# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Cai-Ming Liu' _publ_contact_author_address ; Institute of Chemistry, CAS Beijing 100080 CHINA ; _publ_contact_author_email CMLIU@ICCAS.AC.CN _publ_section_title ; Solvatomagnetic effect and spin-glass behavior in A 1D coordination polymer constructed from EE-azido bridged MnIII3O Units ; loop_ _publ_author_name 'Cai-Ming Liu' 'De-Qing Zhang' 'Daoben Zhu' # Attachment 'complex1-revised.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 662330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Br3 Mn3 N9 O9' _chemical_formula_weight 1093.23 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' Br Br -0.2901 2.4595 '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' _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 19.1576(12) _cell_length_b 8.2244(5) _cell_length_c 25.5724(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.152(3) _cell_angle_gamma 90.00 _cell_volume 3988.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 31302 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.00 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2164 _exptl_absorpt_coefficient_mu 4.003 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.4729 _exptl_absorpt_correction_T_max 0.6903 _exptl_absorpt_process_details Abscor _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP Area Detector' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31302 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7714 _reflns_number_gt 6171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO (Rigaku, 2001)' _computing_cell_refinement 'RAPID AUTO (Rigaku, 2001)' _computing_data_reduction 'RAPID AUTO (Rigaku, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. DFIX, ISOR and SIMU restraints were used to deal with disordered methanol molecules and lower non-solvent C Ueq(max)/Ueq(min). ; _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^)+(0.0517P)^2^+16.4361P] 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 7714 _refine_ls_number_parameters 537 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.26045(3) 0.70574(9) 0.40879(3) 0.0287(2) Uani 1 1 d . . . Br2 Br 0.86688(4) -0.41004(9) 0.68720(3) 0.02885(19) Uani 1 1 d . . . Br3 Br 0.93561(4) 0.36429(9) 0.13029(3) 0.02731(19) Uani 1 1 d . . . Mn1 Mn 0.61874(5) 0.38220(12) 0.38024(4) 0.0186(2) Uani 1 1 d . . . Mn2 Mn 0.68175(5) 0.09490(11) 0.46540(4) 0.0164(2) Uani 1 1 d . . . Mn3 Mn 0.78167(5) 0.24129(12) 0.38040(4) 0.0174(2) Uani 1 1 d . . . O1 O 0.5407(2) 0.4957(6) 0.34640(19) 0.0253(11) Uani 1 1 d . . . O2 O 0.6709(2) -0.0392(5) 0.52163(18) 0.0228(10) Uani 1 1 d . . . O3 O 0.8655(2) 0.2399(6) 0.35083(18) 0.0247(11) Uani 1 1 d . . . O4 O 0.6962(2) 0.2512(5) 0.41248(17) 0.0183(10) Uani 1 1 d . . . N1 N 0.5640(3) 0.3182(6) 0.4358(2) 0.0181(12) Uani 1 1 d . . . N2 N 0.5896(3) 0.2019(6) 0.4727(2) 0.0186(12) Uani 1 1 d . . . N3 N 0.7830(3) 0.0391(6) 0.4746(2) 0.0181(12) Uani 1 1 d . . . N4 N 0.8248(3) 0.0950(6) 0.4386(2) 0.0189(12) Uani 1 1 d . . . N5 N 0.7390(3) 0.3781(6) 0.3215(2) 0.0190(12) Uani 1 1 d . . . N6 N 0.6737(3) 0.4460(7) 0.3221(2) 0.0199(12) Uani 1 1 d . . . C1 C 0.4803(3) 0.5429(8) 0.3634(3) 0.0197(14) Uani 1 1 d . . . C2 C 0.4566(3) 0.4810(8) 0.4098(3) 0.0199(14) Uani 1 1 d . . . C3 C 0.3919(3) 0.5328(8) 0.4231(3) 0.0225(15) Uani 1 1 d . . . H3 H 0.3760 0.4922 0.4541 0.027 Uiso 1 1 calc R . . C4 C 0.3506(3) 0.6431(8) 0.3913(3) 0.0236(16) Uani 1 1 d . . . C5 C 0.3729(4) 0.7042(9) 0.3457(3) 0.0284(17) Uani 1 1 d . . . H5 H 0.3443 0.7791 0.3240 0.034 Uiso 1 1 calc R . . C6 C 0.4376(4) 0.6546(8) 0.3323(3) 0.0269(16) Uani 1 1 d . . . H6 H 0.4530 0.6975 0.3014 0.032 Uiso 1 1 calc R . . C7 C 0.4984(3) 0.3592(8) 0.4436(3) 0.0173(14) Uani 1 1 d . . . C8 C 0.4808(3) 0.2711(8) 0.4874(3) 0.0209(15) Uani 1 1 d . . . H8 H 0.4383 0.2762 0.5025 0.025 Uiso 1 1 calc R . . C9 C 0.5398(3) 0.1753(8) 0.5034(3) 0.0202(14) Uani 1 1 d . . . H9 H 0.5441 0.1012 0.5321 0.024 Uiso 1 1 calc R . . C10 C 0.7178(3) -0.1186(7) 0.5583(3) 0.0197(14) Uani 1 1 d . . . C11 C 0.7905(3) -0.1308(8) 0.5543(3) 0.0212(15) Uani 1 1 d . . . C12 C 0.8340(4) -0.2167(8) 0.5940(3) 0.0229(15) Uani 1 1 d . . . H12 H 0.8832 -0.2235 0.5924 0.027 Uiso 1 1 calc R . . C13 C 0.8068(4) -0.2913(8) 0.6350(3) 0.0221(15) Uani 1 1 d . . . C14 C 0.7347(3) -0.2814(8) 0.6385(3) 0.0208(14) Uani 1 1 d . . . H14 H 0.7159 -0.3355 0.6662 0.025 Uiso 1 1 calc R . . C15 C 0.6906(3) -0.1917(8) 0.6011(3) 0.0222(15) Uani 1 1 d . . . H15 H 0.6421 -0.1797 0.6044 0.027 Uiso 1 1 calc R . . C16 C 0.8221(3) -0.0543(8) 0.5111(3) 0.0186(14) Uani 1 1 d . . . C17 C 0.8910(4) -0.0610(8) 0.4981(3) 0.0236(15) Uani 1 1 d . . . H17 H 0.9301 -0.1181 0.5165 0.028 Uiso 1 1 calc R . . C18 C 0.8902(3) 0.0323(8) 0.4530(3) 0.0225(15) Uani 1 1 d . . . H18 H 0.9295 0.0498 0.4349 0.027 Uiso 1 1 calc R . . C19 C 0.8784(3) 0.2719(8) 0.3016(3) 0.0228(15) Uani 1 1 d . . . C20 C 0.9428(3) 0.2183(8) 0.2873(3) 0.0209(14) Uani 1 1 d . . . H20 H 0.9748 0.1608 0.3125 0.025 Uiso 1 1 calc R . . C21 C 0.9612(4) 0.2472(8) 0.2372(3) 0.0247(16) Uani 1 1 d . . . H21 H 1.0046 0.2084 0.2281 0.030 Uiso 1 1 calc R . . C22 C 0.9145(3) 0.3341(8) 0.2009(3) 0.0210(15) Uani 1 1 d . . . C23 C 0.8510(3) 0.3908(8) 0.2136(3) 0.0202(14) Uani 1 1 d . . . H23 H 0.8202 0.4500 0.1881 0.024 Uiso 1 1 calc R . . C24 C 0.8316(3) 0.3619(8) 0.2637(3) 0.0186(14) Uani 1 1 d . . . C25 C 0.7636(3) 0.4206(8) 0.2761(3) 0.0187(14) Uani 1 1 d . . . C26 C 0.7129(4) 0.5214(8) 0.2473(3) 0.0251(16) Uani 1 1 d . . . H26 H 0.7154 0.5711 0.2141 0.030 Uiso 1 1 calc R . . C27 C 0.6583(4) 0.5333(8) 0.2774(3) 0.0231(15) Uani 1 1 d . . . H27 H 0.6163 0.5942 0.2679 0.028 Uiso 1 1 calc R . . N7 N 0.6561(3) 0.6246(7) 0.4272(2) 0.0303(14) Uani 1 1 d . . . N8 N 0.6489(3) 0.7637(7) 0.4172(2) 0.0217(13) Uani 1 1 d . . . N9 N 0.6418(3) 0.9051(7) 0.4071(2) 0.0278(14) Uani 1 1 d . . . O5 O 0.5788(3) 0.1464(6) 0.3337(2) 0.0297(12) Uani 1 1 d . . . H5A H 0.605(4) 0.075(11) 0.345(3) 0.045 Uiso 1 1 d . . . C28 C 0.5062(5) 0.1093(13) 0.3215(4) 0.062(3) Uani 1 1 d . . . H28A H 0.4883 0.0716 0.3535 0.093 Uiso 1 1 calc R . . H28B H 0.4997 0.0236 0.2947 0.093 Uiso 1 1 calc R . . H28C H 0.4803 0.2068 0.3080 0.093 Uiso 1 1 calc R . . O6 O 0.8254(3) 0.4629(6) 0.4288(2) 0.0285(11) Uani 1 1 d D . . H6A H 0.8696(10) 0.462(10) 0.440(3) 0.043 Uiso 1 1 d D . . C29 C 0.8140(5) 0.4831(10) 0.4823(3) 0.040(2) Uani 1 1 d . . . H29A H 0.7633 0.4935 0.4837 0.060 Uiso 1 1 calc R . . H29B H 0.8383 0.5814 0.4969 0.060 Uiso 1 1 calc R . . H29C H 0.8324 0.3884 0.5030 0.060 Uiso 1 1 calc R . . O7 O 0.7363(3) 0.0146(6) 0.33422(19) 0.0295(12) Uani 1 1 d . . . H7A H 0.7667 -0.0602 0.3420 0.044 Uiso 1 1 d R . . C30 C 0.7163(4) 0.0047(9) 0.2773(3) 0.0324(18) Uani 1 1 d . . . H30A H 0.6802 0.0869 0.2659 0.049 Uiso 1 1 calc R . . H30B H 0.6972 -0.1037 0.2679 0.049 Uiso 1 1 calc R . . H30C H 0.7577 0.0242 0.2597 0.049 Uiso 1 1 calc R . . O8 O 0.1924(5) 0.2390(7) 0.1354(3) 0.069(2) Uani 1 1 d . . . H8A H 0.1927 0.1476 0.1208 0.104 Uiso 1 1 calc R . . C31 C 0.1339(5) 0.2497(11) 0.1628(4) 0.055(3) Uani 1 1 d . . . H31A H 0.1002 0.1631 0.1508 0.083 Uiso 1 1 calc R . . H31B H 0.1110 0.3557 0.1559 0.083 Uiso 1 1 calc R . . H31C H 0.1496 0.2376 0.2008 0.083 Uiso 1 1 calc R . . C32 C 0.0084(14) 0.446(3) 0.4172(11) 0.049(6) Uani 0.456(17) 1 d PDU A 1 H32A H 0.0012 0.4752 0.3797 0.074 Uiso 0.456(17) 1 calc PR A 1 H32B H -0.0011 0.3295 0.4209 0.074 Uiso 0.456(17) 1 calc PR A 1 H32C H 0.0572 0.4692 0.4324 0.074 Uiso 0.456(17) 1 calc PR A 1 O9 O -0.0393(6) 0.540(2) 0.4448(6) 0.054(6) Uani 0.456(17) 1 d PD A 1 O9' O -0.0195(6) 0.3799(15) 0.4546(5) 0.053(5) Uani 0.544(17) 1 d PD A 2 C32' C 0.0054(13) 0.504(2) 0.4215(9) 0.049(5) Uani 0.544(17) 1 d PDU A 2 H32D H -0.0108 0.6112 0.4318 0.074 Uiso 0.544(17) 1 calc PR A 2 H32E H -0.0132 0.4833 0.3845 0.074 Uiso 0.544(17) 1 calc PR A 2 H32F H 0.0571 0.5029 0.4260 0.074 Uiso 0.544(17) 1 calc PR 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 Br1 0.0195(3) 0.0249(4) 0.0413(5) -0.0066(3) 0.0029(3) 0.0049(3) Br2 0.0305(4) 0.0316(4) 0.0230(4) 0.0095(3) -0.0016(3) 0.0010(3) Br3 0.0293(4) 0.0319(4) 0.0220(4) 0.0029(3) 0.0081(3) 0.0030(3) Mn1 0.0179(5) 0.0182(5) 0.0195(6) 0.0041(4) 0.0027(4) 0.0028(4) Mn2 0.0170(5) 0.0140(5) 0.0176(6) 0.0017(4) 0.0006(4) 0.0010(4) Mn3 0.0178(5) 0.0172(5) 0.0168(6) 0.0033(4) 0.0013(4) 0.0031(4) O1 