Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 0222 _publ_contact_author_name 'Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; September 2006 Dear Sirs, This file contains crystallographic data for eight structures. It is being offered as supporting information for a manuscript being submitted to Dalton Trans. Gillian Reid ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Transition Metal Complexes with Wide-angle Dithio-, Diseleno- and Ditelluroethers - Properties and Structural Systematics ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address # Commonwealth Commission split-site PhD scholarship W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Nirwan ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK Department of Pure and Applied Chemistry M.D.S. University Ajmer-305001 India ; R.Ratnani ; Department of Pure and Applied Chemistry M.D.S. University Ajmer-305001 India ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; N.Tsoureas ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 06mn005 data_06mn005 _database_code_depnum_ccdc_archive 'CCDC 621497' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-06-21 _chemical_name_systematic ; 1,2-bis(methylthiomethyl)benzene ; _chemical_name_common 1,2-bis(methylthiomethyl)benzene _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 S2' _chemical_formula_sum 'C10 H14 S2' _chemical_formula_weight 198.33 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' 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 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.004(3) _cell_length_b 7.906(2) _cell_length_c 9.4253(15) _cell_angle_alpha 90.00 _cell_angle_beta 110.785(15) _cell_angle_gamma 90.00 _cell_volume 1045.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1241 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9027 # shelxl 0.9227 _exptl_absorpt_correction_T_max 1.0000 # 0.9645 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6475 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1187 _reflns_number_gt 1073 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.0318P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1187 _refine_ls_number_parameters 56 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 S1 S 0.33574(2) 1.13878(4) 0.15256(4) 0.02077(12) Uani 1 1 d . . . C1 C 0.25219(10) 0.96836(19) 0.08769(19) 0.0325(4) Uani 1 1 d . . . H1A H 0.2830 0.8728 0.0574 0.049 Uiso 1 1 calc R . . H1B H 0.1974 1.0062 0.0005 0.049 Uiso 1 1 calc R . . H1C H 0.2305 0.9330 0.1697 0.049 Uiso 1 1 calc R . . C2 C 0.42365(9) 1.04067(17) 0.31897(14) 0.0198(3) Uani 1 1 d . . . H2A H 0.4761 1.1220 0.3656 0.024 Uiso 1 1 calc R . . H2B H 0.3932 1.0163 0.3944 0.024 Uiso 1 1 calc R . . C3 C 0.46506(9) 0.87932(15) 0.28406(14) 0.0165(3) Uani 1 1 d . . . C4 C 0.43252(9) 0.72503(17) 0.31834(15) 0.0217(3) Uani 1 1 d . . . H4 H 0.3862 0.7244 0.3657 0.026 Uiso 1 1 calc R . . C5 C 0.46627(10) 0.57226(18) 0.28489(16) 0.0252(3) Uani 1 1 d . . . H5 H 0.4434 0.4684 0.3096 0.030 