5) Uani 1 1 d . . . H1 H 0.2795 0.6116 0.7096 0.028 Uiso 1 1 calc R . . N2 N 0.2943(2) 0.57282(15) 0.88565(15) 0.0261(5) Uani 1 1 d . . . H2 H 0.2872 0.5348 0.9147 0.031 Uiso 1 1 calc R . . N3 N 0.0029(3) 0.13143(15) 0.69687(16) 0.0280(5) Uani 1 1 d . . . H3 H 0.0498 0.1006 0.6485 0.034 Uiso 1 1 calc R . . N4 N -0.0709(2) 0.25348(15) 0.80869(15) 0.0244(5) Uani 1 1 d . . . H4 H -0.0783 0.3123 0.8425 0.029 Uiso 1 1 calc R . . N5 N 0.4244(2) 0.31124(15) 0.46463(15) 0.0242(5) Uani 1 1 d . . . H5 H 0.4793 0.3632 0.5002 0.029 Uiso 1 1 calc R . . N6 N 0.2418(2) 0.19348(15) 0.42286(15) 0.0265(5) Uani 1 1 d . . . H6 H 0.1604 0.1600 0.4271 0.032 Uiso 1 1 calc R . . O2W O -0.2169(2) 0.38706(15) 0.41247(14) 0.0336(5) Uani 1 1 d D . . O3W O -0.0759(3) 0.19056(18) 0.25930(17) 0.0529(6) Uani 1 1 d D . . H3W H -0.092(5) 0.181(3) 0.3070(15) 0.064(13) Uiso 1 1 d D . . H4W H -0.046(4) 0.2450(10) 0.265(3) 0.061(12) Uiso 1 1 d D . . H5W H -0.1225(4) 0.397(3) 0.421(2) 0.055(11) Uiso 1 1 d D . . H6W H -0.262(4) 0.424(2) 0.4546(19) 0.061(12) 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 C1M 0.034(3) 0.086(7) 0.037(5) 0.008(4) -0.015(3) 0.011(4) O1M 0.047(3) 0.064(3) 0.031(3) 0.008(2) 0.006(2) -0.002(3) C12M 0.230(16) 0.094(10) 0.100(12) 0.068(10) 0.039(11) 0.047(11) O12M 0.070(5) 0.054(4) 0.064(5) 0.007(3) -0.008(4) 0.031(4) O4W 0.071(2) 0.111(3) 0.088(3) 0.014(2) 0.0064(18) -0.012(2) C1 0.0293(13) 0.0235(14) 0.0202(15) 0.0072(11) -0.0034(10) 0.0041(10) C2 0.0279(13) 0.0236(13) 0.0150(14) 0.0069(10) -0.0004(10) 0.0030(10) C3 0.0253(13) 0.0252(13) 0.0212(16) 0.0061(11) 0.0021(10) 0.0040(10) C4 0.0248(12) 0.0209(13) 0.0199(15) 0.0037(10) -0.0008(10) 0.0031(10) C5 0.0251(13) 0.0221(13) 0.0223(16) 0.0059(11) 0.0006(11) 0.0043(10) C6 0.0248(13) 0.0190(12) 0.0248(16) 0.0079(11) -0.0013(11) 0.0033(10) Cr1 0.0197(2) 0.0189(2) 0.0178(2) 0.00527(16) 0.00170(15) 0.00350(15) Fe2 0.0468(4) 0.0199(3) 0.0290(3) 0.0059(2) -0.0125(3) -0.0003(2) O1 0.0449(12) 0.0205(10) 0.0407(13) 0.0073(9) -0.0160(9) 0.0050(8) O2 0.0342(10) 0.0238(9) 0.0256(11) 0.0070(8) -0.0098(8) -0.0010(8) O1W 0.0661(16) 0.0405(14) 0.0460(16) 0.0186(12) -0.0005(12) -0.0110(12) O3 0.0246(9) 0.0217(9) 0.0242(10) 0.0074(8) -0.0044(7) 0.0028(7) O4 0.0249(9) 0.0218(9) 0.0217(10) 0.0061(7) -0.0020(7) 0.0051(7) O5 0.0226(9) 0.0302(10) 0.0190(10) 0.0065(8) 0.0005(7) -0.0014(7) O6 0.0227(9) 