# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_pireol1scn _database_code_depnum_ccdc_archive 'CCDC 911727' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(N-(N'',N''-diethylaminothiocarbonyl)-N'(N''', N'''-methylphenylcarbothioamide) benzamidineto)(isothiocyanate)oxorhenium(V)' ; _chemical_name_common '[ReO(mptsc)(SCN)]' _chemical_melting_point ? _chemical_formula_moiety 'C21 H23 N6 O Re S3' _chemical_formula_sum 'C21 H23 N6 O Re S3' _chemical_formula_weight 657.83 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.2080(8) _cell_length_b 14.1464(10) _cell_length_c 16.7610(10) _cell_angle_alpha 101.908(5) _cell_angle_beta 90.361(6) _cell_angle_gamma 111.658(6) _cell_volume 2406.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14799 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 29.52 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.091 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 5.335 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3029 _exptl_absorpt_correction_T_max 0.5461 _exptl_absorpt_process_details X-Area _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25604 _diffrn_reflns_av_R_equivalents 0.0928 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 29.24 _reflns_number_total 12813 _reflns_number_gt 7310 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00455(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12813 _refine_ls_number_parameters 584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _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 0.07689(3) 0.09476(2) 0.238170(17) 0.02708(9) Uani 1 1 d . . . S2A S 0.0136(2) 0.09636(14) 0.36699(12) 0.0337(4) Uani 1 1 d . . . S1A S -0.0158(2) 0.10167(14) 0.11711(11) 0.0341(4) Uani 1 1 d . . . S6A S -0.2370(3) -0.25637(17) 0.17593(16) 0.0511(6) Uani 1 1 d . . . N6A N -0.0589(7) -0.0539(5) 0.2096(4) 0.0356(16) Uani 1 1 d . . . N3A N 0.1405(6) 0.2976(5) 0.3639(4) 0.0308(14) Uani 1 1 d . . . N1A N 0.1358(6) 0.3098(4) 0.1581(4) 0.0302(13) Uani 1 1 d . . . N5A N -0.0427(6) 0.2597(5) 0.0693(4) 0.0314(13) Uani 1 1 d . . . O1A O 0.2168(6) 0.0800(4) 0.2268(4) 0.0424(14) Uani 1 1 d . . . N2A N 0.1250(6) 0.2469(4) 0.2802(4) 0.0272(13) Uani 1 1 d . . . C22A C 0.3337(7) 0.4985(6) 0.2360(5) 0.0310(16) Uani 1 1 d . . . H22A H 0.2703 0.5075 0.2058 0.037 Uiso 1 1 calc R . . N4A N 0.0884(7) 0.2669(5) 0.4918(4) 0.0338(15) Uani 1 1 d . . . C21A C 0.3073(8) 0.4048(6) 0.2600(4) 0.0295(16) Uani 1 1 d . . . C6A C -0.1358(8) -0.1376(6) 0.1941(5) 0.0341(17) Uani 1 1 d . . . C26A C 0.4032(8) 0.3934(6) 0.3068(5) 0.0374(19) Uani 1 1 d . . . H26A H 0.3862 0.3322 0.3249 0.045 Uiso 1 1 calc R . . C2A C 0.1824(7) 0.3159(5) 0.2315(4) 0.0294(16) Uani 1 1 d . . . C24A C 0.5474(9) 0.5662(7) 0.3018(5) 0.042(2) Uani 1 1 d . . . H24A H 0.6273 0.6206 0.3161 0.051 Uiso 1 1 calc R . . C23A C 0.4533(9) 0.5781(6) 0.2566(5) 0.040(2) Uani 1 1 d . . . H23A H 0.4703 0.6402 0.2398 0.048 Uiso 1 1 calc R . . C1A C 0.0292(8) 0.2340(6) 0.1161(4) 0.0335(16) Uani 1 1 d . . . C3A C 0.0851(8) 0.2329(6) 0.4089(5) 0.0300(16) Uani 1 1 d . . . C41A C -0.0132(7) 0.2139(5) 0.5355(5) 0.0304(17) Uani 1 1 d . . . C42A C -0.1410(8) 0.1758(7) 0.5031(5) 0.039(2) Uani 1 1 d . . . H42A H -0.1609 0.1853 0.4522 0.047 Uiso 1 1 calc R . . C43A C -0.2380(9) 0.1240(7) 0.5469(6) 0.043(2) Uani 1 1 d . . . H43A H -0.3231 0.0959 0.5243 0.052 Uiso 1 1 calc R . . C47A C 0.1685(11) 0.3765(7) 0.5275(6) 0.055(3) Uani 1 1 d . . . H47A H 0.2522 0.3933 0.5075 0.082 Uiso 1 1 calc R . . H47B H 0.1771 0.3875 0.5861 0.082 Uiso 1 1 calc R . . H47C H 0.1286 0.4205 0.5124 0.082 Uiso 1 1 calc R . . C51A C -0.1558(8) 0.1803(6) 0.0133(5) 0.0386(18) Uani 1 1 d . . . H51A H -0.2045 0.1267 0.0415 0.046 Uiso 1 1 calc R . . H51B H -0.2119 0.2137 -0.0010 0.046 Uiso 1 1 calc R . . C52A C -0.1136(9) 0.1312(8) -0.0627(6) 0.051(2) Uani 1 1 d . . . H52A H -0.0676 0.1839 -0.0915 0.076 Uiso 1 1 calc R . . H52B H -0.1878 0.0803 -0.0970 0.076 Uiso 1 1 calc R . . H52C H -0.0584 0.0978 -0.0487 0.076 Uiso 1 1 calc R . . C25A C 0.5238(8) 0.4739(6) 0.3260(6) 0.041(2) Uani 1 1 d . . . H25A H 0.5887 0.4655 0.3552 0.049 Uiso 1 1 calc R . . C45A C -0.0834(8) 0.1526(6) 0.6565(5) 0.0361(18) Uani 1 1 d . . . H45A H -0.0646 0.1454 0.7085 0.043 Uiso 1 1 calc R . . C46A C 0.0154(8) 0.2020(6) 0.6126(5) 0.0315(16) Uani 1 1 d . . . H46A H 0.1006 0.2272 0.6346 0.038 Uiso 1 1 calc R . . C44A C -0.2096(9) 0.1138(6) 0.6236(6) 0.045(2) Uani 1 1 d . . . H44A H -0.2757 0.0806 0.6535 0.054 Uiso 1 1 calc R . . C53A C -0.0083(9) 0.3714(7) 0.0671(5) 0.0429(19) Uani 1 1 d . . . H53C H 0.0275 0.4147 0.1211 0.051 Uiso 1 1 calc R . . H53D H -0.0858 0.3820 0.0530 0.051 Uiso 1 1 calc R . . C54A C 0.0893(13) 0.4059(9) 0.0052(7) 0.069(3) Uani 1 1 d . . . H54D H 0.1613 0.3869 0.0143 0.104 Uiso 1 1 calc R . . H54E H 0.1188 0.4803 0.0119 0.104 Uiso 1 1 calc R . . H54F H 0.0491 0.3723 -0.0493 0.104 Uiso 1 1 calc R . . S2B S 0.5148(2) 0.09199(14) 0.35707(12) 0.0356(5) Uani 1 1 d . . . S1B S 0.5012(2) 0.08800(15) 0.10474(12) 0.0383(5) Uani 1 1 d . . . S6B S 0.2770(3) -0.26830(17) 0.16451(16) 0.0517(6) Uani 1 1 d . . . N6B N 0.4495(7) -0.0636(5) 0.2005(4) 0.0393(17) Uani 1 1 d . . . O1B O 0.7256(6) 0.0689(5) 0.2247(4) 0.0466(16) Uani 1 1 d . . . N2B N 0.6357(6) 0.2390(5) 0.2671(4) 0.0296(14) Uani 1 1 d . . . N3B N 0.6434(6) 0.2910(5) 0.3499(4) 0.0317(14) Uani 1 1 d . . . C21B C 0.8166(7) 0.3978(5) 0.2518(5) 0.0301(16) Uani 1 1 d . . . N1B N 0.6616(7) 0.2951(5) 0.1404(4) 0.0376(15) Uani 1 1 d . . . C22B C 0.8385(8) 0.4897(6) 0.2241(5) 0.0347(18) Uani 1 1 d . . . H22B H 0.7764 0.4943 0.1897 0.042 Uiso 1 1 calc R . . N4B N 0.5838(7) 0.2655(5) 0.4776(4) 0.0392(16) Uani 1 1 d . . . C6B C 0.3762(8) -0.1492(7) 0.1851(5) 0.0359(18) Uani 1 1 d . . . C26B C 0.9082(8) 0.3923(6) 0.3039(5) 0.0356(18) Uani 1 1 d . . . H26B H 0.8919 0.3327 0.3241 0.043 Uiso 1 1 calc R . . C25B C 1.0246(8) 0.4762(6) 0.3260(5) 0.041(2) Uani 1 1 d . . . H25B H 1.0891 0.4712 0.3582 0.049 Uiso 1 1 calc R . . C24B C 1.0450(8) 0.5671(6) 0.3003(5) 0.041(2) Uani 1 1 d . . . H24B H 1.1212 0.6247 0.3180 0.049 Uiso 1 1 calc R . . C2B C 0.6975(7) 0.3051(5) 0.2182(5) 0.0311(16) Uani 1 1 d . . . C23B C 0.9544(9) 0.5731(6) 0.2494(5) 0.041(2) Uani 1 1 d . . . H23B H 0.9706 0.6341 0.2313 0.049 Uiso 1 1 calc R . . C1B C 0.5599(8) 0.2169(6) 0.0952(5) 0.0347(16) Uani 1 1 d . . . N5B N 0.5132(7) 0.2411(5) 0.0326(4) 0.0406(15) Uani 1 1 d . . . C3B C 0.5876(8) 0.2297(6) 0.3966(5) 0.0305(16) Uani 1 1 d . . . C53B C 0.5601(10) 0.3503(7) 0.0217(5) 0.048(2) Uani 1 1 d . . . H53A H 0.6533 0.3811 0.0318 0.057 Uiso 1 1 calc R . . H53B H 0.5379 0.3496 -0.0346 0.057 Uiso 1 1 calc R . . C54B C 0.5051(12) 0.4143(9) 0.0763(7) 0.068(3) Uani 1 1 d . . . H54A H 0.4143 0.3903 0.0611 0.101 Uiso 1 1 calc R . . H54B H 0.5460 0.4857 0.0723 0.101 Uiso 1 1 calc R . . H54C H 0.5187 0.4091 0.1316 0.101 Uiso 1 1 calc R . . C51B C 0.4037(9) 0.1613(7) -0.0242(5) 0.0452(19) Uani 1 1 d . . . H51C H 0.4126 0.0943 -0.0331 0.054 Uiso 1 1 calc R . . H51D H 0.4051 0.1806 -0.0766 0.054 Uiso 1 1 calc R . . C52B C 0.2767(9) 0.1520(8) 0.0106(6) 0.056(2) Uani 1 1 d . . . H52D H 0.2777 0.1379 0.0641 0.084 Uiso 1 1 calc R . . H52E H 0.2077 0.0960 -0.0246 0.084 Uiso 1 1 calc R . . H52F H 0.2639 0.2162 0.0142 0.084 Uiso 1 1 calc R . . C47B C 0.6639(11) 0.3754(7) 0.5133(6) 0.061(3) Uani 1 1 d . . . H47D H 0.7512 0.3893 0.5003 0.091 Uiso 1 1 calc R . . H47E H 0.6615 0.3891 0.5717 0.091 Uiso 1 1 calc R . . H47F H 0.6314 0.4196 0.4913 0.091 Uiso 1 1 calc R . . C41B C 0.4850(8) 0.2119(6) 0.5237(5) 0.0309(16) Uani 1 1 d . . . C42B C 0.3568(8) 0.1712(7) 0.4911(5) 0.0385(19) Uani 1 1 d . . . H42B H 0.3354 0.1791 0.4399 0.046 Uiso 1 1 calc R . . C46B C 0.5154(8) 0.2039(6) 0.6008(5) 0.0366(19) Uani 1 1 d . . . H46B H 0.6007 0.2321 0.6230 0.044 Uiso 1 1 calc R . . C45B C 0.4177(9) 0.1533(6) 0.6448(5) 0.039(2) Uani 1 1 d . . . H45B H 0.4382 0.1479 0.6971 0.047 Uiso 1 1 calc R . . C44B C 0.2914(9) 0.1109(7) 0.6135(6) 0.044(2) Uani 1 1 d . . . H44B H 0.2268 0.0773 0.6441 0.053 Uiso 1 1 calc R . . C43B C 0.2617(8) 0.1186(7) 0.5365(5) 0.043(2) Uani 1 1 d . . . H43B H 0.1763 0.0882 0.5142 0.052 Uiso 1 1 calc R . . Re2 Re 0.58513(3) 0.08464(2) 0.230053(18) 0.02960(10) 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 0.02987(19) 0.02283(15) 0.02645(16) 0.00588(12) 0.00189(13) 0.00743(14) S2A 0.0409(12) 0.0243(8) 0.0280(9) 0.0072(7) 0.0027(8) 0.0026(8) S1A 0.0388(11) 0.0286(8) 0.0293(9) 0.0064(7) -0.0035(8) 0.0064(8) S6A 0.0512(15) 0.0324(10) 0.0532(13) 0.0100(10) -0.0022(12) -0.0031(11) N6A 0.042(4) 0.021(3) 0.037(4) 0.005(3) -0.002(3) 0.006(3) N3A 0.038(4) 0.023(3) 0.027(3) 0.005(2) 0.004(3) 0.007(3) N1A 0.036(3) 0.024(3) 0.029(3) 0.011(2) 0.001(3) 0.006(3) N5A 0.033(3) 0.033(3) 0.028(3) 0.010(2) -0.002(2) 0.010(3) O1A 0.043(3) 0.040(3) 0.041(3) 0.005(3) 0.006(3) 0.014(3) N2A 0.029(3) 0.024(3) 0.026(3) 0.006(2) 0.005(2) 0.009(3) C22A 0.027(4) 0.029(3) 0.035(4) 0.011(3) 0.005(3) 0.007(3) N4A 0.041(4) 0.024(3) 0.025(3) 0.002(2) -0.001(3) 0.000(3) C21A 0.033(4) 0.030(4) 0.028(3) 0.009(3) 0.004(3) 0.013(3) C6A 0.031(4) 0.034(4) 0.034(4) 0.011(3) 0.003(3) 0.007(4) C26A 0.040(5) 0.029(4) 0.043(5) 0.012(3) 0.003(4) 0.011(4) C2A 0.033(4) 0.028(3) 0.027(3) 0.005(3) 0.002(3) 0.012(3) C24A 0.034(5) 0.035(4) 0.049(5) 0.010(4) 0.003(4) 0.004(4) C23A 0.046(5) 0.027(4) 0.045(5) 0.013(3) 0.010(4) 0.010(4) C1A 0.035(4) 0.036(4) 0.029(4) 0.006(3) 0.004(3) 0.015(3) C3A 0.031(4) 0.025(3) 0.030(4) 0.009(3) 0.003(3) 0.006(3) C41A 0.029(4) 0.024(3) 0.033(4) 0.002(3) 0.006(3) 0.007(3) C42A 0.036(5) 0.047(5) 0.034(4) 0.004(4) -0.006(3) 0.018(4) C43A 0.030(4) 0.047(5) 0.046(5) 0.005(4) 0.008(4) 0.009(4) C47A 0.066(7) 0.032(4) 0.035(4) 0.000(4) 0.005(4) -0.013(4) C51A 0.035(4) 0.042(4) 0.039(4) 0.008(3) -0.007(3) 0.016(4) C52A 0.047(5) 0.057(5) 0.045(5) 0.003(4) -0.001(4) 0.022(5) C25A 0.033(5) 0.035(4) 0.053(5) 0.015(4) 0.004(4) 0.009(4) C45A 0.044(5) 0.031(4) 0.035(4) 0.015(3) 0.009(4) 0.012(4) C46A 0.034(4) 0.030(3) 0.032(4) 0.011(3) 0.003(3) 0.012(3) C44A 0.035(5) 0.035(4) 0.054(5) 0.011(4) 0.023(4) -0.001(4) C53A 0.049(5) 0.041(4) 0.045(5) 0.021(4) 0.001(4) 0.019(4) C54A 0.094(9) 0.061(6) 0.068(7) 0.045(5) 0.032(6) 0.031(6) S2B 0.0401(12) 0.0251(8) 0.0341(10) 0.0067(8) 0.0073(9) 0.0036(9) S1B 0.0458(12) 0.0305(9) 0.0326(10) 0.0062(8) -0.0021(9) 0.0079(9) S6B 0.0552(15) 0.0317(10) 0.0590(14) 0.0116(10) -0.0038(12) 0.0052(11) N6B 0.049(5) 0.027(3) 0.038(4) 0.010(3) 0.000(3) 0.008(3) O1B 0.049(4) 0.060(4) 0.042(3) 0.017(3) 0.005(3) 0.032(3) N2B 0.026(3) 0.029(3) 0.030(3) 0.006(2) 0.005(3) 0.006(3) N3B 0.032(3) 0.028(3) 0.030(3) 0.006(2) 0.001(3) 0.005(3) C21B 0.030(4) 0.026(3) 0.034(4) 0.007(3) 0.003(3) 0.010(3) N1B 0.034(3) 0.038(3) 0.035(3) 0.011(3) -0.002(3) 0.006(3) C22B 0.041(5) 0.029(4) 0.036(4) 0.014(3) 0.007(3) 0.012(4) N4B 0.041(4) 0.034(3) 0.030(3) 0.006(3) 0.005(3) 0.001(3) C6B 0.041(5) 0.044(5) 0.029(4) 0.014(3) 0.002(3) 0.021(4) C26B 0.028(4) 0.035(4) 0.042(4) 0.013(3) -0.001(4) 0.009(4) C25B 0.035(5) 0.041(4) 0.047(5) 0.006(4) -0.007(4) 0.015(4) C24B 0.028(4) 0.034(4) 0.050(5) 0.004(4) 0.010(4) 0.002(4) C2B 0.026(4) 0.023(3) 0.043(4) 0.009(3) 0.006(3) 0.007(3) C23B 0.043(5) 0.023(3) 0.049(5) 0.012(3) 0.009(4) 0.003(4) C1B 0.033(4) 0.032(4) 0.036(4) 0.011(3) 0.003(3) 0.008(3) N5B 0.041(4) 0.041(4) 0.038(4) 0.012(3) 0.000(3) 0.012(3) C3B 0.030(4) 0.028(3) 0.030(4) 0.008(3) 0.000(3) 0.006(3) C53B 0.056(5) 0.049(5) 0.037(4) 0.015(4) 0.000(4) 0.017(4) C54B 0.071(7) 0.064(7) 0.071(7) 0.015(6) -0.001(6) 0.030(6) C51B 0.048(5) 0.046(4) 0.038(4) 0.011(4) -0.002(4) 0.013(4) C52B 0.039(5) 0.054(5) 0.061(6) 0.014(5) -0.008(4) 0.000(4) C47B 0.070(7) 0.037(5) 0.046(5) 0.006(4) 0.016(5) -0.012(5) C41B 0.035(4) 0.026(3) 0.032(4) 0.007(3) 0.005(3) 0.012(3) C42B 0.033(4) 0.047(5) 0.035(4) 0.005(4) 0.001(3) 0.017(4) C46B 0.037(4) 0.034(4) 0.037(4) -0.001(3) -0.006(3) 0.016(4) C45B 0.053(6) 0.039(4) 0.029(4) 0.009(3) 0.006(4) 0.020(4) C44B 0.038(5) 0.041(5) 0.044(5) 0.003(4) 0.016(4) 0.006(4) C43B 0.028(4) 0.050(5) 0.042(5) -0.002(4) 0.004(4) 0.011(4) Re2 0.03062(19) 0.02704(16) 0.03141(18) 0.00780(13) 0.00441(14) 0.01052(15) _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 O1A 1.664(6) . ? Re1 N2A 1.982(5) . ? Re1 N6A 2.045(6) . ? Re1 S2A 2.275(2) . ? Re1 S1A 2.310(2) . ? S2A C3A 1.777(7) . ? S1A C1A 1.753(8) . ? S6A C6A 1.607(8) . ? N6A C6A 1.152(10) . ? N3A C3A 1.291(10) . ? N3A N2A 1.415(8) . ? N1A C2A 1.308(9) . ? N1A C1A 1.343(9) . ? N5A C1A 1.313(10) . ? N5A C53A 1.491(10) . ? N5A C51A 1.499(9) . ? N2A C2A 1.380(10) . ? C22A C23A 1.380(11) . ? C22A C21A 1.393(11) . ? C22A H22A 0.9300 . ? N4A C3A 1.368(9) . ? N4A C41A 1.416(11) . ? N4A C47A 1.467(10) . ? C21A C26A 1.402(11) . ? C21A C2A 1.488(11) . ? C26A C25A 1.391(12) . ? C26A H26A 0.9300 . ? C24A C23A 1.374(12) . ? C24A C25A 1.381(12) . ? C24A H24A 0.9300 . ? C23A H23A 0.9300 . ? C41A C46A 1.388(11) . ? C41A C42A 1.391(11) . ? C42A C43A 1.379(13) . ? C42A H42A 0.9300 . ? C43A C44A 1.371(14) . ? C43A H43A 0.9300 . ? C47A H47A 0.9600 . ? C47A H47B 0.9600 . ? C47A H47C 0.9600 . ? C51A C52A 1.488(11) . ? C51A H51A 0.9700 . ? C51A H51B 0.9700 . