Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Juan Faus' _publ_contact_author_address ;C\'atedra de Qu\'imica Inorg\'anica Facultad de Qu\'imica de la Universidad de la Rep\'ublica Avda. General Flores 2124 CC 1157 Montevideo Uruguay ; _publ_contact_author_email JUAN.FAUS@UV.ES loop_ _publ_author_name _publ_author_address C.Kremer ;C\'atedra de Qu\'imica Inorg\'anica Facultad de Qu\'imica de la Universidad de la Rep\'ublica Avda. General Flores 2124 CC 1157 Montevideo Uruguay ; A.Cuevas ;C\'atedra de Qu\'imica Inorg\'anica Facultad de Qu\'imica de la Universidad de la Rep\'ublica Avda. General Flores 2124 CC 1157 Montevideo Uruguay ; M.Hummert ;Institut f\"ur Chemie Technische Universitaet Berlin Strasse des 17. Juni 135 D-10623 Berlin Germany, ; H.Schumann ;Institut f\"ur Chemie Technische Universitaet Berlin Strasse des 17. Juni 135 D-10623 Berlin Germany, ; F.Lloret ;Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia Molecular Facultad de Qu\'imica de la Universidad de Valencia Dr. Moliner 50 46100 Burjassot Valencia Spain ; M.Julve ;Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia Molecular Facultad de Qu\'imica de la Universidad de Valencia Dr. Moliner 50 46100 Burjassot Valencia Spain ; J.Faus ;Departamento de Qu\'imica Inorg\'anica Instituto de Ciencia Molecular Facultad de Qu\'imica de la Universidad de Valencia Dr. Moliner 50 46100 Burjassot Valencia Spain ; _publ_section_title ; Magnetic Properties and Molecular Structures of Binuclear (2-pyrazinecarboxylato)-Bridged Complexes Containing Re(IV) and M(II) Metal Ions (M= Co, Ni). ; data_xmh179_comp1 _database_code_depnum_ccdc_archive 'CCDC 618027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 Br5 N3 O3 Re' _chemical_formula_weight 1012.40 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5320(5) _cell_length_b 11.9704(4) _cell_length_c 20.2072(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.215(1) _cell_angle_gamma 90.00 _cell_volume 3657.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3400 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 30.57 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 8.811 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.206302 _exptl_absorpt_correction_T_max 0.474406 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17415 _diffrn_reflns_av_R_equivalents 0.1638 _diffrn_reflns_av_sigmaI/netI 0.2145 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6402 _reflns_number_gt 2433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0239P)^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 SHELXL _refine_ls_extinction_coef 0.00036(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6402 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2295 _refine_ls_R_factor_gt 0.0775 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _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 C1 C 0.2584(12) 0.3581(15) 0.5792(10) 0.046(6) Uani 1 1 d . . . H1 H 0.2564 0.4232 0.5538 0.055 Uiso 1 1 calc R . . C2 C 0.2487(14) 0.3666(18) 0.6451(12) 0.058(6) Uani 1 1 d . . . C3 C 0.2669(14) 0.1846(19) 0.6545(13) 0.070(8) Uani 1 1 d . . . H3 H 0.2668 0.1191 0.6794 0.083 Uiso 1 1 calc R . . C4 C 0.2740(14) 0.1737(17) 0.5908(13) 0.068(7) Uani 1 1 d . . . H4 H 0.2815 0.1028 0.5742 0.082 Uiso 1 1 calc R . . C5 C 0.2313(13) 0.4784(18) 0.6744(12) 0.058(6) Uani 1 1 d . . . C6 C 0.1500(12) 0.2136(14) 0.0472(8) 0.052(6) Uani 1 1 d . . . H6A H 0.1815 0.1465 0.0398 0.063 Uiso 1 1 calc R . . H6B H 0.0879 0.1943 0.0405 0.063 Uiso 1 1 calc R . . C7 C 0.1593(13) 0.2983(16) -0.0055(10) 0.068(7) Uani 1 1 d . . . H7A H 0.2213 0.3163 -0.0006 0.082 Uiso 1 1 calc R . . H7B H 0.1286 0.3663 0.0015 0.082 Uiso 1 1 calc R . . C8 C 0.1212(13) 0.254(2) -0.0779(10) 0.086(7) Uani 1 1 d . . . H8A H 0.1566 0.1914 -0.0861 0.103 Uiso 1 1 calc R . . H8B H 0.0617 0.2273 -0.0803 0.103 Uiso 1 1 calc R . . C9 C 0.1180(16) 0.339(2) -0.1334(12) 0.118(11) Uani 1 1 d . . . H9A H 0.0792 0.3991 -0.1280 0.177 Uiso 1 1 calc R . . H9B H 0.0965 0.3041 -0.1768 0.177 Uiso 1 1 calc R . . H9C H 0.1764 0.3680 -0.1309 0.177 Uiso 1 1 calc R . . C10 C 0.2804(10) 0.2885(14) 0.1354(10) 0.054(6) Uani 1 1 d . . . H10A H 0.2836 0.3577 0.1110 0.065 Uiso 1 1 calc R . . H10B H 0.2988 0.3050 0.1836 0.065 Uiso 1 1 calc R . . C11 C 0.3452(12) 0.2079(15) 0.1175(11) 0.072(7) Uani 1 1 d . . . H11A H 0.3401 0.1367 0.1392 0.087 Uiso 1 1 calc R . . H11B H 0.3309 0.1960 0.0688 0.087 Uiso 1 1 calc R . . C12 C 0.4372(12) 0.249(2) 0.1391(13) 0.123(10) Uani 1 1 d . . . H12A H 0.4422 0.3166 0.1142 0.147 Uiso 1 1 calc R . . H12B H 0.4482 0.2681 0.1869 0.147 Uiso 1 1 calc R . . C13 C 0.5057(15) 0.173(2) 0.1300(16) 0.165(15) Uani 1 1 d . . . H13A H 0.5004 0.1040 0.1527 0.248 Uiso 1 1 calc R . . H13B H 0.5625 0.2059 0.1489 0.248 Uiso 1 1 calc R . . H13C H 0.5000 0.1595 0.0824 0.248 Uiso 1 1 calc R . . C14 C 0.1753(14) 0.1507(15) 0.1659(10) 0.062(6) Uani 1 1 d . . . H14A H 0.2053 0.0871 0.1516 0.074 Uiso 1 1 calc R . . H14B H 0.2058 0.1688 0.2121 0.074 Uiso 1 1 calc R . . C15 C 0.0811(14) 0.1167(16) 0.1659(9) 0.064(7) Uani 1 1 d . . . H15A H 0.0504 0.1798 0.1801 0.076 Uiso 1 1 calc R . . H15B H 0.0504 0.0965 0.1201 0.076 Uiso 1 1 calc R . . C16 C 0.0788(17) 0.0196(17) 0.2128(11) 