#Supplementary Material (ESI) for Dalton Transaction #This journal is (c) The Royal Society of Chemistry 2001 data_first_block _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, structure and hydroformylation activity of monomer rhodium and iridium pyrimidine thiolate complexes. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Rojas, S.' ; Instituto de Catalisis y Petroleoquimica, CSIC Campus UAM Cantoblanco 28049 Madrid Spain ; 'Garcia Fierro, J. L.' ; Instituto de Catalisis y Petroleoquimica, CSIC Campus UAM Cantoblanco 28049 Madrid Spain ; 'Fandos, R.' ; Universidad de Castilla-La Mancha Departamento de Quimica Inorganica, Organica y Bioquimica Facultad de Ciencias del Medio Ambiente Toledo Spain ; 'Rodriguez, A.' ; Universidad de Castilla-La Mancha Departamento de Quimica Inorganica, Organica y Bioquimica Escuela Tecnica Superior de Ingenieros Industriales Campus de Ciudad Real 13071 Ciudad Real Spain ; 'Terreros, P.' ; Instituto de Catalisis y Petroleoquimica, CSIC Campus UAM Cantoblanco 28049 Madrid Spain ; _publ_contact_author_name 'Dr Pilar Terreros' _publ_contact_author_address ; Dr Pilar Terreros Instituto de Catalisis y Petroleoquimica CSIC Campus UAM Cantoblanco 28049 Madrid SPAIN ; _publ_contact_author_email 'PTERREROS@ICP.CSIC.ES' #=========================================================================== #========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #========================================================================== data_Ir1A _database_code_CSD 160865 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H20 Cl Ir N2 S' _chemical_formula_weight 476.03 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ir' 'Ir' -1.4442 7.9887 '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 7.539(8) _cell_length_b 8.272(4) _cell_length_c 12.473(2) _cell_angle_alpha 81.78(3) _cell_angle_beta 82.77(5) _cell_angle_gamma 88.05(8) _cell_volume 763.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 9.042 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four circle diffractometer Nonius-Mach3' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3675 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3675 _reflns_number_observed 3272 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w==1/[\s^2^(Fo^2^)+(0.0972P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3675 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_obs 0.0253 _refine_ls_wR_factor_all 0.0857 _refine_ls_wR_factor_obs 0.0740 _refine_ls_goodness_of_fit_all 0.718 _refine_ls_goodness_of_fit_obs 0.659 _refine_ls_restrained_S_all 0.718 _refine_ls_restrained_S_obs 0.659 _refine_ls_shift/esd_max -0.279 _refine_ls_shift/esd_mean 0.014 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ir1 Ir 0.08507(2) 0.19437(2) 0.217273(13) 0.03402(8) Uani 1 d . . H1 H 0.2120(84) -0.0428(69) 0.0431(50) 0.035(15) Uiso 1 d . . Cl2 Cl 0.0515(2) -0.0870(2) 0.20390(11) 0.0442(3) Uani 1 d . . S3 S 0.1909(2) 0.28908(15) 0.03518(11) 0.0415(3) Uani 1 d . . N4 N 0.3680(6) 0.2129(5) -0.1448(3) 0.0400(9) Uani 1 d . . N5 N 0.2707(6) -0.0116(5) -0.0182(4) 0.0383(9) Uani 1 d . . C1 C 0.2813(6) 0.1517(6) -0.0485(4) 0.0349(9) Uani 1 d . . C2 C 0.4378(7) 0.1059(7) -0.2118(4) 0.0427(11) Uani 1 d . . C3 C 