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 S1 0.02139(19) 0.01677(18) 0.02317(19) 0.00037(12) 0.00668(14) 0.00223(12) C1 0.0229(7) 0.0239(8) 0.0412(9) -0.0006(6) -0.0003(6) -0.0022(6) C2 0.0210(6) 0.0209(6) 0.0173(6) -0.0020(5) 0.0068(5) 0.0007(5) C3 0.0164(6) 0.0179(6) 0.0128(6) -0.0001(4) 0.0020(5) 0.0003(5) C4 0.0201(6) 0.0228(7) 0.0210(7) 0.0015(5) 0.0061(5) -0.0017(5) C5 0.0251(7) 0.0175(6) 0.0287(7) 0.0029(5) 0.0041(6) -0.0032(5) _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 S1 C1 1.7936(15) . ? S1 C2 1.8257(14) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.5057(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.3939(18) . ? C3 C3 1.410(2) 2_655 ? C4 C5 1.389(2) . ? C4 H4 0.9500 . ? C5 C5 1.389(3) 2_655 ? C5 H5 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 C1 S1 C2 100.26(7) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 113.61(9) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C3 118.93(7) . 2_655 ? C4 C3 C2 119.02(11) . . ? C3 C3 C2 122.05(7) 2_655 . ? C5 C4 C3 121.51(12) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C5 119.56(8) . 2_655 ? C4 C5 H5 120.2 . . ? C5 C5 H5 120.2 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 S1 C2 C3 57.11(11) . . . . ? S1 C2 C3 C4 -102.32(12) . . . . ? S1 C2 C3 C3 76.86(17) . . . 2_655 ? C3 C3 C4 C5 -1.0(2) 2_655 . . . ? C2 C3 C4 C5 178.23(12) . . . . ? C3 C4 C5 C5 -0.3(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.330 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.045 #===END OF CIF ============================================================== # 05mfd035 data_05mfd035 _database_code_depnum_ccdc_archive 'CCDC 621498' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-12-28 _chemical_name_systematic ; Bis(1,2-bis(methylthiomethyl)benzene)palladium(II) hexafluorophosphate(V) ; _chemical_name_common ;Bis(1,2-bis(methylthiomethyl)benzene)palladium(ii) hexafluorophosphate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Pd S4 2+, 2(F6 P 1-)' _chemical_formula_sum 'C20 H28 F12 P2 Pd S4' _chemical_formula_weight 793.00 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 '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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 15.614(2) _cell_length_b 9.1855(15) _cell_length_c 20.982(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.356(10) _cell_angle_gamma 90.00 _cell_volume 2839.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5982 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7260 # shelxl 0.6559 _exptl_absorpt_correction_T_max 1.0000 # 0.8935 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29669 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6458 _reflns_number_gt 5524 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+25.5697P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6458 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1469 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 Pd1 Pd 0.49945(2) 0.03811(4) 0.248789(18) 0.01447(12) Uani 1 1 d . . . S1 