Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Raul Chiozzone' _publ_contact_author_address ; Catedra de Quimica Inorganica Facultad de Quimica General Flores 2124 Montevideo CC-1157 URUGUAY ; _publ_contact_author_email RCHIOZZO@FQ.EDU.UY _publ_section_title ; A novel series of rhenium-bipyrimidine complexes: synthesis, crystal structure and electrochemical properties ; loop_ _publ_author_name 'Raul Chiozzone' 'Donatella Armentano' 'Maria Fernandez Cerda' 'G.De Munno' 'Juan Faus' ; R.Gonzalez ; 'Carlos Kremer' 'Jose Martinez-Lillo' # Attachment 'Compound_1_CCDC_623923_1.CIF' data_rebpma4n _database_code_depnum_ccdc_archive 'CCDC 623923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Cl4 N4 Re' _chemical_formula_weight 486.17 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.154(2) _cell_length_b 10.703(3) _cell_length_c 13.401(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1313.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description IRREGUALR _exptl_crystal_colour GOLDEN _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 10.049 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.0931 _exptl_absorpt_correction_T_max 0.1965 _exptl_absorpt_process_details XABS _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 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.9 _diffrn_reflns_number 4577 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 30.06 _reflns_number_total 3835 _reflns_number_gt 3552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0655P)^2^+4.6335P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(15) _refine_ls_number_reflns 3835 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Re1 Re 0.10883(3) 0.41532(3) 0.11461(2) 0.03343(10) Uani 1 1 d . . . Cl3 Cl 0.1180(4) 0.2006(2) 0.1265(2) 0.0619(7) Uani 1 1 d . . . Cl1 Cl -0.1448(2) 0.4195(3) 0.13811(18) 0.0539(6) Uani 1 1 d . . . Cl4 Cl 0.3526(2) 0.4320(3) 0.0686(2) 0.0493(5) Uani 1 1 d . . . Cl2 Cl 0.1579(3) 0.4496(3) 0.28201(17) 0.0534(6) Uani 1 1 d . . . N1 N 0.0606(7) 0.4177(7) -0.0412(5) 0.0337(13) Uani 1 1 d . . . N2 N 0.0950(8) 0.6092(6) 0.0800(5) 0.0322(13) Uani 1 1 d . . . C1 C 0.0545(10) 0.3169(8) -0.1018(8) 0.0402(18) Uani 1 1 d . . . H1A H 0.0832 0.2388 -0.0785 0.048 Uiso 1 1 calc R . . C5 C 0.0560(10) 0.6396(8) -0.0141(6) 0.0346(16) Uani 1 1 d . . . C4 C 0.0257(9) 0.5311(8) -0.0798(6) 0.0300(15) Uani 1 1 d . . . C8 C 0.1347(11) 0.7049(9) 0.1417(7) 0.045(2) Uani 1 1 d . . . H8A H 0.1616 0.6879 0.2072 0.054 Uiso 1 1 calc R . . C7 C 0.1352(11) 0.8253(9) 0.1078(8) 0.045(2) Uani 1 1 d . . . H7A H 0.1618 0.8910 0.1495 0.054 Uiso 1 1 calc R . . C6 C 0.0952(16) 0.8468(9) 0.0096(8) 0.056(3) Uani 1 1 d . . . H6A H 0.0955 0.9283 -0.0146 0.067 Uiso 1 1 calc R . . N3 N -0.0296(9) 0.5493(7) -0.1701(5) 0.0369(15) Uani 1 1 d . . . C3 C -0.0412(11) 0.4479(9) -0.2286(6) 0.0392(18) Uani 1 1 d . . . H3B H -0.0822 0.4566 -0.2917 0.047 Uiso 1 1 calc R . . C2 C 0.0056(11) 0.3309(8) -0.1984(7) 0.041(2) Uani 1 1 d . . . H2A H 0.0040 0.2635 -0.2421 0.050 Uiso 1 1 calc R . . N4 N 0.0552(11) 0.7520(7) -0.0526(6) 0.0464(19) 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 Re1 0.03093(14) 0.03873(15) 0.03061(14) 0.00946(12) -0.00322(12) -0.00254(13) Cl3 0.0689(16) 0.0415(11) 0.0754(18) 0.0224(12) -0.0180(17) -0.0076(12) Cl1 0.0344(9) 0.0858(18) 0.0415(11) 0.0104(12) -0.0002(8) -0.0044(11) Cl4 0.0351(10) 0.0517(14) 0.0612(14) 0.0073(11) 0.0041(9) 0.0032(9) Cl2 0.0479(12) 0.0790(18) 0.0333(9) 0.0121(10) -0.0078(9) -0.0109(12) N1 0.034(3) 0.034(3) 0.034(3) 0.005(3) -0.003(2) -0.002(3) N2 0.035(3) 0.038(3) 0.023(2) 0.001(2) 0.000(2) 0.007(3) C1 0.043(4) 0.033(4) 0.045(5) 0.000(4) 0.006(4) -0.005(3) C5 0.035(4) 0.039(4) 0.030(4) -0.001(3) -0.004(3) 0.009(3) C4 0.028(3) 0.033(4) 0.029(3) 0.004(3) 0.002(3) 0.005(3) C8 0.049(5) 0.047(5) 0.038(4) -0.002(3) -0.006(4) 0.003(4) C7 0.049(5) 0.040(4) 0.045(5) -0.015(4) -0.007(4) -0.001(3) C6 0.078(8) 0.034(4) 0.056(6) -0.005(4) -0.007(6) 0.016(5) N3 0.042(4) 0.044(4) 0.025(3) -0.002(3) -0.002(3) 0.008(3) C3 0.045(5) 0.043(5) 0.030(4) -0.005(3) -0.003(3) -0.004(4) C2 0.055(6) 0.035(4) 0.034(4) -0.008(3) 0.000(4) -0.010(4) N4 0.074(6) 0.028(3) 0.037(3) 0.000(3) -0.009(4) 0.011(4) _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 N2 2.131(7) . ? Re1 N1 2.134(7) . ? Re1 Cl3 2.306(3) . ? Re1 Cl2 2.317(2) . ? Re1 Cl4 2.322(2) . ? Re1 Cl1 2.344(2) . ? N1 C1 1.351(12) . ? N1 C4 1.358(11) . ? N2 C5 1.349(10) . ? N2 C8 1.366(12) . ? C1 C2 1.378(13) . ? C5 N4 1.309(11) . ? C5 C4 1.484(12) . ? C4 N3 1.326(10) . ? C8 C7 1.366(14) . ? C7 C6 1.386(15) . ? C6 N4 1.364(13) . ? N3 C3 1.343(11) . ? C3 C2 1.384(13) . ? 