# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef '- Crystal1.cif' _journal_coden_Cambridge 222 _publ_contact_author_name "Catalina Ruiz P\'erez" _publ_contact_author_address ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; _publ_contact_author_email caruiz@ull.es _publ_contact_author_phone +34922318236 _publ_contact_author_fax +34922318320 loop_ _publ_author_name _publ_author_address "Professor Catalina Ruiz P\'erez" ;Laboratorio de Rayos X y Materiales Moleculares Dpto. F\'isica Fundamental II. Facultad de F\'isica Universidad de La Laguna E-38204. La Laguna. Tenerife Spain ; data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 806213' #TrackingRef '- Crystal1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Cr Mn N8 O7' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 293(2) _chemical_formula_weight 747.60 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.6900(10) _cell_length_b 15.1020(10) _cell_length_c 22.7070(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 98.684(10) _cell_angle_gamma 90.000(10) _cell_volume 7352.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6095 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6095 _reflns_number_gt 5067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+24.9489P] 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 6095 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.23074(3) 0.67263(4) 1.08813(3) 0.0408(2) Uani 1 1 d . . . Cr1 Cr 0.12920(3) 0.37001(5) 1.13107(3) 0.0453(2) Uani 1 1 d . . . C1 C 0.1432(2) 0.5042(3) 1.11741(19) 0.0484(10) Uani 1 1 d . . . C2 C 0.2236(3) 0.3551(4) 1.1565(2) 0.0667(14) Uani 1 1 d . . . C3 C 0.1183(2) 0.2363(3) 1.1464(2) 0.0505(11) Uani 1 1 d . . . C4 C 0.1156(2) 0.3980(4) 1.2159(2) 0.0607(13) Uani 1 1 d . . . C5 C 0.1823(3) 0.3373(3) 1.0150(2) 0.0616(13) Uani 1 1 d . . . H5 H 0.2211 0.3389 1.0388 0.074 Uiso 1 1 calc R . . C6 C 0.1797(3) 0.3214(4) 0.9552(3) 0.0812(18) Uani 1 1 d . . . H6 H 0.2161 0.3125 0.9390 0.097 Uiso 1 1 calc R . . C7 C 0.1231(4) 0.3187(5) 0.9201(3) 0.0843(18) Uani 1 1 d . . . H7 H 0.1201 0.3060 0.8797 0.101 Uiso 1 1 calc R . . C8 C 0.0702(3) 0.3352(4) 0.9453(2) 0.0718(15) Uani 1 1 d . . . H8 H 0.0312 0.3346 0.9217 0.086 Uiso 1 1 calc R . . C9 C 0.0752(2) 0.3525(3) 1.00533(19) 0.0479(10) Uani 1 1 d . . . C10 C 0.0220(2) 0.3744(3) 1.03593(18) 0.0435(10) Uani 1 1 d . . . C11 C -0.0377(2) 0.3876(3) 1.0065(2) 0.0528(11) Uani 1 1 d . . . H11 H -0.0463 0.3809 0.9653 0.063 Uiso 1 1 calc R . . C12 C -0.0846(2) 0.4110(4) 1.0384(2) 0.0591(12) Uani 1 1 d . . . H12 H -0.1248 0.4218 1.0191 0.071 Uiso 1 1 calc R . . C13 C -0.0708(2) 0.4178(3) 1.0992(2) 0.0588(12) Uani 1 1 d . . . H13 H -0.1019 0.4315 1.1218 0.071 Uiso 1 1 calc R . . C14 C -0.0106(2) 0.4043(3) 1.1265(2) 0.0522(11) Uani 1 1 d . . . H14 H -0.0015 0.4093 1.1677 0.063 Uiso 1 1 calc R . . C15 C 0.2751(3) 0.7076(4) 1.2122(2) 0.0771(17) Uani 1 1 d . . . H15A H 0.2624 0.7170 1.2509 0.093 Uiso 1 1 calc R . . H15B H 0.3117 0.7436 1.2097 0.093 Uiso 1 1 calc R . . C16 C 0.1798(3) 0.7848(4) 1.1731(3) 0.0705(15) Uani 1 1 d . . . H16 H 0.1788 0.8031 1.2121 0.085 Uiso 1 1 calc R . . C17 C 0.1322(3) 0.8174(4) 1.1283(3) 0.0677(14) Uani 1 1 d . . . C18 C 0.0853(4) 0.8712(5) 1.1463(4) 0.100(2) Uani 1 1 d . . . H18 H 0.0856 0.8824 1.1866 0.120 Uiso 1 1 calc R . . C19 C 0.0406(4) 0.9064(6) 1.1065(4) 0.117(3) Uani 1 1 d . . . H19 H 0.0108 0.9426 1.1195 0.141 Uiso 1 1 calc R . . C20 C 0.0376(3) 0.8901(4) 1.0457(4) 0.094(2) Uani 1 1 d . . . H20 H 0.0057 0.9141 1.0184 0.112 Uiso 1 1 calc R . . C21 C 0.0833(2) 0.8373(3) 1.0266(3) 0.0650(14) Uani 1 1 d . . . C22 C 0.1302(2) 0.7986(3) 1.0676(2) 0.0526(11) Uani 1 1 d . . . C23 C 0.0400(3) 0.8479(5) 0.9222(4) 0.100(2) Uani 1 1 d . . . H23A H 0.0489 0.8280 0.8842 0.120 Uiso 1 1 calc R . . H23B H 0.0393 0.9115 0.9229 0.120 Uiso 1 1 calc R . . H23C H 0.0001 0.8255 0.9285 0.120 Uiso 1 1 calc R . . C24 C 0.2894(3) 0.6126(4) 1.2041(2) 0.0699(15) Uani 1 1 d . . . H24A H 0.3298 0.5980 1.2266 0.084 Uiso 1 1 calc R . . H24B H 0.2581 0.5758 1.2183 0.084 Uiso 1 1 calc R . . C25 C 0.3219(2) 0.5328(3) 1.1231(2) 0.0503(11) Uani 1 1 d . . . H25 H 0.3478 0.5019 1.1525 0.060 Uiso 1 1 calc R . . C26 C 0.3213(2) 0.5046(3) 1.0624(2) 0.0467(10) Uani 1 1 d . . . C27 C 0.3607(2) 0.4345(3) 1.0521(2) 0.0607(13) Uani 1 1 d . . . H27 H 0.3857 0.4076 1.0840 0.073 Uiso 1 1 calc R . . C28 C 0.3627(3) 0.4055(3) 0.9956(3) 0.0667(14) Uani 1 1 d . . . H28 H 0.3897 0.3598 0.9892 0.080 Uiso 1 1 calc R . . C29 C 0.3251(2) 0.4434(3) 0.9476(2) 0.0608(13) Uani 1 1 d . . . H29 H 0.3268 0.4229 0.9093 0.073 Uiso 1 1 calc R . . C30 C 0.2848(2) 0.5114(3) 0.9564(2) 0.0494(10) Uani 1 1 d . . . C31 C 0.28213(19) 0.5438(3) 1.01404(19) 0.0416(9) Uani 1 1 d . . . C32 C 0.2421(3) 0.5180(4) 0.8531(2) 0.0796(17) Uani 1 1 d . . . H32A H 0.2127 0.5521 0.8265 0.096 Uiso 1 1 calc R . . H32B H 0.2290 0.4572 0.8523 0.096 Uiso 1 1 calc R . . H32C H 0.2825 0.5219 0.8409 0.096 Uiso 1 1 calc R . . N1 N 0.15384(19) 0.5763(3) 1.10808(18) 0.0575(10) Uani 1 1 d . . . N2 N 0.2762(2) 0.3446(4) 1.1710(3) 0.0960(19) Uani 1 1 d . . . N3 N 0.1127(2) 0.1641(3) 1.1586(2) 0.0726(12) Uani 1 1 d . . . N4 N 0.1059(3) 0.4150(5) 1.2617(2) 0.106(2) Uani 1 1 d . . . N5 N 0.13110(18) 0.3506(2) 1.04054(16) 0.0501(9) Uani 1 1 d . . . N6 N 0.03570(16) 0.3840(2) 1.09566(15) 0.0441(8) Uani 1 1 d . . . N7 N 0.2240(2) 0.7322(3) 1.16426(17) 0.0559(10) Uani 1 1 d . . . N8 N 0.28981(17) 0.5967(2) 1.14029(16) 0.0476(9) Uani 1 1 d . . . O1 O 0.24239(14) 0.60872(19) 1.01932(12) 0.0461(7) Uani 1 1 d . . . O2 O 0.17189(14) 0.7484(2) 1.04580(13) 0.0493(7) Uani 1 1 d . . . O1W O 0.30766(19) 0.7672(3) 1.07735(18) 0.0553(9) Uani 1 1 d . . . O3 O 0.24527(17) 0.5520(2) 0.91227(14) 0.0621(9) Uani 1 1 d . . . O2W O 0.4099(5) 0.3504(13) 0.2002(6) 0.309(9) Uani 1 1 d . . . O4 O 0.08684(16) 0.8165(2) 0.96806(19) 0.0710(10) Uani 1 1 d . . . O3W O 0.4477(8) 0.5520(11) 0.2569(6) 0.317(8) Uani 1 1 d . . . H1A H 0.292(3) 0.812(5) 1.068(3) 0.08(2) Uiso 1 1 d . . . H1B H 0.327(3) 0.752(4) 1.053(3) 0.08(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0376(4) 0.0417(4) 0.0410(4) -0.0015(2) -0.0010(3) 0.0051(3) Cr1 0.0378(4) 0.0539(4) 0.0412(4) 0.0084(3) -0.0034(3) -0.0038(3) C1 0.037(2) 0.062(3) 0.043(2) 0.005(2) -0.0038(18) -0.005(2) C2 0.052(3) 0.078(4) 0.067(3) 0.032(3) -0.001(3) -0.008(3) C3 0.041(3) 0.055(3) 0.054(3) 0.001(2) 0.002(2) 0.001(2) C4 0.058(3) 0.079(3) 0.040(3) 