0.092(10) Uani 1 1 d . . . H16A H 0.1083 0.0400 0.2589 0.110 Uiso 1 1 calc R . . H16B H 0.1100 -0.0434 0.1991 0.110 Uiso 1 1 calc R . . C17 C -0.0205(17) -0.015(2) 0.2106(13) 0.132(12) Uani 1 1 d . . . H17A H -0.0483 0.0423 0.2315 0.198 Uiso 1 1 calc R . . H17B H -0.0211 -0.0840 0.2348 0.198 Uiso 1 1 calc R . . H17C H -0.0520 -0.0246 0.1642 0.198 Uiso 1 1 calc R . . C18 C 0.1267(12) 0.3482(14) 0.1338(10) 0.059(6) Uani 1 1 d . . . H18A H 0.1351 0.4103 0.1051 0.071 Uiso 1 1 calc R . . H18B H 0.0651 0.3261 0.1204 0.071 Uiso 1 1 calc R . . C19 C 0.1455(14) 0.3883(17) 0.2067(10) 0.077(8) Uani 1 1 d . . . H19A H 0.2020 0.4267 0.2175 0.093 Uiso 1 1 calc R . . H19B H 0.1494 0.3246 0.2368 0.093 Uiso 1 1 calc R . . C20 C 0.0728(15) 0.4676(18) 0.2184(12) 0.081(9) Uani 1 1 d . . . H20A H 0.0951 0.5098 0.2597 0.097 Uiso 1 1 calc R . . H20B H 0.0587 0.5202 0.1810 0.097 Uiso 1 1 calc R . . C21 C -0.0059(17) 0.411(2) 0.2239(13) 0.116(10) Uani 1 1 d . . . H21A H 0.0092 0.3419 0.2477 0.175 Uiso 1 1 calc R . . H21B H -0.0414 0.3964 0.1793 0.175 Uiso 1 1 calc R . . H21C H -0.0385 0.4572 0.2484 0.175 Uiso 1 1 calc R . . N1 N 0.2707(9) 0.2607(14) 0.5499(7) 0.053(4) Uani 1 1 d . . . N2 N 0.2598(12) 0.2805(16) 0.6865(8) 0.067(6) Uani 1 1 d . . . N3 N 0.1837(8) 0.2504(13) 0.1201(6) 0.043(3) Uani 1 1 d . . . Br1 Br 0.33003(15) 0.2299(2) 0.33639(10) 0.0779(8) Uani 1 1 d . . . Br2 Br 0.41740(14) 0.11268(16) 0.49713(11) 0.0556(7) Uani 1 1 d . . . Br3 Br 0.40294(15) 0.40337(16) 0.48236(11) 0.0564(7) Uani 1 1 d . . . Br4 Br 0.17570(16) 0.38253(18) 0.40900(12) 0.0718(8) Uani 1 1 d . . . Br5 Br 0.18774(16) 0.09023(18) 0.42736(14) 0.0805(9) Uani 1 1 d . . . Re Re 0.29691(5) 0.24624(8) 0.44901(4) 0.0434(3) Uani 1 1 d . . . O1 O 0.2177(10) 0.5541(12) 0.6294(7) 0.090(6) Uani 1 1 d . . . H1A H 0.2084 0.6136 0.6466 0.135 Uiso 1 1 calc R . . O2 O 0.2360(12) 0.4872(12) 0.7324(8) 0.098(6) Uani 1 1 d . . . O3 O 0.1761(10) 0.7522(14) 0.6660(7) 0.088(5) Uani 1 1 d . . . H3A H 0.1903 0.7673 0.7066 0.132 Uiso 1 1 calc R . . C22 C 0.0964(19) 0.919(2) 0.6184(17) 0.184(18) Uani 1 1 d . . . H22A H 0.1086 0.9641 0.6589 0.277 Uiso 1 1 calc R . . H22B H 0.0409 0.9418 0.5897 0.277 Uiso 1 1 calc R . . H22C H 0.1426 0.9297 0.5945 0.277 Uiso 1 1 calc R . . C23 C 0.092(2) 0.803(2) 0.6365(12) 0.109(10) Uani 1 1 d . . . H23 H 0.0510 0.7925 0.6664 0.131 Uiso 1 1 calc R . . C24 C 0.060(2) 0.742(3) 0.5720(18) 0.23(2) Uani 1 1 d . . . H24A H 0.1057 0.7391 0.5475 0.348 Uiso 1 1 calc R . . H24B H 0.0095 0.7810 0.5451 0.348 Uiso 1 1 calc R . . H24C H 0.0427 0.6680 0.5813 0.348 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 C1 0.042(13) 0.025(11) 0.065(15) -0.008(10) 0.000(11) 0.004(9) C2 0.058(15) 0.060(15) 0.067(16) -0.037(13) 0.035(13) -0.002(12) C3 0.072(18) 0.055(17) 0.08(2) 0.033(15) 0.024(16) -0.020(14) C4 0.073(18) 0.042(14) 0.09(2) 0.024(14) 0.022(16) 0.008(12) C5 0.043(13) 0.066(16) 0.061(15) -0.027(14) 0.003(12) 0.010(11) C6 0.050(12) 0.059(14) 0.044(12) -0.015(10) 0.003(10) -0.011(10) C7 0.072(16) 0.065(14) 0.062(15) -0.007(12) 0.005(13) -0.004(12) C8 0.073(15) 0.099(18) 0.092(17) -0.02(2) 0.034(13) -0.008(18) C9 0.14(2) 0.11(2) 0.09(2) 0.052(18) -0.001(19) 0.014(19) C10 0.025(10) 0.049(13) 0.086(16) -0.002(10) 0.005(11) -0.006(9) C11 0.057(14) 0.055(14) 0.086(17) 0.005(11) -0.023(13) 0.014(11) C12 0.043(13) 0.13(2) 0.17(3) 0.01(2) -0.019(15) 0.02(2) C13 0.06(2) 0.20(4) 0.22(4) -0.03(3) 0.01(2) 0.05(2) C14 0.092(18) 0.040(12) 0.056(14) 0.003(11) 0.023(13) -0.004(12) C15 0.082(18) 0.055(14) 0.049(13) 0.006(11) 0.005(13) -0.010(12) C16 0.15(3) 0.063(17) 0.057(17) 0.003(13) 0.013(18) -0.020(17) C17 0.12(3) 0.15(3) 0.13(3) 0.06(2) 0.06(2) -0.01(2) C18 0.064(15) 0.030(11) 0.075(16) 0.005(10) -0.003(13) 0.005(11) C19 0.081(17) 0.064(16) 0.070(16) -0.039(13) -0.016(14) 0.007(13) C20 0.09(2) 0.057(16) 0.09(2) 0.004(14) 0.008(17) -0.001(15) C21 0.12(3) 0.08(2) 0.15(3) -0.002(18) 0.04(2) -0.012(18) N1 0.070(10) 0.031(9) 0.045(9) -0.002(9) -0.009(7) -0.022(10) N2 0.091(15) 0.062(14) 0.050(11) -0.004(10) 0.021(10) 0.011(11) N3 0.047(8) 0.035(7) 0.039(8) 0.008(9) -0.009(7) 0.004(10) Br1 0.0917(17) 0.094(2) 0.0421(12) -0.0061(13) 0.0036(11) 0.0250(16) Br2 0.0496(14) 0.0443(13) 0.0637(15) 0.0005(11) -0.0060(12) 0.0105(10) Br3 0.0609(16) 0.0409(13) 0.0632(15) 0.0013(10) 0.0051(12) -0.0073(10) Br4 0.0648(17) 0.0639(16) 0.0753(17) 0.0073(13) -0.0076(14) 0.0230(13) Br5 0.0609(16) 0.0482(14) 0.118(2) -0.0189(14) -0.0090(16) -0.0072(12) Re 0.0463(4) 0.0338(4) 0.0431(4) -0.0026(4) -0.0040(3) 0.0059(4) O1 0.145(16) 0.049(10) 0.076(11) -0.003(9) 0.023(11) 0.019(10) O2 0.152(17) 0.069(11) 0.075(13) -0.042(10) 0.031(12) 0.002(10) O3 0.122(13) 0.068(10) 0.065(9) -0.025(11) 0.002(9) 0.031(12) C22 0.15(3) 0.08(2) 0.30(5) 0.01(3) -0.02(3) 0.00(2) C23 0.18(3) 0.09(2) 0.055(17) -0.010(15) 0.021(19) 0.01(2) C24 0.16(3) 0.28(5) 0.23(4) -0.13(4) 0.00(3) 0.04(3) _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 C1 N1 1.34(2) . ? C1 C2 1.38(3) . ? C2 N2 1.31(2) . ? C2 C5 1.51(3) . ? C3 C4 1.32(3) . ? C3 N2 1.33(3) . ? C4 N1 1.32(2) . ? C5 O2 1.16(2) . ? C5 O1 1.27(2) . ? C6 C7 1.50(2) . ? C6 N3 1.512(18) . ? C7 C8 1.54(2) . ? C8 C9 1.51(3) . ? C10 C11 1.50(2) . ? C10 N3 1.531(18) . ? C11 C12 1.48(2) . ? C12 C13 1.44(3) . ? C14 C15 1.52(2) . ? C14 N3 1.53(2) . ? C15 C16 1.51(2) . ? C16 C17 1.59(3) . ? C18 C19 1.51(2) . ? C18 N3 1.53(2) . ? C19 C20 1.53(3) . ? C20 C21 1.42(3) . ? N1 Re 2.175(14) . ? Br1 Re 2.453(2) . ? Br2 Re 2.484(2) . ? Br3 Re 2.489(2) . ? Br4 Re 2.483(2) . ? Br5 Re 2.493(2) . ? O3 C23 1.44(3) . ? C22 C23 1.45(3) . ? C23 C24 1.47(3) . ? 