data_Compound 1_re2mn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H80 Br8 Mn N6 O8 Re2' _chemical_formula_weight 1863.74 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' 'Re' 'Re' -1.0185 7.2310 '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 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.1814(4) _cell_length_b 16.5320(4) _cell_length_c 35.0505(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.6510(10) _cell_angle_gamma 90.00 _cell_volume 6435.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'hexagonal pltes' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3572 _exptl_absorpt_coefficient_mu 8.958 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.299 _exptl_absorpt_correction_T_max 0.378 _exptl_absorpt_process_details 'sadabs' _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 detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48843 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 29.87 _reflns_number_total 9235 _reflns_number_gt 7086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius X8 APEX' _computing_cell_refinement 'Bruker-Nonius X8 APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0334P)^2^+18.3699P] 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 9235 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0898 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Re1 Re 0.685763(14) -0.099640(10) 0.374831(5) 0.04661(6) Uani 1 1 d . . . Mn1 Mn 0.5000 0.09394(5) 0.2500 0.04357(19) Uani 1 2 d S . . Br3 Br 0.85181(5) -0.19735(3) 0.380693(17) 0.07008(15) Uani 1 1 d . . . Br2 Br 0.62753(5) -0.12083(4) 0.439267(15) 0.07385(16) Uani 1 1 d . . . Br4 Br 0.82303(5) 0.01377(3) 0.396458(19) 0.07555(16) Uani 1 1 d . . . Br1 Br 0.53928(6) -0.20302(4) 0.34703(2) 0.08578(18) Uani 1 1 d . . . O3 O 0.6361(3) -0.00396(19) 0.26713(9) 0.0573(8) Uani 1 1 d . . . O1 O 0.7140(3) -0.07438(18) 0.31826(9) 0.0541(7) Uani 1 1 d . . . O4 O 0.4889(3) 0.07189(18) 0.31256(8) 0.0521(7) Uani 1 1 d . . . O2 O 0.5550(3) -0.01193(19) 0.36012(9) 0.0547(7) Uani 1 1 d . . . N2 N 1.2666(3) 0.5323(2) 0.09156(11) 0.0542(9) Uani 1 1 d . . . N1 N 0.6407(4) 0.1841(2) 0.25067(11) 0.0589(10) Uani 1 1 d . . . C7 C 0.5530(3) 0.0169(2) 0.32621(11) 0.0441(9) Uani 1 1 d . . . C6 C 0.6417(4) -0.0229(2) 0.30124(12) 0.0460(9) Uani 1 1 d . . . C20 C 1.1547(4) 0.5843(3) 0.08844(14) 0.0528(10) Uani 1 1 d . . . H20A H 1.1123 0.5734 0.1105 0.063 Uiso 1 1 calc R . . H20B H 1.1795 0.6406 0.0900 0.063 Uiso 1 1 calc R . . C21 C 1.0675(4) 0.5735(3) 0.05260(16) 0.0635(12) Uani 1 1 d . . . H21A H 1.0458 0.5169 0.0495 0.076 Uiso 1 1 calc R . . H21B H 1.1053 0.5901 0.0303 0.076 Uiso 1 1 calc R . . C16 C 