0.4303(7) -0.0606(7) -0.1812(4) 0.0426(11) Uani 1 d . . H3 H 0.4857 -0.1309 -0.2275 0.051 Uiso 1 calc . . C4 C 0.3409(7) -0.1219(6) -0.0822(5) 0.0409(11) Uani 1 d . . C5 C 0.3187(8) -0.2968(7) -0.0393(5) 0.0493(13) Uani 1 d . . H5A H 0.2517 -0.3076 0.0320 0.074 Uiso 1 calc . . H5B H 0.4341 -0.3482 -0.0348 0.074 Uiso 1 calc . . H5C H 0.2558 -0.3482 -0.0872 0.074 Uiso 1 calc . . C6 C 0.5246(9) 0.1817(9) -0.3212(5) 0.058(2) Uani 1 d . . H6A H 0.5154 0.2985 -0.3263 0.087 Uiso 1 calc . . H6B H 0.4657 0.1461 -0.3774 0.087 Uiso 1 calc . . H6C H 0.6484 0.1490 -0.3300 0.087 Uiso 1 calc . . C7 C 0.1945(10) 0.4071(7) 0.2578(5) 0.057(2) Uani 1 d . . H7 H 0.2914 0.4553 0.2042 0.069 Uiso 1 calc . . C8 C 0.0171(11) 0.4421(7) 0.2267(5) 0.057(2) Uani 1 d . . H8 H 0.0156 0.5097 0.1556 0.069 Uiso 1 calc . . C9 C -0.1441(12) 0.4640(10) 0.3062(7) 0.076(2) Uani 1 d . . H9A H -0.1216 0.5511 0.3470 0.091 Uiso 1 calc . . H9B H -0.2436 0.4991 0.2656 0.091 Uiso 1 calc . . C10 C -0.1982(14) 0.3169(12) 0.3849(7) 0.087(3) Uani 1 d . . H10A H -0.3249 0.3002 0.3848 0.105 Uiso 1 calc . . H10B H -0.1804 0.3370 0.4575 0.105 Uiso 1 calc . . C11 C -0.0979(9) 0.1633(8) 0.3615(5) 0.0530(14) Uani 1 d . . H11 H -0.1742 0.0680 0.3681 0.064 Uiso 1 calc . . C12 C 0.0753(9) 0.1251(8) 0.3883(4) 0.0499(14) Uani 1 d . . H12 H 0.0973 0.0083 0.4102 0.060 Uiso 1 calc . . C13 C 0.1802(15) 0.2341(11) 0.4406(6) 0.086(3) Uani 1 d . . H13A H 0.1100 0.2567 0.5077 0.104 Uiso 1 calc . . H13B H 0.2873 0.1752 0.4605 0.104 Uiso 1 calc . . C14 C 0.2337(13) 0.3900(10) 0.3755(6) 0.075(2) Uani 1 d . . H14A H 0.3610 0.4028 0.3759 0.090 Uiso 1 calc . . H14B H 0.1722 0.4777 0.4098 0.090 Uiso 1 calc . . 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 Ir1 0.03451(12) 0.03410(12) 0.03359(12) -0.00495(7) -0.00452(7) -0.00016(7) Cl2 0.0492(7) 0.0388(6) 0.0442(6) -0.0045(5) -0.0030(5) -0.0113(5) S3 0.0510(8) 0.0327(5) 0.0383(6) -0.0029(4) 0.0014(5) 0.0010(5) N4 0.038(2) 0.042(2) 0.038(2) 0.001(2) -0.005(2) -0.001(2) N5 0.041(2) 0.034(2) 0.039(2) -0.003(2) -0.002(2) -0.004(2) C1 0.030(2) 0.041(2) 0.036(2) -0.008(2) -0.009(2) 0.000(2) C2 0.033(3) 0.054(3) 0.040(3) -0.007(2) -0.003(2) 0.006(2) C3 0.036(3) 0.047(3) 0.045(3) -0.011(2) -0.001(2) 0.004(2) C4 0.031(2) 0.038(2) 0.056(3) -0.010(2) -0.008(2) 0.000(2) C5 0.047(3) 0.035(2) 0.067(4) -0.010(2) -0.010(3) 0.001(2) C6 0.053(4) 0.076(4) 0.039(3) -0.001(3) 0.010(3) 0.009(3) C7 0.077(5) 0.038(3) 0.058(3) -0.016(2) 0.001(3) -0.015(3) C8 0.077(5) 0.040(3) 0.051(3) -0.004(2) 0.000(3) 0.015(3) C9 0.077(5) 0.077(5) 0.067(4) -0.010(4) 0.006(4) 0.034(4) C10 0.088(6) 0.088(6) 0.076(5) -0.018(4) 0.028(5) 0.026(5) C11 0.050(3) 0.064(4) 0.041(3) -0.007(3) 0.014(2) -0.002(3) C12 0.063(4) 0.053(3) 0.033(2) -0.002(2) -0.007(2) -0.010(3) C13 0.130(8) 0.089(6) 0.047(4) -0.002(4) -0.037(4) -0.033(5) C14 0.105(7) 0.068(4) 0.059(4) -0.017(3) -0.020(4) -0.025(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 Ir1 C11 2.114(6) . ? Ir1 C8 2.112(6) . ? Ir1 C12 2.120(5) . ? Ir1 C7 2.119(6) . ? Ir1 S3 2.342(2) . ? Ir1 Cl2 2.382(2) . ? S3 C1 1.719(5) . ? N4 C1 1.333(6) . ? N4 C2 1.352(7) . ? N5 C4 1.349(7) . ? N5 C1 1.352(6) . ? C2 C3 1.377(8) . ? C2 C6 1.497(8) . ? C3 C4 1.368(8) . ? C4 C5 1.476(7) . ? C7 C8 1.447(11) . ? C7 C14 1.519(10) . ? C8 C9 1.492(10) . ? C9 C10 1.484(13) . ? C10 C11 1.503(10) . ? C11 C12 1.403(10) . ? C12 C13 1.487(10) . ? C13 C14 1.462(11) . ? 