# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Qiao-hua Wei' _publ_contact_author_email qhw76@fzu.edu.cn loop_ _publ_author_name 'Qiao-hua Wei' 'Guo-nan Chen' data_Compoumd_1 _database_code_depnum_ccdc_archive 'CCDC 806767' #TrackingRef '- crystal data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H35 Br2 Cl2 N7 O7 Re2' _chemical_formula_weight 1340.88 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2187(6) _cell_length_b 13.2825(5) _cell_length_c 14.5639(6) _cell_angle_alpha 96.440(2) _cell_angle_beta 114.512(2) _cell_angle_gamma 105.043(2) _cell_volume 2175.44(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6720 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.00 _exptl_crystal_description block _exptl_crystal_colour yollow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 7.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3769 _exptl_absorpt_correction_T_max 0.7032 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 47665 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9947 _reflns_number_gt 8251 _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. ; _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^)+(0.0777P)^2^+33.3693P] 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 9947 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.43789(3) 0.76499(3) 0.14700(3) 0.02394(10) Uani 1 1 d . . . Re2 Re 0.19242(3) 0.30812(3) 0.49387(3) 0.02680(11) Uani 1 1 d . . . Br1 Br 0.77220(11) 1.29295(10) 0.67988(10) 0.0525(3) Uani 1 1 d . . . Br2 Br 0.78402(12) 0.87466(12) 0.87140(11) 0.0616(3) Uani 1 1 d . . . Cl1 Cl 0.33386(15) 0.70768(13) -0.05109(12) 0.0144(3) Uani 1 1 d . . . Cl2 Cl -0.02730(14) 0.23096(13) 0.37186(14) 0.0185(3) Uani 1 1 d . . . O1 O 0.2819(7) 0.5510(5) 0.1506(6) 0.0416(17) Uani 1 1 d . . . O01 O 0.9622(11) 0.726(2) 0.0817(11) 0.163(10) Uani 1 1 d . . . O2 O 0.2584(6) 0.8729(5) 0.1469(5) 0.0346(14) Uani 1 1 d . . . O3 O 0.5659(6) 0.8376(5) 0.3853(5) 0.0321(14) Uani 1 1 d . . . O4 O 0.2325(7) 0.1249(6) 0.3816(6) 0.0412(16) Uani 1 1 d . . . O5 O 0.2235(7) 0.4426(6) 0.3435(5) 0.0398(16) Uani 1 1 d . . . O6 O 0.4590(6) 0.4052(5) 0.6415(6) 0.0363(15) Uani 1 1 d . . . N1 N 0.5664(6) 0.6963(6) 0.1314(5) 0.0248(14) Uani 1 1 d . . . N01 N 1.0124(9) 0.7226(15) -0.0464(9) 0.083(5) Uani 1 1 d . . . N2 N 0.5627(6) 0.8926(6) 0.1290(6) 0.0258(14) Uani 1 1 d . . . N3 N 0.5802(6) 0.9972(6) 0.1275(5) 0.0264(15) Uani 1 1 d . . . N4 N 0.1420(7) 0.2156(6) 0.5928(6) 0.0311(17) Uani 1 1 d . . . N5 N 0.1453(6) 0.4113(6) 0.5833(6) 0.0272(15) Uani 1 1 d . . . N6 N 0.1440(6) 0.5138(6) 0.5943(6) 0.0280(15) Uani 1 1 d . . . C1 C 0.3397(8) 0.6324(7) 0.1518(7) 0.0311(19) Uani 1 1 d . . . C01 C 1.0003(18) 0.609(2) -0.074(2) 0.139(12) Uani 1 1 d . . . H01A H 0.9740 0.5705 -0.0304 0.208 Uiso 1 1 calc R . . H01B H 1.0767 0.6038 -0.0637 0.208 Uiso 1 1 calc R . . H01C H 0.9420 0.5771 -0.1477 0.208 Uiso 1 1 calc R . . C2 C 0.3258(8) 0.8319(7) 0.1475(6) 0.0264(17) Uani 1 1 d . . . C02 C 1.0499(13) 0.7859(15) -0.1046(11) 0.074(4) Uani 1 1 d . . . H02A H 1.0549 0.8601 -0.0819 0.111 Uiso 1 1 calc R . . H02B H 0.9932 0.7570 -0.1787 0.111 Uiso 1 1 calc R . . H02C H 1.1278 0.7847 -0.0939 0.111 Uiso 1 1 calc R . . C3 C 0.5181(8) 0.8100(7) 0.2952(7) 0.0268(17) Uani 1 1 d . . . C03 C 0.9962(14) 0.767(3) 0.0322(12) 0.149(13) Uani 1 1 d . . . H03A H 1.0163 0.8434 0.0474 0.179 Uiso 1 1 calc R . . C4 C 0.5657(8) 0.5957(7) 0.1365(7) 0.0288(18) Uani 1 1 d . . . H4A H 0.5128 0.5530 0.1569 0.035 Uiso 1 1 calc R . . C5 C 0.6391(8) 0.5520(7) 0.1132(7) 0.0317(19) Uani 1 1 d . . . H5A H 0.6367 0.4807 0.1177 0.038 Uiso 1 1 calc R . . C6 