Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Alegria, A.C.B.' 'Martins, L.M.D.R.S.' 'Haukka, M.' 'Pombeiro, A.J.L.' _publ_contact_author_name 'Armando J L Pombeiro' _publ_contact_author_address ; Centro de Quinica Estructural Complexo 1 Instituto Superior Tecnico Av. Rovisco Pais 1096 Lisboa Codex Lisboa PORTUGAL ; _publ_contact_author_email POMBEIRO@IST.UTL.PT _publ_section_title ; Rhenium Complexes of Tris(Pyrazoyl)methanes and Sulfonate Derivative ; data_struct_5 _database_code_depnum_ccdc_archive 'CCDC 616743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 Cl4 N6 Re' _chemical_formula_sum 'C10 H10 Cl4 N6 Re' _chemical_formula_weight 542.24 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.6713(4) _cell_length_b 11.7518(3) _cell_length_c 11.3972(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.162(2) _cell_angle_gamma 90.00 _cell_volume 1547.39(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5648 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 8.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1509 _exptl_absorpt_correction_T_max 0.3588 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19508 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3537 _reflns_number_gt 3067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.1 (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0291P)^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 3537 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0543 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.689636(12) 0.047200(11) -0.217554(13) 0.01661(6) Uani 1 1 d . . . Cl1 Cl 0.53679(8) -0.02031(8) -0.34845(9) 0.0277(2) Uani 1 1 d . . . Cl2 Cl 0.82087(8) -0.07435(8) -0.29403(8) 0.0212(2) Uani 1 1 d . . . Cl3 Cl 0.73123(9) 0.19030(7) -0.34530(9) 0.0298(2) Uani 1 1 d . . . Cl4 Cl 0.56898(8) 0.16504(8) -0.12507(9) 0.0275(2) Uani 1 1 d . . . N1 N 0.8279(3) 0.0983(2) -0.0871(3) 0.0179(6) Uani 1 1 d . . . N2 N 0.8385(3) 0.0734(2) 0.0306(3) 0.0181(7) Uani 1 1 d . . . N3 N 0.6647(3) -0.0850(2) -0.0980(3) 0.0188(7) Uani 1 1 d . . . N4 N 0.7098(3) -0.0868(2) 0.0194(3) 0.0177(6) Uani 1 1 d . . . N5 N 0.7772(3) 0.0002(3) 0.2044(3) 0.0210(7) Uani 1 1 d . . . N6 N 0.8696(3) -0.0703(3) 0.2429(3) 0.0292(8) Uani 1 1 d . . . C1 C 0.9252(3) 0.1542(3) -0.1023(4) 0.0235(8) Uani 1 1 d . . . H1 H 0.9424 0.1816 -0.1762 0.028 Uiso 1 1 calc R . . C2 C 0.9969(3) 0.1661(3) 0.0052(4) 0.0266(9) Uani 1 1 d . . . H2 H 1.0704 0.2024 0.0186 0.032 Uiso 1 1 calc R . . C3 C 0.9393(3) 0.1145(3) 0.0883(4) 0.0239(9) Uani 1 1 d . . . H3 