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 N2 Re1 N1 76.3(3) . . ? N2 Re1 Cl3 171.27(19) . . ? N1 Re1 Cl3 95.0(2) . . ? N2 Re1 Cl2 93.90(19) . . ? N1 Re1 Cl2 170.2(2) . . ? Cl3 Re1 Cl2 94.82(11) . . ? N2 Re1 Cl4 85.7(2) . . ? N1 Re1 Cl4 86.4(2) . . ? Cl3 Re1 Cl4 93.46(11) . . ? Cl2 Re1 Cl4 93.37(10) . . ? N2 Re1 Cl1 87.2(2) . . ? N1 Re1 Cl1 85.77(20) . . ? Cl3 Re1 Cl1 92.62(12) . . ? Cl2 Re1 Cl1 93.37(9) . . ? Cl4 Re1 Cl1 170.51(9) . . ? C1 N1 C4 118.4(7) . . ? C1 N1 Re1 125.9(6) . . ? C4 N1 Re1 115.6(6) . . ? C5 N2 C8 117.1(7) . . ? C5 N2 Re1 117.0(5) . . ? C8 N2 Re1 125.6(6) . . ? N1 C1 C2 119.4(8) . . ? N4 C5 N2 126.3(8) . . ? N4 C5 C4 118.9(7) . . ? N2 C5 C4 114.5(7) . . ? N3 C4 N1 124.6(8) . . ? N3 C4 C5 119.9(7) . . ? N1 C4 C5 115.4(7) . . ? N2 C8 C7 120.5(9) . . ? C8 C7 C6 118.1(9) . . ? N4 C6 C7 121.9(9) . . ? C4 N3 C3 116.4(8) . . ? N3 C3 C2 122.4(8) . . ? C1 C2 C3 118.3(8) . . ? C5 N4 C6 116.1(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.362 _refine_diff_density_min -1.844 _refine_diff_density_rms 0.227 # Attachment 'Compound_2_CCDC_623924_.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 623924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H6 Br4 N4 Re' _chemical_formula_weight 664.01 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.6216(9) _cell_length_b 10.8583(10) _cell_length_c 13.4431(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1404.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8317 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 31.27 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 20.015 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0653 _exptl_absorpt_correction_T_max 0.1232 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_% 2.2 _diffrn_reflns_number 17330 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 32.86 _reflns_number_total 4872 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _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^)+(0.0289P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.030(14) _refine_ls_number_reflns 4872 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 Re1 Re 0.10896(2) 0.415233(19) 0.113088(13) 0.02996(6) Uani 1 1 d . . . Br3 Br 0.11977(8) 0.19146(6) 0.12714(5) 0.05649(19) Uani 1 1 d . . . Br1 Br -0.14833(6) 0.42062(8) 0.13664(4) 0.05168(16) Uani 1 1 d . . . Br4 Br 0.35362(6) 0.43321(6) 0.06186(4) 0.04579(15) Uani 1 1 d . . . Br2 Br 0.15865(7) 0.44858(7) 0.28916(4) 0.05078(18) Uani 1 1 d . . . N1 N 0.0618(5) 0.4192(4) -0.0430(3) 0.0300(9) Uani 1 1 d . . . N2 N 0.0964(5) 0.6074(4) 0.0776(3) 0.0307(9) Uani 1 1 d . . . C1 C 0.0528(6) 0.3210(5) -0.1042(4) 0.0406(13) Uani 1 1 d . . . H1A H 0.0803 0.2438 -0.0817 0.049 Uiso 1 1 calc R . . C5 C 0.0594(6) 0.6363(5) -0.0165(4) 0.0321(11) Uani 1 1 d . . . C4 C 0.0266(6) 0.5288(5) -0.0808(3) 0.0299(11) Uani 1 1 d . . . C8 C 0.1374(7) 0.7023(5) 0.1381(4) 0.0436(14) Uani 1 1 d . . . H8A H 0.1640 0.6865 0.2034 0.052 Uiso 1 1 calc R . . C7 C 0.1392(8) 0.8203(5) 0.1025(5) 0.0480(15) Uani 1 1 d . . . H7A H 0.1658 0.8859 0.1427 0.058 Uiso 1 1 calc R . . C6 C 0.1003(7) 0.8386(5) 0.0054(5) 0.0489(15) Uani 1 1 d . . . H6A H 0.1056 0.9178 -0.0207 0.059 Uiso 1 1 calc R . . N3 N -0.0264(5) 0.5475(5) -0.1690(3) 0.0397(11) Uani 1 1 d . . . C3 C -0.0404(6) 0.4476(6) -0.2271(4) 0.0426(14) Uani 1 1 d . . . H3B H -0.0816 0.4561 -0.2893 0.051 Uiso 1 1 calc R . . C2 C 0.0044(7) 0.3335(5) -0.1975(4) 0.0409(15) Uani 1 1 d . . . H2A H 0.0014 0.2667 -0.2407 0.049 Uiso 1 1 calc R . . N4 N 0.0551(6) 0.7477(5) -0.0534(4) 0.0462(13) 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 Re1 0.02747(10) 0.04024(10) 0.02216(8) 0.00688(8) -0.00218(7) -0.00135(9) Br3 0.0667(5) 0.0426(3) 0.0602(4) 0.0163(3) -0.0161(4) -0.0075(3) Br1 0.0282(3) 0.0908(5) 0.0360(3) 0.0081(3) 0.0013(2) -0.0027(3) Br4 0.0284(3) 0.0628(4) 0.0461(3) 0.0065(3) 0.0046(2) 0.0026(3) Br2 0.0439(4) 0.0831(5) 0.0253(2) 0.0061(3) -0.0057(2) -0.0064(3) N1 0.036(2) 0.033(2) 0.0211(17) 0.0043(17) -0.0004(16) 0.001(2) N2 0.028(2) 0.039(2) 0.0246(17) -0.0031(15) -0.0010(17) 0.0033(19) C1 0.043(3) 0.042(3) 0.036(3) 0.000(3) 0.003(3) -0.005(2) C5 0.033(3) 0.037(3) 0.025(2) 0.000(2) -0.002(2) 0.010(2) C4 0.030(3) 0.040(3) 0.020(2) 0.0031(18) -0.0013(19) 0.006(2) C8 0.050(4) 0.052(3) 0.029(3) -0.003(2) -0.009(2) 0.007(3) C7 0.059(4) 0.040(3) 0.045(3) -0.012(3) 0.002(3) 0.002(3) C6 0.059(4) 0.039(3) 0.049(3) -0.001(3) -0.001(3) 0.009(3) N3 0.042(3) 0.052(3) 0.025(2) -0.0022(19) -0.006(2) 0.011(2) C3 0.039(3) 0.066(4) 0.023(2) -0.008(2) -0.009(2) -0.005(3) C2 0.060(4) 0.041(3) 0.022(2) -0.006(2) 0.001(2) -0.016(3) N4 0.062(4) 0.035(3) 0.042(3) 0.001(2) -0.005(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.144(4) . ? Re1 N1 2.147(4) . ? Re1 Br3 2.4394(7) . ? Re1 Br2 2.4418(6) . ? Re1 Br4 2.4604(6) . ? Re1 Br1 2.4964(7) . ? N1 C4 1.338(7) . ? N1 C1 1.350(7) . ? N2 C5 1.351(6) . ? N2 C8 1.372(7) . ? C1 C2 1.343(8) . ? C5 N4 1.308(7) . ? C5 C4 1.486(7) . ? C4 N3 1.307(6) . ? C8 C7 1.368(8) . ? C7 C6 1.373(9) . ? C6 N4 1.337(8) . ? N3 C3 1.344(7) . ? C3 C2 1.371(9) . ? 