0.003(2) -0.010(2) -0.010(3) C5 0.055(3) 0.064(3) 0.067(3) 0.012(2) 0.014(3) 0.004(2) C6 0.093(5) 0.082(4) 0.079(4) 0.008(3) 0.043(4) 0.011(3) C7 0.098(5) 0.106(5) 0.049(3) -0.001(3) 0.012(3) 0.018(4) C8 0.080(4) 0.090(4) 0.044(3) -0.001(3) 0.002(3) 0.011(3) C9 0.049(3) 0.049(2) 0.043(2) 0.0045(18) -0.002(2) -0.0004(19) C10 0.046(3) 0.041(2) 0.040(2) 0.0044(17) -0.0030(18) -0.0045(18) C11 0.047(3) 0.061(3) 0.045(2) 0.002(2) -0.012(2) -0.003(2) C12 0.034(3) 0.074(3) 0.065(3) 0.007(2) -0.008(2) -0.007(2) C13 0.039(3) 0.074(3) 0.063(3) 0.002(2) 0.007(2) -0.003(2) C14 0.044(3) 0.065(3) 0.046(2) 0.000(2) 0.001(2) -0.001(2) C15 0.093(4) 0.083(4) 0.049(3) -0.017(3) -0.011(3) 0.016(3) C16 0.080(4) 0.068(3) 0.067(3) -0.016(3) 0.022(3) 0.009(3) C17 0.060(3) 0.064(3) 0.081(4) -0.006(3) 0.019(3) 0.016(3) C18 0.086(5) 0.109(5) 0.109(5) -0.015(4) 0.027(4) 0.038(4) C19 0.094(6) 0.129(7) 0.133(7) -0.012(6) 0.031(5) 0.054(5) C20 0.055(4) 0.078(4) 0.143(7) 0.006(4) -0.002(4) 0.028(3) C21 0.043(3) 0.052(3) 0.098(4) 0.006(3) 0.003(3) 0.004(2) C22 0.035(2) 0.043(2) 0.080(3) 0.004(2) 0.008(2) 0.0058(19) C23 0.071(4) 0.086(4) 0.125(6) 0.023(4) -0.046(4) 0.005(3) C24 0.079(4) 0.082(4) 0.042(3) -0.001(2) -0.010(2) 0.016(3) C25 0.044(3) 0.051(3) 0.052(3) 0.007(2) -0.006(2) 0.003(2) C26 0.033(2) 0.050(2) 0.056(3) 0.0030(19) 0.0026(19) 0.0054(18) C27 0.049(3) 0.056(3) 0.075(3) 0.006(2) 0.000(2) 0.015(2) C28 0.058(3) 0.058(3) 0.086(4) -0.006(3) 0.018(3) 0.018(2) C29 0.059(3) 0.062(3) 0.064(3) -0.010(2) 0.018(3) 0.005(2) C30 0.045(3) 0.049(2) 0.054(3) -0.004(2) 0.007(2) 0.000(2) C31 0.032(2) 0.040(2) 0.052(2) -0.0016(18) 0.0045(18) 0.0006(17) C32 0.100(5) 0.087(4) 0.048(3) -0.013(3) 0.000(3) 0.003(3) N1 0.053(2) 0.060(3) 0.056(2) 0.0076(19) 0.0008(19) -0.0078(19) N2 0.044(3) 0.131(5) 0.109(4) 0.058(4) -0.001(3) -0.004(3) N3 0.083(3) 0.061(3) 0.073(3) 0.001(2) 0.009(2) 0.005(2) N4 0.104(5) 0.163(6) 0.048(3) -0.015(3) 0.000(3) -0.013(4) N5 0.053(2) 0.049(2) 0.048(2) 0.0056(16) 0.0082(18) 0.0010(17) N6 0.040(2) 0.048(2) 0.0430(19) 0.0036(15) -0.0004(16) -0.0034(15) N7 0.062(3) 0.053(2) 0.050(2) -0.0087(17) 0.0017(19) 0.0049(19) N8 0.043(2) 0.051(2) 0.045(2) 0.0008(16) -0.0057(16) 0.0060(16) O1 0.0425(17) 0.0508(17) 0.0426(15) -0.0033(12) -0.0013(13) 0.0133(13) O2 0.0401(17) 0.0496(17) 0.0568(18) 0.0040(14) 0.0027(14) 0.0074(13) O1W 0.045(2) 0.057(2) 0.061(2) 0.0050(18) -0.0024(18) -0.0043(16) O3 0.065(2) 0.072(2) 0.0450(18) -0.0101(15) -0.0030(15) 0.0116(17) O2W 0.152(9) 0.54(3) 0.217(11) 0.056(13) -0.010(8) 0.093(12) O4 0.048(2) 0.062(2) 0.095(3) 0.0165(19) -0.0179(19) 0.0089(16) O3W 0.375(18) 0.339(17) 0.229(11) -0.032(11) 0.017(12) 0.208(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.869(3) . ? Mn1 O1 1.886(3) . ? Mn1 N7 1.973(4) . ? Mn1 N8 1.975(4) . ? Mn1 O1W 2.238(4) . ? Mn1 N1 2.309(4) . ? Cr1 C4 2.037(5) . ? Cr1 C2 2.055(6) . ? Cr1 C3 2.069(5) . ? Cr1 N6 2.076(4) . ? Cr1 C1 2.079(5) . ? Cr1 N5 2.083(4) . ? C1 N1 1.140(6) . ? C2 N2 1.148(7) . ? C3 N3 1.136(6) . ? C4 N4 1.120(7) . ? C5 N5 1.344(6) . ? C5 C6 1.370(8) . ? C6 C7 1.361(10) . ? C7 C8 1.381(9) . ? C8 C9 1.377(7) . ? C9 N5 1.349(6) . ? C9 C10 1.471(6) . ? C10 N6 1.352(5) . ? C10 C11 1.379(6) . ? C11 C12 1.383(7) . ? C12 C13 1.372(7) . ? C13 C14 1.373(7) . ? C14 N6 1.343(6) . ? C15 N7 1.478(7) . ? C15 C24 1.485(8) . ? C16 N7 1.284(7) . ? C16 C17 1.424(8) . ? C17 C22 1.403(8) . ? C17 C18 1.409(8) . ? C18 C19 1.332(11) . ? C19 C20 1.393(11) . ? C20 C21 1.391(8) . ? C21 O4 1.380(7) . ? C21 C22 1.398(7) . ? C22 O2 1.331(5) . ? C23 O4 1.423(7) . ? C24 N8 1.470(6) . ? C25 N8 1.285(6) . ? C25 C26 1.441(6) . ? C26 C27 1.403(6) . ? C26 C31 1.413(6) . ? C27 C28 1.362(7) . ? C28 C29 1.383(8) . ? C29 C30 1.382(7) . ? C30 O3 1.362(6) . ? C30 C31 1.407(6) . ? C31 O1 1.323(5) . ? C32 O3 1.430(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 93.09(13) . . ? O2 Mn1 N7 92.07(15) . . ? O1 Mn1 N7 174.84(15) . . ? O2 Mn1 N8 174.17(14) . . ? O1 Mn1 N8 92.50(14) . . ? N7 Mn1 N8 82.33(16) . . ? O2 Mn1 O1W 90.87(15) . . ? O1 Mn1 O1W 92.33(16) . . ? N7 Mn1 O1W 87.71(18) . . ? N8 Mn1 O1W 90.54(16) . . ? O2 Mn1 N1 91.69(14) . . ? O1 Mn1 N1 91.78(15) . . ? N7 Mn1 N1 87.94(17) . . ? N8 Mn1 N1 86.49(16) . . ? O1W Mn1 N1 175.03(14) . . ? C4 Cr1 C2 92.1(2) . . ? C4 Cr1 C3 90.4(2) . . ? C2 Cr1 C3 88.8(2) . . ? C4 Cr1 N6 94.20(18) . . ? C2 Cr1 N6 173.65(19) . . ? C3 Cr1 N6 92.01(16) . . ? C4 Cr1 C1 89.1(2) . . ? C2 Cr1 C1 89.25(19) . . ? C3 Cr1 C1 177.99(18) . . ? N6 Cr1 C1 89.96(15) . . ? C4 Cr1 N5 171.87(19) . . ? C2 Cr1 N5 95.5(2) . . ? C3 Cr1 N5 92.80(17) . . ? N6 Cr1 N5 78.22(15) . . ? C1 Cr1 N5 87.97(16) . . ? N1 C1 Cr1 175.8(4) . . ? N2 C2 Cr1 178.3(5) . . ? N3 C3 Cr1 175.7(4) . . ? N4 C4 Cr1 177.1(6) . . ? N5 C5 C6 122.7(5) . . ? C7 C6 C5 119.0(6) . . ? C6 C7 C8 119.0(5) . . ? C9 C8 C7 119.9(6) . . ? N5 C9 C8 120.8(5) . . ? N5 C9 C10 115.1(4) . . ? C8 C9 C10 124.1(4) . . ? N6 C10 C11 121.3(4) . . ? N6 C10 C9 115.4(4) . . ? C11 C10 C9 123.3(4) . . ? C10 C11 C12 119.6(4) . . ? C13 C12 C11 118.7(5) . . ? C12 C13 C14 119.5(5) . . ? N6 C14 C13 122.2(4) . . ? N7 C15 C24 107.4(4) . . ? N7 C16 C17 125.4(5) . . ? C22 C17 C18 119.0(6) . . ? C22 C17 C16 123.0(4) . . ? C18 C17 C16 118.0(6) . . ? C19 C18 C17 121.1(7) . . ? C18 C19 C20 121.5(7) . . ? C21 C20 C19 118.7(6) . . ? O4 C21 C20 125.2(6) . . ? O4 C21 C22 113.9(4) . . ? C20 C21 C22 120.9(6) . . ? O2 C22 C21 117.2(5) . . ? O2 C22 C17 124.0(4) . . ? C21 C22 C17 118.7(5) . . ? N8 C24 C15 108.2(4) . . ? N8 C25 C26 125.8(4) . . ? C27 C26 C31 119.8(4) . . ? C27 C26 C25 117.7(4) . . ? C31 C26 C25 122.5(4) . . ? C28 C27 C26 120.4(5) . . ? C27 C28 C29 120.7(5) . . ? C30 C29 C28 120.3(5) . . ? O3 C30 C29 124.8(4) . . ? O3 C30 C31 114.7(4) . . ? C29 C30 C31 120.5(4) . . ? O1 C31 C30 117.4(4) . . ? O1 C31 C26 124.3(4) . . ? C30 C31 C26 118.3(4) . . ? C1 N1 Mn1 144.2(4) . . ? C5 N5 C9 118.4(4) . . ? C5 N5 Cr1 126.0(4) . . ? C9 N5 Cr1 115.6(3) . . ? C14 N6 C10 118.7(4) . . ? C14 N6 Cr1 125.7(3) . . ? C10 N6 Cr1 115.5(3) . . ? C16 N7 C15 122.3(4) . . ? C16 N7 Mn1 125.1(4) . . ? C15 N7 Mn1 112.6(3) . . ? C25 N8 C24 120.4(4) . . ? C25 N8 Mn1 125.9(3) . . ? C24 N8 Mn1 113.3(3) . . ? C31 O1 Mn1 128.7(3) . . ? C22 O2 Mn1 127.4(3) . . ? C30 O3 C32 117.7(4) . . ? C21 O4 C23 119.5(5) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.167 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.076 # Attachment '- Crystal2.cif' data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 806214' #TrackingRef '- Crystal2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H54 Cl Cr Mn2 N10 O17' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 293(2) _chemical_formula_weight 1216.