Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Rhenium (V) Oxocomplexes with Novel Pyrazolyl-Based N4- and N3S-Donor Chelators ; _publ_contact_author_name 'Isabel Santos' _publ_contact_author_email ISANTOS@ITN.PT loop_ _publ_author_name 'Isabel Santos' 'Leonor Maria' 'Carolina Moura' 'Antonio Paulo' 'Isabel Santos' 'Rute F. Vitor' # Attachment 'renios-11-131.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 616646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H25 N5 O2 Re, C24 H20 B' _chemical_formula_sum 'C36 H45 B N5 O2 Re' _chemical_formula_weight 776.78 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.101(2) _cell_length_b 14.3993(15) _cell_length_c 19.975(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.285(13) _cell_angle_gamma 90.00 _cell_volume 3459.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 12 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 3.551 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4155 _exptl_absorpt_correction_T_max 0.4155 _exptl_absorpt_process_details 'North A.C.T.,Phillips D.C.,Mathews F.S.(1968) Acta.Cryst.A24,351' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 CAD4 _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 6 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 7102 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.1187 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.04 _reflns_number_total 6767 _reflns_number_gt 3812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3(Farrugia,1997 _computing_publication_material 'WinGX (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^)+(0.0310P)^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 6767 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.004 _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 Re1 Re 0.53494(3) 0.13521(3) 0.92000(2) 0.03868(13) Uani 1 1 d . . . O1 O 0.4830(6) 0.1038(4) 0.9929(3) 0.0530(19) Uani 1 1 d . . . O2 O 0.5339(6) 0.1640(4) 0.8246(3) 0.0502(19) Uani 1 1 d . . . N1 N 0.5468(7) 0.2784(5) 0.9365(4) 0.043(2) Uani 1 1 d . . . N2 N 0.6391(8) 0.3159(6) 0.9717(4) 0.053(3) Uani 1 1 d . . . N3 N 0.6933(7) 0.1258(6) 0.9361(4) 0.053(2) Uani 1 1 d . . . N4 N 0.5477(7) -0.0033(5) 0.8886(4) 0.048(2) Uani 1 1 d . . . H4 H 0.5447 -0.0396 0.9257 0.057 Uiso 1 1 calc R . . N5 N 0.3561(6) 0.1072(5) 0.8729(4) 0.055(2) Uani 1 1 d . . . H5A H 0.3067 0.1275 0.9001 0.066 Uiso 1 1 calc R . . H5B H 0.3427 0.1358 0.8328 0.066 Uiso 1 1 calc R . . C1 C 0.7206(9) 0.2581(8) 1.0094(6) 0.069(4) Uani 1 1 d . . . H1A H 0.6851 0.2234 1.0428 0.083 Uiso 1 1 calc R . . H1B H 0.7773 0.2972 1.0331 0.083 Uiso 1 1 calc R . . C2 C 0.7747(10) 0.1911(8) 0.9650(7) 0.080(4) Uani 1 1 d . . . H2A H 0.8059 0.2249 0.9295 0.096 Uiso 1 1 calc R . . H2B H 0.8346 0.1584 0.9914 0.096 Uiso 1 1 calc R . . C3 C 0.7383(9) 0.0348(8) 0.9175(6) 0.066(4) Uani 1 1 d . . . H3A H 0.7523 -0.0033 0.9576 0.079 Uiso 1 1 calc R . . H3B H 0.8087 0.0444 0.8995 0.079 Uiso 1 1 calc R . . C4 C 0.6604(9) -0.0158(8) 0.8662(5) 0.055(3) Uani 1 1 d . . . H4A H 0.6632 0.0104 0.8217 0.066 Uiso 1 1 calc R . . H4B H 0.6795 -0.0812 0.8650 0.066 Uiso 1 1 calc R . . C5 C 0.4536(9) -0.0309(7) 0.8391(6) 0.062(3) Uani 1 1 d . . . H5C H 0.4505 -0.0979 0.8347 0.074 Uiso 1 1 calc R . . H5D H 0.4622 -0.0043 0.7953 0.074 Uiso 1 1 calc R . . C6 