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C25A H25A 0.9300 . ? C45A C44A 1.378(12) . ? C45A C46A 1.381(12) . ? C45A H45A 0.9300 . ? C46A H46A 0.9300 . ? C44A H44A 0.9300 . ? C53A C54A 1.529(14) . ? C53A H53C 0.9700 . ? C53A H53D 0.9700 . ? C54A H54D 0.9600 . ? C54A H54E 0.9600 . ? C54A H54F 0.9600 . ? S2B C3B 1.785(7) . ? S2B Re2 2.271(2) . ? S1B C1B 1.738(8) . ? S1B Re2 2.313(2) . ? S6B C6B 1.602(9) . ? N6B C6B 1.159(11) . ? N6B Re2 2.040(7) . ? O1B Re2 1.670(6) . ? N2B C2B 1.368(10) . ? N2B N3B 1.416(8) . ? N2B Re2 1.999(6) . ? N3B C3B 1.281(10) . ? C21B C26B 1.377(11) . ? C21B C22B 1.407(11) . ? C21B C2B 1.488(10) . ? N1B C2B 1.325(10) . ? N1B C1B 1.345(10) . ? C22B C23B 1.384(12) . ? C22B H22B 0.9300 . ? N4B C3B 1.355(10) . ? N4B C41B 1.425(11) . ? N4B C47B 1.470(11) . ? C26B C25B 1.385(12) . ? C26B H26B 0.9300 . ? C25B C24B 1.380(13) . ? C25B H25B 0.9300 . ? C24B C23B 1.360(13) . ? C24B H24B 0.9300 . ? C23B H23B 0.9300 . ? C1B N5B 1.329(10) . ? N5B C51B 1.485(11) . ? N5B C53B 1.489(11) . ? C53B C54B 1.453(13) . ? C53B H53A 0.9700 . ? C53B H53B 0.9700 . ? C54B H54A 0.9600 . ? C54B H54B 0.9600 . ? C54B H54C 0.9600 . ? C51B C52B 1.512(13) . ? C51B H51C 0.9700 . ? C51B H51D 0.9700 . ? C52B H52D 0.9600 . ? C52B H52E 0.9600 . ? C52B H52F 0.9600 . ? C47B H47D 0.9600 . ? C47B H47E 0.9600 . ? C47B H47F 0.9600 . ? C41B C46B 1.371(12) . ? C41B C42B 1.395(11) . ? C42B C43B 1.389(13) . ? C42B H42B 0.9300 . ? C46B C45B 1.382(13) . ? C46B H46B 0.9300 . ? C45B C44B 1.368(12) . ? C45B H45B 0.9300 . ? C44B C43B 1.366(13) . ? C44B H44B 0.9300 . ? C43B H43B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Re1 N2A 104.6(3) . . ? O1A Re1 N6A 104.6(3) . . ? N2A Re1 N6A 150.5(3) . . ? O1A Re1 S2A 113.7(2) . . ? N2A Re1 S2A 80.04(19) . . ? N6A Re1 S2A 84.8(2) . . ? O1A Re1 S1A 112.4(2) . . ? N2A Re1 S1A 90.95(19) . . ? N6A Re1 S1A 81.5(2) . . ? S2A Re1 S1A 133.79(8) . . ? C3A S2A Re1 98.8(3) . . ? C1A S1A Re1 107.0(3) . . ? C6A N6A Re1 179.5(7) . . ? C3A N3A N2A 111.7(6) . . ? C2A N1A C1A 126.4(7) . . ? C1A N5A C53A 119.8(6) . . ? C1A N5A C51A 122.7(6) . . ? C53A N5A C51A 117.5(6) . . ? C2A N2A N3A 112.0(5) . . ? C2A N2A Re1 120.5(4) . . ? N3A N2A Re1 125.1(5) . . ? C23A C22A C21A 120.4(8) . . ? C23A C22A H22A 119.8 . . ? C21A C22A H22A 119.8 . . ? C3A N4A C41A 120.3(6) . . ? C3A N4A C47A 117.2(7) . . ? C41A N4A C47A 118.5(6) . . ? C22A C21A C26A 119.1(7) . . ? C22A C21A C2A 120.2(7) . . ? C26A C21A C2A 120.6(7) . . ? N6A C6A S6A 176.2(8) . . ? C25A C26A C21A 119.8(8) . . ? C25A C26A H26A 120.1 . . ? C21A C26A H26A 120.1 . . ? N1A C2A N2A 124.7(7) . . ? N1A C2A C21A 114.3(7) . . ? N2A C2A C21A 121.0(6) . . ? C23A C24A C25A 120.3(9) . . ? C23A C24A H24A 119.8 . . ? C25A C24A H24A 119.8 . . ? C24A C23A C22A 120.4(8) . . ? C24A C23A H23A 119.8 . . ? C22A C23A H23A 119.8 . . ? N5A C1A N1A 118.3(7) . . ? N5A C1A S1A 118.1(6) . . ? N1A C1A S1A 123.6(6) . . ? N3A C3A N4A 120.7(6) . . ? N3A C3A S2A 121.3(5) . . ? N4A C3A S2A 117.8(6) . . ? C46A C41A C42A 119.8(8) . . ? C46A C41A N4A 119.2(7) . . ? C42A C41A N4A 121.0(8) . . ? C43A C42A C41A 119.8(8) . . ? C43A C42A H42A 120.1 . . ? C41A C42A H42A 120.1 . . ? C44A C43A C42A 120.3(9) . . ? C44A C43A H43A 119.8 . . ? C42A C43A H43A 119.8 . . ? N4A C47A H47A 109.5 . . ? N4A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? N4A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C52A C51A N5A 111.3(7) . . ? C52A C51A H51A 109.4 . . ? N5A C51A H51A 109.4 . . ? C52A C51A H51B 109.4 . . ? N5A C51A H51B 109.4 . . ? H51A C51A H51B 108.0 . . ? C51A C52A H52A 109.5 . . ? C51A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C24A C25A C26A 120.1(8) . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C44A C45A C46A 120.4(8) . . ? C44A C45A H45A 119.8 . . ? C46A C45A H45A 119.8 . . ? C45A C46A C41A 119.6(8) . . ? C45A C46A H46A 120.2 . . ? C41A C46A H46A 120.2 . . ? C43A C44A C45A 120.1(8) . . ? C43A C44A H44A 119.9 . . ? C45A C44A H44A 119.9 . . ? N5A C53A C54A 112.4(7) . . ? N5A C53A H53C 109.1 . . ? C54A C53A H53C 109.1 . . ? N5A C53A H53D 109.1 . . ? C54A C53A H53D 109.1 . . ? H53C C53A H53D 107.8 . . ? C53A C54A H54D 109.5 . . ? C53A C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C53A C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C3B S2B Re2 98.9(3) . . ? C1B S1B Re2 107.7(3) . . ? C6B N6B Re2 177.0(7) . . ? C2B N2B N3B 113.0(6) . . ? C2B N2B Re2 121.3(4) . . ? N3B N2B Re2 123.6(5) . . ? C3B N3B N2B 113.6(6) . . ? C26B C21B C22B 120.4(8) . . ? C26B C21B C2B 121.3(7) . . ? C22B C21B C2B 118.2(7) . . ? C2B N1B C1B 126.0(8) . . ? C23B C22B C21B 118.4(8) . . ? C23B C22B H22B 120.8 . . ? C21B C22B H22B 120.8 . . ? C3B N4B C41B 122.9(7) . . ? C3B N4B C47B 117.2(8) . . ? C41B N4B C47B 117.8(6) . . ? N6B C6B S6B 178.9(8) . . ? C21B C26B C25B 119.6(8) . . ? C21B C26B H26B 120.2 . . ? C25B C26B H26B 120.2 . . ? C24B C25B C26B 119.9(8) . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C23B C24B C25B 120.5(8) . . ? C23B C24B H24B 119.8 . . ? C25B C24B H24B 119.8 . . ? N1B C2B N2B 126.0(7) . . ? N1B C2B C21B 114.3(7) . . ? N2B C2B C21B 119.8(7) . . ? C24B C23B C22B 121.0(8) . . ? C24B C23B H23B 119.5 . . ? C22B C23B H23B 119.5 . . ? N5B C1B N1B 114.7(7) . . ? N5B C1B S1B 119.2(6) . . ? N1B C1B S1B 125.6(6) . . ? C1B N5B C51B 120.6(7) . . ? C1B N5B C53B 121.3(7) . . ? C51B N5B C53B 117.9(7) . . ? N3B C3B N4B 122.0(7) . . ? N3B C3B S2B 120.7(5) . . ? N4B C3B S2B 117.2(6) . . ? C54B C53B N5B 112.3(8) . . ? C54B C53B H53A 109.1 . . ? N5B C53B H53A 109.1 . . ? C54B C53B H53B 109.1 . . ? N5B C53B H53B 109.1 . . ? H53A C53B H53B 107.9 . . ? C53B C54B H54A 109.5 . . ? C53B C54B H54B 109.5 . . ? H54A C54B H54B 109.5 . . ? C53B C54B H54C 109.5 . . ? H54A C54B H54C 109.5 . . ? H54B C54B H54C 109.5 . . ? N5B C51B C52B 110.7(7) . . ? N5B C51B H51C 109.5 . . ? C52B C51B H51C 109.5 . . ? N5B C51B H51D 109.5 . . ? C52B C51B H51D 109.5 . . ? H51C C51B H51D 108.1 . . ? C51B C52B H52D 109.5 . . ? C51B C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51B C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? N4B C47B H47D 109.5 . . ? N4B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? N4B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C46B C41B C42B 120.3(8) . . ? C46B C41B N4B 120.2(8) . . ? C42B C41B N4B 119.5(8) . . ? C43B C42B C41B 118.8(8) . . ? C43B C42B H42B 120.6 . . ? C41B C42B H42B 120.6 . . ? C41B C46B C45B 119.1(8) . . ? C41B C46B H46B 120.4 . . ? C45B C46B H46B 120.4 . . ? C44B C45B C46B 121.7(8) . . ? C44B C45B H45B 119.2 . . ? C46B C45B H45B 119.2 . . ? C43B C44B C45B 119.0(9) . . ? C43B C44B H44B 120.5 . . ? C45B C44B H44B 120.5 . . ? C44B C43B C42B 121.0(9) . . ? C44B C43B H43B 119.5 . . ? C42B C43B H43B 119.5 . . ? O1B Re2 N2B 104.0(3) . . ? O1B Re2 N6B 104.4(3) . . ? N2B Re2 N6B 151.5(3) . . ? O1B Re2 S2B 113.3(2) . . ? N2B Re2 S2B 80.65(19) . . ? N6B Re2 S2B 86.0(2) . . ? O1B Re2 S1B 112.6(2) . . ? N2B Re2 S1B 90.41(19) . . ? N6B Re2 S1B 80.9(2) . . ? S2B Re2 S1B 134.02(8) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.748 _refine_diff_density_min -1.941 _refine_diff_density_rms 0.242 data_pireol42eq _database_code_depnum_ccdc_archive 'CCDC 911728' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(N-(N'',N''-diethylaminothiocarbonyl)-N'(N''', N'''-hexamethylenecarbo thioamide)benzamidineto)(isothiocyanate)oxorhenium(V)' ; _chemical_name_common '[ReO(Aztsc)(SCN)]' _chemical_melting_point ? _chemical_formula_moiety 'C20 H27 N6 O Re S3' _chemical_formula_sum 'C20 H27 N6 O Re S3' _chemical_formula_weight 649.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.336(5) _cell_length_b 11.117(5) _cell_length_c 11.842(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 102.937(5) _cell_angle_gamma 90.000(5) _cell_volume 1197.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5968 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 29.53 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.167 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.088 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 5.358 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5070 _exptl_absorpt_correction_T_max 0.7524 _exptl_absorpt_process_details X-Area _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8209 _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.22 _reflns_number_total 5437 _reflns_number_gt 3695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1181P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 5437 _refine_ls_number_parameters 283 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1972 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 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 Re Re 0.16712(6) 0.86295(7) 0.26622(5) 0.0320(2) Uani 1 1 d . . . S1 S -0.0749(5) 0.8137(4) 0.2514(4) 0.0369(9) Uani 1 1 d . . . S2 S 0.3128(5) 0.9541(4) 0.1609(4) 0.0367(10) Uani 1 1 d . . . S6 S 0.1258(7) 0.5508(6) -0.0187(5) 0.0540(14) Uani 1 1 d . . . O1 O 0.2683(16) 0.8013(13) 0.3841(13) 0.047(3) Uani 1 1 d . . . N1 N -0.0968(16) 1.0253(13) 0.3586(12) 0.032(3) Uani 1 1 d . . . N2 N 0.1292(13) 1.0392(11) 0.3018(10) 0.021(2) Uani 1 1 d . . . N3 N 0.2375(17) 1.1240(13) 0.2951(12) 0.032(3) Uani 1 1 d . . . N4 N 0.4467(18) 1.1620(16) 0.2294(13) 0.040(4) Uani 1 1 d . . . N5 N -0.2022(14) 0.869(2) 0.4255(10) 0.030(3) Uani 1 1 d . . . N6 N 0.149(2) 0.7297(15) 0.1425(15) 0.045(4) Uani 1 1 d . . . C1 C -0.126(2) 0.9116(19) 0.3562(15) 0.039(4) Uani 1 1 d . . . C2 C 0.0070(18) 1.0868(17) 0.3224(12) 0.029(3) Uani 1 1 d . . . C3 C 0.334(2) 1.0959(16) 0.2348(15) 0.033(3) Uani 1 1 d . . . C6 C 0.134(3) 0.652(2) 0.0786(18) 0.049(5) Uani 1 1 d . . . C21 C -0.0246(19) 1.2222(19) 0.3090(14) 0.034(4) Uani 1 1 d . . . C22 C -0.094(2) 1.2722(18) 0.3882(16) 0.036(4) Uani 1 1 d . . . H22 H -0.1113 1.2287 0.4508 0.043 Uiso 1 1 calc R . . C23 C -0.139(2) 1.400(3) 0.3682(19) 0.064(10) Uani 1 1 d . . . H23 H -0.1818 1.4405 0.4211 0.076 Uiso 1 1 calc R . . C24 C -0.119(3) 1.4546(16) 0.2738(19) 0.043(5) Uani 1 1 d . . . H24 H -0.1523 1.5332 0.2610 0.051 Uiso 1 1 calc R . . C25 C -0.053(3) 1.4054(18) 0.1956(16) 0.039(5) Uani 1 1 d . . . H25 H -0.0393 1.4487 0.1317 0.047 Uiso 1 1 calc R . . C26 C -0.004(2) 1.2804(15) 0.2147(16) 0.030(4) Uani 1 1 d . . . H26 H 0.0418 1.2420 0.1623 0.036 Uiso 1 1 calc R . . C41 C 0.477(3) 1.262(2) 0.2963(18) 0.054(6) Uani 1 1 d . . . H41A H 0.5824 1.2668 0.3259 0.065 Uiso 1 1 calc R . . H41B H 0.4319 1.2534 0.3622 0.065 Uiso 1 1 calc R . . C42 C 0.422(3) 1.382(6) 0.2316(19) 0.105(18) Uani 1 1 d . . . H42A H 0.3156 1.3837 0.2188 0.125 Uiso 1 1 calc R . . H42B H 0.4594 1.4480 0.2832 0.125 Uiso 1 1 calc R . . C43 C 0.462(3) 1.407(2) 0.115(2) 0.062(6) Uani 1 1 d . . . H43A H 0.5681 1.4144 0.1266 0.074 Uiso 1 1 calc R . . H43B H 0.4185 1.4824 0.0835 0.074 Uiso 1 1 calc R . . C44 C 0.406(3) 1.301(2) 0.024(2) 0.057(6) Uani 1 1 d . . . H44A H 0.3076 1.2803 0.0313 0.068 Uiso 1 1 calc R . . H44B H 0.3967 1.3351 -0.0528 0.068 Uiso 1 1 calc R . . C45 C 0.485(3) 1.194(3) 0.0278(19) 0.059(6) Uani 1 1 d . . . H45A H 0.5674 1.2085 -0.0078 0.071 Uiso 1 1 calc R . . H45B H 0.4220 1.1353 -0.0195 0.071 Uiso 1 1 calc R . . C46 C 0.544(2) 1.139(2) 0.1466(17) 0.042(4) Uani 1 1 d . . . H46A H 0.5545 1.0530 0.1381 0.051 Uiso 1 1 calc R . . H46B H 0.6407 1.1720 0.1789 0.051 Uiso 1 1 calc R . . C51 C -0.241(2) 0.9467(15) 0.5193(18) 0.040(4) Uani 1 1 d . . . H51A H -0.2336 0.9004 0.5898 0.048 Uiso 1 1 calc R . . H51B H -0.1750 1.0149 0.5360 0.048 Uiso 1 1 calc R . . C52 C -0.388(3) 0.986(3) 0.477(2) 0.074(9) Uani 1 1 d . . . H52A H -0.4487 0.9566 0.5261 0.111 Uiso 1 1 calc R . . H52B H -0.4236 0.9569 0.3995 0.111 Uiso 1 1 calc R . . H52C H -0.3902 1.0728 0.4763 0.111 Uiso 1 1 calc R . . C53 C -0.250(2) 0.7412(16) 0.4227(16) 0.039(4) Uani 1 1 d . . . H53A H -0.2699 0.7205 0.4974 0.047 Uiso 1 1 calc R . . H53B H -0.1709 0.6903 0.4104 0.047 Uiso 1 1 calc R . . C54 C -0.387(2) 0.715(2) 0.329(2) 0.057(6) Uani 1 1 d . . . H54A H -0.3719 0.7428 0.2556 0.085 Uiso 1 1 calc R . . H54B H -0.4695 0.7562 0.3468 0.085 Uiso 1 1 calc R . . H54C H -0.4051 0.6302 0.3252 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0305(3) 0.0268(3) 0.0419(3) 0.0009(6) 0.01461(19) 0.0011(6) S1 0.035(2) 0.033(2) 0.046(2) -0.0038(17) 0.0165(18) -0.0058(18) S2 0.038(2) 0.032(2) 0.045(2) -0.0026(17) 0.0206(19) -0.0002(19) S6 0.066(4) 0.050(3) 0.049(3) -0.006(2) 0.017(2) -0.001(3) O1 0.041(8) 0.030(7) 0.077(9) 0.020(6) 0.028(7) 0.001(6) N1 0.027(7) 0.023(7) 0.050(7) 0.002(6) 0.016(6) 0.004(6) N2 0.014(5) 0.016(6) 0.035(6) -0.004(5) 0.012(5) -0.003(5) N3 0.032(8) 0.025(7) 0.041(7) -0.004(6) 0.015(6) -0.003(6) N4 0.039(9) 0.041(9) 0.047(8) 0.001(7) 0.023(7) -0.010(7) N5 0.032(6) 0.018(7) 0.046(5) 0.001(9) 0.018(5) 0.003(10) N6 0.050(10) 0.026(8) 0.064(10) -0.018(7) 0.020(8) -0.009(8) C1 0.026(8) 0.047(11) 0.046(9) 0.010(8) 0.013(7) 0.013(8) C2 0.024(8) 0.039(9) 0.024(6) 0.000(6) 0.007(6) -0.001(7) C3 0.032(8) 0.024(8) 0.044(8) 0.003(7) 0.009(6) -0.003(8) C6 0.044(11) 0.046(13) 0.058(11) 0.014(10) 0.017(9) 0.005(10) C21 0.021(8) 