# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Youxuan Zheng' _publ_contact_author_email YXZHENG@NJU.EDU.CN _publ_section_title ; Synthesis, structural characterization and photoluminescence properties of rhenium(I) complexes based on bipyridine derivatives with carbazole moieties ; loop_ _publ_author_name 'Youxuan Zheng' 'Ling-Chen Kang' 'Dong-Ping Li' 'Hong-Yan Li' 'Yan Sui' ; Jing Wu ; 'Xiao-Zeng You' 'Xin-Hui Zhou' 'Yong-Hui Zhou' 'Jing-Lin Zuo' data_L3 _database_code_depnum_ccdc_archive 'CCDC 736413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 N4' _chemical_formula_sum 'C34 H22 N4' _chemical_formula_weight 486.56 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.1236(14) _cell_length_b 16.074(3) _cell_length_c 10.1949(17) _cell_angle_alpha 90.00 _cell_angle_beta 113.274(3) _cell_angle_gamma 90.00 _cell_volume 1222.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 497 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 19.57 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508.0 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9843 _exptl_absorpt_correction_T_max 0.9889 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 7116 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.00 _reflns_number_total 2661 _reflns_number_gt 1174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0521P)^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 2661 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _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 N1 N 0.9131(3) 0.03843(11) 0.81932(18) 0.0449(5) Uani 1 1 d . . . C1 C 0.9449(3) 0.03534(12) 0.9595(2) 0.0373(6) Uani 1 1 d . . . N2 N 0.6355(3) 0.22774(11) 0.71106(18) 0.0448(5) Uani 1 1 d . . . C4 C 0.7408(3) 0.16312(13) 0.7989(2) 0.0420(6) Uani 1 1 d . . . C5 C 0.8136(3) 0.10163(13) 0.7431(2) 0.0464(6) Uani 1 1 d . . . H5 H 0.7919 0.1044 0.6465 0.056 Uiso 1 1 calc R . . C2 C 0.8770(3) 0.09451(13) 1.0229(2) 0.0428(6) Uani 1 1 d . . . H2 H 0.9004 0.0908 1.1197 0.051 Uiso 1 1 calc R . . C3 C 0.7748(3) 0.15886(13) 0.9428(2) 0.0438(6) Uani 1 1 d . . . H3 H 0.7291 0.1990 0.9849 0.053 Uiso 1 1 calc R . . C6 C 0.4865(3) 0.21735(14) 0.5812(2) 0.0445(6) Uani 1 1 d . . . C12 C 0.5126(3) 0.35552(14) 0.6388(2) 0.0467(6) Uani 1 1 d . . . C17 C 0.6509(4) 0.31193(13) 0.7455(2) 0.0451(6) Uani 1 1 d . . . C11 C 0.4089(3) 0.29536(15) 0.5343(2) 0.0485(7) Uani 1 1 d . . . C16 C 0.7823(4) 0.35292(15) 0.8593(2) 0.0550(7) Uani 1 1 d . . . H16 H 0.8751 0.3240 0.9288 0.066 Uiso 1 1 calc R . . C7 C 0.4179(4) 0.14553(15) 0.5022(3) 0.0561(7) Uani 1 1 d . . . H7 H 0.4693 0.0938 0.5343 0.067 Uiso 1 1 calc R . . C15 C 0.7687(4) 0.43894(16) 0.8644(3) 0.0673(9) Uani 1 1 d . . . H15 H 0.8538 0.4682 0.9393 0.081 Uiso 1 1 calc R . . C14 C 0.6304(5) 0.48226(16) 0.7596(3) 0.0691(9) Uani 1 1 d . . . H14 H 0.6244 0.5398 0.7656 0.083 Uiso 1 1 calc R . . C13 C 0.5032(4) 0.44109(16) 0.6479(3) 0.0620(8) Uani 1 1 d . . . H13 H 0.4110 0.4705 0.5786 0.074 Uiso 1 1 calc R . . C8 C 0.2720(4) 0.15348(17) 0.3755(3) 0.0671(8) Uani 1 1 d . . . H8 H 0.2234 0.1063 0.3211 0.080 Uiso 1 1 calc R . . C10 C 0.2606(4) 0.30157(17) 0.4042(3) 0.0637(8) Uani 1 1 d . . . H10 H 0.2076 0.3529 0.3712 0.076 Uiso 1 1 calc R . . C9 C 0.1952(4) 0.23123(19) 0.3266(3) 0.0758(9) Uani 1 1 d . . . H9 H 0.0976 0.2350 0.2394 0.091 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 N1 0.0514(14) 0.0428(12) 0.0381(11) 0.0047(9) 0.0150(9) 0.0074(10) C1 0.0358(15) 0.0337(13) 0.0368(13) 0.0004(10) 0.0085(11) -0.0027(11) N2 0.0516(14) 0.0357(11) 0.0395(11) 0.0044(9) 0.0098(10) 0.0077(10) C4 0.0413(16) 