# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Michael David Ward' 'Andrea Barbieri' 'Francesco Barigelletti' 'Zoe R. Bell' 'Nail M. Shavaleev' _publ_contact_author_name 'Prof Michael David Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Brook Hill Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; New ligands in the 2,2'-dipyridylamine series and their Re(I) complexes; synthesis, structures and luminescence properties ; data_test _database_code_depnum_ccdc_archive 'CCDC 222972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H39 Cl N3 O10 Re' _chemical_formula_sum 'C33 H39 Cl N3 O10 Re' _chemical_formula_weight 859.32 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 11.170(4) _cell_length_b 11.937(4) _cell_length_c 16.536(5) _cell_angle_alpha 74.20(3) _cell_angle_beta 80.21(4) _cell_angle_gamma 62.56(2) _cell_volume 1880.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 0.835189 _cell_measurement_theta_max 1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 3.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.25 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21637 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8612 _reflns_number_gt 7322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0278P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8612 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 0.258276(17) -0.354052(15) 0.328174(11) 0.01270(5) Uani 1 1 d . . . Cl1 Cl 0.11197(11) -0.29546(10) 0.45350(7) 0.0248(2) Uani 1 1 d . . . O31 O 0.4959(3) -0.5667(3) 0.4325(2) 0.0272(7) Uani 1 1 d . . . O41 O 0.1732(3) -0.5630(3) 0.3246(2) 0.0301(8) Uani 1 1 d . . . O51 O 0.4364(3) -0.4161(3) 0.1711(2) 0.0278(7) Uani 1 1 d . . . O71 O 0.4402(3) -0.0748(2) -0.10078(17) 0.0146(6) Uani 1 1 d . . . O74 O 0.4375(3) -0.1814(3) -0.22981(18) 0.0208(7) Uani 1 1 d . . . O77 O 0.3684(3) -0.0276(3) -0.40407(18) 0.0225(7) Uani 1 1 d . . . O80 O 0.2531(3) 0.2391(3) -0.41040(18) 0.0214(7) Uani 1 1 d . . . O83 O 0.2411(3) 0.3604(3) -0.28742(18) 0.0184(6) Uani 1 1 d . . . O86 O 0.3450(3) 0.1758(2) -0.12945(17) 0.0157(6) Uani 1 1 d . . . N1 N 0.2386(3) -0.0950(3) 0.1856(2) 0.0141(7) Uani 1 1 d . . . N11 N 0.3015(3) -0.1931(3) 0.3267(2) 0.0133(7) Uani 1 1 d . . . N21 N 0.0945(3) -0.1929(3) 0.2557(2) 0.0133(7) Uani 1 1 d . . . C12 C 0.3089(4) -0.1105(4) 0.2541(3) 0.0152(8) Uani 1 1 d . . . C13 C 0.3894(4) -0.0464(4) 0.2460(3) 0.0192(9) Uani 1 1 d . . . H13A H 0.4019 0.0035 0.1942 0.023 Uiso 1 1 calc R . . C14 C 0.4501(4) -0.0577(4) 0.3152(3) 0.0211(10) Uani 1 1 d . . . H14A H 0.5064 -0.0178 0.3102 0.025 Uiso 1 1 calc R . . C15 C 0.4273(4) -0.1287(4) 0.3928(3) 0.0188(9) Uani 1 1 d . . . H15A H 0.4607 -0.1309 0.4413 0.023 Uiso 1 1 calc R . . C16 C 0.3539(4) -0.1955(4) 0.3957(3) 0.0154(8) Uani 1 1 d . . . H16A H 0.3393 -0.2446 0.4472 0.018 Uiso 1 1 calc R . . C22 C 0.1125(4) -0.1008(4) 0.1943(2) 0.0132(8) Uani 1 1 d . . . C23 C 0.0115(5) -0.0147(4) 0.1392(3) 0.0216(10) Uani 1 1 d . . . H23A H 0.0273 0.0443 0.0943 0.026 Uiso 1 1 calc R . . C24 C -0.1115(5) -0.0174(4) 0.1517(3) 0.0266(11) Uani 1 1 d . . . H24A H -0.1799 0.0408 0.1155 0.032 Uiso 1 1 calc R . . C25 C -0.1348(4) -0.1059(4) 0.2178(3) 0.0213(10) Uani 1 1 d . . . H25A H -0.2188 -0.1071 0.2279 0.026 Uiso 1 1 calc R . . C26 C -0.0297(4) -0.1918(4) 0.2678(3) 0.0177(9) Uani 1 1 d . . . H26A H -0.0437 -0.2525 0.3122 0.021 Uiso 1 1 calc R . . C31 C 0.4051(5) -0.4856(4) 0.3943(3) 0.0186(9) Uani 1 1 d . . . C41 C 0.2044(4) -0.4839(4) 0.3267(3) 0.0197(9) Uani 1 1 d . . . C51 C 0.3712(4) -0.3905(4) 0.2261(3) 0.0181(9) Uani 1 1 d . . . C61 C 0.2658(4) -0.0207(4) 0.1055(2) 0.0146(8) Uani 1 1 d . . . C62 C 0.3427(4) -0.0871(4) 0.0432(2) 0.0119(8) Uani 1 1 d . . . H62A H 0.3770 -0.1767 0.0540 0.014 Uiso 1 1 calc R . . C63 C 0.3678(4) -0.0197(4) -0.0344(3) 0.0142(8) Uani 1 1 d . . . C64 C 0.3170(4) 0.1161(4) -0.0509(3) 0.0155(8) Uani 1 1 d . . . C65 C 0.2432(4) 0.1804(4) 0.0128(3) 0.0165(9) Uani 1 1 d . . . H65A H 0.2114 0.2696 0.0032 0.020 Uiso 1 1 calc R . . C66 C 0.2165(4) 0.1116(4) 0.0908(3) 0.0171(9) Uani 1 1 d . . . H66A H 0.1656 0.1551 0.1327 0.021 Uiso 1 1 calc R . . C72 C 0.4839(4) -0.2110(4) -0.0892(3) 0.0169(9) Uani 1 1 d . . . H72A H 0.4081 -0.2320 -0.0697 0.020 Uiso 1 1 calc R . . H72B H 0.5518 -0.2587 -0.0476 0.020 Uiso 1 1 calc R . . C73 C 0.5415(4) -0.2472(4) -0.1719(3) 0.0178(9) Uani 1 1 d . . . H73A H 0.6148 -0.2229 -0.1925 0.021 Uiso 1 1 calc R . . H73B H 0.5768 -0.3400 -0.1653 0.021 Uiso 1 1 calc R . . C75 C 0.4744(5) -0.2273(4) -0.3051(3) 0.0291(11) Uani 1 1 d . . . H75A H 0.4899 -0.3170 -0.2928 0.035 Uiso 1 1 calc R . . H75B H 0.5572 -0.2222 -0.3306 0.035 Uiso 1 1 calc R . . C76 C 0.3623(5) -0.1456(4) -0.3644(3) 0.0283(11) Uani 1 1 d . . . H76A H 0.3703 -0.1917 -0.4066 0.034 Uiso 1 1 calc R . . H76B H 0.2759 -0.1284 -0.3336 0.034 Uiso 1 1 calc R . . C78 C 0.2473(4) 0.0622(4) -0.4460(3) 0.0213(10) Uani 1 1 d . . . H78A H 0.1697 0.0710 -0.4070 0.026 Uiso 1 1 calc R . . H78B H 0.2395 0.0304 -0.4920 0.026 Uiso 1 1 calc R . . C79 C 0.2493(5) 0.1908(4) -0.4792(3) 0.0232(10) Uani 1 1 d . . . H79A H 0.3280 0.1819 -0.5172 0.028 Uiso 1 1 calc R . . H79B H 0.1692 0.2505 -0.5103 0.028 Uiso 1 1 calc R . . C81 C 0.2008(5) 0.3764(4) -0.4287(3) 0.0222(10) Uani 1 1 d . . . H81A H 0.1037 0.4152 -0.4176 0.027 Uiso 1 1 calc R . . H81B H 0.2201 0.4084 -0.4876 0.027 Uiso 1 1 calc R . . C82 C 0.2671(5) 0.4112(4) -0.3736(2) 0.0189(9) Uani 1 1 d . . . H82A H 0.3637 0.3756 -0.3869 0.023 Uiso 1 1 calc R . . H82B H 0.2317 0.5046 -0.3839 0.023 Uiso 1 1 calc R . . C84 C 0.3273(4) 0.3643(4) -0.2354(3) 0.0193(9) Uani 1 1 d . . . H84A H 0.3147 0.4526 -0.2434 0.023 Uiso 1 1 calc R . . H84B H 0.4209 0.3116 -0.2504 0.023 Uiso 1 1 calc R . . C85 C 0.2943(4) 0.3140(4) -0.1449(3) 0.0170(9) Uani 1 1 d . . . H85A H 0.3353 0.3360 -0.1082 0.020 Uiso 1 1 calc R . . H85B H 0.1973 0.3532 -0.1334 0.020 Uiso 1 1 calc R . . C202 C 0.2687(7) -0.4243(6) -0.0176(4) 0.0549(17) Uani 1 1 d . . . H20C H 0.2774 -0.4050 -0.0786 0.066 Uiso 1 1 calc R . . H20D H 0.3557 -0.4515 0.0041 0.066 Uiso 1 1 calc R . . C203 C 0.1656(7) -0.3105(6) 0.0127(5) 0.074(2) Uani 1 1 d . . . H20G H 0.0973 -0.2558 -0.0283 0.088 Uiso 1 1 calc R . . H20H H 0.2059 -0.2600 0.0240 0.088 Uiso 1 1 calc R . . C204 C 0.1064(6) -0.3662(6) 0.0916(4) 0.0509(17) Uani 1 1 d . . . H20A H 0.1563 -0.3841 0.1398 0.061 Uiso 1 1 calc R . . H20B H 0.0124 -0.3082 0.1014 0.061 Uiso 1 1 calc R . . C205 C 0.1196(7) -0.4864(6) 0.0751(5) 0.063(2) Uani 1 1 d . . . H20E H 0.1413 -0.5542 0.1260 0.076 Uiso 1 1 calc R . . H20F H 0.0355 -0.4727 0.0559 0.076 Uiso 1 1 calc R . . O201 O 0.2239(4) -0.5222(4) 0.0126(3) 0.0599(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 0.01409(9) 0.01189(8) 0.01058(8) -0.00170(5) -0.00098(6) -0.00471(6) Cl1 0.0244(6) 0.0266(6) 0.0200(6) -0.0020(4) -0.0008(5) -0.0101(5) O31 0.032(2) 0.0203(16) 0.0254(19) -0.0046(13) -0.0122(16) -0.0052(15) O41 0.038(2) 0.0233(17) 0.035(2) -0.0040(14) -0.0020(16) -0.0193(16) O51 0.034(2) 0.0290(18) 0.0254(19) -0.0023(15) -0.0060(17) -0.0181(16) O71 0.0202(16) 0.0124(13) 0.0112(14) -0.0024(11) 0.0020(12) -0.0080(12) O74 0.0243(17) 0.0206(15) 0.0139(16) -0.0064(12) -0.0018(13) -0.0050(13) O77 0.0232(17) 0.0222(16) 0.0173(17) -0.0027(12) -0.0062(14) -0.0050(13) O80 0.0325(19) 0.0180(15) 0.0168(16) -0.0007(12) -0.0051(14) -0.0139(14) O83 0.0216(16) 0.0221(15) 0.0127(15) 0.0009(12) -0.0015(13) -0.0130(13) O86 0.0196(16) 0.0131(14) 0.0125(15) -0.0004(11) -0.0002(12) -0.0071(12) N1 0.0161(18) 0.0134(16) 0.0125(18) -0.0005(13) 0.0004(14) -0.0079(14) N11 0.0123(18) 0.0149(17) 0.0108(18) -0.0055(13) 0.0001(14) -0.0032(14) N21 0.0126(18) 0.0149(16) 0.0111(18) -0.0041(13) -0.0012(14) -0.0041(14) C12 0.013(2) 0.0139(19) 0.014(2) -0.0028(15) -0.0031(17) -0.0009(16) C13 0.019(2) 0.017(2) 0.018(2) -0.0019(17) -0.0032(18) -0.0047(18) C14 0.018(2) 0.017(2) 0.028(3) -0.0030(18) -0.003(2) -0.0080(18) C15 0.020(2) 0.021(2) 0.018(2) -0.0098(17) -0.0074(19) -0.0052(18) C16 0.012(2) 0.020(2) 0.011(2) -0.0037(16) -0.0015(17) -0.0036(17) C22 0.012(2) 0.0159(19) 0.011(2) -0.0055(15) 0.0005(16) -0.0046(16) C23 0.026(3) 0.019(2) 0.018(2) 0.0046(17) -0.0065(19) -0.0111(19) C24 0.018(2) 0.026(2) 0.031(3) -0.002(2) -0.011(2) -0.004(2) C25 0.016(2) 0.027(2) 0.023(2) -0.0089(19) -0.0011(19) -0.0098(19) C26 0.016(2) 0.022(2) 0.015(2) -0.0073(17) 0.0057(18) -0.0084(18) C31 0.024(2) 0.018(2) 0.015(2) -0.0046(17) -0.0034(19) -0.0093(19) C41 0.022(2) 0.015(2) 0.017(2) 0.0018(16) -0.0037(19) -0.0064(18) C51 0.013(2) 0.0079(19) 0.034(3) -0.0072(18) -0.007(2) -0.0023(16) C61 0.017(2) 0.017(2) 0.010(2) -0.0007(15) -0.0019(17) -0.0081(17) C62 0.0086(19) 0.0126(19) 0.013(2) -0.0040(15) -0.0015(16) -0.0024(15) C63 0.013(2) 0.018(2) 0.013(2) -0.0056(16) -0.0033(17) -0.0069(17) C64 0.016(2) 0.015(2) 0.016(2) -0.0005(16) -0.0049(17) -0.0078(17) C65 0.020(2) 0.0125(19) 0.016(2) -0.0024(16) -0.0056(18) -0.0051(17) C66 0.018(2) 0.016(2) 0.014(2) -0.0066(16) 0.0008(18) -0.0039(17) C72 0.020(2) 0.0132(19) 