0.044(11) 0.036(8) -0.005(7) 0.002(6) -0.002(8) C22 0.027(9) 0.032(10) 0.042(9) 0.000(8) -0.005(7) -0.006(8) C23 0.032(10) 0.11(3) 0.049(10) -0.035(13) 0.014(8) 0.006(12) C24 0.052(13) 0.007(7) 0.071(12) 0.008(7) 0.016(10) 0.007(8) C25 0.054(13) 0.023(9) 0.039(9) 0.008(7) 0.008(8) -0.012(9) C26 0.034(10) 0.007(7) 0.050(9) 0.006(7) 0.012(8) 0.005(7) C41 0.051(13) 0.074(17) 0.043(10) 0.002(10) 0.021(9) 0.012(12) C42 0.057(14) 0.21(5) 0.053(11) 0.04(3) 0.023(10) 0.07(3) C43 0.063(15) 0.056(14) 0.075(14) 0.000(11) 0.032(12) -0.023(12) C44 0.062(15) 0.050(14) 0.057(12) 0.010(10) 0.012(11) -0.002(12) C45 0.053(13) 0.076(17) 0.059(12) 0.000(11) 0.038(11) 0.004(12) C46 0.033(9) 0.046(11) 0.059(10) 0.000(9) 0.032(8) 0.000(9) C51 0.047(11) 0.008(7) 0.070(12) -0.001(7) 0.023(9) -0.001(7) C52 0.072(18) 0.10(2) 0.052(12) 0.003(13) 0.007(12) 0.038(17) C53 0.053(12) 0.016(8) 0.050(10) -0.002(7) 0.019(9) -0.001(8) C54 0.037(11) 0.034(11) 0.107(18) -0.002(11) 0.033(11) -0.003(9) _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 Re O1 1.650(15) . ? Re N2 2.051(12) . ? Re N6 2.064(15) . ? Re S2 2.278(4) . ? Re S1 2.294(5) . ? S1 C1 1.795(19) . ? S2 C3 1.792(19) . ? S6 C6 1.60(2) . ? N1 C1 1.29(3) . ? N1 C2 1.33(2) . ? N2 C2 1.33(2) . ? N2 N3 1.398(19) . ? N3 C3 1.30(2) . ? N4 C3 1.30(2) . ? N4 C41 1.35(3) . ? N4 C46 1.50(2) . ? N5 C1 1.29(2) . ? N5 C53 1.49(3) . ? N5 C51 1.51(3) . ? N6 C6 1.13(3) . ? C2 C21 1.54(3) . ? C21 C26 1.34(3) . ? C21 C22 1.37(3) . ? C22 C23 1.48(4) . ? C22 H22 0.9300 . ? C23 C24 1.33(3) . ? C23 H23 0.9300 . ? C24 C25 1.34(3) . ? C24 H24 0.9300 . ? C25 C26 1.47(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C42 1.57(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.54(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.60(3) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.40(4) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.52(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C51 C52 1.42(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.52(3) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re N2 108.4(7) . . ? O1 Re N6 104.0(8) . . ? N2 Re N6 147.3(7) . . ? O1 Re S2 110.4(5) . . ? N2 Re S2 80.8(3) . . ? N6 Re S2 83.9(5) . . ? O1 Re S1 109.5(5) . . ? N2 Re S1 91.8(3) . . ? N6 Re S1 81.5(5) . . ? S2 Re S1 139.73(18) . . ? C1 S1 Re 102.3(7) . . ? C3 S2 Re 97.9(6) . . ? C1 N1 C2 131.4(15) . . ? C2 N2 N3 113.8(13) . . ? C2 N2 Re 127.8(11) . . ? N3 N2 Re 118.2(9) . . ? C3 N3 N2 117.7(14) . . ? C3 N4 C41 119.9(17) . . ? C3 N4 C46 123.6(17) . . ? C41 N4 C46 116.4(17) . . ? C1 N5 C53 122.8(19) . . ? C1 N5 C51 121(2) . . ? C53 N5 C51 116.0(13) . . ? C6 N6 Re 175.4(17) . . ? N5 C1 N1 119(2) . . ? N5 C1 S1 119.3(19) . . ? N1 C1 S1 121.3(13) . . ? N2 C2 N1 124.8(16) . . ? N2 C2 C21 121.6(14) . . ? N1 C2 C21 113.5(15) . . ? N4 C3 N3 123.9(17) . . ? N4 C3 S2 118.3(14) . . ? N3 C3 S2 117.7(13) . . ? N6 C6 S6 173(2) . . ? C26 C21 C22 124(2) . . ? C26 C21 C2 119.9(15) . . ? C22 C21 C2 115.9(16) . . ? C21 C22 C23 116.2(19) . . ? C21 C22 H22 121.9 . . ? C23 C22 H22 121.9 . . ? C24 C23 C22 118.9(19) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 124.9(19) . . ? C23 C24 H24 117.5 . . ? C25 C24 H24 117.5 . . ? C24 C25 C26 117.3(17) . . ? C24 C25 H25 121.4 . . ? C26 C25 H25 121.4 . . ? C21 C26 C25 119.0(18) . . ? C21 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N4 C41 C42 114(2) . . ? N4 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? N4 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C43 C42 C41 118(3) . . ? C43 C42 H42A 107.7 . . ? C41 C42 H42A 107.7 . . ? C43 C42 H42B 107.7 . . ? C41 C42 H42B 107.7 . . ? H42A C42 H42B 107.1 . . ? C42 C43 C44 111(3) . . ? C42 C43 H43A 109.4 . . ? C44 C43 H43A 109.4 . . ? C42 C43 H43B 109.4 . . ? C44 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 121(2) . . ? C45 C44 H44A 107.1 . . ? C43 C44 H44A 107.1 . . ? C45 C44 H44B 107.1 . . ? C43 C44 H44B 107.1 . . ? H44A C44 H44B 106.8 . . ? C44 C45 C46 116.9(19) . . ? C44 C45 H45A 108.1 . . ? C46 C45 H45A 108.1 . . ? C44 C45 H45B 108.1 . . ? C46 C45 H45B 108.1 . . ? H45A C45 H45B 107.3 . . ? N4 C46 C45 113.0(17) . . ? N4 C46 H46A 109.0 . . ? C45 C46 H46A 109.0 . . ? N4 C46 H46B 109.0 . . ? C45 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C52 C51 N5 106.8(18) . . ? C52 C51 H51A 110.4 . . ? N5 C51 H51A 110.4 . . ? C52 C51 H51B 110.4 . . ? N5 C51 H51B 110.4 . . ? H51A C51 H51B 108.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 C54 113.4(16) . . ? N5 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? N5 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.906 _refine_diff_density_min -1.798 _refine_diff_density_rms 0.375 data_pireolicn _database_code_depnum_ccdc_archive 'CCDC 911729' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(N-(N'',N''-diethylaminothiocarbonyl)-N'(N''', N'''-methylphenylcarbothioamide) benzamidineto)(cyanate)oxorhenium(V)' ; _chemical_name_common '[ReO(mptsc)(CN)]' _chemical_melting_point ? _chemical_formula_moiety 'C21 H23 N6 O Re S2' _chemical_formula_sum 'C21 H23 N6 O Re S2' _chemical_formula_weight 625.77 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9759(6) _cell_length_b 10.7569(7) _cell_length_c 21.8824(14) _cell_angle_alpha 90.00 _cell_angle_beta 91.5310(10) _cell_angle_gamma 90.00 _cell_volume 2347.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 16253 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 29.63 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.193 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.118 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 5.380 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1709 _exptl_absorpt_correction_T_max 0.5387 _exptl_absorpt_process_details X-Area _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14594 _diffrn_reflns_av_R_equivalents 0.1038 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.28 _reflns_number_total 6276 _reflns_number_gt 5158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0147(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6276 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1675 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3502(7) -0.0118(6) 0.7907(3) 0.0341(12) Uani 1 1 d . . . C2 C 0.3974(6) 0.1171(5) 0.8770(3) 0.0302(11) Uani 1 1 d . . . C3 C 0.2009(7) 0.3774(6) 0.8991(3) 0.0331(12) Uani 1 1 d . . . C4 C -0.0745(8) 0.1013(7) 0.8147(3) 0.0426(15) Uani 1 1 d . . . C21 C 0.4962(6) 0.1347(6) 0.9277(3) 0.0301(11) Uani 1 1 d . . . C22 C 0.4535(7) 0.1633(6) 0.9871(3) 0.0343(12) Uani 1 1 d . . . H22 H 0.3635 0.1796 0.9939 0.041 Uiso 1 1 calc R . . C23 C 0.5462(8) 0.1670(7) 1.0349(3) 0.0405(14) Uani 1 1 d . . . H23 H 0.5181 0.1844 1.0742 0.049 Uiso 1 1 calc R . . C24 C 0.6798(8) 0.1450(7) 1.0252(3) 0.0429(15) Uani 1 1 d . . . H24 H 0.7412 0.1481 1.0579 0.052 Uiso 1 1 calc R . . C25 C 0.7233(8) 0.1186(7) 0.9678(4) 0.0452(17) Uani 1 1 d . . . H25 H 0.8141 0.1060 0.9614 0.054 Uiso 1 1 calc R . . C26 C 0.6318(7) 0.1108(6) 0.9195(3) 0.0370(13) Uani 1 1 d . . . H26 H 0.6611 0.0893 0.8809 0.044 Uiso 1 1 calc R . . C41 C 0.1096(8) 0.5833(7) 0.9163(3) 0.0383(13) Uani 1 1 d . . . C42 C 0.0776(10) 0.6223(8) 0.8561(3) 0.0455(18) Uani 1 1 d . . . H42 H 0.1204 0.5858 0.8233 0.055 Uiso 1 1 calc R . . C43 C -0.0162(10) 0.7137(8) 0.8454(4) 0.0553(19) Uani 1 1 d . . . H43 H -0.0372 0.7376 0.8055 0.066 Uiso 1 1 calc R . . C44 C -0.0798(9) 0.7704(8) 0.8930(4) 0.0552(19) Uani 1 1 d . . . H44 H -0.1421 0.8332 0.8853 0.066 Uiso 1 1 calc R . . C45 C -0.0501(8) 0.7333(8) 0.9522(4) 0.0505(17) Uani 1 1 d . . . H45 H -0.0922 0.7711 0.9848 0.061 Uiso 1 1 calc R . . C46 C 0.0424(8) 0.6397(7) 0.9629(3) 0.0433(15) Uani 1 1 d . . . H46 H 0.0598 0.6139 1.0029 0.052 Uiso 1 1 calc R . . C47 C 0.3255(10) 0.5216(9) 0.9628(4) 0.059(2) Uani 1 1 d . . . H47A H 0.3613 0.4478 0.9818 0.089 Uiso 1 1 calc R . . H47B H 0.3046 0.5813 0.9937 0.089 Uiso 1 1 calc R . . H47C H 0.3907 0.5560 0.9361 0.089 Uiso 1 1 calc R . . C51 C 0.3411(9) -0.1226(9) 0.6921(4) 0.057(2) Uani 1 1 d . . . H51A H 0.2575 -0.1570 0.7062 0.069 Uiso 1 1 calc R . . H51B H 0.3954 -0.1909 0.6778 0.069 Uiso 1 1 calc R . . C52 C 0.3113(11) -0.0348(14) 0.6396(4) 0.078(4) Uani 1 1 d . . . H52A H 0.2432 0.0232 0.6510 0.118 Uiso 1 1 calc R . . H52B H 0.2803 -0.0815 0.6046 0.118 Uiso 1 1 calc R . . H52C H 0.3913 0.0096 0.6298 0.118 Uiso 1 1 calc R . . C53 C 0.5581(8) -0.0622(10) 0.7411(3) 0.053(2) Uani 1 1 d . . . H53A H 0.5934 0.0119 0.7610 0.064 Uiso 1 1 calc R . . H53B H 0.5839 -0.0600 0.6987 0.064 Uiso 1 1 calc R . . C54 C 0.6194(12) -0.1758(13) 0.7716(6) 0.083(4) Uani 1 1 d . . . H54A H 0.6246 -0.1632 0.8150 0.124 Uiso 1 1 calc R . . H54B H 0.7078 -0.1890 0.7566 0.124 Uiso 1 1 calc R . . H54C H 0.5646 -0.2471 0.7625 0.124 Uiso 1 1 calc R . . N1 N 0.4265(5) 0.0295(5) 0.8376(2) 0.0320(10) Uani 1 1 d . . . N2 N 0.2873(5) 0.1903(5) 0.8735(2) 0.0286(9) Uani 1 1 d . . . N3 N 0.3089(5) 0.3101(5) 0.8982(2) 0.0315(10) Uani 1 1 d . . . N4 N 0.2042(6) 0.4905(6) 0.9276(3) 0.0393(12) Uani 1 1 d . . . N5 N 0.4119(6) -0.0612(6) 0.7436(2) 0.0385(12) Uani 1 1 d . . . N6 N -0.1755(7) 0.0936(8) 0.7884(3) 0.0579(19) Uani 1 1 d . . . O O 0.0710(5) 0.0363(5) 0.9292(2) 0.0429(11) Uani 1 1 d . . . Re1 Re 0.10201(2) 0.11504(2) 0.864508(10) 0.03158(14) Uani 1 1 d . . . S1 S 0.17463(17) -0.01308(18) 0.78831(7) 0.0409(4) Uani 1 1 d . . . S2 S 0.04635(16) 0.32079(16) 0.86943(7) 0.0370(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(3) 0.034(3) 0.032(2) -0.005(2) 0.008(2) -0.001(2) C2 0.030(3) 0.034(3) 0.026(2) -0.0020(18) 0.005(2) -0.002(2) C3 0.036(3) 0.035(3) 0.028(3) -0.0003(19) 0.005(2) 0.003(2) C4 0.037(3) 0.054(4) 0.037(3) -0.007(3) 0.007(3) -0.001(3) C21 0.029(3) 0.031(3) 0.030(2) 0.000(2) -0.002(2) -0.002(2) C22 0.036(3) 0.035(3) 0.032(3) -0.001(2) 0.005(2) -0.003(2) C23 0.056(4) 0.034(3) 0.031(3) 0.001(2) -0.006(3) -0.002(3) C24 0.045(4) 0.040(3) 0.043(3) 0.005(3) -0.012(3) -0.006(3) C25 0.034(3) 0.050(4) 0.051(4) 0.001(3) 0.000(3) -0.004(3) C26 0.033(3) 0.041(4) 0.037(3) 0.003(2) 0.005(2) 0.001(2) C41 0.046(4) 0.033(3) 0.036(3) 0.000(2) 0.003(3) -0.002(3) C42 0.057(4) 0.048(5) 0.031(3) 0.003(2) 0.003(3) 0.009(3) C43 0.067(5) 0.050(5) 0.049(4) 0.006(3) -0.002(4) 0.006(4) C44 0.056(5) 0.037(4) 0.072(5) 0.002(3) -0.004(4) 0.008(3) C45 0.050(4) 0.047(4) 0.054(4) -0.017(3) 0.004(3) 0.005(3) C46 0.045(4) 0.047(4) 0.038(3) -0.004(3) 0.001(3) 0.006(3) C47 0.060(5) 0.053(5) 0.063(5) -0.020(4) -0.021(4) 0.012(4) C51 0.047(4) 0.079(6) 0.046(4) -0.035(4) -0.001(3) -0.004(4) C52 0.051(5) 0.138(12) 0.046(4) -0.003(5) -0.002(4) -0.006(6) C53 0.036(4) 0.077(6) 0.047(4) -0.023(4) 0.012(3) 0.008(4) C54 0.069(7) 0.090(9) 0.088(7) -0.029(6) -0.013(6) 0.035(6) N1 0.032(2) 0.033(3) 0.031(2) -0.0060(18) 0.0038(18) -0.004(2) N2 0.025(2) 0.027(2) 0.033(2) -0.0047(17) 0.0000(17) -0.0025(17) N3 0.036(3) 0.025(2) 0.033(2) -0.0012(17) -0.0007(19) 0.0022(19) N4 0.044(3) 0.033(3) 0.041(3) -0.004(2) -0.003(2) 0.003(2) N5 0.037(3) 0.042(3) 0.037(2) -0.015(2) 0.003(2) 0.003(2) N6 0.034(3) 0.092(6) 0.048(3) -0.015(3) 0.000(3) -0.012(3) O 0.042(3) 0.041(3) 0.046(2) 0.001(2) 0.010(2) 0.005(2) Re1 0.02957(18) 0.03505(19) 0.03034(17) -0.00408(8) 0.00475(10) -0.00259(8) S1 0.0320(7) 0.0497(10) 0.0412(7) -0.0178(7) 0.0058(6) -0.0069(7) S2 0.0326(7) 0.0383(8) 0.0399(7) -0.0052(6) -0.0008(6) 0.0033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N5 1.325(7) . ? C1 N1 1.337(8) . ? C1 S1 1.751(7) . ? C2 N1 1.314(7) . ? C2 N2 1.352(8) . ? C2 C21 1.477(8) . ? C3 N3 1.298(8) . ? C3 N4 1.367(8) . ? C3 S2 1.765(7) . ? C4 N6 1.151(11) . ? C4 Re1 2.051(8) . ? C21 C26 1.393(9) . ? C21 C22 1.412(8) . ? C22 C23 1.379(9) . ? C22 H22 0.9300 . ? C23 C24 1.377(11) . ? C23 H23 0.9300 . ? C24 C25 1.369(11) . ? C24 H24 0.9300 . ? C25 C26 1.381(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C46 1.377(10) . ? C41 N4 1.392(9) . ? C41 C42 1.412(9) . ? C42 C43 1.373(12) . ? C42 H42 0.9300 . ? C43 C44 1.376(12) . ? C43 H43 0.9300 . ? C44 C45 1.381(12) . ? C44 H44 0.9300 . ? C45 C46 1.381(11) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 N4 1.456(10) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C51 N5 1.470(9) . ? C51 C52 1.511(16) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 N5 1.461(9) . ? C53 C54 1.513(16) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? N2 N3 1.411(7) . ? N2 Re1 2.023(5) . ? O Re1 1.686(5) . ? Re1 S2 2.2851(17) . ? Re1 S1 2.2954(16) . ? 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 N5 C1 N1 117.6(6) . . ? N5 C1 S1 117.3(5) . . ? N1 C1 S1 125.0(5) . . ? N1 C2 N2 125.0(6) . . ? N1 C2 C21 115.5(6) . . ? N2 C2 C21 119.5(5) . . ? N3 C3 N4 119.5(6) . . ? N3 C3 S2 121.3(5) . . ? N4 C3 S2 119.0(5) . . ? N6 C4 Re1 178.0(7) . . ? C26 C21 C22 118.5(6) . . ? C26 C21 C2 120.7(6) . . ? C22 C21 C2 120.5(6) . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 120.7(6) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.7(7) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 119.7(7) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.9(7) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C46 C41 N4 121.7(6) . . ? C46 C41 C42 117.3(7) . . ? N4 C41 C42 121.0(6) . . ? C43 C42 C41 120.4(7) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 121.0(8) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C45 119.3(8) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C44 C45 C46 119.7(7) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 122.1(7) . . ? C41 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N5 C51 C52 112.6(8) . . ? N5 C51 H51A 109.1 . . ? C52 C51 H51A 109.1 . . ? N5 C51 H51B 109.1 . . ? C52 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 C54 112.4(9) . . ? N5 C53 H53A 109.1 . . ? C54 C53 H53A 109.1 . . ? N5 C53 H53B 109.1 . . ? C54 C53 H53B 109.1 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C2 N1 C1 127.6(6) . . ? C2 N2 N3 113.3(5) . . ? C2 N2 Re1 120.7(4) . . ? N3 N2 Re1 122.2(4) . . ? C3 N3 N2 113.3(5) . . ? C3 N4 C41 123.3(6) . . ? C3 N4 C47 117.1(6) . . ? C41 N4 C47 118.6(6) . . ? C1 N5 C53 121.1(6) . . ? C1 N5 C51 123.5(6) . . ? C53 N5 C51 115.3(6) . . ? O Re1 N2 107.9(2) . . ? O Re1 C4 103.6(3) . . ? N2 Re1 C4 148.2(3) . . ? O Re1 S2 113.38(18) . . ? N2 Re1 S2 80.22(15) . . ? C4 Re1 S2 83.6(2) . . ? O Re1 S1 112.15(18) . . ? N2 Re1 S1 90.34(14) . . ? C4 Re1 S1 81.6(2) . . ? S2 Re1 S1 134.23(7) . . ? C1 S1 Re1 108.0(2) . . ? C3 S2 Re1 98.1(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 29.28 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 4.599 _refine_diff_density_min -4.041 _refine_diff_density_rms 0.388 data_sml1f _database_code_depnum_ccdc_archive 'CCDC 911730' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '(N-(N'',N''-diethylaminothiocarbonyl)-N'(N''', N'''-hexamethylene- carbothioamide)benzamidineto)(diisothiocyanate)oxorhenium(V)' ; _chemical_name_common '[ReO(HAztsc)(SCN)2]' _chemical_melting_point ? _chemical_formula_moiety 'C21 H28 N7 O Re S4' _chemical_formula_sum 'C21 H28 N7 O Re S4' _chemical_formula_weight 708.94 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 14.2273(15) _cell_length_b 12.9103(9) _cell_length_c 14.6062(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.9810(10) _cell_angle_gamma 90.00 _cell_volume 2676.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5317 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.57 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.177 _exptl_crystal_size_mid 0.145 _exptl_crystal_size_min 0.107 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.881 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6603 _exptl_absorpt_correction_T_max 0.8647 _exptl_absorpt_process_details X-AREA _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17994 _diffrn_reflns_av_R_equivalents 0.1507 _diffrn_reflns_av_sigmaI/netI 0.2828 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.22 _reflns_number_total 7171 _reflns_number_gt 2869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7171 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1677 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.792 _refine_ls_restrained_S_all 0.792 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.83436(4) 0.33713(5) 0.04277(4) 0.02469(16) Uani 1 1 d . . . S4 S 0.6679(2) 0.3174(3) 0.0370(3) 0.0320(10) Uani 1 1 d . . . S5 S 0.9900(2) 0.4017(3) 0.0680(3) 0.0339(9) Uani 1 1 d . . . S6 S 0.8126(3) 0.4743(4) -0.2661(3) 0.0403(10) Uani 1 1 d . . . S7 S 0.6915(3) 0.6779(4) 0.0968(3) 0.0508(13) Uani 1 1 d . . . O1 O 0.8636(7) 0.2179(9) 0.0091(9) 0.040(3) Uani 1 1 d . . . N1 N 0.9663(7) 0.3659(9) 0.2463(9) 0.029(3) Uani 1 1 d . . . N2 N 0.8201(7) 0.3131(9) 0.1762(8) 0.025(3) Uani 1 1 d . . . N3 N 0.7332(8) 0.2782(10) 0.2068(9) 0.030(3) Uani 1 1 d . . . H3 H 0.7280 0.2637 0.2637 0.036 Uiso 1 1 calc R . . N4 N 0.5791(7) 0.2245(11) 0.1707(10) 0.033(3) Uani 1 1 d . . . N5 N 1.0945(7) 0.2846(11) 0.1870(9) 0.030(3) Uani 1 1 d . . . N6 N 0.8290(9) 0.3953(11) -0.0916(8) 0.033(3) Uani 1 1 d . . . N7 N 0.7940(8) 0.4995(10) 0.0664(10) 0.032(3) Uani 1 1 d . . . C1 C 1.0185(8) 0.3417(13) 0.1723(10) 0.026(3) Uani 1 1 d . . . C2 C 0.8746(9) 0.3633(11) 0.2494(11) 0.030(3) Uani 1 1 d . . . C3 C 0.6581(10) 0.2682(12) 0.1446(10) 0.030(3) Uani 1 1 d . . . C6 C 0.8202(9) 0.4303(12) -0.1630(13) 0.034(4) Uani 1 1 d . . . C7 C 0.7488(9) 0.5734(13) 0.0781(12) 0.033(4) Uani 1 1 d . . . C24 C 0.7705(11) 0.5352(12) 0.4696(12) 0.036(4) Uani 1 1 d . . . H24 H 0.7480 0.5727 0.5178 0.043 Uiso 1 1 calc R . . C21 C 0.8348(9) 0.4192(11) 0.3232(9) 0.021(3) Uani 1 1 d . . . C22 C 0.8880(11) 0.4256(13) 0.4109(11) 0.034(4) Uani 1 1 d . . . H22 H 0.9445 0.3896 0.4203 0.040 Uiso 1 1 calc R . . C23 C 0.8560(12) 0.4835(14) 0.4792(12) 0.041(4) Uani 1 1 d . . . H23 H 0.8925 0.4888 0.5344 0.049 Uiso 1 1 calc R . . C25 C 0.7188(11) 0.5288(12) 0.3833(12) 0.034(4) Uani 1 1 d . . . H25 H 0.6626 0.5653 0.3746 0.041 Uiso 1 1 calc R . . C26 C 0.7478(9) 0.4721(12) 0.3137(10) 0.027(3) Uani 1 1 d . . . H26 H 0.7105 0.4676 0.2590 0.032 Uiso 1 1 calc R . . C41 C 0.5715(10) 0.1817(12) 0.2620(12) 0.035(4) Uani 1 1 d . . . H41A H 0.6290 0.1442 0.2796 0.043 Uiso 1 1 calc R . . H41B H 0.5202 0.1320 0.2592 0.043 Uiso 1 1 calc R . . C42 C 0.5544(11) 0.2615(16) 0.3379(14) 0.051(5) Uani 1 1 d . . . H42A H 0.5234 0.2269 0.3865 0.061 Uiso 1 1 calc R . . H42B H 0.6149 0.2862 0.3638 0.061 Uiso 1 1 calc R . . C43 C 0.4945(13) 0.3553(16) 0.3052(19) 0.073(8) Uani 1 1 d . . . H43A H 0.5353 0.4046 0.2772 0.088 Uiso 1 1 calc R . . H43B H 0.4710 0.3886 0.3586 0.088 Uiso 1 1 calc R . . C44 C 0.4102(11) 0.3324(19) 0.2364(12) 0.049(4) Uani 1 1 d . . . H44A H 0.3816 0.2676 0.2535 0.059 Uiso 1 1 calc R . . H44B H 0.3635 0.3865 0.2413 0.059 Uiso 1 1 calc R . . C45 C 0.4339(11) 0.3252(19) 0.1403(12) 0.052(5) Uani 1 1 d . . . H45A H 0.4682 0.3876 0.1268 0.062 Uiso 1 1 calc R . . H45B H 0.3750 0.3272 0.1026 0.062 Uiso 1 1 calc R . . C46 C 0.4914(11) 0.2320(16) 0.1069(13) 0.052(5) Uani 1 1 d . . . H46A H 0.4549 0.1687 0.1090 0.062 Uiso 1 1 calc R . . H46B H 0.5078 0.2432 0.0443 0.062 Uiso 1 1 calc R . . C51 C 1.1574(10) 0.2592(16) 0.1210(13) 0.048(5) Uani 1 1 d . . . H51A H 1.2199 0.2516 0.1512 0.058 Uiso 1 1 calc R . . H51B H 1.1595 0.3162 0.0779 0.058 Uiso 1 1 calc R . . C52 C 1.1321(15) 0.159(2) 0.0673(15) 0.073(6) Uani 1 1 d . . . H52A H 1.1247 0.1035 0.1097 0.109 Uiso 1 1 calc R . . H52B H 1.1817 0.1428 0.0284 0.109 Uiso 1 1 calc R . . H52C H 1.0743 0.1693 0.0305 0.109 Uiso 1 1 calc R . . C53 C 1.1143(11) 0.2371(15) 0.2798(14) 0.047(5) Uani 1 1 d . . . H53A H 1.1015 0.2881 0.3261 0.056 Uiso 1 1 calc R . . H53B H 1.1807 0.2199 0.2876 0.056 Uiso 1 1 calc R . . C54 C 1.0574(13) 0.1405(15) 0.2964(16) 0.057(5) Uani 1 1 d . . . H54A H 0.9925 0.1590 0.3012 0.085 Uiso 1 1 calc R . . H54B H 1.0814 0.1080 0.3524 0.085 Uiso 1 1 calc R . . H54C H 1.0622 0.0933 0.2462 0.085 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0265(2) 0.0243(3) 0.0237(3) 0.0005(4) 0.00453(16) -0.0030(3) S4 0.0300(16) 0.041(3) 0.0249(18) 0.0003(17) 0.0018(13) -0.0049(16) S5 0.0275(17) 0.037(2) 0.037(2) 0.0070(19) 0.0053(15) -0.0057(16) S6 0.045(2) 0.048(3) 0.028(2) 0.006(2) 0.0006(17) -0.0028(19) S7 0.053(2) 0.046(3) 0.051(3) -0.017(2) -0.011(2) 0.024(2) O1 0.031(5) 0.027(6) 0.064(8) -0.019(6) 0.016(5) -0.001(4) N1 0.016(5) 0.030(8) 0.043(8) 0.002(6) 0.008(5) 0.004(4) N2 0.028(5) 0.026(7) 0.020(6) 0.003(5) 0.003(4) 0.004(5) N3 0.027(6) 0.034(8) 0.030(7) -0.006(6) 0.005(5) -0.012(5) N4 0.021(5) 0.038(8) 0.039(8) -0.005(7) 0.006(5) -0.010(5) N5 0.023(6) 0.039(8) 0.029(7) -0.003(6) 0.003(5) 0.004(5) N6 0.044(7) 0.043(8) 0.011(6) 0.010(6) 0.000(5) 0.003(6) N7 0.031(6) 0.019(6) 0.045(8) -0.008(6) -0.003(6) 0.001(5) C1 0.023(5) 0.022(7) 0.032(7) 0.006(8) -0.003(5) 0.001(6) C2 0.026(6) 0.023(9) 0.040(9) 0.005(6) -0.001(6) -0.001(5) C3 0.031(7) 0.033(9) 0.025(8) 0.010(7) 0.003(6) -0.004(6) C6 0.024(7) 0.026(8) 0.051(11) -0.002(8) -0.006(7) -0.005(6) C7 0.026(7) 0.032(9) 0.042(10) 0.005(8) 0.007(6) -0.001(6) C24 0.044(9) 0.023(8) 0.043(10) -0.003(7) 0.013(7) 0.001(7) C21 0.037(7) 0.022(7) 0.005(6) 0.006(5) 0.005(5) -0.001(6) C22 0.038(8) 0.032(9) 0.030(9) 0.005(7) -0.006(7) -0.008(7) C23 0.054(10) 0.032(10) 0.036(10) 0.017(8) -0.005(8) 0.000(8) C25 0.042(8) 0.015(7) 0.046(10) -0.007(7) 0.009(7) 0.005(6) C26 0.031(7) 0.026(8) 0.024(7) 0.004(6) 0.004(6) 0.005(6) C41 0.029(7) 0.029(10) 0.049(10) 0.004(8) 0.005(6) -0.017(6) C42 0.039(9) 0.061(13) 0.052(12) 0.031(11) -0.005(8) -0.014(8) C43 0.044(10) 0.047(14) 0.12(2) 0.004(14) -0.034(11) 0.004(9) C44 0.044(8) 0.063(12) 0.042(10) -0.003(12) 0.007(7) -0.004(10) C45 0.038(8) 0.081(15) 0.036(9) 0.005(11) -0.002(7) -0.003(10) C46 0.039(9) 0.076(15) 0.040(11) -0.003(10) -0.002(8) -0.034(9) C51 0.029(8) 0.071(14) 0.046(11) 0.003(10) 0.009(7) 0.021(8) C52 0.087(14) 0.076(16) 0.054(13) -0.017(15) 0.004(11) 0.030(14) C53 0.035(8) 0.047(12) 0.057(13) 0.012(10) -0.002(8) 0.003(8) C54 0.057(11) 0.046(14) 0.069(14) 0.009(11) 0.010(10) -0.001(9) _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 O1 1.677(11) . ? Re1 N2 1.997(12) . ? Re1 N6 2.098(12) . ? Re1 N7 2.207(13) . ? Re1 S5 2.370(4) . ? Re1 S4 2.377(3) . ? S4 C3 1.710(15) . ? S5 C1 1.732(14) . ? S6 C6 1.606(18) . ? S7 C7 1.610(17) . ? N1 C2 1.310(16) . ? N1 C1 1.388(18) . ? N2 N3 1.417(16) . ? N2 C2 1.432(18) . ? N3 C3 1.359(18) . ? N3 H3 0.8600 . ? N4 C3 1.336(18) . ? N4 C41 1.46(2) . ? N4 C46 1.51(2) . ? N5 C1 1.314(17) . ? N5 C51 1.40(2) . ? N5 C53 1.50(2) . ? N6 C6 1.14(2) . ? N7 C7 1.170(19) . ? C2 C21 1.44(2) . ? C24 C23 1.39(2) . ? C24 C25 1.42(2) . ? C24 H24 0.9300 . ? C21 C26 1.412(18) . ? C21 C22 1.445(19) . ? C22 C23 1.35(2) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 C26 1.34(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C42 1.54(3) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.54(3) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.54(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.47(2) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.55(3) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C51 C52 1.54(3) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.52(3) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 N2 100.8(6) . . ? O1 Re1 N6 92.7(6) . . ? N2 Re1 N6 165.6(5) . . ? O1 Re1 N7 172.0(6) . . ? N2 Re1 N7 87.1(5) . . ? N6 Re1 N7 79.2(5) . . ? O1 Re1 S5 96.9(3) . . ? N2 Re1 S5 93.5(3) . . ? N6 Re1 S5 89.6(4) . . ? N7 Re1 S5 83.8(3) . . ? O1 Re1 S4 99.1(3) . . ? N2 Re1 S4 81.3(3) . . ? N6 Re1 S4 91.9(4) . . ? N7 Re1 S4 80.7(3) . . ? S5 Re1 S4 163.83(14) . . ? C3 S4 Re1 98.7(5) . . ? C1 S5 Re1 98.0(4) . . ? C2 N1 C1 127.6(13) . . ? N3 N2 C2 110.3(12) . . ? N3 N2 Re1 120.5(8) . . ? C2 N2 Re1 124.9(9) . . ? C3 N3 N2 118.8(13) . . ? C3 N3 H3 120.6 . . ? N2 N3 H3 120.6 . . ? C3 N4 C41 122.7(12) . . ? C3 N4 C46 118.2(14) . . ? C41 N4 C46 118.7(12) . . ? C1 N5 C51 125.2(14) . . ? C1 N5 C53 118.6(13) . . ? C51 N5 C53 116.1(13) . . ? C6 N6 Re1 175.0(13) . . ? C7 N7 Re1 161.6(11) . . ? N5 C1 N1 118.5(12) . . ? N5 C1 S5 122.3(11) . . ? N1 C1 S5 118.6(10) . . ? N1 C2 N2 118.3(14) . . ? N1 C2 C21 117.1(13) . . ? N2 C2 C21 124.3(11) . . ? N4 C3 N3 119.1(14) . . ? N4 C3 S4 122.9(11) . . ? N3 C3 S4 117.9(11) . . ? N6 C6 S6 176.2(16) . . ? N7 C7 S7 176.9(14) . . ? C23 C24 C25 117.3(16) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C26 C21 C22 117.5(13) . . ? C26 C21 C2 123.7(12) . . ? C22 C21 C2 118.8(13) . . ? C23 C22 C21 120.2(14) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 122.0(16) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C26 C25 C24 122.6(14) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C25 C26 C21 120.2(13) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? N4 C41 C42 115.5(13) . . ? N4 C41 H41A 108.4 . . ? C42 C41 H41A 108.4 . . ? N4 C41 H41B 108.4 . . ? C42 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? C43 C42 C41 114.5(16) . . ? C43 C42 H42A 108.6 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 116.2(18) . . ? C42 C43 H43A 108.2 . . ? C44 C43 H43A 108.2 . . ? C42 C43 H43B 108.2 . . ? C44 C43 H43B 108.2 . . ? H43A C43 H43B 107.4 . . ? C45 C44 C43 114.5(16) . . ? C45 C44 H44A 108.6 . . ? C43 C44 H44A 108.6 . . ? C45 C44 H44B 108.6 . . ? C43 C44 H44B 108.6 . . ? H44A C44 H44B 107.6 . . ? C44 C45 C46 120.7(18) . . ? C44 C45 H45A 107.2 . . ? C46 C45 H45A 107.2 . . ? C44 C45 H45B 107.2 . . ? C46 C45 H45B 107.2 . . ? H45A C45 H45B 106.8 . . ? N4 C46 C45 106.7(14) . . ? N4 C46 H46A 110.4 . . ? C45 C46 H46A 110.4 . . ? N4 C46 H46B 110.4 . . ? C45 C46 H46B 110.4 . . ? H46A C46 H46B 108.6 . . ? N5 C51 C52 114.2(16) . . ? N5 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? N5 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 C54 114.4(16) . . ? N5 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? N5 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 S7 0.86 2.52 3.261(14) 144.3 2_645 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.631 _refine_diff_density_min -3.255 _refine_diff_density_rms 0.458 data_pirel4ncs1 _database_code_depnum_ccdc_archive 'CCDC 911731' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (N-(N'',N''-diethylaminothiocarbonyl)-N'(N''', N'''-hexamethylenecarbothioamide) benzamidineto)(isothiocyanato)(dimethylsufoxide)oxorhenium(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H33 N6 O2 Re S4' _chemical_formula_sum 'C22 H33 N6 O2 Re S4' _chemical_formula_weight 727.98 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.551(1) _cell_length_b 14.471(1) _cell_length_c 24.043(2) _cell_angle_alpha 76.67(1) _cell_angle_beta 83.92(1) _cell_angle_gamma 89.56(1) _cell_volume 2878.