C 0.3489(9) 0.0053(7) 0.8648(6) 0.062(3) Uani 1 1 d . . . H6A H 0.2850 -0.0105 0.8333 0.075 Uiso 1 1 calc R . . H6B H 0.3396 -0.0234 0.9078 0.075 Uiso 1 1 calc R . . C7 C 0.6144(10) 0.2183(8) 0.7964(5) 0.081(4) Uani 1 1 d . . . H7A H 0.6038 0.2129 0.7482 0.121 Uiso 1 1 calc R . . H7B H 0.6874 0.1968 0.8129 0.121 Uiso 1 1 calc R . . H7C H 0.6065 0.2821 0.8090 0.121 Uiso 1 1 calc R . . C8 C 0.3812(9) 0.3394(7) 0.8689(6) 0.071(4) Uani 1 1 d . . . H8A H 0.3337 0.3005 0.8923 0.106 Uiso 1 1 calc R . . H8B H 0.3934 0.3108 0.8269 0.106 Uiso 1 1 calc R . . H8C H 0.3465 0.3988 0.8604 0.106 Uiso 1 1 calc R . . C9 C 0.7274(11) 0.4693(8) 1.0021(7) 0.094(5) Uani 1 1 d . . . H9A H 0.7699 0.4344 1.0369 0.141 Uiso 1 1 calc R . . H9B H 0.6939 0.5217 1.0216 0.141 Uiso 1 1 calc R . . H9C H 0.7756 0.4905 0.9701 0.141 Uiso 1 1 calc R . . C11 C 0.4878(8) 0.3517(7) 0.9101(5) 0.049(3) Uani 1 1 d . . . C12 C 0.5424(11) 0.4324(7) 0.9279(6) 0.056(3) Uani 1 1 d . . . H12 H 0.5188 0.4921 0.9156 0.067 Uiso 1 1 calc R . . C13 C 0.6390(10) 0.4090(8) 0.9673(5) 0.054(3) Uani 1 1 d . . . C21 C 0.5791(9) 0.6746(6) 0.8132(5) 0.046(3) Uani 1 1 d . . . C22 C 0.5559(9) 0.7110(7) 0.8751(5) 0.047(3) Uani 1 1 d . . . H22 H 0.4829 0.7271 0.8805 0.056 Uiso 1 1 calc R . . C23 C 0.6375(11) 0.7239(7) 0.9287(6) 0.071(4) Uani 1 1 d . . . H23 H 0.6189 0.7504 0.9684 0.085 Uiso 1 1 calc R . . C24 C 0.7437(10) 0.6983(8) 0.9239(6) 0.069(4) Uani 1 1 d . . . H24 H 0.7978 0.7073 0.9602 0.082 Uiso 1 1 calc R . . C25 C 0.7715(10) 0.6592(9) 0.8656(6) 0.078(4) Uani 1 1 d . . . H25 H 0.8439 0.6394 0.8623 0.094 Uiso 1 1 calc R . . C26 C 0.6901(9) 0.6496(8) 0.8116(5) 0.061(3) Uani 1 1 d . . . H26 H 0.7108 0.6250 0.7718 0.073 Uiso 1 1 calc R . . C31 C 0.5010(8) 0.5817(8) 0.6990(5) 0.048(3) Uani 1 1 d . . . C32 C 0.5462(10) 0.4981(8) 0.7215(6) 0.067(4) Uani 1 1 d . . . H32 H 0.5752 0.4934 0.7664 0.080 Uiso 1 1 calc R . . C33 C 0.5509(12) 0.4201(8) 0.6807(8) 0.090(5) Uani 1 1 d . . . H33 H 0.5846 0.3659 0.6981 0.108 Uiso 1 1 calc R . . C34 C 0.5052(13) 0.4237(11) 0.6141(7) 0.091(5) Uani 1 1 d . . . H34 H 0.5061 0.3719 0.5864 0.110 Uiso 1 1 calc R . . C35 C 0.4595(10) 0.5037(11) 0.5906(6) 0.074(4) Uani 1 1 d . . . H35 H 0.4270 0.5066 0.5462 0.088 Uiso 1 1 calc R . . C36 C 0.4593(9) 0.5827(8) 0.6310(6) 0.062(3) Uani 1 1 d . . . H36 H 0.4306 0.6378 0.6120 0.074 Uiso 1 1 calc R . . C41 C 0.3623(9) 0.6710(8) 0.7702(5) 0.052(3) Uani 1 1 d . . . C42 C 0.3144(10) 0.5879(9) 0.7874(6) 0.064(3) Uani 1 1 d . . . H42 H 0.3546 0.5336 0.7829 0.077 Uiso 1 1 calc R . . C43 C 0.2115(11) 0.5800(11) 0.8105(6) 0.084(5) Uani 1 1 d . . . H43 H 0.1825 0.5223 0.8199 0.101 Uiso 1 1 calc R . . C44 C 0.1530(11) 0.6608(12) 0.8193(6) 0.086(5) Uani 1 1 d . . . H44 H 0.0839 0.6574 0.8353 0.104 Uiso 1 1 calc R . . C45 C 0.1939(10) 0.7427(11) 0.8051(6) 0.078(4) Uani 1 1 d . . . H45 H 0.1543 0.7967 0.8117 0.094 Uiso 1 1 calc R . . C46 C 0.2993(9) 0.7477(8) 0.7796(5) 0.060(3) Uani 1 1 d . . . H46 H 0.3263 0.8057 0.7689 0.072 Uiso 1 1 calc R . . C51 C 0.5066(9) 0.7696(7) 0.7034(5) 0.046(3) Uani 1 1 d . . . C52 C 0.6033(9) 0.8219(7) 0.7103(6) 0.054(3) Uani 1 1 d . . . H52 H 0.6604 0.8043 0.7429 0.065 Uiso 1 1 calc R . . C53 C 0.6193(11) 0.8998(8) 0.6707(7) 0.073(4) Uani 1 1 d . . . H53 H 0.6852 0.9334 0.6776 0.087 Uiso 1 1 calc R . . C54 