# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_2 _database_code_depnum_ccdc_archive 'CCDC 610271' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 Br N6 O3 Re' _chemical_formula_weight 648.54 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 11.9161(18) _cell_length_b 11.8438(18) _cell_length_c 15.996(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2257.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5141 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 7.184 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.2901 _exptl_absorpt_correction_T_max 0.5336 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.543663 ; _diffrn_ambient_temperature 100(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 19193 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2886 _reflns_number_gt 2586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. Hydrogen atoms were placed in ideal positions and were refined isotropically. ; _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^)+(0.0154P)^2^+4.9420P] 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 2886 _refine_ls_number_parameters 158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.47841(4) 0.2500 0.37506(3) 0.01683(11) Uani 1 2 d S . . C1 C 0.8569(3) 0.0410(3) 0.6844(2) 0.0161(7) Uani 1 1 d . . . C2 C 0.7554(3) -0.0026(3) 0.6544(2) 0.0174(7) Uani 1 1 d . . . H2 H 0.7175 -0.0677 0.6746 0.021 Uiso 1 1 calc R . . C3 C 0.7209(3) 0.0664(3) 0.5902(2) 0.0142(7) Uani 1 1 d . . . C4 C 1.0710(4) 0.2500 0.4439(3) 0.0177(10) Uani 1 2 d S . . C5 C 1.0079(4) 0.2500 0.3696(3) 0.0184(11) Uani 1 2 d S . . H5 H 1.0372 0.2500 0.3143 0.022 Uiso 1 2 calc SR . . C6 C 0.8970(4) 0.2500 0.3911(3) 0.0145(10) Uani 1 2 d S . . C7 C 0.9289(3) -0.0022(3) 0.7534(2) 0.0218(8) Uani 1 1 d . . . H7A H 1.0067 -0.0073 0.7341 0.033 Uiso 1 1 calc R . . H7B H 0.9026 -0.0772 0.7705 0.033 Uiso 1 1 calc R . . H7C H 0.9246 0.0495 0.8012 0.033 Uiso 1 1 calc R . . C8 C 0.6223(3) 0.0564(3) 0.5330(2) 0.0192(7) Uani 1 1 d . . . H8A H 0.5770 0.1254 0.5364 0.029 Uiso 1 1 calc R . . H8B H 0.5766 -0.0086 0.5496 0.029 Uiso 1 1 calc R . . H8C H 0.6486 0.0460 0.4755 0.029 Uiso 1 1 calc R . . C9 C 1.1945(4) 0.2500 0.4553(3) 0.0219(11) Uani 1 2 d S . . H9A H 1.2183 0.3230 0.4779 0.033 Uiso 0.50 1 calc PR . . H9B H 1.2310 0.2372 0.4012 0.033 Uiso 0.50 1 calc PR . . H9C H 1.2156 0.1897 0.4942 0.033 Uiso 0.50 1 calc PR . . C10 C 0.7936(5) 0.2500 0.3379(3) 0.0248(12) Uani 1 2 d S . . H10A H 0.7406 