C 0.7160(9) 0.6137(8) 0.0831(7) 0.034(2) Uani 1 1 d . . . H6A H 0.7657 0.5848 0.0649 0.041 Uiso 1 1 calc R . . C7 C 0.7192(8) 0.7177(8) 0.0801(7) 0.0313(19) Uani 1 1 d . . . H7A H 0.7727 0.7622 0.0614 0.038 Uiso 1 1 calc R . . C8 C 0.6432(7) 0.7573(7) 0.1049(6) 0.0251(16) Uani 1 1 d . . . C9 C 0.6419(8) 0.8656(7) 0.1049(7) 0.0275(17) Uani 1 1 d . . . C10 C 0.7100(8) 0.9544(7) 0.0882(7) 0.0310(19) Uani 1 1 d . . . H10A H 0.7712 0.9572 0.0694 0.037 Uiso 1 1 calc R . . C11 C 0.6696(8) 1.0369(8) 0.1049(7) 0.0315(19) Uani 1 1 d . . . H11A H 0.6993 1.1087 0.1012 0.038 Uiso 1 1 calc R . . C12 C 0.5225(8) 1.0582(7) 0.1664(7) 0.0276(17) Uani 1 1 d . . . H12A H 0.4366 1.0180 0.1322 0.033 Uiso 1 1 calc R . . H12B H 0.5341 1.1281 0.1475 0.033 Uiso 1 1 calc R . . C13 C 0.5702(8) 1.0783(7) 0.2830(7) 0.0269(17) Uani 1 1 d . . . C14 C 0.4961(8) 1.0799(7) 0.3288(7) 0.0278(17) Uani 1 1 d . . . H14A H 0.4145 1.0667 0.2860 0.033 Uiso 1 1 calc R . . C15 C 0.5408(8) 1.1006(7) 0.4369(8) 0.0318(19) Uani 1 1 d . . . H15A H 0.4895 1.1017 0.4670 0.038 Uiso 1 1 calc R . . C16 C 0.6591(8) 1.1196(7) 0.5002(7) 0.0285(18) Uani 1 1 d . . . C17 C 0.7337(8) 1.1178(7) 0.4550(7) 0.0304(18) Uani 1 1 d . . . H17A H 0.8153 1.1311 0.4982 0.036 Uiso 1 1 calc R . . C18 C 0.6897(8) 1.0966(7) 0.3477(7) 0.0296(18) Uani 1 1 d . . . H18A H 0.7411 1.0945 0.3179 0.036 Uiso 1 1 calc R . . C19 C 0.7064(9) 1.1394(7) 0.6160(7) 0.0320(19) Uani 1 1 d . . . H19A H 0.7683 1.1064 0.6444 0.038 Uiso 1 1 calc R . . H19B H 0.6420 1.1056 0.6326 0.038 Uiso 1 1 calc R . . C31 C 0.2187(8) 0.1949(7) 0.4228(7) 0.0309(19) Uani 1 1 d . . . C32 C 0.2126(8) 0.3928(8) 0.4015(7) 0.033(2) Uani 1 1 d . . . C33 C 0.3581(8) 0.3682(7) 0.5874(7) 0.0308(19) Uani 1 1 d . . . C34 C 0.1438(9) 0.1140(7) 0.5957(8) 0.036(2) Uani 1 1 d . . . H34A H 0.1809 0.0841 0.5616 0.043 Uiso 1 1 calc R . . C35 C 0.0934(9) 0.0527(8) 0.6468(8) 0.040(2) Uani 1 1 d . . . H35A H 0.0960 -0.0180 0.6477 0.048 Uiso 1 1 calc R . . C36 C 0.0393(8) 0.0960(8) 0.6963(8) 0.038(2) Uani 1 1 d . . . H36A H 0.0020 0.0543 0.7297 0.046 Uiso 1 1 calc R . . C37 C 0.0396(8) 0.1995(8) 0.6971(7) 0.035(2) Uani 1 1 d . . . H37A H 0.0055 0.2314 0.7331 0.042 Uiso 1 1 calc R . . C38 C 0.0911(8) 0.2567(7) 0.6436(7) 0.0294(18) Uani 1 1 d . . . C39 C 0.0959(8) 0.3671(7) 0.6406(7) 0.0308(19) Uani 1 1 d . . . C40 C 0.0635(8) 0.4413(7) 0.6879(8) 0.034(2) Uani 1 1 d . . . H40A H 0.0275 0.4304 0.7322 0.041 Uiso 1 1 calc R . . C41 C 0.0947(8) 0.5338(8) 0.6569(8) 0.036(2) Uani 1 1 d . . . H41A H 0.0837 0.5995 0.6756 0.043 Uiso 1 1 calc R . . C42 C 0.2057(8) 0.5917(7) 0.5569(7) 0.0292(18) Uani 1 1 d . . . H42A H 0.1814 0.6560 0.5593 0.035 Uiso 1 1 calc R . . H42B H 0.1834 0.5603 0.4834 0.035 Uiso 1 1 calc R . . C43 C 0.3398(8) 0.6255(7) 0.6222(7) 0.0273(17) Uani 1 1 d . . . C44 C 0.4129(8) 0.6341(7) 0.5746(7) 0.032(2) Uani 1 1 d . . . H44A H 0.3804 0.6195 0.5009 0.039 Uiso 1 1 calc R . . C45 C 0.5369(8) 0.6649(7) 0.6384(7) 0.0290(18) Uani 1 1 d . . . H45A H 0.5873 0.6696 0.6066 0.035 Uiso 1 1 calc R . . C46 C 0.5843(8) 0.6876(7) 0.7431(7) 0.0321(19) Uani 1 1 d . . . C47 C 0.5096(8) 0.6760(8) 0.7910(7) 0.0299(18) Uani 1 1 d . . . H47A H 0.5419 0.6880 0.8645 0.036 Uiso 1 1 calc R . . C48 C 0.3886(8) 0.6470(7) 0.7291(7) 0.0284(18) Uani 1 1 d . . . H48A H 0.3385 0.6419 0.7612 0.034 Uiso 1 1 calc R . . C49 C 0.7134(8) 0.7198(8) 0.8093(8) 0.036(2) Uani 1 1 d . . . H49B H 0.7502 0.6990 0.7667 0.043 Uiso 1 1 calc R . . H49C H 0.7294 0.6812 0.8654 0.043 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 0.02506(17) 0.02004(17) 0.02474(17) 0.00478(12) 0.00954(13) 0.00831(13) Re2 