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 N1 C1 C2 123.4(19) . . ? N2 C2 C1 121.9(19) . . ? N2 C2 C5 117(2) . . ? C1 C2 C5 121(2) . . ? C4 C3 N2 126(2) . . ? N1 C4 C3 122(2) . . ? O2 C5 O1 128(2) . . ? O2 C5 C2 120(2) . . ? O1 C5 C2 112(2) . . ? C7 C6 N3 115.3(14) . . ? C6 C7 C8 111.4(16) . . ? C9 C8 C7 115(2) . . ? C11 C10 N3 116.2(14) . . ? C12 C11 C10 112.0(17) . . ? C13 C12 C11 117(2) . . ? C15 C14 N3 115.0(15) . . ? C16 C15 C14 111.6(18) . . ? C15 C16 C17 110.4(19) . . ? C19 C18 N3 115.4(14) . . ? C18 C19 C20 111.2(17) . . ? C21 C20 C19 113(2) . . ? C4 N1 C1 113.3(17) . . ? C4 N1 Re 122.3(16) . . ? C1 N1 Re 124.1(14) . . ? C2 N2 C3 112.4(18) . . ? C6 N3 C18 108.2(12) . . ? C6 N3 C10 112.9(13) . . ? C18 N3 C10 108.5(14) . . ? C6 N3 C14 107.6(14) . . ? C18 N3 C14 110.7(14) . . ? C10 N3 C14 108.9(12) . . ? N1 Re Br1 178.7(4) . . ? N1 Re Br4 87.8(4) . . ? Br1 Re Br4 93.12(9) . . ? N1 Re Br2 88.3(4) . . ? Br1 Re Br2 90.74(8) . . ? Br4 Re Br2 176.08(10) . . ? N1 Re Br3 86.6(4) . . ? Br1 Re Br3 92.60(9) . . ? Br4 Re Br3 89.84(8) . . ? Br2 Re Br3 89.30(7) . . ? N1 Re Br5 87.6(4) . . ? Br1 Re Br5 93.21(10) . . ? Br4 Re Br5 90.02(8) . . ? Br2 Re Br5 90.45(8) . . ? Br3 Re Br5 174.19(11) . . ? O3 C23 C22 115(3) . . ? O3 C23 C24 105(2) . . ? C22 C23 C24 106(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.929 _refine_diff_density_min -1.162 _refine_diff_density_rms 0.190 #===END data_xmh55_comp3 _database_code_depnum_ccdc_archive 'CCDC 618028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H33 Br5 N8 Ni O2 Re' _chemical_formula_weight 1266.17 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' Ni Ni 0.3393 1.1124 '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' Re Re -1.0185 7.2310 '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 23.399(5) _cell_length_b 17.198(5) _cell_length_c 20.778(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.377(5) _cell_angle_gamma 90.00 _cell_volume 8167(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5871 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 30.59 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.060 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4840 _exptl_absorpt_coefficient_mu 8.359 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2607 _exptl_absorpt_correction_T_max 0.6339 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24636 _diffrn_reflns_av_R_equivalents 0.1243 _diffrn_reflns_av_sigmaI/netI 0.1294 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7196 _reflns_number_gt 4074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0342P)^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 7196 _refine_ls_number_parameters 492 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1346 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.007 _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 C1 C 0.6476(5) 0.6335(7) 0.1374(5) 0.034(3) Uani 1 1 d . . . H1 H 0.6403 0.6667 0.1713 0.041 Uiso 1 1 calc R . . C2 C 0.6966(4) 0.5861(7) 0.1506(5) 0.033(3) Uani 1 1 d . . . C3 C 0.6727(5) 0.5413(7) 0.0462(5) 0.046(4) Uani 1 1 d . . . H3 H 0.6796 0.5077 0.0124 0.055 Uiso 1 1 calc R . . C4 C 0.6229(5) 0.5861(7) 0.0337(6) 0.042(3) Uani 1 1 d . . . H4 H 0.5968 0.5827 -0.0081 0.051 Uiso 1 1 calc R . . C5 C 0.7358(5) 0.5831(8) 0.2179(5) 0.037(3) Uani 1 1 d . . . C6 C 0.9053(5) 0.4096(8) 0.2284(5) 0.039(3) Uani 1 1 d . . . C7 C 0.9471(5) 0.4066(8) 0.2899(6) 0.044(3) Uani 1 1 d . . . H7 H 0.9633 0.3584 0.3073 0.053 Uiso 1 1 calc R . . C8 C 0.9630(5) 0.4729(9) 0.3224(6) 0.050(4) Uani 1 1 d . . . H8 H 0.9889 0.4712 0.3644 0.061 Uiso 1 1 calc R . . C9 C 0.9419(5) 0.5457(8) 0.2953(5) 0.039(3) Uani 1 1 d . . . C10 C 0.9599(5) 0.6188(10) 0.3253(6) 0.061(4) Uani 1 1 d . . . H10 H 0.9870 0.6200 0.3665 0.073 Uiso 1 1 calc R . . C11 C 0.9394(6) 0.6856(9) 0.2964(7) 0.060(4) Uani 1 1 d . . . H11 H 0.9525 0.7336 0.3170 0.072 Uiso 1 1 calc R . . C12 C 0.8980(6) 0.6855(8) 0.2348(6) 0.046(3) Uani 1 1 d . . . C13 C 0.8759(7) 0.7529(9) 0.2011(8) 0.064(4) Uani 1 1 d . . . H13 H 0.8878 0.8024 0.2197 0.076 Uiso 1 1 calc R . . C14 C 0.8383(7) 0.7485(8) 0.1430(8) 0.064(4) Uani 1 1 d . . . H14 H 0.8232 0.7944 0.1199 0.077 Uiso 1 1 calc R . . C15 C 0.8217(6) 0.6766(8) 0.1173(7) 0.051(4) Uani 1 1 d . . . C16 C 0.8793(5) 0.6145(7) 0.2067(6) 0.036(3) Uani 1 1 d . . . C17 C 0.9015(5) 0.5434(7) 0.2365(5) 0.034(3) Uani 1 1 d . . . C18 C 0.8884(5) 0.3357(7) 0.1924(6) 0.045(3) Uani 1 1 d . . . H18A H 0.8632 0.3470 0.1493 0.067 Uiso 1 1 calc R . . H18B H 0.8672 0.3028 0.2178 0.067 Uiso 1 1 calc R . . H18C H 0.9236 0.3085 0.1862 0.067 Uiso 1 1 calc R . . C19 C 0.7827(6) 0.6690(8) 0.0473(6) 0.068(5) Uani 1 1 d . . . H19A H 0.7995 0.7000 0.0163 0.102 Uiso 1 1 calc R . . H19B H 0.7433 0.6880 0.0475 0.102 Uiso 1 1 calc R . . H19C H 0.7807 0.6144 0.0337 0.102 Uiso 1 1 calc R . . C20 C 0.8496(4) 