S 0.53157(8) 0.21815(14) 0.18143(6) 0.0187(3) Uani 1 1 d . . . S2 S 0.35086(8) -0.02708(14) 0.18493(6) 0.0186(3) Uani 1 1 d . . . S3 S 0.46616(8) -0.13799(14) 0.31720(6) 0.0185(3) Uani 1 1 d . . . S4 S 0.64970(8) 0.09900(14) 0.31085(6) 0.0195(3) Uani 1 1 d . . . C1 C 0.5149(5) 0.3853(6) 0.2198(3) 0.0317(13) Uani 1 1 d . . . H1A H 0.5535 0.3862 0.2674 0.047 Uiso 1 1 calc R . . H1B H 0.4511 0.3937 0.2167 0.047 Uiso 1 1 calc R . . H1C H 0.5312 0.4674 0.1963 0.047 Uiso 1 1 calc R . . C2 C 0.4544(3) 0.2407(6) 0.0949(3) 0.0213(10) Uani 1 1 d . . . H2A H 0.4815 0.3125 0.0720 0.026 Uiso 1 1 calc R . . H2B H 0.4507 0.1467 0.0711 0.026 Uiso 1 1 calc R . . C3 C 0.3601(3) 0.2889(6) 0.0868(2) 0.0184(10) Uani 1 1 d . . . C4 C 0.3397(4) 0.4367(6) 0.0782(3) 0.0256(11) Uani 1 1 d . . . H4 H 0.3859 0.5041 0.0783 0.031 Uiso 1 1 calc R . . C5 C 0.2526(4) 0.4867(7) 0.0696(3) 0.0313(13) Uani 1 1 d . . . H5 H 0.2398 0.5881 0.0656 0.038 Uiso 1 1 calc R . . C6 C 0.1842(4) 0.3870(7) 0.0667(3) 0.0333(14) Uani 1 1 d . . . H6 H 0.1242 0.4203 0.0596 0.040 Uiso 1 1 calc R . . C7 C 0.2033(4) 0.2405(7) 0.0740(3) 0.0288(12) Uani 1 1 d . . . H7 H 0.1559 0.1733 0.0710 0.035 Uiso 1 1 calc R . . C8 C 0.2916(3) 0.1891(6) 0.0856(2) 0.0205(10) Uani 1 1 d . . . C9 C 0.3098(4) 0.0290(6) 0.0966(3) 0.0225(11) Uani 1 1 d . . . H9A H 0.3552 0.0003 0.0753 0.027 Uiso 1 1 calc R . . H9B H 0.2530 -0.0247 0.0732 0.027 Uiso 1 1 calc R . . C10 C 0.2778(4) 0.0731(7) 0.2204(3) 0.0287(12) Uani 1 1 d . . . H10A H 0.2943 0.0506 0.2686 0.043 Uiso 1 1 calc R . . H10B H 0.2145 0.0453 0.1972 0.043 Uiso 1 1 calc R . . H10C H 0.2851 0.1777 0.2146 0.043 Uiso 1 1 calc R . . C11 C 0.4812(4) -0.3085(6) 0.2795(3) 0.0283(12) Uani 1 1 d . . . H11A H 0.4418 -0.3107 0.2322 0.042 Uiso 1 1 calc R . . H11B H 0.4652 -0.3891 0.3040 0.042 Uiso 1 1 calc R . . H11C H 0.5447 -0.3182 0.2818 0.042 Uiso 1 1 calc R . . C12 C 0.5448(3) -0.1595(6) 0.4034(3) 0.0227(11) Uani 1 1 d . . . H12A H 0.5529 -0.0636 0.4262 0.027 Uiso 1 1 calc R . . H12B H 0.5167 -0.2255 0.4282 0.027 Uiso 1 1 calc R . . C13 C 0.6366(3) -0.2184(6) 0.4090(2) 0.0195(10) Uani 1 1 d . . . C14 C 0.6523(4) -0.3684(7) 0.4182(3) 0.0268(12) Uani 1 1 d . . . H14 H 0.6050 -0.4305 0.4210 0.032 Uiso 1 1 calc R . . C15 C 0.7359(4) -0.4270(6) 0.4235(3) 0.0294(12) Uani 1 1 d . . . H15 H 0.7450 -0.5293 0.4278 0.035 Uiso 1 1 calc R . . C16 C 0.8065(4) -0.3370(7) 0.4223(3) 0.0291(12) Uani 1 1 d . . . H16 H 0.8644 -0.3769 0.4272 0.035 Uiso 1 1 calc R . . C17 C 0.7922(4) -0.1890(7) 0.4141(3) 0.0281(12) Uani 1 1 d . . . H17 H 0.8408 -0.1274 0.4135 0.034 Uiso 1 1 calc R . . C18 C 0.7072(4) -0.1279(6) 0.4067(2) 0.0201(10) Uani 1 1 d . . . C19 C 0.6952(4) 0.0342(6) 0.3981(3) 0.0234(11) Uani 1 1 d . . . H19A H 0.7548 0.0811 0.4200 0.028 Uiso 1 1 calc R . . H19B H 0.6541 0.0669 0.4225 0.028 Uiso 1 1 calc R . . C20 C 0.7180(4) -0.0015(7) 0.2717(3) 0.0293(12) Uani 1 1 d . . . H20A H 0.6999 0.0239 0.2237 0.044 Uiso 1 1 calc R . . H20B H 0.7092 -0.1061 0.2763 0.044 Uiso 1 1 calc R . . H20C H 0.7822 