0.0241(9) 0.0224(11) 0.0066(7) 0.0014(7) 0.0007(7) O7 0.0341(10) 0.0452(12) 0.0199(12) 0.0109(9) 0.0034(8) -0.0010(9) O8 0.0327(10) 0.0351(11) 0.0250(11) 0.0086(9) -0.0073(8) -0.0066(8) O9 0.0276(9) 0.0280(9) 0.0265(11) 0.0122(8) 0.0094(7) 0.0122(7) O10 0.0284(9) 0.0222(9) 0.0220(10) 0.0064(7) 0.0072(7) 0.0090(7) O11 0.0489(12) 0.0428(12) 0.0279(12) 0.0182(9) 0.0170(9) 0.0180(9) O12 0.0445(11) 0.0245(10) 0.0289(11) 0.0113(8) 0.0040(8) 0.0116(8) C22 0.0262(14) 0.0475(18) 0.0266(17) 0.0051(13) -0.0055(11) 0.0142(12) C23 0.0382(17) 0.074(2) 0.0323(19) 0.0043(17) 0.0010(14) 0.0248(17) C24 0.0310(15) 0.055(2) 0.0293(18) 0.0100(14) 0.0029(12) -0.0059(13) C25 0.0523(18) 0.0291(15) 0.0306(18) 0.0072(13) -0.0035(13) 0.0162(13) C26 0.0411(16) 0.0280(14) 0.0321(17) 0.0137(12) 0.0007(12) 0.0056(12) C27 0.0342(15) 0.0335(15) 0.0302(17) 0.0072(13) 0.0005(12) -0.0075(12) C28 0.0238(13) 0.0276(14) 0.0230(15) 0.0081(11) -0.0025(10) 0.0050(10) O13 0.0449(13) 0.0593(15) 0.0417(14) 0.0044(11) 0.0166(10) -0.0147(11) O14 0.0588(15) 0.0747(18) 0.0297(14) -0.0019(12) -0.0089(11) 0.0282(13) O15 0.0776(17) 0.0371(12) 0.0667(17) 0.0246(12) 0.0437(14) 0.0286(12) S1 0.0278(3) 0.0258(3) 0.0257(4) 0.0069(3) 0.0030(3) 0.0037(3) C7 0.0213(12) 0.0233(13) 0.0192(14) 0.0082(10) 0.0024(10) 0.0053(10) C8 0.0215(12) 0.0247(13) 0.0198(14) 0.0097(11) 0.0001(10) 0.0060(10) C9 0.0174(11) 0.0241(13) 0.0203(16) 0.0060(11) 0.0048(9) 0.0053(9) C10 0.0214(12) 0.0253(13) 0.0183(14) 0.0069(10) 0.0033(9) 0.0073(10) C11 0.0203(12) 0.0237(13) 0.0189(14) 0.0090(10) 0.0011(9) 0.0053(9) C12 0.0249(12) 0.0221(12) 0.0193(14) 0.0053(10) 0.0010(10) 0.0033(10) C13 0.0214(12) 0.0252(13) 0.0167(14) 0.0058(10) 0.0022(9) 0.0049(10) C14 0.0209(12) 0.0239(13) 0.0206(14) 0.0079(10) 0.0027(10) 0.0034(10) C15 0.0200(12) 0.0225(12) 0.0203(14) 0.0064(10) 0.0014(9) 0.0050(9) C16 0.0240(13) 0.0259(13) 0.0221(15) 0.0010(11) 0.0006(10) 0.0067(10) C17 0.0263(13) 0.0225(13) 0.0276(16) 0.0029(11) 0.0056(11) 0.0020(10) C18 0.0349(14) 0.0290(14) 0.0171(15) 0.0031(11) 0.0061(11) 0.0022(11) C19 0.0272(13) 0.0300(14) 0.0185(15) 0.0061(11) 0.0063(10) 0.0043(11) C20 0.0414(16) 0.0286(14) 0.0375(18) 0.0195(13) 0.0092(13) 0.0062(12) C21 0.0331(14) 0.0314(14) 0.0271(16) 0.0164(12) 0.0057(11) 0.0028(11) N1 0.0273(11) 0.0224(11) 0.0188(12) 0.0048(9) 0.0021(8) 0.0035(8) N2 0.0341(12) 0.0244(11) 0.0179(14) 0.0061(9) 