0.022(2) 0.024(3) 0.030(3) 0.007(2) 0.005(2) 0.004(2) O2 0.021(2) 0.020(2) 0.027(3) 0.007(2) -0.001(2) 0.0022(19) O3 0.023(2) 0.033(3) 0.017(3) 0.006(2) 0.002(2) 0.007(2) O4 0.020(2) 0.016(2) 0.018(3) 0.0010(19) -0.0004(19) 0.0016(18) N1 0.023(3) 0.013(3) 0.018(3) 0.003(2) 0.000(2) 0.000(2) N2 0.021(3) 0.014(3) 0.020(3) 0.000(2) -0.002(2) 0.004(2) N3 0.022(3) 0.013(3) 0.019(3) 0.004(2) 0.003(2) 0.003(2) N4 0.021(3) 0.017(3) 0.018(3) 0.001(2) 0.004(2) 0.003(2) N5 0.016(3) 0.020(3) 0.020(3) -0.001(2) -0.002(2) 0.000(2) N6 0.017(3) 0.021(3) 0.022(3) -0.002(2) 0.002(2) 0.003(2) C1 0.016(3) 0.017(3) 0.025(4) 0.002(3) 0.000(3) 0.000(3) C2 0.019(3) 0.016(3) 0.023(4) -0.002(3) 0.000(3) -0.003(3) C3 0.023(3) 0.016(3) 0.028(4) -0.005(3) 0.003(3) -0.004(3) C4 0.016(3) 0.020(4) 0.034(4) -0.011(3) 0.000(3) 0.000(3) C5 0.030(4) 0.021(4) 0.032(4) 0.004(3) -0.001(3) 0.008(3) C6 0.030(4) 0.026(4) 0.023(4) 0.006(3) -0.001(3) 0.006(3) C7 0.014(3) 0.017(3) 0.021(4) -0.001(3) 0.000(3) -0.005(2) C8 0.018(3) 0.021(3) 0.025(4) 0.002(3) 0.006(3) -0.002(3) C9 0.025(3) 0.012(3) 0.024(4) -0.002(3) 0.006(3) -0.002(3) C10 0.027(4) 0.009(3) 0.021(4) -0.001(3) 0.000(3) -0.003(3) C11 0.026(3) 0.017(3) 0.022(4) 0.000(3) 0.004(3) 0.000(3) C12 0.023(3) 0.020(4) 0.024(4) -0.001(3) 0.000(3) 0.000(3) C13 0.036(4) 0.017(3) 0.011(4) -0.001(3) -0.002(3) -0.007(3) C14 0.030(4) 0.017(3) 0.015(4) -0.003(3) 0.001(3) -0.004(3) C15 0.020(3) 0.025(4) 0.022(4) -0.006(3) 0.002(3) -0.002(3) C16 0.024(3) 0.014(3) 0.016(4) 0.000(3) -0.003(3) 0.001(3) C17 0.023(3) 0.029(4) 0.018(4) 0.003(3) 0.001(3) 0.003(3) C18 0.016(3) 0.027(4) 0.024(4) 0.004(3) 0.001(3) 0.004(3) C19 0.021(3) 0.022(4) 0.024(4) 0.000(3) 0.002(3) -0.004(3) C20 0.016(3) 0.023(4) 0.023(4) 0.002(3) -0.001(3) 0.002(3) C21 0.022(3) 0.020(4) 0.033(4) -0.002(3) 0.006(3) -0.002(3) C22 0.026(3) 0.021(3) 0.016(4) 0.005(3) 0.003(3) -0.007(3) C23 0.024(3) 0.016(3) 0.021(4) -0.002(3) 0.002(3) -0.002(3) C24 0.017(3) 0.016(3) 0.021(4) 0.001(3) -0.001(3) -0.001(3) C25 0.023(3) 0.016(3) 0.015(4) -0.002(3) -0.002(3) -0.004(3) C26 0.028(4) 0.027(4) 0.021(4) 0.003(3) 0.004(3) -0.001(3) C27 0.030(4) 0.020(4) 0.019(4) 0.009(3) 0.002(3) 0.004(3) N7 0.042(4) 0.020(3) 0.028(4) -0.001(3) 0.000(3) -0.005(3) N8 0.019(3) 0.027(4) 0.019(3) -0.005(3) 0.004(2) -0.002(2) N9 0.034(3) 0.015(3) 0.032(4) -0.006(3) -0.004(3) 0.001(2) O5 0.031(3) 0.024(3) 0.029(3) -0.003(2) -0.011(2) 0.001(2) C28 0.052(6) 0.064(7) 0.067(7) -0.021(6) 0.001(5) -0.029(5) O6 0.034(3) 0.025(3) 0.025(3) -0.002(2) 0.000(2) -0.008(2) C29 0.049(5) 0.037(5) 0.035(5) -0.004(4) 0.007(4) 0.007(4) O7 0.038(3) 0.026(3) 0.025(3) -0.009(2) 0.005(2) 0.003(2) C30 0.046(5) 0.027(4) 0.023(4) -0.005(3) 0.002(4) -0.002(3) O8 0.138(7) 0.026(3) 0.055(4) -0.001(3) 0.051(5) 0.021(4) C31 0.037(5) 0.037(5) 0.086(8) -0.007(5) -0.007(5) -0.006(4) C32 0.045(8) 0.051(10) 0.053(9) -0.002(8) 0.011(7) -0.003(8) O9 0.017(6) 0.091(14) 0.058(10) -0.012(9) 0.015(6) -0.008(7) O9' 0.050(7) 0.053(9) 0.052(8) 0.012(6) -0.011(6) -0.010(6) C32' 0.044(8) 0.050(9) 0.052(8) 0.010(8) 0.001(7) -0.006(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 Br1 C4 1.915(6) . ? Br2 C13 1.903(7) . ? Br3 C22 1.921(7) . ? Mn1 O1 1.867(5) . ? Mn1 O4 1.922(4) . ? Mn1 N1 1.954(5) . ? Mn1 N6 2.008(6) . ? Mn1 O5 2.346(5) . ? Mn1 N7 2.383(6) . ? Mn2 O2 1.847(5) . ? Mn2 O4 1.915(4) . ? Mn2 N3 1.975(5) . ? Mn2 N2 2.005(5) . ? Mn2 N9 2.217(6) 1_545 ? Mn3 O3 1.869(5) . ? Mn3 O4 1.935(4) . ? Mn3 N5 1.964(5) . ? Mn3 N4 1.999(5) . ? Mn3 O6 2.294(5) . ? Mn3 O7 2.310(5) . ? O1 C1 1.350(8) . ? O2 C10 1.369(8) . ? O3 C19 1.343(8) . ? N1 C7 1.343(8) . ? N1 N2 1.384(7) . ? N2 C9 1.336(8) . ? N3 C16 1.351(8) . ? N3 N4 1.382(7) . ? N4 C18 1.356(8) . ? N5 C25 1.359(8) . ? N5 N6 1.373(7) . ? N6 C27 1.348(8) . ? C1 C6 1.400(9) . ? C1 C2 1.423(9) . ? C2 C3 1.398(9) . ? C2 C7 1.482(9) . ? C3 C4 1.388(9) . ? C3 H3 0.9500 . ? C4 C5 1.391(10) . ? C5 C6 1.392(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.415(9) . ? C8 C9 1.390(9) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.412(9) . ? C10 C11 1.414(9) . ? C11 C12 1.408(9) . ? C11 C16 1.473(9) . ? C12 C13 1.382(9) . ? C12 H12 0.9500 . ? C13 C14 1.397(9) . ? C14 C15 1.395(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.407(9) . ? C17 C18 1.384(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.407(9) . ? C19 C24 1.430(9) . ? C20 C21 1.396(10) . ? C20 H20 0.9500 . ? C21 C22 1.393(9) . ? C21 H21 0.9500 . ? C22 C23 1.383(9) . ? C23 C24 1.402(9) . ? C23 H23 0.9500 . ? C24 C25 1.466(9) . ? C25 C26 1.404(9) . ? C26 C27 1.386(9) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? N7 N8 1.176(8) . ? N8 N9 1.195(8) . ? N9 Mn2 2.217(6) 1_565 ? O5 C28 1.416(10) . ? O5 H5A 0.79(8) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O6 C29 1.425(9) . ? O6 H6A 0.852(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? O7 C30 1.454(8) . ? O7 H7A 0.8500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O8 C31 1.406(11) . ? O8 H8A 0.8400 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O9 1.453(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O9' C32' 1.450(10) . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? 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 O4 175.8(2) . . ? O1 Mn1 N1 89.7(2) . . ? O4 Mn1 N1 89.9(2) . . ? O1 Mn1 N6 89.8(2) . . ? O4 Mn1 N6 90.6(2) . . ? N1 Mn1 N6 179.0(2) . . ? O1 Mn1 O5 89.8(2) . . ? O4 Mn1 O5 86.00(18) . . ? N1 Mn1 O5 88.6(2) . . ? N6 Mn1 O5 90.5(2) . . ? O1 Mn1 N7 88.8(2) . . ? O4 Mn1 N7 95.4(2) . . ? N1 Mn1 N7 90.7(2) . . ? N6 Mn1 N7 90.1(2) . . ? O5 Mn1 N7 178.4(2) . . ? O2 Mn2 O4 174.0(2) . . ? O2 Mn2 N3 89.2(2) . . ? O4 Mn2 N3 90.1(2) . . ? O2 Mn2 N2 89.5(2) . . ? O4 Mn2 N2 89.3(2) . . ? N3 Mn2 N2 162.6(2) . . ? O2 Mn2 N9 92.1(2) . 1_545 ? O4 Mn2 N9 93.9(2) . 1_545 ? N3 Mn2 N9 99.0(2) . 1_545 ? N2 Mn2 N9 98.5(2) . 1_545 ? O3 Mn3 O4 177.6(2) . . ? O3 Mn3 N5 88.9(2) . . ? O4 Mn3 N5 90.9(2) . . ? O3 Mn3 N4 90.5(2) . . ? O4 Mn3 N4 89.7(2) . . ? N5 Mn3 N4 177.9(2) . . ? O3 Mn3 O6 87.4(2) . . ? O4 Mn3 O6 90.24(18) . . ? N5 Mn3 O6 92.3(2) . . ? N4 Mn3 O6 89.7(2) . . ? O3 Mn3 O7 94.04(19) . . ? O4 Mn3 O7 88.36(18) . . ? N5 Mn3 O7 89.1(2) . . ? N4 Mn3 O7 88.9(2) . . ? O6 Mn3 O7 178.04(18) . . ? C1 O1 Mn1 131.4(4) . . ? C10 O2 Mn2 133.0(4) . . ? C19 O3 Mn3 131.4(4) . . ? Mn2 O4 Mn1 120.0(2) . . ? Mn2 O4 Mn3 119.1(2) . . ? Mn1 O4 Mn3 119.3(2) . . ? C7 N1 N2 108.7(5) . . ? C7 N1 Mn1 130.5(4) . . ? N2 N1 Mn1 120.5(4) . . ? C9 N2 N1 107.5(5) . . ? C9 N2 Mn2 134.0(5) . . ? N1 N2 Mn2 118.1(4) . . ? C16 N3 N4 109.5(5) . . ? C16 N3 Mn2 130.8(4) . . ? N4 N3 Mn2 119.7(4) . . ? C18 N4 N3 107.0(5) . . ? C18 N4 Mn3 134.4(5) . . ? N3 N4 Mn3 118.6(4) . . ? C25 N5 N6 109.5(5) . . ? C25 N5 Mn3 130.2(4) . . ? N6 N5 Mn3 120.3(4) . . ? C27 N6 N5 107.2(5) . . ? C27 N6 Mn1 133.9(4) . . ? N5 N6 Mn1 118.5(4) . . ? O1 C1 C6 117.7(6) . . ? O1 C1 C2 123.7(6) . . ? C6 C1 C2 118.6(6) . . ? C3 C2 C1 119.5(6) . . ? C3 C2 C7 119.3(6) . . ? C1 C2 C7 121.2(6) . . ? C4 C3 C2 120.6(6) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.6(6) . . ? C3 C4 Br1 119.8(5) . . ? C5 C4 Br1 119.6(5) . . ? C4 C5 C6 119.4(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C5 C6 C1 121.3(7) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N1 C7 C8 108.8(6) . . ? N1 C7 C2 121.6(6) . . ? C8 C7 C2 129.6(6) . . ? C9 C8 C7 104.4(6) . . ? C9 C8 H8 127.8 . . ? C7 C8 H8 127.8 . . ? N2 C9 C8 110.7(6) . . ? N2 C9 H9 124.7 . . ? C8 C9 H9 124.7 . . ? O2 C10 C15 117.0(6) . . ? O2 C10 C11 122.8(6) . . ? C15 C10 C11 120.2(6) . . ? C12 C11 C10 118.2(6) . . ? C12 C11 C16 119.3(6) . . ? C10 C11 C16 122.5(6) . . ? C13 C12 C11 121.4(6) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 120.3(6) . . ? C12 C13 Br2 120.3(5) . . ? C14 C13 Br2 119.4(5) . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 120.1(6) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? N3 C16 C17 107.7(6) . . ? N3 C16 C11 121.0(6) . . ? C17 C16 C11 131.3(6) . . ? C18 C17 C16 106.0(6) . . ? C18 C17 H17 127.0 . . ? C16 C17 H17 127.0 . . ? N4 C18 C17 109.7(6) . . ? N4 C18 H18 125.1 . . ? C17 C18 H18 125.1 . . ? O3 C19 C20 117.9(6) . . ? O3 C19 C24 123.8(6) . . ? C20 C19 C24 118.3(6) . . ? C21 C20 C19 122.0(6) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C20 118.5(6) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 121.2(6) . . ? C23 C22 Br3 119.2(5) . . ? C21 C22 Br3 119.5(5) . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 119.0(6) . . ? C23 C24 C25 120.1(6) . . ? C19 C24 C25 120.9(6) . . ? N5 C25 C26 107.5(6) . . ? N5 C25 C24 121.8(6) . . ? C26 C25 C24 130.7(6) . . ? C27 C26 C25 105.8(6) . . ? C27 C26 H26 127.1 . . ? C25 C26 H26 127.1 . . ? N6 C27 C26 110.0(6) . . ? N6 C27 H27 125.0 . . ? C26 C27 H27 125.0 . . ? N8 N7 Mn1 133.4(5) . . ? N7 N8 N9 179.8(8) . . ? N8 N9 Mn2 121.5(5) . 1_565 ? C28 O5 Mn1 122.0(5) . . ? C28 O5 H5A 118(6) . . ? Mn1 O5 H5A 106(6) . . ? O5 C28 H28A 109.5 . . ? O5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 O6 Mn3 121.1(4) . . ? C29 O6 H6A 88(6) . . ? Mn3 O6 H6A 116(6) . . ? O6 C29 H29A 109.5 . . ? O6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 O7 Mn3 125.7(4) . . ? C30 O7 H7A 105.6 . . ? Mn3 O7 H7A 105.6 . . ? O7 C30 H30A 109.5 . . ? O7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 O8 H8A 109.5 . . ? O8 C31 H31A 109.5 . . ? O8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O9' C32' H32D 109.5 . . ? O9' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? O9' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mn1 O1 C1 99(3) . . . . ? N1 Mn1 O1 C1 14.5(6) . . . . ? N6 Mn1 O1 C1 -166.4(6) . . . . ? O5 Mn1 O1 C1 103.1(6) . . . . ? N7 Mn1 O1 C1 -76.2(6) . . . . ? O4 Mn2 O2 C10 -74(2) . . . . ? N3 Mn2 O2 C10 9.4(6) . . . . ? N2 Mn2 O2 C10 -153.2(6) . . . . ? N9 Mn2 O2 C10 108.4(6) 1_545 . . . ? O4 Mn3 O3 C19 -105(5) . . . . ? N5 Mn3 O3 C19 -19.5(6) . . . . ? N4 Mn3 O3 C19 158.5(6) . . . . ? O6 Mn3 O3 C19 -111.8(6) . . . . ? O7 Mn3 O3 C19 69.5(6) . . . . ? O2 Mn2 O4 Mn1 -94.2(18) . . . . ? N3 Mn2 O4 Mn1 -177.6(3) . . . . ? N2 Mn2 O4 Mn1 -15.0(3) . . . . ? N9 Mn2 O4 Mn1 83.4(3) 1_545 . . . ? O2 Mn2 O4 Mn3 100.1(18) . . . . ? N3 Mn2 O4 Mn3 16.6(3) . . . . ? N2 Mn2 O4 Mn3 179.2(3) . . . . ? N9 Mn2 O4 Mn3 -82.4(3) 1_545 . . . ? O1 Mn1 O4 Mn2 -70(3) . . . . ? N1 Mn1 O4 Mn2 14.2(3) . . . . ? N6 Mn1 O4 Mn2 -164.9(3) . . . . ? O5 Mn1 O4 Mn2 -74.5(3) . . . . ? N7 Mn1 O4 Mn2 104.9(3) . . . . ? O1 Mn1 O4 Mn3 95(3) . . . . ? N1 Mn1 O4 Mn3 179.9(3) . . . . ? N6 Mn1 O4 Mn3 0.8(3) . . . . ? O5 Mn1 O4 Mn3 91.2(3) . . . . ? N7 Mn1 O4 Mn3 -89.4(3) . . . . ? O3 Mn3 O4 Mn2 -112(5) . . . . ? N5 Mn3 O4 Mn2 162.6(3) . . . . ? N4 Mn3 O4 Mn2 -15.4(3) . . . . ? O6 Mn3 O4 Mn2 -105.1(3) . . . . ? O7 Mn3 O4 Mn2 73.5(3) . . . . ? O3 Mn3 O4 Mn1 82(5) . . . . ? N5 Mn3 O4 Mn1 -3.3(3) . . . . ? N4 Mn3 O4 Mn1 178.8(3) . . . . ? O6 Mn3 O4 Mn1 89.0(3) . . . . ? O7 Mn3 O4 Mn1 -92.4(3) . . . . ? O1 Mn1 N1 C7 -4.3(6) . . . . ? O4 Mn1 N1 C7 179.9(6) . . . . ? N6 Mn1 N1 C7 -63(13) . . . . ? O5 Mn1 N1 C7 -94.1(6) . . . . ? N7 Mn1 N1 C7 84.5(6) . . . . ? O1 Mn1 N1 N2 169.4(4) . . . . ? O4 Mn1 N1 N2 -6.4(4) . . . . ? N6 Mn1 N1 N2 111(12) . . . . ? O5 Mn1 N1 N2 79.6(4) . . . . ? N7 Mn1 N1 N2 -101.8(5) . . . . ? C7 N1 N2 C9 -1.2(7) . . . . ? Mn1 N1 N2 C9 -176.1(4) . . . . ? C7 N1 N2 Mn2 172.2(4) . . . . ? Mn1 N1 N2 Mn2 -2.7(6) . . . . ? O2 Mn2 N2 C9 -4.4(6) . . . . ? O4 Mn2 N2 C9 -178.5(6) . . . . ? N3 Mn2 N2 C9 -90.2(9) . . . . ? N9 Mn2 N2 C9 87.6(6) 1_545 . . . ? O2 Mn2 N2 N1 -175.7(4) . . . . ? O4 Mn2 N2 N1 10.2(4) . . . . ? N3 Mn2 N2 N1 98.5(8) . . . . ? N9 Mn2 N2 N1 -83.7(4) 1_545 . . . ? O2 Mn2 N3 C16 -3.2(6) . . . . ? O4 Mn2 N3 C16 170.8(6) . . . . ? N2 Mn2 N3 C16 82.6(9) . . . . ? N9 Mn2 N3 C16 -95.2(6) 1_545 . . . ? O2 Mn2 N3 N4 174.4(5) . . . . ? O4 Mn2 N3 N4 -11.6(5) . . . . ? N2 Mn2 N3 N4 -99.8(8) . . . . ? N9 Mn2 N3 N4 82.4(5) 1_545 . . . ? C16 N3 N4 C18 1.0(7) . . . . ? Mn2 N3 N4 C18 -177.0(4) . . . . ? C16 N3 N4 Mn3 -178.7(4) . . . . ? Mn2 N3 N4 Mn3 3.3(6) . . . . ? O3 Mn3 N4 C18 4.9(6) . . . . ? O4 Mn3 N4 C18 -172.7(6) . . . . ? N5 Mn3 N4 C18 79(6) . . . . ? O6 Mn3 N4 C18 -82.4(6) . . . . ? O7 Mn3 N4 C18 99.0(6) . . . . ? O3 Mn3 N4 N3 -175.5(4) . . . . ? O4 Mn3 N4 N3 6.9(4) . . . . ? N5 Mn3 N4 N3 -101(6) . . . . ? O6 Mn3 N4 N3 97.1(4) . . . . ? O7 Mn3 N4 N3 -81.5(4) . . . . ? O3 Mn3 N5 C25 9.2(6) . . . . ? O4 Mn3 N5 C25 -173.2(6) . . . . ? N4 Mn3 N5 C25 -65(6) . . . . ? O6 Mn3 N5 C25 96.5(6) . . . . ? O7 Mn3 N5 C25 -84.9(6) . . . . ? O3 Mn3 N5 N6 -171.6(5) . . . . ? O4 Mn3 N5 N6 6.0(5) . . . . ? N4 Mn3 N5 N6 114(6) . . . . ? O6 Mn3 N5 N6 -84.3(5) . . . . ? O7 Mn3 N5 N6 94.3(5) . . . . ? C25 N5 N6 C27 -1.1(7) . . . . ? Mn3 N5 N6 C27 179.6(4) . . . . ? C25 N5 N6 Mn1 172.6(4) . . . . ? Mn3 N5 N6 Mn1 -6.8(6) . . . . ? O1 Mn1 N6 C27 -0.7(6) . . . . ? O4 Mn1 N6 C27 175.1(6) . . . . ? N1 Mn1 N6 C27 58(13) . . . . ? O5 Mn1 N6 C27 89.1(6) . . . . ? N7 Mn1 N6 C27 -89.5(6) . . . . ? O1 Mn1 N6 N5 -172.3(5) . . . . ? O4 Mn1 N6 N5 3.5(4) . . . . ? N1 Mn1 N6 N5 -114(12) . . . . ? O5 Mn1 N6 N5 -82.5(4) . . . . ? N7 Mn1 N6 N5 99.0(5) . . . . ? Mn1 O1 C1 C6 167.5(5) . . . . ? Mn1 O1 C1 C2 -14.9(10) . . . . ? O1 C1 C2 C3 -177.6(6) . . . . ? C6 C1 C2 C3 0.0(10) . . . . ? O1 C1 C2 C7 0.8(10) . . . . ? C6 C1 C2 C7 178.4(6) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C7 C2 C3 C4 -178.1(6) . . . . ? C2 C3 C4 C5 -0.1(10) . . . . ? C2 C3 C4 Br1 177.5(5) . . . . ? C3 C4 C5 C6 -0.5(11) . . . . ? Br1 C4 C5 C6 -178.1(5) . . . . ? C4 C5 C6 C1 0.8(11) . . . . ? O1 C1 C6 C5 177.2(6) . . . . ? C2 C1 C6 C5 -0.5(10) . . . . ? N2 N1 C7 C8 1.5(7) . . . . ? Mn1 N1 C7 C8 175.7(4) . . . . ? N2 N1 C7 C2 -179.5(5) . . . . ? Mn1 N1 C7 C2 -5.2(9) . . . . ? C3 C2 C7 N1 -172.9(6) . . . . ? C1 C2 C7 N1 8.7(9) . . . . ? C3 C2 C7 C8 6.0(10) . . . . ? C1 C2 C7 C8 -172.5(7) . . . . ? N1 C7 C8 C9 -1.1(7) . . . . ? C2 C7 C8 C9 179.9(6) . . . . ? N1 N2 C9 C8 0.5(7) . . . . ? Mn2 N2 C9 C8 -171.5(5) . . . . ? C7 C8 C9 N2 0.4(7) . . . . ? Mn2 O2 C10 C15 170.4(4) . . . . ? Mn2 O2 C10 C11 -10.3(9) . . . . ? O2 C10 C11 C12 -179.3(6) . . . . ? C15 C10 C11 C12 -0.1(9) . . . . ? O2 C10 C11 C16 2.0(10) . . . . ? C15 C10 C11 C16 -178.8(6) . . . . ? C10 C11 C12 C13 1.7(10) . . . . ? C16 C11 C12 C13 -179.6(6) . . . . ? C11 C12 C13 C14 -0.7(10) . . . . ? C11 C12 C13 Br2 178.8(5) . . . . ? C12 C13 C14 C15 -1.9(10) . . . . ? Br2 C13 C14 C15 178.6(5) . . . . ? C13 C14 C15 C10 3.5(10) . . . . ? O2 C10 C15 C14 176.8(6) . . . . ? C11 C10 C15 C14 -2.5(10) . . . . ? N4 N3 C16 C17 -0.8(7) . . . . ? Mn2 N3 C16 C17 177.0(5) . . . . ? N4 N3 C16 C11 -179.7(5) . . . . ? Mn2 N3 C16 C11 -1.9(9) . . . . ? C12 C11 C16 N3 -175.1(6) . . . . ? C10 C11 C16 N3 3.5(10) . . . . ? C12 C11 C16 C17 6.4(11) . . . . ? C10 C11 C16 C17 -175.0(7) . . . . ? N3 C16 C17 C18 0.3(7) . . . . ? C11 C16 C17 C18 179.0(7) . . . . ? N3 N4 C18 C17 -0.8(7) . . . . ? Mn3 N4 C18 C17 178.8(5) . . . . ? C16 C17 C18 N4 0.3(8) . . . . ? Mn3 O3 C19 C20 -162.8(5) . . . . ? Mn3 O3 C19 C24 19.5(10) . . . . ? O3 C19 C20 C21 -179.4(6) . . . . ? C24 C19 C20 C21 -1.6(10) . . . . ? C19 C20 C21 C22 1.1(10) . . . . ? C20 C21 C22 C23 -0.2(10) . . . . ? C20 C21 C22 Br3 -176.2(5) . . . . ? C21 C22 C23 C24 -0.2(10) . . . . ? Br3 C22 C23 C24 175.8(5) . . . . ? C22 C23 C24 C19 -0.3(9) . . . . ? C22 C23 C24 C25 -179.0(6) . . . . ? O3 C19 C24 C23 178.8(6) . . . . ? C20 C19 C24 C23 1.1(9) . . . . ? O3 C19 C24 C25 -2.5(10) . . . . ? C20 C19 C24 C25 179.8(6) . . . . ? N6 N5 C25 C26 1.1(7) . . . . ? Mn3 N5 C25 C26 -179.6(4) . . . . ? N6 N5 C25 C24 -178.3(5) . . . . ? Mn3 N5 C25 C24 1.0(9) . . . . ? C23 C24 C25 N5 171.6(6) . . . . ? C19 C24 C25 N5 -7.0(9) . . . . ? C23 C24 C25 C26 -7.5(11) . . . . ? C19 C24 C25 C26 173.8(7) . . . . ? N5 C25 C26 C27 -0.7(7) . . . . ? C24 C25 C26 C27 178.6(7) . . . . ? N5 N6 C27 C26 0.6(7) . . . . ? Mn1 N6 C27 C26 -171.6(5) . . . . ? C25 C26 C27 N6 0.0(8) . . . . ? O1 Mn1 N7 N8 -29.3(7) . . . . ? O4 Mn1 N7 N8 151.0(7) . . . . ? N1 Mn1 N7 N8 -119.0(7) . . . . ? N6 Mn1 N7 N8 60.4(7) . . . . ? O5 Mn1 N7 N8 -53(8) . . . . ? Mn1 N7 N8 N9 -119(100) . . . . ? N7 N8 N9 Mn2 -64(100) . . . 1_565 ? O1 Mn1 O5 C28 -35.6(7) . . . . ? O4 Mn1 O5 C28 144.1(7) . . . . ? N1 Mn1 O5 C28 54.1(7) . . . . ? N6 Mn1 O5 C28 -125.4(7) . . . . ? N7 Mn1 O5 C28 -12(8) . . . . ? O3 Mn3 O6 C29 -141.6(5) . . . . ? O4 Mn3 O6 C29 38.6(5) . . . . ? N5 Mn3 O6 C29 129.6(5) . . . . ? N4 Mn3 O6 C29 -51.1(5) . . . . ? O7 Mn3 O6 C29 -6(6) . . . . ? O3 Mn3 O7 C30 -66.3(5) . . . . ? O4 Mn3 O7 C30 113.5(5) . . . . ? N5 Mn3 O7 C30 22.6(5) . . . . ? N4 Mn3 O7 C30 -156.7(5) . . . . ? O6 Mn3 O7 C30 158(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O8 0.85 1.88 2.703(9) 161.3 2_645 O8 H8A O6 0.84 1.98 2.795(8) 164.0 2_645 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.501 _refine_diff_density_min -1.121 _refine_diff_density_rms 0.141 # Attachment 'complex2-revised.