0.02684(18) 0.02031(18) 0.02787(18) 0.00534(13) 0.00763(14) 0.00852(13) Br1 0.0533(7) 0.0494(7) 0.0471(6) 0.0075(5) 0.0215(5) 0.0104(5) Br2 0.0535(7) 0.0614(8) 0.0540(7) 0.0025(6) 0.0147(6) 0.0171(6) Cl1 0.0229(8) 0.0098(7) 0.0105(7) 0.0024(5) 0.0050(6) 0.0104(6) Cl2 0.0122(7) 0.0089(7) 0.0251(8) 0.0038(6) 0.0002(6) 0.0037(6) O1 0.043(4) 0.025(3) 0.053(4) 0.010(3) 0.023(3) 0.004(3) O01 0.050(7) 0.37(3) 0.073(8) 0.080(13) 0.033(7) 0.062(12) O2 0.029(3) 0.032(3) 0.039(4) 0.006(3) 0.011(3) 0.014(3) O3 0.037(3) 0.031(3) 0.024(3) 0.006(3) 0.011(3) 0.013(3) O4 0.050(4) 0.031(4) 0.042(4) 0.005(3) 0.020(3) 0.016(3) O5 0.055(4) 0.032(4) 0.034(4) 0.011(3) 0.021(3) 0.016(3) O6 0.029(3) 0.029(3) 0.042(4) 0.011(3) 0.008(3) 0.008(3) N1 0.025(3) 0.025(4) 0.019(3) 0.002(3) 0.006(3) 0.008(3) N01 0.026(5) 0.163(15) 0.049(6) 0.040(8) 0.015(5) 0.013(7) N2 0.030(4) 0.020(3) 0.028(4) 0.007(3) 0.012(3) 0.012(3) N3 0.030(4) 0.024(4) 0.022(3) 0.007(3) 0.008(3) 0.011(3) N4 0.026(4) 0.023(4) 0.028(4) 0.005(3) 0.000(3) 0.005(3) N5 0.026(3) 0.022(3) 0.024(3) 0.002(3) 0.003(3) 0.008(3) N6 0.027(4) 0.021(3) 0.034(4) 0.007(3) 0.010(3) 0.010(3) C1 0.029(4) 0.027(5) 0.035(5) 0.004(4) 0.013(4) 0.009(4) C01 0.067(12) 0.14(2) 0.15(2) 0.082(19) 0.000(13) 0.000(13) C2 0.027(4) 0.025(4) 0.018(4) 0.002(3) 0.005(3) 0.004(3) C02 0.054(8) 0.112(13) 0.053(8) 0.031(8) 0.020(7) 0.029(8) C3 0.027(4) 0.024(4) 0.031(4) 0.010(3) 0.013(4) 0.012(3) C03 0.040(8) 0.37(4) 0.039(8) 0.049(15) 0.021(7) 0.061(15) C4 0.032(4) 0.025(4) 0.027(4) 0.008(3) 0.010(4) 0.012(4) C5 0.038(5) 0.025(4) 0.028(4) 0.004(3) 0.011(4) 0.014(4) C6 0.036(5) 0.035(5) 0.029(4) 0.002(4) 0.009(4) 0.020(4) C7 0.025(4) 0.036(5) 0.028(4) 0.006(4) 0.007(3) 0.012(4) C8 0.025(4) 0.027(4) 0.019(4) 0.002(3) 0.007(3) 0.009(3) C9 0.028(4) 0.030(4) 0.024(4) 0.007(3) 0.012(3) 0.009(3) C10 0.034(5) 0.028(5) 0.030(4) 0.007(4) 0.015(4) 0.009(4) C11 0.034(5) 0.029(5) 0.032(5) 0.012(4) 0.016(4) 0.009(4) C12 0.029(4) 0.024(4) 0.027(4) 0.002(3) 0.012(3) 0.009(3) C13 0.026(4) 0.020(4) 0.032(4) 0.005(3) 0.012(3) 0.007(3) C14 0.025(4) 0.026(4) 0.028(4) 0.001(3) 0.010(3) 0.009(3) C15 0.032(5) 0.023(4) 0.038(5) -0.001(4) 0.019(4) 0.004(3) C16 0.036(5) 0.022(4) 0.026(4) 0.003(3) 0.013(4) 0.010(3) C17 0.028(4) 0.028(4) 0.030(4) 0.005(4) 0.010(4) 0.008(3) C18 0.025(4) 0.032(5) 0.028(4) 0.007(4) 0.008(3) 0.010(3) C19 0.036(5) 0.022(4) 0.034(5) 0.000(3) 0.015(4) 0.007(4) C31 0.032(4) 0.024(4) 0.030(4) 0.006(3) 0.007(4) 0.011(4) C32 0.031(5) 0.030(5) 0.033(5) 0.002(4) 0.010(4) 0.012(4) C33 0.033(5) 0.023(4) 0.035(5) 0.007(4) 0.013(4) 0.012(4) C34 0.035(5) 0.024(4) 0.035(5) 0.009(4) 0.001(4) 0.012(4) C35 0.036(5) 0.030(5) 0.036(5) 0.013(4) 0.001(4) 0.006(4) C36 0.028(5) 0.034(5) 0.039(5) 0.017(4) 0.006(4) 0.002(4) C37 0.026(4) 0.038(5) 0.029(4) 0.011(4) 0.007(4) 0.001(4) C38 0.029(4) 0.022(4) 0.029(4) 0.004(3) 0.006(3) 0.008(3) C39 0.024(4) 0.028(4) 0.034(5) 0.009(4) 0.010(4) 0.005(3) C40 0.033(5) 0.026(5) 0.043(5) 0.007(4) 0.016(4) 0.010(4) C41 0.026(4) 0.031(5) 0.043(5) 0.006(4) 0.009(4) 0.010(4) C42 0.026(4) 0.023(4) 0.035(5) 0.010(4) 0.010(4) 0.010(3) C43 0.030(4) 0.019(4) 0.029(4) 0.008(3) 0.009(4) 0.009(3) C44 0.031(5) 0.027(5) 0.024(4) 0.004(3) 0.005(4) 0.002(4) C45 0.028(4) 0.025(4) 0.030(4) 0.002(3) 0.014(4) 0.002(3) C46 0.029(4) 0.025(4) 0.036(5) 0.005(4) 0.011(4) 0.007(3) C47 0.029(4) 0.034(5) 0.025(4) 0.006(4) 0.009(3) 0.014(4) C48 0.032(4) 0.026(4) 0.027(4) 0.007(3) 0.014(4) 0.008(3) C49 0.034(5) 0.026(5) 0.036(5) -0.003(4) 0.011(4) 0.008(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 C3 1.904(9) . ? Re1 C2 1.918(9) . ? Re1 C1 