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 N2 Re1 N1 75.59(16) . . ? N2 Re1 Br3 171.53(11) . . ? N1 Re1 Br3 95.99(12) . . ? N2 Re1 Br2 94.74(11) . . ? N1 Re1 Br2 170.30(12) . . ? Br3 Re1 Br2 93.69(3) . . ? N2 Re1 Br4 85.09(12) . . ? N1 Re1 Br4 85.83(12) . . ? Br3 Re1 Br4 93.43(3) . . ? Br2 Re1 Br4 94.14(2) . . ? N2 Re1 Br1 87.11(12) . . ? N1 Re1 Br1 85.05(12) . . ? Br3 Re1 Br1 93.20(3) . . ? Br2 Re1 Br1 93.88(2) . . ? Br4 Re1 Br1 169.23(2) . . ? C4 N1 C1 117.1(4) . . ? C4 N1 Re1 116.2(3) . . ? C1 N1 Re1 126.5(4) . . ? C5 N2 C8 117.2(4) . . ? C5 N2 Re1 116.7(3) . . ? C8 N2 Re1 125.7(4) . . ? C2 C1 N1 120.7(6) . . ? N4 C5 N2 125.3(5) . . ? N4 C5 C4 119.9(5) . . ? N2 C5 C4 114.7(4) . . ? N3 C4 N1 125.5(5) . . ? N3 C4 C5 119.3(5) . . ? N1 C4 C5 115.1(4) . . ? C7 C8 N2 120.0(5) . . ? C8 C7 C6 117.7(5) . . ? N4 C6 C7 122.9(6) . . ? C4 N3 C3 116.2(5) . . ? N3 C3 C2 121.9(5) . . ? C1 C2 C3 118.1(5) . . ? C5 N4 C6 116.6(5) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 32.86 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.549 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.156 # Attachment 'Compound_3_CCDC_623925_1.CIF' data_rebpmpph _database_code_depnum_ccdc_archive 'CCDC 623925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Cl4 N4 P Re' _chemical_formula_weight 825.54 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0661(9) _cell_length_b 12.6350(12) _cell_length_c 14.2539(13) _cell_angle_alpha 89.361(2) _cell_angle_beta 86.606(2) _cell_angle_gamma 82.236(2) _cell_volume 1615.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6489 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 32.14 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 4.172 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4892 _exptl_absorpt_correction_T_max 0.6804 _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 20306 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 32.93 _reflns_number_total 10366 _reflns_number_gt 9342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX II' _computing_cell_refinement 'Bruker APEX II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0226P)^2^+0.3058P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10366 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.005 _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 0.719824(7) 0.864277(5) 0.752955(5) 0.03868(3) Uani 1 1 d . . . Cl1 Cl 0.92685(7) 0.78983(5) 0.65430(4) 0.06262(14) Uani 1 1 d . . . Cl2 Cl 0.71796(6) 0.70849(4) 0.84777(4) 0.05517(12) Uani 1 1 d . . . Cl3 Cl 0.55095(6) 0.80201(4) 0.65178(4) 0.05639(12) Uani 1 1 d . . . N1 N 0.54354(16) 0.95037(12) 0.82748(11) 0.0390(3) Uani 1 1 d . . . N2 N 0.70150(16) 1.01010(12) 0.68799(11) 0.0382(3) Uani 1 1 d . . . N3 N 0.59328(17) 1.19313(12) 0.70463(12) 0.0433(3) Uani 1 1 d . . . N4 N 0.42461(18) 1.12798(13) 0.86076(12) 0.0471(4) Uani 1 1 d . . . C1 C 0.4458(2) 0.91196(17) 0.88958(15) 0.0500(4) Uani 1 1 d . . . H1A H 0.4519 0.8386 0.8993 0.060 Uiso 1 1 calc R . . C2 C 0.3386(2) 0.97869(19) 0.93828(16) 0.0568(5) Uani 1 1 d . . . H2A H 0.2700 0.9519 0.9802 0.068 Uiso 1 1 calc R . . C3 C 0.3343(2) 1.08754(19) 0.92374(15) 0.0546(5) Uani 1 1 d . . . H3B H 0.2655 1.1340 0.9596 0.066 Uiso 1 1 calc R . . C4 C 0.52341(19) 1.05817(14) 0.81245(12) 0.0373(3) Uani 1 1 d . . . C5 C 0.61145(19) 1.09176(13) 0.73321(12) 0.0369(3) Uani 1 1 d . . . C6 C 0.7727(2) 1.03564(17) 0.60622(14) 0.0491(4) Uani 1 1 d . . . H6A H 0.8346 0.9827 0.5727 0.059 Uiso 1 1 calc R . . C7 C 0.7552(3) 1.13722(17) 0.57241(15) 0.0532(5) Uani 1 1 d . . . H7A H 0.8024 1.1542 0.5156 0.064 Uiso 1 1 calc R . . C8 C 0.6648(2) 1.21481(16) 0.62508(15) 0.0493(4) Uani 1 1 d . . . H8A H 0.6543 1.2850 0.6034 0.059 Uiso 1 1 calc R . . P1 P 0.94932(5) 0.64795(3) 0.26218(3) 0.03494(9) Uani 1 1 d . . . C9 C 0.85923(19) 0.77614(14) 0.30128(13) 0.0378(3) Uani 1 1 d . . . C10 C 0.7498(2) 0.78240(17) 0.37432(15) 0.0477(4) Uani 1 1 d . . . H10A H 0.7198 0.7206 0.4007 0.057 Uiso 1 1 calc R . . C11 C 0.6863(2) 0.88165(19) 0.40733(16) 0.0555(5) Uani 1 1 d . . . H11A H 0.6136 0.8866 0.4565 0.067 Uiso 1 1 calc R . . C12 C 0.7296(3) 0.97246(17) 0.36802(17) 0.0580(6) Uani 1 1 d . . . H12A H 0.6847 1.0388 0.3899 0.070 Uiso 1 1 calc R . . C13 C 0.8391(3) 0.96687(16) 0.29646(17) 0.0572(5) Uani 1 1 d . . . H13A H 0.8689 1.0292 0.2709 0.069 Uiso 1 1 calc R . . C14 C 0.9048(2) 0.86838(15) 0.26263(15) 0.0468(4) Uani 1 1 d . . . H14A H 0.9790 0.8641 0.2144 0.056 Uiso 1 1 calc R . . C15 C 1.07501(18) 0.59437(13) 0.34852(12) 0.0363(3) Uani 1 1 d . . . C16 C 1.1862(2) 0.51013(16) 0.32578(15) 0.0485(4) Uani 1 1 d . . . H16A H 1.1971 0.4821 0.2653 0.058 Uiso 1 1 calc R . . C17 C 1.2808(3) 0.46805(18) 0.39415(19) 0.0602(6) Uani 1 1 d . . . H17A H 1.3548 0.4112 0.3797 0.072 Uiso 1 1 calc R . . C18 C 1.2647(3) 0.51065(18) 0.48340(17) 0.0569(5) Uani 1 1 d . . . H18A H 1.3286 0.4827 0.5289 0.068 Uiso 1 1 calc R . . C19 C 1.1557(2) 0.59371(18) 0.50544(14) 0.0510(5) Uani 1 1 d . . . H19A H 1.1463 0.6222 0.5657 0.061 Uiso 1 1 calc R . . C20 C 1.0596(2) 0.63560(15) 0.43893(13) 0.0414(4) Uani 1 1 d . . . H20A H 0.9846 0.6914 0.4546 0.050 Uiso 1 1 calc R . . C21 C 1.05077(19) 0.66410(14) 0.15269(12) 0.0393(4) Uani 1 1 d . . . C22 C 0.9825(2) 0.6574(2) 0.06878(15) 0.0577(5) Uani 1 1 d . . . H22A H 0.8879 0.6367 0.0687 0.069 Uiso 1 1 calc R . . C23 C 1.0562(3) 0.6817(3) -0.01453(16) 0.0750(8) Uani 1 1 d . . . H23A H 1.0105 0.6788 -0.0710 0.090 Uiso 1 1 calc R . . C24 C 1.1972(3) 0.7103(3) -0.01403(17) 0.0757(8) Uani 1 1 d . . . H24A H 1.2468 0.7256 -0.0705 0.091 Uiso 1 1 calc R . . C25 