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7336(14) _cell_length_b 14.412(4) _cell_length_c 16.884(3) _cell_angle_alpha 69.745(17) _cell_angle_beta 80.807(15) _cell_angle_gamma 82.609(18) _cell_volume 2636.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1254 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30628 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1043 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 6.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11679 _reflns_number_gt 6574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+2.6521P] 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 11679 _refine_ls_number_parameters 719 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.91623(5) 0.16405(4) 0.41916(4) 0.02890(15) Uani 1 1 d . . . Mn2 Mn 0.18699(5) 0.41388(4) 0.99165(4) 0.02741(15) Uani 1 1 d . . . Cr1 Cr 0.46684(5) 0.33048(4) 0.41843(4) 0.03143(16) Uani 1 1 d . . . Cl1 Cl 0.35892(11) 0.05124(10) 0.87869(9) 0.0620(3) Uani 1 1 d . . . N1 N 0.9921(3) 0.2445(2) 0.3074(2) 0.0358(8) Uani 1 1 d . . . N2 N 0.9334(3) 0.2826(2) 0.4489(2) 0.0359(8) Uani 1 1 d . . . N3 N 0.7282(3) 0.2319(2) 0.3916(2) 0.0392(8) Uani 1 1 d . . . N4 N 0.5669(4) 0.5431(3) 0.3512(3) 0.0678(12) Uani 1 1 d . . . N5 N 0.4073(4) 0.3314(3) 0.2385(3) 0.0633(11) Uani 1 1 d . . . N6 N 0.2207(4) 0.4434(3) 0.4535(3) 0.0741(13) Uani 1 1 d . . . N7 N 0.4095(2) 0.1915(2) 0.4905(2) 0.0329(7) Uani 1 1 d . . . N8 N 0.4978(3) 0.3198(2) 0.5397(2) 0.0372(8) Uani 1 1 d . . . H8D H 0.5720 0.2976 0.5466 0.045 Uiso 1 1 calc R . . H8E H 0.4857 0.3802 0.5455 0.045 Uiso 1 1 calc R . . N9 N 0.2341(2) 0.3318(2) 0.91774(19) 0.0303(7) Uani 1 1 d . . . N10 N 0.3234(2) 0.4848(2) 0.92603(19) 0.0311(7) Uani 1 1 d . . . C1 C 1.0414(3) 0.2112(3) 0.2484(3) 0.0367(10) Uani 1 1 d . . . H1 H 1.0818 0.2552 0.2015 0.044 Uiso 1 1 calc R . . C2 C 1.0398(3) 0.1118(3) 0.2484(2) 0.0331(9) Uani 1 1 d . . . C3 C 1.1037(3) 0.0868(4) 0.1794(3) 0.0464(11) Uani 1 1 d . . . H3 H 1.1464 0.1340 0.1367 0.056 Uiso 1 1 calc R . . C4 C 1.1035(4) -0.0049(4) 0.1746(3) 0.0529(12) Uani 1 1 d . . . H4 H 1.1461 -0.0205 0.1288 0.063 Uiso 1 1 calc R . . C5 C 1.0401(4) -0.0757(4) 0.2376(3) 0.0488(11) Uani 1 1 d . . . H5 H 1.0399 -0.1384 0.2334 0.059 Uiso 1 1 calc R . . C6 C 0.9776(3) -0.0547(3) 0.3062(3) 0.0358(9) Uani 1 1 d . . . C7 C 0.9755(3) 0.0409(3) 0.3129(2) 0.0304(9) Uani 1 1 d . . . C8 C 0.8992(4) -0.2141(3) 0.3657(3) 0.0533(12) Uani 1 1 d . . . H8A H 0.8548 -0.2529 0.4166 0.080 Uiso 1 1 calc R . . H8B H 0.9730 -0.2491 0.3578 0.080 Uiso 1 1 calc R . . H8C H 0.8584 -0.2027 0.3178 0.080 Uiso 1 1 calc R . . C9 C 0.9979(4) 0.3486(3) 0.3004(3) 0.0525(12) Uani 1 1 d . . . H9A H 0.9266 0.3873 0.2831 0.063 Uiso 1 1 calc R . . H9B H 1.0617 0.3773 0.2584 0.063 Uiso 1 1 calc R . . C10 C 1.0158(4) 0.3490(3) 0.3866(3) 0.0503(12) Uani 1 1 d . . . H10A H 1.0947 0.3252 0.3979 0.060 Uiso 1 1 calc R . . H10B H 1.0008 0.4156 0.3895 0.060 Uiso 1 1 calc R . . C11 C 0.8767(4) 0.3042(3) 0.5122(3) 0.0395(10) Uani 1 1 d . . . H11 H 0.8850 0.3660 0.5154 0.047 Uiso 1 1 calc R . . C12 C 0.8018(3) 0.2413(3) 0.5783(3) 0.0350(9) Uani 1 1 d . . . C13 C 0.7382(4) 0.2792(3) 0.6405(3) 0.0451(11) Uani 1 1 d . . . H13 H 0.7440 0.3446 0.6362 0.054 Uiso 1 1 calc R . . C013 C 0.7930(3) 0.1422(3) 0.5855(2) 0.0310(9) Uani 1 1 d . . . C14 C 0.6691(4) 0.2215(4) 0.7063(3) 0.0501(12) Uani 1 1 d . . . H14 H 0.6270 0.2477 0.7463 0.060 Uiso 1 1 calc R . . C15 C 0.6608(3) 0.1235(4) 0.7144(3) 0.0460(11) Uani 1 1 d . . . H15 H 0.6132 0.0845 0.7600 0.055 Uiso 1 1 calc R . . C16 C 0.7216(3) 0.0833(3) 0.6560(2) 0.0344(9) Uani 1 1 d . . . C17 C 0.6534(4) -0.0771(4) 0.7294(3) 0.0528(12) Uani 1 1 d . . . H17A H 0.6605 -0.1420 0.7244 0.079 Uiso 1 1 calc R . . H17B H 0.5737 -0.0515 0.7298 0.079 Uiso 1 1 calc R . . H17C H 0.6803 -0.0811 0.7814 0.079 Uiso 1 1 calc R . . C18 C 0.6350(4) 0.2658(3) 0.3985(2) 0.0331(9) Uani 1 1 d . . . C19 C 0.5316(4) 0.4672(3) 0.3705(3) 0.0430(10) Uani 1 1 d . . . C20 C 0.4294(4) 0.3318(3) 0.3020(3) 0.0433(10) Uani 1 1 d . . . C21 C 0.3059(4) 0.4014(3) 0.4398(3) 0.0441(11) Uani 1 1 d . . . C22 C 0.4199(3) 0.2510(3) 0.6054(3) 0.0387(10) Uani 1 1 d . . . H22A H 0.3463 0.2866 0.6161 0.046 Uiso 1 1 calc R . . H22B H 0.4543 0.2239 0.6581 0.046 Uiso 1 1 calc R . . C23 C 0.4012(3) 0.1695(3) 0.5754(3) 0.0333(9) Uani 1 1 d . . . C24 C 0.3716(3) 0.0775(3) 0.6305(3) 0.0432(10) Uani 1 1 d . . . H24 H 0.3669 0.0635 0.6889 0.052 Uiso 1 1 calc R . . C25 C 0.3490(3) 0.0064(3) 0.5987(3) 0.0449(11) Uani 1 1 d . . . H25 H 0.3293 -0.0559 0.6353 0.054 Uiso 1 1 calc R . . C26 C 0.3561(3) 0.0289(3) 0.5129(3) 0.0433(11) Uani 1 1 d . . . H26 H 0.3405 -0.0174 0.4898 0.052 Uiso 1 1 calc R . . C27 C 0.3868(3) 0.1215(3) 0.4612(3) 0.0388(10) Uani 1 1 d . . . H27 H 0.3920 0.1363 0.4027 0.047 Uiso 1 1 calc R . . C28 C 0.1748(3) 0.2663(3) 0.9112(2) 0.0331(9) Uani 1 1 d . . . H28 H 0.2051 0.2362 0.8709 0.040 Uiso 1 1 calc R . . C29 C 0.0667(3) 0.2355(3) 0.9600(2) 0.0319(9) Uani 1 1 d . . . C30 C 0.0179(4) 0.1582(3) 0.9466(3) 0.0428(10) Uani 1 1 d . . . H30 H 0.0547 0.1309 0.9058 0.051 Uiso 1 1 calc R . . C31 C -0.0833(4) 0.1237(3) 0.9936(3) 0.0500(12) Uani 1 1 d . . . H31 H -0.1148 0.0726 0.9847 0.060 Uiso 1 1 calc R . . C32 C -0.1398(3) 0.1638(3) 1.0544(3) 0.0409(10) Uani 1 1 d . . . H32 H -0.2087 0.1396 1.0860 0.049 Uiso 1 1 calc R . . C33 C -0.0940(3) 0.2394(3) 1.0682(2) 0.0304(9) Uani 1 1 d . . . C34 C 0.0117(3) 0.2758(3) 1.0222(2) 0.0265(8) Uani 1 1 d . . . C35 C -0.2388(4) 0.2408(3) 1.1845(3) 0.0505(12) Uani 1 1 d . . . H35A H -0.2653 0.2787 1.2216 0.076 Uiso 1 1 calc R . . H35B H -0.2157 0.1739 1.2175 0.076 Uiso 1 1 calc R . . H35C H -0.3002 0.2404 1.1533 0.076 Uiso 1 1 calc R . . C36 C 0.3479(3) 0.3524(3) 0.8660(3) 0.0404(10) Uani 1 1 d . . . H36A H 0.3499 0.3392 0.8132 0.048 Uiso 1 1 calc R . . H36B H 0.4090 0.3104 0.8968 0.048 Uiso 1 1 calc R . . C37 C 0.3651(4) 0.4610(3) 0.8475(3) 0.0412(10) Uani 1 1 d . . . H37A H 0.4464 0.4726 0.8304 0.049 Uiso 1 1 calc R . . H37B H 0.3218 0.5027 0.8017 0.049 Uiso 1 1 calc R . . C38 C 0.3701(3) 0.5500(3) 0.9436(3) 0.0348(9) Uani 1 1 d . . . H38 H 0.4362 0.5756 0.9085 0.042 Uiso 1 1 calc R . . C39 