0.4848(7) 0.0111(5) 0.032(3) Uani 1 1 d . . . C21 C 0.8392(5) 0.4683(7) -0.0560(5) 0.044(3) Uani 1 1 d . . . H21 H 0.8630 0.4907 -0.0829 0.052 Uiso 1 1 calc R . . C22 C 0.7938(6) 0.4190(8) -0.0832(6) 0.051(4) Uani 1 1 d . . . H22 H 0.7869 0.4068 -0.1288 0.061 Uiso 1 1 calc R . . C23 C 0.7577(5) 0.3866(7) -0.0444(5) 0.038(3) Uani 1 1 d . . . C24 C 0.7099(6) 0.3347(8) -0.0684(6) 0.053(4) Uani 1 1 d . . . H24 H 0.6997 0.3233 -0.1142 0.064 Uiso 1 1 calc R . . C25 C 0.6800(6) 0.3026(8) -0.0286(6) 0.054(4) Uani 1 1 d . . . H25 H 0.6481 0.2692 -0.0462 0.065 Uiso 1 1 calc R . . C26 C 0.6944(5) 0.3172(8) 0.0408(6) 0.043(3) Uani 1 1 d . . . C27 C 0.6680(5) 0.2795(8) 0.0864(7) 0.057(4) Uani 1 1 d . . . H27 H 0.6369 0.2438 0.0721 0.069 Uiso 1 1 calc R . . C28 C 0.6876(5) 0.2948(8) 0.1515(7) 0.055(4) Uani 1 1 d . . . H28 H 0.6706 0.2682 0.1829 0.066 Uiso 1 1 calc R . . C29 C 0.7322(5) 0.3489(7) 0.1734(5) 0.037(3) Uani 1 1 d . . . C30 C 0.7394(5) 0.3710(7) 0.0661(5) 0.035(3) Uani 1 1 d . . . C31 C 0.7707(5) 0.4073(7) 0.0228(5) 0.034(3) Uani 1 1 d . . . C32 C 0.8995(5) 0.5338(7) 0.0410(5) 0.040(3) Uani 1 1 d . . . H32A H 0.8911 0.5880 0.0279 0.060 Uiso 1 1 calc R . . H32B H 0.9344 0.5165 0.0261 0.060 Uiso 1 1 calc R . . H32C H 0.9065 0.5296 0.0891 0.060 Uiso 1 1 calc R . . C33 C 0.7527(6) 0.3614(8) 0.2459(6) 0.061(4) Uani 1 1 d . . . H33A H 0.7908 0.3876 0.2545 0.091 Uiso 1 1 calc R . . H33B H 0.7565 0.3111 0.2686 0.091 Uiso 1 1 calc R . . H33C H 0.7243 0.3938 0.2622 0.091 Uiso 1 1 calc R . . C34 C 0.6051(7) 0.4328(10) 0.8157(7) 0.096(6) Uani 1 1 d D . . H34A H 0.5888 0.3989 0.8452 0.143 Uiso 1 1 calc R . . H34B H 0.6332 0.4033 0.7964 0.143 Uiso 1 1 calc R . . H34C H 0.5735 0.4520 0.7805 0.143 Uiso 1 1 calc R . . C35 C 0.6340(8) 0.4967(10) 0.8521(9) 0.085(6) Uani 1 1 d D . . N7 N 0.6541(8) 0.5475(9) 0.8815(8) 0.116(6) Uani 1 1 d D . . N1 N 0.6105(4) 0.6344(6) 0.0792(4) 0.033(2) Uani 1 1 d . . . N2 N 0.7118(4) 0.5425(6) 0.1034(4) 0.036(2) Uani 1 1 d . . . N3 N 0.8813(3) 0.4749(5) 0.2037(4) 0.028(2) Uani 1 1 d . . . N4 N 0.8383(4) 0.6090(6) 0.1459(4) 0.035(2) Uani 1 1 d . . . N5 N 0.8146(4) 0.4579(5) 0.0487(4) 0.028(2) Uani 1 1 d . . . N6 N 0.7554(4) 0.3900(6) 0.1319(4) 0.038(3) Uani 1 1 d . . . O1 O 0.7241(3) 0.6280(6) 0.2606(4) 0.058(3) Uani 1 1 d . . . O2 O 0.7762(3) 0.5338(5) 0.2256(3) 0.034(2) Uani 1 1 d . . . Ni1 Ni 0.80053(6) 0.49612(9) 0.14127(6) 0.0275(4) Uani 1 1 d . . . Br1 Br 0.46564(6) 0.82452(8) 0.03711(7) 0.0515(4) Uani 1 1 d . . . Br2 Br 0.55862(6) 0.73583(9) -0.05464(6) 0.0552(4) Uani 1 1 d . . . Br3 Br 0.62057(5) 0.81493(8) 0.09952(6) 0.0473(4) Uani 1 1 d . . . Br4 Br 0.52323(6) 0.69589(8) 0.17102(6) 0.0435(3) Uani 1 1 d . . . Br5 Br 0.46884(6) 0.61456(8) 0.01723(7) 0.0578(4) Uani 1 1 d . . . Re Re 0.53998(2) 0.72045(3) 0.05791(2) 0.03181(15) Uani 1 1 d . . . C36A C 0.5075(11) 0.547(2) 0.6436(18) 0.131(7) Uani 0.671(16) 1 d PD A 1 H36A H 0.4898 0.5302 0.6799 0.197 Uiso 0.671(16) 1 calc PR A 1 H36B H 0.5005 0.5076 0.6087 0.197 Uiso 0.671(16) 1 calc PR A 1 H36C H 0.4900 0.5964 0.6259 0.197 Uiso 0.671(16) 1 calc PR A 1 C37A C 0.5682(12) 0.557(3) 0.667(3) 0.131(7) Uani 0.671(16) 1 d PD A 1 N8A N 0.6159(10) 0.5545(16) 0.6892(14) 0.131(7) Uani 0.671(16) 1 d PD A 1 C36B C 0.563(3) 0.542(6) 0.653(5) 0.131(7) Uani 0.329(16) 1 d PD A 2 H36D H 0.5925 0.5173 0.6877 0.197 Uiso 0.329(16) 1 calc PR A 2 H36E H 0.5821 0.5777 0.6278 0.197 Uiso 0.329(16) 1 calc PR A 2 H36F H 0.5422 0.5016 0.6237 0.197 Uiso 0.329(16) 1 calc PR A 2 C37B C 0.523(3) 0.583(5) 0.682(3) 0.131(7) Uani 0.329(16) 1 d PD A 2 N8B N 0.506(2) 0.616(3) 0.721(2) 0.131(7) Uani 0.329(16) 1 d PD . 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 C1 0.038(7) 0.044(8) 0.023(6) -0.004(6) 0.008(5) 0.014(6) C2 0.023(6) 0.048(8) 0.030(6) 0.013(6) 0.009(5) 0.004(6) C3 0.056(9) 0.053(9) 0.025(7) -0.006(7) 0.000(6) 0.025(7) C4 0.032(7) 0.048(9) 0.040(7) -0.003(7) -0.006(6) 0.002(6) C5 0.031(7) 0.059(9) 0.019(6) -0.002(7) 0.004(5) -0.002(7) C6 0.038(7) 0.046(9) 0.035(7) 0.009(7) 0.013(6) -0.001(7) C7 0.045(8) 0.046(9) 0.038(7) 0.024(7) 0.002(6) 0.002(7) C8 0.032(7) 0.092(12) 0.026(7) 0.004(8) 0.002(6) -0.007(8) C9 0.027(7) 0.061(10) 0.026(7) -0.003(7) -0.001(5) -0.003(7) C10 0.040(9) 0.096(14) 0.044(8) -0.018(10) 0.005(7) 0.003(9) C11 0.062(10) 0.061(11) 0.057(10) -0.011(9) 0.013(8) -0.011(9) C12 0.061(9) 0.030(8) 0.054(9) -0.005(8) 0.031(7) 0.001(7) C13 0.078(12) 0.042(10) 0.086(12) -0.016(9) 0.050(10) -0.015(8) C14 0.094(13) 0.029(8) 0.084(12) 0.001(9) 0.053(10) 0.014(8) C15 0.054(9) 0.043(9) 0.068(10) 0.020(9) 0.041(7) 0.013(8) C16 0.036(7) 0.038(8) 0.040(7) -0.001(7) 0.021(6) 0.004(6) C17 0.033(7) 0.031(7) 0.041(7) 0.001(6) 0.010(6) -0.001(6) C18 0.040(8) 0.029(7) 0.059(8) 0.012(7) -0.004(6) 0.012(6) C19 0.080(11) 0.073(11) 0.053(9) 0.044(9) 0.019(8) 0.033(9) C20 0.021(6) 0.039(8) 0.035(7) -0.001(6) 0.003(5) 0.008(6) C21 0.052(8) 0.052(9) 0.029(7) -0.007(7) 0.014(6) -0.005(7) C22 0.062(9) 0.061(10) 0.026(7) -0.011(7) 0.002(7) 0.014(8) C23 0.035(7) 0.043(8) 0.030(7) -0.007(7) -0.005(6) 0.010(6) C24 0.053(9) 0.066(11) 0.030(7) -0.007(8) -0.014(7) 0.029(8) C25 0.057(9) 0.048(10) 0.050(9) -0.020(8) -0.007(7) 0.005(7) C26 0.016(6) 0.059(9) 0.054(8) 0.000(8) 0.005(6) 