1.3508(5) 0.5585(4) 0.12663(14) 0.0673(13) Uani 1 1 d . . . H16A H 1.4259 0.5290 0.1268 0.081 Uiso 1 1 calc R . . H16B H 1.3687 0.6155 0.1241 0.081 Uiso 1 1 calc R . . C12 C 1.2286(4) 0.4439(3) 0.09486(18) 0.0720(15) Uani 1 1 d . . . H12A H 1.1781 0.4397 0.1155 0.086 Uiso 1 1 calc R . . H12B H 1.1801 0.4287 0.0712 0.086 Uiso 1 1 calc R . . C8 C 1.3336(4) 0.5407(4) 0.05649(15) 0.0697(14) Uani 1 1 d . . . H8A H 1.4063 0.5083 0.0607 0.084 Uiso 1 1 calc R . . H8B H 1.2838 0.5177 0.0347 0.084 Uiso 1 1 calc R . . C9 C 1.3680(6) 0.6232(4) 0.04605(18) 0.0869(18) Uani 1 1 d . . . H9A H 1.4162 0.6487 0.0675 0.104 Uiso 1 1 calc R . . H9B H 1.2967 0.6559 0.0392 0.104 Uiso 1 1 calc R . . C10 C 1.4432(8) 0.6153(5) 0.0106(2) 0.110(2) Uani 1 1 d . . . H10A H 1.5164 0.5853 0.0186 0.132 Uiso 1 1 calc R . . H10B H 1.3966 0.5846 -0.0095 0.132 Uiso 1 1 calc R . . C13 C 1.3313(6) 0.3839(4) 0.1024(3) 0.107(3) Uani 1 1 d . . . H13A H 1.3892 0.4043 0.1229 0.129 Uiso 1 1 calc R . . H13B H 1.3719 0.3788 0.0795 0.129 Uiso 1 1 calc R . . C17 C 1.3036(6) 0.5457(5) 0.16466(16) 0.093(2) Uani 1 1 d . . . H17A H 1.2801 0.4896 0.1671 0.111 Uiso 1 1 calc R . . H17B H 1.2331 0.5793 0.1661 0.111 Uiso 1 1 calc R . . N3 N 0.7285(5) 0.2906(3) 0.23094(17) 0.1013(18) Uani 1 1 d . . . H3A H 0.7430 0.3310 0.2168 0.122 Uiso 1 1 calc R . . C22 C 0.9553(5) 0.6234(3) 0.05519(16) 0.0662(13) Uani 1 1 d . . . H22A H 0.9774 0.6800 0.0582 0.079 Uiso 1 1 calc R . . H22B H 0.9184 0.6070 0.0777 0.079 Uiso 1 1 calc R . . C2 C 0.6459(6) 0.2351(4) 0.22294(17) 0.0819(17) Uani 1 1 d . . . H2A H 0.5963 0.2326 0.1998 0.098 Uiso 1 1 calc R . . C23 C 0.8649(6) 0.6135(4) 0.01971(19) 0.0871(18) Uani 1 1 d . . . H23A H 0.7953 0.6462 0.0222 0.131 Uiso 1 1 calc R . . H23B H 0.8414 0.5578 0.0170 0.131 Uiso 1 1 calc R . . H23C H 0.9009 0.6303 -0.0026 0.131 Uiso 1 1 calc R . . C4 C 0.7853(9) 0.2723(6) 0.2651(3) 0.154(4) Uani 1 1 d . . . H4A H 0.8507 0.2994 0.2781 0.185 Uiso 1 1 calc R . . C5 C 0.7297(7) 0.2067(5) 0.2773(2) 0.124(3) Uani 1 1 d . . . H5A H 0.7500 0.1809 0.3008 0.148 Uiso 1 1 calc R . . C14 C 1.2861(8) 0.2975(5) 0.1140(3) 0.133(3) Uani 1 1 d . . . H14A H 1.3547 0.2621 0.1203 0.159 Uiso 1 1 calc R . . H14B H 1.2443 0.3024 0.1367 0.159 Uiso 1 1 calc R . . C15 C 1.2113(10) 0.2651(6) 0.0851(3) 0.158(4) Uani 1 1 d . . . H15A H 1.1860 0.2124 0.0925 0.237 Uiso 1 1 calc R . . H15B H 1.2526 0.2604 0.0627 0.237 Uiso 1 1 calc R . . H15C H 1.1422 0.2993 0.0795 0.237 Uiso 1 1 calc R . . C18 C 1.4020(9) 0.5678(6) 0.1977(3) 0.148(3) Uiso 1 1 d . . . H18A H 1.3672 0.5751 0.2215 0.178 Uiso 1 1 calc R . . H18B H 1.4428 0.6172 0.1919 0.178 Uiso 1 1 calc R . . C19 C 1.4945(13) 0.4923(9) 0.2009(4) 