H 0.9656 0.1088 0.1709 0.029 Uiso 1 1 calc R . . C4 C 0.7435(3) 0.0197(3) 0.0817(3) 0.0193(8) Uani 1 1 d . . . H4 H 0.6755 0.0725 0.0716 0.023 Uiso 1 1 calc R . . C5 C 0.6288(3) -0.1912(3) -0.1252(4) 0.0236(9) Uani 1 1 d . . . H5 H 0.5941 -0.2154 -0.2015 0.028 Uiso 1 1 calc R . . C6 C 0.6494(3) -0.2607(3) -0.0264(4) 0.0267(9) Uani 1 1 d . . . H6 H 0.6322 -0.3395 -0.0220 0.032 Uiso 1 1 calc R . . C7 C 0.7003(3) -0.1919(3) 0.0640(4) 0.0225(8) Uani 1 1 d . . . H7 H 0.7243 -0.2145 0.1437 0.027 Uiso 1 1 calc R . . C8 C 0.8860(4) -0.0557(3) 0.3582(4) 0.0308(10) Uani 1 1 d . . . H8 H 0.9442 -0.0942 0.4102 0.037 Uiso 1 1 calc R . . C9 C 0.8083(4) 0.0230(3) 0.3968(4) 0.0331(10) Uani 1 1 d . . . H9 H 0.8040 0.0468 0.4757 0.040 Uiso 1 1 calc R . . C10 C 0.7408(4) 0.0576(3) 0.2958(4) 0.0245(9) Uani 1 1 d . . . H10 H 0.6798 0.1116 0.2902 0.029 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 0.01917(10) 0.01607(8) 0.01443(10) 0.00062(5) 0.00188(6) 0.00136(5) Cl1 0.0242(5) 0.0356(5) 0.0213(5) -0.0020(4) -0.0039(4) 0.0010(4) Cl2 0.0211(5) 0.0228(4) 0.0196(5) -0.0044(4) 0.0025(4) 0.0019(3) Cl3 0.0494(6) 0.0191(4) 0.0223(5) 0.0049(4) 0.0097(5) -0.0009(4) Cl4 0.0287(5) 0.0313(5) 0.0226(5) -0.0010(4) 0.0042(4) 0.0133(4) N1 0.0192(16) 0.0189(14) 0.0163(17) -0.0025(13) 0.0044(13) 0.0004(12) N2 0.0194(16) 0.0183(14) 0.0163(17) -0.0001(12) 0.0017(13) 0.0033(12) N3 0.0187(16) 0.0221(14) 0.0153(17) 0.0016(13) 0.0017(13) -0.0005(12) N4 0.0193(16) 0.0176(14) 0.0162(17) 0.0018(13) 0.0023(13) -0.0010(12) N5 0.0228(16) 0.0249(16) 0.0153(17) -0.0012(14) 0.0022(13) 0.0070(14) N6 0.030(2) 0.0327(17) 0.022(2) 0.0034(15) -0.0054(16) 0.0084(15) C1 0.024(2) 0.0180(17) 0.030(2) -0.0033(16) 0.0093(17) -0.0010(15) C2 0.0186(19) 0.0232(19) 0.038(3) -0.0085(19) 0.0034(18) -0.0019(16) C3 0.021(2) 0.0231(18) 0.026(2) -0.0079(16) -0.0039(17) 0.0016(15) C4 0.0185(19) 0.0215(17) 0.017(2) -0.0006(15) 0.0004(16) 0.0016(14) C5 0.024(2) 0.0215(18) 0.026(2) -0.0070(16) 0.0055(17) -0.0071(15) C6 0.032(2) 0.0174(17) 0.033(3) 0.0009(16) 0.0104(19) -0.0030(15) C7 0.026(2) 0.0201(17) 0.023(2) 0.0052(16) 0.0088(17) 0.0015(15) C8 0.037(3) 0.030(2) 0.023(2) 0.0041(17) -0.005(2) 0.0018(17) C9 0.053(3) 0.033(2) 0.014(2) 0.0016(17) 0.007(2) -0.007(2) C10 0.030(2) 0.0238(19) 0.023(2) -0.0004(16) 0.0133(18) -0.0014(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N3 2.113(3) . ? Re1 N1 2.119(3) . ? Re1 Cl1 2.2982(9) . ? Re1 Cl3 2.3204(9) . ? Re1 Cl4 2.3310(9) . ? Re1 Cl2 2.3506(9) . ? N1 C1 1.344(5) . ? N1 N2 1.362(4) . ? N2 C3 1.353(4) . ? N2 