0.1936 0.3591 0.037 Uiso 0.50 1 calc PR . . H10B H 0.8139 0.2315 0.2801 0.037 Uiso 0.50 1 calc PR . . H10C H 0.7587 0.3249 0.3396 0.037 Uiso 0.50 1 calc PR . . C11 C 0.7989(4) 0.2500 0.5324(3) 0.0118(9) Uani 1 2 d S . . H11 H 0.7286 0.2500 0.4982 0.014 Uiso 1 2 calc SR . . C12 C 1.0408(4) 0.2500 0.7635(3) 0.0173(10) Uani 1 2 d S . . C13 C 1.1384(3) 0.1347(3) 0.6394(2) 0.0217(8) Uani 1 1 d . . . N1 N 0.8843(2) 0.1336(2) 0.64138(17) 0.0132(6) Uani 1 1 d . . . N2 N 0.7999(2) 0.1492(2) 0.58376(17) 0.0128(6) Uani 1 1 d . . . N3 N 0.9997(3) 0.2500 0.5095(3) 0.0153(9) Uani 1 2 d S . . N4 N 0.8940(3) 0.2500 0.4763(2) 0.0139(8) Uani 1 2 d S . . O1 O 1.0540(4) 0.2500 0.8345(2) 0.0307(10) Uani 1 2 d S . . O2 O 1.2042(2) 0.0638(3) 0.63638(18) 0.0341(7) Uani 1 1 d . . . Re1 Re 1.025220(16) 0.2500 0.644343(12) 0.01318(6) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0164(2) 0.0167(2) 0.0174(2) 0.000 0.00223(19) 0.000 C1 0.0192(17) 0.0146(16) 0.0144(17) 0.0000(13) 0.0009(14) -0.0005(14) C2 0.0198(17) 0.0135(17) 0.0188(19) 0.0022(13) 0.0030(14) -0.0024(13) C3 0.0149(16) 0.0128(16) 0.0150(17) -0.0019(13) 0.0023(14) -0.0006(13) C4 0.018(2) 0.016(2) 0.019(3) 0.000 0.004(2) 0.000 C5 0.022(3) 0.020(2) 0.013(3) 0.000 0.004(2) 0.000 C6 0.017(2) 0.013(2) 0.013(2) 0.000 -0.0020(19) 0.000 C7 0.026(2) 0.0188(18) 0.0210(19) 0.0051(15) -0.0026(16) 0.0008(15) C8 0.0164(17) 0.0203(18) 0.0209(18) -0.0013(14) -0.0028(15) -0.0051(14) C9 0.014(2) 0.026(3) 0.026(3) 0.000 0.009(2) 0.000 C10 0.029(3) 0.035(3) 0.011(3) 0.000 -0.001(2) 0.000 C11 0.014(2) 0.014(2) 0.007(2) 0.000 -0.0043(18) 0.000 C12 0.012(2) 0.020(2) 0.021(3) 0.000 -0.002(2) 0.000 C13 0.0135(17) 0.030(2) 0.0212(19) 0.0007(16) -0.0025(15) 0.0028(15) N1 0.0105(13) 0.0141(13) 0.0151(14) -0.0001(11) -0.0030(11) 0.0019(11) N2 0.0117(13) 0.0129(14) 0.0137(14) 0.0011(11) -0.0026(11) 0.0005(11) N3 0.0065(19) 0.015(2) 0.024(2) 0.000 -0.0050(16) 0.000 N4 0.012(2) 0.017(2) 0.012(2) 0.000 0.0007(16) 0.000 O1 0.042(3) 0.030(2) 0.020(2) 0.000 -0.0105(17) 0.000 O2 0.0293(16) 0.0428(18) 0.0301(16) 0.0067(14) 0.0009(13) 0.0186(14) Re1 0.01020(10) 0.01516(10) 0.01418(10) 0.000 -0.00225(8) 0.000 _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 1.337(4) . ? C1 C2 1.400(5) . ? C1 C7 1.488(5) . ? C2 C3 1.375(5) . ? C3 N2 1.364(4) . ? C3 C8 1.494(5) . ? C4 N3 1.349(6) . ? C4 C5 1.407(7) . ? C4 C9 1.483(7) . ? C5 C6 1.366(7) . ? C6 N4 1.363(6) . ? C6 C10 1.498(7) . ? C11 N4 1.446(6) . ? C11 N2 1.449(4) 7_565 ? C11 N2 1.449(4) . ? C12 O1 1.147(6) . ? C12 Re1 1.914(5) . ? C13 O2 1.150(4) . ? C13 Re1 1.921(4) . ? N1 N2 1.377(4) . ? N1 Re1 2.173(3) . ? N3 N4 1.366(5) . ? N3 Re1 2.179(4) . ? Re1 C13 1.921(4) 7_565 ? Re1 N1 2.173(3) 7_565 ? 