0.015(2) -0.0005(16) -0.0034(18) -0.0058(17) C73 0.021(2) 0.014(2) 0.014(2) -0.0022(16) -0.0020(18) -0.0040(17) C75 0.042(3) 0.020(2) 0.018(2) -0.0116(18) -0.003(2) -0.003(2) C76 0.044(3) 0.021(2) 0.020(3) -0.0084(19) -0.007(2) -0.011(2) C78 0.020(2) 0.027(2) 0.016(2) -0.0089(18) -0.0021(19) -0.0067(19) C79 0.020(2) 0.027(2) 0.017(2) -0.0037(18) -0.0014(19) -0.0056(19) C81 0.030(3) 0.020(2) 0.013(2) 0.0045(17) -0.006(2) -0.010(2) C82 0.027(2) 0.017(2) 0.009(2) 0.0045(16) -0.0004(18) -0.0105(19) C84 0.022(2) 0.017(2) 0.020(2) 0.0006(17) -0.0022(19) -0.0111(18) C85 0.021(2) 0.0116(19) 0.017(2) -0.0019(16) 0.0004(18) -0.0067(17) C202 0.061(4) 0.058(4) 0.047(4) -0.010(3) 0.014(3) -0.033(4) C203 0.065(5) 0.025(3) 0.125(7) -0.016(4) 0.011(5) -0.019(3) C204 0.030(3) 0.076(4) 0.063(4) -0.047(4) 0.004(3) -0.021(3) C205 0.049(4) 0.041(3) 0.084(5) -0.012(3) 0.026(4) -0.019(3) O201 0.057(3) 0.041(2) 0.092(4) -0.041(2) 0.039(3) -0.030(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 C31 1.911(4) . ? Re1 C41 1.911(4) . ? Re1 C51 1.950(5) . ? Re1 N21 2.175(3) . ? Re1 N11 2.179(3) . ? Re1 Cl1 2.4575(16) . ? O31 C31 1.159(5) . ? O41 C41 1.156(5) . ? O51 C51 1.082(5) . ? O71 C63 1.375(5) . ? O71 C72 1.432(4) . ? O74 C75 1.417(5) . ? O74 C73 1.418(5) . ? O77 C76 1.410(5) . ? O77 C78 1.428(5) . ? O80 C81 1.424(5) . ? O80 C79 1.424(5) . ? O83 C84 1.419(5) . ? O83 C82 1.427(5) . ? O86 C64 1.363(5) . ? O86 C85 1.437(4) . ? N1 C12 1.411(5) . ? N1 C22 1.423(5) . ? N1 C61 1.451(5) . ? N11 C12 1.349(5) . ? N11 C16 1.355(5) . ? N21 C22 1.344(5) . ? N21 C26 1.362(5) . ? C12 C13 1.396(6) . ? C13 C14 1.373(6) . ? C14 C15 1.387(6) . ? C15 C16 1.371(6) . ? C22 C23 1.390(6) . ? C23 C24 1.368(6) . ? C24 C25 1.380(6) . ? C25 C26 1.368(6) . ? C61 C66 1.375(5) . ? C61 C62 1.394(5) . ? C62 C63 1.377(5) . ? C63 C64 1.410(5) . ? C64 C65 1.392(6) . ? C65 C66 1.394(6) . ? C72 C73 1.495(6) . ? C75 C76 1.501(6) . ? C78 C79 1.492(6) . ? C81 C82 1.506(6) . ? C84 C85 1.504(6) . ? C202 O201 1.414(7) . ? C202 C203 1.468(8) . ? C203 C204 1.491(9) . ? C204 C205 1.469(8) . ? C205 O201 1.407(7) . ? 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 C31 Re1 C41 88.20(18) . . ? C31 Re1 C51 89.66(18) . . ? C41 Re1 C51 89.09(17) . . ? C31 Re1 N21 175.40(15) . . ? C41 Re1 N21 96.27(16) . . ? C51 Re1 N21 91.50(15) . . ? C31 Re1 N11 96.67(15) . . ? C41 Re1 N11 174.86(16) . . ? C51 Re1 N11 92.57(14) . . ? N21 Re1 N11 78.82(12) . . ? C31 Re1 Cl1 92.51(13) . . ? C41 Re1 Cl1 93.21(14) . . ? C51 Re1 Cl1 176.88(12) . . ? N21 Re1 Cl1 86.16(10) . . ? N11 Re1 Cl1 84.96(9) . . ? C63 O71 C72 116.8(3) . . ? C75 O74 C73 112.8(3) . . ? C76 O77 C78 110.8(3) . . ? C81 O80 C79 113.2(3) . . ? C84 O83 C82 110.6(3) . . ? C64 O86 C85 116.1(3) . . ? C12 N1 C22 123.7(3) . . ? C12 N1 C61 116.4(3) . . ? C22 N1 C61 115.3(3) . . ? C12 N11 C16 118.5(3) . . ? C12 N11 Re1 121.2(3) . . ? C16 N11 Re1 118.3(3) . . ? C22 N21 C26 118.3(4) . . ? C22 N21 Re1 123.2(3) . . ? C26 N21 Re1 118.3(3) . . ? N11 C12 C13 120.6(4) . . ? N11 C12 N1 118.5(4) . . ? C13 C12 N1 120.9(4) . . ? C14 C13 C12 119.3(4) . . ? C13 C14 C15 119.8(4) . . ? C16 C15 C14 117.9(4) . . ? N11 C16 C15 122.9(4) . . ? N21 C22 C23 120.9(4) . . ? N21 C22 N1 118.6(3) . . ? C23 C22 N1 120.5(4) . . ? C24 C23 C22 119.4(4) . . ? C23 C24 C25 120.5(4) . . ? C26 C25 C24 117.5(4) . . ? N21 C26 C25 123.3(4) . . ? O31 C31 Re1 178.2(4) . . ? O41 C41 Re1 178.9(4) . . ? O51 C51 Re1 177.0(4) . . ? C66 C61 C62 120.6(4) . . ? C66 C61 N1 121.2(3) . . ? C62 C61 N1 118.1(3) . . ? C63 C62 C61 119.9(4) . . ? O71 C63 C62 124.8(3) . . ? O71 C63 C64 114.9(3) . . ? C62 C63 C64 120.3(4) . . ? O86 C64 C65 124.3(3) . . ? O86 C64 C63 116.7(3) . . ? C65 C64 C63 119.0(4) . . ? C64 C65 C66 120.3(4) . . ? C61 C66 C65 119.8(4) . . ? O71 C72 C73 108.1(3) . . ? O74 C73 C72 108.5(3) . . ? O74 C75 C76 108.8(4) . . ? O77 C76 C75 110.1(4) . . ? O77 C78 C79 109.9(4) . . ? O80 C79 C78 108.9(4) . . ? O80 C81 C82 108.0(3) . . ? O83 C82 C81 109.4(3) . . ? O83 C84 C85 109.1(3) . . ? O86 C85 C84 109.0(3) . . ? O201 C202 C203 105.9(5) . . ? C202 C203 C204 104.0(5) . . ? C205 C204 C203 103.1(5) . . ? O201 C205 C204 107.5(5) . . ? C205 O201 C202 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.623 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.147 #=END data_fuses _database_code_depnum_ccdc_archive 'CCDC 222973' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H30 Cl2 N6 O6 Re2' _chemical_formula_sum 'C46 H30 Cl2 N6 O6 Re2' _chemical_formula_weight 1206.06 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 12.1864(13) _cell_length_b 13.9338(15) _cell_length_c 14.076(2) _cell_angle_alpha 61.504(12) _cell_angle_beta 85.830(8) _cell_angle_gamma 79.965(9) _cell_volume 2068.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 237 _cell_measurement_theta_min 0.841117 _cell_measurement_theta_max 1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 6.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.05 _exptl_absorpt_correction_T_max 0.31 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23744 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9457 _reflns_number_gt 8280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0211P)^2^+1.4703P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9457 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 1.132753(10) 0.726658(11) 0.274001(10) 0.01321(4) Uani 1 1 d . . . Cl1 Cl 0.99906(7) 0.85837(8) 0.31366(7) 0.02219(19) Uani 1 1 d . . . O31 O 1.28754(19) 0.5681(2) 0.2117(2) 0.0203(5) Uani 1 1 d . . . O41 O 1.3268(2) 0.7561(2) 0.3805(2) 0.0278(6) Uani 1 1 d . . . O51 O 1.1094(2) 0.5329(2) 0.4999(2) 0.0229(6) Uani 1 1 d . . . N1 N 1.0799(2) 0.7790(2) 0.0262(2) 0.0148(6) Uani 1 1 d . . . N11 N 0.9902(2) 0.7179(2) 0.1950(2) 0.0149(6) Uani 1 1 d . . . N21 N 1.1463(2) 0.8673(2) 0.1152(2) 0.0155(6) Uani 1 1 d . . . C1 C 1.0394(3) 0.8187(3) -0.1582(3) 0.0196(7) Uani 1 1 d . . . H1A H 0.9818 0.8745 -0.1634 0.023 Uiso 1 1 calc R . . C2 C 1.1010(3) 0.7578(3) -0.0652(3) 0.0160(7) Uani 1 1 d . . . C3 C 1.1885(3) 0.6721(3) -0.0549(3) 0.0199(8) Uani 1 1 d . . . H3A H 1.2293 0.6310 0.0094 0.024 Uiso 1 1 calc R . . C4A C 1.1507(3) 0.7114(3) -0.2365(3) 0.0193(8) Uani 1 1 d . . . C4 C 1.2133(3) 0.6496(3) -0.1393(3) 0.0200(8) Uani 1 1 d . . . H4A H 1.2713 0.5936 -0.1327 0.024 Uiso 1 1 calc R . . C5 C 1.1763(3) 0.6927(3) -0.3279(3) 0.0230(8) Uani 1 1 d . . . H5A H 1.2341 0.6374 -0.3234 0.028 Uiso 1 1 calc R . . C6 C 1.1162(3) 0.7555(3) -0.4212(3) 0.0230(8) Uani 1 1 d . . . H6A H 1.1331 0.7428 -0.4802 0.028 Uiso 1 1 calc R . . C7A C 1.0629(3) 0.7972(3) -0.2472(3) 0.0177(7) Uani 1 1 d . . . C7 C 1.0280(3) 0.8403(3) -0.4294(3) 0.0264(9) Uani 1 1 d . . . H7A H 0.9877 0.8827 -0.4938 0.032 Uiso 1 1 calc R . . C8 C 1.0013(3) 0.8606(3) -0.3444(3) 0.0216(8) Uani 1 1 d . . . H8A H 0.9428 0.9159 -0.3505 0.026 Uiso 1 1 calc R . . C12 C 0.9910(3) 0.7333(3) 0.0935(3) 0.0138(7) Uani 1 1 d . . . C13 C 0.9068(3) 0.7038(3) 0.0547(3) 0.0175(7) Uani 1 1 d . . . H13A H 0.9096 0.7132 -0.0154 0.021 Uiso 1 1 calc R . . C14 C 0.8198(3) 0.6608(3) 0.1212(3) 0.0196(8) Uani 1 1 d . . . H14A H 0.7637 0.6401 0.0968 0.024 Uiso 1 1 calc R . . C15 C 0.8169(3) 0.6488(3) 0.2247(3) 0.0196(8) Uani 1 1 d . . . H15A H 0.7591 0.6200 0.2711 0.024 Uiso 1 1 calc R . . C16 C 0.9013(3) 0.6805(3) 0.2573(3) 0.0186(7) Uani 1 1 d . . . H16A H 0.8973 0.6760 0.3255 0.022 Uiso 1 1 calc R . . C22 C 1.1271(3) 0.8670(3) 0.0218(3) 0.0152(7) Uani 1 1 d . . . C23 C 1.1561(3) 0.9503(3) -0.0774(3) 0.0174(7) Uani 1 1 d . . . H23A H 1.1422 0.9497 -0.1412 0.021 Uiso 1 1 calc R . . C24 C 1.2052(3) 1.0331(3) -0.0804(3) 0.0205(8) Uani 1 1 d . . . H24A H 1.2263 1.0877 -0.1462 0.025 Uiso 1 1 calc R . . C25 C 1.2233(3) 1.0354(3) 0.0139(3) 0.0206(8) Uani 1 1 d . . . H25A H 1.2564 1.0910 0.0132 0.025 Uiso 1 1 calc R . . C26 C 1.1906(3) 0.9525(3) 0.1091(3) 0.0206(8) Uani 1 1 d . . . H26A H 1.1995 0.9553 0.1728 0.025 Uiso 1 1 calc R . . C31 C 1.2297(3) 0.6289(3) 0.2349(3) 0.0168(7) Uani 1 1 d . . . C41 C 1.2555(3) 0.7457(3) 0.3379(3) 0.0180(7) Uani 1 1 d . . . C51 C 1.1160(3) 0.6052(3) 0.4137(3) 0.0157(7) Uani 1 1 d . . . Re2 Re 0.595025(11) 0.762163(12) 0.769585(11) 0.01612(4) Uani 1 1 d . . . Cl2 Cl 0.71916(8) 0.84269(8) 0.83331(8) 0.0257(2) Uani 1 1 d . . . O131 O 0.4539(2) 0.6522(2) 0.6902(2) 0.0306(7) Uani 1 1 d . . . O141 O 0.3839(2) 0.8874(2) 0.8165(2) 0.0349(7) Uani 1 1 d . . . O151 O 0.5836(2) 0.5733(3) 1.0005(2) 0.0380(7) Uani 1 1 d . . . N2 N 0.6887(2) 0.7666(2) 0.5519(2) 0.0169(6) Uani 1 1 d . . . N111 N 0.7513(2) 0.6835(2) 0.7311(2) 0.0171(6) Uani 1 1 d . . . N121 N 0.6268(2) 0.8989(2) 0.6108(2) 0.0160(6) Uani 1 1 d . . . C04A C 0.5678(3) 0.6638(3) 0.3452(3) 0.0226(8) Uani 1 1 d . . . C08A C 0.5723(3) 0.7773(3) 0.3065(3) 0.0227(8) Uani 1 1 d . . . C101 C 0.6142(3) 0.8123(3) 0.3744(3) 0.0204(8) Uani 1 1 d . . . H10A H 0.6171 0.8869 0.3489 0.024 Uiso 1 1 calc R . . C102 C 0.6507(3) 0.7366(3) 0.4777(3) 0.0185(7) Uani 1 1 d . . . C103 C 0.6454(3) 0.6236(3) 0.5156(3) 0.0214(8) Uani 1 1 d . . . H10B H 0.6693 0.5723 0.5857 0.026 Uiso 