C 0.5363(13) 0.9266(8) 0.6212(6) 0.078(4) Uani 1 1 d . . . H54 H 0.5456 0.9781 0.5943 0.093 Uiso 1 1 calc R . . C55 C 0.4414(11) 0.8763(9) 0.6128(7) 0.082(4) Uani 1 1 d . . . H55 H 0.3855 0.8927 0.5792 0.098 Uiso 1 1 calc R . . C56 C 0.4267(10) 0.8015(8) 0.6532(6) 0.069(4) Uani 1 1 d . . . H56 H 0.3592 0.7700 0.6468 0.083 Uiso 1 1 calc R . . B1 B 0.4875(10) 0.6746(8) 0.7464(6) 0.045(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0393(2) 0.0371(2) 0.0393(2) 0.0026(3) 0.00291(15) 0.0017(3) O1 0.068(5) 0.039(4) 0.056(4) 0.000(3) 0.023(4) -0.003(4) O2 0.055(5) 0.059(5) 0.037(4) 0.011(3) 0.009(3) 0.004(4) N1 0.047(6) 0.038(5) 0.041(6) 0.001(4) -0.010(5) -0.005(4) N2 0.071(7) 0.040(6) 0.047(6) -0.004(5) 0.000(5) -0.003(6) N3 0.045(5) 0.052(6) 0.058(5) 0.000(5) -0.007(4) 0.015(5) N4 0.052(6) 0.046(5) 0.046(5) 0.003(4) 0.008(5) 0.005(5) N5 0.043(5) 0.048(6) 0.072(6) -0.001(5) 0.000(5) -0.003(4) C1 0.051(8) 0.075(9) 0.068(9) 0.002(7) -0.044(7) -0.008(7) C2 0.052(8) 0.066(9) 0.113(11) -0.020(8) -0.029(8) 0.009(7) C3 0.051(8) 0.064(8) 0.085(10) 0.019(7) 0.018(7) 0.016(7) C4 0.056(8) 0.064(8) 0.046(7) -0.007(6) 0.008(6) 0.017(6) C5 0.070(9) 0.039(6) 0.073(8) -0.009(6) -0.007(7) -0.001(6) C6 0.057(8) 0.054(7) 0.071(8) -0.005(6) -0.011(7) -0.004(6) C7 0.101(11) 0.089(10) 0.057(8) 0.029(7) 0.031(8) -0.007(8) C8 0.072(9) 0.035(7) 0.099(10) 0.006(6) -0.015(8) 0.012(6) C9 0.122(13) 0.060(9) 0.099(11) -0.014(8) 0.004(10) -0.022(9) C11 0.048(6) 0.041(7) 0.054(7) -0.006(6) -0.009(5) 0.001(6) C12 0.078(9) 0.032(6) 0.057(7) 0.000(6) 0.002(7) -0.003(7) C13 0.068(9) 0.053(7) 0.040(7) -0.009(6) 0.002(6) 0.004(7) C21 0.059(7) 0.038(6) 0.042(6) 0.004(5) 0.016(6) 0.004(5) C22 0.037(6) 0.061(7) 0.040(6) 0.000(5) -0.006(5) 0.012(5) C23 0.091(11) 0.057(8) 0.062(8) -0.014(6) -0.006(8) 0.027(7) C24 0.062(9) 0.077(9) 0.061(9) 0.027(7) -0.023(7) 0.004(7) C25 0.059(8) 0.114(12) 0.063(8) 0.018(8) 0.019(7) 0.019(8) C26 0.061(8) 0.073(9) 0.049(7) 0.005(7) 0.004(6) 0.016(7) C31 0.035(6) 0.064(7) 0.046(7) 0.005(6) 0.007(5) -0.005(6) C32 0.084(10) 0.050(7) 0.063(8) 0.011(7) -0.011(7) 0.000(7) C33 0.126(13) 0.033(7) 0.114(13) 0.008(8) 0.033(11) -0.003(8) C34 0.111(13) 0.105(13) 0.059(9) -0.022(9) 0.018(9) -0.047(11) C35 0.048(8) 0.112(11) 0.062(9) -0.004(10) 0.009(6) -0.014(9) C36 0.049(7) 0.067(8) 0.070(8) -0.011(7) 0.009(6) -0.004(6) C41 0.046(7) 0.064(7) 0.046(7) 0.001(6) 0.000(5) -0.009(6) C42 0.051(8) 0.069(8) 0.070(9) 0.007(7) 0.001(7) -0.004(7) C43 0.060(10) 0.124(13) 0.066(9) 0.029(9) -0.006(7) -0.028(9) C44 0.056(9) 0.162(18) 0.041(7) 0.014(9) 0.006(6) 0.001(10) C45 0.043(8) 0.139(14) 0.053(8) -0.014(9) 0.004(6) 0.004(9) C46 0.053(8) 0.074(8) 0.051(7) 0.002(6) 0.001(6) -0.004(7) C51 0.048(7) 0.041(6) 0.049(7) -0.009(5) 0.005(6) 0.010(5) C52 0.047(7) 0.044(6) 0.073(8) -0.005(6) 0.014(6) 0.003(6) C53 0.073(9) 0.055(8) 0.093(11) -0.005(7) 0.022(8) -0.017(7) C54 0.109(12) 0.053(8) 0.070(9) 0.010(7) 0.007(9) 0.019(8) C55 0.078(10) 0.070(10) 0.091(10) 0.001(8) -0.015(8) 0.002(9) C56 0.056(8) 0.065(9) 0.087(10) 0.011(7) 0.010(7) -0.001(7) B1 0.045(8) 0.046(7) 0.046(7) -0.002(6) 0.011(6) -0.011(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 Re1 O1 1.708(6) . ? Re1 N3 1.913(8) . ? Re1 O2 1.948(6) . ? Re1 N1 2.090(8) . ? Re1 N4 2.101(8) . ? Re1 N5 2.299(8) . ? O2 