0.0024(9) 0.0026(9) N3 0.0371(12) 0.0226(11) 0.0250(13) 0.0087(9) 0.0102(10) 0.0058(9) N4 0.0304(11) 0.0226(11) 0.0220(13) 0.0096(9) 0.0080(9) 0.0053(9) N5 0.0253(11) 0.0246(11) 0.0173(12) 0.0032(9) 0.0030(8) -0.0021(9) N6 0.0288(11) 0.0257(11) 0.0189(12) 0.0025(9) 0.0071(9) -0.0022(9) O2W 0.0337(11) 0.0376(11) 0.0241(12) 0.0073(9) 0.0033(9) -0.0027(9) O3W 0.0828(18) 0.0414(14) 0.0336(15) 0.0146(11) 0.0140(12) -0.0025(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1M O1M 1.5380(16) . ? C1M H1MA 0.9600 . ? C1M H1MB 0.9600 . ? C1M H1MC 0.9600 . ? O1M H1M 0.8200 . ? C12M O12M 1.5390(11) . ? C12M H12A 0.9600 . ? C12M H12B 0.9600 . ? C12M H12C 0.9600 . ? O12M H12M 0.8200 . ? O4W H4WA 0.8734 . ? O4W H4WB 0.8647 . ? C1 O1 1.232(3) . ? C1 O3 1.268(3) . ? C1 C2 1.548(3) . ? C2 O2 1.236(3) . ? C2 O4 1.263(3) . ? C3 O11 1.214(3) . ? C3 O9 1.289(3) . ? C3 C4 1.554(3) . ? C4 O12 1.222(3) . ? C4 O10 1.282(3) . ? C5 O7 1.221(3) . ? C5 O5 1.287(3) . ? C5 C6 1.552(3) . ? C6 O8 1.228(3) . ? C6 O6 1.273(3) . ? Cr1 O9 1.9504(18) . ? Cr1 O10 1.9599(17) . ? Cr1 O6 1.9731(17) . ? Cr1 O5 1.9739(18) . ? Cr1 O4 1.9772(17) . ? Cr1 O3 1.9898(17) . ? Fe2 O1W 2.077(3) 2 ? Fe2 O1W 2.077(3) . ? Fe2 O2 2.1309(18) . ? Fe2 O2 2.1309(18) 2 ? Fe2 O1 2.1538(19) . ? Fe2 O1 2.1538(19) 2 ? O1W H1W 0.8203(9) . ? O1W H2W 0.820(2) . ? C22 C25 1.380(5) . ? C22 C24 1.384(5) . ? C22 C23 1.511(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C27 1.382(4) . ? C24 H24 0.9300 . ? C25 C26 1.383(4) . ? C25 H25 0.9300 . ? C26 C28 1.384(4) . ? C26 H26 0.9300 . ? C27 C28 1.383(4) . ? C27 H27 0.9300 . ? C28 S1 1.769(3) . ? O13 S1 1.435(2) . ? O14 S1 1.448(2) . ? O15 S1 1.433(2) . ? C7 N5 1.305(3) . ? C7 N6 1.317(3) . ? C7 C13 1.472(3) . ? C8 N4 1.303(3) . ? C8 N3 1.310(3) . ? C8 C11 1.474(3) . ? C9 N2 1.304(3) . ? C9 N1 1.311(3) . ? C9 C15 1.482(3) . ? C10 C15 1.391(4) . ? C10 C11 1.392(4) . ? C10 H10 0.9300 . ? C11 C12 1.386(4) . ? C12 C13 1.393(4) . ? C12 H12 0.9300 . ? C13 C14 1.396(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9300 . ? C16 N2 1.463(3) . ? C16 C17 1.537(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N1 1.473(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N6 1.463(3) . ? C18 C19 1.531(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.468(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.462(3) . ? C20 C21 