# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name C.S.Hong K.J.Cho J.W.Lee D.W.Ryu W.R.Lee K.S.Lim E.K.Koh _publ_contact_author_name 'Chang Seop Hong' _publ_contact_author_email cshong@korea.ac.kr data_squeezed _database_code_depnum_ccdc_archive 'CCDC 873485' #TrackingRef '- cif-complex1_revise.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H104 B2 Br4 Fe2 Mn2 N22 O4' _chemical_formula_weight 2144.81 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.414(3) _cell_length_b 14.003(3) _cell_length_c 15.544(3) _cell_angle_alpha 98.07(3) _cell_angle_beta 105.42(3) _cell_angle_gamma 98.98(3) _cell_volume 2525.6(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12392 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1094 _exptl_absorpt_coefficient_mu 2.167 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8125 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details HKL2000-Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.85000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Fixed gap multipole wiggler beamline' _diffrn_radiation_monochromator 'Pt coated Si double crystal' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7063 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 31.64 _reflns_number_total 4889 _reflns_number_gt 3313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'PAL ADSC Quantum-210' _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _computing_structure_solution SHELXTL _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WingX _computing_publication_material WingX _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.We employed the restraint DELU for some atoms (delu c21 > c30B) to restrain the anisotripic displacement parameters to behave reasonably. ; _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^)+(0.1666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4889 _refine_ls_number_parameters 580 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2315 _refine_ls_wR_factor_gt 0.2075 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _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 Fe1 Fe 0.24117(11) 0.82991(10) 0.18787(10) 0.0665(5) Uani 1 1 d . . . C1 C 0.1623(9) 0.8757(8) 0.2702(8) 0.070(3) Uani 1 1 d . . . C2 C 0.3713(10) 0.9336(9) 0.2608(8) 0.081(3) Uani 1 1 d . . . C3 C 0.2939(10) 0.7465(8) 0.2735(9) 0.074(3) Uani 1 1 d . . . N1 N 0.1186(8) 0.9089(6) 0.3214(7) 0.080(3) Uani 