Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Berthold Kersting' _publ_contact_author_address ; Fakultat fur Chemie und Mineralogie Universitat Leipzig Johannisallee 29 Leipzig 04103 GERMANY ; _publ_contact_author_email B.KERSTING@UNI-LEIPZIG.DE _publ_section_title ; Preparation and Characterization of CrIII, MnII, FeII, CoII and NiII complexes of a hexaaza-dithiophenolate macrocycle ; loop_ _publ_author_name 'Berthold Kersting' 'Thorsten Glaser' 'Yves Journaux' 'Vasile Logan' 'Gunther Steinfeld' data_1 _database_code_depnum_ccdc_archive 'CCDC 281645' _chemical_formula_structural ; [(LMe)CrH2(OAc)](ClO4)2 ; _chemical_formula_sum 'C40 H69 Cl2 Cr N6 O10 S2' _chemical_formula_weight 981.03 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown from methanol ; #CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.490(3) _cell_length_b 24.163(5) _cell_length_c 13.777(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.84(3) _cell_angle_gamma 90.00 _cell_volume 4789.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 0.497 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30037 _diffrn_reflns_av_R_equivalents 0.0991 _diffrn_reflns_av_sigmaI/netI 0.2277 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 28.33 #REFINEMENT DATA _reflns_number_total 11424 _reflns_number_gt 3881 _reflns_threshold_expression >2sigma(I) _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^)+(0.1078P)^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 11424 _refine_ls_number_parameters 545 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.2049 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2192 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_restrained_S_all 0.791 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.719 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.090 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cr Cr 0.25395(6) 0.02085(4) 0.22744(6) 0.0290(2) Uani 1 1 d . . . S1 S 0.39627(9) 0.00967(7) 0.16204(10) 0.0342(4) Uani 1 1 d . . . S2 S 0.20906(10) 0.09363(6) 0.11801(10) 0.0331(4) Uani 1 1 d . . . N1 N 0.1902(3) -0.04290(19) 0.1231(3) 0.0306(11) Uani 1 1 d . . . N2 N 0.2714(3) -0.0499(2) 0.3244(3) 0.0344(11) Uani 1 1 d . . . N3 N 0.1404(3) 0.0397(2) 0.3128(3) 0.0321(11) Uani 1 1 d . . . N4 N 0.1531(3) 0.1763(2) -0.0547(3) 0.0376(12) Uani 1 1 d . . . N5 N 0.2758(3) 0.2268(2) 0.0800(4) 0.0434(13) Uani 1 1 d . . . H5 H 0.2495 0.1926 0.0724 0.052 Uiso 1 1 calc R . . N6 N 0.4674(3) 0.13043(19) 0.0858(3) 0.0346(11) Uani 1 1 d . . . H6 H 0.4362 0.1162 0.1336 0.042 Uiso 1 1 calc R . . C1 C 0.3626(3) 0.0138(2) 0.0368(4) 0.0288(12) Uani 1 1 d . . . C2 C 0.2936(3) -0.0207(2) -0.0088(4) 0.0275(12) Uani 1 1 d . . . C3 C 0.2703(4) -0.0180(2) -0.1087(4) 0.0327(13) Uani 1 1 d . . . H3 H 0.2231 -0.0409 -0.1373 0.039 Uiso 1 1 calc R . . C4 C 0.3141(4) 0.0176(2) -0.1690(4) 0.0339(13) Uani 1 1 d . . . C5 C 0.3838(4) 0.0510(2) -0.1236(4) 0.0337(13) Uani 1 1 d . . . H7 H 0.4151 0.0749 -0.1614 0.040 Uiso 1 1 calc R . . C6 C 0.4083(4) 0.0499(2) -0.0225(4) 0.0302(13) Uani 1 1 d . . . C7 C 0.2544(4) -0.0634(2) 0.0518(4) 0.0336(13) Uani 1 1 d . . . H7A H 0.3056 -0.0831 0.0884 0.040 Uiso 1 1 calc R . . H7B H 0.2205 -0.0900 0.0083 0.040 Uiso 1 1 calc R . . C8 C 0.1027(4) -0.0272(3) 0.0627(4) 0.0389(14) Uani 1 1 d . . . H8A H 0.0748 -0.0595 0.0310 0.058 Uiso 1 1 calc R . . H8B H 0.1159 -0.0008 0.0142 0.058 Uiso 1 1 calc R . . H8C H 0.0607 -0.0111 0.1036 0.058 Uiso 1 1 calc R . . C9 C 0.1726(4) -0.0911(2) 0.1865(4) 0.0393(15) Uani 1 1 d . . . H9A H 0.1623 -0.1240 0.1464 0.047 Uiso 1 1 calc R . . H9B H 0.1168 -0.0842 0.2172 0.047 Uiso 1 1 calc R . . C10 C 0.2538(4) -0.1006(3) 0.2647(4) 0.0401(15) Uani 1 1 d . . . H10A H 0.2400 -0.1313 0.3061 0.048 Uiso 1 1 calc R . . H10B H 0.3088 -0.1101 0.2343 0.048 Uiso 1 1 calc R . . C11 C 0.3668(4) -0.0548(3) 0.3796(4) 0.0451(16) Uani 1 1 d . . . H11A H 0.3716 -0.0891 0.4150 0.068 Uiso 1 1 calc R . . H11B H 0.3774 -0.0245 0.4246 0.068 Uiso 1 1 calc R . . H11C H 0.4123 -0.0539 0.3344 0.068 Uiso 1 1 calc R . . C12 C 0.2013(4) -0.0450(2) 0.3954(4) 0.0378(14) Uani 1 1 d . . . H12A H 0.2269 -0.0606 0.4577 0.045 Uiso 1 1 calc R . . H12B H 0.1464 -0.0662 0.3714 0.045 Uiso 1 1 calc R . . C13 C 0.1739(4) 0.0145(3) 0.4100(4) 0.0401(15) Uani 1 1 d . . . H13A H 0.1251 0.0161 0.4523 0.048 Uiso 1 1 calc R . . H13B H 0.2270 0.0351 0.4408 0.048 Uiso 1 1 calc R . . C14 C 0.0421(3) 0.0200(3) 0.2873(4) 0.0424(15) Uani 1 1 d . . . H14A H 0.0367 -0.0174 0.3098 0.064 Uiso 1 1 calc R . . H14B H 0.0260 0.0212 0.2176 0.064 Uiso 1 1 calc R . . H14C H 0.0007 0.0434 0.3181 0.064 Uiso 1 1 calc R . . C15 C 0.1360(4) 0.1015(2) 0.3246(4) 0.0352(14) Uani 1 1 d . . . H15A H 0.1087 0.1099 0.3839 0.042 Uiso 1 1 calc R . . H15B H 0.1987 0.1163 0.3321 0.042 Uiso 1 1 calc R . . C16 C 0.0806(4) 0.1296(2) 0.2403(4) 0.0352(14) Uani 1 1 d . . . C17 C 0.1062(4) 0.1265(2) 0.1455(4) 0.0341(13) Uani 1 1 d . . . C18 C 0.0477(4) 0.1526(2) 0.0683(4) 0.0357(14) Uani 1 1 d . . . C19 C -0.0322(4) 0.1804(2) 0.0891(4) 0.0378(14) Uani 1 1 d . . . H19 H -0.0695 0.1974 0.0380 0.045 Uiso 1 1 calc R . . C20 C -0.0586(4) 0.1838(2) 0.1829(5) 0.0380(14) Uani 1 1 d . . . C21 C -0.0004(4) 0.1577(3) 0.2560(4) 0.0394(15) Uani 1 1 d . . . H21 H -0.0164 0.1589 0.3194 0.047 Uiso 1 1 calc R . . C22 C 0.0681(4) 0.1476(3) -0.0366(4) 0.0364(14) Uani 1 1 d . . . H22A H 0.0735 0.1088 -0.0527 0.044 Uiso 1 1 calc R . . H22B H 0.0162 0.1628 -0.0794 0.044 Uiso 1 1 calc R . . C23 C 0.1853(5) 0.1559(3) -0.1453(4) 0.0567(19) Uani 1 1 d . . . H23A H 0.1333 0.1527 -0.1951 0.085 Uiso 1 1 calc R . . H23B H 0.2140 0.1203 -0.1337 0.085 Uiso 1 1 calc R . . H23C H 0.2297 0.1814 -0.1663 0.085 Uiso 1 1 calc R . . C24 C 0.1480(4) 0.2366(3) -0.0502(5) 0.0442(16) Uani 1 1 d . . . H24A H 0.1032 0.2478 -0.0070 0.053 Uiso 1 1 calc R . . H24B H 0.1288 0.2516 -0.1147 0.053 Uiso 1 1 calc R . . C25 C 0.2450(4) 0.2579(3) -0.0115(5) 0.0473(16) Uani 1 1 d . . . H25A H 0.2878 0.2517 -0.0594 0.057 Uiso 1 1 calc R . . H25B H 0.2428 0.2972 0.0019 0.057 Uiso 1 1 calc R . . C26 C 0.2416(5) 0.2515(3) 0.1686(5) 0.061(2) Uani 1 1 d . . . H26A H 0.2401 0.2236 0.2178 0.092 Uiso 1 1 calc R . . H26B H 0.1802 0.2661 0.1514 0.092 Uiso 1 1 calc R . . H26C H 0.2826 0.2808 0.1933 0.092 Uiso 1 1 calc R . . C27 C 0.3772(4) 0.2178(3) 0.0977(5) 0.0489(17) Uani 1 1 d . . . H27A H 0.3945 0.2075 0.1654 0.059 Uiso 1 1 calc R . . H27B H 0.4093 0.2519 0.0854 0.059 Uiso 1 1 calc R . . C28 C 0.4063(4) 0.1720(3) 0.0307(5) 0.0504(17) Uani 1 1 d . . . H28A H 0.3511 0.1537 -0.0010 0.060 Uiso 1 1 calc R . . H28B H 0.4388 0.1883 -0.0198 0.060 Uiso 1 1 calc R . . C29 C 0.5550(4) 0.1551(3) 0.1330(6) 0.062(2) Uani 1 1 d . . . H29A H 0.5914 0.1679 0.0837 0.093 Uiso 1 1 calc R . . H29B H 0.5895 0.1277 0.1727 0.093 Uiso 1 1 calc R . . H29C H 0.5410 0.1857 0.1732 0.093 Uiso 1 1 calc R . . C30 C 0.4905(3) 0.0833(2) 0.0209(4) 0.0332(13) Uani 1 1 d . . . H30A H 0.5216 0.0983 -0.0319 0.040 Uiso 1 1 calc R . . H30B H 0.5340 0.0588 0.0587 0.040 Uiso 1 1 calc R . . C31 C 0.2901(4) 0.0171(3) -0.2809(4) 0.0401(15) Uani 1 1 d . . . C32 C 0.1868(5) 0.0049(4) -0.3101(4) 0.070(2) Uani 1 1 d . . . H32A H 0.1517 0.0385 -0.3071 0.105 Uiso 1 1 calc R . . H32B H 0.1661 -0.0218 -0.2659 0.105 Uiso 1 1 calc R . . H32C H 0.1780 -0.0095 -0.3754 0.105 Uiso 1 1 calc R . . C33 C 0.3132(6) 0.0722(4) -0.3250(5) 0.083(3) Uani 1 1 d . . . H33A H 0.3092 0.1011 -0.2778 0.124 Uiso 1 1 calc R . . H33B H 0.2698 0.0795 -0.3819 0.124 Uiso 1 1 calc R . . H33C H 0.3751 0.0709 -0.3432 0.124 Uiso 1 1 calc R . . C34 C 0.3481(5) -0.0284(4) -0.3204(5) 0.078(3) Uani 1 1 d . . . H34A H 0.3429 -0.0259 -0.3903 0.117 Uiso 1 1 calc R . . H34B H 0.3260 -0.0638 -0.3018 0.117 Uiso 1 1 calc R . . H34C H 0.4120 -0.0240 -0.2937 0.117 Uiso 1 1 calc R . . C35 C -0.1462(4) 0.2127(3) 0.2070(5) 0.0477(17) Uani 1 1 d . . . C36 C -0.1212(5) 0.2578(3) 0.2830(6) 0.065(2) Uani 1 1 d . . . H36A H -0.0961 0.2411 0.3438 0.098 Uiso 1 1 calc R . . H36B H -0.1759 0.2785 0.2925 0.098 Uiso 1 1 calc R . . H36C H -0.0757 0.2821 0.2607 0.098 Uiso 1 1 calc R . . C37 C -0.2024(5) 0.2380(3) 0.1169(6) 0.070(2) Uani 1 1 d . . . H37A H -0.2496 0.2619 0.1371 0.105 Uiso 1 1 calc R . . H37B H -0.2311 0.2091 0.0762 0.105 Uiso 1 1 calc R . . H37C H -0.1619 0.2591 0.0808 0.105 Uiso 1 1 calc R . . C38 C -0.2086(4) 0.1695(3) 0.2526(6) 0.065(2) Uani 1 1 d . . . H38A H -0.1997 0.1729 0.3225 0.097 Uiso 1 1 calc R . . H38B H -0.1917 0.1329 0.2343 0.097 Uiso 1 1 calc R . . H38C H -0.2726 0.1763 0.2291 0.097 Uiso 1 1 calc R . . O1 O 0.3298(2) 0.06157(17) 0.3309(3) 