0.0392(13) 0.0417(13) 0.0043(11) 0.0121(11) 0.0031(12) C5 0.0567(18) 0.0466(14) 0.0339(13) 0.0019(11) 0.0157(12) 0.0032(13) C2 0.0506(17) 0.0416(14) 0.0342(12) 0.0021(11) 0.0146(12) 0.0029(12) C3 0.0492(17) 0.0412(14) 0.0418(14) 0.0001(11) 0.0190(12) 0.0061(12) C6 0.0440(17) 0.0462(15) 0.0403(14) 0.0052(12) 0.0135(12) 0.0020(13) C12 0.0537(18) 0.0407(15) 0.0515(15) 0.0055(12) 0.0270(14) 0.0071(13) C17 0.0528(18) 0.0418(14) 0.0436(14) 0.0016(12) 0.0221(13) 0.0032(13) C11 0.0444(18) 0.0529(16) 0.0473(15) 0.0096(12) 0.0173(13) 0.0097(13) C16 0.066(2) 0.0489(16) 0.0487(15) -0.0011(13) 0.0212(14) -0.0002(14) C7 0.057(2) 0.0530(16) 0.0526(15) 0.0040(13) 0.0155(14) 0.0001(14) C15 0.095(3) 0.0501(17) 0.0650(18) -0.0106(15) 0.0404(18) -0.0157(17) C14 0.103(3) 0.0421(16) 0.0765(19) 0.0006(15) 0.0511(19) 0.0036(18) C13 0.070(2) 0.0512(18) 0.0708(18) 0.0121(15) 0.0348(17) 0.0186(15) C8 0.055(2) 0.0651(19) 0.0669(19) -0.0106(15) 0.0095(16) -0.0063(16) C10 0.050(2) 0.0635(18) 0.0682(18) 0.0164(15) 0.0131(16) 0.0137(15) C9 0.057(2) 0.084(2) 0.0655(19) -0.0031(17) 0.0020(16) 0.0010(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 N1 C5 1.339(3) . ? N1 C1 1.349(2) . ? C1 C2 1.382(3) . ? C1 C1 1.480(4) 3_757 ? N2 C17 1.391(2) . ? N2 C6 1.407(3) . ? N2 C4 1.417(3) . ? C4 C3 1.384(3) . ? C4 C5 1.384(3) . ? C5 H5 0.9300 . ? C2 C3 1.375(3) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C6 C7 1.392(3) . ? C6 C11 1.400(3) . ? C12 C13 1.383(3) . ? C12 C17 1.404(3) . ? C12 C11 1.439(3) . ? C17 C16 1.393(3) . ? C11 C10 1.399(3) . ? C16 C15 1.390(3) . ? C16 H16 0.9300 . ? C7 C8 1.371(3) . ? C7 H7 0.9300 . ? C15 C14 1.393(4) . ? C15 H15 0.9300 . ? C14 C13 1.368(4) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C8 C9 1.398(3) . ? C8 H8 0.9300 . ? C10 C9 1.362(3) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? 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 C5 N1 C1 117.51(19) . . ? N1 C1 C2 121.71(19) . . ? N1 C1 C1 116.1(2) . 3_757 ? C2 C1 C1 122.2(2) . 3_757 ? C17 N2 C6 108.13(18) . . ? C17 N2 C4 125.59(19) . . ? C6 N2 C4 126.01(18) . . ? C3 C4 C5 117.5(2) . . ? C3 C4 N2 121.6(2) . . ? C5 C4 N2 120.9(2) . . ? N1 C5 C4 124.1(2) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C3 C2 C1 119.96(19) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.2(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C7 C6 C11 121.4(2) . . ? C7 C6 N2 129.9(2) . . ? C11 C6 N2 108.6(2) . . ? C13 C12 C17 119.5(2) . . ? C13 C12 C11 133.3(2) . . ? C17 C12 C11 107.1(2) . . ? N2 C17 C16 129.3(2) . . ? N2 C17 C12 109.0(2) . . ? C16 C17 C12 121.6(2) . . ? C10 C11 C6 119.4(2) . . ? C10 C11 C12 133.4(2) . . ? C6 C11 C12 107.2(2) . . ? C15 C16 C17 117.1(2) . . ? C15 C16 H16 121.4 . . ? C17 C16 H16 121.4 . . ? C8 C7 C6 117.9(2) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C16 C15 C14 121.4(3) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C13 C12 119.6(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C7 C8 C9 121.2(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C9 C10 C11 118.9(2) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 0.4(3) . . . . ? C5 N1 C1 C1 179.9(2) . . . 3_757 ? C17 N2 C4 C3 45.6(3) . . . . ? C6 N2 C4 C3 -127.7(2) . . . . ? C17 N2 C4 C5 -134.5(2) . . . . ? C6 N2 C4 C5 52.2(3) . . . . ? C1 N1 C5 C4 -0.5(3) . . . . ? C3 C4 C5 N1 0.5(4) . . . . ? N2 C4 C5 N1 -179.5(2) . . . . ? N1 C1 C2 C3 -0.3(3) . . . . ? C1 C1 C2 C3 -179.8(2) 3_757 . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C5 C4 C3 C2 -0.3(3) . . . . ? N2 C4 C3 C2 179.6(2) . . . . ? C17 N2 C6 C7 179.0(3) . . . . ? C4 N2 C6 C7 -6.7(4) . . . . ? C17 N2 C6 C11 0.1(3) . . . . ? C4 N2 C6 C11 174.3(2) . . . . ? C6 N2 C17 C16 -176.2(2) . . . . ? C4 N2 C17 C16 9.5(4) . . . . ? C6 N2 C17 C12 0.1(3) . . . . ? C4 N2 C17 C12 -174.1(2) . . . . ? C13 C12 C17 N2 -178.3(2) . . . . ? C11 C12 C17 N2 -0.3(3) . . . . ? C13 C12 C17 C16 -1.6(4) . . . . ? C11 C12 C17 C16 176.4(2) . . . . ? C7 C6 C11 C10 -1.0(4) . . . . ? N2 C6 C11 C10 178.1(2) . . . . ? C7 C6 C11 C12 -179.3(2) . . . . ? N2 C6 C11 C12 -0.3(3) . . . . ? C13 C12 C11 C10 -0.1(5) . . . . ? C17 C12 C11 C10 -177.7(3) . . . . ? C13 C12 C11 C6 177.9(3) . . . . ? C17 C12 C11 C6 0.4(3) . . . . ? N2 C17 C16 C15 177.2(2) . . . . ? C12 C17 C16 C15 1.3(4) . . . . ? C11 C6 C7 C8 0.6(4) . . . . ? N2 C6 C7 C8 -178.2(2) . . . . ? C17 C16 C15 C14 -0.5(4) . . . . ? C16 C15 C14 C13 0.0(4) . . . . ? C15 C14 C13 C12 -0.3(4) . . . . ? C17 C12 C13 C14 1.1(4) . . . . ? C11 C12 C13 C14 -176.3(3) . . . . ? C6 C7 C8 C9 0.4(4) . . . . ? C6 C11 C10 C9 0.2(4) . . . . ? C12 C11 C10 C9 178.1(3) . . . . ? C11 C10 C9 C8 0.8(4) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.155 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.042 data_ReL1 _database_code_depnum_ccdc_archive 'CCDC 736414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H6 Br2 Cl N2 O3 Re' _chemical_formula_sum 'C13 H6 Br2 Cl N2 O3 Re' _chemical_formula_weight 619.67 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0009(11) _cell_length_b 9.4772(13) _cell_length_c 11.7020(15) _cell_angle_alpha 103.284(2) _cell_angle_beta 104.631(2) _cell_angle_gamma 97.333(2) _cell_volume 819.17(19) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5101 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 2.512 _exptl_crystal_density_diffrn 2.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 12.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1337 _exptl_absorpt_correction_T_max 0.1701 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'Bruker Smart Apex CCD' _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 4408 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3123 _reflns_number_gt 2740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0297P)^2^+13.7381P] 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 3123 _refine_ls_number_parameters 199 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 0.31616(6) 0.69728(5) 0.80837(4) 0.03183(15) Uani 1 1 d U . . Br1 Br 0.26627(19) 0.05372(14) 0.60153(13) 0.0527(3) Uani 1 1 d . . . Br2 Br 0.86050(19) 1.19114(15) 0.82037(16) 0.0630(4) Uani 1 1 d . . . Cl1 Cl 0.1603(4) 0.6991(3) 0.5967(3) 0.0393(6) Uani 1 1 d . . . C1 C 0.4490(17) 0.6947(15) 0.9700(11) 0.045(3) Uani 1 1 d U . . C2 C 0.1108(16) 0.5946(12) 0.8334(12) 0.041(3) Uani 1 1 d . . . C3 C 0.2626(17) 0.8776(14) 0.8802(11) 0.046(3) Uani 1 1 d . . . C4 C 0.3223(15) 0.3680(12) 0.6911(11) 0.039(3) Uani 1 1 d . . . H4 H 0.2234 0.3487 0.7173 0.046 Uiso 1 1 calc R . . C5 C 0.3808(16) 0.2513(13) 0.6286(11) 0.040(3) Uani 1 1 d . . . C6 C 0.5251(17) 0.2790(13) 0.5906(11) 0.044(3) Uani 1 1 d . . . H6 H 0.5647 0.2019 0.5471 0.053 Uiso 1 1 calc R . . C7 C 0.6132(17) 0.4244(13) 0.6177(11) 0.041(3) Uani 1 1 d . . . H7 H 0.7136 0.4452 0.5934 0.049 Uiso 1 1 calc R . . C8 C 0.5532(15) 0.5330(13) 0.6783(9) 0.035(2) Uani 1 1 d . . . C9 C 0.6311(13) 0.6921(12) 0.7066(10) 0.033(2) Uani 1 1 d . . . C10 C 0.7789(14) 0.7406(14) 0.6750(11) 0.039(3) Uani 1 1 d . . . H10 H 0.8289 0.6722 0.6309 0.047 Uiso 1 1 calc R . . C11 C 0.8524(16) 0.8867(13) 0.7073(12) 0.044(3) Uani 1 1 d U . . H11 H 0.9534 0.9192 0.6876 0.053 Uiso 1 1 calc R . . C12 C 0.7707(16) 