0.0230 0.2937 0.044 Uiso 1 1 calc R . . P1 P 0.44528(10) 0.30579(16) 0.39525(8) 0.0260(3) Uani 1 1 d . . . F1 F 0.4425(4) 0.1350(5) 0.3870(4) 0.097(2) Uani 1 1 d . . . F2 F 0.5415(3) 0.3092(5) 0.3832(2) 0.0463(10) Uani 1 1 d . . . F3 F 0.4945(4) 0.2999(9) 0.4721(2) 0.094(2) Uani 1 1 d . . . F4 F 0.4424(3) 0.4768(4) 0.3959(3) 0.0527(12) Uani 1 1 d . . . F5 F 0.3959(4) 0.3178(8) 0.3146(2) 0.0818(18) Uani 1 1 d . . . F6 F 0.3494(3) 0.3009(5) 0.4056(3) 0.0578(13) Uani 1 1 d . . . P2 P 0.55071(10) -0.23816(16) 0.10305(8) 0.0270(3) Uani 1 1 d . . . F7 F 0.5497(4) -0.4054(6) 0.0871(4) 0.109(3) Uani 1 1 d . . . F8 F 0.6413(3) -0.2211(5) 0.0861(3) 0.0685(16) Uani 1 1 d . . . F9 F 0.6063(4) -0.2823(7) 0.1795(3) 0.092(2) Uani 1 1 d . . . F10 F 0.5574(3) -0.0744(5) 0.1273(3) 0.0605(13) Uani 1 1 d . . . F11 F 0.4585(3) -0.2554(5) 0.1201(2) 0.0461(10) Uani 1 1 d . . . F12 F 0.4956(4) -0.1948(13) 0.0314(2) 0.141(4) 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 Pd1 0.01264(19) 0.01291(19) 0.01827(19) -0.00105(13) 0.00566(14) -0.00053(13) S1 0.0170(6) 0.0176(6) 0.0227(6) -0.0001(5) 0.0082(5) -0.0018(5) S2 0.0160(6) 0.0177(6) 0.0206(6) -0.0003(5) 0.0043(5) -0.0028(5) S3 0.0170(6) 0.0179(6) 0.0212(6) 0.0018(5) 0.0073(5) -0.0004(5) S4 0.0162(6) 0.0183(6) 0.0224(6) -0.0015(5) 0.0042(5) -0.0025(5) C1 0.048(4) 0.016(3) 0.034(3) -0.005(2) 0.017(3) 0.000(3) C2 0.021(2) 0.025(3) 0.019(2) 0.002(2) 0.008(2) 0.001(2) C3 0.021(2) 0.018(2) 0.017(2) -0.0003(19) 0.0078(19) 0.005(2) C4 0.029(3) 0.022(3) 0.026(3) 0.001(2) 0.009(2) 0.001(2) C5 0.036(3) 0.027(3) 0.031(3) 0.006(2) 0.012(3) 0.012(3) C6 0.027(3) 0.041(4) 0.035(3) 0.016(3) 0.014(2) 0.015(3) C7 0.019(3) 0.037(3) 0.030(3) 0.013(2) 0.008(2) 0.004(2) C8 0.020(2) 0.024(3) 0.017(2) 0.001(2) 0.0060(19) 0.000(2) C9 0.024(3) 0.022(3) 0.018(2) 0.001(2) 0.003(2) -0.002(2) C10 0.017(2) 0.041(3) 0.028(3) -0.001(2) 0.007(2) 0.002(2) C11 0.040(3) 0.017(2) 0.025(3) 0.000(2) 0.006(2) -0.003(2) C12 0.019(2) 0.030(3) 0.020(2) -0.001(2) 0.007(2) 0.003(2) C13 0.019(2) 0.023(3) 0.017(2) 0.0012(19) 0.0058(19) 0.002(2) C14 0.023(3) 0.032(3) 0.025(3) 0.004(2) 0.007(2) 0.000(2) C15 0.037(3) 0.021(3) 0.030(3) 0.003(2) 0.010(2) 0.009(2) C16 0.022(3) 0.036(3) 0.031(3) 0.005(2) 0.011(2) 0.011(2) C17 0.019(2) 0.035(3) 0.030(3) 0.001(2) 0.008(2) -0.003(2) C18 0.024(3) 0.019(2) 0.017(2) -0.0026(19) 0.0071(19) 0.000(2) C19 0.024(3) 0.019(3) 0.022(3) -0.004(2) 0.001(2) -0.004(2) C20 0.024(3) 0.038(3) 0.027(3) -0.002(2) 0.010(2) 0.001(2) P1 0.0283(7) 0.0194(7) 0.0355(8) -0.0019(6) 0.0175(6) 0.0005(6) F1 0.095(4) 0.022(2) 0.212(8) -0.011(3) 0.103(5) -0.003(3) F2 0.038(2) 0.047(2) 0.065(3) -0.006(2) 0.032(2) 0.0035(18) F3 0.076(4) 0.172(7) 0.032(2) 0.039(3) 0.016(2) 0.031(4) F4 0.046(2) 0.025(2) 0.094(4) 0.006(2) 0.033(2) 0.0011(18) F5 0.076(4) 0.118(5) 0.042(3) -0.025(3) 0.006(2) -0.022(4) F6 0.045(2) 0.035(2) 0.114(4) 0.000(2) 0.054(3) -0.0019(19) P2 0.0270(7) 0.0201(7) 0.0392(8) -0.0044(6) 0.0180(6) 0.0002(6) F7 0.099(4) 0.043(3) 0.233(8) -0.067(4) 