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 C11 Ir1 C8 81.2(3) . . ? C11 Ir1 C12 38.7(3) . . ? C8 Ir1 C12 95.2(2) . . ? C11 Ir1 C7 93.0(3) . . ? C8 Ir1 C7 40.0(3) . . ? C12 Ir1 C7 81.0(2) . . ? C11 Ir1 S3 157.3(2) . . ? C8 Ir1 S3 84.5(2) . . ? C12 Ir1 S3 161.5(2) . . ? C7 Ir1 S3 87.0(2) . . ? C11 Ir1 Cl2 88.4(2) . . ? C8 Ir1 Cl2 159.8(2) . . ? C12 Ir1 Cl2 87.2(2) . . ? C7 Ir1 Cl2 159.1(2) . . ? S3 Ir1 Cl2 99.54(6) . . ? C1 S3 Ir1 119.2(2) . . ? C1 N4 C2 117.5(4) . . ? C4 N5 C1 123.4(5) . . ? N4 C1 N5 120.7(5) . . ? N4 C1 S3 117.0(4) . . ? N5 C1 S3 122.3(4) . . ? N4 C2 C3 122.3(5) . . ? N4 C2 C6 115.2(5) . . ? C3 C2 C6 122.5(5) . . ? C4 C3 C2 119.5(5) . . ? N5 C4 C3 116.4(5) . . ? N5 C4 C5 117.9(5) . . ? C3 C4 C5 125.7(5) . . ? C8 C7 C14 122.7(7) . . ? C8 C7 Ir1 69.7(4) . . ? C14 C7 Ir1 113.4(4) . . ? C7 C8 C9 123.7(6) . . ? C7 C8 Ir1 70.3(3) . . ? C9 C8 Ir1 113.1(5) . . ? C10 C9 C8 115.4(6) . . ? C9 C10 C11 114.3(6) . . ? C12 C11 C10 123.5(7) . . ? C12 C11 Ir1 70.9(3) . . ? C10 C11 Ir1 113.8(5) . . ? C11 C12 C13 123.5(7) . . ? C11 C12 Ir1 70.4(3) . . ? C13 C12 Ir1 112.9(4) . . ? C14 C13 C12 116.4(6) . . ? C13 C14 C7 114.3(6) . . ? _refine_diff_density_max 0.604 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.171 #========END data_Rh3A _database_code_CSD 160866 _cell_length_a 6.9019(2) _cell_length_b 13.3935(4) _cell_length_c 11.25340(10) _cell_angle_alpha 90 _cell_angle_beta 103.257(2) _cell_angle_gamma 90 _cell_volume 1012.55(4) _cell_formula_units_Z 4 _cell_measurement_temperature 178.2 _cell_measurement_reflns_used 2359 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 45.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y, -z' ' -x, -y, -z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'needlelike' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.955 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _chemical_formula_weight 298.12 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H7 N2 O2 S Rh ' _chemical_formula_moiety 'C8 H7 N2 O2 S Rh ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 584.00 _exptl_absorpt_coefficient_mu 1.862 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_correction_T_min 0.81 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 178.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method \w-scan _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4869 _reflns_number_total 1875 _reflns_number_observed 1042 _reflns_observed_criterion 'I>3.00sigma' _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.13 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1042 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0266 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0277 _refine_ls_goodness_of_fit_obs 0.960 _refine_ls_shift/esd_max 0.0010 _refine_diff_density_min -0.60 _refine_diff_density_max 0.47 #------------------------------------------------------------------------------ # COMPUTATION AND REFINEMENT PROGRAMS _computing_data_collection 'Bruker SMART v5.052d' _computing_cell_refinement 'Bruker SAINT v5.04' _computing_data_reduction 'Bruker