C7 1.413(11) . ? N1 C11 1.349(11) . ? N1 N2 1.364(11) . ? N2 C13 1.343(12) . ? N2 C1 1.439(12) . ? N3 C2 1.437(12) . ? N3 C3 1.482(12) . ? N4 C5 1.479(12) . ? N4 C4 1.492(12) . ? N5 C6 1.478(11) . ? C1 C2 1.508(15) . ? C3 C4 1.503(14) . ? C5 C6 1.511(14) . ? C8 C11 1.464(13) . ? C9 C13 1.489(15) . ? C11 C12 1.365(13) . ? C12 C13 1.378(15) . ? C21 C26 1.394(14) . ? C21 C22 1.400(13) . ? C21 B1 1.639(15) . ? C22 C23 1.388(14) . ? C23 C24 1.350(15) . ? C24 C25 1.369(15) . ? C25 C26 1.386(14) . ? C31 C32 1.376(13) . ? C31 C36 1.398(14) . ? C31 B1 1.656(15) . ? C32 C33 1.392(15) . ? C33 C34 1.385(17) . ? C34 C35 1.340(17) . ? C35 C36 1.394(15) . ? C41 C46 1.367(14) . ? C41 C42 1.389(14) . ? C41 B1 1.639(15) . ? C42 C43 1.379(15) . ? C43 C44 1.383(17) . ? C44 C45 1.322(16) . ? C45 C46 1.425(15) . ? C51 C52 1.386(13) . ? C51 C56 1.392(14) . ? C51 B1 1.645(15) . ? C52 C53 1.399(14) . ? C53 C54 1.386(16) . ? C54 C55 1.352(16) . ? C55 C56 1.370(15) . ? 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 N3 107.1(3) . . ? O1 Re1 O2 157.8(3) . . ? N3 Re1 O2 94.5(3) . . ? O1 Re1 N1 98.7(3) . . ? N3 Re1 N1 89.6(4) . . ? O2 Re1 N1 86.4(3) . . ? O1 Re1 N4 92.8(3) . . ? N3 Re1 N4 83.0(3) . . ? O2 Re1 N4 84.4(3) . . ? N1 Re1 N4 167.7(3) . . ? O1 Re1 N5 83.4(3) . . ? N3 Re1 N5 159.6(3) . . ? O2 Re1 N5 74.5(3) . . ? N1 Re1 N5 106.4(3) . . ? N4 Re1 N5 78.9(3) . . ? C7 O2 Re1 125.2(6) . . ? C11 N1 N2 105.1(8) . . ? C11 N1 Re1 133.3(7) . . ? N2 N1 Re1 120.7(7) . . ? C13 N2 N1 111.5(10) . . ? C13 N2 C1 127.4(11) . . ? N1 N2 C1 121.1(9) . . ? C2 N3 C3 115.1(9) . . ? C2 N3 Re1 130.7(7) . . ? C3 N3 Re1 114.2(7) . . ? C5 N4 C4 115.4(8) . . ? C5 N4 Re1 112.2(6) . . ? C4 N4 Re1 107.7(6) . . ? C6 N5 Re1 105.1(6) . . ? N2 C1 C2 112.3(10) . . ? N3 C2 C1 109.4(10) . . ? N3 C3 C4 112.3(9) . . ? N4 C4 C3 105.2(8) . . ? N4 C5 C6 107.0(9) . . ? N5 C6 C5 109.7(9) . . ? N1 C11 C12 110.1(9) . . ? N1 C11 C8 121.4(9) . . ? C12 C11 C8 128.4(10) . . ? C11 C12 C13 107.2(10) . . ? N2 C13 C12 106.0(11) . . ? N2 C13 C9 123.7(12) . . ? C12 C13 C9 130.2(12) . . ? C26 C21 C22 113.8(10) . . ? C26 C21 B1 123.3(9) . . ? C22 C21 B1 122.5(9) . . ? C23 C22 C21 122.5(10) . . ? C24 C23 C22 120.8(12) . . ? C23 C24 C25 119.8(12) . . ? C24 C25 C26 118.9(12) . . ? C25 C26 C21 124.1(11) . . ? C32 C31 C36 114.4(11) . . ? C32 C31 B1 125.5(10) . . ? C36 C31 B1 120.0(10) . . ? C31 C32 C33 123.8(12) . . ? C34 C33 C32 119.6(13) . . ? C35 C34 C33 118.4(14) . . ? C34 C35 C36 121.6(13) . . ? C35 C36 C31 122.1(12) . . ? C46 C41 C42 114.1(10) . . ? C46 C41 B1 124.2(10) . . ? C42 C41 B1 121.5(10) . . ? C43 C42 C41 124.7(13) . . ? C42 C43 C44 117.9(14) . . ? C45 C44 C43 121.0(14) . . ? C44 C45 C46 119.4(14) . . ? C41 C46 C45 122.9(12) . . ? C52 C51 C56 113.9(10) . . ? C52 C51 B1 124.4(10) . . ? C56 C51 B1 121.6(10) . . ? C51 C52 C53 123.1(12) . . ? C54 C53 C52 119.6(12) . . ? C55 C54 C53 118.6(12) . . ? C54 C55 C56 120.8(12) . . ? C55 C56 C51 124.0(12) . . ? C41 B1 C21 109.1(9) . . ? C41 B1 C51 111.4(9) . . ? C21 B1 C51 107.7(8) . . ? C41 B1 C31 107.0(8) . . ? C21 B1 C31 111.4(9) . . ? C51 B1 C31 110.3(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.192 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.169 #===END data_13 _database_code_depnum_ccdc_archive 'CCDC 616647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H15 N4 O4 Re S, C11 H15 N4 O3 Re S' _chemical_formula_sum 'C22 H30 N8 O7 Re2 S2' _chemical_formula_weight 955.