1.537(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.464(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? O2W H5W 0.820(2) . ? O2W H6W 0.8210(16) . ? O3W H3W 0.8208(16) . ? O3W H4W 0.820(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 O12M C12M H12A 109.5 . . ? O12M C12M H12B 109.5 . . ? H12A C12M H12B 109.5 . . ? O12M C12M H12C 109.5 . . ? H12A C12M H12C 109.5 . . ? H12B C12M H12C 109.5 . . ? C12M O12M H12M 109.5 . . ? H4WA O4W H4WB 109.3 . . ? O1 C1 O3 126.4(2) . . ? O1 C1 C2 118.5(2) . . ? O3 C1 C2 115.1(2) . . ? O2 C2 O4 125.8(2) . . ? O2 C2 C1 118.6(2) . . ? O4 C2 C1 115.5(2) . . ? O11 C3 O9 125.3(2) . . ? O11 C3 C4 121.4(2) . . ? O9 C3 C4 113.3(2) . . ? O12 C4 O10 126.1(2) . . ? O12 C4 C3 119.8(2) . . ? O10 C4 C3 114.1(2) . . ? O7 C5 O5 125.6(2) . . ? O7 C5 C6 120.9(2) . . ? O5 C5 C6 113.6(2) . . ? O8 C6 O6 126.4(2) . . ? O8 C6 C5 118.7(2) . . ? O6 C6 C5 114.9(2) . . ? O9 Cr1 O10 82.93(7) . . ? O9 Cr1 O6 97.12(8) . . ? O10 Cr1 O6 92.11(7) . . ? O9 Cr1 O5 179.82(9) . . ? O10 Cr1 O5 97.03(7) . . ? O6 Cr1 O5 82.70(7) . . ? O9 Cr1 O4 90.42(8) . . ? O10 Cr1 O4 92.60(7) . . ? O6 Cr1 O4 171.55(7) . . ? O5 Cr1 O4 89.76(7) . . ? O9 Cr1 O3 90.23(7) . . ? O10 Cr1 O3 171.89(7) . . ? O6 Cr1 O3 93.06(7) . . ? O5 Cr1 O3 89.83(7) . . ? O4 Cr1 O3 83.06(7) . . ? O1W Fe2 O1W 180.00(18) 2 . ? O1W Fe2 O2 91.76(9) 2 . ? O1W Fe2 O2 88.24(9) . . ? O1W Fe2 O2 88.24(9) 2 2 ? O1W Fe2 O2 91.76(9) . 2 ? O2 Fe2 O2 180.00(9) . 2 ? O1W Fe2 O1 91.93(9) 2 . ? O1W Fe2 O1 88.07(9) . . ? O2 Fe2 O1 79.11(7) . . ? O2 Fe2 O1 100.89(7) 2 . ? O1W Fe2 O1 88.07(9) 2 2 ? O1W Fe2 O1 91.93(9) . 2 ? O2 Fe2 O1 100.89(7) . 2 ? O2 Fe2 O1 79.11(7) 2 2 ? O1 Fe2 O1 180.00(19) . 2 ? C1 O1 Fe2 111.59(16) . . ? C2 O2 Fe2 112.10(16) . . ? Fe2 O1W H1W 122(4) . . ? Fe2 O1W H2W 112(3) . . ? H1W O1W H2W 123(4) . . ? C1 O3 Cr1 112.97(15) . . ? C2 O4 Cr1 113.28(15) . . ? C5 O5 Cr1 114.18(15) . . ? C6 O6 Cr1 114.09(15) . . ? C3 O9 Cr1 114.60(15) . . ? C4 O10 Cr1 114.37(15) . . ? C25 C22 C24 118.2(3) . . ? C25 C22 C23 120.9(3) . . ? C24 C22 C23 120.9(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 C27 121.2(3) . . ? C22 C24 H24 119.4 . . ? C27 C24 H24 119.4 . . ? C22 C25 C26 121.6(3) . . ? C22 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C28 C26 C25 119.2(3) . . ? C28 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C24 119.6(3) . . ? C28 C27 H27 120.2 . . ? C24 C27 