0.9868(13) 0.7716(11) 0.041(3) Uani 1 1 d U . . C13 C 0.6212(14) 0.9323(12) 0.7987(9) 0.035(2) Uani 1 1 d . . . H13 H 0.5677 0.9991 0.8413 0.042 Uiso 1 1 calc R . . N1 N 0.4040(12) 0.5070(10) 0.7144(8) 0.034(2) Uani 1 1 d . . . N2 N 0.5499(11) 0.7891(9) 0.7667(8) 0.0311(19) Uani 1 1 d . . . O1 O 0.5272(17) 0.6900(14) 1.0642(9) 0.082(4) Uani 1 1 d U . . O2 O -0.0077(13) 0.5313(12) 0.8492(11) 0.067(3) Uani 1 1 d . . . O3 O 0.2229(14) 0.9886(10) 0.9245(9) 0.061(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 Re1 0.0355(2) 0.0264(2) 0.0374(2) 0.00814(17) 0.01767(18) 0.00630(17) Br1 0.0691(9) 0.0283(6) 0.0632(8) 0.0101(6) 0.0270(7) 0.0074(6) Br2 0.0567(8) 0.0381(7) 0.0926(11) 0.0203(7) 0.0238(8) -0.0041(6) Cl1 0.0390(14) 0.0416(16) 0.0388(14) 0.0076(12) 0.0162(12) 0.0099(12) C1 0.045(7) 0.050(8) 0.044(6) 0.009(6) 0.022(5) 0.015(6) C2 0.049(7) 0.023(6) 0.068(8) 0.022(6) 0.035(6) 0.012(5) C3 0.054(8) 0.039(7) 0.042(7) 0.006(6) 0.013(6) 0.006(6) C4 0.042(6) 0.026(6) 0.051(7) 0.016(5) 0.016(5) 0.004(5) C5 0.044(6) 0.030(6) 0.049(7) 0.011(5) 0.019(5) 0.010(5) C6 0.055(8) 0.033(6) 0.048(7) 0.006(5) 0.023(6) 0.018(6) C7 0.054(7) 0.031(6) 0.042(6) 0.014(5) 0.016(6) 0.010(5) C8 0.037(6) 0.041(7) 0.027(5) 0.008(5) 0.009(5) 0.008(5) C9 0.029(5) 0.035(6) 0.032(5) 0.005(5) 0.007(4) 0.011(5) C10 0.030(6) 0.045(7) 0.052(7) 0.021(6) 0.018(5) 0.015(5) C11 0.039(6) 0.039(7) 0.063(8) 0.027(6) 0.020(6) 0.003(5) C12 0.042(6) 0.035(6) 0.042(6) 0.020(5) 0.002(5) -0.003(5) C13 0.035(6) 0.035(6) 0.027(5) -0.001(4) 0.002(4) 0.011(5) N1 0.036(5) 0.034(5) 0.034(5) 0.009(4) 0.014(4) 0.007(4) N2 0.030(4) 0.025(5) 0.040(5) 0.008(4) 0.014(4) 0.004(4) O1 0.100(9) 0.095(9) 0.046(5) 0.028(6) 0.003(5) 0.023(7) O2 0.062(6) 0.057(6) 0.094(8) 0.030(6) 0.041(6) 0.002(5) O3 0.080(7) 0.042(6) 0.058(6) 0.004(5) 0.019(5) 0.022(5) _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 C3 1.876(13) . ? Re1 C2 1.924(11) . ? Re1 C1 1.929(13) . ? Re1 N2 2.175(8) . ? Re1 N1 2.181(9) . ? Re1 Cl1 2.481(3) . ? Br1 C5 1.894(12) . ? Br2 C12 1.877(12) . ? C1 O1 1.135(15) . ? C2 O2 1.134(14) . ? C3 O3 1.181(15) . ? C4 N1 1.328(14) . ? C4 C5 1.382(16) . ? C4 H4 0.9300 . ? C5 C6 1.355(17) . ? C6 C7 1.391(17) . ? C6 H6 0.9300 . ? C7 C8 1.325(16) . ? C7 H7 0.9300 . ? C8 N1 1.375(14) . ? C8 C9 1.483(16) . ? C9 N2 1.359(13) . ? C9 C10 1.381(15) . ? C10 C11 1.358(17) . ? C10 H10 0.9300 . ? C11 C12 1.404(18) . ? C11 H11 0.9300 . ? C12 C13 1.381(16) . ? C13 N2 1.331(14) . ? C13 H13 0.9300 . ? 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 C3 Re1 C2 89.3(5) . . ? C3 Re1 C1 88.4(5) . . ? C2 Re1 C1 88.6(5) . . ? C3 Re1 N2 97.2(5) . . ? C2 Re1 N2 173.4(4) . . ? C1 Re1 N2 92.9(4) . . ? C3 Re1 N1 171.5(5) . . ? C2 Re1 N1 98.9(4) . . ? C1 Re1 N1 94.2(4) . . ? N2 Re1 N1 74.6(3) . . ? C3 Re1 Cl1 93.5(4) . . ? C2 Re1 Cl1 94.1(4) . . ? C1 Re1 Cl1 176.8(4) . . ? N2 Re1 Cl1 84.3(2) . . ? N1 Re1 Cl1 83.6(2) . . ? O1 C1 Re1 178.5(12) . . ? O2 C2 Re1 178.1(11) . . ? O3 C3 Re1 177.7(12) . . ? N1 C4 C5 121.5(11) . . ? N1 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 119.4(11) . . ? C6 C5 Br1 120.0(9) . . ? C4 C5 Br1 120.5(9) . . ? C5 C6 C7 119.1(11) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 119.5(12) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 N1 122.1(11) . . ? C7 C8 C9 124.1(11) . . ? N1 C8 C9 113.7(10) . . ? N2 C9 C10 121.2(10) . . ? N2 C9 C8 116.4(9) . . ? C10 C9 C8 122.4(10) . . ? C11 C10 C9 121.1(11) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 117.7(11) . . ? C10 C11 H11 121.2 . . ? C12 C11 H11 121.2 . . ? C13 C12 C11 118.7(10) . . ? C13 