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 662331' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Br3 Mn3 N9 O7' _chemical_formula_weight 1030.16 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' Mn Mn 0.3368 0.7283 '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 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 18.476(4) _cell_length_b 8.138(2) _cell_length_c 25.446(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.25(3) _cell_angle_gamma 90.00 _cell_volume 3819.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19311 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.00 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 4.170 _exptl_absorpt_correction_type 'empirical(SADABS, Sheldrick 1996)' _exptl_absorpt_correction_T_min 0.721672 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area dtetector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean '15x15 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19311 _diffrn_reflns_av_R_equivalents 0.1184 _diffrn_reflns_av_sigmaI/netI 0.1789 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7450 _reflns_number_gt 3111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ISOR and EADP restraints were used to deal with disordered methanol molecules and lower non-solvent C Ueq(max)/Ueq(min). ; _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^)+(0.0655P)^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 7450 _refine_ls_number_parameters 473 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1878 _refine_ls_R_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.12153(7) 0.87012(17) 0.37938(6) 0.0459(4) Uani 1 1 d . . . Mn2 Mn 0.18716(7) 0.59104(15) 0.46305(5) 0.0374(4) Uani 1 1 d . . . Mn3 Mn 0.29012(7) 0.74033(17) 0.37405(5) 0.0430(4) Uani 1 1 d . A . Br1 Br 0.37138(8) 0.10516(17) 0.67788(5) 0.0923(5) Uani 1 1 d . . . Br2 Br 0.45216(8) 0.82538(18) 0.11739(5) 0.0921(5) Uani 1 1 d . . . Br3 Br -0.24721(6) 1.17749(15) 0.42796(6) 0.0898(5) Uani 1 1 d . . . C1 C 0.2225(5) 0.3898(10) 0.5553(3) 0.040(2) Uani 1 1 d . . . C2 C 0.1955(5) 0.3178(11) 0.5986(4) 0.045(2) Uani 1 1 d . . . H2A H 0.1461 0.3266 0.6034 0.054 Uiso 1 1 calc R . . C3 C 0.2373(6) 0.2344(11) 0.6349(4) 0.053(3) Uani 1 1 d . . . H3A H 0.2165 0.1845 0.6632 0.063 Uiso 1 1 calc R . . C4 C 0.3104(6) 0.2241(11) 0.6295(4) 0.055(3) Uani 1 1 d . . . C5 C 0.3396(5) 0.2939(11) 0.5871(4) 0.051(3) Uani 1 1 d . . . H5A H 0.3892 0.2843 0.5833 0.061 Uiso 1 1 calc R . . C6 C 0.2979(5) 0.3786(10) 0.5494(3) 0.035(2) Uani 1 1 d . . . C7 C 0.3294(5) 0.4564(11) 0.5043(3) 0.040(2) Uani 1 1 d . . . C8 C 0.4020(5) 0.4555(13) 0.4891(4) 0.054(3) Uani 1 1 d . . . H8A H 0.4413 0.4029 0.5062 0.065 Uiso 1 1 calc R . . C9 C 0.4025(5) 0.5472(13) 0.4443(4) 0.056(3) Uani 1 1 d . . . H9A H 0.4431 0.5685 0.4254 0.067 Uiso 1 1 calc R . . C10 C 0.3909(5) 0.7691(12) 0.2908(4) 0.050(3) Uani 1 1 d . . . C11 C 0.4557(6) 0.7112(13) 0.2762(4) 0.063(3) Uani 1 1 d . . . H11A H 0.4873 0.6595 0.3007 0.076 Uiso 1 1 calc R . . C12 C 0.4746(6) 0.7297(13) 0.2244(4) 0.061(3) Uani 1 1 d . . . H12A H 0.5187 0.6892 0.2141 0.073 Uiso 1 1 calc R . . C13 C 0.4291(6) 0.8063(13) 0.1893(4) 0.059(3) Uani 1 1 d . . . C14 C 0.3634(6) 0.8633(12) 0.2041(4) 0.054(3) Uani 1 1 d . . . H14A H 0.3321 0.9149 0.1794 0.065 Uiso 1 1 calc R . . C15 C 0.3432(5) 0.8454(11) 0.2548(4) 0.044(2) Uani 1 1 d . . . C16 C 0.2723(5) 0.9066(11) 0.2692(4) 0.044(2) Uani 1 1 d . . . C17 C 0.2187(7) 0.9948(14) 0.2420(5) 0.072(3) Uani 1 1 d . . . H17A H 0.2204 1.0361 0.2080 0.086 Uiso 1 1 calc R . . C18 C 0.1634(6) 1.0098(13) 0.2737(5) 0.065(3) Uani 1 1 d . . . H18A H 0.1210 1.0682 0.2655 0.078 Uiso 1 1 calc R . . C19 C -0.0201(6) 1.0289(13) 0.3725(5) 0.056(3) Uani 1 1 d . . . C20 C -0.0639(7) 1.1400(14) 0.3430(5) 0.085(4) Uani 1 1 d . . . H20A H -0.0474 1.1824 0.3119 0.103 Uiso 1 1 calc R . . C21 C -0.1320(6) 1.1887(14) 0.3591(6) 0.083(4) Uani 1 1 d . . . H21A H -0.1605 1.2648 0.3401 0.100 Uiso 1 1 calc R . . C22 C -0.1540(5) 1.1179(14) 0.4042(6) 0.067(3) Uani 1 1 d . . . C23 C -0.1127(5) 1.0130(12) 0.4345(5) 0.060(3) Uani 1 1 d . . . H23A H -0.1295 0.9735 0.4658 0.072 Uiso 1 1 calc R . . C24 C -0.0452(5) 0.9647(11) 0.4184(4) 0.050(3) Uani 1 1 d . . . C25 C -0.0025(5) 0.8476(10) 0.4483(4) 0.041(2) Uani 1 1 d . . . C26 C -0.0190(5) 0.7610(12) 0.4936(4) 0.052(3) Uani 1 1 d . . . H26A H -0.0613 0.7661 0.5116 0.063 Uiso 1 1 calc R . . C27 C 0.0415(5) 0.6668(11) 0.5055(4) 0.051(3) Uani 1 1 d . . . H27A H 0.0456 0.5928 0.5334 0.061 Uiso 1 1 calc R . . C30 C 0.0119(9) 0.597(2) 0.3216(7) 0.172(8) Uani 1 1 d . . . H30A H 0.0097 0.4937 0.3032 0.206 Uiso 1 1 calc R . . H30B H -0.0097 0.6810 0.2995 0.206 Uiso 1 1 calc R . . H30C H -0.0140 0.5877 0.3531 0.206 Uiso 1 1 calc R . . N1 N 0.2908(4) 0.5441(9) 0.4688(3) 0.0405(19) Uani 1 1 d . . . N2 N 0.3348(4) 0.6022(9) 0.4318(3) 0.047(2) Uani 1 1 d . . . N3 N 0.2458(4) 0.8664(9) 0.3156(3) 0.048(2) Uani 1 1 d . . . N4 N 0.1782(4) 0.9287(9) 0.3187(3) 0.049(2) Uani 1 1 d . . . N5 N 0.0658(4) 0.8057(8) 0.4377(3) 0.0372(18) Uani 1 1 d . . . N6 N 0.0932(4) 0.6940(8) 0.4727(3) 0.0426(19) Uani 1 1 d . . . N7 N 0.1706(5) 1.1093(10) 0.4263(3) 0.058(2) Uani 1 1 d . . . N8 N 0.1621(4) 1.2466(11) 0.4166(3) 0.048(2) Uani 1 1 d . . . N9 N 0.1543(4) 1.3885(10) 0.4071(3) 0.054(2) Uani 1 1 d . . . O1 O 0.1751(3) 0.4623(7) 0.5207(2) 0.0472(16) Uani 1 1 d . . . O2 O 0.3772(3) 0.7459(8) 0.3419(3) 0.0533(17) Uani 1 1 d . . . O3 O 0.0443(4) 0.9926(8) 0.3525(3) 0.0606(19) Uani 1 1 d . . . O4 O 0.2002(3) 0.7403(7) 0.4068(2) 0.0392(15) Uani 1 1 d . . . O5 O 0.3175(4) 0.9699(8) 0.4204(3) 0.080(2) Uani 1 1 d . . . H5B H 0.2803 1.0135 0.4334 0.096 Uiso 1 1 d R A . O6 O 0.2570(4) 0.5001(8) 0.3307(3) 0.076(2) Uani 1 1 d . . . H6A H 0.2234 0.4598 0.3469 0.091 Uiso 1 1 d R A . O7 O 0.0810(4) 0.6351(8) 0.3342(3) 0.080(2) Uani 1 1 d . . . H7A H 0.1161 0.5615 0.3240 0.096 Uiso 1 1 d R . . C29 C 0.3129(4) 0.3591(8) 0.3271(3) 0.128(8) Uani 0.670(18) 1 d PRU A 1 H29A H 0.2910 0.2688 0.3079 0.153 Uiso 0.670(18) 1 calc PR A 1 H29B H 0.3283 0.3235 0.3619 0.153 Uiso 0.670(18) 1 calc PR A 1 H29C H 0.3541 0.3978 0.3093 0.153 Uiso 0.670(18) 1 calc PR A 1 C29' C 0.241(3) 0.467(6) 0.2833(19) 0.128(8) Uani 0.33 1 d PU A 2 H29D H 0.2312 0.3515 0.2798 0.153 Uiso 0.330(18) 1 calc PR A 2 H29E H 0.2811 0.4952 0.2625 0.153 Uiso 0.330(18) 1 calc PR A 2 H29F H 0.1991 0.5285 0.2713 0.153 Uiso 0.330(18) 1 calc PR A 2 C28 C 0.3807(13) 1.012(3) 0.4532(10) 0.132(8) Uani 0.670(18) 1 d PU A 1 H28A H 0.3739 1.1178 0.4688 0.159 Uiso 0.670(18) 1 calc PR A 1 H28B H 0.4222 1.0154 0.4322 0.159 Uiso 0.670(18) 1 calc PR A 1 H28C H 0.3882 0.9311 0.4803 0.159 Uiso 0.670(18) 1 calc PR A 1 C28' C 0.366(3) 1.087(6) 0.401(2) 0.132(8) Uani 0.33 1 d PU A 2 H28D H 0.3714 1.1768 0.4255 0.159 Uiso 0.330(18) 1 calc PR A 2 H28E H 0.3472 1.1272 0.3676 0.159 Uiso 0.330(18) 1 calc PR A 2 H28F H 0.4123 1.0364 0.3971 0.159 Uiso 0.330(18) 1 calc PR 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 Mn1 0.0410(9) 0.0330(9) 0.0634(10) 0.0090(7) 0.0003(7) 0.0077(6) Mn2 0.0362(8) 0.0240(8) 0.0518(9) 0.0037(6) 0.0012(7) 0.0022(6) Mn3 0.0403(9) 0.0365(9) 0.0522(9) 0.0083(7) 0.0035(7) 0.0025(7) Br1 0.1121(11) 0.0823(10) 0.0784(9) 0.0335(7) -0.0309(8) 0.0027(8) Br2 0.1046(11) 0.1001(11) 0.0749(9) 0.0140(8) 0.0333(8) -0.0065(8) Br3 0.0428(7) 0.0585(8) 0.1664(14) -0.0407(8) -0.0092(8) 0.0140(6) C1 0.057(7) 0.025(5) 0.039(6) 0.001(4) -0.001(5) -0.002(5) C2 0.052(6) 0.039(6) 0.045(6) 0.000(5) 0.004(5) -0.008(5) C3 0.085(9) 0.034(6) 0.037(6) 0.000(5) -0.002(6) -0.011(6) C4 0.077(8) 0.036(6) 0.049(7) -0.002(5) -0.020(6) -0.009(6) C5 0.047(6) 0.041(6) 0.063(7) 0.009(5) -0.011(6) 0.003(5) C6 0.048(6) 0.029(5) 0.027(5) 0.002(4) 0.002(4) 0.001(4) C7 0.048(6) 0.037(6) 0.035(6) 0.003(4) -0.008(5) 0.005(5) C8 0.037(6) 0.075(8) 0.051(7) 0.020(6) 0.000(5) 0.016(5) C9 0.030(6) 0.070(8) 0.069(8) -0.003(6) 0.003(5) 0.014(5) C10 0.043(6) 0.057(7) 0.051(7) 0.012(5) 0.010(5) -0.007(5) C11 0.063(8) 0.066(8) 0.062(8) 0.006(6) 0.014(6) -0.005(6) C12 0.046(7) 0.068(8) 0.068(8) -0.009(6) 0.006(6) -0.008(6) C13 0.065(8) 0.056(7) 0.056(7) 0.002(6) -0.001(6) -0.023(6) C14 0.057(7) 0.046(7) 0.060(7) 0.007(5) 0.013(6) -0.015(5) C15 0.052(6) 0.041(6) 0.040(6) 