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4388(2) _cell_length_b 10.3213(3) _cell_length_c 14.9377(3) _cell_angle_alpha 89.0390(10) _cell_angle_beta 80.1750(10) _cell_angle_gamma 89.2970(10) _cell_volume 1433.63(6) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour carmine _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 8.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2769 _exptl_absorpt_correction_T_max 0.5449 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS APEX- CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17158 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 38.88 _reflns_number_total 12499 _reflns_number_gt 9566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART, (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART, (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT, (Bruker, 2004)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3(Farrugia,1997) _computing_publication_material 'WinGX (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^)+(0.0562P)^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 12499 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.308716(19) 0.772502(17) 0.408333(12) 0.01249(5) Uani 1 1 d . . . S1 S 0.53351(14) 0.68191(13) 0.37764(9) 0.0201(2) Uani 1 1 d . . . O1 O 0.2129(4) 0.7540(4) 0.3236(2) 0.0216(8) Uani 1 1 d . . . N1 N 0.2426(4) 0.6084(4) 0.4904(3) 0.0147(7) Uani 1 1 d . . . N2 N 0.1700(4) 0.6101(4) 0.5781(3) 0.0138(7) Uani 1 1 d . . . N3 N 0.2108(4) 0.8851(4) 0.5081(3) 0.0151(7) Uani 1 1 d . . . N4 N 0.4187(5) 0.9349(4) 0.3820(3) 0.0172(8) Uani 1 1 d . . . C1 C 0.2346(5) 0.4844(5) 0.4629(4) 0.0171(9) Uani 1 1 d . . . C2 C 0.1579(5) 0.4108(5) 0.5327(4) 0.0181(9) Uani 1 1 d . . . H2 H 0.1372 0.3231 0.5309 0.022 Uiso 1 1 calc R . . C3 C 0.1186(5) 0.4907(5) 0.6044(4) 0.0171(9) Uani 1 1 d . . . C4 C 0.3030(6) 0.4395(5) 0.3711(4) 0.0241(11) Uani 1 1 d . . . H4A H 0.2905 0.5047 0.3264 0.036 Uiso 1 1 calc R . . H4B H 0.2589 0.3605 0.3575 0.036 Uiso 1 1 calc R . . H4C H 0.4038 0.4245 0.3702 0.036 Uiso 1 1 calc R . . C5 C 0.0436(6) 0.4605(6) 0.6992(4) 0.0234(11) Uani 1 1 d . . . H5A H -0.0147 0.5334 0.7223 0.035 Uiso 1 1 calc R . . H5B H 0.1138 0.4427 0.7374 0.035 Uiso 1 1 calc R . . H5C H -0.0163 0.3861 0.6985 0.035 Uiso 1 1 calc R . . C6 C 0.1674(5) 0.7258(5) 0.6329(3) 0.0170(9) Uani 1 1 d . . . H6A H 0.2642 0.7435 0.6428 0.020 Uiso 1 1 calc R . . H6B H 0.1084 0.7098 0.6918 0.020 Uiso 1 1 calc R . . C7 C 0.1091(5) 0.8434(5) 0.5887(3) 0.0155(9) Uani 1 1 d . . . H7A H 0.0178 0.8224 0.5712 0.019 Uiso 1 1 calc R . . H7B H 0.0928 0.9135 0.6318 0.019 Uiso 1 1 calc R . . C8 C 0.2256(6) 1.0176(5) 0.4962(3) 0.0171(9) Uani 1 1 d . . . C9 C 0.3446(6) 1.0536(5) 0.4193(4) 0.0186(9) Uani 1 1 d . . . H9A H 0.3048 1.0999 0.3721 0.022 Uiso 1 1 calc R . . H9B H 0.4123 1.1099 0.4412 0.022 Uiso 1 1 calc R . . C10 C 0.5580(6) 0.9440(5) 0.3378(3) 0.0190(9) Uani 1 1 d . . . C11 C 0.6343(6) 0.8159(6) 0.3163(4) 0.0229(11) Uani 1 1 d . . . H11A H 0.7291 0.8189 0.3329 0.028 Uiso 1 1 calc R . . H11B H 0.6462 0.8011 0.2515 0.028 Uiso 1 1 calc R . . O2 O 0.1521(4) 1.0990(4) 0.5415(3) 0.0239(8) Uani 1 1 d . . . O3 O 0.6192(4) 