C12 Br2 119.9(10) . . ? C11 C12 Br2 121.3(9) . . ? N2 C13 C12 123.2(10) . . ? N2 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C4 N1 C8 118.3(10) . . ? C4 N1 Re1 123.7(8) . . ? C8 N1 Re1 118.0(7) . . ? C13 N2 C9 118.0(9) . . ? C13 N2 Re1 124.7(7) . . ? C9 N2 Re1 117.3(7) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.753 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.292 data_90517bm _database_code_depnum_ccdc_archive 'CCDC 736415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H22 Cl N4 O3 Re, C H2 Cl2' _chemical_formula_sum 'C38 H24 Cl3 N4 O3 Re' _chemical_formula_weight 877.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' 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 28.810(3) _cell_length_b 12.8548(12) _cell_length_c 21.063(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.103(2) _cell_angle_gamma 90.00 _cell_volume 6815.7(12) _cell_formula_units_Z 8 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1328 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 15.75 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 3.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4716 _exptl_absorpt_correction_T_max 0.5286 _exptl_absorpt_process_details 'SADABS,2000; Bruker' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 18099 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.1082 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6689 _reflns_number_gt 4272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0753P)^2^+80.9041P] 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 6689 _refine_ls_number_parameters 442 _refine_ls_number_restraints 367 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1876 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.061 _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 0.0575(6) 0.8107(11) 0.4968(7) 0.054(3) Uani 1 1 d U . . C2 C 0.0798(7) 1.0022(15) 0.4699(9) 0.081(5) Uani 1 1 d U . . C3 C 0.0311(6) 0.8706(11) 0.3621(8) 0.063(4) Uani 1 1 d U . . C4 C 0.2658(8) 1.1159(17) 0.6603(12) 0.104(4) Uani 1 1 d U . . C5 C 0.2399(9) 1.1494(18) 0.5939(13) 0.115(5) Uani 1 1 d U . . H5 H 0.2191 1.1044 0.5560 0.138 Uiso 1 1 calc R . . C6 C 0.2440(9) 1.253(2) 0.5807(14) 0.131(5) Uani 1 1 d U . . H6 H 0.2260 1.2813 0.5343 0.157 Uiso 1 1 calc R . . C7 C 0.2764(10) 1.311(2) 0.6408(15) 0.134(5) Uani 1 1 d U . . H7 H 0.2798 1.3809 0.6319 0.161 Uiso 1 1 calc R . . C8 C 0.3028(9) 1.2828(19) 0.7079(13) 0.118(5) Uani 1 1 d U . . H8 H 0.3230 1.3299 0.7446 0.142 Uiso 1 1 calc R . . C9 C 0.2998(9) 1.178(2) 0.7229(13) 0.116(4) Uani 1 1 d U . . C10 C 0.3211(8) 1.1170(17) 0.7813(12) 0.105(4) Uani 1 1 d U . . C11 C 0.3574(9) 1.1406(19) 0.8558(13) 0.122(5) Uani 1 1 d U . . H11 H 0.3712 1.2071 0.8707 0.147 Uiso 1 1 calc R . . C12 C 0.3710(9) 1.0580(19) 0.9051(13) 0.117(5) Uani 1 1 d U . . H12 H 0.3936 1.0744 0.9536 0.141 Uiso 1 1 calc R . . C13 C 0.3562(8) 0.961(2) 0.8916(11) 0.125(5) Uani 1 1 d DU . . H13 H 0.3681 0.9124 0.9287 0.150 Uiso 1 1 calc R . . C14 C 0.3188(8) 0.931(2) 0.8137(10) 0.116(4) Uani 1 1 d DU . . H14 H 0.3064 0.8638 0.7997 0.139 Uiso 1 1 calc R . . C15 C 0.3057(8) 1.0076(19) 0.7682(13) 0.111(4) Uani 1 1 d U . . C16 C 0.1970(6) 0.9227(13) 0.5970(8) 0.071(4) Uani 1 1 d U . . H16 H 0.1769 0.9803 0.5953 0.085 Uiso 1 1 calc R . . C17 C 0.2492(7) 0.9182(14) 0.6505(9) 0.081(3) Uani 1 1 d U . . C18 C 0.2779(7) 0.8283(13) 0.6576(9) 0.077(4) Uani 1 1 d U . . H18 H 0.3126 0.8211 0.6951 0.093 Uiso 1 1 calc R . . C19 C 0.2535(6) 0.7491(12) 0.6074(8) 0.065(4) Uani 1 1 d U . . H19 H 0.2718 0.6880 0.6108 0.078 Uiso 1 1 calc R . . C20 C 0.2008(5) 0.7618(11) 0.5511(7) 0.055(3) Uani 1 1 d U . . C21 C 0.1749(5) 0.6857(10) 0.4927(6) 0.046(3) Uani 1 1 d U . . C22 C 0.1965(5) 0.5921(10) 0.4888(7) 0.051(3) Uani 1 1 d U . . H22 H 0.2299 0.5730 0.5258 0.062 Uiso 1 1 calc R . . C23 C 0.1690(5) 0.5262(10) 0.4307(7) 0.054(3) Uani 1 1 d U . . H23 H 0.1839 0.4636 0.4275 0.065 Uiso 1 1 calc R . . C24 C 0.1191(5) 0.5552(11) 0.3774(7) 0.053(3) Uani 1 1 d U . . C25 C 0.0987(5) 0.6461(11) 0.3859(7) 0.056(3) Uani 1 1 d U . . H25 H 0.0643 0.6635 0.3510 0.067 Uiso 1 1 calc R . . C26 C 0.0877(6) 0.3828(12) 0.3167(8) 0.065(4) Uani 1 1 d U . . C27 C 0.1054(7) 0.3134(14) 0.3731(10) 0.080(5) Uani 1 1 d U . . H27 H 0.1228 0.3361 0.4211 0.096 Uiso 1 1 calc R . . C28 C 0.0969(7) 0.2090(15) 0.3568(11) 0.094(6) Uani 1 1 d U . . H28 H 0.1089 0.1607 0.3943 0.113 Uiso 1 1 calc R . . C29 C 0.0720(7) 0.1764(15) 0.2891(11) 0.092(5) Uani 1 1 d U . . H29 H 0.0676 0.1052 0.2803 0.110 Uiso 1 1 calc R . . C30 C 0.0520(7) 0.2434(14) 0.2302(10) 0.087(5) Uani 1 1 d U . . H30 H 0.0345 0.2183 0.1828 0.104 Uiso 1 1 calc R . . C31 C 0.0591(6) 0.3503(12) 0.2444(9) 0.065(4) Uani 1 1 d U . . C32 C 0.0444(6) 0.4399(11) 0.1980(8) 0.060(4) Uani 1 1 d U . . C33 C 0.0177(6) 0.4557(14) 0.1237(9) 0.079(4) Uani 1 1 d U . . H33 H 0.0024 0.3999 0.0923 0.094 Uiso 1 1 calc R . . C34 C 0.0141(7) 0.5528(15) 0.0971(10) 0.087(5) Uani 1 1 d U . . H34 H -0.0025 0.5623 0.0470 0.105 Uiso 1 1 calc R . . C35 C 0.0346(6) 0.6395(13) 0.1425(9) 0.078(4) Uani 1 1 d U . . H35 H 0.0315 0.7058 0.1231 0.093 Uiso 1 1 calc R . . C36 C 0.0598(6) 0.6245(11) 0.2169(8) 0.064(4) Uani 1 1 d U . . H36 H 0.0731 0.6810 0.2482 0.077 Uiso 1 1 calc R . . C37 C 0.0650(6) 0.5255(11) 0.2440(7) 0.059(3) Uani 1 1 d U . . C38 C 0.1181(10) 0.064(2) 0.7094(14) 0.152(6) Uani 1 1 d U . . H38A H 0.0977 0.1284 0.6966 0.183 Uiso 1 1 calc R . . H38B H 0.1192 0.0378 0.7532 0.183 Uiso 1 1 calc R . . Cl1 Cl 0.15015(17) 0.9286(3) 0.3977(2) 0.0754(11) Uani 1 1 d . . . Cl2 Cl 0.1790(3) 0.0927(8) 0.7285(5) 0.204(4) Uani 1 1 d U . . Cl3 Cl 0.0849(3) -0.0228(5) 0.6418(3) 0.127(2) Uani 1 1 d U . . N1 N 0.2723(6) 1.0114(13) 0.6943(9) 0.103(3) Uani 1 1 d U . . N2 N 0.1734(4) 0.8472(8) 0.5467(6) 0.055(3) Uani 1 1 d . . . N3 N 0.1249(4) 0.7125(9) 0.4412(6) 0.054(3) Uani 1 1 d . . . N4 N 0.0894(4) 0.4909(8) 0.3157(6) 0.055(3) Uani 1 1 d U . . O1 O 0.0336(4) 0.7813(9) 0.5229(6) 0.080(3) Uani 1 1 d . . . O2 O 0.0707(6) 1.0838(10) 0.4812(7) 0.116(5) Uani 1 1 d . . . O3 O -0.0085(5) 0.8720(10) 0.3097(6) 0.099(4) Uani 1 1 d . . . Re1 Re 0.09631(2) 0.86412(4) 0.45216(3) 0.0542(2) 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 0.062(7) 0.052(7) 0.049(6) -0.008(5) 0.027(6) 0.007(6) C2 0.091(9) 0.078(9) 0.087(8) -0.011(7) 0.053(7) 0.006(7) C3 0.060(7) 0.075(8) 0.056(7) 0.007(6) 0.029(6) 0.009(6) C4 0.096(6) 0.113(6) 0.111(6) -0.021(5) 0.057(5) 0.000(5) C5 0.110(7) 0.117(7) 0.122(7) -0.009(6) 0.060(5) -0.001(6) C6 0.122(7) 0.129(7) 0.137(7) -0.009(6) 0.059(6) 0.002(6) C7 0.124(7) 0.135(7) 0.140(7) -0.009(6) 0.061(6) -0.004(6) C8 0.110(7) 0.123(7) 0.128(7) -0.014(6) 0.063(5) -0.003(6) C9 0.106(6) 0.123(6) 0.123(6) -0.017(5) 0.059(5) 0.001(5) C10 0.097(6) 0.120(6) 0.112(6) -0.020(5) 0.061(5) 0.004(5) C11 0.110(7) 0.132(7) 0.128(7) -0.019(6) 0.060(5) 0.005(6) C12 0.107(7) 0.131(7) 0.120(7) -0.018(6) 0.061(5) 0.007(6) C13 0.113(7) 0.143(7) 0.126(7) -0.015(6) 0.063(5) 0.008(6) C14 0.106(7) 0.137(7) 0.115(7) -0.016(6) 0.061(5) 0.006(6) C15 0.099(6) 0.129(6) 0.114(6) -0.016(5) 0.058(5) 0.003(5) C16 0.067(6) 0.080(7) 0.077(6) -0.013(6) 0.045(5) 0.001(6) C17 0.075(5) 