1 1 d . C . N2 N 0.4453(8) 0.9948(7) 0.3045(7) 0.091(3) Uani 1 1 d . . . N3 N 0.3246(8) 0.7005(7) 0.3252(8) 0.086(3) Uani 1 1 d . . . N4 N 0.1948(6) 0.9225(5) 0.1037(6) 0.061(2) Uani 1 1 d . . . N5 N 0.1692(6) 0.8873(6) 0.0122(6) 0.065(2) Uani 1 1 d . . . C4 C 0.2188(9) 1.0875(7) 0.2031(7) 0.071(3) Uani 1 1 d . . . H4A H 0.1854 1.0523 0.2431 0.107 Uiso 1 1 calc R . . H4B H 0.1846 1.1451 0.1936 0.107 Uiso 1 1 calc R . . H4C H 0.3014 1.1090 0.2313 0.107 Uiso 1 1 calc R . . C5 C 0.1960(8) 1.0202(7) 0.1133(8) 0.069(3) Uani 1 1 d . . . C6 C 0.1723(9) 1.0461(7) 0.0305(8) 0.071(3) Uani 1 1 d . . . C7 C 0.1640(9) 1.1445(7) 0.0023(8) 0.075(3) Uani 1 1 d . . . H7A H 0.2411 1.1870 0.0216 0.090 Uiso 1 1 calc R . . H7B H 0.1160 1.1771 0.0337 0.090 Uiso 1 1 calc R . . C8 C 0.1125(11) 1.1340(9) -0.1015(9) 0.093(4) Uani 1 1 d . . . H8A H 0.0283 1.1150 -0.1177 0.111 Uiso 1 1 calc R . . H8B H 0.1318 1.1982 -0.1192 0.111 Uiso 1 1 calc R . . C9 C 0.1577(11) 1.0562(8) -0.1539(9) 0.090(4) Uani 1 1 d . . . H9A H 0.1233 1.0519 -0.2199 0.108 Uiso 1 1 calc R . . H9B H 0.2413 1.0777 -0.1401 0.108 Uiso 1 1 calc R . . C10 C 0.1320(8) 0.9539(7) -0.1309(7) 0.071(3) Uani 1 1 d . . . H10A H 0.0504 0.9237 -0.1605 0.085 Uiso 1 1 calc R . . H10B H 0.1782 0.9114 -0.1549 0.085 Uiso 1 1 calc R . . C11 C 0.1578(8) 0.9597(8) -0.0326(7) 0.062(3) Uani 1 1 d . . . N6 N 0.1041(6) 0.7282(5) 0.1141(6) 0.061(2) Uani 1 1 d . . . N7 N 0.0793(6) 0.7158(6) 0.0217(6) 0.064(2) Uani 1 1 d . . . C12 C 0.0180(8) 0.6575(7) 0.2252(7) 0.070(3) Uani 1 1 d . . . H12A H 0.0955 0.6612 0.2640 0.105 Uiso 1 1 calc R . . H12B H -0.0299 0.5941 0.2232 0.105 Uiso 1 1 calc R . . H12C H -0.0138 0.7111 0.2499 0.105 Uiso 1 1 calc R . . C13 C 0.0212(9) 0.6667(7) 0.1309(7) 0.062(3) Uani 1 1 d . . . C14 C -0.0578(7) 0.6172(7) 0.0483(8) 0.063(3) Uani 1 1 d . . . C15 C -0.1678(8) 0.5439(8) 0.0331(7) 0.076(3) Uani 1 1 d . . . H15A H -0.2245 0.5778 0.0519 0.092 Uiso 1 1 calc R . . H15B H -0.1534 0.4925 0.0699 0.092 Uiso 1 1 calc R . . C16 C -0.2142(8) 0.4965(8) -0.0685(7) 0.072(3) Uani 1 1 d . . . H16A H -0.1718 0.4447 -0.0815 0.087 Uiso 1 1 calc R . . H16B H -0.2955 0.4646 -0.0823 0.087 Uiso 1 1 calc R . . C17 C -0.2041(8) 0.5712(7) -0.1310(7) 0.075(3) Uani 1 1 d . . . H17A H -0.2464 0.6233 -0.1185 0.090 Uiso 1 1 calc R . . H17B H -0.2387 0.5375 -0.1952 0.090 Uiso 1 1 calc R . . C18 C -0.0780(8) 0.6182(7) -0.1158(7) 0.068(3) Uani 1 1 d . . . H18A