0.0365(10) Uani 1 1 d . . . O2 O 0.4039(4) 0.1310(2) 0.2668(4) 0.0742(16) Uani 1 1 d . . . C39 C 0.3873(4) 0.1026(3) 0.3346(4) 0.0439(16) Uani 1 1 d . . . C40 C 0.43899(9) 0.11179(5) 0.43477(9) 0.084(3) Uani 1 1 d . . . H40A H 0.5034 0.1186 0.4291 0.126 Uiso 1 1 calc R . . H40B H 0.4334 0.0795 0.4743 0.126 Uiso 1 1 calc R . . H40C H 0.4131 0.1432 0.4647 0.126 Uiso 1 1 calc R . . Cl1 Cl 0.01581(9) 0.13143(5) 0.57087(9) 0.0543(5) Uani 1 1 d R . . O3 O -0.00654(9) 0.07976(5) 0.52086(9) 0.0853(19) Uani 1 1 d R . . O4 O -0.00539(9) 0.12723(5) 0.66785(9) 0.0804(17) Uani 1 1 d R . . O5 O 0.11216(9) 0.14182(5) 0.56906(9) 0.094(2) Uani 1 1 d R . . O6 O -0.03236(9) 0.17457(5) 0.51704(9) 0.133(3) Uani 1 1 d R . . Cl2 Cl 0.46969(9) 0.69853(5) 0.70874(9) 0.0938(8) Uani 1 1 d RD . . O7A O 0.42157(9) 0.66263(5) 0.64078(9) 0.145(7) Uani 0.631(12) 1 d PRDU A 1 O8A O 0.55027(9) 0.71741(5) 0.67247(9) 0.175(8) Uani 0.631(12) 1 d PRDU A 1 O9A O 0.49403(9) 0.67040(5) 0.79691(9) 0.272(14) Uani 0.631(12) 1 d PRD A 1 O10A O 0.41290(9) 0.74369(5) 0.72479(9) 0.235(10) Uani 0.631(12) 1 d PRDU A 1 O7B O 0.41524(9) 0.71597(5) 0.78039(9) 0.067(6) Uani 0.369(12) 1 d PRDU A 2 O8B O 0.56414(9) 0.70481(5) 0.74245(9) 0.216(13) Uani 0.369(12) 1 d PRDU A 2 O9B O 0.45037(9) 0.73078(5) 0.62434(9) 0.39(4) Uani 0.369(12) 1 d PRD A 2 O10B O 0.44959(9) 0.64287(5) 0.68742(9) 0.230(14) Uani 0.369(12) 1 d PRDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0240(5) 0.0350(6) 0.0280(5) 0.0026(4) 0.0030(4) 0.0013(4) S1 0.0230(7) 0.0465(10) 0.0330(7) 0.0006(7) 0.0035(6) 0.0018(6) S2 0.0300(8) 0.0358(9) 0.0347(8) 0.0054(7) 0.0087(6) 0.0058(6) N1 0.029(3) 0.034(3) 0.029(2) 0.004(2) 0.003(2) -0.005(2) N2 0.032(3) 0.040(3) 0.030(3) 0.002(2) 0.001(2) 0.001(2) N3 0.031(3) 0.036(3) 0.029(2) 0.005(2) 0.003(2) 0.002(2) N4 0.040(3) 0.036(3) 0.039(3) 0.001(2) 0.009(2) 0.003(2) N5 0.047(3) 0.031(3) 0.051(3) -0.005(3) 0.005(3) 0.003(2) N6 0.030(3) 0.032(3) 0.041(3) -0.003(2) 0.000(2) -0.001(2) C1 0.024(3) 0.024(3) 0.038(3) -0.003(3) 0.002(2) 0.004(2) C2 0.025(3) 0.029(3) 0.029(3) -0.001(3) 0.006(2) 0.003(2) C3 0.032(3) 0.034(3) 0.032(3) -0.002(3) 0.004(2) -0.003(3) C4 0.032(3) 0.043(4) 0.027(3) -0.006(3) 0.008(2) -0.001(3) C5 0.031(3) 0.033(4) 0.038(3) 0.001(3) 0.008(3) 0.000(2) C6 0.025(3) 0.030(3) 0.036(3) -0.003(3) 0.006(2) 0.001(2) C7 0.031(3) 0.033(3) 0.039(3) 0.000(3) 0.010(3) 0.001(2) C8 0.031(3) 0.047(4) 0.039(3) 0.001(3) 0.003(3) 0.000(3) C9 0.048(4) 0.032(4) 0.039(3) 0.003(3) 0.008(3) -0.011(3) C10 0.049(4) 0.034(4) 0.038(3) 0.011(3) 0.006(3) 0.001(3) C11 0.033(3) 0.060(5) 0.040(3) 0.017(3) -0.005(3) 0.004(3) C12 0.037(3) 0.045(4) 0.032(3) 0.011(3) 0.007(3) -0.001(3) C13 0.038(3) 0.050(4) 0.033(3) 0.008(3) 0.010(3) 0.004(3) C14 0.025(3) 0.061(5) 0.041(3) 0.003(3) 0.006(3) -0.003(3) C15 0.036(3) 0.037(4) 0.033(3) -0.005(3) 0.006(3) 0.002(3) C16 0.032(3) 0.035(4) 0.038(3) -0.003(3) 0.006(3) 0.001(3) C17 0.030(3) 0.036(4) 0.036(3) 0.000(3) 0.005(3) -0.005(3) C18 0.033(3) 0.035(4) 0.039(3) 0.004(3) 0.004(3) -0.002(3) C19 0.028(3) 0.036(4) 0.048(4) 0.004(3) -0.002(3) 0.000(3) C20 0.026(3) 0.030(4) 0.059(4) 0.002(3) 0.010(3) 0.001(2) C21 0.039(3) 0.039(4) 0.043(4) -0.005(3) 0.015(3) 0.000(3) C22 0.032(3) 0.037(4) 0.039(3) 0.002(3) -0.001(3) 0.004(3) C23 0.059(5) 0.066(5) 0.046(4) -0.004(4) 0.011(3) -0.005(4) C24 0.045(4) 0.038(4) 0.049(4) 0.009(3) 0.004(3) 0.008(3) C25 0.050(4) 0.037(4) 0.055(4) 0.003(3) 0.006(3) 0.004(3) C26 0.066(5) 0.058(5) 0.061(4) -0.022(4) 0.014(4) 0.012(4) C27 0.040(4) 0.050(4) 0.055(4) -0.014(3) 0.000(3) 0.011(3) C28 0.053(4) 0.048(5) 0.050(4) -0.003(3) 0.005(3) 0.013(3) C29 0.040(4) 0.046(5) 0.095(6) -0.023(4) -0.014(4) -0.008(3) C30 0.025(3) 0.036(4) 0.041(3) -0.003(3) 0.015(3) 0.001(2) C31 0.043(3) 0.051(4) 0.025(3) 0.000(3) 0.003(3) -0.001(3) C32 0.052(4) 0.113(7) 0.039(4) 0.012(4) -0.016(3) -0.012(4) C33 0.118(7) 0.089(7) 0.039(4) 0.004(4) 0.004(4) -0.028(5) C34 0.077(6) 0.115(8) 0.040(4) -0.024(4) 0.002(4) 0.025(5) C35 0.032(3) 0.035(4) 0.077(5) -0.006(3) 0.009(3) 0.007(3) C36 0.046(4) 0.045(5) 0.106(6) -0.023(4) 0.014(4) 0.005(3) C37 0.040(4) 0.070(6) 0.101(6) -0.004(5) 0.006(4) 0.019(4) C38 0.034(4) 0.056(5) 0.109(6) -0.008(4) 0.025(4) -0.004(3) O1 0.030(2) 0.045(3) 0.034(2) -0.0019(19) 0.0027(17) -0.0043(19) O2 0.101(4) 0.063(4) 0.059(3) -0.008(3) 0.010(3) -0.033(3) C39 0.040(4) 0.059(5) 0.034(3) -0.006(3) 0.008(3) -0.013(3) C40 0.086(6) 0.110(8) 0.051(5) -0.015(5) -0.015(4) -0.045(5) Cl1 0.0617(11) 0.0477(11) 0.0581(11) 0.0041(9) 0.0269(9) -0.0033(9) O3 0.104(4) 0.074(4) 0.087(4) -0.038(3) 0.048(3) -0.036(3) O4 0.101(4) 0.086(4) 0.061(3) -0.015(3) 0.037(3) -0.029(3) O5 0.068(4) 0.118(5) 0.103(4) -0.004(4) 0.036(3) -0.035(3) O6 0.164(7) 0.121(6) 0.120(5) 0.041(5) 0.040(5) 0.078(5) Cl2 0.106(2) 0.0724(17) 0.112(2) -0.0439(15) 0.0472(17) -0.0274(14) O7A 0.170(11) 0.151(12) 0.135(10) -0.111(9) 0.104(9) -0.134(10) O8A 0.165(12) 0.285(17) 0.092(9) -0.113(11) 0.085(9) -0.171(12) O9A 0.23(2) 0.29(3) 0.27(2) 0.15(2) -0.066(17) -0.147(19) O10A 0.225(17) 0.127(14) 0.35(2) -0.122(16) 0.004(16) 0.064(12) O7B 0.097(11) 0.044(10) 0.069(10) -0.043(8) 0.055(8) -0.005(8) O8B 0.076(13) 0.38(3) 0.20(3) -0.13(2) 0.058(15) -0.103(17) O9B 0.26(4) 0.69(10) 0.26(4) 0.18(5) 0.16(4) 0.34(6) O10B 0.22(2) 0.22(2) 0.28(3) -0.19(2) 0.16(2) -0.08(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #BOND LENGTHS AND ANGLES 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 Cr O1 1.958(4) . ? Cr N2 2.165(5) . ? Cr N3 2.181(4) . ? Cr N1 2.231(4) . ? Cr S2 2.3569(17) . ? Cr S1 2.3623(16) . ? S1 C1 1.739(5) . ? S2 C17 1.769(6) . ? N1 C8 1.481(7) . ? N1 C9 1.495(7) . ? N1 C7 1.514(6) . ? N2 C10 1.483(7) . ? N2 C12 1.496(7) . ? N2 C11 1.501(6) . ? N3 C13 1.498(7) . ? N3 C14 1.504(7) . ? N3 C15 1.505(7) . ? N4 C22 1.461(7) . ? N4 C24 1.461(7) . ? N4 C23 1.469(7) . ? N5 C27 1.476(7) . ? N5 C25 1.489(7) . ? N5 C26 1.495(7) . ? N6 C29 1.480(7) . ? N6 C28 1.487(7) . ? N6 C30 1.509(7) . ? C1 C2 1.393(7) . ? C1 C6 1.412(7) . ? C2 C3 1.379(7) . ? C2 C7 1.483(7) . ? C3 C4 1.400(7) . ? C4 C5 1.383(7) . ? C4 C31 1.540(7) . ? C5 C6 1.396(7) . ? C6 C30 1.503(7) . ? C9 C10 1.516(8) . ? C12 C13 1.512(8) . ? C15 C16 1.493(7) . ? C16 C21 1.396(7) . ? C16 C17 1.402(7) . ? C17 C18 1.425(8) . ? C18 C19 1.398(7) . ? C18 C22 1.513(7) . ? C19 C20 1.393(8) . ? C20 C21 1.387(8) . ? C20 C35 1.519(8) . ? C24 C25 1.531(8) . ? C27 C28 1.533(8) . ? C31 C33 1.518(9) . ? C31 C34 1.523(9) . ? C31 C32 1.530(8) . ? C35 C36 1.525(9) . ? C35 C37 1.530(9) . ? C35 C38 1.561(9) . ? O1 C39 1.292(7) . ? O2 C39 1.207(7) . ? C39 C40 1.506(6) . ? Cl1 O4 1.4098 . ? Cl1 O6 1.4144 . ? Cl1 O5 1.4217 . ? Cl1 O3 1.4439 . ? Cl2 O7A 1.3999 . ? Cl2 O10B 1.4000 . ? Cl2 O7B 1.4000 . ? Cl2 O9A 1.4000 . ? Cl2 O9B 1.4000 . ? Cl2 O10A 1.4000 . ? Cl2 O8A 1.4000 . ? Cl2 O8B 1.4001 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cr N2 86.17(17) . . ? O1 Cr N3 84.08(16) . . ? N2 Cr N3 82.64(17) . . ? O1 Cr N1 165.78(17) . . ? N2 Cr N1 82.05(17) . . ? N3 Cr N1 102.17(16) . . ? O1 Cr S2 100.31(13) . . ? N2 Cr S2 170.59(13) . . ? N3 Cr S2 91.19(12) . . ? N1 Cr S2 92.38(12) . . ? O1 Cr S1 83.98(11) . . ? N2 Cr S1 95.87(13) . . ? N3 Cr S1 168.04(13) . . ? N1 Cr S1 89.33(12) . . ? S2 Cr S1 91.62(6) . . ? C1 S1 Cr 102.57(18) . . ? C17 S2 Cr 111.93(19) . . ? C8 N1 C9 109.4(4) . . ? C8 N1 C7 105.6(4) . . ? C9 N1 C7 106.5(4) . . ? C8 N1 Cr 116.5(3) . . ? C9 N1 Cr 104.3(3) . . ? C7 N1 Cr 114.0(3) . . ? C10 N2 C12 110.0(4) . . ? C10 N2 C11 107.6(5) . . ? C12 N2 C11 109.4(4) . . ? C10 N2 Cr 108.1(3) . . ? C12 N2 Cr 107.7(3) . . ? C11 N2 Cr 114.1(3) . . ? C13 N3 C14 106.1(4) . . ? C13 N3 C15 108.7(4) . . ? C14 N3 C15 106.8(4) . . ? C13 N3 Cr 102.2(3) . . ? C14 N3 Cr 124.2(3) . . ? C15 N3 Cr 108.1(3) . . ? C22 N4 C24 114.7(5) . . ? C22 N4 C23 110.3(5) . . ? C24 N4 C23 113.1(5) . . ? C27 N5 C25 114.0(5) . . ? C27 N5 C26 110.1(5) . . ? C25 N5 C26 113.2(5) . . ? C29 N6 C28 112.4(5) . . ? C29 N6 C30 108.9(4) . . ? C28 N6 C30 111.6(4) . . ? C2 C1 C6 118.0(5) . . ? C2 C1 S1 120.9(4) . . ? C6 C1 S1 121.0(4) . . ? C3 C2 C1 120.0(5) . . ? C3 C2 C7 121.9(5) . . ? C1 C2 C7 117.8(5) . . ? C2 C3 C4 123.1(5) . . ? C5 C4 C3 116.7(5) . . ? C5 C4 C31 121.5(5) . . ? C3 C4 C31 121.7(5) . . ? C4 C5 C6 121.6(5) . . ? C5 C6 C1 120.6(5) . . ? C5 C6 C30 118.8(5) . . ? C1 C6 C30 120.3(5) . . ? C2 C7 N1 116.3(5) . . ? N1 C9 C10 111.2(4) . . ? N2 C10 C9 109.6(5) . . ? N2 C12 C13 111.7(4) . . ? N3 C13 C12 109.3(5) . . ? C16 C15 N3 113.1(4) . . ? C21 C16 C17 119.4(5) . . ? C21 C16 C15 119.0(5) . . ? C17 C16 C15 121.6(5) . . ? C16 