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 109.7(3) . . ? N1 C1 C7 121.5(3) . . ? C2 C1 C7 128.7(3) . . ? C3 C2 C1 107.2(3) . . ? N2 C3 C2 106.1(3) . . ? N2 C3 C8 123.6(3) . . ? C2 C3 C8 130.2(3) . . ? N3 C4 C5 108.7(4) . . ? N3 C4 C9 122.0(5) . . ? C5 C4 C9 129.3(5) . . ? C6 C5 C4 107.7(4) . . ? N4 C6 C5 106.1(4) . . ? N4 C6 C10 123.2(4) . . ? C5 C6 C10 130.7(5) . . ? N4 C11 N2 110.2(2) . 7_565 ? N4 C11 N2 110.2(2) . . ? N2 C11 N2 110.9(4) 7_565 . ? O1 C12 Re1 177.7(4) . . ? O2 C13 Re1 178.4(3) . . ? C1 N1 N2 106.0(3) . . ? C1 N1 Re1 134.3(2) . . ? N2 N1 Re1 119.6(2) . . ? C3 N2 N1 110.9(3) . . ? C3 N2 C11 129.1(3) . . ? N1 N2 C11 119.7(3) . . ? C4 N3 N4 106.2(4) . . ? C4 N3 Re1 133.0(3) . . ? N4 N3 Re1 120.9(3) . . ? C6 N4 N3 111.4(4) . . ? C6 N4 C11 129.8(4) . . ? N3 N4 C11 118.8(4) . . ? C12 Re1 C13 88.44(15) . 7_565 ? C12 Re1 C13 88.44(15) . . ? C13 Re1 C13 90.6(2) 7_565 . ? C12 Re1 N1 95.55(13) . . ? C13 Re1 N1 173.02(13) 7_565 . ? C13 Re1 N1 95.22(13) . . ? C12 Re1 N1 95.55(13) . 7_565 ? C13 Re1 N1 95.22(13) 7_565 7_565 ? C13 Re1 N1 173.02(13) . 7_565 ? N1 Re1 N1 78.73(14) . 7_565 ? C12 Re1 N3 177.55(17) . . ? C13 Re1 N3 93.28(13) 7_565 . ? C13 Re1 N3 93.28(13) . . ? N1 Re1 N3 82.56(11) . . ? N1 Re1 N3 82.56(11) 7_565 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.417 _refine_diff_density_min -1.867 _refine_diff_density_rms 0.134 data_3 _database_code_depnum_ccdc_archive 'CCDC 610272' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H9 N6 O6 Re S' _chemical_formula_weight 563.52 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' S S 0.1246 0.1234 '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)/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 8.8316(17) _cell_length_b 8.9876(17) _cell_length_c 20.941(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.909(3) _cell_angle_gamma 90.00 _cell_volume 1650.