0.237(7) Uiso 1 1 d . . . H19A H 1.5556 0.5008 0.2221 0.356 Uiso 1 1 calc R . . H19B H 1.5314 0.4879 0.1776 0.356 Uiso 1 1 calc R . . H19C H 1.4515 0.4433 0.2050 0.356 Uiso 1 1 calc R . . C11 C 1.4727(10) 0.6876(6) -0.0038(3) 0.155(4) Uani 1 1 d . . . H11A H 1.5179 0.6790 -0.0251 0.232 Uiso 1 1 calc R . . H11B H 1.5206 0.7179 0.0157 0.232 Uiso 1 1 calc R . . H11C H 1.4007 0.7172 -0.0123 0.232 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.04290(9) 0.04889(10) 0.04833(10) 0.00829(7) 0.00653(6) 0.00421(7) Mn1 0.0508(5) 0.0390(4) 0.0416(4) 0.000 0.0080(4) 0.000 Br3 0.0651(3) 0.0619(3) 0.0825(4) 0.0145(3) 0.0051(3) 0.0213(2) Br2 0.0767(3) 0.0927(4) 0.0542(3) 0.0192(3) 0.0161(2) 0.0051(3) Br4 0.0601(3) 0.0663(3) 0.1016(4) -0.0129(3) 0.0151(3) -0.0115(2) Br1 0.0756(4) 0.0872(4) 0.0921(4) -0.0055(3) -0.0008(3) -0.0258(3) O3 0.0694(19) 0.0602(18) 0.0459(17) 0.0083(14) 0.0215(15) 0.0191(15) O1 0.0574(17) 0.0536(16) 0.0536(18) 0.0115(14) 0.0164(14) 0.0203(14) O4 0.0542(17) 0.0549(16) 0.0490(17) 0.0066(14) 0.0144(13) 0.0202(14) O2 0.0505(16) 0.0673(19) 0.0486(17) 0.0104(15) 0.0156(13) 0.0183(14) N2 0.0427(18) 0.061(2) 0.062(2) -0.0117(18) 0.0159(16) -0.0022(16) N1 0.064(2) 0.060(2) 0.052(2) 0.0021(18) 0.0035(18) -0.0151(19) C7 0.044(2) 0.050(2) 0.040(2) 0.0034(17) 0.0120(16) 0.0055(17) C6 0.047(2) 0.045(2) 0.049(2) 0.0030(18) 0.0147(18) 0.0055(17) C20 0.050(2) 0.049(2) 0.061(3) -0.007(2) 0.012(2) 0.0012(18) C21 0.053(3) 0.064(3) 0.073(3) -0.016(3) 0.007(2) 0.001(2) C16 0.053(3) 0.091(4) 0.058(3) -0.010(3) 0.008(2) -0.003(3) C12 0.052(3) 0.062(3) 0.103(4) -0.009(3) 0.016(3) 0.008(2) C8 0.048(3) 0.105(4) 0.058(3) -0.020(3) 0.016(2) -0.008(3) C9 0.075(4) 0.117(5) 0.072(4) 0.006(4) 0.023(3) -0.016(3) C10 0.117(6) 0.119(6) 0.096(5) 0.006(5) 0.018(5) -0.013(5) C13 0.072(4) 0.073(4) 0.178(8) -0.009(5) 0.018(4) 0.019(3) C17 0.076(4) 0.144(6) 0.061(3) -0.006(4) 0.019(3) 0.024(4) N3 0.115(4) 0.097(4) 0.093(4) 0.014(3) 0.015(3) -0.056(3) C22 0.063(3) 0.066(3) 0.069(3) -0.008(2) 0.004(2) 0.013(2) C2 0.089(4) 0.091(4) 0.064(3) 0.017(3) 0.001(3) -0.038(3) C23 0.075(4) 0.095(4) 0.088(4) -0.011(3) -0.005(3) 0.018(3) C4 0.157(8) 0.177(9) 0.117(7) 0.021(6) -0.033(6) -0.117(7) C5 0.135(6) 0.143(7) 0.080(5) 0.029(4) -0.040(4) -0.080(6) C14 0.089(5) 0.108(6) 0.197(11) -0.024(7) -0.002(6) 0.029(5) C15 0.151(9) 0.128(8) 0.195(12) -0.011(8) 0.018(8) 0.054(7) C11 0.198(11) 0.144(8) 0.133(8) 0.000(7) 0.063(8) -0.045(8) _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 Re1 O2 2.081(3) . ? Re1 O1 2.086(3) . ? Re1 Br2 2.4471(6) . ? Re1 Br3 2.4516(5) . ? Re1 Br4 2.4852(5) . ? Re1 Br1 2.4866(6) . ? Mn1 N1 2.165(4) . ? Mn1 N1 2.165(4) 2_655 ? Mn1 O4 2.241(3) 2_655 ? Mn1 O4 2.241(3) . ? Mn1 O3 2.255(3) 2_655 ? Mn1 O3 2.255(3) . ? O3 C6 1.230(5) . ? O1 C6 1.274(5) . ? O4 C7 1.220(5) . ? O2 C7 1.278(5) . ? N2 C20 1.511(5) . ? N2 C8 1.518(6) . ? N2 C16 1.522(6) . ? N2 C12 1.529(6) . ? N1 C2 1.293(6) . ? N1 C5 1.337(7) . ? C7 C6 1.544(5) . ? C20 C21 1.509(7) . ? C21 C22 1.513(7) . ? C16 C17 1.505(7) . ? C12 C13 1.518(8) . ? C8 C9 1.475(8) . ? C9 C10 1.582(9) . ? C10 C11 1.354(10) . ? C13 C14 1.584(11) . ? C17 C18 1.546(11) . ? N3 C2 1.308(7) . ? N3 C4 1.325(9) . ? C22 C23 1.517(7) . ? C4 C5 1.345(10) . ? C14 C15 1.349(12) . ? C18 C19 1.617(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 O2 Re1 O1 78.72(11) . . ? O2 Re1 Br2 94.25(8) . . ? O1 Re1 Br2 172.65(8) . . ? O2 Re1 Br3 169.51(8) . . ? O1 Re1 Br3 90.86(8) . . ? Br2 Re1 Br3 96.21(2) . . ? O2 Re1 Br4 86.63(9) . . ? O1 Re1 Br4 89.01(9) . . ? Br2 Re1 Br4 92.72(2) . . ? Br3 Re1 Br4 92.10(2) . . ? O2 Re1 Br1 88.28(10) . . ? O1 Re1 Br1 86.01(9) . . ? Br2 Re1 Br1 91.70(2) . . ? Br3 Re1 Br1 92.18(2) . . ? Br4 Re1 Br1 173.49(2) . . ? N1 Mn1 N1 93.0(2) . 2_655 ? N1 Mn1 O4 90.00(13) . 2_655 ? N1 Mn1 O4 102.94(13) 2_655 2_655 ? N1 Mn1 O4 102.94(13) . . ? N1 Mn1 O4 90.00(13) 2_655 . ? O4 Mn1 O4 161.27(16) 2_655 . ? N1 Mn1 O3 164.61(13) . 2_655 ? N1 Mn1 O3 91.39(15) 2_655 2_655 ? O4 Mn1 O3 74.63(10) 2_655 2_655 ? O4 Mn1 O3 91.80(11) . 2_655 ? N1 Mn1 O3 91.39(14) . . ? N1 Mn1 O3 164.61(13) 2_655 . ? O4 Mn1 O3 91.80(11) 2_655 . ? O4 Mn1 O3 74.63(10) . . ? O3 Mn1 O3 88.27(18) 2_655 . ? C6 O3 Mn1 113.4(3) . . ? C6 O1 Re1 114.9(3) . . ? C7 O4 Mn1 114.1(3) . . ? C7 O2 Re1 115.3(2) . . ? C20 N2 C8 111.8(4) . . ? C20 N2 C16 109.0(4) . . ? C8 N2 C16 108.1(3) . . ? C20 N2 C12 108.3(3) . . ? C8 N2 C12 108.4(4) . . ? C16 N2 C12 111.2(4) . . ? C2 N1 C5 104.4(5) . . ? C2 N1 Mn1 122.5(4) . . ? C5 N1 Mn1 132.9(4) . . ? O4 C7 O2 126.1(4) . . ? O4 C7 C6 118.8(4) . . ? O2 C7 C6 115.1(3) . . ? O3 C6 O1 125.6(4) . . ? O3 C6 C7 118.6(4) . . ? O1 C6 C7 115.7(4) . . ? C21 C20 N2 116.3(4) . . ? C20 C21 C22 110.2(4) . . ? C17 C16 N2 115.3(4) . . ? C13 C12 N2 115.3(4) . . ? C9 C8 N2 116.9(4) . . ? C8 C9 C10 107.2(6) . . ? C11 C10 C9 113.3(8) . . ? C12 C13 C14 112.1(6) . . ? C16 C17 C18 109.7(6) . . ? C2 N3 C4 106.7(5) . . ? C21 C22 C23 111.7(4) . . ? N1 C2 N3 112.8(5) . . ? N3 C4 C5 106.3(6) . . ? N1 C5 C4 109.7(6) . . ? C15 C14 C13 110.7(10) . . ? C17 C18 C19 105.4(8) . . ? 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 N3 H3A O1 0.86 2.08 2.937(6) 177.0 4_655 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.87 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.288 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.111