C17 C18 118.2(5) . . ? C16 C17 S2 123.1(4) . . ? C18 C17 S2 118.7(4) . . ? C19 C18 C17 119.5(5) . . ? C19 C18 C22 119.6(5) . . ? C17 C18 C22 120.8(5) . . ? C20 C19 C18 123.0(5) . . ? C21 C20 C19 115.9(5) . . ? C21 C20 C35 120.1(5) . . ? C19 C20 C35 124.0(6) . . ? C20 C21 C16 124.0(5) . . ? N4 C22 C18 112.9(5) . . ? N4 C24 C25 107.5(5) . . ? N5 C25 C24 107.2(5) . . ? N5 C27 C28 110.2(5) . . ? N6 C28 C27 111.7(5) . . ? C6 C30 N6 114.8(4) . . ? C33 C31 C34 109.5(6) . . ? C33 C31 C32 108.6(6) . . ? C34 C31 C32 109.4(6) . . ? C33 C31 C4 111.1(5) . . ? C34 C31 C4 107.1(5) . . ? C32 C31 C4 111.2(5) . . ? C20 C35 C36 110.0(5) . . ? C20 C35 C37 112.6(5) . . ? C36 C35 C37 109.4(6) . . ? C20 C35 C38 108.7(5) . . ? C36 C35 C38 107.6(6) . . ? C37 C35 C38 108.5(5) . . ? C39 O1 Cr 135.9(4) . . ? O2 C39 O1 126.3(6) . . ? O2 C39 C40 120.2(5) . . ? O1 C39 C40 113.5(5) . . ? O4 Cl1 O6 113.6 . . ? O4 Cl1 O5 110.8 . . ? O6 Cl1 O5 106.6 . . ? O4 Cl1 O3 109.2 . . ? O6 Cl1 O3 108.6 . . ? O5 Cl1 O3 108.0 . . ? O7A Cl2 O10B 35.9 . . ? O7A Cl2 O7B 112.4 . . ? O10B Cl2 O7B 108.4 . . ? O7A Cl2 O9A 109.5 . . ? O10B Cl2 O9A 74.9 . . ? O7B Cl2 O9A 68.9 . . ? O7A Cl2 O9B 75.8 . . ? O10B Cl2 O9B 110.1 . . ? O7B Cl2 O9B 110.1 . . ? O9A Cl2 O9B 174.7 . . ? O7A Cl2 O10A 109.5 . . ? O10B Cl2 O10A 132.1 . . ? O7B Cl2 O10A 42.5 . . ? O9A Cl2 O10A 109.5 . . ? O9B Cl2 O10A 68.5 . . ? O7A Cl2 O8A 109.5 . . ? O10B Cl2 O8A 113.6 . . ? O7B Cl2 O8A 135.9 . . ? O9A Cl2 O8A 109.5 . . ? O9B Cl2 O8A 67.4 . . ? O10A Cl2 O8A 109.5 . . ? O7A Cl2 O8B 132.7 . . ? O10B Cl2 O8B 110.1 . . ? O7B Cl2 O8B 110.1 . . ? O9A Cl2 O8B 68.3 . . ? O9B Cl2 O8B 107.8 . . ? O10A Cl2 O8B 115.7 . . ? O8A Cl2 O8B 42.2 . . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 281646' _chemical_formula_structural ; [(LMe)Mn2(OAc)](BPh4)(MeCN)3 ; _chemical_formula_sum 'C70 H96 B Mn2 N9 O2 S2' _chemical_formula_weight 1280.37 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from a mixed acetonitrile/ethanol solvent system ; #CRYSTAL DATA _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 14.555(3) _cell_length_b 16.707(3) _cell_length_c 17.295(3) _cell_angle_alpha 113.54(3) _cell_angle_beta 110.66(3) _cell_angle_gamma 94.92(3) _cell_volume 3479.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31437 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.29 #REFINEMENT DATA _reflns_number_total 16227 _reflns_number_gt 11386 _reflns_threshold_expression >2sigma(I) _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^)+(0.0458P)^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 16227 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.400 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.043 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.225280(17) 0.395986(16) 0.071453(16) 0.02469(6) Uani 1 1 d . . . Mn2 Mn 0.396975(18) 0.607056(16) 0.196352(17) 0.02536(6) Uani 1 1 d . . . S1 S 0.19773(3) 0.55586(3) 0.10284(3) 0.02719(9) Uani 1 1 d . . . S2 S 0.37888(3) 0.46424(3) 0.05136(3) 0.02680(9) Uani 1 1 d . . . N1 N 0.06313(10) 0.35296(9) 0.07133(9) 0.0293(3) Uani 1 1 d . . . N2 N 0.11625(10) 0.30832(10) -0.08779(9) 0.0316(3) Uani 1 1 d . . . N3 N 0.27538(10) 0.26136(9) 0.03425(10) 0.0293(3) Uani 1 1 d . . . N4 N 0.57781(10) 0.63805(9) 0.24446(10) 0.0321(3) Uani 1 1 d . . . N5 N 0.42963(11) 0.71730(10) 0.15198(10) 0.0328(3) Uani 1 1 d . . . N6 N 0.37668(10) 0.73692(9) 0.30744(10) 0.0322(3) Uani 1 1 d . . . O1 O 0.29034(9) 0.42450(8) 0.21149(8) 0.0378(3) Uani 1 1 d . . . O2 O 0.41379(10) 0.55247(8) 0.28824(8) 0.0418(3) Uani 1 1 d . . . C1 C 0.15672(11) 0.57887(11) 0.19272(11) 0.0263(3) Uani 1 1 d . . . C2 C 0.19745(12) 0.66303(11) 0.27295(11) 0.0279(3) Uani 1 1 d . . . C3 C 0.16439(12) 0.67972(11) 0.34317(12) 0.0297(4) Uani 1 1 d . . . H3 H 0.1927 0.7357 0.3961 0.036 Uiso 1 1 calc R . . C4 C 0.09080(12) 0.61599(11) 0.33701(11) 0.0289(4) Uani 1 1 d . . . C5 C 0.04884(12) 0.53442(11) 0.25521(11) 0.0298(4) Uani 1 1 d . . . H5 H -0.0019 0.4909 0.2483 0.036 Uiso 1 1 calc R . . C6 C 0.07915(11) 0.51497(11) 0.18353(11) 0.0274(3) Uani 1 1 d . . . C7 C 0.01772(12) 0.43131(11) 0.09276(12) 0.0314(4) Uani 1 1 d . . . H7A H -0.0473 0.4113 0.0919 0.038 Uiso 1 1 calc R . . H7B H 0.0041 0.4479 0.0429 0.038 Uiso 1 1 calc R . . C8 C 0.06738(14) 0.31672(13) 0.13753(14) 0.0407(4) Uani 1 1 d . . . H8A H 0.0925 0.2638 0.1221 0.061 Uiso 1 1 calc R . . H8B H 0.0004 0.3010 0.1337 0.061 Uiso 1 1 calc R . . H8C H 0.1120 0.3618 0.1997 0.061 Uiso 1 1 calc R . . C9 C -0.00704(13) 0.28383(12) -0.02514(12) 0.0376(4) Uani 1 1 d . . . H9A H -0.0769 0.2823 -0.0339 0.045 Uiso 1 1 calc R . . H9B H 0.0028 0.2246 -0.0339 0.045 Uiso 1 1 calc R . . C10 C 0.01103(13) 0.30404(13) -0.09632(12) 0.0395(4) Uani 1 1 d . . . H10A H -0.0360 0.2576 -0.1580 0.047 Uiso 1 1 calc R . . H10B H -0.0032 0.3615 -0.0899 0.047 Uiso 1 1 calc R . . C11 C 0.13227(16) 0.34940(15) -0.14514(13) 0.0528(5) Uani 1 1 d . . . H11A H 0.1999 0.3518 -0.1415 0.079 Uiso 1 1 calc R . . H11B H 0.1238 0.4096 -0.1224 0.079 Uiso 1 1 calc R . . H11C H 0.0836 0.3135 -0.2087 0.079 Uiso 1 1 calc R . . C12 C 0.13387(13) 0.21670(12) -0.12012(12) 0.0410(5) Uani 1 1 d . . . H12A H 0.1775 0.2135 -0.1520 0.049 Uiso 1 1 calc R . . H12B H 0.0693 0.1723 -0.1647 0.049 Uiso 1 1 calc R . . C13 C 0.18200(13) 0.19220(12) -0.04257(14) 0.0413(5) Uani 1 1 d . . . H13A H 0.1332 0.1843 -0.0182 0.050 Uiso 1 1 calc R . . H13B H 0.1984 0.1349 -0.0677 0.050 Uiso 1 1 calc R . . C14 C 0.30813(14) 0.23708(13) 0.11143(14) 0.0426(5) Uani 1 1 d . . . H14A H 0.3698 0.2807 0.1615 0.064 Uiso 1 1 calc R . . H14B H 0.3199 0.1781 0.0897 0.064 Uiso 1 1 calc R . . H14C H 0.2559 0.2368 0.1332 0.064 Uiso 1 1 calc R . . C15 C 0.35614(12) 0.26099(11) 0.00021(12) 0.0302(4) Uani 1 1 d . . . H15A H 0.3332 0.2757 -0.0512 0.036 Uiso 1 1 calc R . . H15B H 0.3648 0.2002 -0.0238 0.036 Uiso 1 1 calc R . . C16 C 0.45811(12) 0.32578(11) 0.07247(11) 0.0275(3) Uani 1 1 d . . . C17 C 0.47684(12) 0.41819(11) 0.09767(11) 0.0263(3) Uani 1 1 d . . . C18 C 0.57674(12) 0.47368(11) 0.15783(11) 0.0278(3) Uani 1 1 d . . . C19 C 0.65239(12) 0.43568(12) 0.19231(11) 0.0311(4) Uani 1 1 d . . . H19 H 0.7177 0.4733 0.2326 0.037 Uiso 1 1 calc R . . C20 C 0.63540(12) 0.34433(12) 0.16960(12) 0.0306(4) Uani 1 1 d . . . C21 C 0.53675(12) 0.29087(11) 0.10858(12) 0.0303(4) Uani 1 1 d . . . H21 H 0.5226 0.2292 0.0911 0.036 Uiso 1 1 calc R . . C22 C 0.60612(13) 0.57008(11) 0.17593(12) 0.0322(4) Uani 1 1 d . . . H22A H 0.6793 0.5883 0.1974 0.039 Uiso 1 1 calc R . . H22B H 0.5751 0.5720 0.1172 0.039 Uiso 1 1 calc R . . C23 C 0.63494(14) 0.64419(15) 0.33677(13) 0.0482(5) Uani 1 1 d . . . H23A H 0.6185 0.6889 0.3820 0.072 Uiso 1 1 calc R . . H23B H 0.7066 0.6612 0.3538 0.072 Uiso 1 1 calc R . . H23C H 0.6169 0.5865 0.3347 0.072 Uiso 1 1 calc R . . C24 C 0.60848(14) 0.72610(13) 0.24642(15) 0.0466(5) Uani 1 1 d . . . H24A H 0.6762 0.7343 0.2484 0.056 Uiso 1 1 calc R . . H24B H 0.6111 0.7747 0.3025 0.056 Uiso 1 1 calc R . . C25 C 0.53598(14) 0.73195(14) 0.16282(16) 0.0453(5) Uani 1 1 d . . . H25A H 0.5582 0.7912 0.1683 0.054 Uiso 1 1 calc R . . H25B H 0.5385 0.6871 0.1073 0.054 Uiso 1 1 calc R . . C26 C 0.36279(18) 0.68801(16) 0.05310(15) 0.0596(6) Uani 1 1 d . . . H26A H 0.2929 0.6772 0.0437 0.089 Uiso 1 1 calc R . . H26B H 0.3741 0.6333 0.0146 0.089 Uiso 1 1 calc R . . H26C H 0.3780 0.7345 0.0368 0.089 Uiso 1 1 calc R . . C27 C 0.41147(17) 0.80132(13) 0.21039(16) 0.0495(5) Uani 1 1 d . . . H27A H 0.3410 0.8005 0.1797 0.059 Uiso 1 1 calc R . . H27B H 0.4539 0.8525 0.2149 0.059 Uiso 1 1 calc R . . C28 C 0.43282(16) 0.81517(12) 0.30718(15) 0.0489(5) Uani 1 1 d . . . H28A H 0.5053 0.8252 0.3414 0.059 Uiso 1 1 calc R . . H28B H 0.4139 0.8690 0.3390 0.059 Uiso 1 1 calc R . . C29 C 0.41873(15) 0.74727(14) 0.40303(12) 0.0468(5) Uani 1 1 d . . . H29A H 0.4893 0.7478 0.4226 0.070 Uiso 1 1 calc R . . H29B H 0.3820 0.6976 0.4044 0.070 Uiso 1 1 calc R . . H29C H 0.4122 0.8031 0.4443 0.070 Uiso 1 1 calc R . . C30 C 0.26836(13) 0.73992(11) 0.28063(13) 0.0330(4) Uani 1 1 d . . . H30A H 0.2430 0.7408 0.2211 0.040 Uiso 1 1 calc R . . H30B H 0.2660 0.7963 0.3262 0.040 Uiso 1 1 calc R . . C31 C 0.05201(13) 0.63169(12) 0.41219(12) 0.0325(4) Uani 1 1 d . . . C32 C 0.10702(15) 0.72474(13) 0.49678(12) 0.0433(5) Uani 1 1 d . . . H32A H 0.0965 0.7711 0.4776 0.065 Uiso 1 1 calc R . . H32B H 0.1786 0.7295 0.5237 0.065 Uiso 1 1 calc R . . H32C H 0.0805 0.7320 0.5421 0.065 Uiso 1 1 calc R . . C33 C -0.06214(14) 0.62637(15) 0.37192(14) 0.0493(5) Uani 1 1 d . . . H33A H -0.0726 0.6715 0.3510 0.074 Uiso 1 1 calc R . . H33B H -0.0863 0.6368 0.4192 0.074 Uiso 1 1 calc R . . H33C H -0.0988 0.5675 0.3204 0.074 Uiso 1 1 calc R . . C34 C 0.06735(18) 0.55833(14) 0.44332(15) 0.0540(6) Uani 1 1 d . . . H34A H 0.0419 0.5673 0.4896 0.081 Uiso 1 1 calc R . . H34B H 0.1386 0.5616 0.4692 0.081 Uiso 1 1 calc R . . H34C H 0.0312 0.4999 0.3907 0.081 Uiso 1 1 calc R . . C35 C 0.72317(13) 0.30700(12) 0.20818(13) 0.0361(4) Uani 1 1 d . . . C36 C 0.80684(14) 0.32590(15) 0.17859(15) 0.0471(5) Uani 1 1 d . . . H36A H 0.7812 0.2934 0.1120 0.071 Uiso 1 1 calc R . . H36B H 0.8641 0.3065 0.2067 0.071 Uiso 1 1 calc R . . H36C H 0.8277 0.3896 0.1985 0.071 Uiso 1 1 calc R . . C37 C 0.68974(15) 0.20529(14) 0.17425(17) 0.0579(6) Uani 1 1 d . . . H37A H 0.6678 0.1739 0.1080 0.087 Uiso 1 1 calc R . . H37B H 0.6345 0.1921 0.1891 0.087 Uiso 1 1 calc R . . H37C H 0.7459 0.1859 0.2042 0.087 Uiso 1 1 calc R . . C38 C 0.76803(16) 0.35533(16) 0.31487(14) 0.0548(6) Uani 1 1 d . . . H38A H 0.7164 0.3446 0.3347 0.082 Uiso 1 1 calc R . . H38B H 0.7922 0.4192 0.3372 0.082 Uiso 1 1 calc R . . H38C H 0.8236 0.3324 0.3395 0.082 Uiso 1 1 calc R . . C39 C 0.36055(15) 0.48653(13) 0.28364(12) 0.0413(5) Uani 1 1 d . . . C40 C 0.3818(3) 0.4808(2) 0.37303(16) 0.1106(14) Uani 1 1 d . . . H40A H 0.3912 0.5394 0.4216 0.166 Uiso 1 1 calc R . . H40B H 0.4424 0.4609 0.3902 0.166 Uiso 1 1 calc R . . H40C H 0.3254 0.4386 0.3642 0.166 Uiso 1 1 calc R . . B B 0.25376(15) 0.08837(13) 0.29486(14) 0.0304(4) Uani 1 1 d . . . C101 C 0.20609(12) 0.02229(11) 0.18193(12) 0.0305(4) Uani 1 1 d . . . C102 C 0.22378(14) -0.06302(12) 0.14683(12) 0.0378(4) Uani 1 1 d . . . H102 H 0.2558 -0.0847 0.1884 0.045 Uiso 1 1 calc R . . C103 C 0.19584(16) -0.11695(13) 0.05279(14) 0.0460(5) Uani 1 1 d . . . H103 H 0.2103 -0.1729 0.0329 0.055 Uiso 1 1 calc R . . C104 C 0.14705(15) -0.08836(14) -0.01127(13) 0.0472(5) Uani 1 1 d . . . H104 H 0.1275 -0.1248 -0.0744 0.057 Uiso 1 1 calc R . . C105 C 0.12764(14) -0.00471(14) 0.01981(13) 0.0449(5) Uani 1 1 d . . . H105 H 0.0948 0.0159 -0.0225 0.054 Uiso 1 1 calc R . . C106 C 0.15712(13) 0.04913(13) 0.11462(12) 0.0372(4) Uani 1 1 d . . . H106 H 0.1436 0.1055 0.1340 0.045 Uiso 1 1 calc R . . C201 C 0.24089(13) 0.03161(11) 0.35062(12) 0.0306(4) Uani 1 1 d . . . C202 C 0.15591(13) -0.04012(12) 0.31361(13) 0.0358(4) Uani 1 1 d . . . H202 H 0.1085 -0.0603 0.2526 0.043 Uiso 1 1 calc R . . C203 C 0.13894(15) -0.08266(13) 0.36370(13) 0.0419(5) Uani 1 1 d . . . H203 H 0.0807 -0.1297 0.3363 0.050 Uiso 1 1 calc R . . C204 C 0.20794(16) -0.05551(13) 0.45370(14) 0.0450(5) Uani 1 1 d . . . H204 H 0.1974 -0.0842 0.4873 0.054 Uiso 1 1 calc R . . C205 C 0.29301(16) 0.01499(14) 0.49306(14) 0.0492(5) Uani 1 1 d . . . H205 H 0.3402 0.0345 0.5540 0.059 Uiso 1 1 calc R . . C206 C 0.30855(15) 0.05688(13) 0.44249(13) 0.0413(4) Uani 1 1 d . . . H206 H 0.3668 0.1042 0.4708 0.050 Uiso 1 1 calc R . . C301 C 0.37393(13) 0.12950(12) 0.32197(11) 0.0331(4) Uani 1 1 d . . . C302 C 0.40736(15) 0.20673(13) 0.31600(13) 0.0440(5) Uani 1 1 d . . . H302 H 0.3611 0.2392 0.3014 0.053 Uiso 1 1 calc R . . C303 C 0.50683(17) 0.23700(16) 0.33102(16) 0.0599(6) Uani 1 1 d . . . H303 H 0.5262 0.2893 0.3272 0.072 Uiso 1 1 calc R . . C304 C 0.57672(16) 0.19001(19) 0.35152(16) 0.0653(7) Uani 1 1 d . . . H304 H 0.6435 0.2102 0.3618 0.078 Uiso 1 1 calc R . . C305 C 0.54697(16) 0.11296(18) 0.35673(15) 0.0572(6) Uani 1 1 d . . . H305 H 0.5936 0.0804 0.3701 0.069 Uiso 1 1 calc R . . C306 C 0.44794(14) 0.08353(14) 0.34217(13) 0.0433(5) Uani 1 1 d . . . H306 H 0.4296 0.0309 0.3459 0.052 Uiso 1 1 calc R . . C401 C 0.19486(14) 0.16795(12) 0.32347(12) 0.0358(4) Uani 1 1 d . . . C402 C 0.08944(15) 0.15108(14) 0.27803(14) 0.0449(5) Uani 1 1 d . . . H402 H 0.0525 0.0943 0.2281 0.054 Uiso 1 1 calc R . . C403 C 0.03743(19) 0.21549(17) 0.30431(17) 0.0595(6) Uani 1 1 d . . . H403 H -0.0329 0.2012 0.2721 0.071 Uiso 1 1 calc R . . C404 C 0.0891(2) 0.30001(18) 0.37747(18) 0.0658(7) Uani 1 1 d . . . H404 H 0.0545 0.3435 0.3944 0.079 Uiso 1 1 calc R . . C405 C 0.1927(2) 0.31943(16) 0.42545(17) 0.0646(7) Uani 1 1 d . . . H405 H 0.2285 0.3761 0.4759 0.077 Uiso 1 1 calc R . . C406 C 0.24448(17) 0.25417(13) 0.39863(14) 0.0482(5) Uani 1 1 d . . . H406 H 0.3146 0.2688 0.4321 0.058 Uiso 1 1 calc R . . N7 N 0.5262(2) -0.07790(19) 0.0997(2) 0.1162(10) Uani 1 1 d . . . C41 C 0.4788(2) -0.02706(17) 0.09827(17) 0.0644(6) Uani 1 1 d . . . C42 C 0.41855(17) 0.03510(15) 0.09613(18) 0.0606(6) Uani 1 1 d . . . H42A H 0.3967 0.0354 0.0370 0.091 Uiso 1 1 calc R . . H42B H 0.4581 0.0947 0.1449 0.091 Uiso 1 1 calc R . . H42C H 0.3601 0.0173 0.1050 0.091 Uiso 1 1 calc R . . N8 N -0.1167(2) 0.8550(2) 0.36340(19) 0.1024(9) Uani 1 1 d . . . C43 C -0.10155(19) 0.86306(18) 0.43443(19) 0.0637(6) Uani 1 1 d . . . C44 C -0.0834(2) 0.8725(2) 0.52524(19) 0.0856(9) Uani 1 1 d . . . H44A H -0.0229 0.9204 0.5710 0.128 Uiso 1 1 calc R . . H44B H -0.0746 0.8168 0.5269 0.128 Uiso 1 1 calc R . . H44C H -0.1404 0.8867 0.5385 0.128 Uiso 1 1 calc R . . N9 N 0.1686(5) -0.0260(4) -0.1924(5) 0.272(3) Uani 1 1 d . . . C45 C 0.1990(4) -0.0174(3) -0.2436(3) 0.1207(13) Uani 1 1 d . . . C46 C 0.2504(3) 0.0038(4) -0.2913(3) 0.163(2) Uani 1 1 d . . . H46A H 0.2024 -0.0124 -0.3534 0.245 Uiso 1 1 calc R . . H46B H 0.3009 -0.0294 -0.2938 0.245 Uiso 1 1 calc R . . H46C H 0.2828 0.0675 -0.2591 0.245 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.02132(12) 0.02595(13) 0.02332(13) 0.00971(10) 0.00798(10) 0.00485(10) Mn2 0.02513(13) 0.02525(13) 0.02536(13) 0.01182(10) 0.01058(10) 0.00482(10) S1 0.0256(2) 0.0307(2) 0.0270(2) 0.01362(17) 0.01218(17) 0.00904(17) S2 0.0238(2) 0.0302(2) 0.0262(2) 0.01305(17) 0.01027(16) 0.00758(16) N1 0.0259(7) 0.0276(7) 0.0306(7) 0.0097(6) 0.0129(6) 0.0042(6) N2 0.0267(7) 0.0352(8) 0.0256(7) 0.0103(6) 0.0080(6) 0.0060(6) N3 0.0229(7) 0.0280(7) 0.0350(8) 0.0146(6) 0.0104(6) 0.0049(6) N4 0.0282(7) 0.0297(8) 0.0308(8) 0.0095(6) 0.0098(6) 0.0063(6) N5 0.0348(8) 0.0351(8) 0.0383(8) 0.0218(7) 0.0199(7) 0.0111(6) N6 0.0296(7) 0.0302(8) 0.0317(8) 0.0083(6) 0.0160(6) 0.0011(6) O1 0.0411(7) 0.0362(7) 0.0278(6) 0.0153(6) 0.0077(6) 0.0000(6) O2 0.0478(8) 0.0351(7) 0.0303(7) 0.0175(6) 0.0042(6) -0.0036(6) C1 0.0227(8) 0.0298(9) 0.0291(8) 0.0143(7) 0.0123(7) 0.0105(7) C2 0.0254(8) 0.0272(8) 0.0331(9) 0.0138(7) 0.0144(7) 0.0086(7) C3 0.0281(9) 0.0276(9) 0.0294(9) 0.0090(7) 0.0129(7) 0.0076(7) C4 0.0259(8) 0.0324(9) 0.0295(9) 0.0135(7) 0.0133(7) 0.0099(7) C5 0.0230(8) 0.0315(9) 0.0344(9) 0.0143(8) 0.0130(7) 0.0053(7) C6 0.0221(8) 0.0285(8) 0.0289(9) 0.0113(7) 0.0098(7) 0.0083(7) C7 0.0229(8) 0.0341(9) 0.0313(9) 0.0100(8) 0.0113(7) 0.0067(7) C8 0.0413(11) 0.0399(11) 0.0505(12) 0.0239(9) 0.0260(9) 0.0096(9) C9 0.0234(8) 0.0329(10) 0.0399(10) 0.0044(8) 0.0116(8) 0.0012(7) C10 0.0254(9) 0.0454(11) 0.0277(9) 0.0052(8) 0.0033(7) 0.0099(8) C11 0.0527(13) 0.0670(15) 0.0307(10) 0.0241(10) 0.0098(9) 0.0051(11) C12 0.0264(9) 0.0378(10) 0.0334(10) -0.0010(8) 0.0071(8) 0.0034(8) C13 0.0262(9) 0.0266(9) 0.0567(12) 0.0112(9) 0.0124(9) 0.0036(7) C14 0.0402(11) 0.0477(11) 0.0587(13) 0.0367(10) 0.0251(10) 0.0198(9) C15 0.0246(8) 0.0280(9) 0.0329(9) 0.0090(7) 0.0122(7) 0.0075(7) C16 0.0233(8) 0.0310(9) 0.0282(8) 0.0117(7) 0.0130(7) 0.0077(7) C17 0.0238(8) 0.0321(9) 0.0247(8) 0.0122(7) 0.0128(7) 0.0087(7) C18 0.0240(8) 0.0301(9) 0.0286(8) 0.0110(7) 0.0137(7) 0.0061(7) C19 0.0200(8) 0.0372(10) 0.0305(9) 0.0120(8) 0.0096(7) 0.0042(7) C20 0.0245(8) 0.0375(10) 0.0327(9) 0.0165(8) 0.0143(7) 0.0109(7) C21 0.0275(9) 0.0295(9) 0.0357(9) 0.0151(8) 0.0149(7) 0.0101(7) C22 0.0258(8) 0.0335(9) 0.0361(10) 0.0138(8) 0.0153(7) 0.0047(7) C23 0.0368(11) 0.0591(13) 0.0305(10) 0.0111(9) 0.0055(8) 0.0150(10) C24 0.0320(10) 0.0305(10) 0.0664(14) 0.0145(10) 0.0192(10) 0.0038(8) C25 0.0445(11) 0.0409(11) 0.0733(14) 0.0363(11) 0.0369(11) 0.0151(9) C26 0.0658(15) 0.0680(15) 0.0486(13) 0.0413(12) 0.0142(11) 0.0047(12) C27 0.0630(13) 0.0368(11) 0.0827(16) 0.0379(11) 0.0528(13) 0.0234(10) C28 0.0550(13) 0.0256(9) 0.0631(14) 0.0066(9) 0.0401(11) -0.0003(9) C29 0.0388(11) 0.0564(13) 0.0269(10) 0.0055(9) 0.0125(8) 0.0031(9) C30 0.0355(9) 0.0274(9) 0.0390(10) 0.0134(8) 0.0209(8) 0.0092(7) C31 0.0329(9) 0.0340(9) 0.0306(9) 0.0128(8) 0.0165(8) 0.0062(7) C32 0.0464(11) 0.0437(11) 0.0346(10) 0.0097(9) 0.0226(9) 0.0060(9) C33 0.0369(11) 0.0658(14) 0.0405(11) 0.0149(10) 0.0236(9) 0.0094(10) C34 0.0809(16) 0.0470(12) 0.0455(12) 0.0248(10) 0.0347(12) 0.0177(11) C35 0.0250(9) 0.0426(10) 0.0420(10) 0.0223(9) 0.0115(8) 0.0116(8) C36 0.0317(10) 0.0619(13) 0.0571(13) 0.0317(11) 0.0218(9) 0.0218(9) C37 0.0379(11) 