H -0.0401 0.5697 -0.1426 0.082 Uiso 1 1 calc R . . H18B H -0.0736 0.6754 -0.1466 0.082 Uiso 1 1 calc R . . C19 C -0.0194(8) 0.6503(7) -0.0191(8) 0.063(3) Uani 1 1 d . . . N8 N 0.3320(7) 0.7768(6) 0.1073(7) 0.070(2) Uani 1 1 d . . . N9 N 0.2790(7) 0.7529(6) 0.0169(6) 0.065(2) Uani 1 1 d . . . C20 C 0.5196(9) 0.7646(9) 0.2139(8) 0.090(4) Uani 1 1 d . . . H20A H 0.5165 0.8251 0.2525 0.134 Uiso 1 1 calc R . . H20B H 0.5961 0.7693 0.2065 0.134 Uiso 1 1 calc R . . H20C H 0.5023 0.7081 0.2422 0.134 Uiso 1 1 calc R . . C21 C 0.4350(9) 0.7515(7) 0.1240(8) 0.068(3) Uani 1 1 d U . . C22 C 0.4468(9) 0.7111(8) 0.0409(8) 0.072(3) Uani 1 1 d U B . C23 C 0.5422(9) 0.6649(9) 0.0188(10) 0.101(4) Uani 1 1 d U . . H23A H 0.5335 0.5959 0.0281 0.122 Uiso 0.50 1 calc PR A 1 H23B H 0.6176 0.7023 0.0587 0.122 Uiso 0.50 1 calc PR A 1 H23C H 0.6133 0.7158 0.0369 0.122 Uiso 0.50 1 calc PR A 2 H23D H 0.5562 0.6126 0.0547 0.122 Uiso 0.50 1 calc PR A 2 C24A C 0.532(2) 0.669(2) -0.086(2) 0.098(9) Uiso 0.50 1 d PU B 1 C25A C 0.4004(18) 0.5982(17) -0.1301(17) 0.075(6) Uiso 0.50 1 d PU B 1 H25A H 0.3876 0.5667 -0.1940 0.089 Uiso 0.50 1 calc PR B 1 H25B H 0.3881 0.5465 -0.0943 0.089 Uiso 0.50 1 calc PR B 1 C24B C 0.5144(19) 0.6228(19) -0.0775(15) 0.070(6) Uiso 0.50 1 d PU B 2 H24A H 0.5864 0.6378 -0.0937 0.084 Uiso 0.50 1 calc PR B 2 H24B H 0.4967 0.5505 -0.0822 0.084 Uiso 0.50 1 calc PR B 2 C25B C 0.429(3) 0.644(3) -0.148(2) 0.129(11) Uiso 0.50 1 d PU B 2 H25C H 0.4021 0.5852 -0.1981 0.155 Uiso 0.50 1 calc PR B 2 H25D H 0.4646 0.6983 -0.1726 0.155 Uiso 0.50 1 calc PR B 2 C26 C 0.3200(9) 0.6735(9) -0.1233(8) 0.082(3) Uani 1 1 d U . . H26A H 0.3353 0.7273 -0.1562 0.099 Uiso 0.50 1 calc PR B 1 H26B H 0.2387 0.6403 -0.1483 0.099 Uiso 0.50 1 calc PR B 1 H26C H 0.2942 0.7247 -0.1571 0.099 Uiso 0.50 1 calc PR B 2 H26D H 0.2568 0.6152 -0.1412 0.099 Uiso 0.50 1 calc PR B 2 C27 C 0.3498(9) 0.7113(7) -0.0245(8) 0.074(3) Uani 1 1 d U B . C28 C 0.2833(12) 0.9509(10) 0.5694(11) 0.122(5) Uani 1 1 d U . . C29 C 0.3361(11) 1.0208(10) 0.5261(11) 0.109(4) Uani 1 1 d U C . C30A C 0.2792(13) 0.9896(11) 0.6576(12) 0.078(6) Uiso 0.71(3) 1 d PU C 1 C30B C 0.381(3) 0.963(3) 0.483(3) 0.070(13) Uiso 0.29(3) 1 d PU C 2 B1 B 0.1601(10) 0.7756(8) -0.0204(8) 0.066(3) Uani 1 1 d . . . H1 H 0.1331 0.7577 -0.0883 0.079 Uiso 1 1 calc R . . Mn1 Mn 0.09388(12) 0.99436(10) 0.43905(11) 0.0664(5) Uani 1 1 d . . . N10 N 0.1669(7) 