0.093(6) 0.081(5) -0.017(5) 0.044(4) -0.002(5) C18 0.070(6) 0.089(7) 0.073(6) -0.005(6) 0.034(5) -0.002(5) C19 0.058(7) 0.068(8) 0.064(7) -0.001(6) 0.026(6) 0.000(6) C20 0.051(7) 0.060(7) 0.050(6) 0.004(5) 0.022(5) 0.001(6) C21 0.047(6) 0.047(6) 0.044(6) 0.004(5) 0.021(5) 0.004(5) C22 0.049(6) 0.054(6) 0.049(6) 0.005(5) 0.023(5) 0.006(5) C23 0.054(7) 0.049(6) 0.062(6) 0.001(5) 0.031(5) 0.009(5) C24 0.052(7) 0.061(7) 0.050(5) 0.006(5) 0.029(5) 0.002(5) C25 0.050(6) 0.061(7) 0.060(7) 0.000(6) 0.029(5) 0.007(6) C26 0.062(7) 0.064(8) 0.074(7) -0.006(6) 0.036(6) -0.001(6) C27 0.081(8) 0.072(8) 0.087(8) 0.001(7) 0.042(7) 0.004(7) C28 0.092(9) 0.087(9) 0.107(9) 0.009(7) 0.051(7) 0.003(7) C29 0.089(9) 0.083(9) 0.105(9) -0.004(7) 0.049(7) -0.007(7) C30 0.089(9) 0.080(9) 0.090(9) -0.017(7) 0.042(7) 0.003(7) C31 0.061(7) 0.061(8) 0.080(8) -0.009(6) 0.039(6) 0.004(6) C32 0.057(7) 0.065(7) 0.061(7) -0.014(6) 0.030(6) 0.000(6) C33 0.078(8) 0.089(8) 0.074(7) -0.022(6) 0.041(6) 0.004(6) C34 0.087(7) 0.097(8) 0.075(7) 0.001(6) 0.036(6) 0.008(7) C35 0.078(7) 0.081(8) 0.075(7) 0.001(6) 0.038(6) 0.010(6) C36 0.064(7) 0.064(7) 0.058(7) 0.005(6) 0.023(6) 0.006(6) C37 0.058(7) 0.063(7) 0.056(5) -0.006(5) 0.029(5) 0.001(6) C38 0.148(9) 0.178(9) 0.151(9) -0.036(7) 0.088(7) -0.019(8) Cl1 0.085(3) 0.076(3) 0.079(3) 0.016(2) 0.051(2) 0.014(2) Cl2 0.163(6) 0.283(9) 0.215(8) -0.122(7) 0.130(6) -0.085(6) Cl3 0.151(5) 0.138(5) 0.100(4) -0.038(3) 0.068(4) -0.031(4) N1 0.087(6) 0.120(6) 0.102(6) -0.024(6) 0.047(5) 0.000(5) N2 0.060(7) 0.055(7) 0.048(6) -0.010(5) 0.026(6) -0.004(6) N3 0.043(6) 0.066(8) 0.054(7) 0.008(6) 0.025(6) 0.009(6) N4 0.063(7) 0.048(7) 0.048(6) -0.004(5) 0.024(5) 0.008(5) O1 0.087(8) 0.096(9) 0.067(7) 0.001(6) 0.046(6) 0.004(7) O2 0.176(14) 0.068(8) 0.131(11) -0.003(8) 0.096(11) 0.020(9) O3 0.078(8) 0.125(11) 0.067(7) 0.013(7) 0.014(6) 0.030(7) Re1 0.0591(4) 0.0537(4) 0.0516(3) -0.0014(3) 0.0283(3) 0.0093(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 O1 1.134(16) . ? C1 Re1 1.904(16) . ? C2 O2 1.135(18) . ? C2 Re1 1.920(18) . ? C3 O3 1.138(16) . ? C3 Re1 1.916(15) . ? C4 C5 1.30(3) . ? C4 C9 1.44(3) . ? C4 N1 1.49(2) . ? C5 C6 1.38(3) . ? C5 H5 0.9300 . ? C6 C7 1.37(3) . ? C6 H6 0.9300 . ? C7 C8 1.29(3) . ? C7 H7 0.9300 . ? C8 C9 1.39(3) . ? C8 H8 0.9300 . ? C9 C10 1.33(3) . ? C10 C11 1.43(3) . ? C10 C15 1.46(3) . ? C11 C12 1.40(3) . ? C11 H11 0.9300 . ? C12 C13 1.30(3) . ? C12 H12 0.9300 . ? C13 C14 1.510(10) . ? C13 H13 0.9300 . ? C14 C15 1.29(3) . ? C14 H14 0.9300 . ? C15 N1 1.37(2) . ? C16 N2 1.351(17) . ? C16 C17 1.38(2) . ? C16 H16 0.9300 . ? C17 C18 1.39(2) . ? C17 N1 1.46(2) . ? C18 C19 1.39(2) . ? C18 H18 0.9300 . ? C19 C20 1.409(18) . ? C19 H19 0.9300 . ? C20 N2 1.329(16) . ? C20 C21 1.460(18) . ? C21 N3 1.360(15) . ? C21 C22 1.375(17) . ? C22 C23 1.379(17) . ? C22 H22 0.9300 . ? C23 C24 1.377(17) . ? C23 H23 0.9300 . ? C24 C25 1.358(18) . ? C24 N4 1.422(16) . ? C25 N3 1.341(16) . ? C25 H25 0.9300 . ? C26 C27 1.37(2) . ? C26 N4 1.391(17) . ? C26 C31 1.40(2) . ? C27 C28 1.38(2) . ? C27 H27 0.9300 . ? C28 C29 1.31(2) . ? C28 H28 0.9300 . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 C31 1.40(2) . ? C30 H30 0.9300 . ? C31 C32 1.43(2) . ? C32 C33 1.38(2) . ? C32 C37 1.394(18) . ? C33 C34 1.35(2) . ? C33 H33 0.9300 . ? C34 C35 1.40(2) . ? C34 H34 0.9300 . ? C35 C36 1.38(2) . ? C35 H35 0.9300 . ? C36 C37 1.372(18) . ? C36 H36 0.9300 . ? C37 N4 1.393(16) . ? C38 Cl2 1.64(2) . ? C38 Cl3 1.69(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? Cl1 Re1 2.477(4) . ? N2 Re1 2.154(11) . ? N3 Re1 2.172(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 178.1(13) . . ? O2 C2 Re1 179(2) . . ? O3 C3 Re1 177.4(14) . . ? C5 C4 C9 125(2) . . ? C5 C4 N1 134(2) . . ? C9 C4 N1 101(2) . . ? C4 C5 C6 119(2) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C5 C6 C7 115(3) . . ? C5 C6 H6 122.3 . . ? C7 C6 H6 122.3 . . ? C8 C7 C6 129(3) . . ? C8 C7 H7 115.5 . . ? C6 C7 H7 115.5 . . ? C7 C8 C9 117(3) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? C10 C9 C8 137(2) . . ? C10 C9 C4 109(2) . . ? C8 C9 C4 115(2) . . ? C9 C10 C11 131(2) . . ? C9 C10 C15 116(2) . . ? C11 C10 C15 114(2) . . ? C12 C11 C10 116(2) . . ? C12 C11 H11 121.9 . . ? C10 C11 H11 121.9 . . ? C13 C12 C11 128(2) . . ? C13 C12 H12 115.9 . . ? C11 C12 H12 115.9 . . ? C12 C13 C14 118(2) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? C15 C14 C13 114(2) . . ? C15 C14 H14 122.9 . . ? C13 C14 H14 122.9 . . ? C14 C15 N1 131(2) . . ? C14 C15 C10 130(2) . . ? N1 C15 C10 99(2) . . ? N2 C16 C17 123.1(15) . . ? N2 C16 H16 118.4 . . ? C17 C16 H16 118.4 . . ? C16 C17 C18 118.7(16) . . ? C16 C17 N1 117.7(16) . . ? C18 C17 N1 123.5(16) . . ? C17 C18 C19 118.4(16) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? C18 C19 C20 119.7(15) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N2 C20 C19 121.0(13) . . ? N2 C20 C21 116.8(12) . . ? C19 C20 C21 122.1(13) . . ? N3 C21 C22 120.5(12) . . ? N3 C21 C20 114.4(12) . . ? C22 C21 C20 125.1(12) . . ? C21 C22 C23 120.7(12) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 118.6(12) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 118.1(13) . . ? C25 C24 N4 121.0(12) . . ? C23 C24 N4 120.9(12) . . ? N3 C25 C24 124.4(13) . . ? N3 C25 H25 117.8 . . ? C24 C25 H25 117.8 . . ? C27 C26 N4 131.5(15) . . ? C27 C26 C31 121.6(15) . . ? N4 C26 C31 106.8(13) . . ? C26 C27 C28 118.1(17) . . ? C26 C27 H27 120.9 . . ? C28 C27 H27 120.9 . . ? C29 C28 C27 121.2(19) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 122.9(19) . . ? C28 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C29 C30 C31 117.7(17) . . ? C29 C30 H30 121.1 . . ? C31 C30 H30 121.1 . . ? C26 C31 C30 118.3(15) . . ? C26 C31 C32 109.0(13) . . ? C30 C31 C32 132.7(15) . . ? C33 C32 C37 119.0(15) . . ? C33 C32 C31 134.9(14) . . ? C37 C32 C31 106.0(13) . . ? C34 C33 C32 119.6(16) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 122.1(17) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C36 C35 C34 118.5(16) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C37 C36 C35 119.5(14) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 N4 130.0(13) . . ? C36 C37 C32 121.3(14) . . ? N4 C37 C32 108.7(13) . . ? Cl2 C38 Cl3 117.0(15) . . ? Cl2 C38 H38A 108.1 . . ? Cl3 C38 H38A 108.1 . . ? Cl2 C38 H38B 108.1 . . ? Cl3 C38 H38B 108.1 . . ? H38A C38 H38B 107.3 . . ? C15 N1 C17 122.6(18) . . ? C15 N1 C4 115.6(18) . . ? C17 N1 C4 121.5(16) . . ? C20 N2 C16 118.9(12) . . ? C20 N2 Re1 117.3(8) . . ? C16 N2 Re1 123.5(10) . . ? C25 N3 C21 117.6(11) . . ? C25 N3 Re1 125.5(9) . . ? C21 N3 Re1 116.8(9) . . ? C26 N4 C37 109.5(11) . . ? C26 N4 C24 125.2(11) . . ? C37 N4 C24 124.6(11) . . ? C1 Re1 C3 88.6(6) . . ? C1 Re1 C2 88.7(7) . . ? C3 Re1 C2 86.3(7) . . ? C1 Re1 N2 95.5(5) . . ? C3 Re1 N2 173.4(5) . . ? C2 Re1 N2 98.9(6) . . ? C1 Re1 N3 94.2(5) . . ? C3 Re1 N3 100.0(5) . . ? C2 Re1 N3 173.1(6) . . ? N2 Re1 N3 74.6(4) . . ? C1 Re1 Cl1 177.4(4) . . ? C3 Re1 Cl1 93.5(4) . . ? C2 Re1 Cl1 93.0(5) . . ? N2 Re1 Cl1 82.3(3) . . ? N3 Re1 Cl1 84.0(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.428 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.159