1 1 calc R . . C104 C 0.6057(3) 0.5882(3) 0.4511(3) 0.0238(8) Uani 1 1 d . . . H10C H 0.6038 0.5132 0.4776 0.029 Uiso 1 1 calc R . . C105 C 0.5283(3) 0.6293(4) 0.2751(3) 0.0301(10) Uani 1 1 d . . . H10D H 0.5249 0.5549 0.3001 0.036 Uiso 1 1 calc R . . C106 C 0.4957(3) 0.7046(4) 0.1719(4) 0.0348(10) Uani 1 1 d . . . H10E H 0.4710 0.6814 0.1263 0.042 Uiso 1 1 calc R . . C107 C 0.4992(3) 0.8182(4) 0.1338(3) 0.0334(10) Uani 1 1 d . . . H10F H 0.4758 0.8692 0.0635 0.040 Uiso 1 1 calc R . . C108 C 0.5365(3) 0.8540(4) 0.1989(3) 0.0321(10) Uani 1 1 d . . . H10G H 0.5384 0.9288 0.1726 0.038 Uiso 1 1 calc R . . C112 C 0.7699(3) 0.6929(3) 0.6320(3) 0.0168(7) Uani 1 1 d . . . C113 C 0.8652(3) 0.6397(3) 0.6065(3) 0.0212(8) Uani 1 1 d . . . H11A H 0.8750 0.6472 0.5373 0.025 Uiso 1 1 calc R . . C114 C 0.9452(3) 0.5754(3) 0.6860(3) 0.0241(8) Uani 1 1 d . . . H11B H 1.0096 0.5383 0.6711 0.029 Uiso 1 1 calc R . . C115 C 0.9286(3) 0.5665(3) 0.7875(3) 0.0216(8) Uani 1 1 d . . . H11C H 0.9817 0.5238 0.8421 0.026 Uiso 1 1 calc R . . C116 C 0.8322(3) 0.6220(3) 0.8067(3) 0.0210(8) Uani 1 1 d . . . H11D H 0.8222 0.6171 0.8750 0.025 Uiso 1 1 calc R . . C122 C 0.6760(3) 0.8784(3) 0.5320(3) 0.0166(7) Uani 1 1 d . . . C123 C 0.7191(3) 0.9586(3) 0.4403(3) 0.0214(8) Uani 1 1 d . . . H12A H 0.7578 0.9405 0.3901 0.026 Uiso 1 1 calc R . . C124 C 0.7038(3) 1.0656(3) 0.4246(3) 0.0254(8) Uani 1 1 d . . . H12B H 0.7300 1.1213 0.3626 0.031 Uiso 1 1 calc R . . C125 C 0.6489(3) 1.0888(3) 0.5026(3) 0.0225(8) Uani 1 1 d . . . H12C H 0.6350 1.1608 0.4925 0.027 Uiso 1 1 calc R . . C126 C 0.6151(3) 1.0038(3) 0.5951(3) 0.0201(8) Uani 1 1 d . . . H12D H 0.5828 1.0191 0.6493 0.024 Uiso 1 1 calc R . . C131 C 0.5066(3) 0.6952(3) 0.7185(3) 0.0210(8) Uani 1 1 d . . . C141 C 0.4631(3) 0.8404(3) 0.7981(3) 0.0239(8) Uani 1 1 d . . . C151 C 0.5862(3) 0.6439(3) 0.9126(3) 0.0256(8) 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 0.01473(7) 0.01602(8) 0.00909(7) -0.00630(6) 0.00023(5) -0.00196(5) Cl1 0.0267(4) 0.0263(5) 0.0158(4) -0.0139(4) -0.0029(3) 0.0037(4) O31 0.0195(12) 0.0225(14) 0.0215(14) -0.0129(12) 0.0017(10) -0.0027(10) O41 0.0197(13) 0.0465(19) 0.0279(15) -0.0264(14) 0.0000(11) -0.0044(12) O51 0.0270(14) 0.0244(15) 0.0143(13) -0.0069(12) 0.0043(10) -0.0049(11) N1 0.0188(14) 0.0189(16) 0.0105(14) -0.0096(12) 0.0024(11) -0.0051(12) N11 0.0145(14) 0.0159(15) 0.0127(14) -0.0063(12) 0.0013(10) -0.0008(11) N21 0.0197(14) 0.0158(15) 0.0119(14) -0.0072(12) 0.0010(11) -0.0036(12) C1 0.0209(18) 0.022(2) 0.0188(18) -0.0121(16) 0.0030(14) -0.0044(15) C2 0.0174(16) 0.0206(19) 0.0134(17) -0.0099(15) 0.0060(13) -0.0082(14) C3 0.0218(18) 0.022(2) 0.0167(18) -0.0093(16) 0.0001(14) -0.0050(15) C4A 0.0182(17) 0.024(2) 0.024(2) -0.0157(17) 0.0024(14) -0.0083(15) C4 0.0190(17) 0.020(2) 0.0202(19) -0.0097(16) 0.0006(14) -0.0005(14) C5 0.0199(18) 0.031(2) 0.026(2) -0.0195(18) 0.0084(15) -0.0103(16) C6 0.0254(19) 0.035(2) 0.0167(19) -0.0164(18) 0.0079(14) -0.0151(17) C7A 0.0214(17) 0.0173(18) 0.0147(17) -0.0071(15) 0.0040(13) -0.0067(14) C7 0.031(2) 0.032(2) 0.019(2) -0.0127(18) 0.0023(15) -0.0115(18) C8 0.0254(19) 0.023(2) 0.0158(18) -0.0084(16) 0.0002(14) -0.0034(15) C12 0.0152(16) 0.0102(17) 0.0145(17) -0.0054(14) 0.0021(12) -0.0004(12) C13 0.0190(17) 0.0201(19) 0.0134(17) -0.0085(15) -0.0029(13) -0.0004(14) C14 0.0172(17) 0.0202(19) 0.0196(19) -0.0075(16) -0.0015(13) -0.0035(14) C15 0.0116(16) 0.022(2) 0.0199(18) -0.0071(16) 0.0046(13) -0.0007(14) C16 0.0174(17) 0.0205(19) 0.0138(17) -0.0066(15) 0.0033(13) 0.0013(14) C22 0.0170(16) 0.0154(18) 0.0123(16) -0.0064(14) -0.0006(12) -0.0008(13) C23 0.0224(18) 0.0168(18) 0.0114(16) -0.0055(15) 0.0006(13) -0.0033(14) C24 0.0229(18) 0.0182(19) 0.0186(18) -0.0074(16) 0.0007(14) -0.0030(15) C25 0.0250(19) 0.0143(19) 0.024(2) -0.0100(16) -0.0008(15) -0.0037(14) C26 0.0253(19) 0.021(2) 0.0196(19) -0.0121(16) -0.0031(14) -0.0034(15) C31 0.0166(17) 0.0197(19) 0.0114(17) -0.0045(15) 0.0003(13) -0.0052(14) C41 0.0199(17) 0.0201(19) 0.0144(17) -0.0088(15) 0.0050(13) -0.0040(14) C51 0.0127(16) 0.0198(19) 0.0184(18) -0.0119(16) -0.0007(13) -0.0031(13) Re2 0.01609(7) 0.01741(8) 0.01450(7) -0.00806(6) -0.00032(5) 0.00000(5) Cl2 0.0305(5) 0.0266(5) 0.0252(5) -0.0166(4) -0.0087(4) 0.0003(4) O131 0.0236(14) 0.0358(17) 0.0359(17) -0.0186(15) -0.0002(12) -0.0083(12) O141 0.0317(16) 0.0367(18) 0.0339(17) -0.0190(15) 0.0080(12) 0.0047(13) O151 0.0424(18) 0.0330(18) 0.0240(16) -0.0038(14) 0.0014(13) -0.0005(14) N2 0.0208(15) 0.0170(16) 0.0159(15) -0.0109(13) 0.0007(11) -0.0012(12) N111 0.0168(14) 0.0148(15) 0.0194(16) -0.0083(13) -0.0029(11) 0.0000(11) N121 0.0146(14) 0.0180(16) 0.0150(15) -0.0081(13) -0.0026(11) 0.0007(11) C04A 0.0120(16) 0.034(2) 0.030(2) -0.0218(19) 0.0091(14) -0.0062(15) C08A 0.0119(16) 0.036(2) 0.023(2) -0.0167(18) 0.0061(14) -0.0041(15) C101 0.0171(17) 0.024(2) 0.024(2) -0.0144(17) 0.0027(14) -0.0042(14) C102 0.0124(16) 0.027(2) 0.0221(19) -0.0167(17) 0.0035(13) -0.0030(14) C103 0.0161(17) 0.024(2) 0.027(2) -0.0157(17) -0.0018(14) 0.0009(14) C104 0.0144(17) 0.030(2) 0.037(2) -0.0233(19) 0.0068(15) -0.0061(15) C105 0.0183(18) 0.050(3) 0.038(2) -0.033(2) 0.0081(16) -0.0104(18) C106 0.025(2) 0.058(3) 0.039(3) -0.035(2) 0.0075(18) -0.017(2) C107 0.030(2) 0.050(3) 0.025(2) -0.019(2) 0.0008(16) -0.013(2) C108 0.033(2) 0.039(3) 0.026(2) -0.016(2) 0.0030(17) -0.0118(19) C112 0.0153(16) 0.0176(19) 0.0198(18) -0.0103(15) 0.0013(13) -0.0039(14) C113 0.0184(17) 0.021(2) 0.030(2) -0.0160(17) 0.0048(14) -0.0061(15) C114 0.0141(17) 0.0169(19) 0.042(2) -0.0149(18) 0.0025(15) -0.0024(14) C115 0.0169(17) 0.0129(18) 0.031(2) -0.0061(16) -0.0079(15) -0.0013(14) C116 0.0193(18) 0.0184(19) 0.024(2) -0.0082(16) -0.0050(14) -0.0034(14) C122 0.0152(16) 0.0184(19) 0.0156(17) -0.0078(15) -0.0024(13) -0.0010(13) C123 0.0183(17) 0.025(2) 0.0208(19) -0.0106(17) -0.0001(14) -0.0044(15) C124 0.029(2) 0.026(2) 0.0188(19) -0.0068(17) -0.0013(15) -0.0103(17) C125 0.0270(19) 0.0166(19) 0.024(2) -0.0097(17) -0.0043(15) -0.0025(15) C126 0.0185(17) 0.022(2) 0.0204(19) -0.0111(16) -0.0034(14) 0.0003(14) C131 0.0161(17) 0.022(2) 0.0189(19) -0.0064(16) 0.0021(14) 0.0013(14) C141 0.026(2) 0.027(2) 0.0178(19) -0.0106(17) -0.0005(15) -0.0014(16) C151 0.025(2) 0.026(2) 0.026(2) -0.0140(19) -0.0020(15) 0.0016(16) _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 C31 1.901(4) . ? Re1 C51 1.913(4) . ? Re1 C41 1.918(4) . ? Re1 N21 2.178(3) . ? Re1 N11 2.180(3) . ? Re1 Cl1 2.4774(9) . ? O31 C31 1.159(4) . ? O41 C41 1.157(4) . ? O51 C51 1.158(4) . ? N1 C12 1.412(4) . ? N1 C22 1.416(4) . ? N1 C2 1.447(4) . ? N11 C12 1.339(4) . ? N11 C16 1.356(4) . ? N21 C26 1.351(4) . ? N21 C22 1.354(4) . ? C1 C2 1.364(5) . ? C1 C7A 1.420(5) . ? C2 C3 1.413(5) . ? C3 C4 1.370(5) . ? C4A C4 1.412(5) . ? C4A C7A 1.415(5) . ? C4A C5 1.433(5) . ? C5 C6 1.358(5) . ? C6 C7 1.418(5) . ? C7A C8 1.408(5) . ? C7 C8 1.360(5) . ? C12 C13 1.401(5) . ? C13 C14 1.380(5) . ? C14 C15 1.383(5) . ? C15 C16 1.372(5) . ? C22 C23 1.395(5) . ? C23 C24 1.371(5) . ? C24 C25 1.377(5) . ? C25 C26 1.377(5) . ? Re2 C151 1.909(4) . ? Re2 C141 1.910(4) . ? Re2 C131 1.911(4) . ? Re2 N111 2.193(3) . ? Re2 N121 2.200(3) . ? Re2 Cl2 2.4701(9) . ? O131 C131 1.153(4) . ? O141 C141 1.155(4) . ? O151 C151 1.158(5) . ? N2 C112 1.417(4) . ? N2 C122 1.426(4) . ? N2 C102 1.426(4) . ? N111 C112 1.343(4) . ? N111 C116 1.352(4) . ? N121 C122 1.349(4) . ? N121 C126 1.353(5) . ? C04A C104 1.406(5) . ? C04A C08A 1.416(6) . ? C04A C105 1.428(5) . ? C08A C101 1.419(5) . ? C08A C108 1.419(6) . ? C101 C102 1.375(5) . ? C102 C103 1.413(5) . ? C103 C104 1.371(5) . ? C105 C106 1.361(6) . ? C106 C107 1.416(6) . ? C107 C108 1.368(6) . ? C112 C113 1.386(5) . ? C113 C114 1.379(5) . ? C114 C115 1.378(5) . ? C115 C116 1.374(5) . ? C122 C123 1.386(5) . ? C123 C124 1.379(5) . ? C124 C125 1.383(5) . ? C125 C126 1.374(5) . ? 