0.0494(13) 0.0827(17) 0.0368(12) 0.0130(11) 0.0171(10) C38 0.0486(12) 0.0737(16) 0.0453(12) 0.0350(12) 0.0133(10) 0.0212(11) C39 0.0522(12) 0.0363(10) 0.0274(9) 0.0168(8) 0.0084(9) 0.0007(9) C40 0.151(3) 0.090(2) 0.0356(13) 0.0351(15) -0.0068(16) -0.053(2) B 0.0311(10) 0.0298(10) 0.0312(10) 0.0147(8) 0.0131(8) 0.0090(8) C101 0.0271(8) 0.0320(9) 0.0331(9) 0.0151(8) 0.0137(7) 0.0060(7) C102 0.0456(11) 0.0356(10) 0.0339(10) 0.0159(8) 0.0185(9) 0.0126(8) C103 0.0576(13) 0.0342(10) 0.0432(11) 0.0107(9) 0.0276(10) 0.0070(9) C104 0.0493(12) 0.0464(12) 0.0303(10) 0.0083(9) 0.0152(9) -0.0056(10) C105 0.0405(11) 0.0548(13) 0.0349(10) 0.0230(10) 0.0102(9) 0.0047(9) C106 0.0353(10) 0.0380(10) 0.0372(10) 0.0183(8) 0.0135(8) 0.0080(8) C201 0.0317(9) 0.0287(9) 0.0317(9) 0.0123(7) 0.0151(7) 0.0103(7) C202 0.0344(10) 0.0361(10) 0.0335(10) 0.0128(8) 0.0152(8) 0.0060(8) C203 0.0468(11) 0.0327(10) 0.0437(11) 0.0122(9) 0.0245(9) 0.0023(8) C204 0.0633(13) 0.0370(11) 0.0432(11) 0.0215(9) 0.0288(10) 0.0104(10) C205 0.0577(13) 0.0484(12) 0.0348(11) 0.0224(10) 0.0113(10) 0.0032(10) C206 0.0427(11) 0.0367(10) 0.0346(10) 0.0156(8) 0.0096(8) -0.0022(8) C301 0.0336(9) 0.0349(10) 0.0246(9) 0.0111(7) 0.0100(7) 0.0036(8) C302 0.0429(11) 0.0469(12) 0.0410(11) 0.0228(9) 0.0153(9) 0.0050(9) C303 0.0495(13) 0.0669(16) 0.0588(14) 0.0346(13) 0.0169(11) -0.0079(11) C304 0.0316(11) 0.102(2) 0.0575(14) 0.0436(15) 0.0109(10) -0.0022(12) C305 0.0367(11) 0.0892(18) 0.0537(13) 0.0400(13) 0.0186(10) 0.0209(11) C306 0.0377(10) 0.0509(12) 0.0424(11) 0.0230(10) 0.0163(9) 0.0119(9) C401 0.0474(11) 0.0352(10) 0.0340(10) 0.0194(8) 0.0221(9) 0.0160(8) C402 0.0475(12) 0.0497(12) 0.0470(12) 0.0252(10) 0.0246(10) 0.0225(10) C403 0.0647(15) 0.0791(17) 0.0703(16) 0.0497(15) 0.0425(13) 0.0460(14) C404 0.103(2) 0.0671(16) 0.0707(17) 0.0449(14) 0.0593(16) 0.0593(16) C405 0.107(2) 0.0436(13) 0.0552(14) 0.0204(11) 0.0478(15) 0.0315(14) C406 0.0648(14) 0.0403(11) 0.0410(11) 0.0169(9) 0.0254(10) 0.0177(10) N7 0.132(2) 0.0887(19) 0.113(2) 0.0345(17) 0.0412(19) 0.0657(19) C41 0.0738(17) 0.0521(14) 0.0611(16) 0.0227(12) 0.0253(13) 0.0182(13) C42 0.0573(14) 0.0521(14) 0.0792(17) 0.0300(13) 0.0362(13) 0.0154(11) N8 0.106(2) 0.132(2) 0.0783(18) 0.0480(18) 0.0492(17) 0.0271(18) C43 0.0611(15) 0.0703(17) 0.0683(17) 0.0288(14) 0.0389(14) 0.0222(13) C44 0.116(2) 0.098(2) 0.080(2) 0.0475(17) 0.0643(19) 0.068(2) N9 0.427(10) 0.161(4) 0.302(7) 0.077(5) 0.276(7) 0.042(5) C45 0.148(4) 0.090(3) 0.125(3) 0.032(2) 0.078(3) 0.037(2) C46 0.165(4) 0.277(6) 0.092(3) 0.097(4) 0.073(3) 0.121(4) #BOND LENGHTS AND ANGLES _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 O1 2.0909(14) . ? Mn1 N3 2.3369(15) . ? Mn1 N2 2.3545(19) . ? Mn1 N1 2.4065(14) . ? Mn1 S1 2.6017(7) . ? Mn1 S2 2.6166(8) . ? Mn2 O2 2.0829(13) . ? Mn2 N5 2.3331(15) . ? Mn2 N6 2.3804(16) . ? Mn2 N4 2.4010(16) . ? Mn2 S2 2.5880(13) . ? Mn2 S1 2.6301(12) . ? S1 C1 1.7713(17) . ? S2 C17 1.7723(17) . ? N1 C8 1.480(2) . ? N1 C9 1.489(2) . ? N1 C7 1.490(2) . ? N2 C10 1.478(2) . ? N2 C11 1.480(2) . ? N2 C12 1.485(2) . ? N3 C13 1.476(2) . ? N3 C14 1.480(2) . ? N3 C15 1.488(2) . ? N4 C23 1.473(2) . ? N4 C24 1.484(2) . ? N4 C22 1.488(2) . ? N5 C27 1.476(2) . ? N5 C25 1.478(2) . ? N5 C26 1.479(2) . ? N6 C29 1.476(2) . ? N6 C28 1.484(2) . ? N6 C30 1.490(2) . ? O1 C39 1.249(2) . ? O2 C39 1.249(2) . ? C1 C6 1.404(2) . ? C1 C2 1.404(2) . ? C2 C3 1.396(2) . ? C2 C30 1.508(2) . ? C3 C4 1.388(2) . ? C4 C5 1.393(2) . ? C4 C31 1.533(2) . ? C5 C6 1.388(2) . ? C6 C7 1.503(2) . ? C9 C10 1.498(3) . ? C12 C13 1.510(3) . ? C15 C16 1.507(2) . ? C16 C21 1.393(2) . ? C16 C17 1.398(2) . ? C17 C18 1.410(2) . ? C18 C19 1.389(2) . ? C18 C22 1.503(2) . ? C19 C20 1.390(2) . ? C20 C21 1.390(2) . ? C20 C35 1.528(2) . ? C24 C25 1.506(3) . ? C27 C28 1.504(3) . ? C31 C34 1.527(3) . ? C31 C32 1.530(3) . ? C31 C33 1.537(3) . ? C35 C37 1.526(3) . ? C35 C36 1.532(3) . ? C35 C38 1.534(3) . ? C39 C40 1.510(3) . ? B C201 1.641(3) . ? B C101 1.645(3) . ? B C301 1.646(3) . ? B C401 1.648(3) . ? C101 C102 1.396(2) . ? C101 C106 1.397(2) . ? C102 C103 1.386(3) . ? C103 C104 1.373(3) . ? C104 C105 1.377(3) . ? C105 C106 1.393(3) . ? C201 C202 1.396(2) . ? C201 C206 1.401(2) . ? C202 C203 1.389(3) . ? C203 C204 1.375(3) . ? C204 C205 1.378(3) . ? C205 C206 1.381(3) . ? C301 C302 1.395(3) . ? C301 C306 1.401(3) . ? C302 C303 1.387(3) . ? C303 C304 1.372(3) . ? C304 C305 1.370(3) . ? C305 C306 1.381(3) . ? C401 C402 1.396(3) . ? C401 C406 1.396(3) . ? C402 C403 1.389(3) . ? C403 C404 1.371(4) . ? C404 C405 1.373(4) . ? C405 C406 1.399(3) . ? N7 C41 1.142(3) . ? C41 C42 1.419(3) . ? N8 C43 1.117(3) . ? C43 C44 1.436(4) . ? N9 C45 1.170(5) . ? C45 C46 1.410(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 O1 Mn1 N3 88.79(6) . . ? O1 Mn1 N2 155.22(5) . . ? N3 Mn1 N2 77.48(6) . . ? O1 Mn1 N1 86.75(6) . . ? N3 Mn1 N1 102.69(5) . . ? N2 Mn1 N1 76.50(6) . . ? O1 Mn1 S1 95.47(5) . . ? N3 Mn1 S1 168.15(4) . . ? N2 Mn1 S1 102.14(5) . . ? N1 Mn1 S1 88.62(5) . . ? O1 Mn1 S2 102.63(5) . . ? N3 Mn1 S2 87.87(4) . . ? N2 Mn1 S2 97.42(5) . . ? N1 Mn1 S2 166.13(4) . . ? S1 Mn1 S2 80.41(3) . . ? O2 Mn2 N5 155.82(5) . . ? O2 Mn2 N6 87.04(5) . . ? N5 Mn2 N6 77.63(5) . . ? O2 Mn2 N4 88.67(6) . . ? N5 Mn2 N4 77.12(6) . . ? N6 Mn2 N4 103.64(7) . . ? O2 Mn2 S2 99.38(4) . . ? N5 Mn2 S2 99.48(4) . . ? N6 Mn2 S2 167.19(4) . . ? N4 Mn2 S2 87.67(6) . . ? O2 Mn2 S1 100.40(5) . . ? N5 Mn2 S1 97.55(5) . . ? N6 Mn2 S1 87.56(6) . . ? N4 Mn2 S1 166.02(4) . . ? S2 Mn2 S1 80.41(5) . . ? C1 S1 Mn1 100.66(6) . . ? C1 S1 Mn2 102.01(6) . . ? Mn1 S1 Mn2 82.67(4) . . ? C17 S2 Mn2 103.30(6) . . ? C17 S2 Mn1 103.87(6) . . ? Mn2 S2 Mn1 83.20(4) . . ? C8 N1 C9 109.83(14) . . ? C8 N1 C7 108.50(13) . . ? C9 N1 C7 106.18(13) . . ? C8 N1 Mn1 114.02(10) . . ? C9 N1 Mn1 107.50(10) . . ? C7 N1 Mn1 110.53(10) . . ? C10 N2 C11 108.11(15) . . ? C10 N2 C12 111.23(14) . . ? C11 N2 C12 109.63(15) . . ? C10 N2 Mn1 106.76(10) . . ? C11 N2 Mn1 112.36(11) . . ? C12 N2 Mn1 108.75(11) . . ? C13 N3 C14 108.37(14) . . ? C13 N3 C15 108.56(14) . . ? C14 N3 C15 109.32(13) . . ? C13 N3 Mn1 103.68(10) . . ? C14 N3 Mn1 113.48(11) . . ? C15 N3 Mn1 113.11(10) . . ? C23 N4 C24 109.61(15) . . ? C23 N4 C22 108.64(14) . . ? C24 N4 C22 106.90(14) . . ? C23 N4 Mn2 113.66(12) . . ? C24 N4 Mn2 105.55(11) . . ? C22 N4 Mn2 112.21(10) . . ? C27 N5 C25 111.36(15) . . ? C27 N5 C26 108.92(16) . . ? C25 N5 C26 107.54(16) . . ? C27 N5 Mn2 108.89(10) . . ? C25 N5 Mn2 108.82(11) . . ? C26 N5 Mn2 111.31(12) . . ? C29 N6 C28 108.67(15) . . ? C29 N6 C30 108.11(14) . . ? C28 N6 C30 107.76(15) . . ? C29 N6 Mn2 114.44(12) . . ? C28 N6 Mn2 105.00(10) . . ? C30 N6 Mn2 112.58(11) . . ? C39 O1 Mn1 134.40(12) . . ? C39 O2 Mn2 132.65(12) . . ? C6 C1 C2 118.27(15) . . ? C6 C1 S1 120.77(13) . . ? C2 C1 S1 120.89(12) . . ? C3 C2 C1 120.02(15) . . ? C3 C2 C30 118.56(15) . . ? C1 C2 C30 121.08(15) . . ? C4 C3 C2 122.46(16) . . ? C3 C4 C5 116.36(15) . . ? C3 C4 C31 124.15(15) . . ? C5 C4 C31 119.47(15) . . ? C6 C5 C4 123.13(15) . . ? C5 C6 C1 119.64(15) . . ? C5 C6 C7 118.37(15) . . ? C1 C6 C7 121.43(15) . . ? N1 C7 C6 117.11(14) . . ? N1 C9 C10 111.56(14) . . ? N2 C10 C9 113.02(15) . . ? N2 C12 C13 113.72(15) . . ? N3 C13 C12 112.86(15) . . ? N3 C15 C16 114.82(13) . . ? C21 C16 C17 120.00(15) . . ? C21 C16 C15 118.60(15) . . ? C17 C16 C15 121.19(15) . . ? C16 C17 C18 118.51(15) . . ? C16 C17 S2 121.03(12) . . ? C18 C17 S2 120.41(13) . . ? C19 C18 C17 119.27(15) . . ? C19 C18 C22 118.91(15) . . ? C17 C18 C22 121.37(15) . . ? C18 C19 C20 123.34(15) . . ? C21 C20 C19 116.16(15) . . ? C21 C20 C35 123.49(16) . . ? C19 C20 C35 120.31(15) . . ? C20 C21 C16 122.70(16) . . ? N4 C22 C18 116.60(14) . . ? N4 C24 C25 112.13(15) . . ? N5 C25 C24 113.24(16) . . ? N5 C27 C28 114.33(16) . . ? N6 C28 C27 112.60(16) . . ? N6 C30 C2 115.79(14) . . ? C34 C31 C32 109.24(16) . . ? C34 C31 C4 109.30(15) . . ? C32 C31 C4 112.00(14) . . ? C34 C31 C33 108.94(17) . . ? C32 C31 C33 107.85(16) . . ? C4 C31 C33 109.45(14) . . ? C37 C35 C20 112.51(15) . . ? C37 C35 C36 108.63(17) . . ? C20 C35 C36 109.47(15) . . ? C37 C35 C38 108.70(17) . . ? C20 C35 C38 109.12(16) . . ? C36 C35 C38 108.33(16) . . ? O2 C39 O1 125.91(17) . . ? O2 C39 C40 117.58(18) . . ? O1 C39 C40 116.50(18) . . ? C201 B C101 111.49(14) . . ? C201 B C301 112.31(14) . . ? C101 B C301 103.21(14) . . ? C201 B C401 104.38(14) . . ? C101 B C401 112.92(14) . . ? C301 B C401 112.79(15) . . ? C102 C101 C106 114.67(16) . . ? C102 C101 B 120.63(15) . . ? C106 C101 B 124.25(16) . . ? C103 C102 C101 122.98(18) . . ? C104 