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2808 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.34 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 7.539 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.3015 _exptl_absorpt_correction_T_max 0.5194 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.580541 ; _diffrn_ambient_temperature 100(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 14220 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3962 _reflns_number_gt 3348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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.Hydrogen atoms were placed in ideal positions and were refined isotropically. ; _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^)+(0.0150P)^2^+8.2948P] 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 3962 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0961(7) 1.1360(7) 0.0717(3) 0.0119(12) Uani 1 1 d . . . H1 H 1.0685 1.2382 0.0699 0.014 Uiso 1 1 calc R . . C2 C 1.2068(7) 1.0714(7) 0.0378(3) 0.0138(13) Uani 1 1 d . . . H2 H 1.2673 1.1208 0.0098 0.017 Uiso 1 1 calc R . . C3 C 1.2104(7) 0.9238(7) 0.0529(3) 0.0141(13) Uani 1 1 d . . . H3 H 1.2737 0.8501 0.0373 0.017 Uiso 1 1 calc R . . C4 C 1.0641(7) 0.8532(7) 0.2874(3) 0.0158(13) Uani 1 1 d . . . H4 H 1.0429 0.9156 0.3219 0.019 Uiso 1 1 calc R . . C5 C 1.1327(7) 0.7128(7) 0.2946(3) 0.0154(13) Uani 1 1 d . . . H5 H 1.1655 0.6630 0.3339 0.018 Uiso 1 1 calc R . . C6 C 1.1427(7) 0.6629(7) 0.2348(3) 0.0139(13) Uani 1 1 d . . . H6 H 1.1835 0.5697 0.2240 0.017 Uiso 1 1 calc R . . C7 C 0.6518(7) 0.7991(7) 0.1109(3) 0.0145(13) Uani 1 1 d . . . H7 H 0.5609 0.8464 0.1203 0.017 Uiso 1 1 calc R . . C8 C 0.6557(7) 0.6681(7) 0.0768(3) 0.0134(13) Uani 1 1 d . . . H8 H 0.5705 0.6108 0.0590 0.016 Uiso 1 1 calc R . . C9 C 0.8054(7) 0.6374(7) 0.0736(3) 0.0141(13) Uani 1 1 d . . . H9 H 0.8451 0.5536 0.0535 0.017 Uiso 1 1 calc R . . C10 C 1.0532(6) 0.7629(7) 0.1227(3) 0.0101(12) Uani 1 1 d . . . C11 C 0.9798(6) 1.2198(7) 0.2234(3) 0.0122(12) Uani 1 1 d . . . C12 C 0.7427(7) 1.1845(7) 0.1284(3) 0.0178(14) Uani 1 1 d . . . C13 C 0.7518(7) 1.0474(7) 0.2456(3) 0.0163(13) Uani 1 1 d . . . N1 N 1.0352(6) 1.0334(5) 0.1069(2) 0.0134(11) Uani 1 1 d . . . N2 N 1.1056(6) 0.9024(5) 0.0948(2) 0.0114(10) Uani 1 1 d . . . N3 N 1.0327(5) 0.8865(5) 0.2255(2) 0.0108(10) Uani 1 1 d . . . N4 N 1.0850(5) 0.7679(5) 0.1928(2) 0.0099(10) Uani 1 1 d . . . N5 N 0.7923(5) 0.8510(6) 0.1290(2) 0.0107(10) Uani 1 1 d . . . N6 N 0.8879(5) 0.7497(5) 0.1050(2) 0.0092(10) Uani 1 1 d . . . O1 O 1.3149(5) 0.6341(5) 0.1145(2) 0.0157(9) Uani 1 1 d . . . O2 O 1.1200(5) 0.6222(4) 0.02169(19) 0.0137(9) Uani 1 1 d . . . O3 O 1.0941(5) 0.4747(4) 0.1176(2) 0.0146(9) Uani 1 1 d . . . O4 O 1.0375(5) 1.3156(5) 0.2529(2) 0.0195(10) Uani 1 1 d . . . O5 O 0.6584(6) 1.2612(6) 0.0980(2) 