1.0483(4) 0.3169(3) 0.0237(8) Uani 1 1 d . . . Re2 Re 0.190071(17) 0.175582(17) 0.149195(11) 0.00981(4) Uani 1 1 d . . . S2 S -0.03322(12) 0.23782(12) 0.11395(8) 0.0151(2) Uani 1 1 d . . . O4 O 0.1608(3) 0.1898(4) 0.2629(2) 0.0153(6) Uani 1 1 d . . . O5 O 0.2519(4) 0.1917(3) -0.0067(2) 0.0146(6) Uani 1 1 d . . . N6 N 0.1214(4) -0.0024(4) 0.1292(3) 0.0122(7) Uani 1 1 d . . . N7 N 0.3802(4) 0.0755(4) 0.1265(3) 0.0108(6) Uani 1 1 d . . . N8 N 0.4405(4) 0.3636(4) 0.1496(3) 0.0141(7) Uani 1 1 d . . . N9 N 0.3026(4) 0.3557(4) 0.1299(3) 0.0123(7) Uani 1 1 d . . . C12 C -0.1177(5) 0.0779(5) 0.1256(3) 0.0168(9) Uani 1 1 d . . . H12A H -0.1814 0.0727 0.1838 0.020 Uiso 1 1 calc R . . H12B H -0.1760 0.0695 0.0785 0.020 Uiso 1 1 calc R . . C13 C -0.0127(5) -0.0344(5) 0.1192(3) 0.0145(8) Uani 1 1 d . . . C14 C 0.2260(5) -0.1085(5) 0.1219(3) 0.0132(8) Uani 1 1 d . . . H14A H 0.2212 -0.1581 0.0679 0.016 Uiso 1 1 calc R . . H14B H 0.2042 -0.1659 0.1744 0.016 Uiso 1 1 calc R . . C15 C 0.3779(5) -0.0530(4) 0.1165(3) 0.0117(7) Uani 1 1 d . . . C16 C 0.5230(5) 0.1344(5) 0.1239(3) 0.0133(8) Uani 1 1 d . . . H16A H 0.5620 0.1613 0.0621 0.016 Uiso 1 1 calc R . . H16B H 0.5884 0.0709 0.1435 0.016 Uiso 1 1 calc R . . C17 C 0.5100(5) 0.2512(5) 0.1859(3) 0.0151(8) Uani 1 1 d . . . H17A H 0.4550 0.2269 0.2446 0.018 Uiso 1 1 calc R . . H17B H 0.6053 0.2755 0.1952 0.018 Uiso 1 1 calc R . . C18 C 0.4926(5) 0.4842(5) 0.1355(3) 0.0157(9) Uani 1 1 d . . . C19 C 0.3865(6) 0.5588(5) 0.1036(4) 0.0190(9) Uani 1 1 d . . . H19 H 0.3917 0.6463 0.0876 0.023 Uiso 1 1 calc R . . C20 C 0.2718(5) 0.4770(5) 0.1004(3) 0.0165(9) Uani 1 1 d . . . C21 C 0.1330(5) 0.5088(5) 0.0687(4) 0.0208(10) Uani 1 1 d . . . H21A H 0.0789 0.4309 0.0671 0.031 Uiso 1 1 calc R . . H21B H 0.1528 0.5470 0.0089 0.031 Uiso 1 1 calc R . . H21C H 0.0783 0.5687 0.1097 0.031 Uiso 1 1 calc R . . C22 C 0.6377(6) 0.5230(5) 0.1537(4) 0.0214(10) Uani 1 1 d . . . H22A H 0.7073 0.4574 0.1317 0.032 Uiso 1 1 calc R . . H22B H 0.6338 0.5328 0.2178 0.032 Uiso 1 1 calc R . . H22C H 0.6647 0.6038 0.1230 0.032 Uiso 1 1 calc R . . O6 O -0.0493(4) -0.1460(4) 0.1079(3) 0.0206(7) Uani 1 1 d . . . O7 O 0.4850(3) -0.1270(3) 0.1038(2) 0.0150(6) 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 0.01536(8) 0.01129(8) 0.01144(8) -0.00046(6) -0.00392(6) -0.00201(6) S1 0.0178(5) 0.0176(6) 0.0242(6) -0.0023(5) -0.0010(5) 0.0009(4) O1 0.028(2) 0.0235(19) 0.0151(16) 0.0009(14) -0.0088(14) -0.0054(16) N1 0.0182(18) 0.0110(17) 0.0148(17) -0.0012(14) -0.0025(14) -0.0013(14) N2 0.0172(18) 0.0102(17) 0.0133(16) -0.0003(13) -0.0001(14) -0.0018(14) N3 0.0170(18) 0.0095(17) 0.0196(19) -0.0023(14) -0.0054(15) 0.0024(14) N4 0.022(2) 0.0157(19) 0.0142(17) 0.0039(15) -0.0033(15) -0.0074(16) C1 0.018(2) 0.013(2) 0.022(2) -0.0037(17) -0.0090(18) 0.0027(16) C2 0.019(2) 0.010(2) 0.026(2) -0.0002(18) -0.0074(19) -0.0003(16) C3 0.017(2) 0.013(2) 0.023(2) 0.0041(17) -0.0079(18) -0.0017(16) C4 0.032(3) 0.014(2) 0.027(3) -0.011(2) -0.008(2) 0.000(2) C5 0.022(2) 0.025(3) 0.023(2) 0.005(2) -0.005(2) -0.009(2) C6 0.020(2) 0.015(2) 0.016(2) 0.0005(17) -0.0030(17) -0.0049(17) C7 0.016(2) 0.013(2) 0.0150(19) 0.0000(16) 0.0039(16) 0.0031(16) C8 0.023(2) 0.010(2) 0.020(2) 0.0036(17) -0.0096(18) -0.0002(17) C9 0.023(2) 0.0081(19) 0.026(2) 0.0049(17) -0.0064(19) -0.0044(17) C10 