H27 120.2 . . ? C27 C28 C26 120.1(3) . . ? C27 C28 S1 119.3(2) . . ? C26 C28 S1 120.6(2) . . ? O13 S1 O15 114.26(16) . . ? O13 S1 O14 112.01(17) . . ? O15 S1 O14 111.25(17) . . ? O13 S1 C28 107.07(13) . . ? O15 S1 C28 106.65(13) . . ? O14 S1 C28 104.91(13) . . ? N5 C7 N6 112.0(2) . . ? N5 C7 C13 124.8(2) . . ? N6 C7 C13 123.1(2) . . ? N4 C8 N3 112.4(2) . . ? N4 C8 C11 124.0(2) . . ? N3 C8 C11 123.6(2) . . ? N2 C9 N1 113.0(2) . . ? N2 C9 C15 122.7(2) . . ? N1 C9 C15 124.3(2) . . ? C15 C10 C11 120.0(2) . . ? C15 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0(2) . . ? C12 C11 C8 119.7(2) . . ? C10 C11 C8 120.3(2) . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 120.0(2) . . ? C12 C13 C7 118.9(2) . . ? C14 C13 C7 121.0(2) . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C10 120.3(2) . . ? C14 C15 C9 120.4(2) . . ? C10 C15 C9 119.3(2) . . ? N2 C16 C17 102.5(2) . . ? N2 C16 H16A 111.3 . . ? C17 C16 H16A 111.3 . . ? N2 C16 H16B 111.3 . . ? C17 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? N1 C17 C16 102.7(2) . . ? N1 C17 H17A 111.2 . . ? C16 C17 H17A 111.2 . . ? N1 C17 H17B 111.2 . . ? C16 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? N6 C18 C19 102.8(2) . . ? N6 C18 H18A 111.2 . . ? C19 C18 H18A 111.2 . . ? N6 C18 H18B 111.2 . . ? C19 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? N5 C19 C18 102.5(2) . . ? N5 C19 H19A 111.3 . . ? C18 C19 H19A 111.3 . . ? N5 C19 H19B 111.3 . . ? C18 C19 H19B 111.3 . . ? H19A C19 H19B 109.2 . . ? N3 C20 C21 102.6(2) . . ? N3 C20 H20A 111.2 . . ? C21 C20 H20A 111.2 . . ? N3 C20 H20B 111.2 . . ? C21 C20 H20B 111.2 . . ? H20A C20 H20B 109.2 . . ? N4 C21 C20 102.4(2) . . ? N4 C21 H21A 111.3 . . ? C20 C21 H21A 111.3 . . ? N4 C21 H21B 111.3 . . ? C20 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C9 N1 C17 110.4(2) . . ? C9 N1 H1 124.8 . . ? C17 N1 H1 124.8 . . ? C9 N2 C16 111.3(2) . . ? C9 N2 H2 124.4 . . ? C16 N2 H2 124.4 . . ? C8 N3 C20 111.1(2) . . ? C8 N3 H3 124.4 . . ? C20 N3 H3 124.4 . . ? C8 N4 C21 111.4(2) . . ? C8 N4 H4 124.3 . . ? C21 N4 H4 124.3 . . ? C7 N5 C19 111.5(2) . . ? C7 N5 H5 124.3 . . ? C19 N5 H5 124.3 . . ? C7 N6 C18 111.1(2) . . ? C7 N6 H6 124.5 . . ? C18 N6 H6 124.5 . . ? H5W O2W H6W 115(3) . . ? H3W O3W H4W 118(3) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.734 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.054