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 15314 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 29.30 _exptl_crystal_description plate _exptl_crystal_colour red-brown _exptl_crystal_size_max .3 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 4.542 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min .3274 _exptl_absorpt_correction_T_max .8721 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS' _diffrn_measurement_method 'rotational method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% .1 _diffrn_reflns_number 31690 _diffrn_reflns_av_R_equivalents 0.0971 _diffrn_reflns_av_sigmaI/netI 0.1343 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 29.30 _reflns_number_total 15314 _reflns_number_gt 8403 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution SHELXS-86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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^ > 2\s(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^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15314 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.867 _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 S1A S 0.7286(3) 0.49188(15) 0.25829(9) 0.0448(5) Uani 1 1 d . . . S1B S 0.3494(3) 0.35448(13) 0.04857(8) 0.0388(4) Uani 1 1 d . . . S2A S 0.8991(3) 0.44278(14) 0.43931(9) 0.0434(5) Uani 1 1 d . . . S2B S 0.1358(3) 0.06058(14) 0.05215(8) 0.0388(4) Uani 1 1 d . . . S3A S 0.4576(3) 0.46471(19) 0.36716(13) 0.0628(7) Uani 1 1 d . . . S3B S 0.5259(3) 0.08730(13) 0.03896(9) 0.0400(4) Uani 1 1 d . . . S6A S 0.5844(5) 0.7608(2) 0.3624(2) 0.1111(15) Uani 1 1 d . . . S6B S 0.4617(4) 0.26644(19) -0.14724(11) 0.0689(8) Uani 1 1 d . . . N1A N 0.7807(9) 0.3010(5) 0.2736(3) 0.0402(16) Uani 1 1 d . . . N1B N 0.2390(8) 0.3134(4) 0.1622(3) 0.0360(15) Uani 1 1 d . . . N2A N 0.8895(8) 0.3361(4) 0.3540(3) 0.0348(14) Uani 1 1 d . . . N2B N 0.1467(7) 0.1812(4) 0.1310(2) 0.0299(13) Uani 1 1 d . . . N3A N 0.9587(8) 0.2819(4) 0.4024(3) 0.0395(15) Uani 1 1 d . . . N3B N 0.0618(8) 0.0936(4) 0.1580(3) 0.0369(15) Uani 1 1 d . . . N4A N 1.0488(10) 0.2863(5) 0.4885(3) 0.0483(19) Uani 1 1 d . . . N4B N -0.0429(8) -0.0434(4) 0.1444(3) 0.0394(15) Uani 1 1 d . . . N5A N 0.7704(8) 0.3831(5) 0.1822(3) 0.0420(16) Uani 1 1 d . . . N5B N 0.2748(8) 0.4691(4) 0.1188(3) 0.0363(14) Uani 1 1 d . . . N6A N 0.7585(9) 0.6046(5) 0.3473(3) 0.0483(18) Uani 1 1 d . . . N6B N 0.3165(9) 0.2348(5) -0.0363(3) 0.0424(16) Uani 1 1 d . . . O1A O 1.0347(8) 0.5184(4) 0.3117(3) 0.0543(16) Uani 1 1 d . . . O1B O 0.0349(7) 0.2710(4) 0.0255(2) 0.0472(14) Uani 1 1 d . . . O2A O 0.6137(7) 0.4271(4) 0.3856(3) 0.0468(14) Uani 1 1 d . . . O2B O 0.4368(6) 0.1571(4) 0.0680(2) 0.0376(12) Uani 1 1 d . . . C1A C 0.7664(9) 0.3842(5) 0.2382(3) 0.0359(17) Uani 1 1 d . . . C1B C 0.2773(9) 0.3792(5) 0.1146(3) 0.0353(17) Uani 1 1 d . . . C2A C 0.8143(10) 0.2802(5) 0.3280(3) 0.0340(16) Uani 1 1 d . . . C2B C 0.2044(9) 0.2209(5) 0.1698(3) 0.0319(16) Uani 1 1 d . . . C3A C 0.9716(10) 0.3275(5) 0.4424(3) 0.0404(18) Uani 1 1 d . . . C3B C 0.0466(9) 0.0367(5) 0.1248(3) 0.0333(16) Uani 1 1 d . . . C6A C 0.6854(12) 0.6698(6) 0.3540(4) 0.053(2) Uani 1 1 d . . . C6B C 0.3793(11) 0.2491(5) -0.0828(4) 0.0425(19) Uani 1 1 d . . . C21A C 0.7668(10) 0.1797(5) 0.3580(4) 0.0404(18) Uani 1 1 d . . . C21B C 0.2309(9) 0.1641(5) 0.2272(3) 0.0369(17) Uani 1 1 d . . . C22A C 0.6766(13) 0.1664(6) 0.4107(4) 0.056(2) Uani 1 1 d . . . H22A H 0.6569 0.2169 0.4282 0.067 Uiso 1 1 calc R . . C22B C 0.3108(12) 0.0796(6) 0.2318(4) 0.053(2) Uani 1 1 d . . . H22B H 0.3344 0.0554 0.1993 0.063 Uiso 1 1 calc R . . C23A C 0.6156(15) 0.0755(7) 0.4370(5) 0.070(3) Uani 1 1 d . . . H23A H 0.5521 0.0655 0.4718 0.083 Uiso 1 1 calc R . . C23B C 0.3573(15) 0.0293(7) 0.2849(5) 0.073(3) Uani 1 1 d . . . H23B H 0.4157 -0.0258 0.2881 0.087 Uiso 1 1 calc R . . C24A C 0.6496(14) 0.0013(7) 0.4114(5) 0.064(3) Uani 1 1 d . . . H24A H 0.6109 -0.0591 0.4298 0.077 Uiso 1 1 calc R . . C24B C 0.3109(17) 0.0667(10) 0.3319(5) 0.085(4) Uani 1 1 d . . . H24B H 0.3384 0.0349 0.3677 0.102 Uiso 1 1 calc R . . C25A C 0.7386(14) 0.0139(6) 0.3597(5) 0.062(3) Uani 1 1 d . . . H25A H 0.7613 -0.0371 0.3429 0.074 Uiso 1 1 calc R . . C25B C 0.2252(17) 0.1495(10) 0.3282(4) 0.078(4) Uani 1 1 d . . . H25B H 0.1926 0.1710 0.3611 0.094 Uiso 1 1 calc R . . C26A C 0.7948(12) 0.1053(6) 0.3326(4) 0.050(2) Uani 1 1 d . . . H26A H 0.8523 0.1155 0.2966 0.060 Uiso 1 1 calc R . . C26B C 0.1893(13) 0.1992(7) 0.2751(4) 0.053(2) Uani 1 1 d . . . H26B H 0.1369 0.2565 0.2717 0.064 Uiso 1 1 calc R . . C31A C 0.3572(15) 0.3602(8) 0.3612(6) 0.082(4) Uani 1 1 d . . . H31A H 0.4072 0.3379 0.3291 0.122 Uiso 1 1 calc R . . H31B H 0.2496 0.3746 0.3553 0.122 Uiso 1 1 calc R . . H31C H 0.3609 0.3118 0.3958 0.122 Uiso 1 1 calc R . . C31B C 0.5647(15) -0.0080(7) 0.0963(5) 0.069(3) Uani 1 1 d . . . H31D H 0.6075 0.0164 0.1255 0.103 Uiso 1 1 calc R . . H31E H 0.6389 -0.0496 0.0823 0.103 Uiso 1 1 calc R . . H31F H 0.4687 -0.0425 0.1123 0.103 Uiso 1 1 calc R . . C32A C 0.3512(18) 0.4879(11) 0.4270(8) 0.113(6) Uani 1 1 d . . . H32A H 0.3471 0.4323 0.4579 0.170 Uiso 1 1 calc R . . H32B H 0.2463 0.5053 0.4184 0.170 Uiso 1 1 calc R . . H32C H 0.4007 0.5392 0.4381 0.170 Uiso 1 1 calc R . . C32B C 0.7171(13) 0.1379(8) 0.0205(6) 0.078(4) Uani 1 1 d . . . H32D H 0.7148 0.1941 -0.0098 0.116 Uiso 1 1 calc R . . H32E H 0.7870 0.0930 0.0077 0.116 Uiso 1 1 calc R . . H32F H 0.7535 0.1542 0.0535 0.116 Uiso 1 1 calc R . . C41A C 1.0437(13) 0.3227(6) 0.5410(4) 0.056(2) Uani 1 1 d . . . H41A H 1.0444 0.3915 0.5302 0.067 Uiso 1 1 calc R . . H41B H 1.1383 0.3035 0.5593 0.067 Uiso 1 1 calc R . . C41B C -0.0426(11) -0.1213(6) 0.1154(4) 0.048(2) Uani 1 1 d . . . H41C H -0.0239 -0.0952 0.0743 0.057 Uiso 1 1 calc R . . H41D H -0.1464 -0.1511 0.1231 0.057 Uiso 1 1 calc R . . C42A C 0.9033(15) 0.2894(8) 0.5840(4) 0.067(3) Uani 1 1 d . . . H42A H 0.9171 0.3108 0.6186 0.080 Uiso 1 1 calc R . . H42B H 0.8110 0.3202 0.5686 0.080 Uiso 1 1 calc R . . C42B C 0.0775(15) -0.1973(7) 0.1321(4) 0.064(3) Uani 1 1 d . . . H42C H 0.1816 -0.1707 0.1176 0.077 Uiso 1 1 calc R . . H42D H 0.0601 -0.2487 0.1136 0.077 Uiso 1 1 calc R . . C43A C 0.872(2) 0.1862(10) 0.6004(5) 0.108(5) Uani 1 1 d . . . H43A H 0.7893 0.1727 0.6322 0.129 Uiso 1 1 calc R . . H43B H 0.9659 0.1545 0.6138 0.129 Uiso 1 1 calc R . . C44A C 0.823(2) 0.1447(12) 0.5516(7) 0.121(7) Uani 1 1 d . . . H44A H 0.7640 0.1916 0.5268 0.146 Uiso 1 1 calc R . . H44B H 0.7544 0.0898 0.5677 0.146 Uiso 1 1 calc R . . C45A C 0.966(3) 0.1149(8) 0.5155(7) 0.129(8) Uani 1 1 d . . . H45A H 0.9294 0.0982 0.4822 0.155 Uiso 1 1 calc R . . H45B H 1.0085 0.0578 0.5383 0.155 Uiso 1 1 calc R . . C45B C -0.0130(15) -0.1079(8) 0.2485(4) 0.065(3) Uani 1 1 d . . . H45C H -0.0787 -0.1469 0.2805 0.078 Uiso 1 1 calc R . . H45D H 0.0317 -0.0573 0.2624 0.078 Uiso 1 1 calc R . . C46A C 1.1037(17) 0.1892(8) 0.4938(5) 0.079(4) Uani 1 1 d . . . H46A H 1.1829 0.1771 0.5205 0.095 Uiso 1 1 calc R . . H46B H 1.1521 0.1821 0.4568 0.095 Uiso 1 1 calc R . . C46B C -0.1159(12) -0.0642(7) 0.2042(4) 0.051(2) Uani 1 1 d . . . H46C H -0.2057 -0.1063 0.2074 0.061 Uiso 1 1 calc R . . H46D H -0.1553 -0.0054 0.2127 0.061 Uiso 1 1 calc R . . C43B C 0.0736(17) -0.2386(8) 0.1971(5) 0.080(4) Uani 1 1 d . . . H43C H -0.0318 -0.2627 0.2120 0.096 Uiso 1 1 calc R . . H43D H 0.1441 -0.2920 0.2034 0.096 Uiso 1 1 calc R . . C44B C 0.1202(18) -0.1681(9) 0.2316(5) 0.088(4) Uani 1 1 d . . . H44C H 0.1618 -0.2032 0.2662 0.106 Uiso 1 1 calc R . . H44D H 0.2037 -0.1266 0.2089 0.106 Uiso 1 1 calc R . . C51A C 0.8044(11) 0.2943(7) 0.1637(4) 0.051(2) Uani 1 1 d . . . H51A H 0.8821 0.2593 0.1864 0.061 Uiso 1 1 calc R . . H51B H 0.8489 0.3095 0.1237 0.061 Uiso 1 1 calc R . . C51B C 0.3457(11) 0.5471(5) 0.0730(4) 0.0426(19) Uani 1 1 d . . . H51C H 0.4340 0.5228 0.0521 0.051 Uiso 1 1 calc R . . H51D H 0.3863 0.5949 0.0903 0.051 Uiso 1 1 calc R . . C52A C 0.6587(14) 0.2324(8) 0.1700(5) 0.072(3) Uani 1 1 d . . . H52A H 0.6018 0.2286 0.2071 0.107 Uiso 1 1 calc R . . H52B H 0.6889 0.1699 0.1663 0.107 Uiso 1 1 calc R . . H52C H 0.5931 0.2596 0.1406 0.107 Uiso 1 1 calc R . . C52B C 0.2343(12) 0.5933(7) 0.0309(4) 0.058(3) Uani 1 1 d . . . H52D H 0.1996 0.5477 0.0113 0.087 Uiso 1 1 calc R . . H52E H 0.2871 0.6454 0.0034 0.087 Uiso 1 1 calc R . . H52F H 0.1451 0.6163 0.0512 0.087 Uiso 1 1 calc R . . C53A C 0.7209(11) 0.4644(7) 0.1373(4) 0.049(2) Uani 1 1 d . . . H53A H 0.6582 0.5072 0.1558 0.059 Uiso 1 1 calc R . . H53B H 0.6555 0.4404 0.1130 0.059 Uiso 1 1 calc R . . C53B C 0.2066(10) 0.4933(6) 0.1732(4) 0.0423(19) Uani 1 1 d . . . H53C H 0.1636 0.5565 0.1645 0.051 Uiso 1 1 calc R . . H53D H 0.1214 0.4490 0.1911 0.051 Uiso 1 1 calc R . . C54A C 0.8586(15) 0.5186(9) 0.1005(5) 0.076(3) Uani 1 1 d . . . H54A H 0.9148 0.5507 0.1233 0.114 Uiso 1 1 calc R . . H54B H 0.8216 0.5645 0.0693 0.114 Uiso 1 1 calc R . . H54C H 0.9274 0.4754 0.0855 0.114 Uiso 1 1 calc R . . C54B C 0.3268(12) 0.4895(7) 0.2138(4) 0.056(2) Uani 1 1 d . . . H54D H 0.3728 0.4277 0.2212 0.084 Uiso 1 1 calc R . . H54E H 0.2781 0.5016 0.2492 0.084 Uiso 1 1 calc R . . H54F H 0.4072 0.5367 0.1974 0.084 Uiso 1 1 calc R . . Re2 Re 0.20079(4) 0.21986(2) 0.045315(13) 0.03246(9) Uani 1 1 d . . . Re1 Re 0.85662(4) 0.47677(2) 0.342501(14) 0.03473(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 S1A 0.0550(14) 0.0405(10) 0.0406(11) -0.0088(8) -0.0143(10) 0.0065(9) S1B 0.0445(12) 0.0318(9) 0.0372(10) -0.0051(7) 0.0034(9) -0.0033(8) S2A 0.0520(14) 0.0399(10) 0.0433(11) -0.0165(9) -0.0130(10) 0.0026(9) S2B 0.0438(12) 0.0383(10) 0.0347(9) -0.0091(8) -0.0036(9) -0.0057(9) S3A 0.0398(14) 0.0609(15) 0.0848(19) -0.0119(13) -0.0045(13) -0.0018(11) S3B 0.0426(12) 0.0350(9) 0.0462(11) -0.0157(8) -0.0085(9) 0.0052(8) S6A 0.088(3) 0.0627(19) 0.199(5) -0.060(2) -0.026(3) 0.0269(18) S6B 0.097(2) 0.0582(14) 0.0457(13) -0.0124(11) 0.0234(14) -0.0273(14) N1A 0.048(4) 0.040(3) 0.036(3) -0.012(3) -0.011(3) -0.001(3) N1B 0.036(4) 0.033(3) 0.037(3) -0.006(3) 0.002(3) 0.000(3) N2A 0.035(4) 0.039(3) 0.032(3) -0.013(3) -0.007(3) 0.005(3) N2B 0.032(3) 0.026(3) 0.031(3) -0.005(2) -0.002(3) 0.000(2) N3A 0.045(4) 0.040(3) 0.038(3) -0.014(3) -0.017(3) 0.011(3) N3B 0.033(4) 0.036(3) 0.037(3) -0.001(3) 0.001(3) -0.008(3) N4A 0.068(5) 0.044(4) 0.041(4) -0.015(3) -0.026(4) 0.011(4) N4B 0.039(4) 0.036(3) 0.041(4) -0.007(3) 0.001(3) -0.005(3) N5A 0.036(4) 0.055(4) 0.034(3) -0.008(3) -0.007(3) 0.000(3) N5B 0.039(4) 0.030(3) 0.039(3) -0.006(3) -0.005(3) 0.002(3) N6A 0.051(5) 0.041(4) 0.055(4) -0.011(3) -0.017(4) 0.001(3) N6B 0.051(5) 0.038(4) 0.036(4) -0.005(3) -0.004(3) -0.007(3) O1A 0.042(4) 0.059(4) 0.059(4) -0.010(3) 0.001(3) -0.013(3) O1B 0.043(4) 0.047(3) 0.046(3) 0.003(3) -0.012(3) 0.006(3) O2A 0.030(3) 0.055(3) 0.053(4) -0.008(3) -0.004(3) -0.005(3) O2B 0.035(3) 0.042(3) 0.041(3) -0.017(2) -0.010(2) 0.007(2) C1A 0.030(4) 0.042(4) 0.036(4) -0.009(3) -0.008(3) 0.002(3) C1B 0.030(4) 0.035(4) 0.040(4) -0.006(3) -0.005(3) 0.003(3) C2A 0.038(5) 0.035(4) 0.030(4) -0.010(3) -0.001(3) 0.000(3) C2B 0.031(4) 0.032(4) 0.031(4) -0.007(3) 0.000(3) 0.004(3) C3A 0.041(5) 0.039(4) 0.040(4) -0.006(3) -0.010(4) 0.001(3) C3B 0.028(4) 0.037(4) 0.033(4) -0.004(3) -0.005(3) -0.004(3) C6A 0.052(6) 0.043(5) 0.067(6) -0.016(4) -0.006(5) -0.008(4) C6B 0.048(5) 0.037(4) 0.045(5) -0.012(3) -0.005(4) -0.005(4) C21A 0.041(5) 0.035(4) 0.047(5) -0.007(3) -0.015(4) 0.002(3) C21B 0.031(4) 0.042(4) 0.035(4) -0.003(3) -0.003(3) -0.010(3) C22A 0.072(7) 0.043(5) 0.052(5) -0.013(4) -0.003(5) -0.001(4) C22B 0.051(6) 0.050(5) 0.055(5) -0.003(4) -0.016(5) -0.001(4) C23A 0.086(9) 0.060(6) 0.053(6) -0.002(5) 0.011(6) -0.017(6) C23B 0.088(9) 0.052(6) 0.067(7) 0.021(5) -0.037(7) -0.015(5) C24A 0.072(8) 0.039(5) 0.076(7) 0.001(5) -0.020(6) -0.005(5) C24B 0.101(11) 0.091(9) 0.049(6) 0.025(6) -0.034(7) -0.041(8) C25A 0.075(8) 0.035(5) 0.078(7) -0.018(4) -0.008(6) -0.001(5) C25B 0.097(10) 0.099(9) 0.036(5) -0.009(6) -0.009(6) -0.030(8) C26A 0.053(6) 0.043(5) 0.057(5) -0.018(4) -0.005(5) -0.001(4) C26B 0.056(6) 0.063(6) 0.040(5) -0.008(4) -0.007(4) -0.020(5) C31A 0.060(8) 0.080(8) 0.106(10) -0.024(7) -0.009(7) -0.014(6) C31B 0.084(9) 0.049(5) 0.077(7) -0.014(5) -0.028(6) 0.021(5) C32A 0.073(10) 0.114(11) 0.167(16) -0.074(11) 0.015(10) -0.004(8) C32B 0.053(7) 0.078(7) 0.102(9) -0.040(7) 0.032(7) -0.011(6) C41A 0.076(7) 0.050(5) 0.048(5) -0.018(4) -0.027(5) 0.005(5) C41B 0.051(6) 0.043(5) 0.047(5) -0.010(4) 0.003(4) -0.023(4) C42A 0.081(8) 0.078(7) 0.043(5) -0.016(5) -0.010(5) 0.012(6) C42B 0.085(9) 0.047(5) 0.064(6) -0.021(5) -0.004(6) -0.001(5) C43A 0.160(17) 0.100(10) 0.054(7) -0.001(7) -0.009(9) -0.038(10) C44A 