C4 1.467(5) . ? N3 C5 1.338(4) . ? N3 N4 1.367(4) . ? N4 C7 1.346(4) . ? N4 C4 1.466(5) . ? N5 C10 1.358(5) . ? N5 N6 1.380(5) . ? N5 C4 1.417(5) . ? N6 C8 1.312(6) . ? C1 C2 1.390(6) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 1.0000 . ? C5 C6 1.384(6) . ? C5 H5 0.9500 . ? C6 C7 1.377(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.409(6) . ? C8 H8 0.9500 . ? C9 C10 1.361(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? 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 N3 Re1 N1 85.24(11) . . ? N3 Re1 Cl1 89.96(8) . . ? N1 Re1 Cl1 175.20(8) . . ? N3 Re1 Cl3 175.89(8) . . ? N1 Re1 Cl3 91.64(9) . . ? Cl1 Re1 Cl3 93.16(4) . . ? N3 Re1 Cl4 89.87(9) . . ? N1 Re1 Cl4 87.90(8) . . ? Cl1 Re1 Cl4 92.04(4) . . ? Cl3 Re1 Cl4 92.68(4) . . ? N3 Re1 Cl2 87.09(9) . . ? N1 Re1 Cl2 87.76(8) . . ? Cl1 Re1 Cl2 92.07(3) . . ? Cl3 Re1 Cl2 90.14(3) . . ? Cl4 Re1 Cl2 174.89(3) . . ? C1 N1 N2 105.7(3) . . ? C1 N1 Re1 128.4(3) . . ? N2 N1 Re1 125.8(2) . . ? C3 N2 N1 110.8(3) . . ? C3 N2 C4 127.9(3) . . ? N1 N2 C4 121.0(3) . . ? C5 N3 N4 106.0(3) . . ? C5 N3 Re1 127.1(3) . . ? N4 N3 Re1 125.0(2) . . ? C7 N4 N3 110.1(3) . . ? C7 N4 C4 129.2(3) . . ? N3 N4 C4 120.0(3) . . ? C10 N5 N6 111.7(3) . . ? C10 N5 C4 127.1(3) . . ? N6 N5 C4 120.4(3) . . ? C8 N6 N5 103.7(3) . . ? N1 C1 C2 110.5(4) . . ? N1 C1 H1 124.8 . . ? C2 C1 H1 124.8 . . ? C3 C2 C1 105.7(3) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? N2 C3 C2 107.3(3) . . ? N2 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? N5 C4 N4 110.9(3) . . ? N5 C4 N2 110.0(3) . . ? N4 C4 N2 109.9(3) . . ? N5 C4 H4 108.6 . . ? N4 C4 H4 108.6 . . ? N2 C4 H4 108.6 . . ? N3 C5 C6 110.5(3) . . ? N3 C5 H5 124.7 . . ? C6 C5 H5 124.7 . . ? C7 C6 C5 105.6(3) . . ? C7 C6 H6 127.2 . . ? C5 C6 H6 127.2 . . ? N4 C7 C6 107.8(3) . . ? N4 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? N6 C8 C9 112.9(4) . . ? N6 C8 H8 123.5 . . ? C9 C8 H8 123.5 . . ? C10 C9 C8 104.6(4) . . ? C10 C9 H9 127.7 . . ? C8 C9 H9 127.7 . . ? N5 C10 C9 107.1(4) . . ? N5 C10 H10 126.4 . . ? C9 C10 H10 126.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.029 _refine_diff_density_min -1.614 _refine_diff_density_rms 0.169 #===END======================================================================== data_struct_6 _database_code_depnum_ccdc_archive 'CCDC 616744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 N8 O5 Re S, O4 Re' _chemical_formula_sum 'C16 H18 N8 O9 Re2 S' _chemical_formula_weight 870.84 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/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.500(3) _cell_length_b 12.532(3) _cell_length_c 15.166(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.36(3) _cell_angle_gamma 90.00 _cell_volume 2337.