0.9015(6) 0.5110(6) 0.079(3) Uani 1 1 d . C . N11 N 0.2487(7) 1.0779(6) 0.4814(6) 0.073(2) Uani 1 1 d . C . O1 O -0.0522(5) 0.9192(4) 0.4300(5) 0.0685(18) Uani 1 1 d . . . O2 O 0.0373(5) 1.0866(4) 0.3741(5) 0.0713(19) Uani 1 1 d . C . C31 C 0.1935(10) 0.7460(8) 0.5575(8) 0.088(4) Uani 1 1 d . C . H31A H 0.2331 0.7132 0.5190 0.132 Uiso 1 1 calc R . . H31B H 0.1426 0.6963 0.5748 0.132 Uiso 1 1 calc R . . H31C H 0.2496 0.7866 0.6123 0.132 Uiso 1 1 calc R . . C32 C 0.1259(9) 0.8088(8) 0.5069(8) 0.079(3) Uani 1 1 d . . . C33 C 0.0069(8) 0.7650(7) 0.4462(7) 0.066(3) Uani 1 1 d . C . C34 C -0.0278(9) 0.6625(7) 0.4295(7) 0.071(3) Uani 1 1 d . . . H34 H 0.0253 0.6238 0.4531 0.085 Uiso 1 1 calc R C . C35 C -0.1344(10) 0.6180(7) 0.3809(7) 0.069(3) Uani 1 1 d . C . C36 C -0.2145(9) 0.6705(8) 0.3421(8) 0.076(3) Uani 1 1 d . . . H36 H -0.2884 0.6380 0.3042 0.091 Uiso 1 1 calc R C . C37 C -0.1827(9) 0.7707(7) 0.3605(7) 0.074(3) Uani 1 1 d . C . H37 H -0.2374 0.8083 0.3373 0.088 Uiso 1 1 calc R . . C38 C -0.0743(9) 0.8195(7) 0.4115(8) 0.070(3) Uani 1 1 d . . . C39 C 0.4087(11) 1.2108(11) 0.4851(11) 0.130(6) Uani 1 1 d . C . H39A H 0.4345 1.2538 0.5452 0.194 Uiso 1 1 calc R . . H39B H 0.4200 1.2494 0.4392 0.194 Uiso 1 1 calc R . . H39C H 0.4527 1.1584 0.4852 0.194 Uiso 1 1 calc R . . C40 C 0.2826(10) 1.1651(9) 0.4631(9) 0.088(3) Uani 1 1 d . . . C41 C 0.2006(10) 1.2192(7) 0.4200(8) 0.078(3) Uani 1 1 d . C . C42 C 0.2377(10) 1.3212(9) 0.4215(8) 0.087(4) Uani 1 1 d . . . H42 H 0.3148 1.3526 0.4519 0.104 Uiso 1 1 calc R C . C43 C 0.1628(12) 1.3742(8) 0.3792(8) 0.079(3) Uani 1 1 d . C . C44 C 0.0493(12) 1.3317(9) 0.3329(8) 0.088(3) Uani 1 1 d . . . H44 H -0.0010 1.3696 0.3033 0.105 Uiso 1 1 calc R C . C45 C 0.0124(10) 1.2356(7) 0.3311(7) 0.075(3) Uani 1 1 d . C . H45 H -0.0647 1.2060 0.2990 0.091 Uiso 1 1 calc R . . C46 C 0.0830(10) 1.1782(8) 0.3746(8) 0.073(3) Uani 1 1 d . . . Br1 Br -0.17815(11) 0.47791(8) 0.35918(9) 0.0937(5) Uani 1 1 d . . . Br2 Br 0.21768(13) 1.51130(9) 0.38343(10) 0.1048(6) Uani 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 Fe1 0.0652(9) 0.0566(8) 0.0727(11) 0.0007(7) 0.0173(7) 0.0138(6) C1 0.066(7) 0.064(6) 0.066(9) 0.002(5) 0.001(6) 0.012(5) C2 0.080(7) 0.081(8) 0.084(9) 0.005(6) 0.031(7) 0.023(6) C3 0.091(8) 0.050(6) 0.087(9) 0.013(6) 0.036(7) 0.018(6) N1 0.092(7) 0.064(5) 0.083(8) 0.013(5) 0.017(6) 0.032(5) N2 0.073(6) 0.066(5) 0.104(8) -0.008(5) -0.005(5) 