0.166(19) 0.102(11) 0.081(10) 0.007(9) -0.004(11) -0.062(12) C45A 0.25(2) 0.042(6) 0.111(12) -0.013(7) -0.095(15) 0.010(10) C45B 0.093(9) 0.066(6) 0.033(5) -0.008(4) 0.001(5) 0.003(6) C46A 0.114(11) 0.071(7) 0.067(7) -0.032(6) -0.048(7) 0.058(7) C46B 0.049(6) 0.054(5) 0.046(5) -0.010(4) 0.008(4) -0.012(4) C43B 0.100(10) 0.063(7) 0.069(7) -0.002(6) -0.010(7) 0.021(6) C44B 0.107(11) 0.094(9) 0.066(7) -0.014(7) -0.031(7) 0.032(8) C51A 0.044(5) 0.075(6) 0.040(4) -0.026(4) -0.006(4) 0.012(5) C51B 0.045(5) 0.031(4) 0.050(5) -0.007(3) 0.000(4) -0.006(3) C52A 0.068(8) 0.075(7) 0.084(8) -0.036(6) -0.020(6) -0.010(6) C52B 0.052(6) 0.049(5) 0.065(6) 0.004(4) -0.004(5) 0.002(4) C53A 0.045(5) 0.063(5) 0.039(4) -0.011(4) -0.007(4) 0.002(4) C53B 0.032(4) 0.045(4) 0.054(5) -0.019(4) -0.004(4) -0.002(4) C54A 0.067(8) 0.092(8) 0.059(7) 0.007(6) -0.011(6) -0.008(6) C54B 0.054(6) 0.069(6) 0.046(5) -0.016(4) 0.002(5) -0.005(5) Re2 0.0337(2) 0.03249(16) 0.02925(16) -0.00257(12) -0.00488(14) -0.00003(13) Re1 0.0330(2) 0.03252(17) 0.03937(18) -0.00897(13) -0.00517(15) -0.00229(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S1A C1A 1.753(8) . ? S1A Re1 2.368(2) . ? S1B C1B 1.755(8) . ? S1B Re2 2.355(2) . ? S2A C3A 1.763(8) . ? S2A Re1 2.332(2) . ? S2B C3B 1.787(8) . ? S2B Re2 2.3397(19) . ? S3A O2A 1.510(7) . ? S3A C32A 1.718(15) . ? S3A C31A 1.787(11) . ? S3B O2B 1.513(5) . ? S3B C32B 1.767(11) . ? S3B C31B 1.768(10) . ? S6A C6A 1.610(10) . ? S6B C6B 1.597(9) . ? N1A C1A 1.317(10) . ? N1A C2A 1.333(10) . ? N1B C1B 1.322(9) . ? N1B C2B 1.340(9) . ? N2A C2A 1.336(10) . ? N2A N3A 1.428(9) . ? N2A Re1 2.012(6) . ? N2B C2B 1.339(9) . ? N2B N3B 1.446(8) . ? N2B Re2 2.009(6) . ? N3A C3A 1.299(10) . ? N3B C3B 1.289(10) . ? N4A C3A 1.365(10) . ? N4A C46A 1.458(11) . ? N4A C41A 1.472(11) . ? N4B C3B 1.355(9) . ? N4B C41B 1.457(10) . ? N4B C46B 1.469(10) . ? N5A C1A 1.346(10) . ? N5A C51A 1.472(11) . ? N5A C53A 1.495(11) . ? N5B C1B 1.328(9) . ? N5B C51B 1.467(10) . ? N5B C53B 1.489(10) . ? N6A C6A 1.159(11) . ? N6A Re1 2.048(7) . ? N6B C6B 1.163(10) . ? N6B Re2 2.066(7) . ? O1A Re1 1.674(6) . ? O1B Re2 1.658(6) . ? O2A Re1 2.265(6) . ? O2B Re2 2.274(5) . ? C2A C21A 1.504(10) . ? C2B C21B 1.474(10) . ? C21A C26A 1.364(11) . ? C21A C22A 1.386(12) . ? C21B C26B 1.376(12) . ? C21B C22B 1.385(12) . ? C22A C23A 1.399(13) . ? C22A H22A 0.9300 . ? C22B C23B 1.412(13) . ? C22B H22B 0.9300 . ? C23A C24A 1.370(15) . ? C23A H23A 0.9300 . ? C23B C24B 1.382(18) . ? C23B H23B 0.9300 . ? C24A C25A 1.362(15) . ? C24A H24A 0.9300 . ? C24B C25B 1.390(19) . ? C24B H24B 0.9300 . ? C25A C26A 1.397(12) . ? C25A H25A 0.9300 . ? C25B C26B 1.378(14) . ? C25B H25B 0.9300 . ? C26A H26A 0.9300 . ? C26B H26B 0.9300 . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C31B H31D 0.9600 . ? C31B H31E 0.9600 . ? C31B H31F 0.9600 . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C41A C42A 1.503(15) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C41B C42B 1.514(14) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42A C43A 1.473(16) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C42B C43B 1.536(15) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43A C44A 1.53(2) . ? C43A H43A 0.9700 . ? C43A H43B 0.9700 . ? C44A C45A 1.54(2) . ? C44A H44A 0.9700 . ? C44A H44B 0.9700 . ? C45A C46A 1.56(2) . ? C45A H45A 0.9700 . ? C45A H45B 0.9700 . ? C45B C46B 1.479(14) . ? C45B C44B 1.507(17) . ? C45B H45C 0.9700 . ? C45B H45D 0.9700 . ? C46A H46A 0.9700 . ? C46A H46B 0.9700 . ? C46B H46C 0.9700 . ? C46B H46D 0.9700 . ? C43B C44B 1.534(17) . ? C43B H43C 0.9700 . ? C43B H43D 0.9700 . ? C44B H44C 0.9700 . ? C44B H44D 0.9700 . ? C51A C52A 1.514(14) . ? C51A H51A 0.9700 . ? C51A H51B 0.9700 . ? C51B C52B 1.502(13) . ? C51B H51C 0.9700 . ? C51B H51D 0.9700 . ? C52A H52A 0.9600 . ? C52A H52B 0.9600 . ? C52A H52C 0.9600 . ? C52B H52D 0.9600 . ? C52B H52E 0.9600 . ? C52B H52F 0.9600 . ? C53A C54A 1.502(14) . ? C53A H53A 0.9700 . ? C53A H53B 0.9700 . ? C53B C54B 1.483(13) . ? C53B H53C 0.9700 . ? C53B H53D 0.9700 . ? C54A H54A 0.9600 . ? C54A H54B 0.9600 . ? C54A H54C 0.9600 . ? C54B H54D 0.9600 . ? C54B H54E 0.9600 . ? C54B H54F 0.9600 . ? 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 C1A S1A Re1 103.8(3) . . ? C1B S1B Re2 103.4(3) . . ? C3A S2A Re1 96.5(3) . . ? C3B S2B Re2 96.4(2) . . ? O2A S3A C32A 106.5(7) . . ? O2A S3A C31A 102.8(5) . . ? C32A S3A C31A 100.4(7) . . ? O2B S3B C32B 103.8(4) . . ? O2B S3B C31B 104.3(4) . . ? C32B S3B C31B 99.2(6) . . ? C1A N1A C2A 130.0(7) . . ? C1B N1B C2B 130.5(7) . . ? C2A N2A N3A 111.5(6) . . ? C2A N2A Re1 124.0(5) . . ? N3A N2A Re1 122.2(5) . . ? C2B N2B N3B 111.6(6) . . ? C2B N2B Re2 126.0(5) . . ? N3B N2B Re2 121.4(4) . . ? C3A N3A N2A 113.8(6) . . ? C3B N3B N2B 115.0(6) . . ? C3A N4A C46A 119.1(7) . . ? C3A N4A C41A 123.3(7) . . ? C46A N4A C41A 115.6(7) . . ? C3B N4B C41B 123.9(7) . . ? C3B N4B C46B 118.5(7) . . ? C41B N4B C46B 116.0(6) . . ? C1A N5A C51A 119.9(7) . . ? C1A N5A C53A 123.7(7) . . ? C51A N5A C53A 115.8(7) . . ? C1B N5B C51B 122.8(7) . . ? C1B N5B C53B 119.9(6) . . ? C51B N5B C53B 117.3(6) . . ? C6A N6A Re1 170.7(8) . . ? C6B N6B Re2 175.8(7) . . ? S3A O2A Re1 127.4(3) . . ? S3B O2B Re2 124.9(3) . . ? N1A C1A N5A 115.7(7) . . ? N1A C1A S1A 125.8(6) . . ? N5A C1A S1A 118.4(6) . . ? N1B C1B N5B 117.3(7) . . ? N1B C1B S1B 124.0(6) . . ? N5B C1B S1B 118.4(6) . . ? N1A C2A N2A 126.9(7) . . ? N1A C2A C21A 111.6(6) . . ? N2A C2A C21A 121.4(7) . . ? N2B C2B N1B 125.3(7) . . ? N2B C2B C21B 121.4(6) . . ? N1B C2B C21B 113.3(7) . . ? N3A C3A N4A 119.1(7) . . ? N3A C3A S2A 123.2(6) . . ? N4A C3A S2A 117.7(6) . . ? N3B C3B N4B 119.6(7) . . ? N3B C3B S2B 122.4(5) . . ? N4B C3B S2B 118.0(6) . . ? N6A C6A S6A 179.3(10) . . ? N6B C6B S6B 178.2(8) . . ? C26A C21A C22A 120.2(8) . . ? C26A C21A C2A 122.4(8) . . ? C22A C21A C2A 117.0(7) . . ? C26B C21B C22B 120.4(8) . . ? C26B C21B C2B 120.0(8) . . ? C22B C21B C2B 119.3(8) . . ? C21A C22A C23A 118.7(9) . . ? C21A C22A H22A 120.6 . . ? C23A C22A H22A 120.6 . . ? C21B C22B C23B 121.3(10) . . ? C21B C22B H22B 119.4 . . ? C23B C22B H22B 119.4 . . ? C24A C23A C22A 120.0(10) . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24B C23B C22B 116.2(11) . . ? C24B C23B H23B 121.9 . . ? C22B C23B H23B 121.9 . . ? C25A C24A C23A 121.6(9) . . ? C25A C24A H24A 119.2 . . ? C23A C24A H24A 119.2 . . ? C23B C24B C25B 123.1(10) . . ? C23B C24B H24B 118.5 . . ? C25B C24B H24B 118.5 . . ? C24A C25A C26A 118.4(9) . . ? C24A C25A H25A 120.8 . . ? C26A C25A H25A 120.8 . . ? C26B C25B C24B 119.0(11) . . ? C26B C25B H25B 120.5 . . ? C24B C25B H25B 120.5 . . ? C21A C26A C25A 121.1(9) . . ? C21A C26A H26A 119.5 . . ? C25A C26A H26A 119.5 . . ? C21B C26B C25B 120.0(11) . . ? C21B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? S3A C31A H31A 109.5 . . ? S3A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? S3A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? S3B C31B H31D 109.5 . . ? S3B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? S3B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? S3A C32A H32A 109.5 . . ? S3A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? S3A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? S3B C32B H32D 109.5 . . ? S3B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? S3B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N4A C41A C42A 114.6(8) . . ? N4A C41A H41A 108.6 . . ? C42A C41A H41A 108.6 . . ? N4A C41A H41B 108.6 . . ? C42A C41A H41B 108.6 . . ? H41A C41A H41B 107.6 . . ? N4B C41B C42B 115.5(8) . . ? N4B C41B H41C 108.4 . . ? C42B C41B H41C 108.4 . . ? N4B C41B H41D 108.4 . . ? C42B C41B H41D 108.4 . . ? H41C C41B H41D 107.5 . . ? C43A C42A C41A 116.4(10) . . ? C43A C42A H42A 108.2 . . ? C41A C42A H42A 108.2 . . ? C43A C42A H42B 108.2 . . ? C41A C42A H42B 108.2 . . ? H42A C42A H42B 107.3 . . ? C41B C42B C43B 114.5(9) . . ? C41B C42B H42C 108.6 . . ? C43B C42B H42C 108.6 . . ? C41B C42B H42D 108.6 . . ? C43B C42B H42D 108.6 . . ? H42C C42B H42D 107.6 . . ? C42A C43A C44A 114.1(11) . . ? C42A C43A H43A 108.7 . . ? C44A C43A H43A 108.7 . . ? C42A C43A H43B 108.7 . . ? C44A C43A H43B 108.7 . . ? H43A C43A H43B 107.6 . . ? C43A C44A C45A 111.9(16) . . ? C43A C44A H44A 109.2 . . ? C45A C44A H44A 109.2 . . ? C43A C44A H44B 109.2 . . ? C45A C44A H44B 109.2 . . ? H44A C44A H44B 107.9 . . ? C44A C45A C46A 117.0(11) . . ? C44A C45A H45A 108.0 . . ? C46A C45A H45A 108.0 . . ? C44A C45A H45B 108.0 . . ? C46A C45A H45B 108.0 . . ? H45A C45A H45B 107.3 . . ? C46B C45B C44B 118.0(9) . . ? C46B C45B H45C 107.8 . . ? C44B C45B H45C 107.8 . . ? C46B C45B H45D 107.8 . . ? C44B C45B H45D 107.8 . . ? H45C C45B H45D 107.1 . . ? N4A C46A C45A 111.8(12) . . ? N4A C46A H46A 109.3 . . ? C45A C46A H46A 109.3 . . ? N4A C46A H46B 109.3 . . ? C45A C46A H46B 109.3 . . ? H46A C46A H46B 107.9 . . ? N4B C46B C45B 116.0(8) . . ? N4B C46B H46C 108.3 . . ? C45B C46B H46C 108.3 . . ? N4B C46B H46D 108.3 . . ? C45B C46B H46D 108.3 . . ? H46C C46B H46D 107.4 . . ? C44B C43B C42B 114.8(9) . . ? C44B C43B H43C 108.6 . . ? C42B C43B H43C 108.6 . . ? C44B C43B H43D 108.6 . . ? C42B C43B H43D 108.6 . . ? H43C C43B H43D 107.6 . . ? C45B C44B C43B 114.1(12) . . ? C45B C44B H44C 108.7 . . ? C43B C44B H44C 108.7 . . ? C45B C44B H44D 108.7 . . ? C43B C44B H44D 108.7 . . ? H44C C44B H44D 107.6 . . ? N5A C51A C52A 112.2(8) . . ? N5A C51A H51A 109.2 . . ? C52A C51A H51A 109.2 . . ? N5A C51A H51B 109.2 . . ? C52A C51A H51B 109.2 . . ? H51A C51A H51B 107.9 . . ? N5B C51B C52B 114.1(7) . . ? N5B C51B H51C 108.7 . . ? C52B C51B H51C 108.7 . . ? N5B C51B H51D 108.7 . . ? C52B C51B H51D 108.7 . . ? H51C C51B H51D 107.6 . . ? C51A C52A H52A 109.5 . . ? C51A C52A H52B 109.5 . . ? H52A C52A H52B 109.5 . . ? C51A C52A H52C 109.5 . . ? H52A C52A H52C 109.5 . . ? H52B C52A H52C 109.5 . . ? C51B C52B H52D 109.5 . . ? C51B C52B H52E 109.5 . . ? H52D C52B H52E 109.5 . . ? C51B C52B H52F 109.5 . . ? H52D C52B H52F 109.5 . . ? H52E C52B H52F 109.5 . . ? N5A C53A C54A 112.5(8) . . ? N5A C53A H53A 109.1 . . ? C54A C53A H53A 109.1 . . ? N5A C53A H53B 109.1 . . ? C54A C53A H53B 109.1 . . ? H53A C53A H53B 107.8 . . ? C54B C53B N5B 111.4(7) . . ? C54B C53B H53C 109.3 . . ? N5B C53B H53C 109.3 . . ? C54B C53B H53D 109.3 . . ? N5B C53B H53D 109.3 . . ? H53C C53B H53D 108.0 . . ? C53A C54A H54A 109.5 . . ? C53A C54A H54B 109.5 . . ? H54A C54A H54B 109.5 . . ? C53A C54A H54C 109.5 . . ? H54A C54A H54C 109.5 . . ? H54B C54A H54C 109.5 . . ? C53B C54B H54D 109.5 . . ? C53B C54B H54E 109.5 . . ? H54D C54B H54E 109.5 . . ? C53B C54B H54F 109.5 . . ? H54D C54B H54F 109.5 . . ? H54E C54B H54F 109.5 . . ? O1B Re2 N2B 100.5(3) . . ? O1B Re2 N6B 97.0(3) . . ? N2B Re2 N6B 162.3(3) . . ? O1B Re2 O2B 176.3(2) . . ? N2B Re2 O2B 82.4(2) . . ? N6B Re2 O2B 80.2(3) . . ? O1B Re2 S2B 100.2(2) . . ? N2B Re2 S2B 82.04(16) . . ? N6B Re2 S2B 92.44(18) . . ? O2B Re2 S2B 82.35(14) . . ? O1B Re2 S1B 100.2(2) . . ? N2B Re2 S1B 94.14(17) . . ? N6B Re2 S1B 85.18(19) . . ? O2B Re2 S1B 77.30(14) . . ? S2B Re2 S1B 159.62(8) . . ? O1A Re1 N2A 100.6(3) . . ? O1A Re1 N6A 97.5(3) . . ? N2A Re1 N6A 161.6(3) . . ? O1A Re1 O2A 177.2(3) . . ? N2A Re1 O2A 82.0(2) . . ? N6A Re1 O2A 79.9(3) . . ? O1A Re1 S2A 100.6(2) . . ? N2A Re1 S2A 81.46(18) . . ? N6A Re1 S2A 91.9(2) . . ? O2A Re1 S2A 78.62(17) . . ? O1A Re1 S1A 98.6(2) . . ? N2A Re1 S1A 95.10(19) . . ? N6A Re1 S1A 85.5(2) . . ? O2A Re1 S1A 82.16(17) . . ? S2A Re1 S1A 160.76(8) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.627 _refine_diff_density_min -2.292 _refine_diff_density_rms 0.225 data_pirenl4o_href _database_code_depnum_ccdc_archive 'CCDC 911732' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'mu-(oxo)bis[(N-(N'',N''-diethylaminothiocarbonyl)- N'(N''', N'''-hexamethylenecarbothioamide) benzamidineto)nitridorhenium(V)]' ; _chemical_name_common '[{ReN(L1d)}2(O)]' _chemical_melting_point ? _chemical_formula_moiety "C38 H56 N12 O Re2 S4';'C1 H2 Cl2';'C1 H2 Cl2" _chemical_formula_sum 'C40 H60 Cl4 N12 O Re2 S4' _chemical_formula_weight 1367.44 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 8.250(1) _cell_length_b 12.778(2) _cell_length_c 13.083(2) _cell_angle_alpha 81.51(1) _cell_angle_beta 74.67(1) _cell_angle_gamma 78.56(1) _cell_volume 1297.