SAINT v5.04' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh 0 4 -1.118 0.919 'International Tables' S 0 4 0.125 0.123 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 32 0.003 0.002 'International Tables' H 0 28 0.000 0.000 'International Tables' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Rh1 0.19321(6) 0.24782(4) 0.63968(4) 0.0298 Uij ? ? S1 0.2121(2) 0.3772(1) 0.7844(1) 0.0335 Uij ? ? O1 0.1502(8) 0.3743(3) 0.4178(4) 0.0646 Uij ? ? O2 0.1800(8) 0.0697(3) 0.4751(4) 0.0572 Uij ? ? N1 0.2213(6) 0.1893(3) 0.8138(4) 0.0254 Uij ? ? N2 0.2251(6) 0.2783(3) 0.9978(4) 0.0306 Uij ? ? C1 0.1698(9) 0.3263(5) 0.5024(6) 0.0430 Uij ? ? C2 0.1838(9) 0.1344(5) 0.5409(5) 0.0370 Uij ? ? C3 0.2212(8) 0.2731(3) 0.8796(5) 0.0242 Uij ? ? C4 0.2277(8) 0.0998(4) 0.8718(5) 0.0303 Uij ? ? C5 0.2353(8) 0.0999(4) 0.9948(5) 0.0320 Uij ? ? C6 0.2321(7) 0.1891(4) 1.0556(5) 0.0318 Uij ? ? C7 0.2255(9) 0.0079(4) 0.7986(6) 0.0397 Uij ? ? C8 0.2318(10) 0.1919(5) 1.1878(5) 0.0503 Uij ? ? H1 0.1112 0.0080 0.7329 0.0477 Uij ? ? H2 0.3420 0.0055 0.7674 0.0477 Uij ? ? H3 0.2218 -0.0488 0.8488 0.0477 Uij ? ? H4 0.2428 0.0385 1.0381 0.0384 Uij ? ? H5 0.3133 0.1396 1.2290 0.0604 Uij ? ? H6 0.2821 0.2544 1.2211 0.0604 Uij ? ? H7 0.0996 0.1834 1.1974 0.0604 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh1 0.0345(3) 0.0276(2) 0.0270(2) -0.0036(3) 0.0062(2) 0.0004(3) S1 0.0373(9) 0.0245(8) 0.0368(9) -0.0012(7) 0.0079(7) -0.0019(7) O1 0.101(4) 0.053(3) 0.044(3) -0.019(3) 0.005(3) 0.016(3) O2 0.102(4) 0.043(3) 0.042(3) -0.006(3) 0.020(3) -0.010(2) N1 0.027(3) 0.023(3) 0.027(3) 0.000(2) 0.004(2) 0.000(2) N2 0.026(3) 0.027(3) 0.033(3) -0.001(2) 0.007(2) -0.002(2) C1 0.049(4) 0.038(4) 0.033(4) -0.008(3) 0.006(3) 0.006(3) C2 0.047(4) 0.040(4) 0.027(4) -0.006(3) 0.010(3) 0.006(3) C3 0.026(3) 0.023(4) 0.028(3) 0.000(2) 0.005(2) 0.000(2) C4 0.022(3) 0.026(3) 0.039(4) 0.000(2) 0.005(2) 0.004(3) C5 0.035(4) 0.030(3) 0.029(3) -0.004(3) 0.003(3) 0.003(3) C6 0.011(3) 0.049(4) 0.033(3) 0.000(3) 0.003(2) 0.001(3) C7 0.049(4) 0.022(3) 0.046(4) -0.002(3) 0.006(3) 0.002(3) C8 0.053(4) 0.059(4) 0.036(4) -0.003(4) 0.004(3) 0.005(3) _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RH1 S1 2.361(2) ? ? yes RH1 N1 2.078(4) ? ? yes RH1 C1 1.845(6) ? ? yes RH1 C2 1.875(7) ? ? yes S1 C3 1.750(5) ? ? yes O1 C1 1.131(7) ? ? yes O2 C2 1.135(7) ? ? yes N1 C3 1.345(6) ? ? yes N1 C4 1.360(6) ? ? yes N2 C3 1.326(7) ? ? yes N2 C6 1.356(7) ? ? yes C4 C5 1.373(7) ? ? yes C4 C7 1.480(8) ? ? yes C5 C6 1.379(7) ? ? yes C6 C8 1.489(8) ? ? yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 RH1 N1 69.4(1) ? ? ? yes S1 RH1 C1 98.0(2) ? ? ? yes S1 RH1 C2 173.1(2) ? ? ? yes N1 RH1 C1 167.4(2) ? ? ? yes N1 RH1 C2 103.7(2) ? ? ? yes C1 RH1 C2 88.9(3) ? ? ? yes RH1 S1 C3 80.0(2) ? ? ? yes RH1 N1 C3 101.1(3) ? ? ? yes RH1 N1 C4 140.4(4) ? ? ? yes C3 N1 C4 118.4(4) ? ? ? yes C3 N2 C6 115.2(4) ? ? ? yes RH1 C1 O1 178.2(6) ? ? ? yes RH1 C2 O2 175.6(5) ? ? ? yes S1 C3 N1 109.4(4) ? ? ? yes S1 C3 N2 124.2(4) ? ? ? yes N1 C3 N2 126.4(4) ? ? ? yes N1 C4 C5 118.2(5) ? ? ? yes N1 C4 C7 118.1(5) ? ? ? yes C5 C4 C7 123.7(5) ? ? ? yes C4 C5 C6 120.0(5) ? ? ? yes N2 C6 C5 121.9(5) ? ? ? yes N2 C6 C8 116.7(5) ? ? ? yes C5 C6 C8 121.5(6) ? ? ? yes