0.0311(12) Uani 1 1 d . . . O6 O 0.6780(5) 1.0466(5) 0.2874(2) 0.0215(10) Uani 1 1 d . . . Re1 Re 0.88032(3) 1.05183(3) 0.178051(11) 0.01101(8) Uani 1 1 d . . . S1 S 1.15820(17) 0.60196(16) 0.08997(7) 0.0115(3) 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 0.017(3) 0.007(3) 0.011(3) 0.000(2) -0.002(2) -0.002(2) C2 0.014(3) 0.014(3) 0.013(3) 0.000(2) 0.003(2) -0.005(2) C3 0.016(3) 0.015(3) 0.012(3) -0.001(2) 0.007(2) 0.000(2) C4 0.015(3) 0.019(3) 0.013(3) -0.003(3) 0.002(2) -0.004(3) C5 0.020(3) 0.013(3) 0.013(3) 0.002(2) 0.002(3) -0.003(3) C6 0.013(3) 0.013(3) 0.015(3) -0.001(2) -0.001(2) -0.004(2) C7 0.015(3) 0.014(3) 0.015(3) 0.003(2) 0.005(3) 0.004(2) C8 0.013(3) 0.013(3) 0.014(3) 0.005(2) 0.002(2) -0.002(2) C9 0.017(3) 0.013(3) 0.012(3) -0.003(2) 0.001(2) 0.000(3) C10 0.009(3) 0.012(3) 0.010(3) 0.002(2) 0.002(2) 0.000(2) C11 0.006(3) 0.015(3) 0.017(3) 0.000(3) 0.007(2) 0.003(2) C12 0.017(3) 0.012(3) 0.027(4) -0.004(3) 0.011(3) 0.000(3) C13 0.015(3) 0.012(3) 0.021(3) -0.005(3) 0.001(3) -0.001(3) N1 0.016(3) 0.009(3) 0.017(3) 0.000(2) 0.006(2) 0.003(2) N2 0.017(3) 0.009(2) 0.009(3) 0.0002(19) 0.003(2) -0.002(2) N3 0.011(2) 0.009(2) 0.013(3) 0.000(2) 0.004(2) -0.002(2) N4 0.010(2) 0.010(3) 0.009(2) -0.0015(19) 0.0027(19) -0.001(2) N5 0.007(2) 0.011(3) 0.014(3) 0.001(2) 0.005(2) 0.002(2) N6 0.010(2) 0.006(2) 0.011(3) -0.0019(19) 0.0019(19) -0.0022(19) O1 0.012(2) 0.014(2) 0.020(2) 0.0003(19) 0.0017(18) 0.0025(18) O2 0.024(2) 0.002(2) 0.015(2) -0.0002(16) 0.0023(18) 0.0054(17) O3 0.017(2) 0.010(2) 0.017(2) 0.0017(17) 0.0040(18) 0.0009(17) O4 0.019(2) 0.014(2) 0.026(3) -0.005(2) 0.003(2) 0.0008(19) O5 0.032(3) 0.032(3) 0.030(3) 0.003(2) 0.005(2) 0.010(2) O6 0.016(2) 0.028(3) 0.022(3) -0.005(2) 0.008(2) -0.003(2) Re1 0.01281(12) 0.00897(12) 0.01184(13) -0.00125(10) 0.00398(8) 0.00187(10) S1 0.0121(7) 0.0081(7) 0.0149(8) -0.0004(6) 0.0046(6) 0.0019(6) _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 1.333(7) . ? C1 C2 1.401(8) . ? C2 C3 1.364(8) . ? C3 N2 1.363(8) . ? C4 N3 1.328(8) . ? C4 C5 1.400(9) . ? C5 C6 1.343(8) . ? C6 N4 1.348(8) . ? C7 N5 1.337(8) . ? C7 C8 1.379(9) . ? C8 C9 1.361(8) . ? C9 N6 1.366(7) . ? C10 N4 1.462(7) . ? C10 N6 1.467(7) . ? C10 N2 1.480(7) . ? C10 S1 1.890(6) . ? C11 O4 1.143(7) . ? C11 Re1 1.937(6) . ? C12 O5 1.149(8) . ? C12 Re1 1.918(7) . ? C13 O6 1.152(8) . ? C13 Re1 1.918(7) . ? N1 N2 1.370(7) . ? N1 Re1 2.147(5) . ? N3 N4 1.376(7) . ? N3 Re1 2.165(5) . ? N5 N6 1.378(6) . ? N5 Re1 2.174(5) . ? O1 S1 1.446(4) . ? O2 S1 1.441(4) . ? O3 S1 1.430(4) . ? 