C103 C102 120.53(19) . . ? C103 C104 C105 118.75(18) . . ? C104 C105 C106 120.06(19) . . ? C105 C106 C101 123.00(18) . . ? C202 C201 C206 114.49(16) . . ? C202 C201 B 122.43(15) . . ? C206 C201 B 122.76(15) . . ? C203 C202 C201 123.03(17) . . ? C204 C203 C202 120.24(18) . . ? C203 C204 C205 118.73(18) . . ? C204 C205 C206 120.33(19) . . ? C205 C206 C201 123.17(18) . . ? C302 C301 C306 114.88(17) . . ? C302 C301 B 122.60(16) . . ? C306 C301 B 122.12(16) . . ? C303 C302 C301 122.7(2) . . ? C304 C303 C302 120.2(2) . . ? C305 C304 C303 119.2(2) . . ? C304 C305 C306 120.2(2) . . ? C305 C306 C301 122.8(2) . . ? C402 C401 C406 115.07(18) . . ? C402 C401 B 121.70(17) . . ? C406 C401 B 123.04(17) . . ? C403 C402 C401 122.8(2) . . ? C404 C403 C402 120.4(2) . . ? C403 C404 C405 119.0(2) . . ? C404 C405 C406 120.2(2) . . ? C401 C406 C405 122.5(2) . . ? N7 C41 C42 179.1(3) . . ? N8 C43 C44 179.2(4) . . ? N9 C45 C46 170.1(6) . . ? data_3 _database_code_depnum_ccdc_archive 'CCDC 281647' _chemical_formula_structural ; [(LMe)Fe2(OAc)](BPh4)(MeCN)2(EtOH)0.5 ; _chemical_formula_sum 'C69 H96 B Fe2 N8 O2.50 S2' _chemical_formula_weight 1264.17 _chemical_melting_point ? _chemical_compound_source ; Crystals were grown by recrystallization from a mixed acetonitrile/ethanol solvent system ; #CRYSTAL DATA _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 14.568(3) _cell_length_b 16.775(3) _cell_length_c 17.512(4) _cell_angle_alpha 113.66(3) _cell_angle_beta 110.39(3) _cell_angle_gamma 95.10(3) _cell_volume 3541.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pale-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_F_000 1350 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _diffrn_radiation_type MoK\a _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'BRUKER AXS' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32034 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1399 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.32 #REFINEMENT DATA _reflns_number_total 16460 _reflns_number_gt 6953 _reflns_threshold_expression >2sigma(I) _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^)+(0.0598P)^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 16460 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1371 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.544 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.059 _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (FARRUGIA)' _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. ; #ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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' B B 0.0013 0.0007 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.22607(4) 0.39978(3) 0.06789(3) 0.03752(14) Uani 1 1 d . . . Fe2 Fe 0.39442(4) 0.60906(3) 0.19200(3) 0.03900(14) Uani 1 1 d . . . S1 S 0.20159(7) 0.55614(6) 0.10612(6) 0.0406(2) Uani 1 1 d . . . S2 S 0.37856(7) 0.46849(6) 0.05710(6) 0.0412(2) Uani 1 1 d . . . N1 N 0.0654(2) 0.35525(19) 0.06956(19) 0.0430(7) Uani 1 1 d . . . N2 N 0.1210(2) 0.3218(2) -0.08302(18) 0.0452(8) Uani 1 1 d . . . N3 N 0.2722(2) 0.26554(19) 0.0302(2) 0.0429(7) Uani 1 1 d . . . N4 N 0.5737(2) 0.6398(2) 0.2428(2) 0.0489(8) Uani 1 1 d . . . N5 N 0.4245(2) 0.7130(2) 0.1472(2) 0.0499(8) Uani 1 1 d . . . N6 N 0.3766(2) 0.7382(2) 0.3027(2) 0.0486(8) Uani 1 1 d . . . O1 O 0.28890(19) 0.42446(17) 0.20104(16) 0.0505(7) Uani 1 1 d . . . O2 O 0.4072(2) 0.55637(17) 0.27957(16) 0.0550(7) Uani 1 1 d . . . C1 C 0.1600(2) 0.5788(2) 0.1944(2) 0.0381(8) Uani 1 1 d . . . C2 C 0.2006(3) 0.6621(2) 0.2734(2) 0.0389(8) Uani 1 1 d . . . C3 C 0.1677(3) 0.6766(2) 0.3429(2) 0.0446(9) Uani 1 1 d . . . H3 H 0.1957 0.7324 0.3953 0.053 Uiso 1 1 calc R . . C4 C 0.0962(3) 0.6130(2) 0.3382(2) 0.0433(9) Uani 1 1 d . . . C5 C 0.0542(3) 0.5326(2) 0.2570(2) 0.0448(9) Uani 1 1 d . . . H5 H 0.0042 0.4885 0.2503 0.054 Uiso 1 1 calc R . . C6 C 0.0827(3) 0.5143(2) 0.1853(2) 0.0394(8) Uani 1 1 d . . . C7 C 0.0202(3) 0.4327(2) 0.0945(2) 0.0441(9) Uani 1 1 d . . . H7A H -0.0441 0.4115 0.0943 0.053 Uiso 1 1 calc R . . H7B H 0.0055 0.4513 0.0467 0.053 Uiso 1 1 calc R . . C8 C 0.0694(3) 0.3152(3) 0.1320(3) 0.0617(11) Uani 1 1 d . . . H8A H 0.0948 0.2629 0.1147 0.093 Uiso 1 1 calc R . . H8B H 0.0024 0.2981 0.1277 0.093 Uiso 1 1 calc R . . H8C H 0.1136 0.3588 0.1941 0.093 Uiso 1 1 calc R . . C9 C -0.0054(3) 0.2894(3) -0.0270(2) 0.0552(11) Uani 1 1 d . . . H9A H -0.0750 0.2879 -0.0351 0.066 Uiso 1 1 calc R . . H9B H 0.0033 0.2295 -0.0393 0.066 Uiso 1 1 calc R . . C10 C 0.0147(3) 0.3154(3) -0.0933(2) 0.0548(11) Uani 1 1 d . . . H10A H -0.0311 0.2710 -0.1555 0.066 Uiso 1 1 calc R . . H10B H 0.0006 0.3732 -0.0838 0.066 Uiso 1 1 calc R . . C11 C 0.1377(3) 0.3688(3) -0.1349(3) 0.0769(14) Uani 1 1 d . . . H11A H 0.2049 0.3719 -0.1322 0.115 Uiso 1 1 calc R . . H11B H 0.1302 0.4289 -0.1082 0.115 Uiso 1 1 calc R . . H11C H 0.0887 0.3362 -0.1978 0.115 Uiso 1 1 calc R . . C12 C 0.1371(3) 0.2305(3) -0.1212(3) 0.0605(12) Uani 1 1 d . . . H12A H 0.1833 0.2309 -0.1498 0.073 Uiso 1 1 calc R . . H12B H 0.0728 0.1879 -0.1687 0.073 Uiso 1 1 calc R . . C13 C 0.1797(3) 0.1983(3) -0.0502(3) 0.0614(12) Uani 1 1 d . . . H13A H 0.1285 0.1869 -0.0296 0.074 Uiso 1 1 calc R . . H13B H 0.1961 0.1420 -0.0780 0.074 Uiso 1 1 calc R . . C14 C 0.3003(3) 0.2387(3) 0.1049(3) 0.0636(12) Uani 1 1 d . . . H14A H 0.3617 0.2811 0.1558 0.095 Uiso 1 1 calc R . . H14B H 0.3109 0.1795 0.0825 0.095 Uiso 1 1 calc R . . H14C H 0.2466 0.2383 0.1247 0.095 Uiso 1 1 calc R . . C15 C 0.3569(3) 0.2661(2) 0.0007(2) 0.0458(9) Uani 1 1 d . . . H15A H 0.3372 0.2814 -0.0495 0.055 Uiso 1 1 calc R . . H15B H 0.3653 0.2055 -0.0229 0.055 Uiso 1 1 calc R . . C16 C 0.4577(3) 0.3298(2) 0.0740(2) 0.0402(9) Uani 1 1 d . . . C17 C 0.4760(3) 0.4225(2) 0.1002(2) 0.0404(9) Uani 1 1 d . . . C18 C 0.5766(3) 0.4775(2) 0.1597(2) 0.0426(9) Uani 1 1 d . . . C19 C 0.6514(3) 0.4393(3) 0.1926(2) 0.0487(10) Uani 1 1 d . . . H19 H 0.7167 0.4768 0.2325 0.058 Uiso 1 1 calc R . . C20 C 0.6345(3) 0.3478(3) 0.1693(2) 0.0454(9) Uani 1 1 d . . . C21 C 0.5356(3) 0.2948(3) 0.1091(2) 0.0470(9) Uani 1 1 d . . . H21 H 0.5211 0.2333 0.0916 0.056 Uiso 1 1 calc R . . C22 C 0.6050(3) 0.5731(2) 0.1773(2) 0.0477(10) Uani 1 1 d . . . H22A H 0.6782 0.5925 0.2002 0.057 Uiso 1 1 calc R . . H22B H 0.5755 0.5745 0.1191 0.057 Uiso 1 1 calc R . . C23 C 0.6292(3) 0.6464(3) 0.3349(3) 0.0743(14) Uani 1 1 d . . . H23A H 0.6120 0.6910 0.3789 0.111 Uiso 1 1 calc R . . H23B H 0.7010 0.6634 0.3527 0.111 Uiso 1 1 calc R . . H23C H 0.6105 0.5889 0.3328 0.111 Uiso 1 1 calc R . . C24 C 0.6039(3) 0.7276(3) 0.2451(3) 0.0732(14) Uani 1 1 d . . . H24A H 0.6721 0.7372 0.2486 0.088 Uiso 1 1 calc R . . H24B H 0.6041 0.7759 0.2995 0.088 Uiso 1 1 calc R . . C25 C 0.5312(3) 0.7302(3) 0.1600(3) 0.0696(13) Uani 1 1 d . . . H25A H 0.5519 0.7889 0.1643 0.084 Uiso 1 1 calc R . . H25B H 0.5360 0.6853 0.1064 0.084 Uiso 1 1 calc R . . C26 C 0.3595(4) 0.6800(3) 0.0480(3) 0.0881(16) Uani 1 1 d . . . H26A H 0.2893 0.6689 0.0374 0.132 Uiso 1 1 calc R . . H26B H 0.3722 0.6251 0.0124 0.132 Uiso 1 1 calc R . . H26C H 0.3751 0.7248 0.0301 0.132 Uiso 1 1 calc R . . C27 C 0.4014(4) 0.7966(3) 0.2004(3) 0.0752(14) Uani 1 1 d . . . H27A H 0.3296 0.7912 0.1700 0.090 Uiso 1 1 calc R . . H27B H 0.4393 0.8473 0.2006 0.090 Uiso 1 1 calc R . . C28 C 0.4268(4) 0.8158(3) 0.2981(3) 0.0759(14) Uani 1 1 d . . . H28A H 0.4998 0.8292 0.3312 0.091 Uiso 1 1 calc R . . H28B H 0.4054 0.8685 0.3278 0.091 Uiso 1 1 calc R . . C29 C 0.4236(3) 0.7511(3) 0.3980(3) 0.0728(13) Uani 1 1 d . . . H29A H 0.4937 0.7511 0.4145 0.109 Uiso 1 1 calc R . . H29B H 0.3886 0.7028 0.4022 0.109 Uiso 1 1 calc R . . H29C H 0.4189 0.8076 0.4391 0.109 Uiso 1 1 calc R . . C30 C 0.2685(3) 0.7394(2) 0.2794(3) 0.0476(10) Uani 1 1 d . . . H30A H 0.2407 0.7402 0.2207 0.057 Uiso 1 1 calc R . . H30B H 0.2665 0.7952 0.3252 0.057 Uiso 1 1 calc R . . C31 C 0.0588(3) 0.6276(3) 0.4129(2) 0.0525(10) Uani 1 1 d . . . C32 C 0.1127(3) 0.7195(3) 0.4961(3) 0.0701(13) Uani 1 1 d . . . H32A H 0.0902 0.7242 0.5428 0.105 Uiso 1 1 calc R . . H32B H 0.0974 0.7659 0.4787 0.105 Uiso 1 1 calc R . . H32C H 0.1848 0.7267 0.5196 0.105 Uiso 1 1 calc R . . C33 C -0.0544(3) 0.6216(3) 0.3749(3) 0.0911(17) Uani 1 1 d . . . H33A H -0.0911 0.5626 0.3243 0.137 Uiso 1 1 calc R . . H33B H -0.0658 0.6664 0.3541 0.137 Uiso 1 1 calc R . . H33C H -0.0776 0.6321 0.4222 0.137 Uiso 1 1 calc R . . C34 C 0.0756(4) 0.5554(3) 0.4428(3) 0.0982(18) Uani 1 1 d . . . H34A H 0.0327 0.4978 0.3930 0.147 Uiso 1 1 calc R . . H34B H 0.0594 0.5684 0.4945 0.147 Uiso 1 1 calc R . . H34C H 0.1454 0.5541 0.4599 0.147 Uiso 1 1 calc R . . C35 C 0.7211(3) 0.3098(3) 0.2071(3) 0.0567(11) Uani 1 1 d . . . C36 C 0.8054(3) 0.3287(3) 0.1779(3) 0.0793(14) Uani 1 1 d . . . H36A H 0.7811 0.2940 0.1125 0.119 Uiso 1 1 calc R . . H36B H 0.8636 0.3121 0.2080 0.119 Uiso 1 1 calc R . . H36C H 0.8241 0.3918 0.1951 0.119 Uiso 1 1 calc R . . C37 C 0.6882(4) 0.2087(3) 0.1731(4) 0.1041(19) Uani 1 1 d . . . H37A H 0.6320 0.1949 0.1864 0.156 Uiso 1 1 calc R . . H37B H 0.7438 0.1898 0.2034 0.156 Uiso 1 1 calc R . . H37C H 0.6680 0.1776 0.1079 0.156 Uiso 1 1 calc R . . C38 C 0.7670(4) 0.3589(4) 0.3130(3) 0.0941(17) Uani 1 1 d . . . H38A H 0.7909 0.4226 0.3347 0.141 Uiso 1 1 calc R . . H38B H 0.8226 0.3364 0.3370 0.141 Uiso 1 1 calc R . . H38C H 0.7159 0.3485 0.3333 0.141 Uiso 1 1 calc R . . C39 C 0.3557(3) 0.4882(3) 0.2729(3) 0.0547(11) Uani 1 1 d . . . C40 C 0.3745(5) 0.4809(4) 0.3604(3) 0.142(3) Uani 1 1 d . . . H40A H 0.4416 0.5167 0.4060 0.213 Uiso 1 1 calc R . . H40B H 0.3681 0.4190 0.3478 0.213 Uiso 1 1 calc R . . H40C H 0.3255 0.5025 0.3828 0.213 Uiso 1 1 calc R . . B B 0.2488(3) 0.0870(3) 0.2931(3) 0.0461(11) Uani 1 1 d . . . C101 C 0.2027(3) 0.0214(3) 0.1811(2) 0.0463(9) Uani 1 1 d . . . C102 C 0.2175(3) -0.0650(3) 0.1443(3) 0.0572(11) Uani 1 1 d . . . H102 H 0.2470 -0.0881 0.1844 0.069 Uiso 1 1 calc R . . C103 C 0.1911(3) -0.1173(3) 0.0525(3) 0.0669(12) Uani 1 1 d . . . H103 H 0.2042 -0.1736 0.0322 0.080 Uiso 1 1 calc R . . C104 C 0.1456(3) -0.0872(3) -0.0093(3) 0.0734(14) Uani 1 1 d . . . H104 H 0.1269 -0.1230 -0.0717 0.088 Uiso 1 1 calc R . . C105 C 0.1280(3) -0.0035(3) 0.0217(3) 0.0701(13) Uani 1 1 d . . . H105 H 0.0971 0.0178 -0.0197 0.084 Uiso 1 1 calc R . . C106 C 0.1565(3) 0.0498(3) 0.1154(3) 0.0587(11) Uani 1 1 d . . . H106 H 0.1443 0.1065 0.1350 0.070 Uiso 1 1 calc R . . C201 C 0.2365(3) 0.0304(3) 0.3478(3) 0.0473(9) Uani 1 1 d . . . C202 C 0.1524(3) -0.0422(3) 0.3113(3) 0.0572(11) Uani 1 1 d . . . H202 H 0.1053 -0.0628 0.2510 0.069 Uiso 1 1 calc R . . C203 C 0.1356(3) -0.0850(3) 0.3601(3) 0.0640(12) Uani 1 1 d . . . H203 H 0.0782 -0.1329 0.3327 0.077 Uiso 1 1 calc R . . C204 C 0.2037(4) -0.0568(3) 0.4492(3) 0.0690(13) Uani 1 1 d . . . H204 H 0.1927 -0.0850 0.4826 0.083 Uiso 1 1 calc R . . C205 C 0.2880(4) 0.0134(3) 0.4881(3) 0.0787(14) Uani 1 1 d . . . H205 H 0.3352 0.0328 0.5481 0.094 Uiso 1 1 calc R . . C206 C 0.3030(3) 0.0559(3) 0.4375(3) 0.0659(12) Uani 1 1 d . . . H206 H 0.3606 0.1037 0.4656 0.079 Uiso 1 1 calc R . . C301 C 0.3675(3) 0.1302(3) 0.3206(2) 0.0502(10) Uani 1 1 d . . . C302 C 0.4001(3) 0.2071(3) 0.3157(3) 0.0706(13) Uani 1 1 d . . . H302 H 0.3529 0.2384 0.3008 0.085 Uiso 1 1 calc R . . C303 C 0.4988(4) 0.2400(4) 0.3315(4) 0.0969(18) Uani 1 1 d . . . H303 H 0.5162 0.2917 0.3263 0.116 Uiso 1 1 calc R . . C304 C 0.5703(4) 0.1970(5) 0.3546(4) 0.107(2) Uani 1 1 d . . . H304 H 0.6374 0.2204 0.3677 0.129 Uiso 1 1 calc R . . C305 C 0.5429(4) 0.1184(5) 0.3586(3) 0.0977(18) Uani 1 1 d . . . H305 H 0.5906 0.0870 0.3717 0.117 Uiso 1 1 calc R . . C306 C 0.4431(3) 0.0866(3) 0.3426(3) 0.0688(12) Uani 1 1 d . . . H306 H 0.4258 0.0343 0.3468 0.083 Uiso 1 1 calc R . . C401 C 0.1884(3) 0.1641(3) 0.3199(3) 0.0526(10) Uani 1 1 d . . . C402 C 0.0835(3) 0.1472(3) 0.2735(3) 0.0683(12) Uani 1 1 d . . . H402 H 0.0476 0.0909 0.2232 0.082 Uiso 1 1 calc R . . C403 C 0.0299(4) 0.2099(4) 0.2985(4) 0.0901(16) Uani 1 1 d . . . H403 H -0.0401 0.1954 0.2659 0.108 Uiso 1 1 calc R . . C404 C 0.0821(6) 0.2948(4) 0.3726(4) 0.100(2) Uani 1 1 d . . . H404 H 0.0475 0.3381 0.3892 0.120 Uiso 1 1 calc R . . C405 C 0.1839(5) 0.3140(4) 0.4207(4) 0.0973(18) Uani 1 1 d . . . H405 H 0.2186 0.3702 0.4716 0.117 Uiso 1 1 calc R . . C406 C 0.23754(16) 0.24998(14) 0.39469(15) 0.0749(13) Uani 1 1 d . . . H406 H 0.3075 0.2652 0.4281 0.090 Uiso 1 1 calc R . . N7 N 0.51774(16) -0.07174(14) 0.08929(15) 0.206(3) Uani 1 1 d R . . C41 C 0.47914(16) -0.02304(14) 0.09569(15) 0.111(2) Uani 1 1 d R . . C42 C 0.41864(16) 0.03796(14) 0.10079(15) 0.0955(17) Uani 1 1 d R . . H42A H 0.3953 0.0432 0.0450 0.143 Uiso 1 1 calc R . . H42B H 0.4580 0.0960 0.1519 0.143 Uiso 1 1 calc R . . H42C H 0.3613 0.0163 0.1090 0.143 Uiso 1 1 calc R . . N8 N 0.88193(16) 0.83866(14) 0.36059(15) 0.198(3) Uani 1 1 d R . . C43 C 0.89943(16) 0.85546(14) 0.43079(15) 0.107(2) Uani 1 1 d R . . C44 C 0.91434(16) 0.87256(14) 0.52419(15) 0.134(2) Uani 1 1 d R . . H44A H 0.8640 0.9005 0.5390 0.201 Uiso 1 1 calc R . . H44B H 0.9808 0.9119 0.5674 0.201 Uiso 1 1 calc R . . H44C H 0.9079 0.8164 0.5270 0.201 Uiso 1 1 calc R . . O3 O 0.19581(16) -0.02170(14) -0.25494(15) 0.255(8) Uani 0.50 1 d PR . . H3O H 0.1831 -0.0860 -0.2880 0.382 Uiso 0.50 1 d PR . . C45 C 0.2406(8) -0.0187(10) -0.2979(8) 0.216(13) Uani 0.50 1 d P . . H45A H 0.2022 -0.0374 -0.3620 0.259 Uiso 0.50 1 d PR . . H45B H 0.3048 -0.0328 -0.2891 0.259 Uiso 0.50 1 d PR . . C46 C 0.2528(8) 0.0625(10) -0.2515(8) 0.177(7) Uani 0.50 1 d PR . . H46A H 0.2894 0.0964 -0.2698 0.266 Uiso 0.50 1 calc PR . . H46B H 0.2908 0.0795 -0.1877 0.266 Uiso 0.50 1 calc PR . . H46C H 0.1878 0.0749 -0.2608 0.266 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0322(3) 0.0406(3) 0.0345(3) 0.0149(2) 0.0114(2) 0.0085(2) Fe2 0.0378(3) 0.0399(3) 0.0402(3) 0.0198(3) 0.0164(2) 0.0079(2) S1 0.0383(5) 0.0459(6) 0.0398(5) 0.0203(4) 0.0178(4) 0.0132(5) S2 0.0356(5) 0.0471(6) 0.0417(5) 0.0213(4) 0.0159(4) 0.0128(4) N1 0.0356(17) 0.0438(18) 0.0430(17) 0.0143(15) 0.0174(14) 0.0069(15) N2 0.0350(18) 0.055(2) 0.0352(16) 0.0143(15) 0.0107(14) 0.0114(16) N3 0.0298(17) 0.0436(18) 0.0534(19) 0.0230(16) 0.0151(15) 0.0089(14) N4 0.0417(19) 0.046(2) 0.0481(19) 0.0166(16) 0.0135(16) 0.0086(16) N5 0.051(2) 0.052(2) 0.061(2) 0.0349(18) 0.0296(17) 0.0140(17) N6 0.048(2) 0.0419(19) 0.0456(18) 0.0111(15) 0.0227(16) 0.0001(16) O1 0.0517(16) 0.0488(16) 0.0390(14) 0.0211(13) 0.0087(13) 0.0000(14) O2 0.0615(18) 0.0469(17) 0.0419(15) 0.0223(13) 0.0083(13) -0.0050(14) C1 0.032(2) 0.041(2) 0.043(2) 0.0195(18) 0.0153(17) 0.0134(17) C2 0.037(2) 0.035(2) 0.043(2) 0.0163(18) 0.0182(17) 0.0088(17) C3 0.045(2) 0.040(2) 0.039(2) 0.0110(18) 0.0167(18) 0.0082(19) C4 0.040(2) 0.048(2) 0.041(2) 0.0181(19) 0.0182(18) 0.0113(19) C5 0.036(2) 0.046(2) 0.047(2) 0.0175(19) 0.0182(18) 0.0048(18) C6 0.034(2) 0.040(2) 0.038(2) 0.0134(17) 0.0140(17) 0.0108(17) C7 0.033(2) 0.047(2) 0.044(2) 0.0125(18) 0.0175(17) 0.0100(18) C8 0.062(3) 0.060(3) 0.076(3) 0.035(2) 0.038(2) 0.016(2) C9 0.037(2) 0.048(2) 0.055(2) 0.004(2) 0.017(2) 0.0017(19) C10 0.035(2) 0.063(3) 0.036(2) 0.005(2) 0.0040(18) 0.013(2) C11 0.075(3) 0.106(4) 0.043(2) 0.039(3) 0.015(2) 0.012(3) C12 0.036(2) 0.063(3) 0.044(2) 0.000(2) 0.0047(19) 0.013(2) C13 0.036(2) 0.040(2) 0.082(3) 0.012(2) 0.018(2) 0.005(2) C14 0.059(3) 0.071(3) 0.090(3) 0.056(3) 0.039(3) 0.031(2) C15 0.040(2) 0.040(2) 0.048(2) 0.0125(18) 0.0168(18) 0.0107(18) C16 0.030(2) 0.045(2) 0.041(2) 0.0155(18) 0.0152(17) 0.0096(18) C17 0.035(2) 0.049(2) 0.039(2) 0.0202(18) 0.0184(17) 0.0113(18) C18 0.034(2) 0.047(2) 0.045(2) 0.0191(19) 0.0172(18) 0.0080(19) C19 0.030(2) 0.061(3) 0.048(2) 0.023(2) 0.0131(18) 0.008(2) C20 0.033(2) 0.055(3) 0.050(2) 0.026(2) 0.0158(18) 0.0136(19) C21 0.042(2) 0.048(2) 0.055(2) 0.025(2) 0.022(2) 0.015(2) C22 0.040(2) 0.051(3) 0.053(2) 0.023(2) 0.0224(19) 0.0097(19) C23 0.055(3) 0.089(4) 0.048(3) 0.016(2) 0.008(2) 0.021(3) C24 0.044(3) 0.045(3) 0.111(4) 0.028(3) 0.024(3) 0.001(2) C25 0.068(3) 0.063(3) 0.114(4) 0.058(3) 0.054(3) 0.024(3) C26 0.101(4) 0.108(4) 0.070(3) 0.067(3) 0.025(3) 0.011(3) C27 0.101(4) 0.056(3) 0.120(4) 0.057(3) 0.079(3) 0.035(3) C28 0.086(3) 0.033(2) 0.100(4) 0.007(2) 0.062(3) -0.003(2) C29 0.059(3) 0.083(3) 0.044(2) 0.006(2) 0.018(2) 0.004(3) C30 0.049(2) 0.037(2) 0.055(2) 0.0162(19) 0.026(2) 0.0117(19) C31 0.057(3) 0.052(3) 0.044(2) 0.016(2) 0.027(2) 0.005(2) C32 0.076(3) 0.073(3) 0.051(3) 0.015(2) 0.036(2) 0.008(3) C33 0.061(3) 0.125(5) 0.069(3) 0.018(3) 0.043(3) 0.010(3) C34 0.167(6) 0.080(4) 0.076(3) 0.047(3) 0.069(4) 0.033(4) C35 0.037(2) 0.072(3) 0.069(3) 0.042(2) 0.018(2) 0.022(2) C36 0.050(3) 0.114(4) 0.103(4) 0.066(3) 0.039(3) 0.046(3) C37 0.062(3) 0.083(4) 0.164(6) 0.073(4) 0.022(3) 0.035(3) C38 0.080(4) 0.150(5) 0.076(3) 0.073(4) 0.028(3) 0.050(4) C39 0.063(3) 0.055(3) 0.041(2) 0.029(2) 0.011(2) 0.006(2) C40 0.201(7) 0.112(5) 0.048(3) 0.046(3) -0.004(4) -0.059(5) B 0.044(3) 0.045(3) 0.049(3) 0.023(2) 0.018(2) 0.012(2) C101 0.037(2) 0.047(2) 0.051(2) 0.022(2) 0.0166(19) 0.0042(19) C102 0.066(3) 0.052(3) 0.054(3) 0.024(2) 0.026(2) 0.014(2) C103 0.082(3) 0.052(3) 0.057(3) 0.016(2) 