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 C31 Re1 C51 89.62(14) . . ? C31 Re1 C41 90.40(14) . . ? C51 Re1 C41 85.53(14) . . ? C31 Re1 N21 91.97(13) . . ? C51 Re1 N21 178.12(12) . . ? C41 Re1 N21 95.47(13) . . ? C31 Re1 N11 92.21(12) . . ? C51 Re1 N11 97.68(12) . . ? C41 Re1 N11 175.87(13) . . ? N21 Re1 N11 81.25(10) . . ? C31 Re1 Cl1 176.14(10) . . ? C51 Re1 Cl1 92.77(10) . . ? C41 Re1 Cl1 92.81(11) . . ? N21 Re1 Cl1 85.59(8) . . ? N11 Re1 Cl1 84.47(8) . . ? C12 N1 C22 124.7(3) . . ? C12 N1 C2 116.3(3) . . ? C22 N1 C2 116.4(3) . . ? C12 N11 C16 118.2(3) . . ? C12 N11 Re1 123.9(2) . . ? C16 N11 Re1 117.3(2) . . ? C26 N21 C22 118.1(3) . . ? C26 N21 Re1 118.2(2) . . ? C22 N21 Re1 123.0(2) . . ? C2 C1 C7A 120.2(3) . . ? C1 C2 C3 121.1(3) . . ? C1 C2 N1 121.3(3) . . ? C3 C2 N1 117.6(3) . . ? C4 C3 C2 120.1(3) . . ? C4 C4A C7A 120.2(3) . . ? C4 C4A C5 121.6(3) . . ? C7A C4A C5 118.1(3) . . ? C3 C4 C4A 119.9(3) . . ? C6 C5 C4A 120.2(4) . . ? C5 C6 C7 120.5(3) . . ? C8 C7A C4A 120.6(3) . . ? C8 C7A C1 120.9(3) . . ? C4A C7A C1 118.6(3) . . ? C8 C7 C6 121.0(4) . . ? C7 C8 C7A 119.5(4) . . ? N11 C12 C13 121.3(3) . . ? N11 C12 N1 118.4(3) . . ? C13 C12 N1 120.3(3) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 119.1(3) . . ? C16 C15 C14 118.5(3) . . ? N11 C16 C15 123.2(3) . . ? N21 C22 C23 120.7(3) . . ? N21 C22 N1 119.1(3) . . ? C23 C22 N1 120.1(3) . . ? C24 C23 C22 119.7(3) . . ? C23 C24 C25 120.1(3) . . ? C26 C25 C24 117.7(3) . . ? N21 C26 C25 123.6(3) . . ? O31 C31 Re1 178.8(3) . . ? O41 C41 Re1 177.0(3) . . ? O51 C51 Re1 177.0(3) . . ? C151 Re2 C141 88.12(16) . . ? C151 Re2 C131 89.22(16) . . ? C141 Re2 C131 90.27(16) . . ? C151 Re2 N111 94.93(14) . . ? C141 Re2 N111 175.92(14) . . ? C131 Re2 N111 92.48(13) . . ? C151 Re2 N121 172.59(13) . . ? C141 Re2 N121 95.85(14) . . ? C131 Re2 N121 97.00(13) . . ? N111 Re2 N121 80.83(11) . . ? C151 Re2 Cl2 90.90(12) . . ? C141 Re2 Cl2 93.12(12) . . ? C131 Re2 Cl2 176.61(11) . . ? N111 Re2 Cl2 84.14(8) . . ? N121 Re2 Cl2 82.65(8) . . ? C112 N2 C122 114.3(3) . . ? C112 N2 C102 120.3(3) . . ? C122 N2 C102 122.7(3) . . ? C112 N111 C116 117.2(3) . . ? C112 N111 Re2 121.5(2) . . ? C116 N111 Re2 121.3(2) . . ? C122 N121 C126 117.4(3) . . ? C122 N121 Re2 120.7(2) . . ? C126 N121 Re2 121.0(2) . . ? C104 C04A C08A 118.5(3) . . ? C104 C04A C105 122.1(4) . . ? C08A C04A C105 119.4(4) . . ? C04A C08A C101 119.9(4) . . ? C04A C08A C108 118.9(4) . . ? C101 C08A C108 121.2(4) . . ? C102 C101 C08A 120.5(4) . . ? C101 C102 C103 119.2(3) . . ? C101 C102 N2 123.3(3) . . ? C103 C102 N2 117.4(3) . . ? C104 C103 C102 121.2(4) . . ? C103 C104 C04A 120.8(4) . . ? C106 C105 C04A 120.4(4) . . ? C105 C106 C107 120.1(4) . . ? C108 C107 C106 121.0(4) . . ? C107 C108 C08A 120.3(4) . . ? N111 C112 C113 122.9(3) . . ? N111 C112 N2 115.8(3) . . ? C113 C112 N2 121.2(3) . . ? C114 C113 C112 118.6(4) . . ? C115 C114 C113 119.3(3) . . ? C116 C115 C114 118.8(3) . . ? N111 C116 C115 123.1(4) . . ? N121 C122 C123 122.5(3) . . ? N121 C122 N2 115.9(3) . . ? C123 C122 N2 121.4(3) . . ? C124 C123 C122 119.0(4) . . ? C123 C124 C125 118.8(4) . . ? C126 C125 C124 119.1(4) . . ? N121 C126 C125 122.9(3) . . ? O131 C131 Re2 178.2(3) . . ? O141 C141 Re2 179.2(3) . . ? O151 C151 Re2 177.7(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.735 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.122 #=END data_angrys _database_code_depnum_ccdc_archive 'CCDC 222974' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Cl2 N8 O6 Re2' _chemical_formula_sum 'C36 H24 Cl2 N8 O6 Re2' _chemical_formula_weight 1107.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.975(2) _cell_length_b 13.661(2) _cell_length_c 14.578(3) _cell_angle_alpha 107.544(15) _cell_angle_beta 111.036(13) _cell_angle_gamma 102.713(17) _cell_volume 1808.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 0.783146 _cell_measurement_theta_max 1 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 6.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.13 _exptl_absorpt_correction_T_max 0.54 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20904 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8268 _reflns_number_gt 6727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0205P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8268 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 0.22467(2) 1.148937(15) -0.176392(16) 0.01395(6) Uani 1 1 d . . . Cl1 Cl 0.41674(13) 1.13834(10) -0.22480(10) 0.0185(3) Uani 1 1 d . . . O41 O 0.1623(4) 1.3107(3) -0.2772(3) 0.0298(9) Uani 1 1 d . . . O51 O -0.0080(4) 1.1564(3) -0.1087(3) 0.0250(8) Uani 1 1 d . . . O61 O 0.0046(4) 0.9646(3) -0.3989(3) 0.0300(9) Uani 1 1 d . . . N1 N 0.3117(4) 1.1684(3) 0.0626(3) 0.0160(9) Uani 1 1 d . . . N11 N 0.3962(4) 1.2720(3) -0.0191(3) 0.0145(9) Uani 1 1 d . . . N21 N 0.2823(4) 1.0384(3) -0.0991(3) 0.0137(8) Uani 1 1 d . . . N31 N 0.2344(4) 1.2888(3) 0.1536(3) 0.0213(10) Uani 1 1 d . . . C12 C 0.4096(5) 1.2622(4) 0.0721(4) 0.0141(10) Uani 1 1 d . . . C13 C 0.5176(5) 1.3381(4) 0.1730(4) 0.0190(11) Uani 1 1 d . . . H13A H 0.5254 1.3280 0.2350 0.023 Uiso 1 1 calc R . . C14 C 0.6128(5) 1.4284(4) 0.1803(4) 0.0188(11) Uani 1 1 d . . . H14A H 0.6850 1.4811 0.2470 0.023 Uiso 1 1 calc R . . C15 C 0.5981(5) 1.4387(4) 0.0851(4) 0.0213(11) Uani 1 1 d . . . H15A H 0.6596 1.4996 0.0877 0.026 Uiso 1 1 calc R . . C16 C 0.4936(5) 1.3597(4) -0.0116(4) 0.0174(11) Uani 1 1 d . . . H16A H 0.4882 1.3655 -0.0748 0.021 Uiso 1 1 calc R . . C22 C 0.3076(5) 1.0630(4) 0.0048(4) 0.0145(10) Uani 1 1 d . . . C23 C 0.3391(5) 0.9934(4) 0.0543(4) 0.0203(11) Uani 1 1 d . . . H23A H 0.3598 1.0135 0.1266 0.024 Uiso 1 1 calc R . . C24 C 0.3394(5) 0.8943(4) -0.0053(4) 0.0194(11) Uani 1 1 d . . . H24A H 0.3568 0.8451 0.0253 0.023 Uiso 1 1 calc R . . C25 C 0.3131(5) 0.8683(4) -0.1124(4) 0.0177(11) Uani 1 1 d . . . H25A H 0.3127 0.8015 -0.1542 0.021 Uiso 1 1 calc R . . C26 C 0.2879(5) 0.9427(4) -0.1552(4) 0.0157(10) Uani 1 1 d . . . H26A H 0.2743 0.9263 -0.2257 0.019 Uiso 1 1 calc R . . C32 C 0.2295(5) 1.1858(4) 0.1174(4) 0.0156(10) Uani 1 1 d . . . C33 C 0.1463(5) 1.1013(4) 0.1290(4) 0.0214(11) Uani 1 1 d . . . H33A H 0.1446 1.0297 0.1030 0.026 Uiso 1 1 calc R . . C34 C 0.0676(5) 1.1285(4) 0.1801(4) 0.0261(13) Uani 1 1 d . . . H34A H 0.0120 1.0743 0.1897 0.031 Uiso 1 1 calc R . . C35 C 0.0694(5) 1.2359(4) 0.2181(4) 0.0261(12) Uani 1 1 d . . . H35A H 0.0150 1.2548 0.2517 0.031 Uiso 1 1 calc R . . C36 C 0.1554(6) 1.3114(5) 0.2031(4) 0.0261(12) Uani 1 1 d . . . H36A H 0.1595 1.3838 0.2290 0.031 Uiso 1 1 calc R . . C41 C 0.1856(5) 1.2505(4) -0.2395(4) 0.0181(11) Uani 1 1 d . . . C51 C 0.0816(5) 1.1543(4) -0.1332(4) 0.0189(11) Uani 1 1 d . . . C61 C 0.0861(5) 1.0338(4) -0.3150(4) 0.0178(11) Uani 1 1 d . . . Re2 Re 0.76179(2) 0.310116(15) 0.508123(15) 0.01340(6) Uani 1 1 d . . . Cl2 Cl 0.57417(12) 0.17539(9) 0.32619(10) 0.0176(3) Uani 1 1 d . . . O141 O 0.8162(4) 0.4971(3) 0.4360(3) 0.0258(9) Uani 1 1 d . . . O151 O 0.9886(4) 0.2610(3) 0.4479(3) 0.0263(9) Uani 1 1 d . . . O161 O 0.9882(4) 0.4792(3) 0.7336(3) 0.0303(9) Uani 1 1 d . . . N2 N 0.6649(4) 0.2779(3) 0.6818(3) 0.0165(9) Uani 1 1 d . . . N111 N 0.7190(4) 0.1720(3) 0.5541(3) 0.0142(8) Uani 1 1 d . . . N121 N 0.5826(4) 0.3274(3) 0.5363(3) 0.0151(9) Uani 1 1 d . . . N131 N 0.7168(5) 0.4393(4) 0.8262(4) 0.0257(10) Uani 1 1 d . . . C112 C 0.6796(5) 0.1775(4) 0.6324(4) 0.0150(10) Uani 1 1 d . . . C113 C 0.6481(5) 0.0891(4) 0.6596(4) 0.0215(11) Uani 1 1 d . . . H11A H 0.6182 0.0946 0.7125 0.026 Uiso 1 1 calc R . . C114 C 0.6620(5) -0.0066(4) 0.6066(4) 0.0203(11) Uani 1 1 d . . . H11B H 0.6438 -0.0662 0.6245 0.024 Uiso 1 1 calc R . . C115 C 0.7034(5) -0.0132(4) 0.5267(4) 0.0189(11) Uani 1 1 d . . . H11C H 0.7147 -0.0768 0.4909 0.023 Uiso 1 1 calc R . . C116 C 0.7276(5) 0.0758(4) 0.5004(4) 0.0170(10) Uani 1 1 d . . . H11D H 0.7506 0.0695 0.4439 0.020 Uiso 1 1 calc R . . C122 C 0.5626(5) 0.3069(4) 0.6154(4) 0.0155(10) Uani 1 1 d . . . C123 C 0.4457(5) 0.3098(4) 0.6314(4) 0.0168(10) Uani 1 1 d . . . H12A H 0.4350 0.2943 0.6865 0.020 Uiso 1 1 calc R . . C124 C 0.3465(5) 0.3358(4) 0.5644(4) 0.0188(11) Uani 1 1 d . . . H12B H 0.2674 0.3385 0.5735 0.023 Uiso 1 1 calc R . . C125 C 0.3663(5) 0.3581(4) 0.4827(4) 0.0201(11) Uani 1 1 d . . . H12C H 0.3013 0.3771 0.4370 0.024 Uiso 1 1 calc R . . C126 C 0.4824(5) 0.3519(4) 0.4705(4) 0.0167(10) Uani 1 1 d . . . H12D H 0.4933 0.3651 0.4144 0.020 Uiso 1 1 calc R . . C132 C 0.7277(5) 0.3397(4) 0.7951(4) 0.0159(10) Uani 1 1 d . . . C133 C 0.8008(5) 0.3029(4) 0.8668(4) 0.0208(11) Uani 1 1 d . . . H13C H 0.8093 0.2346 0.8427 0.025 Uiso 1 1 calc R . . C134 C 0.8613(5) 0.3704(5) 0.9760(5) 0.0320(14) Uani 1 1 d . . . H13D H 0.9098 0.3468 1.0264 0.038 Uiso 1 1 calc R . . C135 C 0.8507(6) 0.4710(5) 1.0105(5) 0.0328(14) Uani 1 1 d . . . H13E H 0.8912 0.5167 1.0839 0.039 Uiso 1 1 calc R . . C136 C 0.7786(5) 0.5030(5) 0.9340(5) 0.0284(13) Uani 1 1 d . . . H13F H 0.7716 0.5720 0.9571 0.034 Uiso 1 1 calc R . . C141 C 0.7916(5) 0.4261(4) 0.4619(4) 0.0165(10) Uani 1 1 d . . . C151 C 0.9049(5) 0.2794(4) 0.4725(4) 0.0178(11) Uani 1 1 d . . . C161 C 0.9015(5) 0.4131(4) 0.6498(4) 0.0198(11) 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 0.01506(11) 0.01440(10) 0.01533(11) 0.00800(8) 0.00752(9) 0.00705(8) Cl1 0.0212(6) 0.0223(6) 0.0196(6) 0.0116(5) 0.0135(5) 0.0100(5) O41 0.035(2) 0.025(2) 0.029(2) 0.0173(18) 0.0085(19) 0.0113(18) O51 0.022(2) 0.029(2) 0.034(2) 0.0141(18) 0.0184(19) 0.0158(17) O61 0.030(2) 0.026(2) 0.024(2) 0.0054(18) 0.0048(19) 0.0123(18) N1 0.018(2) 0.014(2) 0.015(2) 0.0056(17) 0.0082(18) 0.0030(17) N11 0.017(2) 0.0109(19) 0.016(2) 0.0050(17) 0.0083(18) 0.0042(17) N21 0.013(2) 0.0124(19) 0.020(2) 0.0087(17) 0.0099(18) 0.0060(16) N31 0.023(2) 0.021(2) 0.020(2) 0.0076(19) 0.011(2) 0.0090(19) C12 0.018(3) 0.011(2) 0.016(3) 0.006(2) 0.010(2) 0.006(2) C13 0.031(3) 0.016(2) 0.019(3) 0.011(2) 0.016(2) 0.013(2) C14 0.022(3) 0.014(2) 0.015(3) 0.003(2) 0.006(2) 0.004(2) C15 0.025(3) 0.014(2) 0.029(3) 0.010(2) 0.017(3) 0.006(2) C16 0.024(3) 0.015(2) 0.019(3) 0.011(2) 0.012(2) 0.007(2) C22 0.010(2) 0.016(2) 0.017(3) 0.010(2) 0.005(2) 0.0029(19) C23 0.016(3) 0.021(3) 0.021(3) 