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 70279 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description purple _exptl_crystal_colour block _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 10.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2403 _exptl_absorpt_correction_T_max 0.4322 _exptl_absorpt_process_details 'SADABS v.2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28197 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4091 _reflns_number_gt 2978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg, 1998-2003)' _computing_data_reduction 'EvalCCD (Duisenberg, 1998-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0291P)^2^+62.7509P] 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 4091 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.20010(5) 0.11197(5) 0.21489(3) 0.03922(18) Uani 1 1 d . . . S1 S 0.2016(3) -0.1870(3) 0.4490(2) 0.0455(9) Uani 1 1 d . . . O1 O 0.3118(9) -0.2240(8) 0.4677(6) 0.047(3) Uani 1 1 d . . . N1 N 0.2990(9) 0.0835(9) 0.3412(7) 0.038(3) Uani 1 1 d . . . C1 C 0.3764(12) 0.1405(13) 0.3871(9) 0.045(4) Uani 1 1 d . . . H1 H 0.4082 0.2008 0.3639 0.054 Uiso 1 1 calc R . . Re2 Re 0.38912(5) 0.43505(5) 0.22905(4) 0.0470(2) Uani 1 1 d . . . O2 O 0.1654(9) -0.1279(9) 0.5195(6) 0.054(3) Uani 1 1 d . . . N2 N 0.2792(10) 0.0036(10) 0.3951(7) 0.042(3) Uani 1 1 d . . . C2 C 0.4078(14) 0.1020(13) 0.4756(11) 0.056(4) Uani 1 1 d . . . H2 H 0.4606 0.1310 0.5224 0.067 Uiso 1 1 calc R . . O3 O 0.1252(9) -0.2612(9) 0.4014(7) 0.055(3) Uani 1 1 d . . . N3 N 0.0771(9) 0.0391(10) 0.2671(7) 0.042(3) Uani 1 1 d . . . C3 C 0.3467(13) 0.0166(14) 0.4781(9) 0.051(4) Uani 1 1 d . . . H3 H 0.3484 -0.0289 0.5285 0.062 Uiso 1 1 calc R . . O4 O 0.2918(9) 0.3774(10) 0.1490(7) 0.059(3) Uani 1 1 d . . . N4 N 0.0949(10) -0.0346(10) 0.3336(7) 0.043(3) Uani 1 1 d . . . C4 C -0.0252(12) 0.0644(14) 0.2548(9) 0.051(4) Uani 1 1 d . . . H4 H -0.0598 0.1129 0.2105 0.061 Uiso 1 1 calc R . . O5 O 0.4863(17) 0.486(2) 0.1807(8) 0.180(13) Uani 1 1 d . . . N5 N 0.2467(9) -0.0613(9) 0.2118(6) 0.036(3) Uani 1 1 d . . . C5 C -0.0767(14) 0.0114(15) 0.3147(10) 0.058(4) Uani 1 1 d . . . H5 H -0.1508 0.0170 0.3209 0.069 Uiso 1 1 calc R . . O6 O 0.3306(14) 0.5315(13) 0.2782(13) 0.134(8) Uani 1 1 d . . . N6 N 0.2385(8) -0.1253(8) 0.2823(6) 0.031(2) Uani 1 1 d . . . C6 C 