0.019(2) 0.024(3) 0.015(2) 0.0027(18) -0.0055(17) -0.0041(19) C11 0.021(2) 0.026(3) 0.020(2) -0.006(2) -0.0004(19) -0.002(2) O2 0.028(2) 0.0121(17) 0.031(2) -0.0042(15) -0.0026(17) 0.0027(14) O3 0.0230(19) 0.023(2) 0.0258(19) 0.0051(16) -0.0065(15) -0.0110(15) Re2 0.00709(7) 0.01197(8) 0.01043(7) -0.00062(6) -0.00176(5) 0.00154(5) S2 0.0092(4) 0.0204(6) 0.0159(5) -0.0001(4) -0.0028(4) 0.0046(4) O4 0.0107(14) 0.0205(17) 0.0143(15) 0.0003(13) -0.0013(12) 0.0010(12) O5 0.0130(14) 0.0206(17) 0.0106(14) -0.0021(12) -0.0031(11) -0.0005(12) N7 0.0070(14) 0.0096(16) 0.0161(17) 0.0003(13) -0.0031(13) 0.0027(12) N6 0.0079(15) 0.0147(18) 0.0136(16) 0.0007(14) -0.0010(13) 0.0007(13) N8 0.0121(16) 0.0167(19) 0.0137(17) -0.0024(14) -0.0025(13) 0.0007(14) N9 0.0107(15) 0.0141(18) 0.0131(16) -0.0002(14) -0.0052(13) -0.0010(13) C12 0.0077(17) 0.026(3) 0.017(2) 0.0005(18) -0.0034(15) -0.0015(17) C13 0.0097(17) 0.023(2) 0.0112(18) 0.0013(17) -0.0027(14) -0.0017(16) C15 0.0135(18) 0.0132(19) 0.0080(16) -0.0003(14) -0.0009(14) 0.0012(15) C14 0.0091(17) 0.014(2) 0.016(2) -0.0012(16) -0.0029(15) 0.0017(15) C16 0.0110(18) 0.014(2) 0.0154(19) 0.0003(16) -0.0047(15) 0.0010(15) C17 0.0125(19) 0.018(2) 0.015(2) -0.0013(17) -0.0039(16) -0.0010(16) C18 0.020(2) 0.0111(19) 0.0135(19) -0.0014(16) 0.0036(16) -0.0040(16) C19 0.021(2) 0.012(2) 0.023(2) -0.0001(18) -0.0019(19) 0.0049(17) C20 0.021(2) 0.014(2) 0.014(2) 0.0003(16) -0.0030(17) 0.0069(17) C21 0.019(2) 0.020(2) 0.025(2) 0.005(2) -0.0074(19) 0.0000(18) C22 0.020(2) 0.020(2) 0.024(2) -0.003(2) -0.0030(19) -0.0052(19) O6 0.0171(16) 0.0195(18) 0.0277(19) -0.0032(15) -0.0099(14) -0.0043(14) O7 0.0102(14) 0.0148(16) 0.0194(16) -0.0018(13) -0.0011(12) 0.0034(12) _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 1.690(4) . ? Re1 N4 1.981(4) . ? Re1 N3 1.997(4) . ? Re1 N1 2.111(4) . ? Re1 S1 2.2847(13) . ? S1 C11 1.830(6) . ? N1 C1 1.358(6) . ? N1 N2 1.371(5) . ? N2 C3 1.357(6) . ? N2 C6 1.456(6) . ? N3 C8 1.381(6) . ? N3 C7 1.468(6) . ? N4 C10 1.370(7) . ? N4 C9 1.473(7) . ? C1 C2 1.385(7) . ? C1 C4 1.491(7) . ? C2 C3 1.360(7) . ? C2 H2 0.9300 . ? C3 C5 1.501(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.515(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O2 1.221(6) . ? C8 C9 1.509(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O3 1.238(7) . ? C10 C11 1.511(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? Re2 O4 1.682(3) . ? Re2 N6 1.999(4) . ? Re2 N7 2.040(3) . ? Re2 N9 2.143(4) . ? Re2 O5 2.306(3) . ? Re2 S2 2.3379(11) . ? S2 C12 1.835(5) . ? N6 C13 1.345(6) . ? N6 C14 1.458(6) . ? N7 C15 1.338(6) . ? N7 C16 1.479(6) . ? N8 C18 1.344(6) . ? N8 N9 1.387(5) . ? N8 C17 1.467(6) . ? N9 C20 1.364(6) . ? C12 C13 1.509(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O6 1.229(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 O7 1.249(5) . ? C15 C14 1.540(6) . ? C16 C17 1.523(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.398(7) . ? C18 C22 1.501(7) . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 C21 1.499(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 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 N4 107.04(18) . . ? O1 Re1 N3 113.44(18) . . ? N4 Re1 N3 78.93(18) . . ? O1 Re1 N1 100.74(18) . . ? N4 Re1 N1 152.19(17) . . ? N3 Re1 N1 88.98(16) . . ? O1 Re1 S1 113.18(14) . . ? N4 Re1 S1 82.15(14) . . ? N3 Re1 S1 132.98(12) . . ? N1 Re1 S1 88.27(12) . . ? C11 S1 Re1 100.59(18) . . ? C1 N1 N2 105.4(4) . . ? C1 N1 Re1 127.3(3) . . ? N2 N1 Re1 125.9(3) . . ? C3 N2 N1 110.6(4) . . ? C3 N2 C6 128.2(4) . . ? N1 N2 C6 120.9(4) . . ? C8 N3 C7 115.3(4) . . ? C8 N3 Re1 117.6(3) . . ? C7 N3 Re1 126.7(3) . . ? C10 N4 C9 118.5(4) . . ? C10 N4 Re1 125.8(4) . . ? C9 N4 Re1 115.6(3) . . ? N1 C1 C2 109.6(4) . . ? N1 C1 C4 123.0(5) . . ? C2 C1 C4 127.4(5) . . ? C3 C2 C1 107.2(4) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? N2 C3 C2 107.2(5) . . ? N2 C3 C5 122.7(5) . . ? C2 C3 C5 130.0(5) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 112.4(4) . . ? N2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C6 110.4(4) . . ? N3 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? N3 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? O2 C8 N3 125.2(5) . . ? O2 C8 C9 122.2(5) . . ? N3 C8 C9 112.5(4) . . ? N4 C9 C8 109.3(4) . . ? N4 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N4 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? O3 C10 N4 123.6(5) . . ? O3 C10 C11 121.5(5) . . ? N4 C10 C11 115.0(5) . . ? C10 C11 S1 111.3(4) . . ? C10 C11 H11A 109.4 . . ? S1 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? S1 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O4 Re2 N6 104.11(17) . . ? O4 Re2 N7 101.95(16) . . ? N6 Re2 N7 79.22(15) . . ? O4 Re2 N9 92.24(16) . . ? N6 Re2 N9 162.16(15) . . ? N7 Re2 N9 90.58(15) . . ? O4 Re2 O5 169.48(15) . . ? N6 Re2 O5 86.31(14) . . ? N7 Re2 O5 78.30(14) . . ? N9 Re2 O5 77.25(14) . . ? O4 Re2 S2 101.63(11) . . ? N6 Re2 S2 83.05(11) . . ? N7 Re2 S2 153.31(11) . . ? N9 Re2 S2 100.84(11) . . ? O5 Re2 S2 80.80(9) . . ? C12 S2 Re2 97.90(15) . . ? C15 N7 C16 116.6(4) . . ? C15 N7 Re2 118.9(3) . . ? C16 N7 Re2 124.5(3) . . ? C13 N6 C14 115.9(4) . . ? C13 N6 Re2 126.3(3) . . ? C14 N6 Re2 117.8(3) . . ? C18 N8 N9 111.5(4) . . ? C18 N8 C17 127.3(4) . . ? N9 N8 C17 121.1(4) . . ? C20 N9 N8 105.1(4) . . ? C20 N9 Re2 135.1(3) . . ? N8 N9 Re2 119.8(3) . . ? C13 C12 S2 114.3(3) . . ? C13 C12 H12A 108.7 . . ? S2 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? S2 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? O6 C13 N6 123.5(5) . . ? O6 C13 C12 121.9(4) . . ? N6 C13 C12 114.6(4) . . ? O7 C15 N7 126.1(4) . . ? O7 C15 C14 119.9(4) . . ? N7 C15 C14 114.0(4) . . ? N6 C14 C15 109.4(4) . . ? N6 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N6 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N7 C16 C17 110.0(4) . . ? N7 C16 H16A 109.7 . . ? C17 C16 H16A 109.7 . . ? N7 C16 H16B 109.7 . . ? C17 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? N8 C17 C16 113.2(4) . . ? N8 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? N8 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? N8 C18 C19 106.7(4) . . ? N8 C18 C22 123.6(5) . . ? C19 C18 C22 129.7(5) . . ? C20 C19 C18 106.7(4) . . ? C20 C19 H19 126.6 . . ? C18 C19 H19 126.6 . . ? N9 C20 C19 109.9(4) . . ? N9 C20 C21 122.2(5) . . ? C19 C20 C21 127.9(5) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.755 _diffrn_reflns_theta_full 38.88 _diffrn_measured_fraction_theta_full 0.755 _refine_diff_density_max 3.082 _refine_diff_density_min -2.636 _refine_diff_density_rms 0.301