1.925(9) . ? Re1 N2 2.161(7) . ? Re1 N1 2.201(7) . ? Re1 Cl1 2.5428(16) . ? Re2 C32 1.904(10) . ? Re2 C33 1.914(9) . ? Re2 C31 1.917(9) . ? Re2 N5 2.163(8) . ? Re2 N4 2.191(8) . ? Re2 Cl2 2.5313(16) . ? Br1 C19 1.940(9) . ? Br2 C49 1.951(9) . ? O1 C1 1.144(11) . ? O01 C03 1.12(3) . ? O2 C2 1.156(11) . ? O3 C3 1.156(11) . ? O4 C31 1.145(12) . ? O5 C32 1.162(12) . ? O6 C33 1.158(11) . ? N1 C8 1.343(11) . ? N1 C4 1.345(11) . ? N01 C03 1.35(2) . ? N01 C02 1.40(2) . ? N01 C01 1.47(3) . ? N2 C9 1.348(11) . ? N2 N3 1.353(10) . ? N3 C11 1.349(12) . ? N3 C12 1.461(11) . ? N4 C38 1.346(13) . ? N4 C34 1.361(12) . ? N5 C39 1.354(12) . ? N5 N6 1.359(10) . ? N6 C41 1.362(13) . ? N6 C42 1.445(12) . ? C01 H01A 0.9800 . ? C01 H01B 0.9800 . ? C01 H01C 0.9800 . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C02 H02C 0.9800 . ? C03 H03A 0.9500 . ? C4 C5 1.385(13) . ? C4 H4A 0.9500 . ? C5 C6 1.383(15) . ? C5 H5A 0.9500 . ? C6 C7 1.378(13) . ? C6 H6A 0.9500 . ? C7 C8 1.396(13) . ? C7 H7A 0.9500 . ? C8 C9 1.443(12) . ? C9 C10 1.398(13) . ? C10 C11 1.377(13) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.508(12) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.398(12) . ? C13 C14 1.398(13) . ? C14 C15 1.396(13) . ? C14 H14A 0.9500 . ? C15 C16 1.381(13) . ? C15 H15A 0.9500 . ? C16 C17 1.398(13) . ? C16 C19 1.498(12) . ? C17 C18 1.386(13) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C34 C35 1.388(15) . ? C34 H34A 0.9500 . ? C35 C36 1.383(17) . ? C35 H35A 0.9500 . ? C36 C37 1.372(14) . ? C36 H36A 0.9500 . ? C37 C38 1.397(13) . ? C37 H37A 0.9500 . ? C38 C39 1.456(12) . ? C39 C40 1.393(14) . ? C40 C41 1.379(14) . ? C40 H40A 0.9500 . ? C41 H41A 0.9500 . ? C42 C43 1.529(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.375(12) . ? C43 C44 1.394(14) . ? C44 C45 1.421(13) . ? C44 H44A 0.9500 . ? C45 C46 1.347(13) . ? C45 H45A 0.9500 . ? C46 C47 1.415(13) . ? C46 C49 1.480(13) . ? C47 C48 1.388(12) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 H49B 0.9900 . ? C49 H49C 0.9900 . ? 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 88.9(4) . . ? C3 Re1 C1 90.6(4) . . ? C2 Re1 C1 89.7(4) . . ? C3 Re1 N2 93.9(3) . . ? C2 Re1 N2 101.3(3) . . ? C1 Re1 N2 168.2(3) . . ? C3 Re1 N1 95.9(3) . . ? C2 Re1 N1 173.4(3) . . ? C1 Re1 N1 94.8(3) . . ? N2 Re1 N1 73.9(3) . . ? C3 Re1 Cl1 178.9(3) . . ? C2 Re1 Cl1 91.4(2) . . ? C1 Re1 Cl1 90.4(3) . . ? N2 Re1 Cl1 84.98(19) . . ? N1 Re1 Cl1 83.70(18) . . ? C32 Re2 C33 90.4(4) . . ? C32 Re2 C31 89.8(4) . . ? C33 Re2 C31 90.0(4) . . ? C32 Re2 N5 100.3(3) . . ? C33 Re2 N5 94.2(3) . . ? C31 Re2 N5 168.9(4) . . ? C32 Re2 N4 170.7(3) . . ? C33 Re2 N4 97.1(3) . . ? C31 Re2 N4 95.7(4) . . ? N5 Re2 N4 73.6(3) . . ? C32 Re2 Cl2 89.7(3) . . ? C33 Re2 Cl2 179.1(3) . . ? C31 Re2 Cl2 91.0(3) . . ? N5 Re2 Cl2 84.86(19) . . ? N4 Re2 Cl2 82.79(19) . . ? C8 N1 C4 118.6(8) . . ? C8 N1 Re1 116.2(6) . . ? C4 N1 Re1 124.9(6) . . ? C03 N01 C02 121(2) . . ? C03 N01 C01 125(2) . . ? C02 N01 C01 114.4(17) . . ? C9 N2 N3 106.2(7) . . ? C9 N2 Re1 116.8(6) . . ? N3 N2 Re1 136.8(6) . . ? C11 N3 N2 110.8(7) . . ? C11 N3 C12 127.1(8) . . ? N2 N3 C12 121.0(7) . . ? C38 N4 C34 117.6(9) . . ? C38 N4 Re2 117.1(6) . . ? C34 N4 Re2 124.7(7) . . ? C39 N5 N6 105.6(7) . . ? C39 N5 Re2 117.5(6) . . ? N6 N5 Re2 136.7(6) . . ? N5 N6 C41 110.8(8) . . ? N5 N6 C42 121.6(7) . . ? C41 N6 C42 126.8(8) . . ? O1 C1 Re1 176.5(9) . . ? N01 C01 H01A 109.5 . . ? N01 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? N01 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? O2 C2 Re1 179.1(8) . . ? N01 C02 H02A 109.5 . . ? N01 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? N01 