0.0038(12) -0.0525(14) 0.3644(10) 0.050(4) Uani 1 1 d . . . H6 H -0.0051 -0.0999 0.4114 0.060 Uiso 1 1 calc R . . O7 O 0.4440(11) 0.3493(12) 0.3109(11) 0.088(4) Uani 1 1 d . . . N7 N 0.3160(9) 0.1290(10) 0.1377(7) 0.042(3) Uani 1 1 d . . . C7 C 0.2869(11) -0.1181(12) 0.1540(9) 0.040(3) Uani 1 1 d . . . H7 H 0.3027 -0.0922 0.0989 0.048 Uiso 1 1 calc R . . N8 N 0.2797(10) 0.1254(11) 0.0501(8) 0.046(3) Uani 1 1 d . . . C8 C 0.3036(11) -0.2232(12) 0.1848(9) 0.041(3) Uani 1 1 d . . . H8 H 0.3301 -0.2816 0.1551 0.049 Uiso 1 1 calc R . . O9 O 0.1187(8) 0.0922(9) 0.0966(6) 0.050(3) Uani 1 1 d . . . C9 C 0.2735(11) -0.2234(12) 0.2669(8) 0.040(3) Uani 1 1 d . . . H9 H 0.2768 -0.2828 0.3062 0.048 Uiso 1 1 calc R . . C10 C 0.2048(11) -0.0797(11) 0.3607(8) 0.035(3) Uani 1 1 d . . . C11 C 0.4226(11) 0.1364(12) 0.1481(10) 0.045(4) Uani 1 1 d . . . H11 H 0.4702 0.1418 0.2043 0.054 Uiso 1 1 calc R . . C12 C 0.4551(13) 0.1351(13) 0.0676(11) 0.053(4) Uani 1 1 d . . . H12 H 0.5276 0.1387 0.0569 0.064 Uiso 1 1 calc R . . C13 C 0.3645(13) 0.1279(14) 0.0065(10) 0.054(4) Uani 1 1 d . . . H13 H 0.3603 0.1250 -0.0566 0.065 Uiso 1 1 calc R . . C14 C 0.1610(12) 0.1249(14) 0.0210(9) 0.050(4) Uani 1 1 d . . . C15 C 0.1285(16) 0.0450(17) -0.0545(12) 0.072(5) Uani 1 1 d . . . H15A H 0.1441 -0.0275 -0.0315 0.109 Uiso 1 1 calc R . . H15B H 0.1700 0.0592 -0.1023 0.109 Uiso 1 1 calc R . . H15C H 0.0506 0.0519 -0.0783 0.109 Uiso 1 1 calc R . . C16 C 0.1189(15) 0.2351(14) -0.0096(11) 0.060(4) Uani 1 1 d . . . H16A H 0.0408 0.2310 -0.0336 0.090 Uiso 1 1 calc R . . H16B H 0.1573 0.2609 -0.0563 0.090 Uiso 1 1 calc R . . H16C H 0.1314 0.2843 0.0414 0.090 Uiso 1 1 calc R . . O8 O 0.1769(8) 0.2329(9) 0.2481(6) 0.053(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 0.0449(3) 0.0484(4) 0.0286(3) 0.0085(2) 0.0178(2) 0.0057(3) S1 0.069(3) 0.047(2) 0.0261(17) 0.0039(15) 0.0217(16) 0.0014(19) O1 0.068(7) 0.051(7) 0.023(4) 0.003(4) 0.010(4) 0.007(5) N1 0.050(7) 0.032(7) 0.039(6) -0.007(5) 0.022(5) -0.001(5) C1 0.047(8) 0.048(9) 0.038(8) -0.004(7) 0.002(6) -0.001(7) Re2 0.0617(4) 0.0438(4) 0.0381(3) 0.0029(3) 0.0159(3) -0.0158(3) O2 0.078(8) 0.062(7) 0.028(5) 0.008(5) 0.023(5) 0.013(6) N2 0.055(7) 0.047(8) 0.027(6) 0.000(5) 0.013(5) -0.002(6) C2 0.070(11) 0.044(10) 0.052(9) -0.017(8) 0.004(8) -0.014(9) O3 0.076(8) 0.050(7) 0.045(6) 0.002(5) 0.030(5) -0.003(6) N3 0.044(7) 0.057(8) 0.031(6) 0.006(5) 0.019(5) 0.004(6) C3 0.067(10) 0.059(11) 0.027(7) -0.008(7) 0.005(7) 0.007(9) O4 0.060(7) 0.071(8) 0.055(6) -0.026(6) 0.030(5) -0.018(6) N4 