0.119(5) -0.038(3) F8 0.053(3) 0.039(2) 0.142(5) -0.007(3) 0.070(3) -0.004(2) F9 0.075(4) 0.094(5) 0.090(4) 0.052(4) 0.004(3) 0.017(3) F10 0.067(3) 0.029(2) 0.102(4) -0.019(2) 0.051(3) -0.007(2) F11 0.043(2) 0.044(2) 0.065(3) -0.013(2) 0.036(2) -0.0087(19) F12 0.070(4) 0.328(13) 0.020(2) 0.030(4) 0.009(2) 0.016(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 Pd1 S3 2.3327(13) . ? Pd1 S1 2.3353(13) . ? Pd1 S2 2.3401(13) . ? Pd1 S4 2.3424(13) . ? S1 C1 1.792(6) . ? S1 C2 1.827(5) . ? S2 C10 1.806(6) . ? S2 C9 1.824(5) . ? S3 C11 1.804(6) . ? S3 C12 1.830(5) . ? S4 C20 1.803(6) . ? S4 C19 1.830(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.492(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.392(7) . ? C3 C8 1.403(7) . ? C4 C5 1.389(8) . ? C4 H4 0.9500 . ? C5 C6 1.393(9) . ? C5 H5 0.9500 . ? C6 C7 1.376(9) . ? C6 H6 0.9500 . ? C7 C8 1.400(7) . ? C7 H7 0.9500 . ? C8 C9 1.501(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.500(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.394(7) . ? C13 C14 1.402(8) . ? C14 C15 1.382(8) . ? C14 H14 0.9500 . ? C15 C16 1.384(9) . ? C15 H15 0.9500 . ? C16 C17 1.379(9) . ? C16 H16 0.9500 . ? C17 C18 1.401(7) . ? C17 H17 0.9500 . ? C18 C19 1.504(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? P1 F3 1.541(5) . ? P1 F4 1.571(4) . ? P1 F1 1.578(5) . ? P1 F6 1.583(4) . ? P1 F2 1.604(4) . ? P1 F5 1.613(5) . ? P2 F12 1.517(5) . ? P2 F7 1.571(5) . ? P2 F8 1.576(4) . ? P2 F10 1.580(4) . ? P2 F11 1.602(4) . ? P2 F9 1.602(6) . ? 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 S3 Pd1 S1 178.80(5) . . ? S3 Pd1 S2 78.11(4) . . ? S1 Pd1 S2 101.87(5) . . ? S3 Pd1 S4 102.12(5) . . ? S1 Pd1 S4 77.93(5) . . ? S2 Pd1 S4 178.39(5) . . ? C1 S1 C2 101.7(3) . . ? C1 S1 Pd1 104.0(2) . . ? C2 S1 Pd1 118.58(18) . . ? C10 S2 C9 102.6(3) . . ? C10 S2 Pd1 105.97(19) . . ? C9 S2 Pd1 117.25(18) . . ? C11 S3 C12 101.4(3) . . ? C11 S3 Pd1 104.14(19) . . ? C12 S3 Pd1 118.05(19) . . ? C20 S4 C19 101.4(3) . . ? C20 S4 Pd1 105.0(2) . . ? C19 S4 Pd1 117.62(18) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 116.6(4) . . ? C3 C2 H2A 108.1 . . ? S1 C2 H2A 108.1 . . ? C3 C2 H2B 108.1 . . ? S1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C8 119.6(5) . . ? C4 C3 C2 118.6(5) . . ? C8 C3 C2 121.7(5) . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 119.4(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.3(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.9(6) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C3 118.9(5) . . ? C7 C8 C9 118.9(5) . . ? C3 C8 C9 122.2(5) . . ? C8 C9 S2 114.6(4) . . ? C8 C9 H9A 108.6 . . ? S2 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? S2 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S3 C11 H11A 109.5 . . ? S3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S3 115.2(4) . . ? C13 C12 H12A 108.5 . . ? S3 C12 H12A 108.5 . . ? C13 C12 H12B 108.5 . . ? S3 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C18 C13 C14 119.1(5) . . ? C18 C13 C12 121.9(5) . . ? C14 