0.010(2) 0.006(2) 0.002(2) C24 0.013(2) 0.018(3) 0.025(3) 0.010(2) 0.006(2) 0.003(2) C25 0.020(3) 0.013(2) 0.023(3) 0.008(2) 0.012(2) 0.008(2) C26 0.014(2) 0.020(3) 0.017(3) 0.008(2) 0.011(2) 0.005(2) C32 0.014(2) 0.018(2) 0.013(3) 0.004(2) 0.006(2) 0.007(2) C33 0.020(3) 0.017(3) 0.024(3) 0.008(2) 0.009(2) 0.004(2) C34 0.022(3) 0.029(3) 0.031(3) 0.014(3) 0.019(3) 0.002(2) C35 0.018(3) 0.036(3) 0.025(3) 0.009(3) 0.014(2) 0.011(2) C36 0.031(3) 0.030(3) 0.021(3) 0.009(2) 0.015(3) 0.016(3) C41 0.017(3) 0.015(2) 0.017(3) 0.005(2) 0.006(2) 0.004(2) C51 0.025(3) 0.013(2) 0.018(3) 0.009(2) 0.007(2) 0.008(2) C61 0.021(3) 0.020(3) 0.016(3) 0.008(2) 0.009(2) 0.011(2) Re2 0.01478(11) 0.01222(10) 0.01459(11) 0.00575(8) 0.00769(9) 0.00551(8) Cl2 0.0191(6) 0.0169(6) 0.0147(6) 0.0054(5) 0.0077(5) 0.0045(5) O141 0.029(2) 0.0185(19) 0.028(2) 0.0119(17) 0.0112(18) 0.0049(17) O151 0.025(2) 0.0198(19) 0.039(2) 0.0087(17) 0.0226(19) 0.0078(16) O161 0.027(2) 0.031(2) 0.020(2) 0.0034(18) 0.0034(18) 0.0113(18) N2 0.020(2) 0.019(2) 0.015(2) 0.0092(18) 0.0076(19) 0.0127(18) N111 0.016(2) 0.013(2) 0.015(2) 0.0059(17) 0.0069(18) 0.0064(17) N121 0.018(2) 0.016(2) 0.012(2) 0.0063(17) 0.0083(18) 0.0060(17) N131 0.023(2) 0.031(3) 0.028(3) 0.013(2) 0.016(2) 0.009(2) C112 0.012(2) 0.017(2) 0.018(3) 0.009(2) 0.005(2) 0.009(2) C113 0.022(3) 0.026(3) 0.027(3) 0.016(2) 0.014(2) 0.013(2) C114 0.018(3) 0.020(3) 0.030(3) 0.015(2) 0.014(2) 0.008(2) C115 0.017(3) 0.012(2) 0.024(3) 0.006(2) 0.007(2) 0.004(2) C116 0.015(3) 0.019(2) 0.016(3) 0.007(2) 0.006(2) 0.006(2) C122 0.018(3) 0.011(2) 0.017(3) 0.006(2) 0.007(2) 0.006(2) C123 0.023(3) 0.014(2) 0.018(3) 0.008(2) 0.012(2) 0.007(2) C124 0.017(3) 0.025(3) 0.020(3) 0.011(2) 0.011(2) 0.010(2) C125 0.024(3) 0.018(3) 0.019(3) 0.010(2) 0.006(2) 0.013(2) C126 0.018(3) 0.021(3) 0.013(3) 0.007(2) 0.007(2) 0.010(2) C132 0.008(2) 0.022(3) 0.021(3) 0.011(2) 0.009(2) 0.006(2) C133 0.019(3) 0.025(3) 0.023(3) 0.017(2) 0.009(2) 0.008(2) C134 0.017(3) 0.053(4) 0.028(3) 0.029(3) 0.006(3) 0.009(3) C135 0.018(3) 0.049(4) 0.019(3) 0.006(3) 0.009(3) 0.002(3) C136 0.020(3) 0.033(3) 0.031(3) 0.008(3) 0.016(3) 0.008(2) C141 0.019(3) 0.018(2) 0.014(3) 0.006(2) 0.009(2) 0.007(2) C151 0.019(3) 0.012(2) 0.018(3) 0.006(2) 0.008(2) 0.000(2) C161 0.022(3) 0.022(3) 0.021(3) 0.012(2) 0.011(2) 0.012(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 C51 1.897(5) . ? Re1 C61 1.922(5) . ? Re1 C41 1.925(5) . ? Re1 N11 2.194(4) . ? Re1 N21 2.210(4) . ? Re1 Cl1 2.4706(13) . ? O41 C41 1.143(6) . ? O51 C51 1.163(6) . ? O61 C61 1.155(6) . ? N1 C12 1.413(5) . ? N1 C22 1.413(6) . ? N1 C32 1.416(6) . ? N11 C12 1.334(6) . ? N11 C16 1.365(5) . ? N21 C26 1.346(6) . ? N21 C22 1.354(6) . ? N31 C32 1.327(6) . ? N31 C36 1.342(6) . ? C12 C13 1.390(7) . ? C13 C14 1.379(6) . ? C14 C15 1.392(7) . ? C15 C16 1.359(7) . ? C22 C23 1.388(6) . ? C23 C24 1.371(7) . ? C24 C25 1.394(7) . ? C25 C26 1.371(6) . ? C32 C33 1.398(6) . ? C33 C34 1.369(7) . ? C34 C35 1.396(8) . ? C35 C36 1.363(7) . ? Re2 C161 1.904(5) . ? Re2 C141 1.909(5) . ? Re2 C151 1.912(5) . ? Re2 N121 2.195(4) . ? Re2 N111 2.198(4) . ? Re2 Cl2 2.4759(15) . ? O141 C141 1.155(5) . ? O151 C151 1.149(6) . ? O161 C161 1.155(6) . ? N2 C132 1.414(6) . ? N2 C122 1.415(6) . ? N2 C112 1.418(6) . ? N111 C112 1.346(6) . ? N111 C116 1.355(6) . ? N121 C122 1.344(6) . ? N121 C126 1.357(6) . ? N131 C132 1.346(6) . ? N131 C136 1.355(7) . ? C112 C113 1.392(6) . ? C113 C114 1.376(7) . ? C114 C115 1.381(7) . ? C115 C116 1.381(6) . ? C122 C123 1.390(7) . ? C123 C124 1.372(7) . ? C124 C125 1.392(7) . ? C125 C126 1.366(7) . ? C132 C133 1.372(7) . ? C133 C134 1.383(7) . ? C134 C135 1.361(8) . ? C135 C136 1.369(8) . ? 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 C51 Re1 C61 89.5(2) . . ? C51 Re1 C41 89.7(2) . . ? C61 Re1 C41 86.3(2) . . ? C51 Re1 N11 94.70(18) . . ? C61 Re1 N11 174.61(18) . . ? C41 Re1 N11 97.07(17) . . ? C51 Re1 N21 92.36(17) . . ? C61 Re1 N21 96.27(18) . . ? C41 Re1 N21 176.74(17) . . ? N11 Re1 N21 80.26(14) . . ? C51 Re1 Cl1 176.81(15) . . ? C61 Re1 Cl1 91.80(15) . . ? C41 Re1 Cl1 93.25(15) . . ? N11 Re1 Cl1 83.79(11) . . ? N21 Re1 Cl1 84.62(10) . . ? C12 N1 C22 118.2(4) . . ? C12 N1 C32 118.0(4) . . ? C22 N1 C32 123.7(4) . . ? C12 N11 C16 118.1(4) . . ? C12 N11 Re1 120.8(3) . . ? C16 N11 Re1 121.1(3) . . ? C26 N21 C22 118.1(4) . . ? C26 N21 Re1 120.9(3) . . ? C22 N21 Re1 121.0(3) . . ? C32 N31 C36 117.8(4) . . ? N11 C12 C13 122.4(4) . . ? N11 C12 N1 117.4(4) . . ? C13 C12 N1 120.2(4) . . ? C14 C13 C12 119.2(4) . . ? C13 C14 C15 118.2(5) . . ? C16 C15 C14 119.9(4) . . ? C15 C16 N11 122.1(4) . . ? N21 C22 C23 122.2(4) . . ? N21 C22 N1 115.7(4) . . ? C23 C22 N1 121.8(4) . . ? C24 C23 C22 118.8(5) . . ? C23 C24 C25 119.2(5) . . ? C26 C25 C24 119.1(5) . . ? N21 C26 C25 122.5(5) . . ? N31 C32 C33 122.8(5) . . ? N31 C32 N1 113.9(4) . . ? C33 C32 N1 123.2(4) . . ? C34 C33 C32 117.3(5) . . ? C33 C34 C35 121.2(5) . . ? C36 C35 C34 116.3(5) . . ? N31 C36 C35 124.6(5) . . ? O41 C41 Re1 179.8(5) . . ? O51 C51 Re1 178.7(5) . . ? O61 C61 Re1 178.8(5) . . ? C161 Re2 C141 87.9(2) . . ? C161 Re2 C151 89.9(2) . . ? C141 Re2 C151 85.5(2) . . ? C161 Re2 N121 95.42(18) . . ? C141 Re2 N121 97.53(18) . . ? C151 Re2 N121 173.90(17) . . ? C161 Re2 N111 94.64(18) . . ? C141 Re2 N111 177.39(18) . . ? C151 Re2 N111 94.92(17) . . ? N121 Re2 N111 81.79(14) . . ? C161 Re2 Cl2 178.07(15) . . ? C141 Re2 Cl2 92.99(15) . . ? C151 Re2 Cl2 91.83(15) . . ? N121 Re2 Cl2 82.77(11) . . ? N111 Re2 Cl2 84.43(11) . . ? C132 N2 C122 117.8(4) . . ? C132 N2 C112 123.6(4) . . ? C122 N2 C112 117.6(4) . . ? C112 N111 C116 117.8(4) . . ? C112 N111 Re2 122.4(3) . . ? C116 N111 Re2 119.8(3) . . ? C122 N121 C126 117.0(4) . . ? C122 N121 Re2 121.2(3) . . ? C126 N121 Re2 121.6(3) . . ? C132 N131 C136 117.1(5) . . ? N111 C112 C113 122.7(4) . . ? N111 C112 N2 115.3(4) . . ? C113 C112 N2 121.9(4) . . ? C114 C113 C112 118.7(5) . . ? C113 C114 C115 119.3(5) . . ? C114 C115 C116 119.3(5) . . ? N111 C116 C115 122.2(4) . . ? N121 C122 C123 123.0(4) . . ? N121 C122 N2 116.9(4) . . ? C123 C122 N2 120.0(4) . . ? C124 C123 C122 118.9(4) . . ? C123 C124 C125 118.7(5) . . ? C126 C125 C124 119.2(5) . . ? N121 C126 C125 123.1(4) . . ? N131 C132 C133 123.0(5) . . ? N131 C132 N2 114.8(4) . . ? C133 C132 N2 122.1(5) . . ? C132 C133 C134 117.9(5) . . ? C135 C134 C133 120.7(5) . . ? C134 C135 C136 118.0(6) . . ? N131 C136 C135 123.3(6) . . ? O141 C141 Re2 176.8(4) . . ? O151 C151 Re2 177.8(4) . . ? O161 C161 Re2 176.5(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.351 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.167 #=END data_polo _database_code_depnum_ccdc_archive 'CCDC 222975' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Cl2 N8 O6 Re2' _chemical_formula_sum 'C36 H24 Cl2 N8 O6 Re2' _chemical_formula_weight 1107.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.125(4) _cell_length_b 14.259(4) _cell_length_c 14.454(6) _cell_angle_alpha 98.149(15) _cell_angle_beta 111.39(2) _cell_angle_gamma 112.669(15) _cell_volume 1860.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 0.62097 _cell_measurement_theta_max 1 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 6.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.04 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17961 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.1150 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8189 _reflns_number_gt 5973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8189 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 0.40018(4) 0.31733(2) 0.23004(2) 0.01587(10) Uani 1 1 d . . . Cl1 Cl 0.3295(2) 0.17444(16) 0.30887(16) 0.0201(4) Uani 1 1 d . . . O41 O 0.4737(8) 0.4956(6) 0.1331(6) 0.0403(18) Uani 1 1 d . . . O51 O 0.5927(7) 0.5000(5) 0.4422(5) 0.0230(13) Uani 1 1 d . . . O61 O 0.6770(7) 0.3017(6) 0.2540(5) 0.0356(17) Uani 1 1 d . . . N1 N 0.1247(8) 0.2758(5) 0.0270(5) 0.0169(15) Uani 1 1 d . . . N11 N 0.1881(7) 0.3069(5) 0.2053(5) 0.0151(14) Uani 1 1 d . . . N21 N 0.2572(7) 0.1828(5) 0.0805(5) 0.0138(14) Uani 1 1 d . . . N31 N 0.0877(8) 0.4865(5) -0.0851(6) 0.0214(16) Uani 1 1 d . . . C12 C 0.0857(9) 0.2896(6) 0.1097(7) 0.0172(17) Uani 1 1 d . . . C13 C -0.0473(9) 0.2832(6) 0.0901(6) 0.0167(17) Uani 1 1 d . . . H13A H -0.1142 0.2721 0.0227 0.020 Uiso 1 1 calc R . . C14 C -0.0800(9) 0.2938(6) 0.1745(6) 0.0179(18) Uani 1 1 d . . . H14A H -0.1700 0.2889 0.1645 0.021 Uiso 1 1 calc R . . C15 C 0.0236(10) 0.3115(7) 0.2720(7) 0.0207(19) Uani 1 1 d . . . H15A H 0.0048 0.3201 0.3294 0.025 Uiso 1 1 calc R . . C16 C 0.1551(10) 0.3166(6) 0.2861(7) 0.0181(18) Uani 1 1 d . . . H16A H 0.2231 0.3270 0.3528 0.022 Uiso 1 1 calc R . . C22 C 0.1433(9) 0.1835(6) 0.0042(7) 0.0175(17) Uani 1 1 d . . . C23 C 0.0442(9) 0.0966(6) -0.0893(6) 0.0172(17) Uani 1 1 d . . . H23A H -0.0360 0.0981 -0.1390 0.021 Uiso 1 1 calc R . . C24 C 0.0675(9) 0.0078(6) -0.1067(6) 0.0184(17) Uani 1 1 d . . . H24A H 0.0057 -0.0495 -0.1695 0.022 Uiso 1 1 calc R . . C25 C 0.1826(10) 0.0065(7) -0.0298(7) 