0.056(7) 0.051(8) 0.029(6) 0.011(5) 0.024(5) 0.000(6) C4 0.044(9) 0.079(12) 0.032(7) -0.001(7) 0.014(6) 0.003(8) O5 0.174(17) 0.33(3) 0.024(6) 0.028(11) -0.011(8) -0.18(2) N5 0.042(6) 0.049(7) 0.017(5) -0.006(5) 0.008(4) -0.003(5) C5 0.055(10) 0.077(13) 0.047(9) 0.005(8) 0.026(7) 0.005(9) O6 0.126(14) 0.084(11) 0.155(16) -0.074(11) -0.078(12) 0.052(10) N6 0.043(6) 0.030(6) 0.021(5) 0.001(4) 0.009(4) -0.003(5) C6 0.045(8) 0.069(11) 0.039(8) 0.004(7) 0.017(7) 0.003(8) O7 0.065(8) 0.083(10) 0.118(12) 0.023(9) 0.020(8) -0.005(7) N7 0.047(7) 0.049(8) 0.034(6) 0.007(5) 0.016(5) 0.006(6) C7 0.047(8) 0.050(9) 0.026(6) -0.008(6) 0.013(6) 0.002(7) N8 0.053(7) 0.054(8) 0.037(7) 0.004(6) 0.022(5) -0.002(6) C8 0.043(8) 0.049(9) 0.033(7) -0.007(6) 0.012(6) -0.004(7) O9 0.058(6) 0.072(8) 0.022(5) 0.014(5) 0.014(4) 0.002(5) C9 0.052(8) 0.045(9) 0.020(6) -0.002(6) 0.002(6) -0.006(7) C10 0.039(7) 0.043(8) 0.026(6) 0.001(6) 0.012(5) 0.007(6) C11 0.040(8) 0.047(9) 0.050(9) 0.009(7) 0.017(6) 0.005(7) C12 0.049(9) 0.055(11) 0.062(10) 0.015(8) 0.027(8) 0.015(8) C13 0.061(10) 0.076(12) 0.032(8) 0.018(7) 0.025(7) 0.007(9) C14 0.049(9) 0.070(11) 0.031(7) 0.009(7) 0.006(6) 0.006(8) C15 0.075(12) 0.088(15) 0.058(11) 0.003(10) 0.021(9) -0.021(11) C16 0.073(11) 0.063(12) 0.047(9) 0.016(8) 0.018(8) 0.006(9) O8 0.060(6) 0.071(8) 0.037(5) 0.017(5) 0.029(5) 0.020(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 O8 1.639(11) . ? Re1 O9 1.912(9) . ? Re1 N7 2.031(11) . ? Re1 N3 2.064(11) . ? Re1 N1 2.115(12) . ? Re1 N5 2.250(12) . ? S1 O3 1.432(12) . ? S1 O1 1.432(11) . ? S1 O2 1.438(10) . ? S1 C10 1.904(13) . ? N1 C1 1.300(18) . ? N1 N2 1.344(16) . ? C1 C2 1.41(2) . ? C1 H1 0.9500 . ? Re2 O5 1.654(15) . ? Re2 O6 1.657(15) . ? Re2 O7 1.691(15) . ? Re2 O4 1.716(11) . ? N2 C3 1.393(18) . ? N2 C10 1.432(18) . ? C2 C3 1.32(2) . ? C2 H2 0.9500 . ? N3 C4 1.299(18) . ? N3 N4 1.357(16) . ? C3 H3 0.9500 . ? N4 C6 1.325(18) . ? N4 C10 1.474(17) . ? C4 C5 1.38(2) . ? C4 H4 0.9500 . ? N5 C7 1.299(16) . ? N5 N6 1.356(14) . ? C5 C6 1.40(2) . ? C5 H5 0.9500 . ? N6 C9 1.339(18) . ? N6 C10 1.449(15) . ? C6 H6 0.9500 . ? N7 C11 1.317(18) . ? N7 N8 1.325(16) . ? C7 C8 1.40(2) . ? C7 H7 0.9500 . ? N8 C13 1.347(18) . ? N8 C14 1.470(19) . ? C8 C9 1.363(18) . ? C8 H8 0.9500 . ? O9 C14 1.408(17) . ? C9 H9 0.9500 . ? C11 C12 1.35(2) . ? C11 H11 0.9500 . ? C12 C13 1.33(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.52(2) . ? C14 C16 1.52(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 O8 Re1 O9 108.3(5) . . ? O8 Re1 N7 105.3(5) . . ? O9 