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 14361 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 29.61 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.154 _exptl_crystal_size_mid 0.136 _exptl_crystal_size_min 0.098 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 5.074 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min .3046 _exptl_absorpt_correction_T_max 0.7013 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13431 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.26 _reflns_number_total 6875 _reflns_number_gt 5405 _reflns_threshold_expression >2\s(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution SHELXS-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material WINGX _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^ > 2\s(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^)+(0.0946P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0328(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6875 _refine_ls_number_parameters 281 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.901 _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 0.05389(3) 0.483538(14) 0.857792(16) 0.04918(11) Uani 1 1 d . . . S2 S 0.30039(17) 0.37068(10) 0.88193(11) 0.0505(3) Uani 1 1 d . . . S1 S -0.2358(2) 0.47717(13) 0.88761(12) 0.0617(3) Uani 1 1 d . . . N1 N -0.1610(6) 0.4424(4) 0.6786(4) 0.0490(9) Uani 1 1 d . . . N2 N 0.0977(6) 0.3858(3) 0.7325(3) 0.0459(8) Uani 1 1 d . . . N3 N 0.2585(5) 0.3201(4) 0.7002(4) 0.0520(10) Uani 1 1 d . . . H3 H 0.2862 0.2883 0.6431 0.062 Uiso 1 1 calc R . . C2 C -0.0120(6) 0.3778(4) 0.6777(4) 0.0418(9) Uani 1 1 d . . . N4 N 0.5212(6) 0.2566(4) 0.7343(4) 0.0554(10) Uani 1 1 d . . . C1 C -0.2566(7) 0.4968(4) 0.7572(5) 0.0493(10) Uani 1 1 d . . . C3 C 0.3591(6) 0.3111(4) 0.7608(4) 0.0467(10) Uani 1 1 d . . . C21 C 0.0254(6) 0.2957(4) 0.5994(4) 0.0439(9) Uani 1 1 d . . . C22 C 0.0798(7) 0.1881(4) 0.6273(4) 0.0502(11) Uani 1 1 d . . . H22 H 0.1031 0.1661 0.6937 0.060 Uiso 1 1 calc R . . C23 C 0.0996(9) 0.1136(5) 0.5569(6) 0.0636(14) Uani 1 1 d . . . H23 H 0.1364 0.0414 0.5760 0.076 Uiso 1 1 calc R . . C25 C 0.0078(9) 0.2523(7) 0.4303(5) 0.0695(17) Uani 1 1 d . . . H25 H -0.0153 0.2736 0.3638 0.083 Uiso 1 1 calc R . . C24 C 0.0648(9) 0.1454(6) 0.4580(5) 0.0681(16) Uani 1 1 d . . . H24 H 0.0798 0.0950 0.4103 0.082 Uiso 1 1 calc R . . C26 C -0.0153(8) 0.3284(5) 0.5010(4) 0.0549(12) Uani 1 1 d . . . H26 H -0.0573 0.4000 0.4831 0.066 Uiso 1 1 calc R . . N6 N 0.0980(7) 0.6017(4) 0.7925(5) 0.0615(12) Uani 1 1 d . . . O O 0.0000 0.5000 1.0000 0.080(2) Uani 1 2 d S . . Cl2 Cl -0.0839(6) 0.1112(3) 1.1888(3) 0.1361(11) Uani 1 1 d . . . Cl1 Cl -0.0125(9) 0.1617(6) 0.9602(4) 0.212(3) Uani 1 1 d . . . C100 C 0.0133(17) 0.1837(10) 1.0749(9) 0.113(4) Uani 1 1 d . . . H10A H -0.0271 0.2593 1.0836 0.136 Uiso 1 1 calc R . . H10B H 0.1347 0.1705 1.0706 0.136 Uiso 1 1 calc R . . C41 C 0.6227(7) 0.2194(5) 0.8120(6) 0.0600(14) Uani 1 1 d . . . H41A H 0.6065 0.2756 0.8578 0.072 Uiso 1 1 calc R . . H41B H 0.7421 0.2072 0.7746 0.072 Uiso 1 1 calc R . . C42 C 0.5804(11) 0.1176(6) 0.8807(8) 0.081(2) Uani 1 1 d . . . H42A H 0.4651 0.1313 0.9247 0.098 Uiso 1 1 calc R . . H42B H 0.6573 0.0958 0.9276 0.098 Uiso 1 1 calc R . . C46 C 0.5835(9) 0.2099(7) 0.6334(6) 0.0775(19) Uani 1 1 d . . . H46A H 0.7068 0.2026 0.6134 0.093 Uiso 1 1 calc R . . H46B H 0.5403 0.2596 0.5794 0.093 Uiso 1 1 calc R . . C43 C 0.596(2) 0.0241(7) 0.8107(15) 0.145(6) Uani 1 1 d . . . H43A H 0.7135 0.0099 0.7697 0.175 Uiso 1 1 calc R . . H43B H 0.5747 -0.0400 0.8586 0.175 Uiso 1 1 calc R . . C45 C 0.5366(12) 0.1041(8) 0.6328(8) 0.094(3) Uani 1 1 d . . . H45A H 0.6330 0.0613 0.5888 0.113 Uiso 1 1 calc R . . H45B H 0.4434 0.1155 0.5980 0.113 Uiso 1 1 calc R . . C44 C 0.485(2) 0.0395(9) 0.7364(15) 0.148(6) Uani 1 1 d . . . H44A H 0.3727 0.0729 0.7726 0.178 Uiso 1 1 calc R . . H44B H 0.4754 -0.0309 0.7217 0.178 Uiso 1 1 calc R . . N5 N -0.3910(7) 0.5703(4) 0.7392(5) 0.0659(13) Uani 1 1 d . . . C53 C -0.5108(9) 0.6322(6) 0.8232(8) 0.079(2) Uani 1 1 d . . . H53A H -0.5289 0.5865 0.8900 0.095 Uiso 1 1 calc R . . H53B H -0.6197 0.6547 0.8047 0.095 Uiso 1 1 calc R . . C54 C -0.4452(14) 0.7299(7) 0.8378(10) 0.103(3) Uani 1 1 d . . . H54A H -0.5260 0.7677 0.8931 0.155 Uiso 1 1 calc R . . H54B H -0.4298 0.7762 0.7724 0.155 Uiso 1 1 calc R . . H54C H -0.3381 0.7079 0.8571 0.155 Uiso 1 1 calc R . . C51 C -0.412(2) 0.6006(14) 0.6228(14) 0.148(4) Uani 1 1 d . . . H51A H -0.4447 0.6776 0.6094 0.178 Uiso 1 1 calc R . . H51B H -0.3049 0.5783 0.5723 0.178 Uiso 1 1 calc R . . C52 C -0.5380(17) 0.5473(11) 0.6126(10) 0.148(4) Uani 1 1 d . . . H52A H -0.5535 0.5631 0.5414 0.222 Uiso 1 1 calc R . . H52B H -0.6431 0.5710 0.6623 0.222 Uiso 1 1 calc R . . H52C H -0.5044 0.4714 0.6271 0.222 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.05509(15) 0.03951(13) 0.05716(15) -0.01957(8) -0.02334(9) 0.00630(8) S2 0.0517(6) 0.0438(6) 0.0572(7) -0.0165(5) -0.0182(5) 0.0048(5) S1 0.0668(8) 0.0558(7) 0.0572(7) -0.0149(6) -0.0111(6) 0.0032(6) N1 0.053(2) 0.045(2) 0.052(2) -0.0116(17) -0.0168(18) -0.0064(18) N2 0.051(2) 0.0396(19) 0.048(2) -0.0139(16) -0.0094(17) -0.0050(16) N3 0.045(2) 0.054(2) 0.059(2) -0.0250(19) -0.0068(18) -0.0068(18) C2 0.047(2) 0.036(2) 0.041(2) -0.0088(16) -0.0072(17) -0.0072(17) N4 0.043(2) 0.051(2) 0.068(3) -0.020(2) -0.0033(19) -0.0032(18) C1 0.051(3) 0.038(2) 0.062(3) -0.011(2) -0.014(2) -0.0077(19) C3 0.047(2) 0.036(2) 0.057(3) -0.0120(18) -0.007(2) -0.0077(18) C21 0.047(2) 0.046(2) 0.040(2) -0.0117(17) -0.0064(18) -0.0117(19) C22 0.055(3) 0.045(2) 0.055(3) -0.015(2) -0.014(2) -0.009(2) C23 0.064(3) 0.051(3) 0.079(4) -0.029(3) -0.016(3) -0.002(2) C25 0.072(4) 0.096(5) 0.048(3) -0.023(3) -0.015(3) -0.019(4) C24 0.065(3) 0.078(4) 0.070(4) -0.046(3) -0.013(3) -0.007(3) C26 0.064(3) 0.058(3) 0.043(2) -0.008(2) -0.009(2) -0.014(2) N6 0.066(3) 0.042(2) 0.089(3) -0.020(2) -0.041(3) 0.001(2) O 0.072(4) 0.080(4) 0.092(5) -0.044(4) -0.036(4) 0.026(3) Cl2 0.161(3) 0.127(3) 0.118(2) -0.0008(19) -0.030(2) -0.032(2) Cl1 0.305(7) 0.264(7) 0.133(3) 0.031(4) -0.092(4) -0.189(6) C100 0.123(8) 0.118(8) 0.108(7) -0.028(6) -0.010(6) -0.054(7) C41 0.044(3) 0.052(3) 0.085(4) -0.021(3) -0.015(3) -0.001(2) C42 0.074(4) 0.067(4) 0.100(6) -0.007(4) -0.024(4) -0.002(3) C46 0.061(4) 0.085(5) 0.075(4) -0.031(4) 0.005(3) 0.003(3) C43 0.190(14) 0.050(4) 0.236(16) 0.015(7) -0.130(13) -0.029(6) C45 0.085(5) 0.094(6) 0.109(6) -0.062(5) -0.019(5) 0.005(4) C44 0.193(15) 0.071(6) 0.221(17) -0.030(8) -0.100(13) -0.037(8) N5 0.053(3) 0.059(3) 0.097(4) -0.035(3) -0.031(3) 0.003(2) C53 0.054(3) 0.064(4) 0.126(6) -0.049(4) -0.020(4) 0.002(3) C54 0.102(6) 0.064(4) 0.154(9) -0.049(5) -0.037(6) -0.002(4) C51 0.154(9) 0.156(9) 0.172(9) -0.032(7) -0.103(8) -0.016(7) C52 0.154(9) 0.156(9) 0.172(9) -0.032(7) -0.103(8) -0.016(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N6 1.677(5) . ? Re1 O 1.8288(3) . ? Re1 N2 2.119(4) . ? Re1 S2 2.3143(13) . ? Re1 S1 2.3330(18) . ? S2 C3 1.769(5) . ? S1 C1 1.737(6) . ? N1 C1 1.313(7) . ? N1 C2 1.336(7) . ? N2 C2 1.321(7) . ? N2 N3 1.417(6) . ? N3 C3 1.270(7) . ? N3 H3 0.8600 . ? C2 C21 1.505(6) . ? N4 C3 1.360(7) . ? N4 C46 1.454(9) . ? N4 C41 1.452(9) . ? C1 N5 1.352(7) . ? C21 C22 1.385(7) . ? C21 C26 1.400(7) . ? C22 C23 1.378(8) . ? C22 H22 0.9300 . ? C23 C24 1.385(10) . ? C23 H23 0.9300 . ? C25 C24 1.381(11) . ? C25 C26 1.391(9) . ? C25 H25 0.9300 . ? C24 H24 0.9300 . ? C26 H26 0.9300 . ? O Re1 1.8288(3) 2_567 ? Cl2 C100 1.726(11) . ? Cl1 C100 1.641(12) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C41 C42 1.514(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.575(16) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C46 C45 1.481(13) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C43 C44 1.471(18) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C45 C44 1.484(19) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? N5 C53 1.478(9) . ? N5 C51 1.560(17) . ? C53 C54 1.509(11) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C51 C52 1.40(2) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 N6 Re1 O 106.73(19) . . ? N6 Re1 N2 102.7(2) . . ? O Re1 N2 150.47(12) . . ? N6 Re1 S2 110.80(18) . . ? O Re1 S2 87.71(4) . . ? N2 Re1 S2 80.01(13) . . ? N6 Re1 S1 110.54(18) . . ? O Re1 S1 83.98(4) . . ? N2 Re1 S1 87.62(13) . . ? S2 Re1 S1 138.50(5) . . ? C3 S2 Re1 98.82(18) . . ? C1 S1 Re1 100.00(19) . . ? C1 N1 C2 126.6(5) . . ? C2 N2 N3 113.4(4) . . ? C2 N2 Re1 126.7(3) . . ? N3 N2 Re1 119.9(3) . . ? C3 N3 N2 116.0(4) . . ? C3 N3 H3 122.0 . . ? N2 N3 H3 122.0 . . ? N2 C2 N1 126.1(4) . . ? N2 C2 C21 122.1(4) . . ? N1 C2 C21 111.7(4) . . ? C3 N4 C46 119.8(6) . . ? C3 N4 C41 122.4(5) . . ? C46 N4 C41 116.0(5) . . ? N1 C1 N5 118.7(5) . . ? N1 C1 S1 125.8(4) . . ? N5 C1 S1 115.4(4) . . ? N3 C3 N4 121.3(5) . . ? N3 C3 S2 122.6(4) . . ? N4 C3 S2 116.0(4) . . ? C22 C21 C26 119.9(5) . . ? C22 C21 C2 121.5(4) . . ? C26 C21 C2 118.2(5) . . ? C23 C22 C21 120.2(6) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C24 C25 C26 120.7(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C24 C23 119.7(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C25 C26 C21 119.1(6) . . ? C25 C26 H26 120.5 . . ? C21 C26 H26 120.5 . . ? Re1 O Re1 180.0 . 2_567 ? Cl1 C100 Cl2 118.3(7) . . ? Cl1 C100 H10A 107.7 . . ? Cl2 C100 H10A 107.7 . . ? Cl1 C100 H10B 107.7 . . ? Cl2 C100 H10B 107.7 . . ? H10A C100 H10B 107.1 . . ? N4 C41 C42 114.3(6) . . ? N4 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? N4 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C41 C42 C43 111.3(8) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? N4 C46 C45 115.4(7) . . ? N4 C46 H46A 108.4 . . ? C45 C46 H46A 108.4 . . ? N4 C46 H46B 108.4 . . ? C45 C46 H46B 108.4 . . ? H46A C46 H46B 107.5 . . ? C44 C43 C42 118.1(10) . . ? C44 C43 H43A 107.8 . . ? C42 C43 H43A 107.8 . . ? C44 C43 H43B 107.8 . . ? C42 C43 H43B 107.8 . . ? H43A C43 H43B 107.1 . . ? C46 C45 C44 118.2(8) . . ? C46 C45 H45A 107.8 . . ? C44 C45 H45A 107.8 . . ? C46 C45 H45B 107.8 . . ? C44 C45 H45B 107.8 . . ? H45A C45 H45B 107.1 . . ? C43 C44 C45 117.9(12) . . ? C43 C44 H44A 107.8 . . ? C45 C44 H44A 107.8 . . ? C43 C44 H44B 107.8 . . ? C45 C44 H44B 107.8 . . ? H44A C44 H44B 107.2 . . ? C1 N5 C53 123.0(6) . . ? C1 N5 C51 119.1(8) . . ? C53 N5 C51 117.6(9) . . ? N5 C53 C54 112.0(7) . . ? N5 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? N5 C53 H53B 109.2 . . ? C54 C53 H53B 109.2 . . ? H53A C53 H53B 107.9 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C51 N5 106.8(14) . . ? C52 C51 H51A 110.4 . . ? N5 C51 H51A 110.4 . . ? C52 C51 H51B 110.4 . . ? N5 C51 H51B 110.4 . . ? H51A C51 H51B 108.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.217 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.313 data_pireol4tu _database_code_depnum_ccdc_archive 'CCDC 911733' #TrackingRef 're_mili.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[ReO(L4)(Ph2btu)]' _chemical_melting_point ? _chemical_formula_moiety 'C39 H42 N7 O2 Re S3' _chemical_formula_sum 'C39 H42 N7 O2 Re S3' _chemical_formula_weight 923.18 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.2241(7) _cell_length_b 11.7497(8) _cell_length_c 20.5128(17) _cell_angle_alpha 93.909(6) _cell_angle_beta 99.602(7) _cell_angle_gamma 93.003(6) _cell_volume 1945.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 13623 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 29.58 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 3.328 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20481 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 29.30 _reflns_number_total 10390 _reflns_number_gt 6647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0194(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10390 _refine_ls_number_parameters 472 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 0.78256(4) 0.87013(3) 0.722993(16) 0.03648(12) Uani 1 1 d . . . S1 S 1.0563(3) 0.8779(2) 0.70330(10) 0.0500(5) Uani 1 1 d . . . S2 S 0.5339(2) 0.79603(17) 0.74716(10) 0.0441(4) Uani 1 1 d . . . S3 S 0.7204(3) 0.79850(19) 0.60833(10) 0.0524(5) Uani 1 1 d . . . O1 O 0.7327(7) 1.0051(5) 0.7138(3) 0.0558(15) Uani 1 1 d . . . O2 O 0.8324(6) 0.6868(4) 0.7298(2) 0.0381(11) Uani 1 1 d . . . N1 N 1.1323(9) 0.9425(6) 0.8353(3) 0.0506(17) Uani 1 1 d . . . N2 N 0.8564(8) 0.8700(6) 0.8230(3) 0.0431(14) Uani 1 1 d . . . N3 N 0.7434(9) 0.8308(6) 0.8643(3) 0.0484(16) Uani 1 1 d . . . N4 N 0.4779(9) 0.7632(7) 0.8685(4) 0.0540(18) Uani 1 1 d . . . N6 N 0.6361(8) 0.5890(5) 0.6472(3) 0.0418(14) Uani 1 1 d . . . N5 N 1.2831(10) 1.0304(7) 0.7673(4) 0.064(2) Uani 1 1 d . . . N7 N 0.4424(7) 0.6635(5) 0.5725(3) 0.0402(14) Uani 1 1 d . . . C1 C 1.1586(9) 0.9562(7) 0.7743(4) 0.0453(18) Uani 1 1 d . . . C2 C 1.0095(10) 0.8875(7) 0.8556(4) 0.0467(18) Uani 1 1 d . . . C3 C 0.5960(10) 0.7971(7) 0.8330(4) 0.0455(18) Uani 1 1 d . . . C6 C 0.7573(8) 0.5975(6) 0.6982(3) 0.0366(15) Uani 1 1 d . . . C7 C 0.5897(9) 0.6765(7) 0.6120(4) 0.0418(16) Uani 1 1 d . . . C21 C 1.0568(10) 0.8529(8) 0.9259(4) 0.0502(19) Uani 1 1 d . . . C22 C 1.0223(12) 0.7435(9) 0.9416(5) 0.058(2) Uani 1 1 d . . . H22 H 0.9604 0.6909 0.9099 0.069 Uiso 1 1 calc R . . C23 C 1.0796(14) 0.7116(11) 1.0043(6) 0.077(3) Uani 1 1 d . . . H23 H 1.0588 0.6369 1.0145 0.092 Uiso 1 1 calc R . . C24 C 1.1682(16) 0.7902(14) 1.0525(6) 0.086(4) Uani 1 1 d . . . H24 H 1.2055 0.7691 1.0951 0.104 Uiso 1 1 calc R . . C25 C 1.1995(15) 0.8986(12) 1.0365(5) 0.078(3) Uani 1 1 d . . . H25 H 1.2585 0.9521 1.0684 0.093 Uiso 1 1 calc R . . C26 C 1.1452(12) 0.9300(9) 0.9738(4) 0.060(2) Uani 1 1 d . . . H26 H 1.1684 1.0044 0.9636 0.072 Uiso 1 1 calc R . . C41 C 0.5194(14) 0.7651(11) 0.9409(5) 0.077(3) Uani 1 1 d . . . H41A H 0.4176 0.7712 0.9586 0.092 Uiso 1 1 calc R . . H41B H 0.5884 0.8342 0.9566 0.092 Uiso 1 1 calc R . . C42 C 0.604(2) 0.6678(15) 0.9698(6) 0.102(4) Uani 1 1 d . . . H42A H 0.5469 0.6423 1.0043 0.123 Uiso 1 1 calc R . . H42B H 0.7153 0.6951 0.9907 0.123 Uiso 1 1 calc R . . C43 C 0.6165(16) 0.5650(12) 0.9218(7) 0.089(4) Uani 1 1 d . . . H43A H 0.6856 0.5893 0.8907 0.107 Uiso 1 1 calc R . . H43B H 0.6746 0.5082 0.9471 0.107 Uiso 1 1 calc R . . C44 C 0.4594(18) 0.5061(12) 0.8819(8) 0.107(5) Uani 1 1 d . . . H44A H 0.4820 0.4289 0.8679 0.128 Uiso 1 1 calc R . . H44B H 0.3771 0.5007 0.9106 0.128 Uiso 1 1 calc R . . C45 C 0.3875(13) 0.5648(10) 0.8214(6) 0.073(3) Uani 1 1 d . . . H45A H 0.4681 0.5680 0.7919 0.088 Uiso 1 1 calc R . . H45B H 0.2909 0.5191 0.7980 0.088 Uiso 1 1 calc R . . C46 C 0.3385(11) 0.6841(9) 0.8367(5) 0.063(3) Uani 1 1 d . . . H46A H 0.2874 0.7138 0.7957 0.076 Uiso 1 1 calc R . . H46B H 0.2567 0.6808 0.8656 0.076 Uiso 1 1 calc R . . C51 C 1.3248(11) 1.0555(8) 0.7033(5) 0.058(2) Uani 1 1 d . . . H51A H 1.3042 0.9859 0.6742 0.070 Uiso 1 1 calc R . . H51B H 1.4424 1.0763 0.7096 0.070 Uiso 1 1 calc R . . C52 C 1.235(2) 1.1483(14) 0.6687(10) 0.126(6) Uani 1 1 d . . . H52A H 1.1187 1.1274 0.6597 0.190 Uiso 1 1 calc R . . H52B H 1.2740 1.1584 0.6278 0.190 Uiso 1 1 calc R . . H52C H 1.2554 1.2184 0.6965 0.190 Uiso 1 1 calc R . . C53 C 1.4021(17) 1.0808(13) 0.8292(7) 0.098(4) Uani 1 1 d . . . H53A H 1.4184 1.0241 0.8615 0.117 Uiso 1 1 calc R . . H53B H 1.5085 1.1021 0.8174 0.117 Uiso 1 1 calc R . . C54 C 1.337(3) 1.1775(15) 0.8568(11) 0.143(7) Uani 1 1 d . . . H54A H 1.3309 1.2362 0.8262 0.214 Uiso 1 1 calc R . . H54B H 1.4075 1.2052 0.8975 0.214 Uiso 1 1 calc R . . H54C H 1.2285 1.1573 0.8654 0.214 Uiso 1 1 calc R . . C61 C 0.8075(10) 0.4856(6) 0.7236(4) 0.0409(16) Uani 1 1 d . . . C62 C 0.9220(10) 0.4852(7) 0.7831(4) 0.052(2) Uani 1 1 d . . . H62 H 0.9660 0.5539 0.8060 0.062 Uiso 1 1 calc R . . C63 C 0.9688(12) 0.3829(8) 0.8074(5) 0.060(2) Uani 1 1 d . . . H63 H 1.0464 0.3832 0.8460 0.072 Uiso 1 1 calc R . . C64 C 0.9025(14) 0.2818(8) 0.7753(6) 0.070(3) Uani 1 1 d . . . H64 H 0.9327 0.2130 0.7922 0.084 Uiso 1 1 calc R . . C65 C 0.7901(15) 0.2824(8) 0.7175(6) 0.075(3) Uani 1 1 d . . . H65 H 0.7465 0.2135 0.6948 0.090 Uiso 1 1 calc R . . C66 C 0.7411(13) 0.3842(8) 0.6928(5) 0.062(2) Uani 1 1 d . . . H66 H 0.6618 0.3829 0.6547 0.074 Uiso 1 1 calc R . . C71 C 0.3295(9) 0.5659(6) 0.5738(4) 0.0403(16) Uani 1 1 d . . . C72 C 0.2698(11) 0.5447(8) 0.6315(4) 0.053(2) Uani 1 1 d . . . H72 H 0.3066 0.5914 0.6702 0.064 Uiso 1 1 calc R . . C73 C 0.1558(12) 0.4543(9) 0.6313(5) 0.060(2) Uani 1 1 d . . . H73 H 0.1162 0.4388 0.6699 0.072 Uiso 1 1 calc R . . C74 C 0.1001(11) 0.3859(8) 0.5723(6) 0.063(3) Uani 1 1 d . . . H74 H 0.0225 0.3251 0.5716 0.076 Uiso 1 1 calc R . . C75 C 0.1590(11) 0.4078(8) 0.5160(5) 0.057(2) Uani 1 1 d . . . H75 H 0.1216 0.3619 0.4770 0.069 Uiso 1 1 calc R . . C76 C 0.2744(10) 0.4982(7) 0.5164(4) 0.0469(18) Uani 1 1 d . . . H76 H 0.3145 0.5129 0.4778 0.056 Uiso 1 1 calc R . . C81 C 0.3751(10) 0.7531(6) 0.5324(4) 0.0414(16) Uani 1 1 d . . . C82 C 0.2388(13) 0.8023(8) 0.5492(5) 0.059(2) Uani 1 1 d . . . H82 H 0.1922 0.7789 0.5848 0.071 Uiso 1 1 calc R . . C83 C 0.1715(15) 0.8884(9) 0.5115(6) 0.076(3) Uani 1 1 d . . . H83 H 0.0792 0.9229 0.5222 0.091 Uiso 1 1 calc R . . C84 C 0.2384(16) 0.9220(9) 0.4599(6) 0.078(3) Uani 1 1 d . . . H84 H 0.1916 0.9792 0.4353 0.094 Uiso 1 1 calc R . . C85 C 0.3728(14) 0.8736(10) 0.4435(5) 0.071(3) Uani 1 1 d . . . H85 H 0.4186 0.8985 0.4081 0.085 Uiso 1 1 calc R . . C86 C 0.4433(12) 0.7869(8) 0.4791(4) 0.056(2) Uani 1 1 d . . . H86 H 0.5344 0.7523 0.4673 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.03908(17) 0.02905(16) 0.04090(17) 0.00626(10) 0.00581(10) -0.00295(9) S1 0.0471(11) 0.0546(12) 0.0480(11) -0.0055(9) 0.0154(8) -0.0122(9) S2 0.0418(9) 0.0361(10) 0.0549(11) 0.0083(8) 0.0095(8) -0.0029(7) S3 0.0662(13) 0.0486(12) 0.0385(10) 0.0095(9) 0.0018(9) -0.0184(10) O1 0.061(3) 0.043(3) 0.064(4) 0.016(3) 0.008(3) 0.000(3) O2 0.043(3) 0.030(3) 0.040(3) 0.002(2) 0.004(2) -0.001(2) N1 0.054(4) 0.050(4) 0.045(4) 0.002(3) 0.008(3) -0.012(3) N2 0.051(4) 0.039(4) 0.039(3) 0.003(3) 0.007(3) -0.006(3) N3 0.054(4) 0.045(4) 0.048(4) 0.004(3) 0.015(3) -0.001(3) N4 0.052(4) 0.061(5) 0.052(4) 0.006(3) 0.020(3) -0.005(3) N6 0.049(3) 0.033(3) 0.040(3) 0.002(3) 0.000(3) -0.004(3) N5 0.063(5) 0.071(5) 0.052(4) -0.003(4) 0.010(3) -0.033(4) N7 0.044(3) 0.038(3) 0.037(3) 0.008(3) 0.003(3) -0.003(3) C1 0.045(4) 0.040(4) 0.049(4) 0.005(3) 0.003(3) -0.006(3) C2 0.058(5) 0.042(4) 0.041(4) -0.001(3) 0.014(3) -0.001(3) C3 0.049(4) 0.039(4) 0.052(5) 0.003(3) 0.018(4) 0.003(3) C6 0.040(4) 0.032(4) 0.038(4) 0.001(3) 0.007(3) -0.002(3) C7 0.046(4) 0.040(4) 0.036(4) -0.001(3) 0.002(3) -0.003(3) C21 0.051(4) 0.057(5) 0.041(4) -0.004(4) 0.005(3) 0.004(4) C22 0.058(5) 0.065(6) 0.053(5) 0.012(4) 0.015(4) -0.003(4) C23 0.079(7) 0.079(8) 0.083(8) 0.034(6) 0.031(6) 0.012(6) C24 0.089(8) 0.124(12) 0.053(6) 0.025(7) 0.019(6) 0.025(8) C25 0.086(7) 0.097(9) 0.046(5) -0.009(6) 0.003(5) 0.004(6) C26 0.073(6) 0.062(6) 0.044(5) -0.006(4) 0.009(4) 0.005(5) C41 0.068(6) 0.095(9) 0.073(7) 0.006(6) 0.033(5) -0.012(6) C42 0.123(11) 0.128(13) 0.057(7) 0.025(8) 0.006(7) 0.021(9) C43 0.086(8) 0.099(10) 0.084(8) 0.038(8) 0.004(6) 0.007(7) C44 0.111(10) 0.078(9) 0.124(11) 0.041(8) -0.006(9) -0.024(8) C45 0.070(6) 0.068(7) 0.078(7) 0.023(6) 0.007(5) -0.019(5) C46 0.049(5) 0.079(7) 0.064(6) 0.014(5) 0.018(4) -0.014(4) C51 0.057(5) 0.055(5) 0.064(6) 0.011(4) 0.020(4) -0.011(4) C52 0.138(13) 0.096(11) 0.176(17) 0.065(11) 0.078(12) 0.048(10) C53 0.099(9) 0.084(9) 0.113(10) -0.004(8) 0.041(8) -0.022(7) C54 0.148(16) 0.083(11) 0.20(2) -0.003(13) 0.039(14) -0.005(11) C61 0.052(4) 0.030(4) 0.040(4) 0.005(3) 0.005(3) 0.001(3) C62 0.054(5) 0.040(4) 0.059(5) 0.007(4) 0.003(4) -0.003(4) C63 0.072(6) 0.057(6) 0.047(5) 0.010(4) -0.006(4) 0.008(4) C64 0.082(7) 0.041(5) 0.087(7) 0.021(5) 0.004(6) 0.011(5) C65 0.100(8) 0.033(5) 0.085(7) 0.005(5) -0.001(6) -0.002(5) C66 0.080(6) 0.037(5) 0.061(5) 0.005(4) -0.008(5) -0.005(4) C71 0.038(4) 0.032(4) 0.050(4) 0.008(3) 0.002(3) 0.003(3) C72 0.060(5) 0.055(5) 0.044(4) 0.005(4) 0.006(4) -0.011(4) C73 0.062(5) 0.065(6) 0.054(5) 0.012(4) 0.013(4) -0.014(4) C74 0.048(5) 0.045(5) 0.094(7) 0.016(5) 0.002(5) -0.004(4) C75 0.049(5) 0.046(5) 0.071(6) -0.010(4) -0.001(4) 0.002(4) C76 0.047(4) 0.041(4) 0.052(5) 0.000(4) 0.006(3) 0.000(3) C81 0.053(4) 0.034(4) 0.035(4) 0.005(3) 0.004(3) 0.001(3) C82 0.081(6) 0.047(5) 0.054(5) 0.012(4) 0.017(5) 0.012(4) C83 0.093(8) 0.053(6) 0.090(8) 0.025(6) 0.027(6) 0.030(5) C84 0.103(9) 0.052(6) 0.079(7) 0.029(5) 0.004(6) 0.005(6) C85 0.077(7) 0.078(7) 0.055(6) 0.020(5) 0.007(5) -0.015(6) C86 0.065(5) 0.062(6) 0.042(4) 0.016(4) 0.004(4) 0.002(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 O1 1.674(6) . ? Re1 N2 2.040(6) . ? Re1 O2 2.223(5) . ? Re1 S2 2.3226(18) . ? Re1 S1 2.351(2) . ? Re1 S3 2.405(2) . ? S1 C1 1.733(8) . ? S2 C3 1.750(9) . ? S3 C7 1.760(7) . ? O2 C6 1.267(8) . ? N1 C2 1.311(10) . ? N1 C1 1.323(10) . ? N2 C2 1.322(10) . ? N2 N3 1.437(9) . ? N3 C3 1.302(11) . ? N4 C3 1.366(10) . ? N4 C41 1.466(13) . ? N4 C46 1.470(12) . ? N6 C6 1.314(9) . ? N6 C7 1.332(10) . ? N5 C1 1.342(10) . ? N5 C51 1.456(11) . ? N5 C53 1.530(16) . ? N7 C7 1.336(9) . ? N7 C71 1.441(9) . ? N7 C81 1.454(9) . ? C2 C21 1.519(11) . ? C6 C61 1.500(10) . ? C21 C26 1.373(12) . ? C21 C22 1.374(13) . ? C22 C23 1.378(14) . ? C22 H22 0.9300 . ? C23 C24 1.388(18) . ? C23 H23 0.9300 . ? C24 C25 1.359(18) . ? C24 H24 0.9300 . ? C25 C26 1.371(14) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C41 C42 1.477(19) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.52(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.515(17) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.511(16) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.505(16) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C51 C52 1.500(17) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.41(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C61 C66 1.353(12) . ? C61 C62 1.412(11) . ? C62 C63 1.381(12) . ? C62 H62 0.9300 . ? C63 C64 1.359(14) . ? C63 H63 0.9300 . ? C64 C65 1.377(15) . ? C64 H64 0.9300 . ? C65 C66 1.384(14) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C71 C76 1.371(11) . ? C71 C72 1.389(11) . ? C72 C73 1.380(12) . ? C72 H72 0.9300 . ? C73 C74 1.402(14) . ? C73 H73 0.9300 . ? C74 C75 1.359(14) . ? C74 H74 0.9300 . ? C75 C76 1.386(12) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? C81 C82 1.371(13) . ? C81 C86 1.381(11) . ? C82 C83 1.397(13) . ? C82 H82 0.9300 . ? C83 C84 1.343(15) . ? C83 H83 0.9300 . ? C84 C85 1.350(17) . ? C84 H84 0.9300 . ? C85 C86 1.389(14) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 N2 102.7(3) . . ? O1 Re1 O2 175.8(2) . . ? N2 Re1 O2 80.5(2) . . ? O1 Re1 S2 98.6(2) . . ? N2 Re1 S2 83.03(18) . . ? O2 Re1 S2 78.97(13) . . ? O1 Re1 S1 101.7(2) . . ? N2 Re1 S1 92.47(19) . . ? O2 Re1 S1 80.77(14) . . ? S2 Re1 S1 159.71(8) . . ? O1 Re1 S3 98.4(2) . . ? N2 Re1 S3 158.9(2) . . ? O2 Re1 S3 78.43(14) . . ? S2 Re1 S3 93.82(7) . . ? S1 Re1 S3 83.25(8) . . ? C1 S1 Re1 101.4(3) . . ? C3 S2 Re1 97.2(3) . . ? C7 S3 Re1 101.6(3) . . ? C6 O2 Re1 130.8(5) . . ? C2 N1 C1 129.9(7) . . ? C2 N2 N3 112.4(6) . . ? C2 N2 Re1 126.4(5) . . ? N3 N2 Re1 120.5(5) . . ? C3 N3 N2 115.0(6) . . ? C3 N4 C41 119.5(7) . . ? C3 N4 C46 119.9(7) . . ? C41 N4 C46 116.1(7) . . ? C6 N6 C7 123.5(6) . . ? C1 N5 C51 123.5(7) . . ? C1 N5 C53 119.1(8) . . ? C51 N5 C53 117.0(7) . . ? C7 N7 C71 121.8(6) . . ? C7 N7 C81 122.6(6) . . ? C71 N7 C81 115.1(6) . . ? N1 C1 N5 117.4(7) . . ? N1 C1 S1 125.2(6) . . ? N5 C1 S1 117.1(6) . . ? N1 C2 N2 126.2(7) . . ? N1 C2 C21 112.2(7) . . ? N2 C2 C21 121.4(7) . . ? N3 C3 N4 119.3(8) . . ? N3 C3 S2 124.3(6) . . ? N4 C3 S2 116.4(6) . . ? O2 C6 N6 128.9(7) . . ? O2 C6 C61 116.4(6) . . ? N6 C6 C61 114.7(6) . . ? N6 C7 N7 116.9(6) . . ? N6 C7 S3 123.3(6) . . ? N7 C7 S3 119.4(6) . . ? C26 C21 C22 119.2(8) . . ? C26 C21 C2 119.5(8) . . ? C22 C21 C2 121.2(8) . . ? C21 C22 C23 119.9(10) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 120.5(11) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 118.8(10) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 120.8(11) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 120.8(10) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? N4 C41 C42 118.1(11) . . ? N4 C41 H41A 107.8 . . ? C42 C41 H41A 107.8 . . ? N4 C41 H41B 107.8 . . ? C42 C41 H41B 107.8 . . ? H41A C41 H41B 107.1 . . ? C41 C42 C43 116.3(10) . . ? C41 C42 H42A 108.2 . . ? C43 C42 H42A 108.2 . . ? C41 C42 H42B 108.2 . . ? C43 C42 H42B 108.2 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 119.0(14) . . ? C44 C43 H43A 107.6 . . ? C42 C43 H43A 107.6 . . ? C44 C43 H43B 107.6 . . ? C42 C43 H43B 107.6 . . ? H43A C43 H43B 107.0 . . ? C45 C44 C43 114.8(10) . . ? C45 C44 H44A 108.6 . . ? C43 C44 H44A 108.6 . . ? C45 C44 H44B 108.6 . . ? C43 C44 H44B 108.6 . . ? H44A C44 H44B 107.5 . . ? C46 C45 C44 113.9(11) . . ? C46 C45 H45A 108.8 . . ? C44 C45 H45A 108.8 . . ? C46 C45 H45B 108.8 . . ? C44 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? N4 C46 C45 113.6(8) . . ? N4 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? N4 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? N5 C51 C52 116.8(10) . . ? N5 C51 H51A 108.1 . . ? C52 C51 H51A 108.1 . . ? N5 C51 H51B 108.1 . . ? C52 C51 H51B 108.1 . . ? H51A C51 H51B 107.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N5 109.7(15) . . ? C54 C53 H53A 109.7 . . ? N5 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? N5 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C66 C61 C62 118.5(8) . . ? C66 C61 C6 122.1(7) . . ? C62 C61 C6 119.4(7) . . ? C63 C62 C61 120.2(8) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C64 C63 C62 120.5(9) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.2(9) . . ? C63 C64 H64 120.4 . . ? C65 C64 H64 120.4 . . ? C64 C65 C66 120.9(9) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C61 C66 C65 120.6(9) . . ? C61 C66 H66 119.7 . . ? C65 C66 H66 119.7 . . ? C76 C71 C72 120.4(7) . . ? C76 C71 N7 119.2(7) . . ? C72 C71 N7 120.3(7) . . ? C73 C72 C71 119.7(8) . . ? C73 C72 H72 120.1 . . ? C71 C72 H72 120.1 . . ? C72 C73 C74 119.3(8) . . ? C72 C73 H73 120.3 . . ? C74 C73 H73 120.3 . . ? C75 C74 C73 120.4(8) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 120.3(9) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C71 C76 C75 119.9(8) . . ? C71 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C82 C81 C86 120.8(8) . . ? C82 C81 N7 117.2(7) . . ? C86 C81 N7 122.0(8) . . ? C81 C82 C83 118.4(9) . . ? C81 C82 H82 120.8 . . ? C83 C82 H82 120.8 . . ? C84 C83 C82 120.8(11) . . ? C84 C83 H83 119.6 . . ? C82 C83 H83 119.6 . . ? C83 C84 C85 120.8(10) . . ? C83 C84 H84 119.6 . . ? C85 C84 H84 119.6 . . ? C84 C85 C86 120.6(9) . . ? C84 C85 H85 119.7 . . ? C86 C85 H85 119.7 . . ? C81 C86 C85 118.6(10) . . ? C81 C86 H86 120.7 . . ? C85 C86 H86 120.7 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.842 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.282 ################### END ###############