0.006(6) C27 0.023(7) 0.052(9) 0.097(11) -0.019(10) 0.010(7) -0.003(7) C28 0.048(8) 0.052(10) 0.063(9) -0.004(8) 0.010(7) -0.022(7) C29 0.030(7) 0.051(9) 0.030(7) 0.017(7) 0.005(5) 0.011(6) C30 0.026(7) 0.037(8) 0.039(7) -0.017(6) 0.001(6) 0.006(6) C31 0.032(7) 0.040(8) 0.027(7) 0.008(6) 0.000(5) 0.009(6) C32 0.034(7) 0.049(8) 0.037(7) 0.024(7) 0.007(6) 0.007(6) C33 0.065(10) 0.059(10) 0.061(9) 0.013(8) 0.019(7) -0.008(8) C34 0.107(15) 0.086(15) 0.088(13) -0.017(12) 0.009(11) -0.008(12) C35 0.104(15) 0.053(12) 0.094(15) 0.000(11) 0.013(12) 0.025(11) N7 0.163(17) 0.083(13) 0.104(13) -0.010(11) 0.033(11) 0.020(13) N1 0.032(6) 0.046(7) 0.022(5) -0.002(5) 0.005(4) 0.008(5) N2 0.037(6) 0.039(6) 0.032(6) -0.002(5) 0.010(5) 0.009(5) N3 0.011(4) 0.031(6) 0.039(6) 0.009(5) 0.001(4) 0.004(4) N4 0.034(6) 0.043(7) 0.034(6) 0.009(5) 0.020(5) 0.016(5) N5 0.019(5) 0.035(6) 0.030(5) -0.006(5) 0.003(4) 0.002(4) N6 0.030(6) 0.050(7) 0.032(6) 0.013(6) 0.005(5) -0.003(5) O1 0.044(6) 0.086(8) 0.038(5) -0.010(5) -0.005(4) 0.019(5) O2 0.027(4) 0.047(5) 0.025(4) 0.005(4) -0.003(3) 0.002(4) Ni1 0.0233(7) 0.0333(9) 0.0243(7) 0.0042(7) 0.0018(6) 0.0053(7) Br1 0.0420(8) 0.0401(9) 0.0669(9) -0.0032(7) -0.0005(7) 0.0145(6) Br2 0.0636(9) 0.0674(11) 0.0346(7) 0.0072(7) 0.0104(6) 0.0134(8) Br3 0.0407(8) 0.0481(9) 0.0515(8) 0.0011(7) 0.0064(6) -0.0101(7) Br4 0.0489(8) 0.0418(8) 0.0447(7) -0.0001(7) 0.0210(6) 0.0017(6) Br5 0.0424(8) 0.0491(9) 0.0765(10) -0.0137(8) 0.0004(7) -0.0058(7) Re 0.0259(2) 0.0340(3) 0.0348(3) -0.0004(3) 0.00479(19) 0.0051(2) C36A 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) C37A 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) N8A 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) C36B 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) C37B 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) N8B 0.122(15) 0.111(14) 0.152(18) 0.021(11) 0.013(15) -0.024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.330(12) . ? C1 C2 1.384(14) . ? C2 N2 1.342(13) . ? C2 C5 1.500(14) . ? C3 N2 1.335(12) . ? C3 C4 1.374(15) . ? C4 N1 1.337(14) . ? C5 O1 1.250(13) . ? C5 O2 1.254(13) . ? C6 N3 1.312(14) . ? C6 C7 1.435(14) . ? C6 C18 1.484(15) . ? C7 C8 1.337(17) . ? C8 C9 1.417(17) . ? C9 C17 1.375(14) . ? C9 C10 1.426(18) . ? C10 C11 1.337(18) . ? C11 C12 1.430(17) . ? C12 C16 1.382(16) . ? C12 C13 1.395(18) . ? C13 C14 1.337(18) . ? C14 C15 1.369(18) . ? C15 N4 1.325(14) . ? C15 C19 1.550(16) . ? C16 N4 1.417(13) . ? C16 C17 1.419(15) . ? C17 N3 1.392(13) . ? C20 N5 1.331(13) . ? C20 C21 1.393(14) . ? C20 C32 1.466(14) . ? C21 C22 1.382(16) . ? C22 C23 1.401(16) . ? C23 C31 1.408(14) . ? C23 C24 1.434(17) . ? C24 C25 1.316(18) . ? C25 C26 1.430(16) . ? C26 C27 1.397(17) . ? C26 C30 1.416(15) . ? C27 C28 1.357(17) . ? C28 C29 1.399(16) . ? C29 N6 1.318(13) . ? C29 C33 1.496(15) . ? C30 N6 1.378(13) . ? C30 C31 1.422(15) . ? C31 N5 1.366(13) . ? C34 C35 1.420(19) . ? C35 N7 1.112(18) . ? N1 Re 2.189(9) . ? N2 Ni1 2.206(9) . ? N3 Ni1 2.081(8) . ? N4 Ni1 2.126(10) . ? N5 Ni1 2.124(8) . ? N6 Ni1 2.096(10) . ? O2 Ni1 2.059(7) . ? Br1 Re 2.4685(14) . ? Br2 Re 2.4832(15) . ? Br3 Re 2.4990(14) . ? Br4 Re 2.5002(14) . ? Br5 Re 2.4897(15) . ? C36A C37A 1.41(2) . ? C37A N8A 1.11(2) . ? C36B C37B 1.42(2) . ? C37B N8B 1.12(3) . ? N8B N8B 1.29(10) 2_656 ? 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 N1 C1 C2 122.6(10) . . ? N2 C2 C1 121.5(9) . . ? N2 C2 C5 117.2(10) . . ? C1 C2 C5 121.3(11) . . ? N2 C3 C4 123.5(11) . . ? N1 C4 C3 121.2(10) . . ? O1 C5 O2 127.0(10) . . ? O1 C5 C2 117.2(11) . . ? O2 C5 C2 115.8(10) . . ? N3 C6 C7 122.2(12) . . ? N3 C6 C18 119.4(10) . . ? C7 C6 C18 118.4(11) . . ? C8 C7 C6 118.8(12) . . ? C7 C8 C9 121.2(11) . . ? C17 C9 C8 116.2(12) . . ? C17 C9 C10 119.8(12) . . ? C8 C9 C10 124.1(11) . . ? C11 C10 C9 121.1(12) . . ? C10 C11 C12 120.6(14) . . ? C16 C12 C13 118.2(12) . . ? C16 C12 C11 118.1(13) . . ? C13 C12 C11 123.6(14) . . ? C14 C13 C12 120.5(14) . . ? C13 C14 C15 118.7(14) . . ? N4 C15 C14 126.0(13) . . ? N4 C15 C19 113.8(12) . . ? C14 C15 C19 120.1(13) . . ? C12 C16 N4 121.9(11) . . ? C12 C16 C17 121.6(11) . . ? N4 C16 C17 116.5(11) . . ? C9 C17 N3 123.9(11) . . ? C9 C17 C16 118.7(11) . . ? N3 C17 C16 117.4(10) . . ? N5 C20 C21 121.3(10) . . ? N5 C20 C32 119.0(9) . . ? C21 C20 C32 119.7(11) . . ? C22 C21 C20 119.3(12) . . ? C21 C22 C23 120.9(11) . . ? C22 C23 C31 116.2(11) . . ? C22 C23 C24 124.5(11) . . ? C31 C23 C24 119.3(12) . . ? C25 C24 C23 121.5(12) . . ? C24 C25 C26 121.2(13) . . ? C27 C26 C30 116.9(12) . . ? C27 C26 C25 124.0(13) . . ? C30 C26 C25 119.0(13) . . ? C28 C27 C26 118.9(12) . . ? C27 C28 C29 121.4(13) . . ? N6 C29 C28 121.9(11) . . ? N6 C29 C33 119.5(11) . . ? C28 C29 C33 118.6(12) . . ? N6 C30 C26 123.1(11) . . ? N6 C30 C31 117.2(10) . . ? C26 C30 C31 119.7(10) . . ? N5 C31 C23 122.5(11) . . ? N5 C31 C30 118.4(10) . . ? C23 C31 C30 119.0(11) . . ? N7 C35 C34 177(2) . . ? C1 N1 C4 116.0(9) . . ? C1 N1 Re 120.6(7) . . ? C4 N1 Re 123.0(7) . . ? C3 N2 C2 114.9(9) . . ? C3 N2 Ni1 136.5(8) . . ? C2 N2 Ni1 108.5(6) . . ? C6 N3 C17 117.4(9) . . ? C6 N3 Ni1 130.5(8) . . ? C17 N3 Ni1 109.0(7) . . ? C15 N4 C16 114.7(11) . . ? C15 N4 Ni1 134.6(9) . . ? C16 N4 Ni1 107.3(7) . . ? C20 