C 1.2657(3) 0.7166(2) 0.06850(16) 0.0613(6) Uani 1 1 d . . . H25A H 1.3611 0.7360 0.0681 0.074 Uiso 1 1 calc R . . C26 C 1.1920(2) 0.69389(18) 0.15194(14) 0.0477(4) Uani 1 1 d . . . H26A H 1.2376 0.6986 0.2082 0.057 Uiso 1 1 calc R . . C27 C 0.81288(19) 0.56065(14) 0.24698(13) 0.0383(3) Uani 1 1 d . . . C28 C 0.6707(2) 0.60169(18) 0.22230(19) 0.0573(5) Uani 1 1 d . . . H28A H 0.6444 0.6749 0.2148 0.069 Uiso 1 1 calc R . . C29 C 0.5690(2) 0.5320(2) 0.2091(2) 0.0691(7) Uani 1 1 d . . . H29A H 0.4741 0.5588 0.1913 0.083 Uiso 1 1 calc R . . C30 C 0.6050(3) 0.4249(2) 0.22166(19) 0.0625(6) Uani 1 1 d . . . H30A H 0.5340 0.3794 0.2143 0.075 Uiso 1 1 calc R . . C31 C 0.7468(3) 0.38368(17) 0.24529(15) 0.0530(5) Uani 1 1 d . . . H31A H 0.7717 0.3104 0.2532 0.064 Uiso 1 1 calc R . . C32 C 0.8512(2) 0.45106(15) 0.25714(13) 0.0423(4) Uani 1 1 d . . . H32A H 0.9473 0.4233 0.2719 0.051 Uiso 1 1 calc R . . Cl4 Cl 0.88158(6) 0.93076(5) 0.85584(4) 0.05423(12) 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 Re1 0.04336(4) 0.02865(3) 0.04342(4) -0.00038(3) -0.00097(3) -0.00320(2) Cl1 0.0620(3) 0.0518(3) 0.0671(3) -0.0075(3) 0.0105(3) 0.0120(2) Cl2 0.0638(3) 0.0378(2) 0.0656(3) 0.0123(2) -0.0142(2) -0.0096(2) Cl3 0.0657(3) 0.0376(2) 0.0670(3) -0.0050(2) -0.0209(2) -0.0034(2) N1 0.0432(7) 0.0332(7) 0.0409(8) 0.0019(6) -0.0018(6) -0.0066(6) N2 0.0441(7) 0.0313(7) 0.0397(7) -0.0025(6) -0.0013(6) -0.0070(6) N3 0.0473(8) 0.0309(7) 0.0528(9) 0.0019(6) -0.0048(7) -0.0084(6) N4 0.0491(8) 0.0427(8) 0.0473(9) -0.0044(7) 0.0021(7) 0.0001(7) C1 0.0544(11) 0.0440(10) 0.0516(11) 0.0079(9) 0.0062(9) -0.0107(8) C2 0.0560(11) 0.0613(13) 0.0515(12) 0.0053(10) 0.0112(9) -0.0089(10) C3 0.0511(11) 0.0593(13) 0.0493(11) -0.0041(10) 0.0060(9) 0.0041(9) C4 0.0386(8) 0.0330(8) 0.0407(9) -0.0025(7) -0.0038(6) -0.0055(6) C5 0.0409(8) 0.0297(7) 0.0409(9) -0.0002(7) -0.0053(7) -0.0070(6) C6 0.0615(11) 0.0427(10) 0.0428(10) -0.0017(8) 0.0076(8) -0.0105(9) C7 0.0706(13) 0.0474(11) 0.0443(10) 0.0049(9) 0.0036(9) -0.0207(10) C8 0.0591(11) 0.0354(9) 0.0561(12) 0.0091(8) -0.0072(9) -0.0152(8) P1 0.03581(19) 0.03197(19) 0.0371(2) -0.00271(17) 0.00104(16) -0.00607(15) C9 0.0387(8) 0.0324(8) 0.0421(9) -0.0027(7) -0.0033(7) -0.0033(6) C10 0.0466(9) 0.0437(10) 0.0514(11) -0.0032(8) 0.0041(8) -0.0035(8) C11 0.0473(10) 0.0583(13) 0.0578(12) -0.0160(10) -0.0004(9) 0.0042(9) C12 0.0620(12) 0.0428(11) 0.0667(14) -0.0159(10) -0.0163(10) 0.0085(9) C13 0.0733(14) 0.0333(9) 0.0656(14) -0.0002(9) -0.0127(11) -0.0054(9) C14 0.0550(10) 0.0373(9) 0.0481(10) 0.0020(8) -0.0026(8) -0.0071(8) C15 0.0371(7) 0.0330(8) 0.0389(8) 0.0000(7) 0.0013(6) -0.0065(6) C16 0.0494(10) 0.0403(9) 0.0536(11) -0.0069(9) 0.0006(8) 0.0008(8) C17 0.0547(11) 0.0427(11) 0.0790(16) 0.0043(11) -0.0032(11) 0.0083(9) C18 0.0598(12) 0.0515(12) 0.0585(13) 0.0185(10) -0.0093(10) -0.0033(9) C19 0.0597(11) 0.0550(12) 0.0382(10) 0.0090(9) -0.0028(8) -0.0090(9) C20 0.0439(9) 0.0401(9) 0.0392(9) 0.0013(7) 0.0040(7) -0.0051(7) C21 0.0410(8) 0.0397(9) 0.0377(8) -0.0034(7) 0.0005(7) -0.0085(7) C22 0.0503(11) 0.0808(16) 0.0458(11) -0.0052(11) -0.0045(9) -0.0211(10) C23 0.0797(16) 0.112(2) 0.0392(11) -0.0022(13) -0.0059(11) -0.0336(16) C24 0.0836(17) 0.106(2) 0.0431(12) -0.0010(13) 0.0121(11) -0.0394(16) C25 0.0568(12) 0.0791(16) 0.0520(12) -0.0035(11) 0.0090(10) -0.0286(11) C26 0.0464(9) 0.0592(12) 0.0395(9) -0.0041(9) -0.0009(7) -0.0153(8) C27 0.0383(8) 0.0365(8) 0.0405(9) -0.0037(7) 0.0029(7) -0.0086(6) C28 0.0399(9) 0.0445(11) 0.0870(16) -0.0067(11) -0.0017(10) -0.0049(8) C29 0.0374(10) 0.0650(15) 0.106(2) -0.0099(14) -0.0054(11) -0.0112(9) C30 0.0556(12) 0.0628(14) 0.0749(15) -0.0084(12) 0.0011(11) -0.0300(11) C31 0.0715(13) 0.0412(10) 0.0500(11) 0.0008(9) -0.0066(10) -0.0202(9) C32 0.0525(10) 0.0370(8) 0.0394(9) 0.0009(7) -0.0062(7) -0.0111(7) Cl4 0.0539(3) 0.0602(3) 0.0518(3) -0.0021(2) -0.0038(2) -0.0190(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.0438(15) . ? Re1 N1 2.0545(14) . ? Re1 Cl4 2.3711(5) . ? Re1 Cl1 2.3717(5) . ? Re1 Cl2 2.3766(6) . ? Re1 Cl3 2.3780(5) . ? N1 C1 1.348(2) . ? N1 C4 1.366(2) . ? N2 C6 1.356(2) . ? N2 C5 1.368(2) . ? N3 C8 1.317(3) . ? N3 C5 1.332(2) . ? N4 C3 1.324(3) . ? N4 C4 1.335(2) . ? C1 C2 1.360(3) . ? C2 C3 1.384(3) . ? C4 C5 1.438(3) . ? C6 C7 1.358(3) . ? C7 C8 1.386(3) . ? P1 C21 1.7880(18) . ? P1 C27 1.7887(18) . ? P1 C9 1.7916(17) . ? P1 C15 1.7918(18) . ? C9 C14 1.386(3) . ? C9 C10 1.390(3) . ? C10 C11 1.383(3) . ? C11 C12 1.366(3) . ? C12 C13 1.376(3) . ? C13 C14 1.384(3) . ? C15 C20 1.388(2) . ? C15 C16 1.390(2) . ? C16 C17 1.390(3) . ? C17 C18 1.379(3) . ? C18 C19 1.366(3) . ? C19 C20 1.379(3) . ? C21 C26 1.382(3) . ? C21 C22 1.387(3) . ? C22 C23 1.380(3) . ? C23 C24 1.375(4) . ? C24 C25 1.370(3) . ? C25 C26 1.376(3) . ? C27 C28 1.387(3) . ? C27 C32 1.389(2) . ? C28 C29 1.379(3) . ? C29 C30 1.362(4) . ? C30 C31 1.379(3) . ? C31 C32 1.374(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 N2 Re1 N1 76.90(6) . . ? N2 Re1 Cl4 87.41(4) . . ? N1 Re1 Cl4 88.32(5) . . ? N2 Re1 Cl1 94.29(4) . . ? N1 Re1 Cl1 171.17(4) . . ? Cl4 Re1 Cl1 