0.012(5) 0.004(5) -0.012(5) C16 0.049(6) 0.037(6) 0.047(6) 0.012(5) 0.003(5) -0.007(5) C17 0.083(9) 0.068(8) 0.065(8) 0.033(6) 0.003(7) 0.001(7) C18 0.050(7) 0.073(8) 0.072(8) 0.032(7) 0.001(7) 0.005(6) C19 0.037(6) 0.049(7) 0.081(8) 0.001(6) -0.020(6) 0.012(5) C20 0.083(10) 0.061(8) 0.113(10) 0.020(7) 0.006(8) 0.027(7) C21 0.056(8) 0.045(8) 0.145(13) -0.006(8) -0.022(8) 0.028(6) C22 0.039(7) 0.036(7) 0.123(11) -0.021(7) -0.011(7) 0.002(5) C23 0.045(7) 0.038(6) 0.095(9) -0.007(6) -0.010(6) 0.000(5) C24 0.042(6) 0.023(5) 0.084(8) -0.004(5) 0.006(6) 0.004(5) C25 0.030(5) 0.015(5) 0.077(7) -0.011(5) 0.003(5) 0.001(4) C26 0.037(6) 0.039(6) 0.080(8) -0.013(6) 0.002(6) -0.007(5) C27 0.056(7) 0.035(6) 0.060(7) -0.001(5) 0.000(6) -0.008(5) C30 0.124(16) 0.170(19) 0.22(2) -0.066(15) -0.052(15) 0.005(13) N1 0.036(5) 0.037(5) 0.047(5) -0.003(4) -0.004(4) -0.001(4) N2 0.046(5) 0.044(5) 0.051(5) 0.008(4) 0.010(4) -0.001(4) N3 0.039(5) 0.051(5) 0.055(5) 0.002(4) 0.009(4) 0.000(4) N4 0.057(6) 0.038(5) 0.053(5) 0.010(4) -0.004(4) 0.000(4) N5 0.037(5) 0.018(4) 0.056(5) 0.001(3) 0.002(4) 0.004(3) N6 0.056(5) 0.027(4) 0.046(5) 0.005(4) 0.003(4) -0.006(4) N7 0.078(6) 0.029(5) 0.069(6) -0.001(4) 0.008(5) 0.002(5) N8 0.050(5) 0.038(6) 0.057(5) -0.012(5) 0.016(4) -0.004(4) N9 0.071(6) 0.033(5) 0.058(5) -0.003(4) -0.009(4) 0.002(4) O1 0.043(4) 0.045(4) 0.053(4) 0.013(3) 0.000(3) -0.001(3) O2 0.040(4) 0.052(4) 0.067(5) 0.012(3) -0.001(3) 0.001(3) O3 0.057(5) 0.052(5) 0.073(5) 0.021(4) 0.001(4) 0.019(4) O4 0.033(3) 0.032(3) 0.052(4) 0.008(3) -0.003(3) 0.004(3) O5 0.066(5) 0.047(5) 0.127(7) -0.019(4) 0.002(5) -0.009(4) O6 0.113(6) 0.046(5) 0.070(5) -0.013(4) 0.009(5) -0.011(4) O7 0.061(5) 0.069(6) 0.107(6) -0.023(4) -0.013(5) 0.003(4) C29 0.128(8) 0.128(8) 0.128(8) -0.0003(7) 0.0073(8) -0.0001(7) C29' 0.128(8) 0.128(8) 0.128(8) -0.0003(7) 0.0073(8) -0.0001(7) C28 0.132(8) 0.132(8) 0.132(8) 0.0000(7) 0.0074(9) 0.0000(7) C28' 0.132(8) 0.132(8) 0.132(8) 0.0000(7) 0.0074(9) 0.0000(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 Mn1 O3 1.840(6) . ? Mn1 O4 1.897(5) . ? Mn1 N5 1.928(7) . ? Mn1 N4 1.972(8) . ? Mn1 O7 2.333(7) . ? Mn1 N7 2.431(8) . ? Mn2 O1 1.827(6) . ? Mn2 O4 1.903(6) . ? Mn2 N1 1.950(7) . ? Mn2 N6 1.955(8) . ? Mn2 N9 2.239(8) 1_545 ? Mn3 O2 1.846(7) . ? Mn3 O4 1.901(6) . ? Mn3 N3 1.948(8) . ? Mn3 N2 1.992(7) . ? Mn3 O5 2.252(7) . ? Mn3 O6 2.311(7) . ? Br1 C4 1.888(10) . ? Br2 C13 1.908(10) . ? Br3 C22 1.920(11) . ? C1 O1 1.343(10) . ? C1 C2 1.366(12) . ? C1 C6 1.413(12) . ? C2 C3 1.351(12) . ? C2 H2A 0.9300 . ? C3 C4 1.368(14) . ? C3 H3A 0.9300 . ? C4 C5 1.358(13) . ? C5 C6 1.379(11) . ? C5 H5A 0.9300 . ? C6 C7 1.461(12) . ? C7 N1 1.327(10) . ? C7 C8 1.416(12) . ? C8 C9 1.362(12) . ? C8 H8A 0.9300 . ? C9 N2 1.349(11) . ? C9 H9A 0.9300 . ? C10 O2 1.352(11) . ? C10 C11 1.358(13) . ? C10 C15 1.381(12) . ? C11 C12 1.390(13) . ? C11 H11A 0.9300 . ? C12 C13 1.345(13) . ? C12 H12A 0.9300 . ? C13 C14 1.372(14) . ? C14 C15 1.370(12) . ? C14 H14A 0.9300 . ? C15 C16 1.467(13) . ? C16 N3 1.346(11) . ? C16 C17 1.378(13) . ? C17 C18 1.342(14) . ? C17 H17A 0.9300 . ? C18 N4 1.337(11) . ? C18 H18A 0.9300 . ? C19 O3 1.353(12) . ? C19 C24 1.385(14) . ? C19 C20 1.403(14) . ? C20 C21 1.402(16) . ? C20 H20A 0.9300 . ? C21 C22 1.366(16) . ? C21 H21A 0.9300 . ? C22 C23 1.356(14) . ? C23 C24 1.392(13) . ? C23 H23A 0.9300 . ? C24 C25 1.428(12) . ? C25 N5 1.349(10) . ? C25 C26 1.398(13) . ? C26 C27 1.375(12) . ? C26 H26A 0.9300 . ? C27 N6 1.323(11) . ? C27 H27A 0.9300 . ? C30 O7 1.336(15) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1 N2 1.364(9) . ? N3 N4 1.354(10) . ? N5 N6 1.350(9) . ? N7 N8 1.153(10) . ? N8 N9 1.187(10) . ? N9 Mn2 2.239(8) 1_565 ? O5 C28' 1.41(5) . ? O5 C28 1.44(2) . ? O5 H5B 0.8563 . ? O6 C29' 1.25(4) . ? O6 C29 1.549(10) . ? O6 H6A 0.8325 . ? O7 H7A 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? 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 O3 Mn1 O4 178.9(3) . . ? O3 Mn1 N5 89.8(3) . . ? O4 Mn1 N5 89.8(3) . . ? O3 Mn1 N4 90.7(3) . . ? O4 Mn1 N4 89.6(3) . . ? N5 Mn1 N4 178.1(3) . . ? O3 Mn1 O7 92.3(3) . . ? O4 Mn1 O7 86.7(2) . . ? N5 Mn1 O7 89.2(3) . . ? N4 Mn1 O7 89.0(3) . . ? O3 Mn1 N7 90.5(3) . . ? O4 Mn1 N7 90.5(3) . . ? N5 Mn1 N7 92.3(3) . . ? N4 Mn1 N7 89.5(3) . . ? O7 Mn1 N7 176.8(3) . . ? O1 Mn2 O4 175.3(3) . . ? O1 Mn2 N1 89.5(3) . . ? O4 Mn2 N1 90.9(3) . . ? O1 Mn2 N6 89.7(3) . . ? O4 Mn2 N6 88.4(3) . . ? N1 Mn2 N6 161.7(3) . . ? O1 Mn2 N9 92.7(3) . 1_545 ? O4 Mn2 N9 91.9(3) . 1_545 ? N1 Mn2 N9 97.7(3) . 1_545 ? N6 Mn2 N9 100.7(3) . 1_545 ? O2 Mn3 O4 178.6(3) . . ? O2 Mn3 N3 89.3(3) . . ? O4 Mn3 N3 89.6(3) . . ? O2 Mn3 N2 90.3(3) . . ? O4 Mn3 N2 90.8(3) . . ? N3 Mn3 N2 177.4(3) . . ? O2 Mn3 O5 92.1(3) . . ? O4 Mn3 O5 87.0(3) . . ? N3 Mn3 O5 92.0(3) . . ? N2 Mn3 O5 90.6(3) . . ? O2 Mn3 O6 91.3(3) . . ? O4 Mn3 O6 89.7(3) . . ? N3 Mn3 O6 89.6(3) . . ? N2 Mn3 O6 87.8(3) . . ? O5 Mn3 O6 176.3(3) . . ? O1 C1 C2 117.6(9) . . ? O1 C1 C6 124.6(8) . . ? C2 C1 C6 117.7(8) . . ? C3 C2 C1 123.0(10) . . ? C3 C2 H2A 118.5 . . ? C1 C2 H2A 118.5 . . ? C2 C3 C4 119.4(10) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 119.6(9) . . ? C5 C4 Br1 118.9(9) . . ? C3 C4 Br1 121.5(9) . . ? C4 C5 C6 122.0(9) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 118.2(8) . . ? C5 C6 C7 122.1(9) . . ? C1 C6 C7 119.7(7) . . ? N1 C7 C8 107.3(8) . . ? N1 C7 C6 123.0(9) . . ? C8 C7 C6 129.7(8) . . ? C9 C8 C7 106.1(9) . . ? C9 C8 H8A 126.9 . . ? C7 C8 H8A 126.9 . . ? N2 C9 C8 109.2(9) . . ? N2 C9 H9A 125.4 . . ? C8 C9 H9A 125.4 . . ? O2 C10 C11 115.5(9) . . ? O2 C10 C15 123.5(9) . . ? C11 C10 C15 120.9(10) . . ? C10 C11 C12 119.6(11) . . ? C10 C11 H11A 120.2 . . ? C12 C11 H11A 120.2 . . ? C13 C12 C11 119.9(11) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.2(10) . . ? C12 C13 Br2 120.6(9) . . ? C14 C13 Br2 119.1(9) . . ? C15 C14 C13 121.1(10) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C10 118.3(9) . . ? C14 C15 C16 119.5(9) . . ? C10 C15 C16 122.2(9) . . ? N3 C16 C17 106.3(9) . . ? N3 C16 C15 120.7(8) . . ? C17 C16 C15 132.8(10) . . ? C18 C17 C16 107.2(10) . . ? C18 C17 H17A 126.4 . . ? C16 C17 H17A 126.4 . . ? N4 C18 C17 110.2(10) . . ? N4 C18 H18A 124.9 . . ? C17 C18 H18A 124.9 . . ? O3 C19 C24 125.3(9) . . ? O3 C19 C20 115.7(11) . . ? C24 C19 C20 119.0(10) . . ? C21 C20 C19 121.7(13) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C22 C21 C20 116.2(11) . . ? C22 C21 H21A 121.9 . . ? C20 C21 H21A 121.9 . . ? C23 C22 C21 123.9(11) . . ? C23 C22 Br3 117.7(11) . . ? C21 C22 Br3 118.3(9) . . ? C22 C23 C24 119.8(11) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C19 C24 C23 119.3(9) . . ? C19 C24 C25 120.0(9) . . ? C23 C24 C25 120.6(10) . . ? N5 C25 C26 106.6(8) . . ? N5 C25 C24 123.8(9) . . ? C26 C25 C24 129.5(9) . . ? C27 C26 C25 104.5(9) . . ? C27 C26 H26A 127.7 . . ? C25 C26 H26A 127.7 . . ? N6 C27 C26 112.0(9) . . ? N6 C27 H27A 124.0 . . ? C26 C27 H27A 124.0 . . ? O7 C30 H30A 109.5 . . ? O7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C7 N1 N2 109.7(7) . . ? C7 N1 Mn2 130.2(7) . . ? N2 N1 Mn2 120.1(5) . . ? C9 N2 N1 107.6(7) . . ? C9 N2 Mn3 134.6(7) . . ? N1 N2 Mn3 117.8(6) . . ? C16 N3 N4 110.0(7) . . ? C16 N3 Mn3 129.8(7) . . ? N4 N3 Mn3 120.2(6) . . ? C18 N4 N3 106.2(8) . . ? C18 N4 Mn1 134.3(8) . . ? N3 N4 Mn1 119.1(6) . . ? C25 N5 N6 111.1(7) . . ? C25 N5 Mn1 129.2(6) . . ? N6 N5 Mn1 119.6(6) . . ? C27 N6 N5 105.7(8) . . ? C27 N6 Mn2 133.3(7) . . ? N5 N6 Mn2 120.6(6) . . ? N8 N7 Mn1 129.0(7) . . ? N7 N8 N9 179.0(11) . . ? N8 N9 Mn2 124.2(6) . 