0.003(5) N3 0.077(6) 0.066(6) 0.111(8) 0.013(6) 0.027(6) 0.011(5) N4 0.069(5) 0.052(4) 0.066(6) 0.011(4) 0.021(4) 0.020(4) N5 0.066(5) 0.056(5) 0.065(6) 0.002(5) 0.012(4) 0.012(4) C4 0.083(7) 0.057(6) 0.069(8) 0.004(5) 0.022(6) 0.009(5) C5 0.055(6) 0.063(6) 0.085(9) 0.011(6) 0.012(6) 0.023(5) C6 0.074(7) 0.062(6) 0.073(8) 0.009(6) 0.016(6) 0.012(5) C7 0.071(6) 0.065(6) 0.089(9) 0.002(6) 0.023(6) 0.021(5) C8 0.099(9) 0.096(9) 0.095(11) 0.026(7) 0.037(8) 0.034(7) C9 0.115(9) 0.068(7) 0.089(9) 0.011(6) 0.033(7) 0.026(6) C10 0.063(6) 0.063(6) 0.079(9) 0.004(5) 0.015(6) 0.011(5) C11 0.060(6) 0.080(7) 0.048(8) 0.012(6) 0.021(5) 0.015(5) N6 0.068(5) 0.055(4) 0.059(6) 0.007(4) 0.018(4) 0.015(4) N7 0.053(5) 0.066(5) 0.072(7) 0.006(4) 0.023(4) 0.011(4) C12 0.078(7) 0.057(6) 0.075(8) 0.003(5) 0.023(6) 0.018(5) C13 0.081(7) 0.053(5) 0.068(8) 0.015(5) 0.037(6) 0.028(5) C14 0.051(5) 0.053(5) 0.075(8) 0.001(5) 0.003(6) 0.019(5) C15 0.071(7) 0.072(7) 0.084(8) 0.012(6) 0.018(6) 0.019(5) C16 0.055(6) 0.069(6) 0.087(8) -0.003(6) 0.020(5) 0.012(5) C17 0.071(7) 0.069(7) 0.072(8) -0.008(6) 0.010(6) 0.012(5) C18 0.063(6) 0.071(6) 0.064(8) -0.008(5) 0.020(5) 0.011(5) C19 0.062(6) 0.056(6) 0.069(8) 0.002(5) 0.023(6) 0.003(5) N8 0.053(5) 0.060(5) 0.096(8) -0.007(4) 0.031(5) 0.012(4) N9 0.066(5) 0.062(5) 0.062(6) -0.002(4) 0.015(5) 0.015(4) C20 0.076(7) 0.090(8) 0.094(10) 0.007(7) 0.011(7) 0.025(6) C21 0.066(7) 0.059(6) 0.078(7) 0.005(5) 0.028(5) 0.009(5) C22 0.065(6) 0.074(6) 0.079(7) 0.007(5) 0.030(5) 0.010(5) C23 0.066(6) 0.092(8) 0.142(12) -0.013(8) 0.047(7) 0.009(5) C26 0.072(7) 0.097(8) 0.083(7) 0.000(6) 0.037(6) 0.024(6) C27 0.082(6) 0.062(6) 0.076(6) -0.007(5) 0.030(6) 0.017(5) C28 0.112(10) 0.092(9) 0.130(14) 0.039(9) -0.017(9) -0.001(8) C29 0.082(8) 0.089(9) 0.148(13) 0.039(8) 0.009(8) 0.026(7) B1 0.081(8) 0.051(6) 0.060(8) -0.012(5) 0.028(7) 0.006(6) Mn1 0.0686(10) 0.0584(9) 0.0701(12) 0.0037(7) 0.0186(8) 0.0171(7) N10 0.069(5) 0.060(5) 0.093(7) 0.006(4) 0.009(5) 0.008(4) N11 0.081(6) 0.069(5) 0.071(6) 0.017(4) 0.019(5) 0.022(5) O1 0.076(4) 0.052(4) 0.077(5) 0.002(3) 0.025(4) 0.015(3) O2 0.080(4) 0.049(4) 0.086(5) 0.004(3) 0.026(4) 0.018(3) C31 0.095(8) 0.067(7) 0.093(9) 0.022(6) 0.003(7) 0.028(6) C32 0.086(7) 0.065(7) 0.085(8) 0.018(6) 0.016(6) 0.024(6) C33 0.073(7) 0.057(6) 0.065(7) 0.009(5) 0.013(5) 0.015(5) C34 0.075(7) 0.063(6) 0.082(8) 0.005(5) 0.037(6) 0.016(5) C35 