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 110.3(5) . . ? C3 C2 C1 106.5(5) . . ? N2 C3 C2 106.8(5) . . ? N3 C4 C5 110.2(6) . . ? C6 C5 C4 106.0(6) . . ? C5 C6 N4 108.2(6) . . ? N5 C7 C8 111.4(5) . . ? C9 C8 C7 106.5(6) . . ? C8 C9 N6 107.0(5) . . ? N4 C10 N6 108.8(4) . . ? N4 C10 N2 109.8(5) . . ? N6 C10 N2 108.5(5) . . ? N4 C10 S1 110.1(4) . . ? N6 C10 S1 111.3(4) . . ? N2 C10 S1 108.4(4) . . ? O4 C11 Re1 176.6(5) . . ? O5 C12 Re1 178.4(6) . . ? O6 C13 Re1 178.0(5) . . ? C1 N1 N2 105.7(5) . . ? C1 N1 Re1 131.6(4) . . ? N2 N1 Re1 122.4(4) . . ? C3 N2 N1 110.8(5) . . ? C3 N2 C10 129.9(5) . . ? N1 N2 C10 119.0(5) . . ? C4 N3 N4 105.6(5) . . ? C4 N3 Re1 130.4(4) . . ? N4 N3 Re1 122.1(4) . . ? C6 N4 N3 109.9(5) . . ? C6 N4 C10 130.2(5) . . ? N3 N4 C10 119.2(5) . . ? C7 N5 N6 104.7(5) . . ? C7 N5 Re1 133.7(4) . . ? N6 N5 Re1 121.4(3) . . ? C9 N6 N5 110.4(5) . . ? C9 N6 C10 129.6(5) . . ? N5 N6 C10 119.3(4) . . ? C12 Re1 C13 91.1(3) . . ? C12 Re1 C11 90.1(3) . . ? C13 Re1 C11 85.9(3) . . ? C12 Re1 N1 95.0(2) . . ? C13 Re1 N1 173.5(2) . . ? C11 Re1 N1 96.4(2) . . ? C12 Re1 N3 174.0(2) . . ? C13 Re1 N3 92.2(2) . . ? C11 Re1 N3 95.2(2) . . ? N1 Re1 N3 81.53(19) . . ? C12 Re1 N5 95.3(2) . . ? C13 Re1 N5 97.0(2) . . ? C11 Re1 N5 173.8(2) . . ? N1 Re1 N5 80.21(18) . . ? N3 Re1 N5 79.27(18) . . ? O3 S1 O2 116.5(3) . . ? O3 S1 O1 115.1(3) . . ? O2 S1 O1 115.3(3) . . ? O3 S1 C10 103.3(3) . . ? O2 S1 C10 101.3(2) . . ? O1 S1 C10 102.0(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.114 _refine_diff_density_min -2.187 _refine_diff_density_rms 0.211 data_4 _database_code_depnum_ccdc_archive 'CCDC 610273' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H19 Br N3 O4 Re' _chemical_formula_weight 499.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7916(9) _cell_length_b 13.0578(16) _cell_length_c 17.449(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.273(2) _cell_angle_gamma 90.00 _cell_volume 1531.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4858 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 10.554 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.0515 _exptl_absorpt_correction_T_max 0.2267 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.227060 ; _diffrn_ambient_temperature 100(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 12780 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3596 _reflns_number_gt 