C13 C12 118.9(5) . . ? C15 C14 C13 120.7(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.2(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.6(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 121.1(5) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 119.2(5) . . ? C13 C18 C19 121.7(5) . . ? C17 C18 C19 119.0(5) . . ? C18 C19 S4 115.7(4) . . ? C18 C19 H19A 108.4 . . ? S4 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? S4 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F3 P1 F4 91.8(4) . . ? F3 P1 F1 93.7(4) . . ? F4 P1 F1 174.4(4) . . ? F3 P1 F6 91.2(3) . . ? F4 P1 F6 89.8(2) . . ? F1 P1 F6 89.6(3) . . ? F3 P1 F2 89.9(3) . . ? F4 P1 F2 90.7(2) . . ? F1 P1 F2 89.8(3) . . ? F6 P1 F2 178.7(3) . . ? F3 P1 F5 177.7(4) . . ? F4 P1 F5 86.3(3) . . ? F1 P1 F5 88.1(4) . . ? F6 P1 F5 90.0(3) . . ? F2 P1 F5 88.8(3) . . ? F12 P2 F7 94.8(5) . . ? F12 P2 F8 90.4(3) . . ? F7 P2 F8 89.8(3) . . ? F12 P2 F10 91.4(5) . . ? F7 P2 F10 173.8(4) . . ? F8 P2 F10 90.5(2) . . ? F12 P2 F11 89.4(3) . . ? F7 P2 F11 90.2(2) . . ? F8 P2 F11 179.8(3) . . ? F10 P2 F11 89.5(2) . . ? F12 P2 F9 178.2(4) . . ? F7 P2 F9 85.9(4) . . ? F8 P2 F9 91.3(3) . . ? F10 P2 F9 87.9(3) . . ? F11 P2 F9 88.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # S3 Pd1 S1 C1 11(2) . . . . ? # S3 Pd1 S1 C2 -101(2) . . . . ? # S4 Pd1 S2 C10 180(100) . . . . ? # S4 Pd1 S2 C9 -66.7(18) . . . . ? # S1 Pd1 S3 C11 169(2) . . . . ? # S1 Pd1 S3 C12 -80(2) . . . . ? # S2 Pd1 S4 C20 1.5(18) . . . . ? # S2 Pd1 S4 C19 -110.3(18) . . . . ? S2 Pd1 S1 C1 99.9(2) . . . . ? S4 Pd1 S1 C1 -81.8(2) . . . . ? S2 Pd1 S1 C2 -12.1(2) . . . . ? S4 Pd1 S1 C2 166.2(2) . . . . ? S3 Pd1 S2 C10 81.2(2) . . . . ? S1 Pd1 S2 C10 -97.5(2) . . . . ? S3 Pd1 S2 C9 -165.1(2) . . . . ? S1 Pd1 S2 C9 16.2(2) . . . . ? S2 Pd1 S3 C11 79.4(2) . . . . ? S4 Pd1 S3 C11 -99.0(2) . . . . ? S2 Pd1 S3 C12 -169.2(2) . . . . ? S4 Pd1 S3 C12 12.4(2) . . . . ? S3 Pd1 S4 C20 99.6(2) . . . . ? S1 Pd1 S4 C20 -81.6(2) . . . . ? S3 Pd1 S4 C19 -12.2(2) . . . . ? S1 Pd1 S4 C19 166.6(2) . . . . ? C1 S1 C2 C3 -48.7(5) . . . . ? Pd1 S1 C2 C3 64.6(4) . . . . ? S1 C2 C3 C4 95.3(5) . . . . ? S1 C2 C3 C8 -86.7(6) . . . . ? C8 C3 C4 C5 1.0(8) . . . . ? C2 C3 C4 C5 179.1(5) . . . . ? C3 C4 C5 C6 -2.6(9) . . . . ? C4 C5 C6 C7 1.5(9) . . . . ? C5 C6 C7 C8 1.2(9) . . . . ? C6 C7 C8 C3 -2.8(8) . . . . ? C6 C7 C8 C9 177.1(5) . . . . ? C4 C3 C8 C7 1.6(8) . . . . ? C2 C3 C8 C7 -176.3(5) . . . . ? C4 C3 C8 C9 -178.2(5) . . . . ? C2 C3 C8 C9 3.8(7) . . . . ? C7 C8 C9 S2 -94.7(5) . . . . ? C3 C8 C9 S2 85.1(6) . . . . ? C10 S2 C9 C8 43.8(5) . . . . ? Pd1 S2 C9 C8 -71.8(4) . . . . ? C11 S3 C12 C13 45.4(5) . . . . ? Pd1 S3 C12 C13 -67.5(5) . . . . ? S3 C12 C13 C18 86.6(6) . . . . ? S3 C12 C13 C14 -94.8(5) . . . . ? C18 C13 C14 C15 -1.5(8) . . . . ? C12 C13 C14 C15 179.9(5) . . . . ? C13 C14 C15 C16 2.6(9) . . . . ? C14 C15 C16 C17 -1.8(9) . . . . ? C15 C16 C17 C18 -0.1(9) . . . . ? C14 C13 C18 C17 -0.4(7) . . . . ? C12 C13 C18 C17 178.2(5) . . . . ? C14 C13 C18 C19 -178.9(5) . . . . ? C12 C13 C18 C19 -0.3(7) . . . . ? C16 C17 C18 C13 1.3(8) . . . . ? C16 C17 C18 C19 179.8(5) . . . . ? C13 C18 C19 S4 -86.4(6) . . . . ? C17 C18 C19 S4 95.1(5) . . . . ? C20 S4 C19 C18 -46.6(5) . . . . ? Pd1 S4 C19 C18 67.