0.095(8) 0.049(5) 0.073(8) 0.009(5) 0.035(6) 0.030(6) C36 0.071(7) 0.074(7) 0.073(8) -0.016(6) 0.027(6) 0.006(6) C37 0.086(8) 0.058(6) 0.078(8) -0.001(5) 0.034(6) 0.013(5) C38 0.070(7) 0.062(6) 0.082(8) 0.016(5) 0.022(6) 0.018(5) C39 0.083(9) 0.114(11) 0.179(15) 0.046(11) 0.014(9) 0.008(8) C40 0.082(8) 0.085(8) 0.096(10) 0.008(7) 0.024(7) 0.026(7) C41 0.093(8) 0.055(6) 0.095(9) 0.007(6) 0.045(7) 0.021(6) C42 0.083(8) 0.082(8) 0.093(9) 0.002(7) 0.034(7) 0.008(7) C43 0.115(10) 0.060(6) 0.078(8) 0.018(6) 0.036(7) 0.041(7) C44 0.114(10) 0.082(8) 0.076(9) 0.024(6) 0.029(7) 0.034(7) C45 0.107(8) 0.056(6) 0.072(8) 0.012(5) 0.036(6) 0.026(6) C46 0.086(8) 0.059(6) 0.082(8) 0.009(6) 0.038(6) 0.024(6) Br1 0.1057(9) 0.0611(7) 0.1104(11) 0.0066(6) 0.0316(7) 0.0145(6) Br2 0.1430(12) 0.0650(7) 0.1115(12) 0.0132(7) 0.0489(9) 0.0193(7) _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 C1 1.908(15) . ? Fe1 C3 1.944(14) . ? Fe1 C2 1.958(12) . ? Fe1 N6 1.997(8) . ? Fe1 N4 2.008(8) . ? Fe1 N8 2.036(8) . ? C1 N1 1.160(13) . ? C2 N2 1.140(12) . ? C3 N3 1.125(13) . ? N1 Mn1 2.161(12) . ? N4 C5 1.353(12) . ? N4 N5 1.371(11) . ? N5 C11 1.313(12) . ? N5 B1 1.552(13) . ? C4 C5 1.501(14) . ? C5 C6 1.356(14) . ? C6 C11 1.400(14) . ? C6 C7 1.514(15) . ? C7 C8 1.545(15) . ? C8 C9 1.533(16) . ? C9 C10 1.531(14) . ? C10 C11 1.462(14) . ? N6 C13 1.341(12) . ? N6 N7 1.365(11) . ? N7 C19 1.348(11) . ? N7 B1 1.542(15) . ? C12 C13 1.499(14) . ? C13 C14 1.399(13) . ? C14 C19 1.369(14) . ? C14 C15 1.516(13) . ? C15 C16 1.539(14) . ? C16 C17 1.536(15) . ? C17 C18 1.542(13) . ? C18 C19 1.455(14) . ? N8 C21 1.348(12) . ? N8 N9 1.351(11) . ? N9 C27 1.371(13) . ? N9 B1 1.536(15) . ? C20 C21 1.475(15) . ? C21 C22 1.390(14) . ? C22 C27 1.354(14) . ? C22 C23 1.527(16) . ? C23 C24B 1.46(2) . ? C23 C24A 1.61(3) . ? C24A C25A 1.68(4) . ? C25A C26 1.57(2) . ? C24B C25B 1.41(4) . ? C25B C26 1.60(3) . ? C26 C27 1.478(15) . ? C28 C30A 1.42(2) . ? C28 C29 1.435(19) . ? C28 N10 1.485(15) . ? C28 C30B 2.04(4) . ? C29 C30B 1.26(4) . ? C29 N11 1.525(15) . ? Mn1 O2 1.859(7) . ? Mn1 O1 1.908(7) . ? Mn1 N11 1.976(9) . ? Mn1 N10 2.000(9) . ? Mn1 O1 2.438(7) 2_576 ? N10 C32 1.304(13) . ? N11 C40 1.324(14) . ? O1 C38 1.354(11) . ? O1 Mn1 2.438(7) 2_576 ? O2 C46 1.316(11) . ? C31 C32 1.474(15) . ? C32 C33 1.503(14) . ? C33 C34 1.398(13) . ? C33 C38 1.399(14) . ? C34 C35 1.338(14) . ? C35 C36 1.388(15) . ? C35 Br1 1.908(9) . ? C36 C37 1.365(14) . ? C37 C38 1.379(14) . ? C39 C40 1.522(16) . ? C40 C41 1.442(16) . ? C41 C42 1.426(15) . ? C41 C46 1.426(15) . ? C42 C43 1.368(16) . ? C43 C44 1.392(16) . ? C43 Br2 1.920(11) . ? C44 C45 1.345(15) . ? C45 C46 1.389(15) . ? 