1_565 ? C1 O1 Mn2 132.4(6) . . ? C10 O2 Mn3 130.2(6) . . ? C19 O3 Mn1 131.2(6) . . ? Mn1 O4 Mn3 120.6(3) . . ? Mn1 O4 Mn2 120.3(3) . . ? Mn3 O4 Mn2 118.7(3) . . ? C28' O5 C28 62.0(19) . . ? C28' O5 Mn3 120(2) . . ? C28 O5 Mn3 130.8(11) . . ? C28' O5 H5B 113.2 . . ? C28 O5 H5B 108.8 . . ? Mn3 O5 H5B 112.5 . . ? C29' O6 C29 84(2) . . ? C29' O6 Mn3 133(2) . . ? C29 O6 Mn3 119.7(5) . . ? C29' O6 H6A 104.7 . . ? C29 O6 H6A 104.8 . . ? Mn3 O6 H6A 106.3 . . ? C30 O7 Mn1 125.8(9) . . ? C30 O7 H7A 117.1 . . ? Mn1 O7 H7A 117.1 . . ? O6 C29 H29A 109.5 . . ? O6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O6 C29' H29D 109.5 . . ? O6 C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? O6 C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? O5 C28 H28A 109.5 . . ? O5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C28' H28D 109.5 . . ? O5 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? O5 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 176.8(8) . . . . ? C6 C1 C2 C3 -1.5(13) . . . . ? C1 C2 C3 C4 1.9(14) . . . . ? C2 C3 C4 C5 -1.8(14) . . . . ? C2 C3 C4 Br1 -178.5(7) . . . . ? C3 C4 C5 C6 1.4(14) . . . . ? Br1 C4 C5 C6 178.2(7) . . . . ? C4 C5 C6 C1 -0.9(13) . . . . ? C4 C5 C6 C7 178.8(8) . . . . ? O1 C1 C6 C5 -177.1(8) . . . . ? C2 C1 C6 C5 1.0(12) . . . . ? O1 C1 C6 C7 3.1(13) . . . . ? C2 C1 C6 C7 -178.8(8) . . . . ? C5 C6 C7 N1 -177.1(8) . . . . ? C1 C6 C7 N1 2.6(13) . . . . ? C5 C6 C7 C8 3.3(15) . . . . ? C1 C6 C7 C8 -176.9(9) . . . . ? N1 C7 C8 C9 0.7(11) . . . . ? C6 C7 C8 C9 -179.7(9) . . . . ? C7 C8 C9 N2 -0.2(12) . . . . ? O2 C10 C11 C12 -179.9(8) . . . . ? C15 C10 C11 C12 0.4(16) . . . . ? C10 C11 C12 C13 0.7(16) . . . . ? C11 C12 C13 C14 -1.3(16) . . . . ? C11 C12 C13 Br2 -177.5(7) . . . . ? C12 C13 C14 C15 0.8(15) . . . . ? Br2 C13 C14 C15 177.0(7) . . . . ? C13 C14 C15 C10 0.4(14) . . . . ? C13 C14 C15 C16 -179.5(9) . . . . ? O2 C10 C15 C14 179.4(8) . . . . ? C11 C10 C15 C14 -0.9(14) . . . . ? O2 C10 C15 C16 -0.7(15) . . . . ? C11 C10 C15 C16 178.9(9) . . . . ? C14 C15 C16 N3 168.5(8) . . . . ? C10 C15 C16 N3 -11.4(14) . . . . ? C14 C15 C16 C17 -5.3(16) . . . . ? C10 C15 C16 C17 174.9(10) . . . . ? N3 C16 C17 C18 2.4(12) . . . . ? C15 C16 C17 C18 176.8(10) . . . . ? C16 C17 C18 N4 -2.9(13) . . . . ? O3 C19 C20 C21 -179.9(11) . . . . ? C24 C19 C20 C21 0.7(17) . . . . ? C19 C20 C21 C22 -2.0(18) . . . . ? C20 C21 C22 C23 3.6(18) . . . . ? C20 C21 C22 Br3 -179.3(8) . . . . ? C21 C22 C23 C24 -3.7(16) . . . . ? Br3 C22 C23 C24 179.2(7) . . . . ? O3 C19 C24 C23 180.0(9) . . . . ? C20 C19 C24 C23 -0.7(15) . . . . ? O3 C19 C24 C25 -1.3(15) . . . . ? C20 C19 C24 C25 178.1(9) . . . . ? C22 C23 C24 C19 2.1(15) . . . . ? C22 C23 C24 C25 -176.6(9) . . . . ? C19 C24 C25 N5 7.2(14) . . . . ? C23 C24 C25 N5 -174.1(8) . . . . ? C19 C24 C25 C26 -175.9(9) . . . . ? C23 C24 C25 C26 2.8(15) . . . . ? N5 C25 C26 C27 -2.4(9) . . . . ? C24 C25 C26 C27 -179.7(9) . . . . ? C25 C26 C27 N6 2.3(10) . . . . ? C8 C7 N1 N2 -0.9(10) . . . . ? C6 C7 N1 N2 179.5(8) . . . . ? C8 C7 N1 Mn2 177.6(6) . . . . ? C6 C7 N1 Mn2 -2.1(13) . . . . ? O1 Mn2 N1 C7 -2.3(8) . . . . ? O4 Mn2 N1 C7 173.0(8) . . . . ? N6 Mn2 N1 C7 85.2(13) . . . . ? N9 Mn2 N1 C7 -95.0(8) 1_545 . . . ? O1 Mn2 N1 N2 176.0(6) . . . . ? O4 Mn2 N1 N2 -8.7(6) . . . . ? N6 Mn2 N1 N2 -96.5(11) . . . . ? N9 Mn2 N1 N2 83.3(6) 1_545 . . . ? C8 C9 N2 N1 -0.3(11) . . . . ? C8 C9 N2 Mn3 179.9(7) . . . . ? C7 N1 N2 C9 0.8(10) . . . . ? Mn2 N1 N2 C9 -177.9(6) . . . . ? C7 N1 N2 Mn3 -179.4(6) . . . . ? Mn2 N1 N2 Mn3 1.9(8) . . . . ? O2 Mn3 N2 C9 4.8(9) . . . . ? O4 Mn3 N2 C9 -174.3(9) . . . . ? N3 Mn3 N2 C9 87(7) . . . . ? O5 Mn3 N2 C9 -87.3(9) . . . . ? O6 Mn3 N2 C9 96.1(9) . . . . ? O2 Mn3 N2 N1 -174.9(6) . . . . ? O4 Mn3 N2 N1 6.0(6) . . . . ? N3 Mn3 N2 N1 -93(7) . . . . ? O5 Mn3 N2 N1 93.0(6) . . . . ? O6 Mn3 N2 N1 -83.7(6) . . . . ? C17 C16 N3 N4 -1.1(10) . . . . ? C15 C16 N3 N4 -176.3(8) . . . . ? C17 C16 N3 Mn3 179.2(7) . . . . ? C15 C16 N3 Mn3 4.0(13) . . . . ? O2 Mn3 N3 C16 9.5(8) . . . . ? O4 Mn3 N3 C16 -171.5(8) . . . . ? N2 Mn3 N3 C16 -73(7) . . . . ? O5 Mn3 N3 C16 101.5(8) . . . . ? O6 Mn3 N3 C16 -81.8(8) . . . . ? O2 Mn3 N3 N4 -170.2(7) . . . . ? O4 Mn3 N3 N4 8.8(7) . . . . ? N2 Mn3 N3 N4 108(7) . . . . ? O5 Mn3 N3 N4 -78.1(7) . . . . ? O6 Mn3 N3 N4 98.5(7) . . . . ? C17 C18 N4 N3 2.2(12) . . . . ? C17 C18 N4 Mn1 -170.9(8) . . . . ? C16 N3 N4 C18 -0.6(10) . . . . ? Mn3 N3 N4 C18 179.1(6) . . . . ? C16 N3 N4 Mn1 173.7(6) . . . . ? Mn3 N3 N4 Mn1 -6.6(9) . . . . ? O3 Mn1 N4 C18 -6.3(10) . . . . ? O4 Mn1 N4 C18 172.7(10) . . . . ? N5 Mn1 N4 C18 100(9) . . . . ? O7 Mn1 N4 C18 86.1(10) . . . . ? N7 Mn1 N4 C18 -96.7(10) . . . . ? O3 Mn1 N4 N3 -178.7(7) . . . . ? O4 Mn1 N4 N3 0.3(6) . . . . ? N5 Mn1 N4 N3 -72(10) . . . . ? O7 Mn1 N4 N3 -86.4(6) . . . . ? N7 Mn1 N4 N3 90.9(7) . . . . ? C26 C25 N5 N6 1.7(9) . . . . ? C24 C25 N5 N6 179.2(8) . . . . ? C26 C25 N5 Mn1 176.7(6) . . . . ? C24 C25 N5 Mn1 -5.7(13) . . . . ? O3 Mn1 N5 C25 -0.4(7) . . . . ? O4 Mn1 N5 C25 -179.4(7) . . . . ? N4 Mn1 N5 C25 -107(9) . . . . ? O7 Mn1 N5 C25 -92.8(7) . . . . ? N7 Mn1 N5 C25 90.0(7) . . . . ? O3 Mn1 N5 N6 174.3(6) . . . . ? O4 Mn1 N5 N6 -4.7(6) . . . . ? N4 Mn1 N5 N6 68(10) . . . . ? O7 Mn1 N5 N6 81.9(6) . . . . ? N7 Mn1 N5 N6 -95.3(6) . . . . ? C26 C27 N6 N5 -1.3(10) . . . . ? C26 C27 N6 Mn2 -173.5(6) . . . . ? C25 N5 N6 C27 -0.3(9) . . . . ? Mn1 N5 N6 C27 -175.9(6) . . . . ? C25 N5 N6 Mn2 173.1(5) . . . . ? Mn1 N5 N6 Mn2 -2.5(8) . . . . ? O1 Mn2 N6 C27 -5.0(9) . . . . ? O4 Mn2 N6 C27 179.3(8) . . . . ? N1 Mn2 N6 C27 -92.5(13) . . . . ? N9 Mn2 N6 C27 87.7(9) 1_545 . . . ? O1 Mn2 N6 N5 -176.2(6) . . . . ? O4 Mn2 N6 N5 8.1(6) . . . . ? N1 Mn2 N6 N5 96.3(11) . . . . ? N9 Mn2 N6 N5 -83.5(6) 1_545 . . . ? O3 Mn1 N7 N8 -25.4(9) . . . . ? O4 Mn1 N7 N8 154.9(9) . . . . ? N5 Mn1 N7 N8 -115.2(9) . . . . ? N4 Mn1 N7 N8 65.3(9) . . . . ? O7 Mn1 N7 N8 127(5) . . . . ? Mn1 N7 N8 N9 -159(100) . . . . ? N7 N8 N9 Mn2 -33(72) . . . 1_565 ? C2 C1 O1 Mn2 171.7(6) . . . . ? C6 C1 O1 Mn2 -10.2(13) . . . . ? O4 Mn2 O1 C1 -87(3) . . . . ? N1 Mn2 O1 C1 8.4(7) . . . . ? N6 Mn2 O1 C1 -153.2(7) . . . . ? N9 Mn2 O1 C1 106.1(7) 1_545 . . . ? C11 C10 O2 Mn3 -157.9(7) . . . . ? C15 C10 O2 Mn3 21.8(13) . . . . ? O4 Mn3 O2 C10 -65(11) . . . . ? N3 Mn3 O2 C10 -22.4(8) . . . . ? N2 Mn3 O2 C10 155.0(8) . . . . ? O5 Mn3 O2 C10 -114.4(8) . . . . ? O6 Mn3 O2 C10 67.2(8) . . . . ? C24 C19 O3 Mn1 -6.5(15) . . . . ? C20 C19 O3 Mn1 174.1(7) . . . . ? O4 Mn1 O3 C19 76(16) . . . . ? N5 Mn1 O3 C19 6.4(9) . . . . ? N4 Mn1 O3 C19 -175.4(9) . . . . ? O7 Mn1 O3 C19 95.6(9) . . . . ? N7 Mn1 O3 C19 -85.9(9) . . . . ? O3 Mn1 O4 Mn3 115(16) . . . . ? N5 Mn1 O4 Mn3 -175.6(3) . . . . ? N4 Mn1 O4 Mn3 6.2(4) . . . . ? O7 Mn1 O4 Mn3 95.2(4) . . . . ? N7 Mn1 O4 Mn3 -83.3(4) . . . . ? O3 Mn1 O4 Mn2 -59(16) . . . . ? N5 Mn1 O4 Mn2 10.8(4) . . . . ? N4 Mn1 O4 Mn2 -167.4(4) . . . . ? O7 Mn1 O4 Mn2 -78.4(3) . . . . ? N7 Mn1 O4 Mn2 103.1(4) . . . . ? O2 Mn3 O4 Mn1 34(11) . . . . ? N3 Mn3 O4 Mn1 -8.6(4) . . . . ? N2 Mn3 O4 Mn1 174.0(4) . . . . ? O5 Mn3 O4 Mn1 83.4(4) . . . . ? O6 Mn3 O4 Mn1 -98.2(3) . . . . ? O2 Mn3 O4 Mn2 -152(11) . . . . ? N3 Mn3 O4 Mn2 165.1(3) . . . . ? N2 Mn3 O4 Mn2 -12.3(4) . . . . ? O5 Mn3 O4 Mn2 -102.8(3) . . . . ? O6 Mn3 O4 Mn2 75.5(3) . . . . ? O1 Mn2 O4 Mn1 -78(3) . . . . ? N1 Mn2 O4 Mn1 -173.2(3) . . . . ? N6 Mn2 O4 Mn1 -11.5(4) . . . . ? N9 Mn2 O4 Mn1 89.1(4) 1_545 . . . ? O1 Mn2 O4 Mn3 108(3) . . . . ? N1 Mn2 O4 Mn3 13.0(4) . . . . ? N6 Mn2 O4 Mn3 174.7(3) . . . . ? N9 Mn2 O4 Mn3 -84.7(4) 1_545 . . . ? O2 Mn3 O5 C28' 26(2) . . . . ? O4 Mn3 O5 C28' -153(2) . . . . ? N3 Mn3 O5 C28' -63(2) . . . . ? N2 Mn3 O5 C28' 117(2) . . . . ? O6 Mn3 O5 C28' -179(100) . . . . ? O2 Mn3 O5 C28 -51.4(15) . . . . ? O4 Mn3 O5 C28 129.7(15) . . . . ? N3 Mn3 O5 C28 -140.8(15) . . . . ? N2 Mn3 O5 C28 38.9(15) . . . . ? O6 Mn3 O5 C28 104(4) . . . . ? O2 Mn3 O6 C29' -68(3) . . . . ? O4 Mn3 O6 C29' 111(3) . . . . ? N3 Mn3 O6 C29' 21(3) . . . . ? N2 Mn3 O6 C29' -158(3) . . . . ? O5 Mn3 O6 C29' 137(5) . . . . ? O2 Mn3 O6 C29 44.5(6) . . . . ? O4 Mn3 O6 C29 -136.5(6) . . . . ? N3 Mn3 O6 C29 133.8(6) . . . . ? N2 Mn3 O6 C29 -45.8(6) . . . . ? O5 Mn3 O6 C29 -111(4) . . . . ? O3 Mn1 O7 C30 -30.7(12) . . . . ? O4 Mn1 O7 C30 149.0(12) . . . . ? N5 Mn1 O7 C30 59.1(12) . . . . ? N4 Mn1 O7 C30 -121.4(12) . . . . ? N7 Mn1 O7 C30 177(84) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.775 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.126 # Attachment 'new complex-unpublished.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 666042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H32.50 Br3 Mn3 N6 O9.50' _chemical_formula_weight 1063.70 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' Mn Mn 0.3368 0.7283 '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 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 7.604(2) _cell_length_b 33.436(7) _cell_length_c 15.726(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.95(3) _cell_angle_gamma 90.00 _cell_volume 3996.