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? O3 C3 Re1 179.3(8) . . ? O01 C03 N01 128(3) . . ? O01 C03 H03A 115.9 . . ? N01 C03 H03A 115.9 . . ? N1 C4 C5 122.5(9) . . ? N1 C4 H4A 118.8 . . ? C5 C4 H4A 118.8 . . ? C6 C5 C4 119.0(9) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C7 C6 C5 118.8(9) . . ? C7 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? C6 C7 C8 119.4(9) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? N1 C8 C7 121.7(8) . . ? N1 C8 C9 115.4(8) . . ? C7 C8 C9 122.9(8) . . ? N2 C9 C10 109.9(8) . . ? N2 C9 C8 116.6(8) . . ? C10 C9 C8 133.5(8) . . ? C11 C10 C9 105.5(8) . . ? C11 C10 H10A 127.3 . . ? C9 C10 H10A 127.3 . . ? N3 C11 C10 107.6(8) . . ? N3 C11 H11A 126.2 . . ? C10 C11 H11A 126.2 . . ? N3 C12 C13 112.3(7) . . ? N3 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N3 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C18 C13 C14 118.5(8) . . ? C18 C13 C12 120.8(8) . . ? C14 C13 C12 120.7(8) . . ? C15 C14 C13 120.7(8) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C16 C15 C14 120.4(9) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.3(8) . . ? C15 C16 C19 120.3(8) . . ? C17 C16 C19 120.4(8) . . ? C18 C17 C16 120.6(8) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C13 120.6(9) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C16 C19 Br1 110.0(6) . . ? C16 C19 H19A 109.7 . . ? Br1 C19 H19A 109.7 . . ? C16 C19 H19B 109.7 . . ? Br1 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? O4 C31 Re2 177.7(9) . . ? O5 C32 Re2 178.7(9) . . ? O6 C33 Re2 178.0(9) . . ? N4 C34 C35 122.2(10) . . ? N4 C34 H34A 118.9 . . ? C35 C34 H34A 118.9 . . ? C36 C35 C34 119.0(10) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? C37 C36 C35 119.7(10) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C38 118.4(10) . . ? C36 C37 H37A 120.8 . . ? C38 C37 H37A 120.8 . . ? N4 C38 C37 123.0(9) . . ? N4 C38 C39 114.8(8) . . ? C37 C38 C39 122.2(9) . . ? N5 C39 C40 110.6(8) . . ? N5 C39 C38 115.7(8) . . ? C40 C39 C38 133.6(9) . . ? C41 C40 C39 105.5(9) . . ? C41 C40 H40A 127.3 . . ? C39 C40 H40A 127.3 . . ? N6 C41 C40 107.5(9) . . ? N6 C41 H41A 126.2 . . ? C40 C41 H41A 126.2 . . ? N6 C42 C43 111.7(7) . . ? N6 C42 H42A 109.3 . . ? C43 C42 H42A 109.3 . . ? N6 C42 H42B 109.3 . . ? C43 C42 H42B 109.3 . . ? H42A C42 H42B 107.9 . . ? C48 C43 C44 119.7(8) . . ? C48 C43 C42 119.6(8) . . ? C44 C43 C42 120.8(8) . . ? C43 C44 C45 118.8(8) . . ? C43 C44 H44A 120.6 . . ? C45 C44 H44A 120.6 . . ? C46 C45 C44 121.2(9) . . ? C46 C45 H45A 119.4 . . ? C44 C45 H45A 119.4 . . ? C45 C46 C47 119.8(8) . . ? C45 C46 C49 121.1(9) . . ? C47 C46 C49 119.0(9) . . ? C48 C47 C46 119.1(8) . . ? C48 C47 H47A 120.4 . . ? C46 C47 H47A 120.4 . . ? C43 C48 C47 121.3(9) . . ? C43 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C46 C49 Br2 111.3(7) . . ? C46 C49 H49B 109.4 . . ? Br2 C49 H49B 109.4 . . ? C46 C49 H49C 109.4 . . ? Br2 C49 H49C 109.4 . . ? H49B C49 H49C 108.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.706 _refine_diff_density_min -3.520 _refine_diff_density_rms 0.261 #===END data_Compoumd_2 _database_code_depnum_ccdc_archive 'CCDC 806768' #TrackingRef '- crystal data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H20 Cl N6 O3 Re' _chemical_formula_weight 698.14 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.360(2) _cell_length_b 10.530(2) _cell_length_c 12.400(3) _cell_angle_alpha 72.32(3) _cell_angle_beta 85.05(3) _cell_angle_gamma 69.03(3) _cell_volume 1203.