0.031(3) 0.010(2) C104 0.072(3) 0.073(4) 0.050(3) 0.013(3) 0.022(3) -0.006(3) C105 0.066(3) 0.089(4) 0.051(3) 0.039(3) 0.014(2) 0.008(3) C106 0.059(3) 0.059(3) 0.059(3) 0.030(2) 0.024(2) 0.016(2) C201 0.048(2) 0.044(2) 0.046(2) 0.0167(19) 0.0196(19) 0.014(2) C202 0.056(3) 0.058(3) 0.051(2) 0.022(2) 0.021(2) 0.008(2) C203 0.072(3) 0.050(3) 0.068(3) 0.022(2) 0.036(3) 0.002(2) C204 0.099(4) 0.056(3) 0.066(3) 0.034(3) 0.044(3) 0.017(3) C205 0.092(4) 0.076(4) 0.053(3) 0.032(3) 0.016(3) 0.005(3) C206 0.074(3) 0.055(3) 0.050(3) 0.021(2) 0.015(2) -0.005(2) C301 0.051(3) 0.051(3) 0.043(2) 0.020(2) 0.0162(19) 0.007(2) C302 0.059(3) 0.071(3) 0.076(3) 0.035(3) 0.024(3) 0.006(3) C303 0.076(4) 0.105(5) 0.102(4) 0.058(4) 0.026(3) -0.007(4) C304 0.054(4) 0.156(6) 0.093(4) 0.067(4) 0.012(3) -0.021(4) C305 0.053(3) 0.166(6) 0.087(4) 0.075(4) 0.024(3) 0.033(4) C306 0.053(3) 0.084(3) 0.072(3) 0.041(3) 0.025(2) 0.015(3) C401 0.059(3) 0.055(3) 0.053(2) 0.030(2) 0.027(2) 0.020(2) C402 0.071(3) 0.074(3) 0.071(3) 0.036(3) 0.035(3) 0.033(3) C403 0.091(4) 0.119(5) 0.105(4) 0.071(4) 0.057(4) 0.066(4) C404 0.148(6) 0.101(5) 0.114(5) 0.067(4) 0.092(5) 0.084(5) C405 0.138(6) 0.066(4) 0.101(4) 0.032(3) 0.069(4) 0.039(4) C406 0.090(4) 0.060(3) 0.071(3) 0.022(3) 0.038(3) 0.025(3) N7 0.271(9) 0.138(6) 0.194(7) 0.057(5) 0.090(6) 0.126(6) C41 0.137(6) 0.080(4) 0.108(5) 0.034(4) 0.048(4) 0.047(4) C42 0.077(4) 0.088(4) 0.120(5) 0.044(4) 0.045(3) 0.023(3) N8 0.175(6) 0.300(9) 0.128(5) 0.100(6) 0.081(5) 0.036(6) C43 0.092(4) 0.129(5) 0.110(5) 0.047(4) 0.060(4) 0.033(4) C44 0.175(7) 0.134(6) 0.134(6) 0.065(5) 0.093(5) 0.090(5) O3 0.235(15) 0.131(11) 0.32(2) 0.029(11) 0.134(14) 0.006(10) C45 0.166(18) 0.31(3) 0.091(11) 0.009(14) 0.052(12) 0.132(19) C46 0.148(15) 0.23(2) 0.129(14) 0.101(15) 0.021(11) 0.003(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 Fe1 O1 2.029(2) . ? Fe1 N2 2.256(3) . ? Fe1 N3 2.311(3) . ? Fe1 N1 2.406(3) . ? Fe1 S2 2.5122(12) . ? Fe1 S1 2.5256(12) . ? Fe2 O2 2.021(2) . ? Fe2 N5 2.248(3) . ? Fe2 N6 2.366(3) . ? Fe2 N4 2.377(3) . ? Fe2 S2 2.4992(15) . ? Fe2 S1 2.5461(15) . ? S1 C1 1.767(3) . ? S2 C17 1.760(4) . ? N1 C8 1.484(4) . ? N1 C7 1.486(4) . ? N1 C9 1.492(4) . ? N2 C12 1.483(5) . ? N2 C11 1.483(5) . ? N2 C10 1.484(4) . ? N3 C13 1.484(4) . ? N3 C14 1.488(4) . ? N3 C15 1.496(4) . ? N4 C24 1.478(5) . ? N4 C22 1.483(4) . ? N4 C23 1.483(5) . ? N5 C25 1.474(5) . ? N5 C27 1.484(5) . ? N5 C26 1.486(5) . ? N6 C29 1.480(5) . ? N6 C28 1.480(5) . ? N6 C30 1.486(4) . ? O1 C39 1.247(4) . ? O2 C39 1.251(4) . ? C1 C2 1.396(5) . ? C1 C6 1.410(5) . ? C2 C3 1.400(4) . ? C2 C30 1.503(5) . ? C3 C4 1.380(5) . ? C4 C5 1.387(5) . ? C4 C31 1.526(5) . ? C5 C6 1.386(4) . ? C6 C7 1.501(5) . ? C9 C10 1.498(5) . ? C12 C13 1.511(5) . ? C15 C16 1.501(5) . ? C16 C21 1.391(5) . ? C16 C17 1.402(5) . ? C17 C18 1.417(5) . ? C18 C19 1.384(5) . ? C18 C22 1.495(5) . ? C19 C20 1.395(5) . ? C20 C21 1.392(5) . ? C20 C35 1.527(5) . ? C24 C25 1.518(6) . ? C27 C28 1.504(6) . ? C31 C34 1.507(5) . ? C31 C32 1.517(5) . ? C31 C33 1.526(5) . ? C35 C37 1.518(6) . ? C35 C36 1.539(5) . ? C35 C38 1.543(6) . ? C39 C40 1.517(5) . ? B C301 1.631(6) . ? B C201 1.634(6) . ? B C401 1.634(6) . ? B C101 1.651(5) . ? C101 C106 1.400(5) . ? C101 C102 1.403(5) . ? C102 C103 1.371(5) . ? C103 C104 1.365(6) . ? C104 C105 1.372(6) . ? C105 C106 1.395(5) . ? C201 C206 1.385(5) . ? C201 C202 1.399(5) . ? C202 C203 1.384(5) . ? C203 C204 1.373(6) . ? C204 C205 1.370(6) . ? C205 C206 1.397(6) . ? C301 C302 1.381(5) . ? C301 C306 1.403(5) . ? C302 C303 1.381(6) . ? C303 C304 1.359(7) . ? C304 C305 1.378(7) . ? C305 C306 1.392(6) . ? C401 C402 1.397(5) . ? C401 C406 1.397(4) . ? C402 C403 1.386(6) . ? C403 C404 1.388(7) . ? C404 C405 1.357(7) . ? C405 C406 1.406(6) . ? N7 C41 1.0238 . ? C41 C42 1.4049 . ? N8 C43 1.0707 . ? C43 C44 1.4729 . ? O3 C45 1.166(10) . ? O3 C46 1.541(14) . ? C45 C46 1.2310 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N2 156.35(11) . . ? O1 Fe1 N3 87.75(11) . . ? N2 Fe1 N3 79.33(11) . . ? O1 Fe1 N1 85.90(10) . . ? N2 Fe1 N1 77.32(10) . . ? N3 Fe1 N1 100.87(10) . . ? O1 Fe1 S2 100.14(8) . . ? N2 Fe1 S2 99.39(9) . . ? N3 Fe1 S2 89.14(8) . . ? N1 Fe1 S2 168.56(8) . . ? O1 Fe1 S1 94.14(8) . . ? N2 Fe1 S1 101.93(9) . . ? N3 Fe1 S1 170.34(7) . . ? N1 Fe1 S1 88.72(8) . . ? S2 Fe1 S1 81.20(4) . . ? O2 Fe2 N5 157.35(11) . . ? O2 Fe2 N6 86.16(11) . . ? N5 Fe2 N6 78.54(11) . . ? O2 Fe2 N4 88.38(11) . . ? N5 Fe2 N4 78.78(11) . . ? N6 Fe2 N4 102.16(11) . . ? O2 Fe2 S2 97.63(8) . . ? N5 Fe2 S2 100.49(9) . . ? N6 Fe2 S2 169.10(8) . . ? N4 Fe2 S2 88.19(9) . . ? O2 Fe2 S1 97.14(8) . . ? N5 Fe2 S1 98.99(9) . . ? N6 Fe2 S1 88.36(9) . . ? N4 Fe2 S1 168.46(8) . . ? S2 Fe2 S1 81.05(6) . . ? C1 S1 Fe1 103.04(12) . . ? C1 S1 Fe2 103.65(12) . . ? Fe1 S1 Fe2 84.79(5) . . ? C17 S2 Fe2 105.87(12) . . ? C17 S2 Fe1 106.16(12) . . ? Fe2 S2 Fe1 86.06(5) . . ? C8 N1 C7 108.2(3) . . ? C8 N1 C9 110.3(3) . . ? C7 N1 C9 105.5(3) . . ? C8 N1 Fe1 114.6(2) . . ? C7 N1 Fe1 111.1(2) . . ? C9 N1 Fe1 106.7(2) . . ? C12 N2 C11 109.8(3) . . ? C12 N2 C10 110.5(3) . . ? C11 N2 C10 107.0(3) . . ? C12 N2 Fe1 109.5(2) . . ? C11 N2 Fe1 111.6(2) . . ? C10 N2 Fe1 108.5(2) . . ? C13 N3 C14 109.8(3) . . ? C13 N3 C15 108.1(3) . . ? C14 N3 C15 108.7(3) . . ? C13 N3 Fe1 103.6(2) . . ? C14 N3 Fe1 113.7(2) . . ? C15 N3 Fe1 112.7(2) . . ? C24 N4 C22 107.1(3) . . ? C24 N4 C23 109.8(3) . . ? C22 N4 C23 108.2(3) . . ? C24 N4 Fe2 104.4(2) . . ? C22 N4 Fe2 112.9(2) . . ? C23 N4 Fe2 114.3(2) . . ? C25 N5 C27 111.7(3) . . ? C25 N5 C26 107.4(3) . . ? C27 N5 C26 108.2(3) . . ? C25 N5 Fe2 109.0(2) . . ? C27 N5 Fe2 109.6(2) . . ? C26 N5 Fe2 111.0(2) . . ? C29 N6 C28 109.1(3) . . ? C29 N6 C30 108.3(3) . . ? C28 N6 C30 106.9(3) . . ? C29 N6 Fe2 114.8(2) . . ? C28 N6 Fe2 105.2(2) . . ? C30 N6 Fe2 112.2(2) . . ? C39 O1 Fe1 133.6(2) . . ? C39 O2 Fe2 133.0(2) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 S1 120.8(3) . . ? C6 C1 S1 120.7(3) . . ? C1 C2 C3 119.1(3) . . ? C1 C2 C30 120.7(3) . . ? C3 C2 C30 119.7(3) . . ? C4 C3 C2 123.8(3) . . ? C3 C4 C5 115.5(3) . . ? C3 C4 C31 124.6(3) . . ? C5 C4 C31 119.8(3) . . ? C6 C5 C4 123.5(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C7 119.1(3) . . ? C1 C6 C7 120.8(3) . . ? N1 C7 C6 116.8(3) . . ? N1 C9 C10 110.6(3) . . ? N2 C10 C9 112.6(3) . . ? N2 C12 C13 113.6(3) . . ? N3 C13 C12 111.9(3) . . ? N3 C15 C16 115.6(3) . . ? C21 C16 C17 120.3(3) . . ? C21 C16 C15 119.0(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 117.9(3) . . ? C16 C17 S2 121.2(3) . . ? C18 C17 S2 120.9(3) . . ? C19 C18 C17 119.4(3) . . ? C19 C18 C22 119.7(3) . . ? C17 C18 C22 120.5(3) . . ? C18 C19 C20 123.7(3) . . ? C21 C20 C19 115.7(3) . . ? C21 C20 C35 123.3(4) . . ? C19 C20 C35 121.0(3) . . ? C16 C21 C20 122.9(4) . . ? N4 C22 C18 116.6(3) . . ? N4 C24 C25 110.8(3) . . ? N5 C25 C24 113.4(3) . . ? N5 C27 C28 113.3(3) . . ? N6 C28 C27 111.6(3) . . ? N6 C30 C2 116.2(3) . . ? C34 C31 C32 109.0(3) . . ? C34 C31 C33 109.1(4) . . ? C32 C31 C33 107.5(3) . . ? C34 C31 C4 109.4(3) . . ? C32 C31 C4 112.3(3) . . ? C33 C31 C4 109.5(3) . . ? C37 C35 C20 113.3(3) . . ? C37 C35 C36 108.1(4) . . ? C20 C35 C36 109.1(3) . . ? C37 C35 C38 109.4(4) . . ? C20 C35 C38 109.2(3) . . ? C36 C35 C38 107.5(4) . . ? O1 C39 O2 126.7(3) . . ? O1 C39 C40 115.5(4) . . ? O2 C39 C40 117.8(4) . . ? C301 B C201 112.5(3) . . ? C301 B C401 112.6(3) . . ? C201 B C401 104.5(3) . . ? C301 B C101 103.2(3) . . ? C201 B C101 111.9(3) . . ? C401 B C101 112.4(3) . . ? C106 C101 C102 114.0(4) . . ? C106 C101 B 123.8(3) . . ? C102 C101 B 121.8(3) . . ? C103 C102 C101 123.6(4) . . ? C104 C103 C102 120.4(4) . . ? C103 C104 C105 119.2(4) . . ? C104 C105 C106 120.0(4) . . ? C105 C106 C101 122.8(4) . . ? C206 C201 C202 114.2(4) . . ? C206 C201 B 122.8(4) . . ? C202 C201 B 122.7(3) . . ? C203 C202 C201 123.5(4) . . ? C204 C203 C202 120.0(4) . . ? C205 C204 C203 119.1(4) . . ? C204 C205 C206 119.9(4) . . ? C201 C206 C205 123.4(4) . . ? C302 C301 C306 114.5(4) . . ? C302 C301 B 123.1(4) . . ? C306 C301 B 122.1(4) . . ? C303 C302 C301 123.6(5) . . ? C304 C303 C302 120.1(5) . . ? C303 C304 C305 119.6(5) . . ? C304 C305 C306 119.3(5) . . ? C305 C306 C301 122.8(5) . . ? C402 C401 C406 115.3(3) . . ? C402 C401 B 122.5(4) . . ? C406 C401 B 122.1(3) . . ? C403 C402 C401 123.5(5) . . ? C402 C403 C404 119.2(5) . . ? C405 C404 C403 119.5(5) . . ? C404 C405 C406 120.8(5) . . ? C401 C406 C405 121.7(4) . . ? N7 C41 C42 175.2 . . ? N8 C43 C44 174.6 . . ? C45 O3 C46 51.9(5) . . ? O3 C45 C46 79.9(8) . . ? C45 C46 O3 48.2(5) . . ? #===END