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21963 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.00 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2102 _exptl_absorpt_coefficient_mu 3.992 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.7059 _exptl_absorpt_correction_T_max 1.2358 _exptl_absorpt_process_details Abscor _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID IP Area Detector' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21963 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7011 _reflns_number_gt 5170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO (Rigaku, 2001)' _computing_cell_refinement 'RAPID AUTO (Rigaku, 2001)' _computing_data_reduction 'RAPID AUTO (Rigaku, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+21.5542P] 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 7011 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1299 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.2017 _refine_ls_wR_factor_gt 0.1878 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.15697(7) 0.356556(15) 0.80274(3) 0.03889(15) Uani 1 1 d . . . Mn2 Mn 0.22982(7) 0.437485(15) 0.68798(3) 0.03877(15) Uani 1 1 d . . . Mn3 Mn 0.37388(7) 0.350060(15) 0.62454(4) 0.03880(15) Uani 1 1 d . . . Br1 Br -0.01299(6) 0.162986(13) 1.01983(3) 0.06660(14) Uani 1 1 d . . . Br2 Br -0.16837(7) 0.625043(13) 0.84758(4) 0.08737(18) Uani 1 1 d . . . Br3 Br 0.66108(9) 0.334635(19) 0.17727(3) 0.0988(2) Uani 1 1 d . . . C1 C 0.0519(5) 0.29398(11) 0.9215(3) 0.0479(12) Uani 1 1 d . . . C2 C -0.0215(6) 0.28661(12) 0.9999(3) 0.0578(13) Uani 1 1 d . . . H2A H -0.0575 0.3081 1.0327 0.069 Uiso 1 1 calc R . . C3 C -0.0417(5) 0.24841(12) 1.0299(3) 0.0573(13) Uani 1 1 d . . . H3A H -0.0912 0.2440 1.0824 0.069 Uiso 1 1 calc R . . C4 C 0.0122(5) 0.21659(11) 0.9814(3) 0.0538(12) Uani 1 1 d . . . C5 C 0.0870(5) 0.22291(10) 0.9044(3) 0.0466(12) Uani 1 1 d . . . H5A H 0.1247 0.2011 0.8732 0.056 Uiso 1 1 calc R . . C6 C 0.1079(5) 0.26142(10) 0.8720(2) 0.0422(11) Uani 1 1 d . . . C7 C 0.1881(5) 0.26711(10) 0.7907(2) 0.0416(11) Uani 1 1 d . . . C8 C 0.2478(6) 0.23938(12) 0.7307(3) 0.0583(14) Uani 1 1 d . . . H8A H 0.2419 0.2116 0.7341 0.070 Uiso 1 1 calc R . . C9 C 0.3154(5) 0.26116(11) 0.6672(3) 0.0498(12) Uani 1 1 d . . . H9A H 0.3658 0.2504 0.6191 0.060 Uiso 1 1 calc R . . C10 C 0.1262(5) 0.52047(10) 0.7161(2) 0.0444(11) Uani 1 1 d . . . C11 C 0.1147(6) 0.55809(12) 0.6800(3) 0.0588(13) Uani 1 1 d . . . H11A H 0.1668 0.5625 0.6282 0.071 Uiso 1 1 calc R . . C12 C 0.0283(6) 0.58966(11) 0.7182(3) 0.0618(14) Uani 1 1 d . . . H12A H 0.0227 0.6148 0.6929 0.074 Uiso 1 1 calc R . . C13 C -0.0478(5) 0.58253(11) 0.7938(3) 0.0522(12) Uani 1 1 d . . . C14 C -0.0399(5) 0.54558(10) 0.8319(3) 0.0481(12) Uani 1 1 d . . . H14A H -0.0929 0.5416 0.8837 0.058 Uiso 1 1 calc R . . C15 C 0.0466(5) 0.51408(10) 0.7939(2) 0.0414(11) Uani 1 1 d . . . C16 C 0.0503(5) 0.47513(10) 0.8360(2) 0.0441(11) Uani 1 1 d . . . C17 C -0.0219(6) 0.46213(12) 0.9116(3) 0.0670(14) Uani 1 1 d . . . H17A H -0.0827 0.4776 0.9500 0.080 Uiso 1 1 calc R . . C18 C 0.0143(6) 0.42257(12) 0.9178(3) 0.0620(14) Uani 1 1 d . . . H18A H -0.0171 0.4062 0.9626 0.074 Uiso 1 1 calc R . . C19 C 0.5099(5) 0.32429(11) 0.4615(2) 0.0452(11) Uani 1 1 d . . . C20 C 0.5741(5) 0.29187(11) 0.4170(3) 0.0519(12) Uani 1 1 d . . . H20A H 0.5845 0.2672 0.4439 0.062 Uiso 1 1 calc R . . C21 C 0.6228(5) 0.29566(13) 0.3336(3) 0.0613(13) Uani 1 1 d . . . H21A H 0.6676 0.2738 0.3047 0.074 Uiso 1 1 calc R . . C22 C 0.6046(5) 0.33134(12) 0.2945(3) 0.0570(13) Uani 1 1 d . . . C23 C 0.5404(5) 0.36416(12) 0.3343(2) 0.0523(12) Uani 1 1 d . . . H23A H 0.5280 0.3882 0.3048 0.063 Uiso 1 1 calc R . . C24 C 0.4930(4) 0.36190(10) 0.4195(2) 0.0417(11) Uani 1 1 d . . . C25 C 0.4290(5) 0.39701(11) 0.4642(2) 0.0418(11) Uani 1 1 d . . . C26 C 0.4106(6) 0.43640(12) 0.4374(3) 0.0615(14) Uani 1 1 d . . . H26A H 0.4354 0.4468 0.3843 0.074 Uiso 1 1 calc R . . C27 C 0.3482(6) 0.45678(12) 0.5057(3) 0.0597(13) Uani 1 1 d . . . H27A H 0.3245 0.4841 0.5064 0.072 Uiso 1 1 calc R . . C28 C -0.2504(4) 0.34740(10) 0.7177(2) 0.0368(10) Uani 1 1 d . . . C29 C -0.2599(7) 0.30384(14) 0.7329(4) 0.090(2) Uani 1 1 d . . . H29A H -0.1487 0.2945 0.7558 0.108 Uiso 1 1 calc R . . H29B H -0.2870 0.2904 0.6801 0.108 Uiso 1 1 calc R . . H29C H -0.3501 0.2984 0.7725 0.108 Uiso 1 1 calc R . . C30 C 0.5062(9) 0.3369(2) 0.9324(4) 0.144(3) Uani 1 1 d . . . H30A H 0.6208 0.3461 0.9511 0.173 Uiso 1 1 calc R . . H30B H 0.5160 0.3109 0.9071 0.173 Uiso 1 1 calc R . . H30C H 0.4314 0.3353 0.9803 0.173 Uiso 1 1 calc R . . C31 C -0.1343(8) 0.44180(18) 0.5656(4) 0.110(2) Uani 1 1 d . . . H31A H -0.2517 0.4312 0.5635 0.132 Uiso 1 1 calc R . . H31B H -0.0747 0.4339 0.5155 0.132 Uiso 1 1 calc R . . H31C H -0.1392 0.4705 0.5684 0.132 Uiso 1 1 calc R . . C32 C 0.6064(9) 0.47337(19) 0.7536(6) 0.149(3) Uani 1 1 d . . . H32A H 0.7183 0.4666 0.7797 0.179 Uiso 1 1 calc R . . H32B H 0.5477 0.4923 0.7887 0.179 Uiso 1 1 calc R . . H32C H 0.6238 0.4849 0.6986 0.179 Uiso 1 1 calc R . . C33 C 0.4990(18) 0.4390(3) 0.9848(11) 0.153(7) Uani 0.50 1 d P . . H33A H 0.4287 0.4158 0.9959 0.183 Uiso 0.50 1 calc PR . . H33B H 0.5923 0.4318 0.9482 0.183 Uiso 0.50 1 calc PR . . H33C H 0.4268 0.4592 0.9577 0.183 Uiso 0.50 1 calc PR . . N1 N 0.2219(4) 0.30426(8) 0.75952(19) 0.0403(9) Uani 1 1 d . . . N2 N 0.2994(4) 0.30087(8) 0.6833(2) 0.0446(9) Uani 1 1 d . . . N3 N 0.1234(4) 0.44302(8) 0.79898(19) 0.0426(9) Uani 1 1 d . . . N4 N 0.1020(4) 0.41043(9) 0.8499(2) 0.0518(10) Uani 1 1 d . . . N5 N 0.3778(4) 0.39496(8) 0.54539(19) 0.0383(8) Uani 1 1 d . . . N6 N 0.3259(4) 0.43201(8) 0.57151(19) 0.0449(9) Uani 1 1 d . . . O1 O 0.0660(4) 0.33221(7) 0.89775(17) 0.0577(9) Uani 1 1 d . . . O2 O 0.2145(4) 0.49247(7) 0.67373(17) 0.0562(9) Uani 1 1 d . . . O3 O 0.4687(4) 0.31803(7) 0.54178(17) 0.0560(9) Uani 1 1 d . . . O4 O 0.2498(3) 0.38119(6) 0.70464(14) 0.0352(7) Uani 1 1 d . . . O5 O -0.1119(4) 0.36414(9) 0.7337(2) 0.0675(10) Uani 1 1 d . . . O6 O -0.3807(4) 0.36532(8) 0.6891(2) 0.0657(10) Uani 1 1 d . . . O7 O 0.4350(4) 0.36322(10) 0.8736(2) 0.0794(12) Uani 1 1 d . . . H7A H 0.5093 0.3644 0.8344 0.095 Uiso 1 1 d R . . O8 O -0.0477(4) 0.42785(8) 0.6340(2) 0.0687(10) Uani 1 1 d . . . O9 O 0.5083(4) 0.44052(9) 0.7449(2) 0.0710(10) Uani 1 1 d . . . O10 O 0.5616(14) 0.4520(5) 1.0518(9) 0.261(9) Uani 0.50 1 d P . . H9B H 0.5797 0.4240 0.7217 0.314 Uiso 1 1 d R . . H8B H -0.1057 0.4101 0.6537 0.314 Uiso 1 1 d R . . H10B H 0.5491 0.4462 1.1039 0.314 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0484(3) 0.0290(3) 0.0394(3) 0.0024(2) 0.0033(2) 0.0034(2) Mn2 0.0468(3) 0.0286(3) 0.0413(3) 0.0018(2) 0.0072(2) 0.0061(2) Mn3 0.0436(3) 0.0307(3) 0.0423(3) 0.0034(2) 0.0053(2) 0.0081(2) Br1 0.0684(3) 0.0484(2) 0.0828(3) 0.0287(2) 0.0005(2) -0.0072(2) Br2 0.1177(4) 0.0439(2) 0.1026(4) -0.0025(2) 0.0342(3) 0.0307(2) Br3 0.1287(4) 0.1084(4) 0.0619(3) -0.0222(3) 0.0407(3) -0.0046(4) C1 0.046(2) 0.044(2) 0.053(2) 0.0112(18) -0.0032(19) 0.0080(17) C2 0.082(3) 0.049(2) 0.043(2) 0.0121(19) 0.014(2) -0.003(2) C3 0.069(3) 0.056(2) 0.047(2) 0.0096(19) 0.009(2) 0.003(2) C4 0.069(2) 0.0381(19) 0.055(2) 0.0270(17) 0.002(2) -0.0060(18) C5 0.046(2) 0.0278(17) 0.065(3) 0.0080(17) -0.0061(19) 0.0047(15) C6 0.049(2) 0.0377(18) 0.040(2) 0.0102(16) 0.0005(17) 0.0050(16) C7 0.0394(19) 0.0374(18) 0.047(2) 0.0017(17) -0.0064(17) 0.0021(15) C8 0.090(3) 0.033(2) 0.051(2) 0.0085(18) 0.001(2) 0.002(2) C9 0.060(2) 0.0401(19) 0.050(2) -0.0068(18) 0.0068(19) 0.0165(17) C10 0.052(2) 0.0304(17) 0.051(2) -0.0157(16) 0.0043(18) 0.0092(16) C11 0.086(3) 0.048(2) 0.044(2) 0.0105(19) 0.011(2) 0.006(2) C12 0.094(3) 0.0339(19) 0.058(3) 0.0048(19) 0.008(2) 0.022(2) C13 0.066(2) 0.042(2) 0.050(2) -0.0081(18) 0.009(2) 0.0111(18) C14 0.058(2) 0.0359(19) 0.051(2) -0.0052(17) 0.0096(19) 0.0067(17) C15 0.046(2) 0.0334(18) 0.045(2) -0.0011(16) 0.0054(17) 0.0037(15) C16 0.051(2) 0.0401(19) 0.042(2) 0.0042(16) 0.0123(17) 0.0115(16) C17 0.103(3) 0.037(2) 0.063(3) -0.0017(19) 0.035(2) 0.018(2) C18 0.098(3) 0.039(2) 0.050(2) 0.0126(18) 0.027(2) 0.005(2) C19 0.0381(19) 0.053(2) 0.045(2) -0.0066(18) 0.0025(17) -0.0006(17) C20 0.061(2) 0.0331(18) 0.062(3) -0.0115(18) 0.007(2) 0.0116(17) C21 0.048(2) 0.070(2) 0.067(3) -0.034(2) 0.016(2) -0.0048(19) C22 0.058(2) 0.057(2) 0.057(2) -0.008(2) 0.017(2) -0.004(2) C23 0.051(2) 0.055(2) 0.052(2) -0.0092(19) 0.0161(18) -0.0097(18) C24 0.0369(18) 0.0397(19) 0.049(2) -0.0045(17) 