C 0.3291(3) 0.5864(3) 1.0123(3) 0.0335(9) Uani 1 1 d . . . C40 C 0.3910(3) 0.6586(3) 1.0224(3) 0.0461(11) Uani 1 1 d . . . H40 H 0.4592 0.6773 0.9867 0.055 Uiso 1 1 calc R . . C41 C 0.3537(4) 0.7012(4) 1.0828(3) 0.0532(12) Uani 1 1 d . . . H41 H 0.3954 0.7489 1.0882 0.064 Uiso 1 1 calc R . . C42 C 0.2516(4) 0.6726(3) 1.1372(3) 0.0477(11) Uani 1 1 d . . . H42 H 0.2261 0.7009 1.1794 0.057 Uiso 1 1 calc R . . C43 C 0.1887(3) 0.6032(3) 1.1287(2) 0.0333(9) Uani 1 1 d . . . C44 C 0.2250(3) 0.5593(3) 1.0658(2) 0.0289(8) Uani 1 1 d . . . C45 C 0.0436(4) 0.6143(4) 1.2419(3) 0.0564(13) Uani 1 1 d . . . H45A H -0.0282 0.5872 1.2708 0.085 Uiso 1 1 calc R . . H45B H 0.0310 0.6850 1.2172 0.085 Uiso 1 1 calc R . . H45C H 0.0990 0.5985 1.2817 0.085 Uiso 1 1 calc R . . O1 O 0.8505(2) 0.09857(17) 0.53185(15) 0.0316(6) Uani 1 1 d . . . O2 O 0.9130(2) 0.05725(18) 0.38032(16) 0.0335(6) Uani 1 1 d . . . O3 O 0.7214(2) -0.0127(2) 0.65892(16) 0.0412(7) Uani 1 1 d . . . O4 O 0.9161(2) -0.1207(2) 0.37318(18) 0.0429(7) Uani 1 1 d . . . O5 O 0.05515(19) 0.34402(17) 1.04284(15) 0.0286(6) Uani 1 1 d . . . O6 O 0.15763(19) 0.49671(18) 1.05862(15) 0.0307(6) Uani 1 1 d . . . O7 O -0.1426(2) 0.2841(2) 1.12654(17) 0.0377(6) Uani 1 1 d . . . O8 O 0.0866(2) 0.57296(19) 1.17653(17) 0.0404(7) Uani 1 1 d . . . O9 O 0.4398(6) 0.1156(5) 0.8604(5) 0.198(4) Uani 1 1 d . . . O10 O 0.2716(6) 0.0909(5) 0.8246(3) 0.179(3) Uani 1 1 d . . . O11 O 0.4059(3) -0.0369(3) 0.8635(3) 0.0907(12) Uani 1 1 d . . . O12 O 0.3043(3) 0.0366(3) 0.9613(2) 0.0868(12) Uani 1 1 d . . . O1W O 1.0967(3) 0.1088(3) 0.4537(3) 0.0377(8) Uani 1 1 d . . . O2W O 0.0878(3) 0.5180(3) 0.88740(19) 0.0344(7) Uani 1 1 d . . . O3W O 0.2993(3) 0.3106(3) 1.0925(2) 0.0471(9) Uani 1 1 d . . . O4W O 0.4041(3) 0.1498(2) 1.0503(2) 0.0697(10) Uani 1 1 d . . . O5W O 0.8113(5) 0.5489(5) 0.3713(4) 0.161(2) Uani 1 1 d . . . H3A H 0.323(4) 0.269(3) 1.086(3) 0.034(16) Uiso 1 1 d . . . H2A H 0.035(4) 0.496(3) 0.891(3) 0.044(17) Uiso 1 1 d . . . H1A H 1.124(4) 0.059(4) 0.439(3) 0.069(18) Uiso 1 1 d . . . H2B H 0.077(4) 0.569(4) 0.890(3) 0.059(19) Uiso 1 1 d . . . H1B H 1.092(4) 0.098(3) 0.493(3) 0.033(18) Uiso 1 1 d . . . H3B H 0.326(5) 0.327(5) 1.127(4) 0.10(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0333(3) 0.0265(3) 0.0238(3) -0.0052(2) -0.0007(2) -0.0038(2) Mn2 0.0285(3) 0.0285(3) 0.0255(3) -0.0109(3) 0.0020(2) -0.0045(2) Cr1 0.0330(3) 0.0316(3) 0.0321(4) -0.0133(3) -0.0062(3) -0.0009(3) Cl1 0.0651(8) 0.0590(8) 0.0578(8) -0.0256(7) 0.0110(6) 0.0042(6) N1 0.0384(18) 0.0351(19) 0.0267(19) 0.0004(15) -0.0049(15) -0.0063(15) N2 0.0423(19) 0.0280(18) 0.034(2) -0.0026(15) -0.0096(16) -0.0052(15) N3 0.037(2) 0.044(2) 0.037(2) -0.0162(17) -0.0033(15) -0.0002(16) N4 0.096(3) 0.055(3) 0.057(3) -0.027(2) 0.008(2) -0.024(2) N5 0.096(3) 0.054(3) 0.045(3) -0.014(2) -0.023(2) -0.016(2) N6 0.045(2) 0.076(3) 0.107(4) -0.042(3) -0.011(2) 0.011(2) N7 0.0328(17) 0.0379(19) 0.032(2) -0.0166(16) -0.0061(14) -0.0026(14) N8 0.0338(17) 0.042(2) 0.040(2) -0.0186(17) -0.0040(15) -0.0033(15) N9 0.0334(17) 0.0312(17) 0.0256(18) -0.0119(14) 0.0010(13) 0.0006(14) N10 0.0294(16) 0.0343(18) 0.0276(18) -0.0098(15) 0.0025(13) -0.0041(14) C1 0.033(2) 0.044(2) 0.023(2) 0.0025(19) -0.0041(17) -0.0039(18) C2 0.032(2) 0.040(2) 0.021(2) -0.0026(17) -0.0074(16) 0.0054(17) C3 0.041(2) 0.067(3) 0.023(2) -0.009(2) -0.0020(18) 0.004(2) C4 0.051(3) 0.079(4) 0.028(3) -0.024(3) -0.002(2) 0.009(3) C5 0.050(3) 0.061(3) 0.042(3) -0.027(2) -0.010(2) 0.006(2) C6 0.033(2) 0.046(2) 0.031(2) -0.016(2) -0.0079(17) 0.0025(18) C7 0.0270(19) 0.043(2) 0.023(2) -0.0143(18) -0.0065(16) 0.0052(17) C8 0.057(3) 0.044(3) 0.070(3) -0.032(3) -0.012(2) -0.001(2) C9 0.067(3) 0.034(2) 0.047(3) 0.000(2) -0.003(2) -0.012(2) C10 0.066(3) 0.037(2) 0.047(3) -0.007(2) -0.007(2) -0.020(2) C11 0.052(3) 0.032(2) 0.039(3) -0.013(2) -0.016(2) -0.0004(19) C12 0.037(2) 0.041(2) 0.032(2) -0.0170(19) -0.0114(17) 0.0034(18) C13 0.050(3) 0.047(3) 0.051(3) -0.030(2) -0.019(2) 0.007(2) C013 0.031(2) 0.037(2) 0.025(2) -0.0110(18) -0.0086(16) 0.0042(17) C14 0.045(3) 0.077(4) 0.042(3) -0.041(3) -0.004(2) 0.002(2) C15 0.042(2) 0.064(3) 0.035(3) -0.023(2) 0.0013(19) -0.005(2) C16 0.031(2) 0.048(3) 0.027(2) -0.0150(19) -0.0049(17) -0.0018(18) C17 0.061(3) 0.064(3) 0.027(2) -0.003(2) 0.001(2) -0.023(2) C18 0.043(2) 0.034(2) 0.027(2) -0.0144(18) -0.0047(18) -0.0063(19) C19 0.057(3) 0.040(3) 0.034(3) -0.017(2) -0.001(2) -0.007(2) C20 0.056(3) 0.034(2) 0.040(3) -0.009(2) -0.011(2) -0.007(2) C21 0.039(2) 0.043(3) 0.053(3) -0.018(2) -0.012(2) 0.001(2) C22 0.043(2) 0.046(2) 0.029(2) -0.014(2) -0.0044(18) -0.0042(19) C23 0.029(2) 0.038(2) 0.033(2) -0.0133(19) -0.0039(17) 0.0007(17) C24 0.049(3) 0.047(3) 0.031(2) -0.011(2) -0.0039(19) -0.005(2) C25 0.038(2) 0.038(2) 0.049(3) -0.005(2) 0.001(2) -0.0047(19) C26 0.041(2) 0.037(2) 0.055(3) -0.016(2) -0.010(2) -0.0084(19) C27 0.043(2) 0.045(3) 0.034(2) -0.017(2) -0.0121(19) -0.0002(19) C28 0.042(2) 0.032(2) 0.027(2) -0.0147(18) -0.0049(17) 0.0045(18) C29 0.036(2) 0.030(2) 0.031(2) -0.0119(18) -0.0055(17) -0.0019(17) C30 0.047(3) 0.040(2) 0.049(3) -0.026(2) -0.006(2) -0.001(2) C31 0.053(3) 0.043(3) 0.067(3) -0.031(2) -0.010(2) -0.013(2) C32 0.035(2) 0.038(2) 0.053(3) -0.017(2) -0.0037(19) -0.0089(18) C33 0.034(2) 0.030(2) 0.027(2) -0.0072(17) -0.0110(16) 0.0007(17) C34 0.0304(19) 0.0246(19) 0.024(2) -0.0057(16) -0.0076(15) -0.0013(16) C35 0.044(2) 0.059(3) 0.041(3) -0.010(2) 0.008(2) -0.012(2) C36 0.037(2) 0.044(2) 0.040(3) -0.020(2) 0.0089(18) -0.0025(18) C37 0.042(2) 0.049(3) 0.031(2) -0.017(2) 0.0114(18) -0.0084(19) C38 0.0259(19) 0.038(2) 0.036(2) -0.0074(19) 0.0026(17) -0.0059(17) C39 0.026(2) 0.037(2) 0.037(2) -0.0130(19) -0.0070(17) -0.0001(17) C40 0.033(2) 0.050(3) 0.058(3) -0.017(2) -0.005(2) -0.015(2) C41 0.043(3) 0.059(3) 0.074(4) -0.038(3) -0.008(2) -0.017(2) C42 0.054(3) 0.059(3) 0.045(3) -0.032(2) -0.007(2) -0.012(2) C43 0.038(2) 0.034(2) 0.030(2) -0.0129(18) -0.0069(17) -0.0039(18) C44 0.0281(19) 0.030(2) 0.028(2) -0.0069(17) -0.0100(16) -0.0019(16) C45 0.073(3) 0.055(3) 0.049(3) -0.032(2) 0.011(2) -0.013(2) O1 0.0388(14) 0.0283(14) 0.0241(15) -0.0072(12) 0.0012(11) -0.0008(11) O2 0.0374(14) 0.0358(15) 0.0277(15) -0.0136(12) 0.0031(11) -0.0052(12) O3 0.0503(17) 0.0414(17) 0.0257(15) -0.0056(13) 0.0052(12) -0.0103(13) O4 0.0495(17) 0.0407(17) 0.0430(18) -0.0206(14) 0.0008(13) -0.0083(13) O5 0.0339(14) 0.0287(14) 