90.62(2) . . ? N2 Re1 Cl2 171.16(4) . . ? N1 Re1 Cl2 94.60(5) . . ? Cl4 Re1 Cl2 89.92(2) . . ? Cl1 Re1 Cl2 94.16(2) . . ? N2 Re1 Cl3 91.73(4) . . ? N1 Re1 Cl3 89.80(5) . . ? Cl4 Re1 Cl3 178.062(17) . . ? Cl1 Re1 Cl3 91.18(2) . . ? Cl2 Re1 Cl3 90.68(2) . . ? C1 N1 C4 116.58(16) . . ? C1 N1 Re1 127.03(13) . . ? C4 N1 Re1 116.39(12) . . ? C6 N2 C5 116.27(16) . . ? C6 N2 Re1 127.03(13) . . ? C5 N2 Re1 116.66(12) . . ? C8 N3 C5 116.76(16) . . ? C3 N4 C4 116.51(18) . . ? N1 C1 C2 121.1(2) . . ? C1 C2 C3 118.1(2) . . ? N4 C3 C2 122.47(19) . . ? N4 C4 N1 124.90(17) . . ? N4 C4 C5 121.06(16) . . ? N1 C4 C5 113.87(14) . . ? N3 C5 N2 125.09(17) . . ? N3 C5 C4 120.60(15) . . ? N2 C5 C4 114.07(15) . . ? N2 C6 C7 121.15(18) . . ? C6 C7 C8 118.04(19) . . ? N3 C8 C7 122.63(18) . . ? C21 P1 C27 109.63(8) . . ? C21 P1 C9 108.81(9) . . ? C27 P1 C9 109.83(8) . . ? C21 P1 C15 109.84(8) . . ? C27 P1 C15 110.16(9) . . ? C9 P1 C15 108.55(8) . . ? C14 C9 C10 120.30(17) . . ? C14 C9 P1 120.02(14) . . ? C10 C9 P1 119.57(15) . . ? C11 C10 C9 119.2(2) . . ? C12 C11 C10 120.3(2) . . ? C11 C12 C13 120.77(19) . . ? C12 C13 C14 119.9(2) . . ? C13 C14 C9 119.5(2) . . ? C20 C15 C16 119.83(17) . . ? C20 C15 P1 119.94(13) . . ? C16 C15 P1 120.21(14) . . ? C17 C16 C15 119.47(19) . . ? C18 C17 C16 119.92(19) . . ? C19 C18 C17 120.5(2) . . ? C18 C19 C20 120.5(2) . . ? C19 C20 C15 119.84(17) . . ? C26 C21 C22 119.79(18) . . ? C26 C21 P1 119.79(14) . . ? C22 C21 P1 120.09(14) . . ? C23 C22 C21 119.5(2) . . ? C24 C23 C22 120.0(2) . . ? C25 C24 C23 121.0(2) . . ? C24 C25 C26 119.4(2) . . ? C25 C26 C21 120.45(19) . . ? C28 C27 C32 119.98(17) . . ? C28 C27 P1 120.25(15) . . ? C32 C27 P1 119.74(14) . . ? C29 C28 C27 118.8(2) . . ? C30 C29 C28 121.3(2) . . ? C29 C30 C31 120.0(2) . . ? C32 C31 C30 119.9(2) . . ? C31 C32 C27 119.92(18) . . ? _diffrn_measured_fraction_theta_max 0.856 _diffrn_reflns_theta_full 32.93 _diffrn_measured_fraction_theta_full 0.856 _refine_diff_density_max 0.851 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.057 # Attachment 'Compound_4_CCDC_623926_1.CIF' data_rebrbpmc _database_code_depnum_ccdc_archive 'CCDC 623926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H84 Br8 N10 Re2' _chemical_formula_weight 1812.93 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.227(3) _cell_length_b 11.094(2) _cell_length_c 18.502(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.87(3) _cell_angle_gamma 90.00 _cell_volume 3203.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description irregular _exptl_crystal_colour red-purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 8.802 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1267 _exptl_absorpt_correction_T_max 0.1919 _exptl_absorpt_process_details psi-scan _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 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.2 _diffrn_reflns_number 6237 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5992 _reflns_number_gt 4070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _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^)+(0.0720P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 5992 _refine_ls_number_parameters 577 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.003 _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 0.34169(5) 0.56154(8) 0.74125(4) 0.0669(2) Uani 1 1 d . . . Br1 Br 0.42226(17) 0.3669(3) 0.77538(16) 0.1012(9) Uani 1 1 d . . . Br2 Br 0.38223(19) 0.6270(3) 0.87703(13) 0.1066(9) Uani 1 1 d . . . Br3 Br 0.20446(17) 0.4617(2) 0.74983(15) 0.0870(7) Uani 1 1 d . . . Br4 Br 0.26567(16) 0.7611(2) 0.70415(14) 0.0860(7) Uani 1 1 d . . . N1 N 0.4433(11) 0.6433(16) 0.7123(10) 0.072(5) Uani 1 1 d . . . N2 N 0.3219(11) 0.5244(16) 0.6278(9) 0.070(5) Uani 1 1 d . . . C1 C 0.5195(18) 0.699(4) 0.7593(16) 0.122(11) Uani 1 1 d . . . H1A H 0.5300 0.6986 0.8113 0.147 Uiso 1 1 calc R . . C2 C 0.5761(16) 0.752(2) 0.727(2) 0.105(9) Uani 1 1 d . . . H2A H 0.6250 0.7915 0.7549 0.126 Uiso 1 1 calc R . . C3 C 0.557(2) 0.745(3) 0.649(2) 0.121(12) Uani 1 1 d . . . H3A H 0.5972 0.7744 0.6265 0.145 Uiso 1 1 calc R . . C4 C 0.4394(12) 0.6509(19) 0.6398(12) 0.068(6) Uani 1 1 d . . . C5 C 0.3691(15) 0.582(2) 0.5912(11) 0.073(6) Uani 1 1 d . . . N3 N 0.4926(15) 0.704(2) 0.6083(12) 0.090(6) Uani 1 1 d . . . N4 N 0.3564(12) 0.5771(19) 0.5163(9) 0.080(5) Uani 1 1 d . . . C6 C 0.2644(14) 0.443(2) 0.5848(11) 0.085(7) Uani 1 1 d . . . H6A H 0.2352 0.3905 0.6083 0.102 Uiso 1 1 calc R . . C7 C 0.2497(14) 0.438(3) 0.5092(14) 0.098(8) Uani 1 1 d . . . H7A H 0.2060 0.3893 0.4809 0.117 Uiso 1 1 calc R . . C8 C 0.2976(15) 0.502(2) 0.4757(12) 0.076(6) Uani 1 1 d . . . H8A H 0.2903 0.4938 0.4243 0.091 Uiso 1 1 calc R . . Re2 Re 0.85407(5) 0.91831(7) 0.76671(4) 0.0580(2) Uani 1 1 d . . . Br5 Br 0.80734(14) 0.7911(2) 0.86124(11) 0.0774(6) Uani 1 1 d . . . Br6 Br 0.71701(14) 1.0383(2) 0.73551(12) 0.0793(6) Uani 1 1 d . . . Br7 Br 0.79178(15) 0.7611(2) 0.66687(11) 0.0751(6) Uani 1 1 d . . . Br8 Br 0.91055(15) 1.0324(2) 0.67249(12) 0.0792(6) Uani 1 1 d . . . N5 N 0.9176(11) 1.0296(19) 0.8542(9) 0.075(5) Uani 1 1 d . . . N6 