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4735 _cell_measurement_theta_min 3.1403 _cell_measurement_theta_max 28.2340 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas 1.927 _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 5.206 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8370 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10282 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 28.25 _reflns_number_total 5640 _reflns_number_gt 5459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0243P)^2^+1.1728P] 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 5640 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.664404(14) 0.439030(14) 1.337181(11) 0.03452(6) Uani 1 1 d . . . Cl1 Cl -0.48460(11) 0.53803(11) 1.27644(10) 0.0503(2) Uani 1 1 d . . . N2 N -0.5863(3) 0.3296(3) 1.2122(3) 0.0342(6) Uani 1 1 d . . . C3 C -0.8158(5) 0.3747(5) 1.3744(4) 0.0531(11) Uani 1 1 d . . . N3 N -0.5029(3) 0.2015(3) 1.2108(3) 0.0368(7) Uani 1 1 d . . . N1 N -0.7557(3) 0.5851(3) 1.1778(3) 0.0398(7) Uani 1 1 d . . . C1 C -0.5690(4) 0.3033(4) 1.4674(3) 0.0447(9) Uani 1 1 d . . . N6 N 0.1914(3) 0.0218(4) 1.2610(3) 0.0431(8) Uani 1 1 d . . . N4 N 0.2996(4) 0.1640(4) 0.9024(3) 0.0451(8) Uani 1 1 d . . . C2 C -0.7368(5) 0.5620(4) 1.4275(4) 0.0493(10) Uani 1 1 d . . . C16 C -0.6189(4) 0.4025(4) 1.1059(3) 0.0368(8) Uani 1 1 d . . . N5 N 0.1457(3) 0.1344(4) 1.1718(3) 0.0464(8) Uani 1 1 d . . . C30 C 0.2323(4) 0.1062(4) 1.0915(3) 0.0369(8) Uani 1 1 d . . . O2 O -0.7786(4) 0.6347(4) 1.4822(3) 0.0780(12) Uani 1 1 d . . . C23 C -0.0245(4) 0.0374(4) 1.3557(3) 0.0413(8) Uani 1 1 d . . . C35 C 0.2148(4) 0.2066(4) 0.9799(3) 0.0391(8) Uani 1 1 d . . . C25 C -0.2585(4) 0.1849(4) 1.3219(4) 0.0445(9) Uani 1 1 d . . . H25A H -0.3256 0.2751 1.3083 0.053 Uiso 1 1 calc R . . O1 O -0.5147(4) 0.2217(4) 1.5467(3) 0.0677(10) Uani 1 1 d . . . C24 C -0.1246(4) 0.1674(4) 1.3352(3) 0.0441(9) Uani 1 1 d . . . H24A H -0.1007 0.2461 1.3301 0.053 Uiso 1 1 calc R . . C22 C -0.0639(4) -0.0749(4) 1.3653(4) 0.0482(10) Uani 1 1 d . . . H22A H 0.0026 -0.1657 1.3818 0.058 Uiso 1 1 calc R . . C14 C -0.7551(5) 0.6345(5) 0.9793(4) 0.0511(10) Uani 1 1 d . . . H14A H -0.7243 0.6043 0.9155 0.061 Uiso 1 1 calc R . . C17 C -0.5551(4) 0.3213(5) 1.0358(3) 0.0450(9) Uani 1 1 d . . . H17A H -0.5609 0.3484 0.9571 0.054 Uiso 1 1 calc R . . C15 C -0.7128(4) 0.5449(4) 1.0850(3) 0.0389(8) Uani 1 1 d . . . C20 C -0.2954(4) 0.0726(4) 1.3282(3) 0.0377(8) Uani 1 1 d . . . C28 C 0.3036(4) -0.0741(4) 1.2382(3) 0.0437(9) Uani 1 1 d . . . H28A H 0.3530 -0.1613 1.2884 0.052 Uiso 1 1 calc R . . C29 C 0.3340(4) -0.0247(4) 1.1309(4) 0.0472(9) Uani 1 1 d . . . H29A H 0.4079 -0.0689 1.0912 0.057 Uiso 1 1 calc R . . C26 C 0.1218(4) 0.0186(5) 1.3666(3) 0.0480(10) Uani 1 1 d . . . H26A H 0.1281 0.0936 1.3936 0.058 Uiso 1 1 calc R . . H26B H 0.1677 -0.0716 1.4223 0.058 Uiso 1 1 calc R . . C19 C -0.4407(4) 0.0908(4) 1.3110(4) 0.0432(9) Uani 1 1 d . . . H19A H -0.4451 0.0021 1.3063 0.052 Uiso 1 1 calc R . . H19B H -0.4931 0.1123 1.3759 0.052 Uiso 1 1 calc R . . C18 C -0.4827(4) 0.1943(5) 1.1053(4) 0.0463(9) Uani 1 1 d . . . H18A H -0.4278 0.1149 1.0836 0.056 Uiso 1 1 calc R . . C34 C 0.1160(4) 0.3389(5) 0.9580(4) 0.0507(10) Uani 1 1 d . . . H34A H 0.0579 0.3667 1.0146 0.061 Uiso 1 1 calc R . . C21 C -0.1966(5) -0.0582(4) 1.3515(4) 0.0476(10) Uani 1 1 d . . . H21A H -0.2208 -0.1372 1.3580 0.057 Uiso 1 1 calc R . . C33 C 0.1047(5) 0.4284(5) 0.8521(4) 0.0576(11) Uani 1 1 d . . . H33A H 0.0370 0.5186 0.8343 0.069 Uiso 1 1 calc R . . C13 C -0.8428(5) 0.7683(5) 0.9692(4) 0.0655(14) Uani 1 1 d . . . H13A H -0.8729 0.8321 0.8981 0.079 Uiso 1 1 calc R . . C32 C 0.1914(5) 0.3865(5) 0.7728(4) 0.0589(12) Uani 1 1 d . . . H32A H 0.1853 0.4468 0.6994 0.071 Uiso 1 1 calc R . . C11 C -0.8420(5) 0.7157(4) 1.1655(4) 0.0563(11) Uani 1 1 d . . . H11A H -0.8733 0.7448 1.2297 0.068 Uiso 1 1 calc R . . C31 C 0.2877(5) 0.2549(5) 0.8020(4) 0.0545(11) Uani 1 1 d . . . H31A H 0.3495 0.2273 0.7474 0.065 Uiso 1 1 calc R . . C12 C -0.8861(6) 0.8082(5) 1.0631(5) 0.0690(14) Uani 1 1 d . . . H12A H -0.9468 0.9000 1.0571 0.083 Uiso 1 1 calc R . . O3 O -0.9024(4) 0.3431(4) 1.3995(4) 0.0860(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 0.03648(8) 0.02916(8) 0.03063(8) -0.00229(5) -0.00287(6) -0.00754(6) Cl1 0.0481(5) 0.0418(5) 0.0588(6) -0.0078(4) -0.0030(5) -0.0178(4) N2 0.0360(15) 0.0284(14) 0.0349(16) -0.0055(12) -0.0033(12) -0.0096(12) C3 0.045(2) 0.046(2) 0.048(2) 0.0054(19) 0.0025(19) -0.0083(19) N3 0.0362(16) 0.0325(15) 0.0409(17) -0.0102(13) -0.0020(13) -0.0108(12) N1 0.0402(16) 0.0315(15) 0.0390(17) 0.0015(13) -0.0117(14) -0.0093(13) C1 0.048(2) 0.042(2) 0.038(2) -0.0074(17) -0.0024(17) -0.0110(17) N6 0.0339(16) 0.0515(19) 0.0326(16) -0.0050(14) 0.0015(13) -0.0079(14) N4 0.0478(19) 0.0489(19) 0.0401(18) -0.0153(15) 0.0118(15) -0.0190(16) C2 0.049(2) 0.038(2) 0.044(2) -0.0027(18) -0.0061(19) -0.0016(17) C16 0.0358(18) 0.0441(19) 0.0302(18) -0.0051(15) -0.0028(14) -0.0175(15) N5 0.0401(18) 0.0497(19) 0.0341(17) -0.0045(15) 0.0001(14) -0.0042(15) C30 0.0314(17) 0.044(2) 0.0349(19) -0.0121(16) 0.0029(14) -0.0129(15) O2 0.092(3) 0.061(2) 0.063(2) -0.034(2) -0.007(2) 0.009(2) C23 0.043(2) 0.049(2) 0.0247(17) -0.0092(16) 0.0033(15) -0.0091(17) C35 0.0379(19) 0.045(2) 0.037(2) -0.0111(16) -0.0004(15) -0.0185(16) C25 0.040(2) 0.0308(17) 0.053(2) -0.0094(17) 0.0015(17) -0.0042(15) O1 0.084(2) 0.058(2) 0.0374(17) 0.0067(15) -0.0206(16) -0.0096(18) C24 0.047(2) 0.0380(19) 0.045(2) -0.0087(17) 0.0018(17) -0.0153(17) C22 0.048(2) 0.036(2) 0.048(2) -0.0112(18) -0.0008(18) -0.0012(17) C14 0.050(2) 0.057(3) 0.039(2) 0.0031(19) -0.0116(18) -0.021(2) C17 0.044(2) 0.059(2) 0.036(2) -0.0161(19) 0.0009(17) -0.0213(19) C15 0.0361(18) 0.0425(19) 0.036(2) -0.0030(16) -0.0083(15) -0.0168(16) C20 0.0405(19) 0.0310(17) 0.0345(19) -0.0070(14) 0.0007(15) -0.0062(15) C28 0.0361(19) 0.043(2) 0.042(2) -0.0072(17) -0.0026(16) -0.0060(16) C29 0.040(2) 0.047(2) 0.048(2) -0.0133(19) 0.0054(17) -0.0080(17) C26 0.044(2) 0.059(2) 0.0302(19) -0.0057(18) -0.0010(16) -0.0120(19) C19 0.043(2) 0.0288(17) 0.050(2) -0.0043(16) -0.0004(17) -0.0093(15) C18 0.044(2) 0.054(2) 0.048(2) -0.028(2) 0.0074(18) -0.0167(19) C34 0.046(2) 0.052(2) 0.044(2) -0.0102(19) 0.0060(18) -0.0100(19) C21 0.051(2) 0.0335(19) 0.052(2) -0.0120(18) -0.0036(19) -0.0064(17) C33 0.056(3) 0.052(3) 0.053(3) -0.004(2) 0.000(2) -0.016(2) C13 0.064(3) 0.055(3) 0.056(3) 0.016(2) -0.025(2) -0.018(2) C32 0.072(3) 0.065(3) 0.040(2) -0.004(2) 0.005(2) -0.034(3) C11 0.063(3) 0.036(2) 0.055(3) -0.0030(19) -0.018(2) -0.0032(19) C31 0.066(3) 0.064(3) 0.041(2) -0.019(2) 0.015(2) -0.032(2) C12 0.076(3) 0.040(2) 0.064(3) 0.008(2) -0.025(3) -0.003(2) O3 0.073(3) 0.077(3) 0.102(3) -0.001(2) -0.006(2) -0.039(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 C1 1.868(4) . ? Re1 C2 1.880(5) . ? Re1 C3 1.891(5) . ? Re1 N2 2.142(3) . ? Re1 N1 2.145(3) . ? Re1 Cl1 2.4073(12) . ? N2 C16 1.311(5) . ? N2 N3 1.320(4) . ? C3 O3 1.056(6) . ? N3 C18 1.327(5) . ? N3 C19 1.427(5) . ? N1 C11 1.315(5) . ? N1 C15 1.332(5) . ? C1 O1 1.122(5) . ? N6 C28 1.314(5) . ? N6 N5 1.321(5) . ? N6 C26 1.437(5) . ? N4 C31 1.303(6) . ? N4 C35 1.316(5) . ? C2 O2 1.124(5) . ? C16 C17 1.368(6) . ? C16 C15 1.423(5) . ? N5 C30 1.311(5) . ? C30 C29 1.374(5) . ? C30 C35 1.443(5) . ? C23 