0.0257(14) -0.0122(11) 0.0011(11) -0.0085(11) O6 0.0300(13) 0.0342(14) 0.0323(15) -0.0172(12) 0.0009(11) -0.0074(11) O7 0.0344(14) 0.0453(16) 0.0333(16) -0.0152(13) 0.0061(12) -0.0095(12) O8 0.0470(16) 0.0416(16) 0.0376(17) -0.0222(14) 0.0071(13) -0.0114(13) O9 0.209(6) 0.166(5) 0.245(7) -0.143(5) 0.170(6) -0.137(5) O10 0.236(7) 0.215(6) 0.102(4) -0.103(4) -0.092(4) 0.158(6) O11 0.093(3) 0.069(2) 0.124(4) -0.056(3) -0.022(2) 0.024(2) O12 0.089(3) 0.114(3) 0.055(2) -0.029(2) 0.016(2) -0.030(2) O1W 0.0379(17) 0.041(2) 0.030(2) -0.0082(17) -0.0036(15) 0.0006(14) O2W 0.0329(18) 0.0337(19) 0.0369(18) -0.0116(15) -0.0058(13) -0.0020(15) O3W 0.057(2) 0.041(2) 0.045(2) -0.0173(17) -0.0188(16) 0.0106(18) O4W 0.090(3) 0.060(2) 0.063(2) -0.0290(18) -0.0202(19) 0.0209(19) O5W 0.108(4) 0.211(6) 0.162(5) -0.080(5) 0.029(4) -0.012(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 Mn1 O2 1.877(3) . ? Mn1 O1 1.892(2) . ? Mn1 N1 1.977(3) . ? Mn1 N2 1.982(3) . ? Mn1 O1W 2.258(3) . ? Mn1 N3 2.345(3) . ? Mn2 O5 1.877(2) . ? Mn2 O6 1.878(2) . ? Mn2 N9 1.974(3) . ? Mn2 N10 1.976(3) . ? Mn2 O2W 2.254(3) . ? Mn2 O3W 2.304(3) . ? Cr1 C19 2.049(5) . ? Cr1 C21 2.069(5) . ? Cr1 C20 2.076(5) . ? Cr1 N7 2.084(3) . ? Cr1 N8 2.087(3) . ? Cr1 C18 2.100(4) . ? Cl1 O9 1.339(5) . ? Cl1 O12 1.395(4) . ? Cl1 O11 1.409(4) . ? Cl1 O10 1.414(5) . ? N1 C1 1.277(5) . ? N1 C9 1.474(5) . ? N2 C11 1.277(5) . ? N2 C10 1.474(5) . ? N3 C18 1.144(5) . ? N4 C19 1.141(5) . ? N5 C20 1.144(5) . ? N6 C21 1.134(5) . ? N7 C27 1.338(5) . ? N7 C23 1.346(5) . ? N8 C22 1.482(5) . ? N9 C28 1.285(5) . ? N9 C36 1.478(5) . ? N10 C38 1.283(5) . ? N10 C37 1.476(5) . ? C1 C2 1.436(6) . ? C2 C7 1.402(5) . ? C2 C3 1.411(5) . ? C3 C4 1.353(6) . ? C4 C5 1.385(6) . ? C5 C6 1.373(5) . ? C6 O4 1.370(5) . ? C6 C7 1.417(5) . ? C7 O2 1.328(4) . ? C8 O4 1.436(5) . ? C9 C10 1.505(6) . ? C11 C12 1.425(6) . ? C12 C013 1.407(5) . ? C12 C13 1.416(5) . ? C13 C14 1.352(6) . ? C013 O1 1.326(4) . ? C013 C16 1.416(5) . ? C14 C15 1.386(6) . ? C15 C16 1.372(5) . ? C16 O3 1.367(5) . ? C17 O3 1.427(5) . ? C22 C23 1.483(5) . ? C23 C24 1.380(5) . ? C24 C25 1.380(6) . ? C25 C26 1.361(6) . ? C26 C27 1.375(6) . ? C28 C29 1.429(5) . ? C29 C34 1.402(5) . ? C29 C30 1.414(5) . ? C30 C31 1.366(6) . ? C31 C32 1.386(6) . ? C32 C33 1.377(5) . ? C33 O7 1.369(4) . ? C33 C34 1.413(5) . ? C34 O5 1.330(4) . ? C35 O7 1.424(4) . ? C36 C37 1.520(5) . ? C38 C39 1.424(5) . ? C39 C44 1.410(5) . ? C39 C40 1.413(5) . ? C40 C41 1.352(6) . ? C41 C42 1.401(6) . ? C42 C43 1.375(5) . ? C43 O8 1.363(4) . ? C43 C44 1.400(5) . ? C44 O6 1.321(4) . ? C45 O8 1.424(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O1 95.47(11) . . ? O2 Mn1 N1 91.58(13) . . ? O1 Mn1 N1 172.55(13) . . ? O2 Mn1 N2 173.41(12) . . ? O1 Mn1 N2 90.70(12) . . ? N1 Mn1 N2 82.16(14) . . ? O2 Mn1 O1W 90.09(13) . . ? O1 Mn1 O1W 91.25(13) . . ? N1 Mn1 O1W 86.34(13) . . ? N2 Mn1 O1W 87.46(14) . . ? O2 Mn1 N3 95.53(11) . . ? O1 Mn1 N3 86.80(11) . . ? N1 Mn1 N3 94.91(12) . . ? N2 Mn1 N3 87.10(12) . . ? O1W Mn1 N3 174.20(14) . . ? O5 Mn2 O6 94.04(10) . . ? O5 Mn2 N9 91.74(12) . . ? O6 Mn2 N9 174.06(12) . . ? O5 Mn2 N10 173.62(12) . . ? O6 Mn2 N10 91.39(12) . . ? N9 Mn2 N10 82.92(13) . . ? O5 Mn2 O2W 90.58(13) . . ? O6 Mn2 O2W 94.03(12) . . ? N9 Mn2 O2W 87.27(13) . . ? N10 Mn2 O2W 85.69(13) . . ? O5 Mn2 O3W 92.92(12) . . ? O6 Mn2 O3W 86.98(14) . . ? N9 Mn2 O3W 91.37(15) . . ? N10 Mn2 O3W 90.71(13) . . ? O2W Mn2 O3W 176.29(13) . . ? C19 Cr1 C21 87.90(17) . . ? C19 Cr1 C20 94.65(16) . . ? C21 Cr1 C20 90.66(17) . . ? C19 Cr1 N7 168.35(15) . . ? C21 Cr1 N7 92.20(15) . . ? C20 Cr1 N7 97.00(14) . . ? C19 Cr1 N8 89.52(15) . . ? C21 Cr1 N8 88.80(15) . . ? C20 Cr1 N8 175.78(14) . . ? N7 Cr1 N8 78.84(13) . . ? C19 Cr1 C18 88.93(16) . . ? C21 Cr1 C18 176.18(16) . . ? C20 Cr1 C18 91.71(16) . . ? N7 Cr1 C18 90.48(13) . . ? N8 Cr1 C18 89.05(14) . . ? O9 Cl1 O12 109.5(3) . . ? O9 Cl1 O11 111.1(3) . . ? O12 Cl1 O11 114.0(3) . . ? O9 Cl1 O10 110.2(5) . . ? O12 Cl1 O10 106.2(3) . . ? O11 Cl1 O10 105.6(3) . . ? C1 N1 C9 121.1(3) . . ? C1 N1 Mn1 125.5(3) . . ? C9 N1 Mn1 113.1(3) . . ? C11 N2 C10 121.9(3) . . ? C11 N2 Mn1 125.3(3) . . ? C10 N2 Mn1 112.7(3) . . ? C18 N3 Mn1 162.6(3) . . ? C27 N7 C23 117.7(3) . . ? C27 N7 Cr1 126.9(3) . . ? C23 N7 Cr1 115.3(2) . . ? C22 N8 Cr1 110.2(2) . . ? C28 N9 C36 120.2(3) . . ? C28 N9 Mn2 126.0(3) . . ? C36 N9 Mn2 113.8(2) . . ? C38 N10 C37 120.9(3) . . ? C38 N10 Mn2 126.2(3) . . ? C37 N10 Mn2 112.8(2) . . ? N1 C1 C2 125.6(4) . . ? C7 C2 C3 119.8(4) . . ? C7 C2 C1 122.3(4) . . ? C3 C2 C1 117.9(4) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 120.2(4) . . ? C6 C5 C4 120.9(4) . . ? O4 C6 C5 125.2(4) . . ? O4 C6 C7 114.4(3) . . ? C5 C6 C7 120.4(4) . . ? O2 C7 C2 124.2(3) . . ? O2 C7 C6 117.8(3) . . ? C2 C7 C6 118.0(3) . . ? N1 C9 C10 107.3(3) . . ? N2 C10 C9 106.4(3) . . ? N2 C11 C12 125.4(4) . . ? C013 C12 C13 119.3(4) . . ? C013 C12 C11 122.2(4) . . ? C13 C12 C11 118.4(4) . . ? C14 C13 C12 120.7(4) . . ? O1 C013 C12 124.3(3) . . ? O1 C013 C16 117.2(3) . . ? C12 C013 C16 118.4(4) . . ? C13 C14 C15 120.4(4) . . ? C16 C15 C14 120.9(4) . . ? O3 C16 C15 125.6(4) . . ? O3 C16 C013 114.2(3) . . ? C15 C16 C013 120.2(4) . . ? N3 C18 Cr1 176.0(3) . . ? N4 C19 Cr1 173.8(4) . . ? N5 C20 Cr1 178.8(4) . . ? N6 C21 Cr1 176.0(4) . . ? N8 C22 C23 109.4(3) . . ? N7 C23 C24 121.3(4) . . ? N7 C23 C22 116.1(3) . . ? C24 C23 C22 122.6(4) . . ? C25 C24 C23 119.9(4) . . ? C26 C25 C24 119.0(4) . . ? C25 C26 C27 118.5(4) . . ? N7 C27 C26 123.6(4) . . ? N9 C28 C29 126.1(4) . . ? C34 C29 C30 119.9(4) . . ? C34 C29 C28 122.4(3) . . ? C30 C29 C28 117.6(4) . . ? C31 C30 C29 120.0(4) . . ? C30 C31 C32 120.9(4) . . ? C33 C32 C31 120.1(4) . . ? O7 C33 C32 124.8(3) . . ? O7 C33 C34 114.3(3) . . ? C32 C33 C34 120.8(4) . . ? O5 C34 C29 123.9(3) . . ? O5 C34 C33 117.7(3) . . ? C29 C34 C33 118.3(3) . . ? N9 C36 C37 107.7(3) . . ? N10 C37 C36 107.7(3) . . ? N10 C38 C39 125.5(3) . . ? C44 C39 C40 118.9(4) . . ? C44 C39 C38 122.7(3) . . ? C40 C39 C38 118.2(4) . . ? C41 C40 C39 121.7(4) . . ? C40 C41 C42 119.3(4) . . ? C43 C42 C41 120.6(4) . . ? O8 C43 C42 125.0(4) . . ? O8 C43 C44 114.1(3) . . ? C42 C43 C44 120.9(4) . . ? O6 C44 C43 117.7(3) . . ? O6 C44 C39 123.7(3) . . ? C43 C44 C39 118.5(3) . . ? C013 O1 Mn1 125.9(2) . . ? C7 O2 Mn1 127.8(2) . . ? C16 O3 C17 117.3(3) . . ? C6 O4 C8 118.0(3) . . ? C34 O5 Mn2 129.3(2) . . ? C44 O6 Mn2 129.1(2) . . ? C33 O7 C35 117.3(3) . . ? C43 O8 C45 117.5(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.694 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.076 # Attachment '- Crystal3.cif' data_max64 _database_code_depnum_ccdc_archive 'CCDC 806215' #TrackingRef '- Crystal3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Fe Mn N10 O8' _chemical_formula_weight 823.