0.0217(19) Uani 1 1 d . . . H25A H 0.2002 -0.0519 -0.0394 0.026 Uiso 1 1 calc R . . C26 C 0.2733(10) 0.0934(7) 0.0631(7) 0.0208(18) Uani 1 1 d . . . H26A H 0.3489 0.0900 0.1160 0.025 Uiso 1 1 calc R . . C32 C 0.0846(10) 0.4211(7) -0.0279(7) 0.0202(13) Uani 1 1 d . . . H32A H 0.0567 0.4316 0.0244 0.024 Uiso 1 1 calc R . . C33 C 0.1199(9) 0.3381(6) -0.0401(6) 0.0168(17) Uani 1 1 d . . . C34 C 0.1578(11) 0.3221(7) -0.1202(7) 0.028(2) Uani 1 1 d . . . H34A H 0.1806 0.2669 -0.1328 0.034 Uiso 1 1 calc R . . C35 C 0.1615(10) 0.3886(7) -0.1812(6) 0.0202(13) Uani 1 1 d . . . H35A H 0.1887 0.3791 -0.2341 0.024 Uiso 1 1 calc R . . C36 C 0.1246(11) 0.4694(7) -0.1634(7) 0.027(2) Uani 1 1 d . . . H36A H 0.1251 0.5128 -0.2059 0.033 Uiso 1 1 calc R . . C41 C 0.4412(9) 0.4243(8) 0.1652(7) 0.024(2) Uani 1 1 d . . . C51 C 0.5183(10) 0.4304(7) 0.3626(7) 0.0217(19) Uani 1 1 d . . . C61 C 0.5715(10) 0.3069(7) 0.2444(7) 0.0220(19) Uani 1 1 d . . . Re2 Re -0.52075(4) 0.12360(2) -0.20464(2) 0.01524(10) Uani 1 1 d . . . Cl2 Cl -0.2901(2) 0.11901(16) -0.17333(15) 0.0191(4) Uani 1 1 d . . . O141 O -0.4049(8) 0.2749(5) 0.0175(5) 0.0316(16) Uani 1 1 d . . . O151 O -0.8034(7) 0.1354(5) -0.2505(5) 0.0257(14) Uani 1 1 d . . . O161 O -0.6246(8) -0.0689(5) -0.1273(6) 0.0354(17) Uani 1 1 d . . . N2 N -0.6636(7) 0.1484(5) -0.4261(5) 0.0183(15) Uani 1 1 d . . . N111 N -0.4386(8) 0.2509(5) -0.2683(5) 0.0159(14) Uani 1 1 d . . . N121 N -0.6016(7) 0.0212(5) -0.3653(5) 0.0136(14) Uani 1 1 d . . . C135 C -1.0360(9) 0.1079(7) -0.5850(7) 0.0208(18) Uani 1 1 d . . . H13B H -1.1257 0.0566 -0.6408 0.025 Uiso 1 1 calc R . . C112 C -0.5222(9) 0.2430(6) -0.3674(6) 0.0167(17) Uani 1 1 d . . . C113 C -0.4763(10) 0.3194(7) -0.4135(7) 0.0215(19) Uani 1 1 d . . . H11A H -0.5365 0.3109 -0.4821 0.026 Uiso 1 1 calc R . . C114 C -0.3401(9) 0.4081(6) -0.3560(6) 0.0179(17) Uani 1 1 d . . . H11B H -0.3075 0.4610 -0.3850 0.021 Uiso 1 1 calc R . . C115 C -0.2525(10) 0.4179(7) -0.2551(7) 0.025(2) Uani 1 1 d . . . H11C H -0.1599 0.4771 -0.2148 0.030 Uiso 1 1 calc R . . C116 C -0.3055(9) 0.3381(7) -0.2154(7) 0.0218(19) Uani 1 1 d . . . H11D H -0.2454 0.3448 -0.1476 0.026 Uiso 1 1 calc R . . C122 C -0.6622(10) 0.0495(6) -0.4499(7) 0.0201(18) Uani 1 1 d . . . C123 C -0.7135(9) -0.0138(7) -0.5526(6) 0.0184(17) Uani 1 1 d . . . H12A H -0.7516 0.0080 -0.6092 0.022 Uiso 1 1 calc R . . C124 C -0.7067(9) -0.1092(7) -0.5690(7) 0.0203(18) Uani 1 1 d . . . H12B H -0.7455 -0.1539 -0.6372 0.024 Uiso 1 1 calc R . . C125 C -0.6431(9) -0.1382(6) -0.4851(6) 0.0164(17) Uani 1 1 d . . . H12C H -0.6369 -0.2017 -0.4951 0.020 Uiso 1 1 calc R . . C126 C -0.5870(9) -0.0679(6) -0.3822(6) 0.0173(17) Uani 1 1 d . . . H12D H -0.5386 -0.0843 -0.3246 0.021 Uiso 1 1 calc R . . C134 C -0.9171(10) 0.0896(7) -0.5509(7) 0.0225(19) Uani 1 1 d . . . H13C H -0.9261 0.0249 -0.5847 0.027 Uiso 1 1 calc R . . C133 C -0.7850(9) 0.1654(7) -0.4678(6) 0.0185(17) Uani 1 1 d . . . C132 C -0.7777(9) 0.2612(7) -0.4197(7) 0.0199(18) Uani 1 1 d . . . H13D H -0.6893 0.3136 -0.3635 0.024 Uiso 1 1 calc R . . N131 N -0.8932(9) 0.2810(6) -0.4512(7) 0.0307(19) Uani 1 1 d . . . C136 C -1.0171(10) 0.2052(8) -0.5333(8) 0.030(2) Uani 1 1 d . . . H13F H -1.0964 0.2189 -0.5573 0.035 Uiso 1 1 calc R . . C141 C -0.4464(10) 0.2180(8) -0.0642(7) 0.026(2) Uani 1 1 d . . . C151 C -0.6993(10) 0.1278(7) -0.2357(7) 0.0203(19) Uani 1 1 d . . . C161 C -0.5875(10) 0.0041(8) -0.1573(6) 0.023(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 Re1 0.01558(19) 0.02035(18) 0.01524(18) 0.00589(14) 0.00998(15) 0.00910(15) Cl1 0.0254(11) 0.0228(10) 0.0159(10) 0.0089(8) 0.0110(9) 0.0128(9) O41 0.038(5) 0.041(4) 0.037(4) 0.025(4) 0.017(4) 0.010(4) O51 0.023(3) 0.022(3) 0.022(3) 0.004(3) 0.012(3) 0.008(3) O61 0.027(4) 0.069(5) 0.024(3) 0.008(3) 0.015(3) 0.034(4) N1 0.019(4) 0.027(4) 0.011(3) 0.004(3) 0.011(3) 0.014(3) N11 0.017(4) 0.021(4) 0.021(4) 0.013(3) 0.011(3) 0.017(3) N21 0.012(3) 0.013(3) 0.014(3) 0.001(3) 0.009(3) 0.002(3) N31 0.021(4) 0.016(3) 0.034(4) 0.009(3) 0.019(4) 0.008(3) C12 0.023(5) 0.021(4) 0.024(4) 0.011(4) 0.019(4) 0.016(4) C13 0.020(5) 0.018(4) 0.012(4) 0.007(3) 0.006(4) 0.011(4) C14 0.026(5) 0.016(4) 0.026(5) 0.007(3) 0.021(4) 0.015(4) C15 0.030(5) 0.031(5) 0.016(4) 0.011(4) 0.019(4) 0.018(4) C16 0.026(5) 0.013(4) 0.019(4) 0.006(3) 0.016(4) 0.007(4) C22 0.015(4) 0.022(4) 0.021(4) 0.005(3) 0.014(4) 0.009(4) C23 0.012(4) 0.026(4) 0.013(4) 0.003(3) 0.009(4) 0.007(4) C24 0.011(4) 0.022(4) 0.016(4) 0.003(3) 0.008(4) 0.001(3) C25 0.029(5) 0.019(4) 0.026(5) 0.008(4) 0.022(4) 0.012(4) C26 0.023(5) 0.027(5) 0.023(5) 0.013(4) 0.018(4) 0.014(4) C32 0.030(4) 0.028(3) 0.021(3) 0.013(3) 0.023(3) 0.018(3) C33 0.017(4) 0.018(4) 0.017(4) 0.003(3) 0.013(4) 0.006(3) C34 0.051(6) 0.033(5) 0.037(5) 0.024(4) 0.037(5) 0.035(5) C35 0.030(4) 0.028(3) 0.021(3) 0.013(3) 0.023(3) 0.018(3) C36 0.039(6) 0.034(5) 0.032(5) 0.025(4) 0.029(5) 0.022(5) C41 0.013(4) 0.039(5) 0.016(4) 0.003(4) 0.003(4) 0.012(4) C51 0.023(5) 0.030(5) 0.022(5) 0.012(4) 0.014(4) 0.017(4) C61 0.017(5) 0.030(5) 0.018(4) 0.010(4) 0.010(4) 0.008(4) Re2 0.01595(19) 0.02003(18) 0.01365(17) 0.00545(13) 0.01038(15) 0.00881(14) Cl2 0.0172(10) 0.0254(10) 0.0163(10) 0.0050(8) 0.0087(9) 0.0112(9) O141 0.038(4) 0.039(4) 0.020(3) 0.005(3) 0.017(3) 0.018(3) O151 0.023(4) 0.036(4) 0.024(3) 0.004(3) 0.015(3) 0.016(3) O161 0.053(5) 0.031(4) 0.049(5) 0.026(3) 0.040(4) 0.025(4) N2 0.010(3) 0.024(4) 0.017(4) 0.001(3) 0.004(3) 0.008(3) N111 0.021(4) 0.019(3) 0.017(3) 0.010(3) 0.010(3) 0.016(3) N121 0.009(3) 0.008(3) 0.021(4) 0.008(3) 0.009(3) -0.001(3) C135 0.013(4) 0.023(4) 0.023(5) 0.009(4) 0.005(4) 0.008(4) C112 0.020(4) 0.012(4) 0.021(4) 0.003(3) 0.013(4) 0.008(3) C113 0.025(5) 0.031(5) 0.018(4) 0.008(4) 0.015(4) 0.018(4) C114 0.021(5) 0.021(4) 0.022(4) 0.009(3) 0.015(4) 0.013(4) C115 0.022(5) 0.028(5) 0.030(5) 0.007(4) 0.018(4) 0.012(4) C116 0.017(5) 0.027(5) 0.026(5) 0.009(4) 0.011(4) 0.014(4) C122 0.021(5) 0.013(4) 0.028(5) 0.008(3) 0.016(4) 0.005(3) C123 0.016(4) 0.029(5) 0.012(4) 0.012(3) 0.007(4) 0.010(4) C124 0.016(4) 0.021(4) 0.019(4) 0.000(3) 0.011(4) 0.004(4) C125 0.015(4) 0.019(4) 0.015(4) -0.002(3) 0.010(4) 0.006(3) C126 0.017(4) 0.025(4) 0.015(4) 0.010(3) 0.012(4) 0.010(4) C134 0.027(5) 0.024(5) 0.021(4) 0.009(4) 0.011(4) 0.016(4) C133 0.013(4) 0.031(5) 0.016(4) 0.013(4) 0.009(4) 0.010(4) C132 0.015(4) 0.024(4) 0.025(5) 0.009(4) 0.014(4) 0.010(4) N131 0.029(5) 0.033(5) 0.045(5) 0.018(4) 0.028(4) 0.015(4) C136 0.017(5) 0.051(6) 0.038(6) 0.029(5) 0.019(5) 0.022(5) C141 0.024(5) 0.047(6) 0.013(4) 0.006(4) 0.010(4) 0.023(5) C151 0.029(5) 0.019(4) 0.028(5) 0.008(4) 0.024(4) 0.015(4) C161 0.025(5) 0.043(6) 0.009(4) 0.008(4) 0.010(4) 0.020(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 C41 1.895(10) . ? Re1 C61 1.907(9) . ? Re1 C51 1.911(9) . ? Re1 N11 2.194(6) . ? Re1 N21 2.201(6) . ? Re1 Cl1 2.479(2) . ? O41 C41 1.164(11) . ? O51 C51 1.159(10) . ? O61 C61 1.164(10) . ? N1 C33 1.405(11) . ? N1 C22 1.421(10) . ? N1 C12 1.426(9) . ? N11 C12 1.344(11) . ? N11 C16 1.351(9) . ? N21 C22 1.347(11) . ? N21 C26 1.357(10) . ? N31 C32 1.330(10) . ? N31 C36 1.360(10) . ? C12 C13 1.363(11) . ? C13 C14 1.398(10) . ? C14 C15 1.368(12) . ? C15 C16 1.371(11) . ? C22 C23 1.401(11) . ? C23 C24 1.395(11) . ? C24 C25 1.364(12) . ? C25 C26 1.390(12) . ? C32 C33 1.391(11) . ? C33 C34 1.386(10) . ? C34 C35 1.384(12) . ? C35 C36 1.386(11) . ? Re2 C151 1.897(9) . ? Re2 C161 1.910(10) . ? Re2 C141 1.939(8) . ? Re2 N111 2.188(7) . ? Re2 N121 2.200(7) . ? Re2 Cl2 2.466(2) . ? O141 C141 1.143(9) . ? O151 C151 1.149(10) . ? O161 C161 1.170(11) . ? N2 C133 1.395(10) . ? N2 C122 1.411(10) . ? N2 C112 1.442(10) . ? N111 C116 1.345(11) . ? N111 C112 1.352(11) . ? N121 C126 1.341(10) . ? N121 C122 1.363(11) . ? C135 C134 1.373(12) . ? C135 C136 1.376(12) . ? C112 C113 1.384(12) . ? C113 C114 1.376(12) . ? C114 C115 1.377(12) . ? C115 C116 1.373(12) . ? C122 C123 1.397(11) . ? C123 C124 1.383(11) . ? C124 C125 1.373(12) . ? C125 C126 1.423(10) . ? C134 C133 1.375(12) . ? C133 C132 1.400(11) . ? C132 N131 1.352(11) . ? N131 C136 1.331(12) . ? 