C22 1.352(6) . ? C23 C24 1.353(5) . ? C23 C26 1.469(6) . ? C35 C34 1.364(6) . ? C25 C20 1.347(5) . ? C25 C24 1.350(6) . ? C25 H25A 0.9300 . ? C24 H24A 0.9300 . ? C22 C21 1.342(6) . ? C22 H22A 0.9300 . ? C14 C13 1.350(7) . ? C14 C15 1.361(5) . ? C14 H14A 0.9300 . ? C17 C18 1.337(6) . ? C17 H17A 0.9300 . ? C20 C21 1.352(5) . ? C20 C19 1.474(5) . ? C28 C29 1.328(6) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C18 H18A 0.9300 . ? C34 C33 1.350(6) . ? C34 H34A 0.9300 . ? C21 H21A 0.9300 . ? C33 C32 1.340(7) . ? C33 H33A 0.9300 . ? C13 C12 1.344(8) . ? C13 H13A 0.9300 . ? C32 C31 1.347(7) . ? C32 H32A 0.9300 . ? C11 C12 1.341(6) . ? C11 H11A 0.9300 . ? C31 H31A 0.9300 . ? C12 H12A 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 C1 Re1 C2 86.76(18) . . ? C1 Re1 C3 89.77(19) . . ? C2 Re1 C3 89.4(2) . . ? C1 Re1 N2 101.38(15) . . ? C2 Re1 N2 170.75(14) . . ? C3 Re1 N2 95.00(18) . . ? C1 Re1 N1 173.95(15) . . ? C2 Re1 N1 98.29(15) . . ? C3 Re1 N1 93.59(16) . . ? N2 Re1 N1 73.33(12) . . ? C1 Re1 Cl1 95.30(14) . . ? C2 Re1 Cl1 90.25(15) . . ? C3 Re1 Cl1 174.88(13) . . ? N2 Re1 Cl1 84.68(9) . . ? N1 Re1 Cl1 81.42(9) . . ? C16 N2 N3 105.6(3) . . ? C16 N2 Re1 117.6(2) . . ? N3 N2 Re1 136.7(2) . . ? O3 C3 Re1 175.8(5) . . ? N2 N3 C18 110.7(3) . . ? N2 N3 C19 122.9(3) . . ? C18 N3 C19 126.3(3) . . ? C11 N1 C15 118.2(4) . . ? C11 N1 Re1 123.9(3) . . ? C15 N1 Re1 117.6(2) . . ? O1 C1 Re1 178.3(4) . . ? C28 N6 N5 111.4(3) . . ? C28 N6 C26 128.6(4) . . ? N5 N6 C26 120.0(3) . . ? C31 N4 C35 117.3(4) . . ? O2 C2 Re1 179.2(4) . . ? N2 C16 C17 110.9(4) . . ? N2 C16 C15 116.4(3) . . ? C17 C16 C15 132.6(4) . . ? C30 N5 N6 105.1(3) . . ? N5 C30 C29 110.6(4) . . ? N5 C30 C35 120.9(3) . . ? C29 C30 C35 128.5(4) . . ? C22 C23 C24 117.6(4) . . ? C22 C23 C26 121.0(4) . . ? C24 C23 C26 121.3(4) . . ? N4 C35 C34 122.6(4) . . ? N4 C35 C30 116.5(4) . . ? C34 C35 C30 120.9(4) . . ? C20 C25 C24 120.5(4) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C24 C23 121.2(4) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C21 C22 C23 121.5(4) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C13 C14 C15 118.4(5) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C18 C17 C16 104.8(4) . . ? C18 C17 H17A 127.6 . . ? C16 C17 H17A 127.6 . . ? N1 C15 C14 122.1(4) . . ? N1 C15 C16 114.5(3) . . ? C14 C15 C16 123.4(4) . . ? C25 C20 C21 118.7(4) . . ? C25 C20 C19 121.0(3) . . ? C21 C20 C19 120.3(4) . . ? N6 C28 C29 108.1(4) . . ? N6 C28 H28A 126.0 . . ? C29 C28 H28A 126.0 . . ? C28 C29 C30 104.9(4) . . ? C28 C29 H29A 127.6 . . ? C30 C29 H29A 127.6 . . ? N6 C26 C23 112.1(3) . . ? N6 C26 H26A 109.2 . . ? C23 C26 H26A 109.2 . . ? N6 C26 H26B 109.2 . . ? C23 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? N3 C19 C20 112.7(3) . . ? N3 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N3 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N3 C18 C17 108.0(4) . . ? N3 C18 H18A 126.0 . . ? C17 C18 H18A 126.0 . . ? C33 C34 C35 118.2(4) . . ? C33 C34 H34A 120.9 . . ? C35 C34 H34A 120.9 . . ? C22 C21 C20 120.4(4) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C32 C33 C34 119.7(5) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C33 C32 C31 118.3(4) . . ? C33 C32 H32A 120.8 . . ? C31 C32 H32A 120.8 . . ? N1 C11 C12 121.9(5) . . ? N1 C11 H11A 119.0 . . ? C12 C11 H11A 119.0 . . ? N4 C31 C32 123.9(4) . . ? N4 C31 H31A 118.0 . . ? C32 C31 H31A 118.0 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.782 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.095 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Sheldrick G.M.(1997), The SHELX-97 Manual ;