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 C1 Fe1 C3 85.6(5) . . ? C1 Fe1 C2 86.3(4) . . ? C3 Fe1 C2 87.5(5) . . ? C1 Fe1 N6 91.9(4) . . ? C3 Fe1 N6 93.9(4) . . ? C2 Fe1 N6 177.6(4) . . ? C1 Fe1 N4 94.3(4) . . ? C3 Fe1 N4 176.6(4) . . ? C2 Fe1 N4 89.0(4) . . ? N6 Fe1 N4 89.6(3) . . ? C1 Fe1 N8 175.8(4) . . ? C3 Fe1 N8 90.4(4) . . ? C2 Fe1 N8 92.5(4) . . ? N6 Fe1 N8 89.5(3) . . ? N4 Fe1 N8 89.7(4) . . ? N1 C1 Fe1 176.0(9) . . ? N2 C2 Fe1 178.2(11) . . ? N3 C3 Fe1 177.9(11) . . ? C1 N1 Mn1 161.4(8) . . ? C5 N4 N5 106.3(8) . . ? C5 N4 Fe1 135.6(8) . . ? N5 N4 Fe1 117.4(6) . . ? C11 N5 N4 110.1(8) . . ? C11 N5 B1 131.6(10) . . ? N4 N5 B1 118.3(9) . . ? N4 C5 C6 109.6(10) . . ? N4 C5 C4 124.0(10) . . ? C6 C5 C4 126.4(9) . . ? C5 C6 C11 106.1(10) . . ? C5 C6 C7 131.6(10) . . ? C11 C6 C7 122.2(11) . . ? C6 C7 C8 112.4(9) . . ? C9 C8 C7 111.2(10) . . ? C10 C9 C8 113.3(10) . . ? C11 C10 C9 111.1(9) . . ? N5 C11 C6 107.8(9) . . ? N5 C11 C10 127.5(10) . . ? C6 C11 C10 124.6(10) . . ? C13 N6 N7 106.4(8) . . ? C13 N6 Fe1 136.4(8) . . ? N7 N6 Fe1 117.2(6) . . ? C19 N7 N6 110.7(8) . . ? C19 N7 B1 129.9(10) . . ? N6 N7 B1 119.4(8) . . ? N6 C13 C14 109.1(10) . . ? N6 C13 C12 123.0(9) . . ? C14 C13 C12 127.9(10) . . ? C19 C14 C13 106.7(9) . . ? C19 C14 C15 125.0(9) . . ? C13 C14 C15 128.3(11) . . ? C14 C15 C16 108.7(9) . . ? C17 C16 C15 112.9(8) . . ? C16 C17 C18 110.8(8) . . ? C19 C18 C17 110.3(8) . . ? N7 C19 C14 107.1(9) . . ? N7 C19 C18 128.5(10) . . ? C14 C19 C18 124.4(8) . . ? C21 N8 N9 109.0(8) . . ? C21 N8 Fe1 133.9(8) . . ? N9 N8 Fe1 116.9(6) . . ? N8 N9 C27 108.2(8) . . ? N8 N9 B1 119.4(8) . . ? C27 N9 B1 132.5(9) . . ? N8 C21 C22 107.3(9) . . ? N8 C21 C20 126.3(10) . . ? C22 C21 C20 126.4(10) . . ? C27 C22 C21 107.8(9) . . ? C27 C22 C23 121.6(11) . . ? C21 C22 C23 130.4(11) . . ? C24B C23 C22 112.0(13) . . ? C24B C23 C24A 25.4(12) . . ? C22 C23 C24A 106.6(14) . . ? C23 C24A C25A 96.6(19) . . ? C26 C25A C24A 103.3(17) . . ? C25B C24B C23 126(2) . . ? C24B C25B C26 117(3) . . ? C27 C26 C25A 103.3(12) . . ? C27 C26 C25B 109.8(15) . . ? C25A C26 C25B 29.4(13) . . ? C22 C27 N9 107.8(10) . . ? C22 C27 C26 128.2(10) . . ? N9 C27 