N 0.9767(11) 0.8437(17) 0.8040(10) 0.074(5) Uani 1 1 d . . . C9 C 0.8887(14) 1.131(2) 0.8759(11) 0.072(5) Uani 1 1 d . . . H9A H 0.8353 1.1606 0.8492 0.086 Uiso 1 1 calc R . . C10 C 0.9372(17) 1.195(2) 0.9386(14) 0.096(8) Uani 1 1 d . . . H10A H 0.9168 1.2673 0.9526 0.115 Uiso 1 1 calc R . . C11 C 1.0145(15) 1.151(3) 0.9786(13) 0.086(7) Uani 1 1 d . . . H11A H 1.0466 1.1914 1.0209 0.104 Uiso 1 1 calc R . . C12 C 0.9982(13) 0.9903(19) 0.8959(11) 0.066(5) Uani 1 1 d . . . N7 N 1.0441(11) 1.047(2) 0.9559(11) 0.093(6) Uani 1 1 d . . . N8 N 1.1084(13) 0.846(2) 0.8957(13) 0.097(6) Uani 1 1 d . . . C13 C 1.0290(13) 0.883(2) 0.8675(10) 0.065(5) Uani 1 1 d . . . C14 C 1.1359(16) 0.757(3) 0.8591(18) 0.095(8) Uani 1 1 d . . . H14A H 1.1905 0.7258 0.8793 0.114 Uiso 1 1 calc R . . C15 C 1.0874(15) 0.712(2) 0.7948(17) 0.092(7) Uani 1 1 d . . . H15A H 1.1085 0.6506 0.7704 0.110 Uiso 1 1 calc R . . C16 C 1.0063(15) 0.756(2) 0.7649(13) 0.082(7) Uani 1 1 d . . . H16A H 0.9721 0.7266 0.7193 0.099 Uiso 1 1 calc R . . N9 N 0.3125(13) 0.1012(18) 0.9194(10) 0.091(6) Uani 1 1 d . . . C17 C 0.2975(18) 0.025(3) 0.9857(15) 0.114(9) Uani 1 1 d . . . H17A H 0.2380 0.0344 0.9854 0.137 Uiso 1 1 calc R . . H17B H 0.3060 -0.0591 0.9756 0.137 Uiso 1 1 calc R . . C18 C 0.349(2) 0.051(6) 1.0593(18) 0.19(2) Uani 1 1 d . . . H18A H 0.3458 0.1370 1.0690 0.228 Uiso 1 1 calc R . . H18B H 0.4082 0.0318 1.0629 0.228 Uiso 1 1 calc R . . C19 C 0.318(3) -0.023(6) 1.121(2) 0.19(2) Uani 1 1 d . . . H19A H 0.3576 -0.0087 1.1704 0.226 Uiso 1 1 calc R . . H19B H 0.2619 0.0040 1.1222 0.226 Uiso 1 1 calc R . . C20 C 0.316(4) -0.150(5) 1.104(3) 0.22(2) Uani 1 1 d . . . H20A H 0.2952 -0.1940 1.1398 0.331 Uiso 1 1 calc R . . H20B H 0.3729 -0.1773 1.1057 0.331 Uiso 1 1 calc R . . H20C H 0.2789 -0.1634 1.0543 0.331 Uiso 1 1 calc R . . C21 C 0.3988 0.0720 0.8881 0.050 Uiso 1 1 d . . . H21A H 0.3842 0.0866 0.8344 0.060 Uiso 1 1 calc R . . H21B H 0.4447 0.1268 0.9121 0.060 Uiso 1 1 calc R . . C22 C 0.4250 -0.0356 0.9012 0.050 Uiso 1 1 d . . . H22A H 0.3943 -0.0862 0.8598 0.060 Uiso 1 1 calc R . . H22B H 0.4113 -0.0636 0.9462 0.060 Uiso 1 1 calc R . . C23 C 0.5294 -0.0522 0.9126 0.050 Uiso 1 1 d . . . H23A H 0.5588 -0.0360 0.9648 0.060 Uiso 1 1 calc R . . H23B H 0.5402 -0.1358 0.9028 0.060 Uiso 1 1 calc R . . C24 C 0.5615 0.0124 0.8727 0.050 Uiso 1 1 d . . . H24A H 0.6217 -0.0041 0.8836 0.075 Uiso 1 1 calc R . . H24B H 0.5531 0.0957 0.8829 0.075 Uiso 1 1 calc R . . H24C H 0.5345 -0.0044 0.8207 0.075 Uiso 1 1 calc R . . C25 C 0.2419(13) 0.047(2) 0.8538(11) 0.090(7) Uani 1 1 d . . . H25A H 0.1870 0.0544 0.8647 0.108 Uiso 1 1 calc R . . H25B H 0.2533 -0.0381 0.8493 0.108 Uiso 1 1 calc R . . C26 C 0.2371(17) 0.111(2) 0.7772(15) 0.104(8) Uani 1 1 d . . . H26A H 0.2372 0.1979 0.7835 0.124 Uiso 1 1 calc R . . H26B H 0.2862 0.0890 0.7597 0.124 Uiso 1 1 calc R . . C27 C 0.1586(18) 0.073(3) 0.7234(16) 0.123(10) Uani 1 1 d . . . H27A H 0.1109 0.0912 0.7438 0.147 Uiso 1 1 calc R . . H27B H 0.1604 -0.0139 0.7178 0.147 Uiso 1 1 calc R . . C28 C 0.141(2) 0.129(4) 0.647(2) 0.180(19) Uani 1 1 d . . . H28A H 0.0883 0.0991 0.6158 0.270 Uiso 1 1 calc R . . H28B H 0.1871 0.1092 0.6257 0.270 Uiso 1 1 calc R . . H28C H 0.1381 0.2150 0.6519 0.270 Uiso 1 1 calc R . . C29 C 0.3044(16) 0.233(3) 0.9311(14) 0.099(8) Uani 1 1 d . . . H29A H 0.3456 0.2556 0.9779 0.119 Uiso 1 1 calc R . . H29B H 0.3201 0.2757 0.8909 0.119 Uiso 1 1 calc R . . C30 C 0.219(2) 0.276(3) 0.9336(15) 0.122(10) Uani 1 1 d . . . H30A H 0.1982 0.2278 0.9690 0.147 Uiso 1 1 calc R . . H30B H 0.1780 0.2679 0.8844 0.147 Uiso 1 1 calc R . . C31 C 0.2256(17) 0.408(3) 0.9579(15) 0.105(8) Uani 1 1 d . . . H31A H 0.2589 0.4152 1.0100 0.126 Uiso 1 1 calc R . . H31B H 0.2541 0.4545 0.9273 0.126 Uiso 1 1 calc R . . C32 C 0.141(2) 0.454(4) 0.9489(17) 0.177(19) Uani 1 1 d . . . H32A H 0.1436 0.5366 0.9650 0.265 Uiso 1 1 calc R . . H32B H 0.1125 0.4069 0.9787 0.265 Uiso 1 1 calc R . . H32C H 0.1087 0.4490 0.8970 0.265 Uiso 1 1 calc R . . N10 N 0.7818(10) 0.3910(14) 0.5739(8) 0.064(4) Uani 1 1 d . . . C33 C 0.8496(13) 0.4437(16) 0.6393(10) 0.067(5) Uani 1 1 d . . . H33A H 0.8222 0.5029 0.6637 0.081 Uiso 1 1 calc R . . H33B H 0.8906 0.4865 0.6193 0.081 Uiso 1 1 calc R . . C34 C 0.8990(16) 0.357(2) 0.6992(14) 0.092(7) Uani 1 1 d . . . H34A H 0.8580 0.3072 0.7151 0.111 Uiso 1 1 calc R . . H34B H 0.9324 0.3040 0.6764 0.111 Uiso 1 1 calc R . . C35 C 0.9570(18) 0.412(3) 0.7663(16) 0.119(10) Uani 1 1 d . . . H35A H 0.9957 0.4674 0.7514 0.143 Uiso 1 1 calc R . . H35B H 0.9911 0.3500 0.7976 0.143 Uiso 1 1 calc R . . C36 C 0.905(2) 0.480(3) 0.8109(16) 0.136(13) Uani 1 1 d . . . H36A H 0.9438 0.5177 0.8538 0.204 Uiso 1 1 calc R . . H36B H 0.8690 0.4243 0.8275 0.204 Uiso 1 1 calc R . . H36C H 0.8709 0.5403 0.7796 0.204 Uiso 1 1 calc R . . C37 C 0.7455(16) 0.494(2) 0.5205(14) 0.086(7) Uani 1 1 d . . . H37A H 0.7914 0.5262 0.5020 0.103 Uiso 1 1 calc R . . H37B H 0.7274 0.5569 0.5490 0.103 Uiso 1 1 calc R . . C38 C 0.6706(19) 0.463(2) 0.4531(14) 0.101(8) Uani 1 1 d . . . H38A H 0.6897 0.4093 0.4198 0.121 Uiso 1 1 calc R . . H38B H 0.6264 