Re1 N7 77.8(4) . . ? O8 Re1 N3 96.1(5) . . ? O9 Re1 N3 89.7(4) . . ? N7 Re1 N3 157.7(5) . . ? O8 Re1 N1 89.1(5) . . ? O9 Re1 N1 162.4(4) . . ? N7 Re1 N1 100.2(4) . . ? N3 Re1 N1 86.1(4) . . ? O8 Re1 N5 163.6(4) . . ? O9 Re1 N5 87.2(4) . . ? N7 Re1 N5 82.8(4) . . ? N3 Re1 N5 78.1(4) . . ? N1 Re1 N5 75.2(4) . . ? O3 S1 O1 114.8(7) . . ? O3 S1 O2 116.0(7) . . ? O1 S1 O2 116.1(6) . . ? O3 S1 C10 101.5(6) . . ? O1 S1 C10 103.1(6) . . ? O2 S1 C10 102.0(6) . . ? C1 N1 N2 106.5(12) . . ? C1 N1 Re1 130.5(10) . . ? N2 N1 Re1 122.4(9) . . ? N1 C1 C2 112.0(14) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? O5 Re2 O6 109.8(13) . . ? O5 Re2 O7 109.6(9) . . ? O6 Re2 O7 106.7(9) . . ? O5 Re2 O4 109.4(6) . . ? O6 Re2 O4 108.1(6) . . ? O7 Re2 O4 113.3(7) . . ? N1 N2 C3 108.4(12) . . ? N1 N2 C10 120.0(11) . . ? C3 N2 C10 131.5(12) . . ? C3 C2 C1 103.9(14) . . ? C3 C2 H2 128.1 . . ? C1 C2 H2 128.1 . . ? C4 N3 N4 107.4(11) . . ? C4 N3 Re1 128.2(10) . . ? N4 N3 Re1 123.6(9) . . ? C2 C3 N2 109.2(14) . . ? C2 C3 H3 125.4 . . ? N2 C3 H3 125.4 . . ? C6 N4 N3 109.9(12) . . ? C6 N4 C10 130.9(12) . . ? N3 N4 C10 119.2(10) . . ? N3 C4 C5 110.7(15) . . ? N3 C4 H4 124.7 . . ? C5 C4 H4 124.7 . . ? C7 N5 N6 107.5(11) . . ? C7 N5 Re1 132.5(10) . . ? N6 N5 Re1 119.9(7) . . ? C4 C5 C6 104.8(14) . . ? C4 C5 H5 127.6 . . ? C6 C5 H5 127.6 . . ? C9 N6 N5 109.4(10) . . ? C9 N6 C10 131.2(11) . . ? N5 N6 C10 119.2(10) . . ? N4 C6 C5 107.2(13) . . ? N4 C6 H6 126.4 . . ? C5 C6 H6 126.4 . . ? C11 N7 N8 106.2(11) . . ? C11 N7 Re1 138.6(10) . . ? N8 N7 Re1 115.0(9) . . ? N5 C7 C8 110.1(12) . . ? N5 C7 H7 125.0 . . ? C8 C7 H7 125.0 . . ? N7 N8 C13 109.5(12) . . ? N7 N8 C14 116.5(10) . . ? C13 N8 C14 133.9(12) . . ? C9 C8 C7 104.9(13) . . ? C9 C8 H8 127.5 . . ? C7 C8 H8 127.5 . . ? C14 O9 Re1 120.7(9) . . ? N6 C9 C8 108.1(13) . . ? N6 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? N2 C10 N6 108.8(10) . . ? N2 C10 N4 109.5(11) . . ? N6 C10 N4 108.5(10) . . ? N2 C10 S1 110.6(9) . . ? N6 C10 S1 110.1(9) . . ? N4 C10 S1 109.3(8) . . ? N7 C11 C12 110.7(14) . . ? N7 C11 H11 124.7 . . ? C12 C11 H11 124.7 . . ? C13 C12 C11 105.8(14) . . ? C13 C12 H12 127.1 . . ? C11 C12 H12 127.1 . . ? C12 C13 N8 107.9(13) . . ? C12 C13 H13 126.1 . . ? N8 C13 H13 126.1 . . ? O9 C14 N8 105.3(11) . . ? O9 C14 C15 109.5(14) . . ? N8 C14 C15 110.4(13) . . ? O9 C14 C16 110.7(13) . . ? N8 C14 C16 111.3(14) . . ? C15 C14 C16 109.7(13) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.727 _refine_diff_density_min -1.979 _refine_diff_density_rms 0.253