N5 C31 119.6(9) . . ? C20 N5 Ni1 131.2(7) . . ? C31 N5 Ni1 107.8(7) . . ? C29 N6 C30 117.3(10) . . ? C29 N6 Ni1 132.6(8) . . ? C30 N6 Ni1 108.8(8) . . ? C5 O2 Ni1 116.3(7) . . ? O2 Ni1 N3 84.6(3) . . ? O2 Ni1 N6 97.3(3) . . ? N3 Ni1 N6 106.1(3) . . ? O2 Ni1 N5 173.0(3) . . ? N3 Ni1 N5 102.3(3) . . ? N6 Ni1 N5 79.6(4) . . ? O2 Ni1 N4 82.1(3) . . ? N3 Ni1 N4 79.6(3) . . ? N6 Ni1 N4 174.3(3) . . ? N5 Ni1 N4 100.4(3) . . ? O2 Ni1 N2 77.2(3) . . ? N3 Ni1 N2 160.9(3) . . ? N6 Ni1 N2 82.2(3) . . ? N5 Ni1 N2 96.1(3) . . ? N4 Ni1 N2 92.1(3) . . ? N1 Re Br1 175.9(3) . . ? N1 Re Br2 89.2(2) . . ? Br1 Re Br2 91.00(5) . . ? N1 Re Br5 89.7(2) . . ? Br1 Re Br5 94.37(5) . . ? Br2 Re Br5 89.87(5) . . ? N1 Re Br3 83.6(2) . . ? Br1 Re Br3 92.31(5) . . ? Br2 Re Br3 89.12(5) . . ? Br5 Re Br3 173.26(5) . . ? N1 Re Br4 87.6(2) . . ? Br1 Re Br4 92.32(5) . . ? Br2 Re Br4 176.25(5) . . ? Br5 Re Br4 88.14(5) . . ? Br3 Re Br4 92.48(5) . . ? N8A C37A C36A 170(6) . . ? N8B C37B C36B 158(8) . . ? C37B N8B N8B 148(5) . 2_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.801 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.194 #===END #===END data_comp2 _database_code_depnum_ccdc_archive 'CCDC 618029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H33 Br5 Co N8 O2 Re' _chemical_formula_weight 1266.39 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' Co Co 0.3494 0.9721 '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' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 23.483(3) _cell_length_b 17.0434(16) _cell_length_c 20.700(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.962(16) _cell_angle_gamma 90.00 _cell_volume 8104.6(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5871 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.59 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4832 _exptl_absorpt_coefficient_mu 8.368 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1347 _exptl_absorpt_correction_T_max 0.5541 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26299 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7327 _reflns_number_gt 5938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0269P)^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 7327 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0466 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 C1 C 0.64642(15) 0.6323(2) 0.63778(16) 0.0201(8) Uani 1 1 d . . . H1 H 0.6384 0.6651 0.6719 0.024 Uiso 1 1 calc R . . C2 C 0.69557(14) 0.5860(2) 0.65020(15) 0.0187(8) Uani 1 1 d . . . C3 C 0.67189(16) 0.5382(2) 0.54509(17) 0.0265(9) Uani 1 1 d . . . H3 H 0.6797 0.5048 0.5112 0.032 Uiso 1 1 calc R . . C4 C 0.62175(16) 0.5828(2) 0.53328(16) 0.0244(8) Uani 1 1 d . . . H4 H 0.5953 0.5782 0.492 0.029 Uiso 1 1 calc R . . C5 C 0.7351(15) 0.5840(2) 0.71808(16) 0.0214(8) Uani 1 1 d . . . C6 C 0.90820(14) 0.4094(2) 0.73158(16) 0.0197(8) Uani 1 1 d . . . C7 C 0.94961(15) 0.4085(2) 0.79234(17) 0.0264(9) Uani 1 1 d . . . H7 H 0.9659 0.3602 0.8102 0.032 Uiso 1 1 calc R . . C8 C 0.96587(15) 0.4767(3) 0.82473(17) 0.0283(9) Uani 1 1 d . . . H8 H 0.9922 0.4757 0.8663 0.034 Uiso 1 1 calc R . . C9 C 0.94411(15) 0.5486(2) 0.79743(17) 0.0246(9) Uani 1 1 d . . . C10 C 0.96055(17) 0.6232(3) 0.82652(19) 0.0342(10) Uani 1 1 d . . . H10 H 0.9868 0.6254 0.8681 0.041 Uiso 1 1 calc R . . C11 C 0.94022(18) 0.6899(3) 0.7970(2) 0.0380(11) Uani 1 1 d . . . H11 H 0.9531 0.7387 0.8171 0.046 Uiso 1 1 calc R . . C12 C 0.89884(17) 0.6890(2) 0.73495(19) 0.0280(9) Uani 1 1 d . . . C13 C 0.8752(2) 0.7575(3) 0.7016(2) 0.0388(11) Uani 1 1 d . . . H13 H 0.8859 0.8077 0.7201 0.047 Uiso 1 1 calc R . . C14 C 0.8370(2) 0.7508(3) 0.6427(2) 0.0375(11) Uani 1 1 d . . . H14 H 0.8209 0.7967 0.6199 0.045 Uiso 1 1 calc R . . C15 C 0.82100(17) 0.6765(2) 0.61523(18) 0.0274(9) Uani 1 1 d . . . C16 C 0.88040(15) 0.6170(2) 0.70586(16) 0.0190(8) Uani 1 1 d . . . C17 C 0.90281(14) 0.5451(2) 0.73700(16) 0.0183(8) Uani 1 1 d . . . C18 C 0.89152(17) 0.3343(2) 0.69578(18) 0.0277(9) Uani 1 1 d . . . H18A H 0.8672 0.3455 0.6523 0.033 Uiso 1 1 calc R . . H18B H 0.8697 0.3017 0.7212 0.033 Uiso 1 1 calc R . . H18C H 0.9267 0.3064 0.6903 0.033 Uiso 1 1 calc R . . C19 C 0.78313(19) 0.6701(3) 0.54785(19) 0.0375(11) Uani 1 1 d . . . H19A H 0.7797 0.6149 0.5344 0.045 Uiso 1 1 calc R . . H19B H 0.8004 0.7001 0.5164 0.045 Uiso 1 1 calc R . . H19C H 0.7444 0.6911 0.5486 0.045 Uiso 1 1 calc R . . C20 C 0.85013(15) 0.4846(2) 0.50857(16) 0.0191(8) Uani 1 1 d . . . C21 C 0.83927(17) 0.4681(2) 0.44065(17) 0.0269(9) Uani 1 1 d . . . H21 H 0.8640 0.4896 0.4142 0.032 Uiso 1 1 calc R . . C22 C 0.79369(17) 0.4218(2) 0.41215(17) 0.0288(9) Uani 1 1 d . . . H22 H 0.7856 0.4130 0.3658 0.035 Uiso 1 1 calc R . . C23 C 0.75876(15) 0.3871(2) 0.45184(16) 0.0232(8) Uani 1 1 d . . . C24 C 0.71151(17) 0.3351(2) 0.42705(18) 0.0301(9) Uani 1 1 d . . . H24 H 0.7019 0.3237 0.3811 0.036 Uiso 1 1 calc R . . C25 C 0.68015(17) 0.3018(2) 0.46776(19) 0.0300(9) Uani 1 1 d . . . H25 H 0.6483 0.2686 0.4499 0.036 Uiso 1 1 calc R . . C26 C 0.69442(15) 0.3161(2) 0.53714(18) 0.0243(8) Uani 1 1 d . . . C27 C 0.66661(17) 0.2772(2) 0.5828(2) 0.0329(9) Uani 1 1 d . . . H27 H 0.6347 0.2430 0.5677 0.040 Uiso 1 1 calc R . . C28 C 0.68655(17) 0.2899(2) 