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 C41 Re1 C61 91.5(4) . . ? C41 Re1 C51 87.8(4) . . ? C61 Re1 C51 88.2(4) . . ? C41 Re1 N11 93.4(3) . . ? C61 Re1 N11 172.7(3) . . ? C51 Re1 N11 97.4(3) . . ? C41 Re1 N21 94.5(3) . . ? C61 Re1 N21 93.3(3) . . ? C51 Re1 N21 177.2(3) . . ? N11 Re1 N21 80.8(2) . . ? C41 Re1 Cl1 176.3(3) . . ? C61 Re1 Cl1 91.9(3) . . ? C51 Re1 Cl1 93.8(3) . . ? N11 Re1 Cl1 83.14(18) . . ? N21 Re1 Cl1 83.77(18) . . ? C33 N1 C22 121.0(6) . . ? C33 N1 C12 122.1(6) . . ? C22 N1 C12 116.0(6) . . ? C12 N11 C16 117.4(7) . . ? C12 N11 Re1 121.7(5) . . ? C16 N11 Re1 120.9(6) . . ? C22 N21 C26 117.0(7) . . ? C22 N21 Re1 120.7(5) . . ? C26 N21 Re1 122.2(6) . . ? C32 N31 C36 117.6(7) . . ? N11 C12 C13 124.1(7) . . ? N11 C12 N1 114.7(7) . . ? C13 C12 N1 121.2(8) . . ? C12 C13 C14 118.0(8) . . ? C15 C14 C13 118.3(7) . . ? C14 C15 C16 120.7(7) . . ? N11 C16 C15 121.5(8) . . ? N21 C22 C23 122.5(7) . . ? N21 C22 N1 115.7(7) . . ? C23 C22 N1 121.7(8) . . ? C24 C23 C22 119.1(8) . . ? C25 C24 C23 118.7(7) . . ? C24 C25 C26 119.4(8) . . ? N21 C26 C25 123.2(8) . . ? N31 C32 C33 125.1(7) . . ? C34 C33 C32 116.5(8) . . ? C34 C33 N1 120.6(7) . . ? C32 C33 N1 122.9(7) . . ? C35 C34 C33 119.8(7) . . ? C34 C35 C36 119.9(7) . . ? N31 C36 C35 121.2(8) . . ? O41 C41 Re1 174.8(8) . . ? O51 C51 Re1 178.2(8) . . ? O61 C61 Re1 179.2(9) . . ? C151 Re2 C161 89.4(4) . . ? C151 Re2 C141 86.7(4) . . ? C161 Re2 C141 88.3(4) . . ? C151 Re2 N111 94.4(3) . . ? C161 Re2 N111 174.2(3) . . ? C141 Re2 N111 96.3(3) . . ? C151 Re2 N121 93.6(3) . . ? C161 Re2 N121 93.6(3) . . ? C141 Re2 N121 178.1(3) . . ? N111 Re2 N121 81.8(2) . . ? C151 Re2 Cl2 177.0(3) . . ? C161 Re2 Cl2 92.7(3) . . ? C141 Re2 Cl2 95.5(3) . . ? N111 Re2 Cl2 83.37(18) . . ? N121 Re2 Cl2 84.16(18) . . ? C133 N2 C122 126.3(7) . . ? C133 N2 C112 116.8(7) . . ? C122 N2 C112 116.0(7) . . ? C116 N111 C112 116.3(7) . . ? C116 N111 Re2 123.9(6) . . ? C112 N111 Re2 119.8(5) . . ? C126 N121 C122 118.5(7) . . ? C126 N121 Re2 120.9(5) . . ? C122 N121 Re2 120.5(5) . . ? C134 C135 C136 117.4(8) . . ? N111 C112 C113 123.0(8) . . ? N111 C112 N2 116.9(7) . . ? C113 C112 N2 120.1(8) . . ? C114 C113 C112 118.8(8) . . ? C113 C114 C115 119.4(8) . . ? C116 C115 C114 118.3(9) . . ? N111 C116 C115 124.3(9) . . ? N121 C122 C123 121.6(7) . . ? N121 C122 N2 115.6(7) . . ? C123 C122 N2 122.7(8) . . ? C124 C123 C122 119.0(8) . . ? C125 C124 C123 120.4(7) . . ? C124 C125 C126 117.8(7) . . ? N121 C126 C125 122.4(8) . . ? C135 C134 C133 121.1(8) . . ? C134 C133 N2 123.4(8) . . ? C134 C133 C132 117.1(8) . . ? N2 C133 C132 119.4(7) . . ? N131 C132 C133 123.0(8) . . ? C136 N131 C132 116.9(8) . . ? N131 C136 C135 124.4(8) . . ? O141 C141 Re2 178.1(8) . . ? O151 C151 Re2 176.5(8) . . ? O161 C161 Re2 178.2(8) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 2.149 _refine_diff_density_min -2.181 _refine_diff_density_rms 0.235 #=END data_mooses _database_code_depnum_ccdc_archive 'CCDC 222976' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 Cl2 N8 O6 Re2' _chemical_formula_weight 1192.09 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 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 9.1998(15) _cell_length_b 21.486(4) _cell_length_c 21.451(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.700(4) _cell_angle_gamma 90.00 _cell_volume 4231.3(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 134 _cell_measurement_theta_min 0.780384 _cell_measurement_theta_max 1 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 5.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27110 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9673 _reflns_number_gt 7677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1998)' _computing_data_reduction 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 1998)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 1998)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0169P)^2^+1.3100P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9673 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0494 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.024417(16) 0.407276(7) 0.162973(7) 0.02216(4) Uani 1 1 d . . . Cl1 Cl 0.05086(12) 0.52027(5) 0.14682(6) 0.0402(3) Uani 1 1 d . . . O51 O -0.1561(4) 0.41881(16) 0.27753(16) 0.0506(9) Uani 1 1 d . . . O61 O -0.2579(3) 0.40253(14) 0.07899(15) 0.0406(8) Uani 1 1 d . . . O71 O -0.0013(3) 0.26839(13) 0.19092(13) 0.0321(7) Uani 1 1 d . . . N11 N 0.2384(3) 0.41412(14) 0.21227(14) 0.0228(7) Uani 1 1 d . . . N21 N 0.1632(3) 0.39552(14) 0.08509(14) 0.0225(7) Uani 1 1 d . . . N31 N 0.3335(3) 0.33648(14) 0.14792(14) 0.0213(7) Uani 1 1 d . . . N41 N 0.6531(4) 0.11248(16) 0.15722(18) 0.0362(9) Uani 1 1 d . . . C12 C 0.3483(4) 0.37565(16) 0.20155(17) 0.0211(8) Uani 1 1 d . . . C13 C 0.4737(4) 0.37381(17) 0.24104(18) 0.0266(9) Uani 1 1 d . . . H13A H 0.5492 0.3453 0.2333 0.032 Uiso 1 1 calc R . . C14 C 0.4885(4) 0.41340(18) 0.29149(19) 0.0298(9) Uani 1 1 d . . . H14A H 0.5730 0.4117 0.3193 0.036 Uiso 1 1 calc R . . C15 C 0.3789(4) 0.45560(18) 0.30108(19) 0.0298(9) Uani 1 1 d . . . H15A H 0.3878 0.4846 0.3345 0.036 Uiso 1 1 calc R . . C16 C 0.2574(4) 0.45435(18) 0.2609(2) 0.0294(9) Uani 1 1 d . . . H16A H 0.1818 0.4833 0.2675 0.035 Uiso 1 1 calc R . . C22 C 0.2806(4) 0.35833(16) 0.08864(18) 0.0226(8) Uani 1 1 d . . . C23 C 0.3466(4) 0.33955(18) 0.03476(19) 0.0278(9) Uani 1 1 d . . . H23A H 0.4274 0.3119 0.0378 0.033 Uiso 1 1 calc R . . C24 C 0.2945(5) 0.3611(2) -0.0223(2) 0.0380(11) Uani 1 1 d . . . H24A H 0.3381 0.3483 -0.0591 0.046 Uiso 1 1 calc R . . C25 C 0.1779(5) 0.4018(2) -0.0258(2) 0.0401(11) Uani 1 1 d . . . H25A H 0.1410 0.4180 -0.0649 0.048 Uiso 1 1 calc R . . C26 C 0.1174(5) 0.4181(2) 0.0279(2) 0.0330(10) Uani 1 1 d . . . H26A H 0.0387 0.4468 0.0254 0.040 Uiso 1 1 calc R . . C31 C 0.4190(4) 0.27931(17) 0.14987(17) 0.0228(8) Uani 1 1 d . . . C32 C 0.3517(4) 0.22409(16) 0.16467(17) 0.0209(8) Uani 1 1 d . . . H32A H 0.2516 0.2243 0.1730 0.025 Uiso 1 1 calc R . . C33 C 0.4280(4) 0.16885(17) 0.16748(18) 0.0244(9) Uani 1 1 d . . . H33A H 0.3800 0.1316 0.1785 0.029 Uiso 1 1 calc R . . C34 C 0.5757(4) 0.16671(18) 0.15433(18) 0.0241(8) Uani 1 1 d . . . C35 C 0.6423(4) 0.22342(18) 0.13943(19) 0.0263(9) Uani 1 1 d . . . H35A H 0.7421 0.2237 0.1304 0.032 Uiso 1 1 calc R . . C36 C 0.5651(4) 0.27849(18) 0.13767(18) 0.0256(9) Uani 1 1 d . . . H36A H 0.6126 0.3162 0.1280 0.031 Uiso 1 1 calc R . . C42 C 0.5772(6) 0.0540(2) 0.1631(3) 0.0597(16) Uani 1 1 d . . . H42A H 0.5246 0.0544 0.2014 0.089 Uiso 1 1 calc R . . H42B H 0.6476 0.0198 0.1649 0.089 Uiso 1 1 calc R . . H42C H 0.5077 0.0484 0.1269 0.089 Uiso 1 1 calc R . . C43 C 0.7981(5) 0.1104(2) 0.1343(2) 0.0417(12) Uani 1 1 d . . . H43A H 0.8628 0.1382 0.1594 0.063 Uiso 1 1 calc R . . H43B H 0.7937 0.1239 0.0905 0.063 Uiso 1 1 calc R . . H43C H 0.8357 0.0678 0.1374 0.063 Uiso 1 1 calc R . . C51 C -0.0878(5) 0.41626(19) 0.2341(2) 0.0333(10) Uani 1 1 d . . . C61 C -0.1527(4) 0.40421(18) 0.11191(19) 0.0287(9) Uani 1 1 d . . . C71 C 0.0117(4) 0.32017(19) 0.17852(18) 0.0235(8) Uani 1 1 d . . . Re2 Re 1.119321(16) 0.152335(7) 0.984360(7) 0.01881(4) Uani 1 1 d . . . Cl2 Cl 1.19681(10) 0.05662(4) 0.93139(4) 0.0259(2) Uani 1 1 d . . . O151 O 1.4389(3) 0.19006(14) 1.01254(13) 0.0363(7) Uani 1 1 d . . . O161 O 1.0098(3) 0.26931(13) 1.04784(13) 0.0359(7) Uani 1 1 d . . . O171 O 1.1286(3) 0.08692(14) 1.11156(13) 0.0372(7) Uani 1 1 d . . . N111 N 1.1133(3) 0.19739(14) 0.89258(14) 0.0199(7) Uani 1 1 d . . . N121 N 0.8981(3) 0.12913(14) 0.94832(14) 0.0203(7) Uani 1 1 d . . . N131 N 0.8672(3) 0.22744(14) 0.89705(14) 0.0217(7) Uani 1 1 d . . . N141 N 0.4957(4) 0.43441(18) 0.8577(2) 0.0505(11) Uani 1 1 d . . . C112 C 1.0046(4) 0.23587(17) 0.87334(17) 0.0215(8) Uani 1 1 d . . . C113 C 1.0284(4) 0.28379(19) 0.83103(19) 0.0293(9) Uani 1 1 d . . . H11A H 0.9540 0.3134 0.8207 0.035 Uiso 1 1 calc R . . C114 C 1.1592(4) 0.2876(2) 0.80480(19) 0.0323(10) Uani 1 1 d . . . H11B H 1.1770 0.3206 0.7768 0.039 Uiso 1 1 calc R . . C115 C 1.2658(4) 0.24361(19) 0.81894(19) 0.0311(10) Uani 1 1 d . . . H11C H 1.3544 0.2437 0.7985 0.037 Uiso 1 1 calc R . . C116 C 1.2399(4) 0.20026(18) 0.86303(18) 0.0251(9) Uani 1 1 d . . . H11D H 1.3137 0.1705 0.8738 0.030 Uiso 1 1 calc R . . C122 C 0.8112(4) 0.16905(16) 0.91483(17) 0.0188(8) Uani 1 1 d . . . C123 C 0.6652(4) 0.15456(18) 0.89937(19) 0.0289(9) Uani 1 1 d . . . H12A H 0.6045 0.1835 0.8765 0.035 Uiso 1 1 calc R . . C124 C 0.6096(4) 0.09842(18) 0.9172(2) 0.0306(9) Uani 1 1 d . . . H12B H 0.5102 0.0885 0.9071 0.037 Uiso 1 1 calc R . . C125 C 0.6991(4) 0.05658(18) 0.94995(19) 0.0274(9) Uani 1 1 d . . . H12C H 0.6634 0.0172 0.9622 0.033 Uiso 1 1 calc R . . C126 C 0.8407(4) 0.07347(17) 0.96419(18) 0.0237(8) Uani 1 1 d . . . H12D H 0.9026 0.0446 0.9865 0.028 Uiso 1 1 calc R . . C131 C 0.7640(4) 0.27835(17) 0.88668(18) 0.0229(8) Uani 1 1 d . . . C132 C 0.6876(4) 0.28683(19) 0.82997(19) 0.0283(9) Uani 1 1 d . . . H13B H 0.6971 0.2572 0.7976 0.034 Uiso 1 1 calc R . . C133 C 0.5968(4) 0.33790(18) 0.8193(2) 0.0302(10) Uani 1 1 d . . . H13C H 0.5438 0.3427 0.7801 0.036 Uiso 1 1 calc R . . C134 C 0.5833(4) 0.38275(19) 0.8670(2) 0.0334(10) Uani 1 1 d . . . C135 C 0.6621(5) 0.37314(19) 0.9237(2) 0.0348(10) Uani 1 1 d . . . H13D H 0.6552 0.4027 0.9564 0.042 Uiso 1 1 calc R . . C136 C 0.7507(4) 0.32113(18) 0.9336(2) 0.0293(9) Uani 1 1 d . . . H13E H 0.8023 0.3152 0.9730 0.035 Uiso 1 1 calc R . . C142 C 0.4071(6) 0.4424(2) 0.8007(3) 0.0600(16) Uani 1 1 d . . . H14B H 0.3505 0.4045 0.7917 0.090 Uiso 1 1 calc R . . H14C H 0.4697 0.4507 0.7664 0.090 Uiso 1 1 calc R . . H14D H 0.3407 0.4776 0.8051 0.090 Uiso 1 1 calc R . . C143 C 0.5159(6) 0.4875(2) 0.8998(3) 0.0639(17) Uani 1 1 d . . . H14E H 0.4755 0.4776 0.9398 0.096 Uiso 1 1 calc R . . H14F H 0.4655 0.5238 0.8811 0.096 Uiso 1 1 calc R . . H14G H 0.6200 0.4966 0.9066 0.096 Uiso 1 1 calc R . . C151 C 1.3196(5) 0.17571(18) 