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8545(6) _cell_length_b 15.3334(4) _cell_length_c 20.9626(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.016(4) _cell_angle_gamma 90.00 _cell_volume 3763.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24617 _cell_measurement_theta_min 4.38 _cell_measurement_theta_max 67.25 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 0.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Stoe-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33773 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0616 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8162 _reflns_number_gt 5798 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0341P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8162 _refine_ls_number_parameters 538 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 O2W O 0.8417(4) 0.0025(3) 0.46785(17) 0.0963(12) Uani 1 1 d D . . O3W O 0.5124(4) 0.3619(2) -0.01566(16) 0.0943(11) Uani 1 1 d D . . O4W O 0.3726(6) 0.2725(4) -0.1310(3) 0.173(2) Uani 1 1 d . . . C11 C 0.8826(3) 0.16568(16) 0.05924(12) 0.0299(6) Uani 1 1 d . . . C3 C 0.9120(3) -0.18019(16) 0.05044(12) 0.0296(6) Uani 1 1 d . . . C2 C 0.9603(3) -0.22329(16) 0.10729(13) 0.0366(7) Uani 1 1 d . . . C10 C 0.9294(3) 0.20655(17) 0.11759(12) 0.0346(6) Uani 1 1 d . . . C24 C 0.5022(3) 0.13628(18) 0.08821(12) 0.0343(6) Uani 1 1 d . . . C12 C 0.8327(3) 0.21874(17) 0.00718(12) 0.0361(7) Uani 1 1 d . . . C1 C 1.0110(3) -0.17696(18) 0.16470(12) 0.0392(7) Uani 1 1 d . . . H016 H 1.0440 -0.2105 0.1997 0.047 Uiso 1 1 calc R . . C18 C 0.6485(3) 0.01841(18) 0.28571(13) 0.0387(7) Uani 1 1 d . . . C22 C 0.3602(3) 0.0313(2) 0.01349(13) 0.0438(7) Uani 1 1 d . . . H019 H 0.3104 -0.0049 -0.0131 0.053 Uiso 1 1 calc R . . C4 C 0.8653(3) -0.23090(17) -0.00376(13) 0.0357(6) Uani 1 1 d . . . C25 C 0.5778(3) 0.19278(18) 0.13335(13) 0.0376(7) Uani 1 1 d . . . C9 C 0.9792(3) 0.15842(18) 0.17404(12) 0.0378(7) Uani 1 1 d . . . H023 H 1.0052 0.1905 0.2111 0.045 Uiso 1 1 calc R . . C21 C 0.4088(3) 0.0050(2) 0.07426(12) 0.0373(6) Uani 1 1 d . . . H024 H 0.3910 -0.0495 0.0893 0.045 Uiso 1 1 calc R . . C19 C 0.5104(3) -0.0830(2) 0.20813(13) 0.0440(8) Uani 1 1 d . . . C17 C 0.6956(3) -0.00838(19) 0.16640(11) 0.0355(6) Uani 1 1 d . . . C15 C 0.9283(3) 0.29834(19) 0.12202(14) 0.0480(8) Uani 1 1 d . . . H029 H 0.9607 0.3254 0.1602 0.058 Uiso 1 1 calc R . . C20 C 0.4316(3) 0.0804(2) 0.23544(13) 0.0437(7) Uani 1 1 d . . . C7 C 0.9603(4) -0.31502(19) 0.10886(16) 0.0553(10) Uani 1 1 d . . . H032 H 0.9932 -0.3438 0.1462 0.066 Uiso 1 1 calc R . . C8 C 0.7683(3) -0.2281(2) -0.11263(15) 0.0520(9) Uani 1 1 d . . . H03C H 0.7426 -0.1872 -0.1465 0.078 Uiso 1 1 calc R . . H03D H 0.7042 -0.2600 -0.1020 0.078 Uiso 1 1 calc R . . H03E H 0.8217 -0.2679 -0.1269 0.078 Uiso 1 1 calc R . . C28 C 0.6843(3) 0.2046(2) 0.23427(15) 0.0467(8) Uani 1 1 d . . . H034 H 0.7132 0.1817 0.2746 0.056 Uiso 1 1 calc R . . C5 C 0.8644(4) -0.3200(2) -0.00020(16) 0.0561(10) Uani 1 1 d . . . H035 H 0.8313 -0.3526 -0.0356 0.067 Uiso 1 1 calc R . . C16 C 0.7336(4) 0.2232(2) -0.10110(15) 0.0580(10) Uani 1 1 d . . . H03F H 0.7066 0.1847 -0.1364 0.087 Uiso 1 1 calc R . . H03G H 0.7869 0.2640 -0.1143 0.087 Uiso 1 1 calc R . . H03H H 0.6702 0.2543 -0.0887 0.087 Uiso 1 1 calc R . . C23 C 0.3875(3) 0.1128(2) -0.00678(14) 0.0461(8) Uani 1 1 d . . . H039 H 0.3550 0.1314 -0.0478 0.055 Uiso 1 1 calc R . . C13 C 0.8311(3) 0.30785(19) 0.01315(15) 0.0494(9) Uani 1 1 d . . . H040 H 0.7972 0.3419 -0.0213 0.059 Uiso 1 1 calc R . . C14 C 0.8803(4) 0.3477(2) 0.07082(16) 0.0575(10) Uani 1 1 d . . . H041 H 0.8803 0.4081 0.0743 0.069 Uiso 1 1 calc R . . C27 C 0.7108(4) 0.2883(2) 0.21950(18) 0.0594(10) Uani 1 1 d . . . H046 H 0.7575 0.3226 0.2493 0.071 Uiso 1 1 calc R . . C26 C 0.6670(4) 0.3203(2) 0.15964(19) 0.0613(10) Uani 1 1 d . . . H047 H 0.6845 0.3772 0.1493 0.074 Uiso 1 1 calc R . . C6 C 0.9131(4) -0.3620(2) 0.05661(17) 0.0657(12) Uani 1 1 d . . . H048 H 0.9132 -0.4226 0.0586 0.079 Uiso 1 1 calc R . . Fe1 Fe 0.56293(4) 0.03394(2) 0.201322(16) 0.02982(10) Uani 1 1 d . . . Mn1 Mn 0.94531(4) -0.00841(2) 0.106736(16) 0.02605(10) Uani 1 1 d . . . N1 N 1.0146(2) -0.09426(14) 0.17183(10) 0.0376(6) Uani 1 1 d . . . N2 N 0.9909(2) 0.07555(14) 0.17791(10) 0.0360(6) Uani 1 1 d . . . N8 N 0.6165(2) 0.15514(15) 0.19079(10) 0.0349(5) Uani 1 1 d . . . N7 N 0.4820(2) 0.05720(14) 0.11226(10) 0.0314(5) Uani 1 1 d . . . N3 N 0.7751(2) -0.02745(19) 0.14514(11) 0.0499(7) Uani 1 1 d . . . N4 N 0.7052(3) 0.01199(17) 0.33507(11) 0.0546(8) Uani 1 1 d . . . N6 N 0.3561(3) 0.1143(3) 0.25243(15) 0.0753(10) Uani 1 1 d . . . N5 N 0.4817(3) -0.1538(2) 0.21190(15) 0.0725(11) Uani 1 1 d . . . N9 N 0.4591(2) 0.16653(17) 0.03026(11) 0.0450(6) Uani 1 1 d . . . N10 N 0.6002(3) 0.27261(17) 0.11562(13) 0.0522(7) Uani 1 1 d . . . O1 O 0.90753(18) -0.09422(11) 0.04339(8) 0.0324(4) Uani 1 1 d . . . O2 O 0.88275(18) 0.08008(11) 0.04972(8) 0.0347(5) Uani 1 1 d . . . O1W O 1.12186(18) 0.00263(14) 0.07888(9) 0.0372(4) Uani 1 1 d D . . O3 O 0.8227(2) -0.18233(12) -0.05696(9) 0.0423(5) Uani 1 1 d . . . O4 O 0.7889(2) 0.17329(12) -0.04738(9) 0.0458(6) Uani 1 1 d . . . C39A C 1.1343(6) 0.0306(3) 0.35290(16) 0.100(2) Uani 0.36 1 d P A 1 H39A H 1.2166 0.0338 0.3559 0.120 Uiso 0.36 1 calc PR A 1 H39B H 1.1150 0.0587 0.3912 0.120 Uiso 0.36 1 calc PR A 1 C40A C 1.0834(3) 0.0855(2) 0.29561(13) 0.0499(9) Uani 0.36 1 d P A 1 H40A H 1.1294 0.1375 0.2937 0.060 Uiso 0.36 1 calc PR A 1 H40B H 1.0070 0.1037 0.3009 0.060 Uiso 0.36 1 calc PR A 1 C41A C 1.1168(4) -0.1057(2) 0.28846(15) 0.0708(14) Uani 0.36 1 d P A 1 H41A H 1.1920 -0.0982 0.2765 0.085 Uiso 0.36 1 calc PR A 1 H41B H 1.0999 -0.1674 0.2907 0.085 Uiso 0.36 1 calc PR A 1 C42A C 1.0218(8) -0.0559(5) 0.2404(3) 0.0297(17) Uani 0.36 1 d P A 1 H42A H 0.9479 -0.0520 0.2557 0.036 Uiso 0.36 1 calc PR A 1 C44A C 1.1063(13) -0.0558(7) 0.3563(4) 0.054(3) Uani 0.36 1 d P A 1 H44A H 1.0287 -0.0610 0.3653 0.065 Uiso 0.36 1 calc PR A 1 H44B H 1.1569 -0.0833 0.3914 0.065 Uiso 0.36 1 calc PR A 1 C43A C 