0.6484(2) 0.0320(9) Uani 1 1 d . . . H28 H 0.6698 0.2617 0.6795 0.038 Uiso 1 1 calc R . . C29 C 0.73154(16) 0.3440(2) 0.67135(17) 0.0249(8) Uani 1 1 d . . . C30 C 0.73957(14) 0.3680(2) 0.56336(16) 0.0192(8) Uani 1 1 d . . . C31 C 0.77181(15) 0.4054(2) 0.51973(16) 0.0182(7) Uani 1 1 d . . . C32 C 0.90146(15) 0.5341(2) 0.53889(17) 0.0245(8) Uani 1 1 d . . . H32A H 0.9104 0.5264 0.5868 0.029 Uiso 1 1 calc R . . H32B H 0.8924 0.5895 0.5290 0.029 Uiso 1 1 calc R . . H32C H 0.9352 0.5188 0.5207 0.029 Uiso 1 1 calc R . . C33 C 0.75165(17) 0.3568(3) 0.74396(18) 0.0322(10) Uani 1 1 d . . . H33A H 0.7889 0.3848 0.7523 0.039 Uiso 1 1 calc R . . H33B H 0.7566 0.3060 0.7666 0.039 Uiso 1 1 calc R . . H33C H 0.7227 0.3879 0.7605 0.039 Uiso 1 1 calc R . . C34 C 0.9921(3) -0.0524(4) 0.8517(3) 0.094(2) Uani 1 1 d . . . H34A H 1.0045 -0.0898 0.8878 0.141 Uiso 1 1 calc R . . H34B H 1.0045 0.0006 0.8669 0.141 Uiso 1 1 calc R . . H34C H 1.0098 -0.0665 0.8144 0.141 Uiso 1 1 calc R . . C35 C 0.9333(3) -0.0543(4) 0.8324(3) 0.0640(16) Uani 1 1 d . . . C36 C 0.8926(2) -0.0712(3) 1.1861(2) 0.0491(12) Uani 1 1 d . . . H36A H 0.8630 -0.0997 1.2039 0.074 Uiso 1 1 calc R . . H36B H 0.9233 -0.0529 1.2226 0.074 Uiso 1 1 calc R . . H36C H 0.9096 -0.1061 1.1575 0.074 Uiso 1 1 calc R . . C37 C 0.8660(2) -0.0044(3) 1.1482(2) 0.0436(11) Uani 1 1 d . . . Co Co 0.802393(19) 0.49377(3) 0.64164(2) 0.01570(10) Uani 1 1 d . . . Br1 Br 0.465844(16) 0.82597(2) 0.53788(18) 0.02862(9) Uani 1 1 d . . . Br4 Br 0.52251(16) 0.69434(2) 0.671083(17) 0.02397(9) Uani 1 1 d . . . Br3 Br 0.620234(16) 0.81486(2) 0.600099(17) 0.02564(9) Uani 1 1 d . . . Br2 Br 0.559244(18) 0.73619(2) 0.445081(17) 0.03077(10) Uani 1 1 d . . . Br5 Br 0.468192(17) 0.61412(2) 0.51622(2) 0.03316(10) Uani 1 1 d . . . N1 N 0.6094(12) 0.63246(18) 0.57876(13) 0.019(6) Uani 1 1 d . . . N2 N 0.70976(12) 0.54066(18) 0.60287(13) 0.0218(7) Uani 1 1 d . . . N3 N 0.88450(12) 0.47583(17) 0.70638(13) 0.0165(6) Uani 1 1 d . . . N4 N 0.84059(12) 0.61108(17) 0.64734(13) 0.0206(7) Uani 1 1 d . . . N5 N 0.81539(12) 0.45650(17) 0.54698(12) 0.0164(6) Uani 1 1 d . . . N6 N 0.75623(12) 0.38414(18) 0.62939(13) 0.0194(7) Uani 1 1 d . . . N7 N 0.8838(3) -0.0555(4) 0.8124(3) 0.0968(19) Uani 1 1 d . . . N8 N 0.8453(2) 0.0471(3) 1.1175(2) 0.0656(13) Uani 1 1 d . . . Re Re 0.53968(6) 0.720136(9) 0.557847(6) 0.01688(4) Uani 1 1 d . . . O1 O 0.72331(12) 0.62909(17) 0.76053(12) 0.034(7) Uani 1 1 d . . . O2 O 0.77631(10) 0.53503(15) 0.72482(11) 0.0214(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0215(19) 0.022(2) 0.0181(17) -0.0003(14) 0.0062(14) 0.0024(16) C2 0.0169(17) 0.024(2) 0.0156(16) 0.0012(14) 0.0034(13) 0.0029(16) C3 0.033(2) 0.026(2) 0.0195(18) -0.0042(15) 0.0039(16) 0.0119(18) C4 0.024(2) 0.026(2) 0.0204(17) -0.0041(15) -0.0016(15) 0.0074(17) C5 0.0185(18) 0.030(2) 0.0153(17) 0.0031(15) 0.0018(14) -0.0004(17) C6 0.0155(18) 0.023(2) 0.0222(17) 0.0050(15) 0.0075(14) 0.0014(15) C7 0.0159(18) 0.034(2) 0.0288(19) 0.0116(17) 0.0035(15) 0.0054(17) C8 0.0170(19) 0.045(3) 0.0193(18) 0.0014(17) -0.0035(15) -0.0006(18) C9 0.0161(18) 0.036(3) 0.0217(18) -0.0038(16) 0.0050(14) -0.0046(17) C10 0.027(2) 0.042(3) 0.032(2) -0.0113(19) 0.0009(17) -0.008(2) C11 0.033(2) 0.037(3) 0.047(2) -0.019(2) 0.0142(19) -0.015(2) C12 0.029(2) 0.022(2) 0.039(2) -0.0039(17) 0.0202(17) -0.0043(18) C13 0.051(3) 0.017(2) 0.058(3) -0.0051(19) 0.032(2) -0.001(2) C14 0.052(3) 0.018(2) 0.051(3) 0.0105(19) 0.030(2) 0.012(2) C15 0.029(2) 0.023(2) 0.035(2) 0.0108(17) 0.0174(17) 0.0083(18) C16 0.0177(18) 0.018(2) 0.0244(18) -0.0010(14) 0.0117(14) -0.0009(15) C17 0.0133(17) 0.023(2) 0.0192(16) -0.0019(14) 0.0045(13) -0.0009(15) C18 0.027(2) 0.024(2) 0.032(2) 0.0055(17) 0.0033(16) 0.0069(17) C19 0.042(3) 0.036(3) 0.037(2) 0.0197(19) 0.0134(19) 0.016(2) C20 0.0192(18) 0.019(2) 0.0193(17) 0.0044(14) 0.0050(14) 0.0055(16) C21 0.031(2) 0.030(2) 0.0211(18) 0.0039(16) 0.0092(16) 0.0031(18) C22 0.033(2) 0.037(3) 0.0145(17) -0.0015(16) 0.0024(15) 0.0060(19) C23 0.023(2) 0.021(2) 0.0229(18) -0.0037(15) -0.0011(15) 0.0083(16) C24 0.027(2) 0.033(2) 0.0258(19) -0.0107(17) -0.0040(16) 0.0029(19) C25 0.021(2) 0.027(2) 0.037(2) -0.0107(17) -0.0050(17) 0.0032(17) C26 0.0142(18) 0.024(2) 0.034(2) -0.0021(16) 0.0022(15) 0.0030(16) C27 0.022(2) 0.027(2) 0.051(2) -0.006(2) 0.0094(18) -0.0052(18) C28 0.030(2) 0.028(3) 0.041(2) 0.0029(18) 0.0143(18) -0.0066(19) C29 0.022(2) 0.025(2) 0.0278(19) 0.0042(16) 0.0065(15) 0.0015(17) C30 0.0144(17) 0.017(2) 0.0252(18) -0.0002(15) 0.0013(14) 0.0067(15) C31 0.0179(18) 0.0131(19) 0.0216(17) -0.0003(14) -0.0004(14) 0.0057(15) C32 0.023(2) 0.027(2) 0.0241(18) 0.0021(16) 0.0075(15) -0.0020(17) C33 0.030(2) 0.037(3) 0.031(2) 0.0106(18) 0.0094(17) -0.0038(19) C34 0.075(5) 0.102(6) 0.100(5) 0.044(4) 0.006(4) 0.000(4) C35 0.052(3) 0.059(4) 0.075(4) 0.017(3) 0.002(3) -0.011(3) C36 0.046(3) 0.051(3) 0.049(3) 0.000(2) 0.009(2) 0.005(3) C37 0.050(3) 0.040(3) 0.042(3) -0.006(2) 0.013(2) -0.006(2) Co 0.0135(2) 0.0179(3) 0.0147(2) 0.00160(18) 0.00080(17) 0.0027(2) Br1 0.0219(2) 0.0226(2) 0.0381(2) -0.00174(16) -0.00105(16) 0.00914(16) Br4 0.02597(19) 0.0233(2) 0.02542(18) 0.00102(15) 0.01181(15) 0.00142(16) Br3 0.02195(19) 0.0258(2) 0.02844(18) 