0.0069(17) 0.0002(15) C25 0.0383(18) 0.048(2) 0.039(2) 0.0052(17) 0.0053(16) -0.0010(16) C26 0.089(3) 0.046(2) 0.051(2) 0.0123(19) 0.015(2) 0.012(2) C27 0.083(3) 0.046(2) 0.052(2) 0.0064(19) 0.019(2) 0.002(2) C28 0.0321(17) 0.0366(18) 0.0421(19) -0.0056(16) 0.0081(15) 0.0004(14) C29 0.070(3) 0.070(3) 0.128(5) 0.013(3) -0.020(3) -0.005(3) C30 0.129(5) 0.185(7) 0.114(5) 0.015(5) -0.063(4) 0.038(5) C31 0.112(4) 0.110(4) 0.105(4) 0.026(4) -0.047(3) 0.000(4) C32 0.099(5) 0.108(5) 0.238(9) -0.065(5) -0.014(5) -0.004(4) C33 0.121(10) 0.044(6) 0.29(2) 0.032(9) 0.008(12) -0.018(6) N1 0.0452(16) 0.0297(14) 0.0459(17) 0.0080(13) 0.0010(14) 0.0033(12) N2 0.0559(18) 0.0310(15) 0.0469(18) -0.0023(14) 0.0056(15) 0.0030(13) N3 0.0547(17) 0.0300(14) 0.0436(17) 0.0037(13) 0.0091(14) 0.0080(13) N4 0.075(2) 0.0319(15) 0.0489(19) 0.0057(14) 0.0092(17) 0.0080(15) N5 0.0352(14) 0.0307(14) 0.0493(17) 0.0031(13) 0.0076(13) 0.0034(12) N6 0.0594(18) 0.0312(15) 0.0449(17) -0.0003(13) 0.0133(15) 0.0080(13) O1 0.0949(19) 0.0308(13) 0.0489(15) 0.0036(12) 0.0224(14) 0.0005(13) O2 0.0768(17) 0.0346(13) 0.0586(16) 0.0056(12) 0.0226(14) 0.0044(13) O3 0.0766(17) 0.0375(13) 0.0543(16) -0.0042(12) 0.0107(14) 0.0158(12) O4 0.0392(12) 0.0327(11) 0.0338(13) 0.0017(10) 0.0035(10) 0.0090(10) O5 0.0541(17) 0.0737(19) 0.074(2) 0.0118(16) -0.0033(16) -0.0035(15) O6 0.0533(16) 0.0500(16) 0.093(2) -0.0042(16) -0.0055(16) 0.0101(13) O7 0.0680(19) 0.091(2) 0.078(2) 0.0051(19) -0.0157(18) -0.0006(17) O8 0.0583(16) 0.0567(16) 0.090(2) 0.0289(15) -0.0160(16) -0.0004(14) O9 0.0502(16) 0.0693(18) 0.093(2) -0.0211(17) -0.0039(16) -0.0084(14) O10 0.108(8) 0.50(3) 0.180(12) -0.052(15) 0.046(8) -0.030(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.856(3) . ? Mn1 O4 1.906(2) . ? Mn1 N1 1.946(3) . ? Mn1 N4 1.998(3) . ? Mn1 O5 2.296(3) . ? Mn1 O7 2.366(3) . ? Mn2 O2 1.855(3) . ? Mn2 O4 1.906(2) . ? Mn2 N3 1.958(3) . ? Mn2 N6 2.003(3) . ? Mn2 O8 2.271(3) . ? Mn2 O9 2.273(3) . ? Mn3 O3 1.850(3) . ? Mn3 O4 1.908(2) . ? Mn3 N5 1.951(3) . ? Mn3 N2 1.978(3) . ? Mn3 O6 2.155(3) 1_655 ? Br1 C4 1.903(4) . ? Br2 C13 1.905(4) . ? Br3 C22 1.910(4) . ? C1 O1 1.337(4) . ? C1 C2 1.393(6) . ? C1 C6 1.412(5) . ? C2 C3 1.372(6) . ? C2 H2A 0.9300 . ? C3 C4 1.380(6) . ? C3 H3A 0.9300 . ? C4 C5 1.371(6) . ? C5 C6 1.396(5) . ? C5 H5A 0.9300 . ? C6 C7 1.448(5) . ? C7 N1 1.363(4) . ? C7 C8 1.408(5) . ? C8 C9 1.352(6) . ? C8 H8A 0.9300 . ? C9 N2 1.358(5) . ? C9 H9A 0.9300 . ? C10 O2 1.342(4) . ? C10 C11 1.381(5) . ? C10 C15 1.400(5) . ? C11 C12 1.390(6) . ? C11 H11A 0.9300 . ? C12 C13 1.361(6) . ? C12 H12A 0.9300 . ? C13 C14 1.374(5) . ? C14 C15 1.388(5) . ? C14 H14A 0.9300 . ? C15 C16 1.461(5) . ? C16 N3 1.350(5) . ? C16 C17 1.396(6) . ? C17 C18 1.354(5) . ? C17 H17A 0.9300 . ? C18 N4 1.341(5) . ? C18 H18A 0.9300 . ? C19 O3 1.328(5) . ? C19 C20 1.387(5) . ? C19 C24 1.424(5) . ? C20 C21 1.382(6) . ? C20 H20A 0.9300 . ? C21 C22 1.347(6) . ? C21 H21A 0.9300 . ? C22 C23 1.363(6) . ? C23 C24 1.401(5) . ? C23 H23A 0.9300 . ? C24 C25 1.460(5) . ? C25 N5 1.350(5) . ? C25 C26 1.388(5) . ? C26 C27 1.370(6) . ? C26 H26A 0.9300 . ? C27 N6 1.340(5) . ? C27 H27A 0.9300 . ? C28 O5 1.211(4) . ? C28 O6 1.230(4) . ? C28 C29 1.478(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 O7 1.375(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 O8 1.326(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 O9 1.332(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O10 1.22(2) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N1 N2 1.359(4) . ? N3 N4 1.365(4) . ? N5 N6 1.367(4) . ? O6 Mn3 2.155(3) 1_455 ? O7 H7A 0.8500 . ? O8 H8B 0.8084 . ? O9 H9B 0.8651 . ? O10 H10B 0.8500 . ? 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 O4 179.54(11) . . ? O1 Mn1 N1 89.60(12) . . ? O4 Mn1 N1 90.02(11) . . ? O1 Mn1 N4 90.47(12) . . ? O4 Mn1 N4 89.93(12) . . ? N1 Mn1 N4 177.19(13) . . ? O1 Mn1 O5 94.52(12) . . ? O4 Mn1 O5 85.29(10) . . ? N1 Mn1 O5 99.57(12) . . ? N4 Mn1 O5 83.22(12) . . ? O1 Mn1 O7 90.81(13) . . ? O4 Mn1 O7 89.46(11) . . ? N1 Mn1 O7 90.91(12) . . ? N4 Mn1 O7 86.28(13) . . ? O5 Mn1 O7 168.25(11) . . ? O2 Mn2 O4 178.65(11) . . ? O2 Mn2 N3 89.30(12) . . ? O4 Mn2 N3 90.25(11) . . ? O2 Mn2 N6 90.20(12) . . ? O4 Mn2 N6 90.32(11) . . ? N3 Mn2 N6 176.96(13) . . ? O2 Mn2 O8 92.39(11) . . ? O4 Mn2 O8 88.86(10) . . ? N3 Mn2 O8 86.55(12) . . ? N6 Mn2 O8 90.48(12) . . ? O2 Mn2 O9 93.28(12) . . ? O4 Mn2 O9 85.47(10) . . ? N3 Mn2 O9 92.99(13) . . ? N6 Mn2 O9 90.03(13) . . ? O8 Mn2 O9 174.31(11) . . ? O3 Mn3 O4 173.30(11) . . ? O3 Mn3 N5 88.96(12) . . ? O4 Mn3 N5 91.14(11) . . ? O3 Mn3 N2 88.38(12) . . ? O4 Mn3 N2 89.40(11) . . ? N5 Mn3 N2 161.50(12) . . ? O3 Mn3 O6 96.69(12) . 1_655 ? O4 Mn3 O6 89.98(11) . 1_655 ? N5 Mn3 O6 94.96(12) . 1_655 ? N2 Mn3 O6 103.54(12) . 1_655 ? O1 C1 C2 117.0(3) . . ? O1 C1 C6 123.7(3) . . ? C2 C1 C6 119.3(3) . . ? C3 C2 C1 121.5(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 Br1 118.3(3) . . ? C3 C4 Br1 121.0(3) . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C1 118.0(3) . . ? C5 C6 C7 120.0(3) . . ? C1 C6 C7 121.9(3) . . ? N1 C7 C8 106.9(3) . . ? N1 C7 C6 121.8(3) . . ? C8 C7 C6 131.3(3) . . ? C9 C8 C7 106.2(3) . . ? C9 C8 H8A 126.9 . . ? C7 C8 H8A 126.9 . . ? C8 C9 N2 110.5(3) . . ? C8 C9 H9A 124.8 . . ? N2 C9 H9A 124.8 . . ? O2 C10 C11 117.2(3) . . ? O2 C10 C15 124.4(3) . . ? C11 C10 C15 118.3(3) . . ? C10 C11 C12 122.6(4) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C13 C12 C11 117.7(4) . . ? C13 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C12 C13 C14 121.7(4) . . ? C12 C13 Br2 118.9(3) . . ? C14 C13 Br2 119.4(3) . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C10 119.1(3) . . ? C14 C15 C16 118.9(3) . . ? C10 C15 C16 122.0(3) . . ? N3 C16 C17 107.4(3) . . ? N3 C16 C15 121.1(3) . . ? C17 C16 C15 131.4(3) . . ? C18 C17 C16 106.3(4) . . ? C18 C17 H17A 126.8 . . ? C16 C17 H17A 126.8 . . ? N4 C18 C17 110.1(4) . . ? N4 C18 H18A 124.9 . . ? C17 C18 H18A 124.9 . . ? O3 C19 C20 117.0(3) . . ? O3 C19 C24 124.0(3) . . ? C20 C19 C24 119.0(3) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C22 C21 C20 119.3(4) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 122.4(4) . . ? C21 C22 Br3 118.0(3) . . ? C23 C22 Br3 119.6(3) . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C23 C24 C19 118.0(3) . . ? C23 C24 C25 121.2(3) . . ? C19 C24 C25 120.9(3) . . ? N5 C25 C26 107.8(3) . . ? N5 C25 C24 121.7(3) . . ? C26 C25 C24 130.5(4) . . ? C27 C26 C25 105.6(4) . . ? C27 C26 H26A 127.2 . . ? C25 C26 H26A 127.2 . . ? N6 C27 C26 110.7(4) . . ? N6 C27 H27A 124.6 . . ? C26 C27 H27A 124.6 . . ? O5 C28 O6 122.3(3) . . ? O5 C28 C29 118.0(3) . . ? O6 C28 C29 119.7(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 C30 H30A 109.5 . . ? O7 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O7 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O8 C31 H31A 109.5 . . ? O8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O9 C32 H32A 109.5 . . ? O9 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O9 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O10 C33 H33A 109.5 . . ? O10 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O10 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 N1 C7 109.5(3) . . ? N2 N1 Mn1 120.4(2) . . ? C7 N1 Mn1 129.8(2) . . ? C9 N2 N1 106.9(3) . . ? C9 N2 Mn3 134.2(3) . . ? N1 N2 Mn3 118.8(2) . . ? C16 N3 N4 108.9(3) . . ? C16 N3 Mn2 130.4(2) . . ? N4 N3 Mn2 120.6(2) . . ? C18 N4 N3 107.3(3) . . ? C18 N4 Mn1 133.2(3) . . ? N3 N4 Mn1 118.1(2) . . ? C25 N5 N6 109.5(3) . . ? C25 N5 Mn3 130.8(2) . . ? N6 N5 Mn3 119.6(2) . . ? C27 N6 N5 106.4(3) . . ? C27 N6 Mn2 135.1(3) . . ? N5 N6 Mn2 118.4(2) . . ? C1 O1 Mn1 132.8(2) . . ? C10 O2 Mn2 131.4(2) . . ? C19 O3 Mn3 133.5(2) . . ? Mn1 O4 Mn2 120.55(12) . . ? Mn1 O4 Mn3 120.24(11) . . ? Mn2 O4 Mn3 119.14(12) . . ? C28 O5 Mn1 143.2(3) . . ? C28 O6 Mn3 136.9(2) . 1_455 ? C30 O7 Mn1 125.5(4) . . ? C30 O7 H7A 105.1 . . ? Mn1 O7 H7A 105.6 . . ? C31 O8 Mn2 133.1(3) . . ? C31 O8 H8B 107.9 . . ? Mn2 O8 H8B 118.2 . . ? C32 O9 Mn2 126.0(4) . . ? C32 O9 H9B 102.3 . . ? Mn2 O9 H9B 113.2 . . ? C33 O10 H10B 134.2 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9B O6 0.87 2.05 2.803(4) 144.7 1_655 O8 H8B O5 0.81 1.99 2.699(4) 146.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.934 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.127