2899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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.Hydrogen atoms were placed in ideal positions on pyrrole and phenyl carbons and were refined isotropically. ; _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^)+(0.1019P)^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 3596 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.85234(14) 0.41102(7) 0.32931(6) 0.0319(3) Uani 1 1 d . . . C1 C 0.6554(14) 0.7729(6) 0.1241(6) 0.0179(18) Uani 1 1 d . . . H1C H 0.7725 0.8068 0.1073 0.022 Uiso 1 1 calc R . . H1D H 0.5420 0.7816 0.0821 0.022 Uiso 1 1 calc R . . C2 C 0.9024(13) 0.6390(6) 0.1822(5) 0.0170(17) Uani 1 1 d . . . H2C H 0.9102 0.5667 0.1994 0.020 Uiso 1 1 calc R . . H2D H 1.0061 0.6496 0.1485 0.020 Uiso 1 1 calc R . . C3 C 0.5332(12) 0.6047(6) 0.1726(5) 0.0196(18) Uani 1 1 d . . . H3C H 0.4037 0.6359 0.1516 0.024 Uiso 1 1 calc R . . H3D H 0.5278 0.5314 0.1582 0.024 Uiso 1 1 calc R . . C4 C 0.6999(12) 0.6575(6) 0.1349(5) 0.0151(17) Uani 1 1 d . . . C5 C 0.6993(14) 0.6100(7) 0.0545(5) 0.026(2) Uani 1 1 d . . . H5A H 0.7824 0.6514 0.0250 0.038 Uiso 1 1 calc R . . H5B H 0.5628 0.6081 0.0272 0.038 Uiso 1 1 calc R . . H5C H 0.7524 0.5402 0.0601 0.038 Uiso 1 1 calc R . . C6 C 0.8203(12) 0.8783(6) 0.3551(5) 0.0173(18) Uani 1 1 d . . . C7 C 0.4603(13) 0.7958(6) 0.3539(5) 0.0189(18) Uani 1 1 d . . . C8 C 0.7874(12) 0.6871(6) 0.4066(5) 0.0145(17) Uani 1 1 d . . . C9 C 0.3111(14) 0.5572(8) 0.4244(6) 0.029(2) Uani 1 1 d . . . H9A H 0.4527 0.5396 0.4300 0.044 Uiso 1 1 calc R . . H9B H 0.2413 0.5077 0.4530 0.044 Uiso 1 1 calc R . . H9C H 0.2957 0.6261 0.4450 0.044 Uiso 1 1 calc R . . N1 N 0.6071(10) 0.8255(5) 0.1951(4) 0.0148(14) Uani 1 1 d . . . H1A H 0.4715 0.8348 0.1888 0.018 Uiso 1 1 calc R . . H1B H 0.6637 0.8896 0.1964 0.018 Uiso 1 1 calc R . . N2 N 0.9467(10) 0.7068(5) 0.2517(4) 0.0141(14) Uani 1 1 d . . . H2A H 1.0080 0.7649 0.2369 0.017 Uiso 1 1 calc R . . H2B H 1.0374 0.6734 0.2874 0.017 Uiso 1 1 calc R . . N3 N 0.5624(9) 0.6135(5) 0.2572(4) 0.0119(13) Uani 1 1 d . . . H3A H 0.6414 0.5596 0.2768 0.014 Uiso 1 1 calc R . . H3B H 0.4405 0.6047 0.2734 0.014 Uiso 1 1 calc R . . O1 O 0.8910(9) 0.9501(4) 0.3850(4) 0.0235(14) Uani 1 1 d . . . O2 O 0.3193(9) 0.8183(5) 0.3796(4) 0.0248(14) Uani 1 1 d . . . O3 O 0.8475(10) 0.6483(4) 0.4640(4) 0.0256(14) Uani 1 1 d . . . O4 O 0.2287(9) 0.5547(5) 0.3443(4) 0.0233(14) Uani 1 1 d . . . H4 H 0.1423 0.5084 0.3369 0.035 Uiso 1 1 calc