0.00037(15) 0.00343(15) -0.00561(16) Br2 0.0372(2) 0.0359(3) 0.01928(18) 0.00421(16) 0.00597(15) 0.00756(19) Br5 0.0245(2) 0.0265(2) 0.0454(2) -0.00950(18) 0.00019(17) -0.00400(17) N1 0.0171(15) 0.0208(17) 0.0180(14) 0.0003(12) 0.0010(11) 0.0028(13) N2 0.0228(16) 0.0225(18) 0.0195(14) -0.0008(13) 0.0030(12) 0.0073(14) N3 0.0134(14) 0.0181(17) 0.0176(14) 0.0018(12) 0.0023(11) 0.0042(12) N4 0.0229(16) 0.0167(17) 0.0250(15) 0.0042(12) 0.0114(13) 0.0045(14) N5 0.0135(14) 0.0180(17) 0.0168(13) 0.0022(12) 0.0009(11) 0.0033(12) N6 0.0143(15) 0.0222(18) 0.0208(14) 0.0038(12) 0.0013(12) 0.0026(13) N7 0.085(4) 0.088(5) 0.118(5) 0.023(4) 0.024(4) -0.010(4) N8 0.091(4) 0.045(3) 0.059(3) 0.002(2) 0.012(3) -0.002(3) Re 0.01338(7) 0.01742(8) 0.01919(7) 0.00020(6) 0.00188(5) 0.00326(6) O1 0.0357(16) 0.0445(19) 0.0201(13) -0.0064(12) 0.0017(11) 0.0165(14) O2 0.0206(13) 0.0270(15) 0.0164(11) 0.0040(10) 0.0035(10) 0.0048(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 C1 N1 1.344(4) . ? C1 C2 1.378(5) . ? C2 N2 1.343(4) . ? C2 C5 1.515(4) . ? C3 N2 1.335(4) . ? C3 C4 1.380(5) . ? C4 N1 1.342(4) . ? C5 O1 1.242(4) . ? C5 O2 1.263(4) . ? C6 N3 1.320(4) . ? C6 C7 1.422(5) . ? C6 C18 1.490(5) . ? C7 C8 1.357(6) . ? C8 C9 1.400(6) . ? C9 C17 1.416(5) . ? C9 C10 1.425(6) . ? C10 C11 1.332(6) . ? C11 C12 1.441(6) . ? C12 C16 1.396(5) . ? C12 C13 1.410(6) . ? C13 C14 1.363(6) . ? C14 C15 1.407(6) . ? C15 N4 1.330(5) . ? C15 C19 1.495(5) . ? C16 N4 1.372(4) . ? C16 C17 1.432(5) . ? C17 N3 1.367(4) . ? C20 N5 1.340(4) . ? C20 C21 1.404(5) . ? C20 C32 1.498(5) . ? C21 C22 1.362(5) . ? C22 C23 1.406(5) . ? C23 C31 1.410(5) . ? C23 C24 1.429(5) . ? C24 C25 1.353(6) . ? C25 C26 1.426(5) . ? C26 C30 1.401(5) . ? C26 C27 1.419(6) . ? C27 C28 1.360(6) . ? C28 C29 1.409(5) . ? C29 N6 1.329(5) . ? C29 C33 1.495(5) . ? C30 N6 1.369(4) . ? C30 C31 1.441(5) . ? C31 N5 1.373(4) . ? C34 C35 1.356(8) . ? C35 N7 1.151(7) . ? C36 C37 1.449(7) . ? C37 N8 1.133(6) . ? Co O2 2.067(2) . ? Co N3 2.130(3) . ? Co N5 2.141(3) . ? Co N6 2.149(3) . ? Co N4 2.185(3) . ? Co N2 2.300(3) . ? Br1 Re 2.4766(4) . ? Br4 Re 2.4983(5) . ? Br3 Re 2.5028(5) . ? Br2 Re 2.4858(5) . ? Br5 Re 2.4951(5) . ? N1 Re 2.193(3) . ? N2 Co 2.300(3) . ? O2 Co 2.067(2) . ? 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 N1 C1 C2 122.0(3) . . ? N2 C2 C1 121.2(3) . . ? N2 C2 C5 117.8(3) . . ? C1 C2 C5 121.0(3) . . ? N2 C3 C4 121.8(3) . . ? N1 C4 C3 121.6(3) . . ? O1 C5 O2 127.5(3) . . ? O1 C5 C2 117.3(3) . . ? O2 C5 C2 115.2(3) . . ? N3 C6 C7 120.9(3) . . ? N3 C6 C18 119.6(3) . . ? C7 C6 C18 119.4(3) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 120.6(3) . . ? C8 C9 C17 116.5(3) . . ? C8 C9 C10 124.4(3) . . ? C17 C9 C10 119.1(4) . . ? C11 C10 C9 121.9(4) . . ? C10 C11 C12 120.7(4) . . ? C16 C12 C13 117.5(4) . . ? C16 C12 C11 119.1(4) . . ? C13 C12 C11 123.4(4) . . ? C14 C13 C12 119.2(4) . . ? C13 C14 C15 120.5(4) . . ? N4 C15 C14 121.1(4) . . ? N4 C15 C19 118.9(4) . . ? C14 C15 C19 120.0(4) . . ? N4 C16 C12 122.6(3) . . ? N4 C16 C17 117.0(3) . . ? C12 C16 C17 120.4(3) . . ? N3 C17 C9 122.5(3) . . ? N3 C17 C16 118.6(3) . . ? C9 C17 C16 118.8(3) . . ? N5 C20 C21 121.0(3) . . ? N5 C20 C32 119.2(3) . . ? C21 C20 C32 119.7(3) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C23 119.5(3) . . ? C22 C23 C31 117.2(3) . . ? C22 C23 C24 123.7(3) . . ? C31 C23 C24 119.2(3) . . ? C25 C24 C23 121.2(3) . . ? C24 C25 C26 120.7(4) . . ? C30 C26 C27 116.9(3) . . ? C30 C26 C25 119.9(4) . . ? C27 C26 C25 123.1(4) . . ? C28 C27 C26 118.7(4) . . ? C27 C28 C29 121.3(4) . . ? N6 C29 C28 121.0(3) . . ? N6 C29 C33 119.5(3) . . ? C28 C29 C33 119.5(3) . . ? N6 C30 C26 123.4(3) . . ? N6 C30 C31 117.3(3) . . ? C26 C30 C31 119.3(3) . . ? N5 C31 C23 122.7(3) . . ? N5 C31 C30 117.8(3) . . ? C23 C31 C30 119.5(3) . . ? N7 C35 C34 176.2(7) . . ? N8 C37 C36 178.7(5) . . ? O2 Co N3 84.87(10) . . ? O2 Co N5 170.57(9) . . ? N3 Co N5 104.54(10) . . ? O2 Co N6 99.49(11) . . ? N3 Co N6 108.56(11) . . ? N5 Co N6 78.36(11) . . ? O2 Co N4 80.38(10) . . ? N3 Co N4 77.84(11) . . ? N5 Co N4 100.72(11) . . ? N6 Co N4 173.59(10) . . ? O2 Co N2 75.54(9) . . ? N3 Co N2 159.51(10) . . ? N5 Co N2 95.03(10) . . ? N6 Co N2 81.00(11) . . ? N4 Co N2 92.80(11) . . ? C4 N1 C1 116.3(3) . . ? C4 N1 Re 123.6(2) . . ? C1 N1 Re 119.8(2) . . ? C3 N2 C2 116.9(3) . . ? C3 N2 Co 135.0(2) . . ? C2 N2 Co 107.8(2) . . ? C6 N3 C17 119.4(3) . . ? C6 N3 Co 128.6(2) . . ? C17 N3 Co 108.9(2) . . ? C15 N4 C16 118.8(3) . . ? C15 N4 Co 130.1(3) . . ? C16 N4 Co 108.2(2) . . ? C20 N5 C31 118.5(3) . . ? C20 N5 Co 131.0(2) . . ? C31 N5 Co 109.2(2) . . ? C29 N6 C30 118.4(3) . . ? C29 N6 Co 130.4(2) . . ? C30 N6 Co 109.0(2) . . ? N1 Re Br1 176.07(8) . . ? N1 Re Br2 89.12(7) . . ? Br1 Re Br2 91.282(17) . . ? N1 Re Br5 89.78(8) . . ? Br1 Re Br5 94.136(17) . . ? Br2 Re Br5 89.854(18) . . ? N1 Re Br4 87.36(7) . . ? Br1 Re Br4 92.361(18) . . ? Br2 Re Br4 175.988(15) . . ? Br5 Re Br4 88.208(18) . . ? N1 Re Br3 83.76(8) . . ? Br1 Re Br3 92.338(18) . . ? Br2 Re Br3 89.068(17) . . ? Br5 Re Br3 173.459(15) . . ? Br4 Re Br3 92.460(17) . . ? C5 O2 Co 119.0(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.901 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.099