1.0780(9) 0.0341(7) 0.2320(5) 0.032(2) Uani 0.36 1 d P A 1 H43A H 1.1536 0.0279 0.2191 0.038 Uiso 0.36 1 calc PR A 1 C39B C 1.1343(6) 0.0306(3) 0.35290(16) 0.100(2) Uani 0.64 1 d P A 2 H39C H 1.1891 0.0664 0.3806 0.120 Uiso 0.64 1 calc PR A 2 H39D H 1.0736 0.0163 0.3772 0.120 Uiso 0.64 1 calc PR A 2 C40B C 1.0834(3) 0.0855(2) 0.29561(13) 0.0499(9) Uani 0.64 1 d P A 2 H40C H 1.1438 0.1177 0.2798 0.060 Uiso 0.64 1 calc PR A 2 H40D H 1.0306 0.1275 0.3092 0.060 Uiso 0.64 1 calc PR A 2 C41B C 1.1168(4) -0.1057(2) 0.28846(15) 0.0708(14) Uani 0.64 1 d P A 2 H41C H 1.1601 -0.1570 0.2802 0.085 Uiso 0.64 1 calc PR A 2 H41D H 1.0466 -0.1241 0.3028 0.085 Uiso 0.64 1 calc PR A 2 C43B C 1.0205(6) 0.0294(4) 0.2412(3) 0.0410(13) Uani 0.64 1 d P A 2 H43B H 0.9498 0.0081 0.2545 0.049 Uiso 0.64 1 calc PR A 2 C42B C 1.0904(6) -0.0483(3) 0.2265(2) 0.0411(12) Uani 0.64 1 d P A 2 H42B H 1.1615 -0.0291 0.2125 0.049 Uiso 0.64 1 calc PR A 2 C44B C 1.1883(10) -0.0466(5) 0.3405(3) 0.091(3) Uani 0.64 1 d P A 2 H44C H 1.2057 -0.0793 0.3804 0.109 Uiso 0.64 1 calc PR A 2 H44D H 1.2602 -0.0325 0.3262 0.109 Uiso 0.64 1 calc PR A 2 H1W H 1.131(4) -0.041(2) 0.0536(17) 0.077(13) Uiso 1 1 d D . . H2W H 1.128(4) 0.0485(18) 0.0554(17) 0.073(13) Uiso 1 1 d D . . H3W H 0.877(5) 0.050(4) 0.474(3) 0.11(2) Uiso 1 1 d . . . H4W H 0.814(6) 0.011(4) 0.4260(13) 0.14(2) Uiso 1 1 d D . . H5W H 0.554(5) 0.404(3) 0.007(3) 0.12(2) Uiso 1 1 d D . . H6W H 0.519(8) 0.314(3) 0.010(3) 0.19(3) 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 O2W 0.103(3) 0.086(2) 0.084(2) 0.0035(18) -0.032(2) -0.007(2) O3W 0.118(3) 0.075(2) 0.080(2) 0.0258(18) -0.013(2) 0.003(2) O4W 0.180(6) 0.181(5) 0.143(4) 0.006(3) -0.025(4) -0.008(4) C11 0.0335(17) 0.0252(13) 0.0303(12) 0.0003(9) 0.0033(11) 0.0020(11) C3 0.0330(17) 0.0265(13) 0.0299(12) 0.0014(9) 0.0066(11) -0.0028(11) C2 0.049(2) 0.0258(13) 0.0345(13) 0.0027(11) 0.0036(12) -0.0035(13) C10 0.0452(19) 0.0269(13) 0.0314(13) -0.0023(10) 0.0056(12) 0.0010(12) C24 0.0310(17) 0.0397(15) 0.0320(12) 0.0030(11) 0.0044(12) 0.0002(12) C12 0.0419(19) 0.0307(14) 0.0329(12) 0.0013(10) -0.0023(12) 0.0049(12) C1 0.054(2) 0.0344(15) 0.0264(12) 0.0076(10) -0.0016(12) 0.0040(13) C18 0.0436(19) 0.0357(16) 0.0357(13) -0.0022(11) 0.0030(13) 0.0015(13) C22 0.0289(17) 0.065(2) 0.0349(13) -0.0042(13) -0.0037(12) -0.0014(15) C4 0.0411(19) 0.0298(14) 0.0334(13) -0.0011(10) -0.0027(12) -0.0052(12) C25 0.0360(18) 0.0374(15) 0.0391(14) 0.0041(11) 0.0049(13) -0.0015(13) C9 0.047(2) 0.0375(16) 0.0264(12) -0.0073(10) -0.0017(12) 0.0027(13) C21 0.0328(17) 0.0423(16) 0.0355(12) -0.0012(11) 0.0009(11) -0.0050(13) C19 0.047(2) 0.0490(19) 0.0314(13) 0.0077(12) -0.0070(13) -0.0104(15) C17 0.0344(17) 0.0447(16) 0.0261(11) -0.0002(11) 0.0005(11) -0.0033(13) C15 0.069(3) 0.0339(15) 0.0392(15) -0.0104(11) 0.0029(15) 0.0040(15) C20 0.0358(19) 0.066(2) 0.0292(13) -0.0022(12) 0.0045(13) -0.0003(16) C7 0.082(3) 0.0342(16) 0.0453(16) 0.0106(13) -0.0029(17) -0.0023(17) C8 0.058(2) 0.0483(18) 0.0418(15) -0.0128(13) -0.0154(15) -0.0024(16) C28 0.049(2) 0.0467(18) 0.0414(15) -0.0055(13) -0.0036(14) -0.0067(15) C5 0.082(3) 0.0331(16) 0.0466(16) -0.0073(13) -0.0094(17) -0.0095(17) C16 0.064(3) 0.056(2) 0.0447(17) 0.0140(14) -0.0190(17) 0.0037(18) C23 0.042(2) 0.061(2) 0.0317(13) 0.0053(13) -0.0049(13) 0.0023(16) C13 0.068(3) 0.0336(16) 0.0435(16) 0.0052(12) -0.0002(16) 0.0099(15) C14 0.089(3) 0.0268(15) 0.0540(18) -0.0029(13) 0.0016(19) 0.0070(17) C27 0.060(3) 0.049(2) 0.064(2) -0.0094(16) -0.0061(19) -0.0175(18) C26 0.069(3) 0.0379(18) 0.074(2) 0.0027(16) 0.004(2) -0.0133(17) C6 0.107(4) 0.0225(15) 0.061(2) 0.0026(13) -0.007(2) -0.0104(18) Fe1 0.0284(2) 0.0356(2) 0.02428(16) 0.00084(14) 0.00064(14) -0.00299(17) Mn1 0.0325(2) 0.02426(19) 0.01988(15) -0.00038(14) -0.00072(14) 0.00161(17) N1 0.0538(18) 0.0309(12) 0.0247(10) 0.0000(8) -0.0051(10) 0.0036(11) N2 0.0511(17) 0.0304(12) 0.0226(9) -0.0014(8) -0.0062(10) 0.0016(11) N8 0.0335(15) 0.0363(12) 0.0332(11) -0.0019(9) -0.0002(10) -0.0047(10) N7 0.0272(13) 0.0385(12) 0.0278(10) 0.0017(8) 0.0023(9) -0.0026(10) N3 0.0387(17) 0.0734(19) 0.0374(12) -0.0002(12) 0.0056(12) 0.0017(14) N4 0.071(2) 0.0483(16) 0.0374(12) 0.0005(11) -0.0133(13) 0.0067(14) N6 0.052(2) 0.123(3) 0.0513(17) -0.0051(18) 0.0106(16) 0.017(2) N5 0.090(3) 0.0554(19) 0.0608(18) 0.0148(14) -0.0244(18) -0.0281(18) N9 0.0462(18) 0.0500(15) 0.0359(12) 0.0091(10) -0.0029(12) 0.0009(13) N10 0.059(2) 0.0383(15) 0.0572(15) 0.0064(12) 0.0022(14) -0.0093(13) O1 0.0465(13) 0.0238(9) 0.0253(8) -0.0008(6) 0.0001(8) -0.0015(8) O2 0.0475(13) 0.0252(9) 0.0273(8) -0.0006(7) -0.0072(8) 0.0031(8) O1W 0.0399(12) 0.0404(11) 0.0315(8) 0.0005(9) 0.0064(8) -0.0023(10) O3 0.0571(16) 0.0312(10) 0.0332(9) -0.0049(7) -0.0097(9) -0.0018(9) O4 0.0597(16) 0.0341(11) 0.0362(10) 0.0030(8) -0.0151(10) 0.0013(10) C39A 0.183(6) 0.066(3) 0.0325(16) -0.0064(16) -0.038(2) 0.016(3) C40A 0.073(3) 0.0433(17) 0.0275(13) -0.0052(11) -0.0107(14) -0.0017(16) C41A 0.122(4) 0.0404(18) 0.0360(15) 0.0037(13) -0.032(2) 0.010(2) C42A 0.029(5) 0.038(5) 0.020(3) -0.001(3) -0.002(3) 0.000(4) C44A 0.080(9) 0.049(6) 0.027(4) 0.008(3) -0.009(5) -0.012(6) C43A 0.028(6) 0.035(5) 0.028(4) -0.002(3) -0.007(4) -0.004(5) C39B 0.183(6) 0.066(3) 0.0325(16) -0.0064(16) -0.038(2) 0.016(3) C40B 0.073(3) 0.0433(17) 0.0275(13) -0.0052(11) -0.0107(14) -0.0017(16) C41B 0.122(4) 0.0404(18) 0.0360(15) 0.0037(13) -0.032(2) 0.010(2) C43B 0.052(4) 0.042(3) 0.025(2) 0.0001(19) -0.008(3) 0.001(3) C42B 0.053(4) 0.037(3) 0.028(2) 0.0023(18) -0.009(2) 0.002(3) C44B 0.145(9) 0.054(4) 0.053(4) 0.002(3) -0.052(5) 0.012(5) _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 O2W H3W 0.85(6) . ? O2W H4W 0.90(2) . ? O3W H5W 0.90(2) . ? O3W H6W 0.90(2) . ? C11 O2 1.328(3) . ? C11 C10 1.409(4) . ? C11 C12 1.414(4) . ? C3 O1 1.326(3) . ? C3 C2 1.404(4) . ? C3 C4 1.416(4) . ? C2 C7 1.407(4) . ? C2 C1 1.445(4) . ? C10 C15 1.411(4) . ? C10 C9 1.440(4) . ? C24 N9 1.326(3) . ? C24 N7 1.349(3) . ? C24 C25 1.478(4) . ? C12 O4 1.370(3) . ? C12 C13 1.372(4) . ? C1 N1 1.277(3) . ? C1 H016 0.9300 . ? C18 N4 1.146(4) . ? C18 Fe1 1.911(3) . ? C22 C21 1.374(4) . ? C22 C23 1.375(5) . ? C22 H019 0.9300 . ? C4 C5 1.368(4) . ? C4 O3 1.370(3) . ? C25 N10 1.318(4) . ? C25 N8 1.349(3) . ? C9 N2 1.279(3) . ? C9 H023 0.9300 . ? C21 N7 1.345(3) . ? C21 H024 0.9300 . ? C19 N5 1.144(4) . ? C19 Fe1 1.911(3) . ? C17 N3 1.142(4) . ? C17 Fe1 1.947(3) . ? C15 C14 1.363(4) . ? C15 H029 0.9300 . ? C20 N6 1.140(4) . ? C20 Fe1 1.947(3) . ? C7 C6 1.357(5) . ? C7 H032 0.9300 . ? C8 O3 1.426(3) . ? C8 H03C 0.9600 . ? C8 H03D 0.9600 . ? C8 H03E 0.9600 . ? C28 N8 1.350(4) . ? C28 C27 1.368(5) . ? C28 H034 0.9300 . ? C5 C6 1.397(5) . ? C5 H035 0.9300 . ? C16 O4 1.432(3) . ? C16 H03F 0.9600 . ? C16 H03G 0.9600 . ? C16 H03H 0.9600 . ? C23 N9 1.340(4) . ? C23 H039 0.9300 . ? C13 C14 1.398(5) . ? C13 H040 0.9300 . ? C14 H041 0.9300 . ? C27 C26 1.371(5) . ? C27 H046 0.9300 . ? C26 N10 1.336(4) . ? C26 H047 0.9300 . ? C6 H048 0.9300 . ? Fe1 N8 1.987(2) . ? Fe1 N7 1.993(2) . ? Mn1 O1 1.8732(17) . ? Mn1 O2 1.8819(17) . ? Mn1 N1 1.980(2) . ? Mn1 N2 1.981(2) . ? Mn1 O1W 2.266(2) . ? Mn1 N3 2.305(3) . ? N1 C42B 1.514(5) . ? N1 C42A 1.544(7) . ? N2 C43B 1.497(6) . ? N2 C43A 1.546(10) . ? O1W H1W 0.867(19) . ? O1W H2W 0.869(19) . ? C39A C44A 1.371(11) . ? C39A C40A 1.512(4) . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C40A C43A 1.542(10) . ? C40A H40A 0.9700 . ? C40A H40B 0.9700 . ? C41A C42A 1.584(8) . ? C41A C44A 1.637(11) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43A 1.555(13) . ? C42A H42A 0.9800 . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C43A H43A 0.9800 . ? C43B C42B 1.510(9) . ? C43B H43B 0.9800 . ? C42B H42B 0.9800 . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? 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 H3W O2W H4W 98(5) . . ? H5W O3W H6W 107(6) . . ? O2 C11 C10 124.1(2) . . ? O2 C11 C12 117.6(2) . . ? C10 C11 C12 118.3(2) . . ? O1 C3 C2 124.5(2) . . ? O1 C3 C4 116.9(2) . . ? C2 C3 C4 118.6(2) . . ? C3 C2 C7 119.3(3) . . ? C3 C2 C1 122.5(2) . . ? C7 C2 C1 118.3(2) . . ? C11 C10 C15 119.6(2) . . ? C11 C10 C9 122.7(2) . . ? C15 C10 C9 117.6(2) . . ? N9 C24 N7 126.3(3) . . ? N9 C24 C25 119.3(2) . . ? N7 C24 C25 114.4(2) . . ? O4 C12 C13 125.0(2) . . ? O4 C12 C11 114.2(2) . . ? C13 C12 C11 120.8(2) . . ? N1 C1 C2 126.0(2) . . ? N1 C1 H016 117.0 . . ? C2 C1 H016 117.0 . . ? N4 C18 Fe1 175.7(3) . . ? C21 C22 C23 117.9(3) . . ? C21 C22 H019 121.0 . . ? C23 C22 H019 121.0 . . ? C5 C4 O3 125.6(2) . . ? C5 C4 C3 120.7(2) . . ? O3 C4 C3 113.7(2) . . ? N10 C25 N8 126.4(3) . . ? N10 C25 C24 119.5(2) . . ? N8 C25 C24 114.1(2) . . ? N2 C9 C10 126.0(2) . . ? N2 C9 H023 117.0 . . ? C10 C9 H023 117.0 . . ? N7 C21 C22 120.8(3) . . ? N7 C21 H024 119.6 . . ? C22 C21 H024 119.6 . . ? N5 C19 Fe1 178.2(4) . . ? N3 C17 Fe1 175.4(3) . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H029 119.7 . . ? C10 C15 H029 119.7 . . ? N6 C20 Fe1 173.9(3) . . ? C6 C7 C2 120.9(3) . . ? C6 C7 H032 119.5 . . ? C2 C7 H032 119.5 . . ? O3 C8 H03C 109.5 . . ? O3 C8 H03D 109.5 . . ? H03C C8 H03D 109.5 . . ? O3 C8 H03E 109.5 . . ? H03C C8 H03E 109.5 . . ? H03D C8 H03E 109.5 . . ? N8 C28 C27 120.5(3) . . ? N8 C28 H034 119.7 . . ? C27 C28 H034 119.7 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H035 120.0 . . ? C6 C5 H035 120.0 . . ? O4 C16 H03F 109.5 . . ? O4 C16 H03G 109.5 . . ? H03F C16 H03G 109.5 . . ? O4 C16 H03H 109.5 . . ? H03F C16 H03H 109.5 . . ? H03G C16 H03H 109.5 . . ? N9 C23 C22 122.5(3) . . ? N9 C23 H039 118.7 . . ? C22 C23 H039 118.7 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H040 119.9 . . ? C14 C13 H040 119.9 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H041 119.8 . . ? C13 C14 H041 119.8 . . ? C28 C27 C26 118.4(3) . . ? C28 C27 H046 120.8 . . ? C26 C27 H046 120.8 . . ? N10 C26 C27 122.3(3) . . ? N10 C26 H047 118.8 . . ? C27 C26 H047 118.8 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H048 119.8 . . ? C5 C6 H048 119.8 . . ? C18 Fe1 C19 86.89(12) . . ? C18 Fe1 C20 92.54(12) . . ? C19 Fe1 C20 91.58(15) . . ? C18 Fe1 C17 87.92(12) . . ? C19 Fe1 C17 90.41(14) . . ? C20 Fe1 C17 177.98(14) . . ? C18 Fe1 N8 94.98(11) . . ? C19 Fe1 N8 177.93(11) . . ? C20 Fe1 N8 89.21(12) . . ? C17 Fe1 N8 88.79(11) . . ? C18 Fe1 N7 175.69(12) . . ? C19 Fe1 N7 97.08(10) . . ? C20 Fe1 N7 89.04(11) . . ? C17 Fe1 N7 90.36(10) . . ? N8 Fe1 N7 81.02(9) . . ? O1 Mn1 O2 91.70(7) . . ? O1 Mn1 N1 92.80(8) . . ? O2 Mn1 N1 175.50(8) . . ? O1 Mn1 N2 175.79(8) . . ? O2 Mn1 N2 92.50(8) . . ? N1 Mn1 N2 83.01(9) . . ? O1 Mn1 O1W 89.87(8) . . ? O2 Mn1 O1W 94.04(9) . . ? N1 Mn1 O1W 85.80(10) . . ? N2 Mn1 O1W 89.53(10) . . ? O1 Mn1 N3 91.92(10) . . ? O2 Mn1 N3 91.93(10) . . ? N1 Mn1 N3 88.09(11) . . ? N2 Mn1 N3 88.25(11) . . ? O1W Mn1 N3 173.71(8) . . ? C1 N1 C42B 123.8(3) . . ? C1 N1 C42A 118.9(3) . . ? C42B N1 C42A 34.7(3) . . ? C1 N1 Mn1 125.23(18) . . ? C42B N1 Mn1 110.2(2) . . ? C42A N1 Mn1 110.2(3) . . ? C9 N2 C43B 122.3(3) . . ? C9 N2 C43A 120.5(4) . . ? C43B N2 C43A 28.1(3) . . ? C9 N2 Mn1 125.72(17) . . ? C43B N2 Mn1 111.0(3) . . ? C43A N2 Mn1 110.9(4) . . ? C25 N8 C28 116.4(2) . . ? C25 N8 Fe1 115.41(18) . . ? C28 N8 Fe1 128.1(2) . . ? C21 N7 C24 116.7(2) . . ? C21 N7 Fe1 128.26(18) . . ? C24 N7 Fe1 115.04(17) . . ? C17 N3 Mn1 157.7(3) . . ? C24 N9 C23 115.7(3) . . ? C25 N10 C26 115.9(3) . . ? C3 O1 Mn1 128.18(15) . . ? C11 O2 Mn1 128.83(15) . . ? Mn1 O1W H1W 108(3) . . ? Mn1 O1W H2W 112(3) . . ? H1W O1W H2W 104(4) . . ? C4 O3 C8 117.4(2) . . ? C12 O4 C16 116.8(2) . . ? C44A C39A C40A 120.7(5) . . ? C44A C39A H39A 107.2 . . ? C40A C39A H39A 107.2 . . ? C44A C39A H39B 107.2 . . ? C40A C39A H39B 107.2 . . ? H39A C39A H39B 106.8 . . ? C39A C40A C43A 111.1(5) . . ? C39A C40A H40A 109.4 . . ? C43A C40A H40A 109.4 . . ? C39A C40A H40B 109.4 . . ? C43A C40A H40B 109.4 . . ? H40A C40A H40B 108.0 . . ? C42A C41A C44A 100.6(6) . . ? C42A C41A H41A 111.7 . . ? C44A C41A H41A 111.7 . . ? C42A C41A H41B 111.7 . . ? C44A C41A H41B 111.7 . . ? H41A C41A H41B 109.4 . . ? N1 C42A C43A 101.2(6) . . ? N1 C42A C41A 109.8(5) . . ? C43A C42A C41A 103.0(7) . . ? N1 C42A H42A 113.9 . . ? C43A C42A H42A 113.9 . . ? C41A C42A H42A 113.9 . . ? C39A C44A C41A 110.7(7) . . ? C39A C44A H44A 109.5 . . ? C41A C44A H44A 109.5 . . ? C39A C44A H44B 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 108.1 . . ? C40A C43A N2 110.9(7) . . ? C40A C43A C42A 108.4(7) . . ? N2 C43A C42A 101.5(6) . . ? C40A C43A H43A 111.9 . . ? N2 C43A H43A 111.9 . . ? C42A C43A H43A 111.9 . . ? N2 C43B C42B 104.6(4) . . ? N2 C43B H43B 108.4 . . ? C42B C43B H43B 108.4 . . ? C43B C42B N1 104.1(4) . . ? C43B C42B H42B 110.4 . . ? N1 C42B H42B 110.4 . . ? H44C C44B H44D 107.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.271 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.052