0.4225 0.4700 0.121 Uiso 1 1 calc R . . C39 C 0.6343(18) 0.576(3) 0.4113(17) 0.122(10) Uani 1 1 d . . . H39A H 0.6783 0.6129 0.3923 0.146 Uiso 1 1 calc R . . H39B H 0.6203 0.6317 0.4464 0.146 Uiso 1 1 calc R . . C40 C 0.5535(18) 0.557(4) 0.3448(16) 0.150(13) Uani 1 1 d . . . H40A H 0.5353 0.6327 0.3210 0.225 Uiso 1 1 calc R . . H40B H 0.5085 0.5233 0.3631 0.225 Uiso 1 1 calc R . . H40C H 0.5666 0.5024 0.3091 0.225 Uiso 1 1 calc R . . C41 C 0.8187(12) 0.2939(19) 0.5352(11) 0.065(5) Uani 1 1 d . . . H41A H 0.8374 0.2286 0.5708 0.078 Uiso 1 1 calc R . . H41B H 0.7727 0.2628 0.4943 0.078 Uiso 1 1 calc R . . C42 C 0.8912(17) 0.325(3) 0.5042(14) 0.102(8) Uani 1 1 d . . . H42A H 0.8713 0.3832 0.4641 0.123 Uiso 1 1 calc R . . H42B H 0.9355 0.3637 0.5434 0.123 Uiso 1 1 calc R . . C43 C 0.9292(15) 0.222(3) 0.4747(14) 0.106(9) Uani 1 1 d . . . H43A H 0.9453 0.1629 0.5150 0.127 Uiso 1 1 calc R . . H43B H 0.8837 0.1853 0.4355 0.127 Uiso 1 1 calc R . . C44 C 0.999(2) 0.235(5) 0.446(2) 0.19(2) Uani 1 1 d . . . H44A H 1.0139 0.1582 0.4292 0.280 Uiso 1 1 calc R . . H44B H 1.0466 0.2662 0.4842 0.280 Uiso 1 1 calc R . . H44C H 0.9845 0.2899 0.4042 0.280 Uiso 1 1 calc R . . C45 C 0.7100(12) 0.3331(19) 0.5999(11) 0.068(5) Uani 1 1 d . . . H45A H 0.6665 0.3049 0.5560 0.082 Uiso 1 1 calc R . . H45B H 0.7328 0.2631 0.6301 0.082 Uiso 1 1 calc R . . C46 C 0.6679(16) 0.413(3) 0.6446(14) 0.106(8) Uani 1 1 d . . . H46A H 0.6543 0.4905 0.6197 0.127 Uiso 1 1 calc R . . H46B H 0.7065 0.4270 0.6941 0.127 Uiso 1 1 calc R . . C47 C 0.5816(19) 0.350(3) 0.6523(16) 0.119(11) Uani 1 1 d . . . H47A H 0.5960 0.2700 0.6734 0.142 Uiso 1 1 calc R . . H47B H 0.5598 0.3958 0.6877 0.142 Uiso 1 1 calc R . . C48 C 0.5155(16) 0.339(3) 0.5846(17) 0.126(11) Uani 1 1 d . . . H48A H 0.4675 0.2976 0.5944 0.188 Uiso 1 1 calc R . . H48B H 0.5360 0.2932 0.5489 0.188 Uiso 1 1 calc R . . H48C H 0.4980 0.4172 0.5647 0.188 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 0.0694(5) 0.0804(6) 0.0532(4) 0.0057(4) 0.0207(4) 0.0031(4) Br1 0.0958(18) 0.1080(19) 0.113(2) 0.0372(16) 0.0507(16) 0.0294(15) Br2 0.120(2) 0.140(2) 0.0578(13) -0.0033(15) 0.0220(14) -0.0033(19) Br3 0.0887(17) 0.0874(17) 0.1007(17) 0.0063(13) 0.0528(14) 0.0032(12) Br4 0.0891(16) 0.0842(15) 0.0864(16) 0.0074(13) 0.0270(13) 0.0088(13) N1 0.074(11) 0.079(12) 0.071(12) -0.022(10) 0.032(10) -0.015(9) N2 0.075(11) 0.081(12) 0.053(9) 0.004(8) 0.016(9) 0.008(9) C1 0.09(2) 0.17(3) 0.083(18) -0.01(2) -0.022(16) 0.02(2) C2 0.067(17) 0.089(18) 0.15(3) -0.008(19) 0.016(18) -0.030(14) C3 0.12(3) 0.13(3) 0.15(3) 0.04(2) 0.09(3) 0.03(2) C4 0.054(12) 0.072(13) 0.072(14) 0.034(11) 0.007(11) 0.015(10) C5 0.095(15) 0.074(14) 0.058(12) 0.029(11) 0.033(11) 0.007(12) N3 0.078(14) 0.114(17) 0.084(15) 0.008(12) 0.035(12) -0.010(13) N4 0.099(13) 0.091(13) 0.054(10) -0.005(10) 0.026(9) -0.012(12) C6 0.083(14) 0.12(2) 0.057(13) -0.013(14) 0.020(11) -0.016(15) C7 0.069(14) 0.12(2) 0.096(18) -0.035(18) 0.017(13) -0.023(17) C8 0.086(16) 0.085(15) 0.055(12) 0.005(12) 0.015(12) 0.003(13) Re2 0.0606(4) 0.0649(5) 0.0467(4) -0.0026(4) 0.0118(3) 0.0032(4) Br5 0.0756(14) 0.1015(17) 0.0538(11) 0.0079(11) 0.0154(10) -0.0045(12) Br6 0.0666(13) 0.0958(17) 0.0710(13) -0.0035(12) 0.0113(10) 0.0176(12) Br7 0.0926(15) 0.0702(13) 0.0584(12) -0.0115(10) 0.0136(11) -0.0013(11) Br8 0.0895(15) 0.0815(15) 0.0696(13) 0.0099(11) 0.0271(12) -0.0009(12) N5 0.057(10) 0.113(16) 0.053(10) -0.009(10) 0.010(8) -0.013(10) N6 0.063(11) 0.094(13) 0.067(11) 0.008(10) 0.023(9) 0.017(9) C9 0.070(14) 0.083(15) 0.063(13) -0.012(11) 0.021(11) -0.003(12) C10 0.11(2) 0.065(14) 0.106(19) -0.037(14) 0.018(16) -0.011(14) C11 0.072(16) 0.11(2) 0.069(15) 0.002(14) 0.000(12) 0.019(14) C12 0.068(13) 0.075(13) 0.049(11) 0.000(10) 0.004(10) -0.018(11) N7 0.064(11) 0.125(18) 0.081(13) -0.008(14) 0.007(10) -0.021(13) N8 0.065(13) 0.105(16) 0.113(17) 0.010(14) 0.007(12) -0.001(12) C13 0.057(12) 0.099(16) 0.036(10) -0.002(9) 0.009(9) 0.003(10) C14 0.059(15) 0.097(19) 0.13(2) 0.027(18) 0.023(16) 0.009(14) C15 0.063(15) 0.092(17) 0.13(2) 0.009(17) 0.035(15) 0.014(13) C16 0.090(17) 0.082(16) 0.078(15) -0.019(13) 0.028(13) -0.007(13) N9 0.107(15) 0.090(15) 0.067(12) 0.008(10) 0.011(11) -0.014(11) C17 0.11(2) 0.10(2) 0.12(2) 0.025(17) 0.008(18) 0.009(16) C18 0.11(2) 0.35(7) 0.10(2) 0.04(4) 0.02(2) -0.03(4) C19 0.15(4) 0.28(7) 0.12(3) 0.00(4) 0.00(3) -0.01(4) C20 0.27(7) 0.16(5) 0.23(6) 0.01(4) 0.07(5) -0.04(5) C25 0.077(15) 0.113(19) 0.077(14) -0.006(15) 0.015(12) 0.002(15) C26 0.10(2) 0.093(18) 0.12(2) -0.020(16) 0.040(17) -0.006(15) C27 0.12(2) 0.13(2) 0.10(2) 0.00(2) -0.010(17) -0.03(2) C28 0.14(3) 0.22(5) 0.15(3) -0.11(3) 0.01(3) 0.01(3) C29 0.082(17) 0.13(2) 0.074(16) -0.025(15) 0.000(13) -0.004(16) C30 0.15(3) 0.15(3) 0.067(16) 0.009(18) 0.028(17) 0.02(2) C31 0.093(18) 0.14(2) 0.087(16) 0.025(19) 0.032(14) -0.013(18) C32 0.19(4) 0.26(5) 0.09(2) 0.04(3) 0.05(2) 0.09(4) N10 0.077(11) 0.067(11) 0.051(9) -0.004(7) 0.024(8) 0.011(8) C33 0.087(14) 0.044(11) 0.062(11) -0.009(9) 0.005(10) -0.009(9) C34 0.089(17) 0.088(16) 0.089(17) -0.017(14) 0.006(14) -0.004(13) C35 