C26 124.0(10) . . ? C30A C28 C29 114.9(13) . . ? C30A C28 N10 109.8(14) . . ? C29 C28 N10 110.9(11) . . ? C30A C28 C30B 142.6(14) . . ? C29 C28 C30B 37.7(12) . . ? N10 C28 C30B 105.6(14) . . ? C30B C29 C28 98(2) . . ? C30B C29 N11 124(2) . . ? C28 C29 N11 109.3(11) . . ? C29 C30B C28 44.3(14) . . ? N9 B1 N7 107.1(9) . . ? N9 B1 N5 107.4(7) . . ? N7 B1 N5 109.5(9) . . ? O2 Mn1 O1 95.3(3) . . ? O2 Mn1 N11 91.2(3) . . ? O1 Mn1 N11 165.6(3) . . ? O2 Mn1 N10 175.5(3) . . ? O1 Mn1 N10 89.1(3) . . ? N11 Mn1 N10 84.4(3) . . ? O2 Mn1 N1 92.9(3) . . ? O1 Mn1 N1 96.8(3) . . ? N11 Mn1 N1 95.7(4) . . ? N10 Mn1 N1 87.0(4) . . ? O2 Mn1 O1 88.1(3) . 2_576 ? O1 Mn1 O1 78.6(3) . 2_576 ? N11 Mn1 O1 88.8(3) . 2_576 ? N10 Mn1 O1 92.3(3) . 2_576 ? N1 Mn1 O1 175.4(3) . 2_576 ? C32 N10 C28 121.9(10) . . ? C32 N10 Mn1 127.6(7) . . ? C28 N10 Mn1 110.3(7) . . ? C40 N11 C29 120.3(9) . . ? C40 N11 Mn1 128.1(8) . . ? C29 N11 Mn1 110.7(7) . . ? C38 O1 Mn1 121.4(6) . . ? C38 O1 Mn1 119.7(6) . 2_576 ? Mn1 O1 Mn1 101.4(3) . 2_576 ? C46 O2 Mn1 131.2(7) . . ? N10 C32 C31 122.1(10) . . ? N10 C32 C33 118.3(9) . . ? C31 C32 C33 119.6(9) . . ? C34 C33 C38 117.6(9) . . ? C34 C33 C32 117.4(9) . . ? C38 C33 C32 124.7(9) . . ? C35 C34 C33 121.3(10) . . ? C34 C35 C36 121.9(9) . . ? C34 C35 Br1 119.9(8) . . ? C36 C35 Br1 118.1(8) . . ? C37 C36 C35 117.3(10) . . ? C36 C37 C38 122.5(11) . . ? O1 C38 C37 118.2(9) . . ? O1 C38 C33 122.3(9) . . ? C37 C38 C33 119.3(9) . . ? N11 C40 C41 120.7(10) . . ? N11 C40 C39 121.4(11) . . ? C41 C40 C39 117.9(11) . . ? C42 C41 C46 116.4(11) . . ? C42 C41 C40 118.8(11) . . ? C46 C41 C40 124.8(10) . . ? C43 C42 C41 120.3(11) . . ? C42 C43 C44 122.2(11) . . ? C42 C43 Br2 118.5(10) . . ? C44 C43 Br2 119.3(9) . . ? C45 C44 C43 118.4(12) . . ? C44 C45 C46 122.4(12) . . ? O2 C46 C45 117.9(10) . . ? O2 C46 C41 121.8(10) . . ? C45 C46 C41 120.2(10) . . ? _diffrn_measured_fraction_theta_max 0.491 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.797 _refine_diff_density_max 0.695 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.106 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.822 0.822 370.6 66.4 _platon_squeeze_details ; The contributions of some 66 electrons were removed from the unit-cell contents, and as Z = 1 in this case, this could/might correspond with the removal of solvent such as 1.5(MeOH) and 1.5(MeCN) [some 60 electrons] from the FeIII2MnIII2 formula unit. ;