1.00454(17) 0.0255(9) Uani 1 1 d . . . C161 C 1.0519(4) 0.22573(18) 1.02384(17) 0.0229(8) Uani 1 1 d . . . C171 C 1.1234(4) 0.11121(18) 1.06361(19) 0.0247(9) 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 0.02049(8) 0.02201(8) 0.02389(8) -0.00022(7) 0.00079(6) 0.00098(6) Cl1 0.0408(7) 0.0246(5) 0.0543(7) 0.0045(5) -0.0047(5) 0.0029(5) O51 0.051(2) 0.056(2) 0.047(2) -0.0133(17) 0.0242(18) -0.0068(17) O61 0.0278(17) 0.0486(19) 0.0437(19) 0.0098(16) -0.0106(14) 0.0008(14) O71 0.0328(17) 0.0340(17) 0.0298(16) 0.0040(13) 0.0041(13) -0.0029(13) N11 0.0240(17) 0.0209(16) 0.0234(17) -0.0022(13) 0.0007(14) 0.0014(13) N21 0.0237(17) 0.0224(16) 0.0213(16) 0.0055(13) 0.0004(13) 0.0020(13) N31 0.0218(17) 0.0212(16) 0.0205(16) -0.0011(13) -0.0010(13) 0.0044(13) N41 0.034(2) 0.0261(19) 0.050(2) -0.0005(17) 0.0102(18) 0.0068(16) C12 0.025(2) 0.0157(18) 0.0220(19) 0.0006(15) -0.0013(16) -0.0029(15) C13 0.031(2) 0.0202(19) 0.028(2) -0.0005(17) -0.0054(18) 0.0049(17) C14 0.031(2) 0.025(2) 0.032(2) -0.0007(18) -0.0071(18) -0.0003(18) C15 0.036(2) 0.030(2) 0.024(2) -0.0063(18) 0.0012(18) -0.0050(19) C16 0.027(2) 0.028(2) 0.033(2) -0.0073(19) 0.0022(18) -0.0003(17) C22 0.024(2) 0.0202(19) 0.0228(19) 0.0008(16) -0.0009(16) -0.0046(16) C23 0.026(2) 0.029(2) 0.029(2) 0.0025(18) 0.0062(17) 0.0023(17) C24 0.037(3) 0.055(3) 0.023(2) 0.004(2) 0.0050(19) 0.004(2) C25 0.038(3) 0.056(3) 0.026(2) 0.016(2) 0.001(2) 0.004(2) C26 0.032(2) 0.036(2) 0.030(2) 0.0116(19) 0.0003(19) 0.0038(19) C31 0.024(2) 0.024(2) 0.0199(19) -0.0014(16) -0.0020(16) 0.0042(16) C32 0.022(2) 0.0200(19) 0.0210(19) 0.0001(15) 0.0029(16) -0.0002(15) C33 0.027(2) 0.0187(19) 0.028(2) 0.0006(16) 0.0002(17) -0.0020(16) C34 0.024(2) 0.026(2) 0.0217(19) -0.0017(16) -0.0005(16) 0.0041(16) C35 0.016(2) 0.030(2) 0.033(2) -0.0020(18) 0.0017(17) 0.0046(16) C36 0.024(2) 0.023(2) 0.030(2) 0.0014(17) -0.0011(17) -0.0062(16) C42 0.058(3) 0.026(3) 0.098(5) 0.003(3) 0.027(3) 0.008(2) C43 0.041(3) 0.036(3) 0.049(3) -0.005(2) 0.008(2) 0.015(2) C51 0.027(2) 0.030(2) 0.043(3) -0.007(2) -0.001(2) -0.0048(18) C61 0.028(2) 0.026(2) 0.033(2) 0.0054(18) 0.0095(19) 0.0053(18) C71 0.018(2) 0.032(2) 0.0213(19) -0.0079(17) 0.0034(16) -0.0032(17) Re2 0.01952(8) 0.02072(8) 0.01603(7) 0.00010(6) -0.00008(6) -0.00051(6) Cl2 0.0307(5) 0.0228(5) 0.0238(5) 0.0002(4) -0.0008(4) 0.0045(4) O151 0.0222(16) 0.056(2) 0.0296(16) -0.0079(15) -0.0020(13) -0.0065(14) O161 0.0419(18) 0.0340(17) 0.0317(16) -0.0141(14) 0.0013(14) 0.0043(14) O171 0.0385(18) 0.0457(19) 0.0271(16) 0.0156(14) -0.0008(13) -0.0069(14) N111 0.0199(17) 0.0216(16) 0.0180(16) -0.0021(13) -0.0010(13) -0.0018(13) N121 0.0239(17) 0.0179(15) 0.0193(16) -0.0008(13) 0.0034(13) 0.0005(13) N131 0.0201(17) 0.0202(16) 0.0248(17) 0.0022(13) 0.0012(13) 0.0025(13) N141 0.045(3) 0.032(2) 0.072(3) 0.000(2) -0.010(2) 0.0157(18) C112 0.025(2) 0.0218(19) 0.0175(19) -0.0032(15) 0.0000(16) -0.0031(16) C113 0.027(2) 0.032(2) 0.029(2) 0.0087(18) -0.0005(18) -0.0020(18) C114 0.033(2) 0.036(2) 0.027(2) 0.0118(19) -0.0029(19) -0.0093(19) C115 0.027(2) 0.042(3) 0.025(2) 0.0014(19) 0.0061(18) -0.0045(19) C116 0.022(2) 0.031(2) 0.023(2) -0.0028(17) 0.0035(16) -0.0004(17) C122 0.021(2) 0.0168(18) 0.0189(18) -0.0004(15) 0.0037(15) 0.0018(15) C123 0.024(2) 0.026(2) 0.035(2) 0.0045(19) -0.0037(18) 0.0025(17) C124 0.020(2) 0.031(2) 0.040(2) 0.003(2) 0.0027(18) -0.0003(17) C125 0.025(2) 0.024(2) 0.033(2) 0.0012(17) 0.0046(18) -0.0051(17) C126 0.025(2) 0.0236(19) 0.023(2) 0.0034(16) 0.0040(17) 0.0008(16) C131 0.024(2) 0.0207(19) 0.024(2) 0.0057(16) 0.0019(16) 0.0033(16) C132 0.025(2) 0.029(2) 0.031(2) -0.0006(18) 0.0024(18) 0.0032(17) C133 0.027(2) 0.029(2) 0.034(2) 0.0095(19) -0.0056(18) -0.0002(17) C134 0.028(2) 0.024(2) 0.048(3) 0.005(2) -0.001(2) 0.0039(18) C135 0.039(3) 0.026(2) 0.039(3) -0.0044(19) 0.002(2) 0.0081(19) C136 0.027(2) 0.030(2) 0.031(2) -0.0005(18) -0.0013(18) 0.0021(18) C142 0.048(3) 0.042(3) 0.088(5) 0.024(3) -0.008(3) 0.010(2) C143 0.062(4) 0.030(3) 0.100(5) -0.005(3) 0.000(3) 0.015(2) C151 0.032(2) 0.028(2) 0.0171(19) -0.0035(16) 0.0029(17) 0.0021(18) C161 0.019(2) 0.032(2) 0.0178(19) 0.0045(17) -0.0016(15) -0.0060(17) C171 0.018(2) 0.029(2) 0.028(2) 0.0013(18) 0.0009(16) -0.0045(16) _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 C61 1.905(4) . ? Re1 C71 1.906(4) . ? Re1 C51 1.907(5) . ? Re1 N11 2.178(3) . ? Re1 N21 2.182(3) . ? Re1 Cl1 2.4666(11) . ? O51 C51 1.158(5) . ? O61 C61 1.162(5) . ? O71 C71 1.152(4) . ? N11 C12 1.338(5) . ? N11 C16 1.358(5) . ? N21 C22 1.342(5) . ? N21 C26 1.361(5) . ? N31 C22 1.412(5) . ? N31 C12 1.425(5) . ? N31 C31 1.458(5) . ? N41 C34 1.365(5) . ? N41 C42 1.446(6) . ? N41 C43 1.452(5) . ? C12 C13 1.387(5) . ? C13 C14 1.376(5) . ? C14 C15 1.381(5) . ? C15 C16 1.367(5) . ? C22 C23 1.399(5) . ? C23 C24 1.366(6) . ? C24 C25 1.382(6) . ? C25 C26 1.357(6) . ? C31 C32 1.384(5) . ? C31 C36 1.387(5) . ? C32 C33 1.378(5) . ? C33 C34 1.406(5) . ? C34 C35 1.410(5) . ? C35 C36 1.379(5) . ? Re2 C161 1.912(4) . ? Re2 C171 1.914(4) . ? Re2 C151 1.932(4) . ? Re2 N121 2.188(3) . ? Re2 N111 2.191(3) . ? Re2 Cl2 2.4765(10) . ? O151 C151 1.142(5) . ? O161 C161 1.148(4) . ? O171 C171 1.152(5) . ? N111 C112 1.341(5) . ? N111 C116 1.363(5) . ? N121 C122 1.348(4) . ? N121 C126 1.359(5) . ? N131 C112 1.404(5) . ? N131 C122 1.418(4) . ? N131 C131 1.456(4) . ? N141 C134 1.378(5) . ? N141 C142 1.436(6) . ? N141 C143 1.458(6) . ? C112 C113 1.399(5) . ? C113 C114 1.363(5) . ? C114 C115 1.382(6) . ? C115 C116 1.360(5) . ? C122 C123 1.397(5) . ? C123 C124 1.374(5) . ? C124 C125 1.380(5) . ? C125 C126 1.368(5) . ? C131 C136 1.374(5) . ? C131 C132 1.377(5) . ? C132 C133 1.389(5) . ? C133 C134 1.416(6) . ? C134 C135 1.392(6) . ? C135 C136 1.392(5) . ? 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 C61 Re1 C71 90.39(16) . . ? C61 Re1 C51 88.66(17) . . ? C71 Re1 C51 85.23(17) . . ? C61 Re1 N11 173.72(15) . . ? C71 Re1 N11 92.59(13) . . ? C51 Re1 N11 97.09(15) . . ? C61 Re1 N21 94.40(14) . . ? C71 Re1 N21 93.78(14) . . ? C51 Re1 N21 176.79(15) . . ? N11 Re1 N21 79.89(12) . . ? C61 Re1 Cl1 92.39(12) . . ? C71 Re1 Cl1 177.18(11) . . ? C51 Re1 Cl1 94.37(13) . . ? N11 Re1 Cl1 84.70(8) . . ? N21 Re1 Cl1 86.47(8) . . ? C12 N11 C16 117.7(3) . . ? C12 N11 Re1 123.0(2) . . ? C16 N11 Re1 118.9(3) . . ? C22 N21 C26 117.7(3) . . ? C22 N21 Re1 122.3(2) . . ? C26 N21 Re1 119.1(3) . . ? C22 N31 C12 122.7(3) . . ? C22 N31 C31 117.4(3) . . ? C12 N31 C31 116.8(3) . . ? C34 N41 C42 119.4(4) . . ? C34 N41 C43 119.9(4) . . ? C42 N41 C43 117.6(4) . . ? N11 C12 C13 121.4(3) . . ? N11 C12 N31 118.0(3) . . ? C13 C12 N31 120.6(3) . . ? C14 C13 C12 119.9(4) . . ? C13 C14 C15 119.1(4) . . ? C16 C15 C14 117.9(4) . . ? N11 C16 C15 123.8(4) . . ? N21 C22 C23 121.0(3) . . ? N21 C22 N31 118.6(3) . . ? C23 C22 N31 120.4(3) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C25 119.3(4) . . ? C26 C25 C24 118.4(4) . . ? C25 C26 N21 123.6(4) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 N31 118.7(3) . . ? C36 C31 N31 122.2(3) . . ? C33 C32 C31 121.0(4) . . ? C32 C33 C34 121.0(3) . . ? N41 C34 C33 121.8(4) . . ? N41 C34 C35 121.0(4) . . ? C33 C34 C35 117.2(3) . . ? C36 C35 C34 121.1(4) . . ? C35 C36 C31 120.6(4) . . ? O51 C51 Re1 176.9(4) . . ? O61 C61 Re1 177.7(4) . . ? O71 C71 Re1 175.8(3) . . ? C161 Re2 C171 88.61(16) . . ? C161 Re2 C151 91.05(16) . . ? C171 Re2 C151 87.54(16) . . ? C161 Re2 N121 91.34(13) . . ? C171 Re2 N121 99.97(13) . . ? C151 Re2 N121 172.16(14) . . ? C161 Re2 N111 92.49(13) . . ? C171 Re2 N111 178.69(14) . . ? C151 Re2 N111 93.16(14) . . ? N121 Re2 N111 79.29(11) . . ? C161 Re2 Cl2 177.74(11) . . ? C171 Re2 Cl2 91.97(12) . . ? C151 Re2 Cl2 91.15(12) . . ? N121 Re2 Cl2 86.41(8) . . ? N111 Re2 Cl2 86.91(8) . . ? C112 N111 C116 118.1(3) . . ? C112 N111 Re2 121.6(2) . . ? C116 N111 Re2 117.7(2) . . ? C122 N121 C126 117.8(3) . . ? C122 N121 Re2 123.4(2) . . ? C126 N121 Re2 118.7(2) . . ? C112 N131 C122 124.3(3) . . ? C112 N131 C131 116.2(3) . . ? C122 N131 C131 117.4(3) . . ? C134 N141 C142 120.9(4) . . ? C134 N141 C143 119.4(4) . . ? C142 N141 C143 118.4(4) . . ? N111 C112 C113 120.6(4) . . ? N111 C112 N131 118.6(3) . . ? C113 C112 N131 120.8(3) . . ? C114 C113 C112 119.4(4) . . ? C113 C114 C115 120.1(4) . . ? C116 C115 C114 117.9(4) . . ? C115 C116 N111 123.2(4) . . ? N121 C122 C123 120.8(3) . . ? N121 C122 N131 119.5(3) . . ? C123 C122 N131 119.6(3) . . ? C124 C123 C122 119.9(4) . . ? C123 C124 C125 119.5(4) . . ? C126 C125 C124 118.0(4) . . ? N121 C126 C125 123.9(4) . . ? C136 C131 C132 119.6(4) . . ? C136 C131 N131 118.6(3) . . ? C132 C131 N131 121.7(3) . . ? C131 C132 C133 121.1(4) . . ? C132 C133 C134 119.9(4) . . ? N141 C134 C135 120.8(4) . . ? N141 C134 C133 121.5(4) . . ? C135 C134 C133 117.8(4) . . ? C136 C135 C134 121.3(4) . . ? C131 C136 C135 120.3(4) . . ? O151 C151 Re2 175.7(3) . . ? O161 C161 Re2 179.0(4) . . ? O171 C171 Re2 178.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.777 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.123 #=END