R . . Re1 Re 0.69510(5) 0.75544(2) 0.311137(19) 0.01239(16) 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 Br1 0.0278(5) 0.0217(5) 0.0435(7) -0.0019(4) -0.0037(4) 0.0001(4) C1 0.020(4) 0.013(3) 0.019(5) -0.001(4) -0.003(4) 0.000(3) C2 0.026(4) 0.013(3) 0.011(5) 0.003(3) -0.001(3) 0.001(3) C3 0.020(4) 0.016(4) 0.021(5) 0.000(3) -0.003(4) -0.003(3) C4 0.020(4) 0.013(4) 0.012(4) -0.001(3) 0.002(3) -0.002(3) C5 0.038(5) 0.017(4) 0.019(5) -0.003(3) -0.008(4) 0.007(4) C6 0.016(4) 0.016(4) 0.021(5) 0.009(3) 0.005(3) 0.002(3) C7 0.027(5) 0.012(4) 0.018(5) 0.002(3) 0.004(4) -0.005(4) C8 0.018(4) 0.013(3) 0.014(5) -0.007(3) 0.005(3) -0.003(3) C9 0.036(6) 0.032(5) 0.018(5) 0.016(4) -0.004(4) -0.002(4) N1 0.015(3) 0.016(3) 0.012(4) 0.003(3) -0.003(3) 0.001(3) N2 0.013(3) 0.013(3) 0.016(4) 0.001(3) 0.002(3) 0.002(3) N3 0.011(3) 0.010(3) 0.014(4) 0.000(3) -0.001(3) -0.002(2) O1 0.032(3) 0.019(3) 0.019(4) -0.003(3) 0.003(3) -0.007(3) O2 0.024(3) 0.024(3) 0.028(4) -0.002(3) 0.006(3) 0.004(3) O3 0.039(4) 0.022(3) 0.015(4) 0.003(3) 0.001(3) 0.003(3) O4 0.020(3) 0.030(3) 0.017(4) 0.010(3) -0.004(3) -0.007(3) Re1 0.0156(2) 0.0094(2) 0.0114(2) 0.00098(11) -0.00049(15) -0.00008(11) _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 1.495(11) . ? C1 C4 1.544(10) . ? C2 N2 1.498(10) . ? C2 C4 1.518(11) . ? C3 N3 1.466(11) . ? C3 C4 1.550(12) . ? C4 C5 1.533(12) . ? C6 O1 1.145(10) . ? C6 Re1 1.922(9) . ? C7 O2 1.153(10) . ? C7 Re1 1.928(9) . ? C8 O3 1.144(10) . ? C8 Re1 1.914(9) . ? C9 O4 1.429(11) . ? N1 Re1 2.223(7) . ? N2 Re1 2.215(6) . ? N3 Re1 2.211(6) . ? 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 C4 114.2(7) . . ? N2 C2 C4 114.0(6) . . ? N3 C3 C4 113.1(7) . . ? C2 C4 C5 108.4(7) . . ? C2 C4 C1 111.6(6) . . ? C5 C4 C1 107.9(7) . . ? C2 C4 C3 111.0(7) . . ? C5 C4 C3 107.6(7) . . ? C1 C4 C3 110.1(7) . . ? O1 C6 Re1 176.2(7) . . ? O2 C7 Re1 178.9(7) . . ? O3 C8 Re1 177.9(7) . . ? C1 N1 Re1 120.2(5) . . ? C2 N2 Re1 118.0(5) . . ? C3 N3 Re1 118.8(5) . . ? C8 Re1 C6 88.3(3) . . ? C8 Re1 C7 88.6(4) . . ? C6 Re1 C7 87.7(3) . . ? C8 Re1 N3 92.4(3) . . ? C6 Re1 N3 177.3(3) . . ? C7 Re1 N3 94.9(3) . . ? C8 Re1 N2 95.5(3) . . ? C6 Re1 N2 95.7(3) . . ? C7 Re1 N2 174.7(3) . . ? N3 Re1 N2 81.7(2) . . ? C8 Re1 N1 174.7(3) . . ? C6 Re1 N1 93.8(3) . . ? C7 Re1 N1 96.4(3) . . ? N3 Re1 N1 85.3(2) . . ? N2 Re1 N1 79.4(3) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 7.055 _refine_diff_density_min -4.451 _refine_diff_density_rms 0.365