0.10(2) 0.11(2) 0.13(2) 0.02(2) -0.001(18) 0.02(2) C36 0.16(3) 0.16(3) 0.11(2) 0.03(2) 0.08(2) 0.04(2) C37 0.088(17) 0.083(15) 0.087(16) 0.012(13) 0.023(14) 0.016(13) C38 0.15(3) 0.077(16) 0.085(17) 0.005(13) 0.045(18) 0.017(15) C39 0.098(19) 0.11(2) 0.14(2) 0.02(2) 0.002(17) 0.036(18) C40 0.11(2) 0.17(3) 0.13(2) 0.03(3) -0.037(19) -0.01(3) C41 0.066(12) 0.066(12) 0.060(12) -0.006(10) 0.010(10) -0.008(10) C42 0.097(19) 0.13(2) 0.077(16) 0.008(16) 0.023(14) 0.008(18) C43 0.082(16) 0.17(3) 0.065(15) -0.006(16) 0.014(13) 0.035(18) C44 0.15(3) 0.28(6) 0.16(3) 0.03(4) 0.10(3) 0.05(4) C45 0.067(13) 0.074(13) 0.068(12) -0.019(10) 0.024(10) -0.014(10) C46 0.104(18) 0.13(2) 0.097(17) -0.014(19) 0.056(15) 0.02(2) C47 0.13(2) 0.16(3) 0.09(2) -0.025(19) 0.06(2) 0.02(2) C48 0.058(15) 0.18(3) 0.12(2) 0.00(2) -0.001(16) -0.007(18) _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 N1 2.076(16) . ? Re1 N2 2.076(16) . ? Re1 Br1 2.514(3) . ? Re1 Br2 2.523(3) . ? Re1 Br3 2.531(3) . ? Re1 Br4 2.536(3) . ? N1 C4 1.33(2) . ? N1 C1 1.44(3) . ? N2 C5 1.32(2) . ? N2 C6 1.38(3) . ? C1 C2 1.36(4) . ? C2 C3 1.39(4) . ? C3 N3 1.20(4) . ? C4 N3 1.30(3) . ? C4 C5 1.46(3) . ? C5 N4 1.35(2) . ? N4 C8 1.34(3) . ? C6 C7 1.35(3) . ? C7 C8 1.32(3) . ? Re2 N5 2.072(17) . ? Re2 N6 2.090(16) . ? Re2 Br6 2.519(2) . ? Re2 Br5 2.520(2) . ? Re2 Br8 2.521(2) . ? Re2 Br7 2.540(2) . ? N5 C9 1.33(3) . ? N5 C12 1.39(3) . ? N6 C13 1.32(2) . ? N6 C16 1.38(3) . ? C9 C10 1.40(3) . ? C10 C11 1.36(3) . ? C11 N7 1.36(3) . ? C12 N7 1.32(3) . ? C12 C13 1.45(3) . ? N8 C13 1.31(3) . ? N8 C14 1.34(3) . ? C14 C15 1.33(4) . ? C15 C16 1.37(3) . ? N9 C29 1.49(3) . ? N9 C25 1.55(3) . ? N9 C17 1.56(3) . ? N9 C21 1.69(2) . ? C17 C18 1.42(4) . ? C18 C19 1.60(6) . ? C19 C20 1.45(6) . ? C21 C22 1.2681 . ? C22 C23 1.6591 . ? C23 C24 1.2411 . ? C25 C26 1.57(3) . ? C26 C27 1.45(3) . ? C27 C28 1.49(4) . ? C29 C30 1.49(4) . ? C30 C31 1.53(5) . ? C31 C32 1.44(4) . ? N10 C41 1.51(2) . ? N10 C33 1.51(2) . ? N10 C37 1.52(3) . ? N10 C45 1.52(2) . ? C33 C34 1.52(3) . ? C34 C35 1.47(3) . ? C35 C36 1.53(4) . ? C37 C38 1.52(4) . ? C38 C39 1.50(4) . ? C39 C40 1.55(3) . ? C41 C42 1.48(3) . ? C42 C43 1.48(4) . ? C43 C44 1.38(3) . ? C45 C46 1.50(3) . ? C46 C47 1.61(4) . ? C47 C48 1.41(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 Re1 N2 74.9(7) . . ? N1 Re1 Br1 92.6(5) . . ? N2 Re1 Br1 90.5(5) . . ? N1 Re1 Br2 97.0(5) . . ? N2 Re1 Br2 171.8(5) . . ? Br1 Re1 Br2 91.21(11) . . ? N1 Re1 Br3 169.1(5) . . ? N2 Re1 Br3 94.7(5) . . ? Br1 Re1 Br3 90.82(9) . . ? Br2 Re1 Br3 93.32(10) . . ? N1 Re1 Br4 84.9(5) . . ? N2 Re1 Br4 88.3(5) . . ? Br1 Re1 Br4 177.39(9) . . ? Br2 Re1 Br4 89.61(10) . . ? Br3 Re1 Br4 91.61(9) . . ? C4 N1 C1 112(2) . . ? C4 N1 Re1 117.8(14) . . ? C1 N1 Re1 130.0(18) . . ? C5 N2 C6 114.7(17) . . ? C5 N2 Re1 118.1(15) . . ? C6 N2 Re1 127.2(14) . . ? C2 C1 N1 119(3) . . ? C1 C2 C3 116(3) . . ? N3 C3 C2 126(3) . . ? N3 C4 N1 129(2) . . ? N3 C4 C5 117(2) . . ? N1 C4 C5 113.8(18) . . ? N2 C5 N4 124(2) . . ? N2 C5 C4 113.8(17) . . ? N4 C5 C4 122.1(19) . . ? C3 N3 C4 117(3) . . ? C8 N4 C5 119.3(19) . . ? C7 C6 N2 122(2) . . ? C8 C7 C6 120(2) . . ? C7 C8 N4 120(2) . . ? N5 Re2 N6 75.7(8) . . ? N5 Re2 Br6 94.8(5) . . ? N6 Re2 Br6 170.3(5) . . ? N5 Re2 Br5 88.4(5) . . ? N6 Re2 Br5 89.4(5) . . ? Br6 Re2 Br5 92.32(8) . . ? N5 Re2 Br8 92.5(5) . . ? N6 Re2 Br8 86.2(5) . . ? Br6 Re2 Br8 92.37(8) . . ? Br5 Re2 Br8 175.14(9) . . ? N5 Re2 Br7 172.3(6) . . ? N6 Re2 Br7 97.0(5) . . ? Br6 Re2 Br7 92.60(8) . . ? Br5 Re2 Br7 89.12(8) . . ? Br8 Re2 Br7 89.40(8) . . ? C9 N5 C12 117.1(18) . . ? C9 N5 Re2 127.0(15) . . ? C12 N5 Re2 115.9(15) . . ? C13 N6 C16 117.8(18) . . ? C13 N6 Re2 119.2(14) . . ? C16 N6 Re2 123.0(15) . . ? N5 C9 C10 121(2) . . ? C11 C10 C9 120(2) . . ? C10 C11 N7 119(2) . . ? N7 C12 N5 123(2) . . ? N7 C12 C13 122(2) . . ? N5 C12 C13 115.0(18) . . ? C12 N7 C11 120(2) . . ? C13 N8 C14 117(2) . . ? N8 C13 N6 125(2) . . ? N8 C13 C12 120(2) . . ? N6 C13 C12 113.0(18) . . ? C15 C14 N8 122(2) . . ? C14 C15 C16 120(3) . . ? C15 C16 N6 118(2) . . ? C29 N9 C25 115(2) . . ? C29 N9 C17 112(2) . . ? C25 N9 C17 99.5(17) . . ? C29 N9 C21 110.6(17) . . ? C25 N9 C21 99.3(14) . . ? C17 N9 C21 119.2(17) . . ? C18 C17 N9 118(3) . . ? C17 C18 C19 111(4) . . ? C20 C19 C18 110(5) . . ? C22 C21 N9 112.4(7) . . ? C21 C22 C23 114.0 . . ? C24 C23 C22 116.1 . . ? N9 C25 C26 112.1(19) . . ? C27 C26 C25 108(2) . . ? C26 C27 C28 115(3) . . ? C30 C29 N9 116(3) . . ? C29 C30 C31 109(3) . . ? C32 C31 C30 108(3) . . ? C41 N10 C33 111.1(15) . . ? C41 N10 C37 111.2(15) . . ? C33 N10 C37 107.4(16) . . ? C41 N10 C45 106.7(15) . . ? C33 N10 C45 111.3(14) . . ? C37 N10 C45 109.2(17) . . ? N10 C33 C34 117.5(16) . . ? C35 C34 C33 116(2) . . ? C34 C35 C36 110(2) . . ? N10 C37 C38 117(2) . . ? C39 C38 C37 111(2) . . ? C38 C39 C40 115(3) . . ? C42 C41 N10 118.5(19) . . ? C43 C42 C41 115(2) . . ? C44 C43 C42 122(3) . . ? C46 C45 N10 115.4(18) . . ? C45 C46 C47 109(2) . . ? C48 C47 C46 115(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.485 _refine_diff_density_min -1.762 _refine_diff_density_rms 0.136