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.667 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.149 #===END OF CIF ============================================================== # 05mfd032 data_05mfd032 _database_code_depnum_ccdc_archive 'CCDC 621499' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-01-20 _chemical_name_systematic ; Cis-dichlorobis(1,2-bis(methylthiomethyl)benzene)rhodium(III) hexafluorophosphate(V) ; _chemical_name_common ; Cis-dichlorobis(1,2-bis(methylthiomethyl)benzene)rhodium(iii) hexafluorophosphate(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Cl2 Rh S4 1+, F6 P 1-' _chemical_formula_sum 'C20 H28 Cl2 F6 P Rh S4' _chemical_formula_weight 715.44 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Rh Rh -1.1178 0.9187 '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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 12.356(2) _cell_length_b 12.027(2) _cell_length_c 18.368(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.621(9) _cell_angle_gamma 90.00 _cell_volume 2711.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6376 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 # +/- 0.02 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4688 # 0.8856 _exptl_absorpt_correction_T_max 1.0000 # 0.9290 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 26273 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1158 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.62 _reflns_number_total 6223 _reflns_number_gt 3820 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.5002P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6223 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Rh1 Rh 0.38197(3) 0.08633(3) 0.188801(18) 0.01886(11) Uani 1 1 d . . . Cl1 Cl 0.51821(9) -0.04332(9) 0.23123(6) 0.0230(3) Uani 1 1 d . . . Cl2 Cl 0.23421(10) -0.03203(9) 0.20138(6) 0.0260(3) Uani 1 1 d . . . S1 S 0.37901(10) 0.14689(9) 0.31166(6) 0.0211(3) Uani 1 1 d . . . S2 S 0.53293(10) 0.18654(10) 0.15568(6) 0.0238(3) Uani 1 1 d . . . S3 S 0.39525(10) -0.00044(9) 0.07291(6) 0.0220(3) Uani 1 1 d . . . S4 S 0.25761(10) 0.23241(9) 0.16029(6) 0.0218(3) Uani 1 1 d . . . P1 P 0.83464(11) 0.31798(10) 0.06306(6) 0.0235(3) Uani 1 1 d . . . F1 F 0.8772(2) 0.2440(2) -0.00034(14) 0.0479(8) Uani 1 1 d . . . F2 F 0.7522(2) 0.2198(2) 0.07919(13) 0.0318(7) Uani 1 1 d . . . F3 F 0.9257(2) 0.2656(2) 0.12145(14) 0.0387(7) Uani 1 1 d . . . F4 F 0.9162(2) 0.4157(2) 0.04668(14) 0.0421(8) Uani 1 1 d . . . F5 F 0.7431(2) 0.3703(2) 0.00459(14) 0.0419(8) Uani 1 1 d . . . F6 F 0.7914(2) 0.3912(2) 0.12605(14) 0.0389(7) Uani 1 1 d . . . C1 C 0.3550(4) 0.0230(4) 0.3632(2) 0.0290(12) Uani 1 1 d . . . H1 H 0.2827 -0.0068 0.3462 0.044 Uiso 1 1 calc R . . H2 H 0.3586 0.0415 0.4154 0.044 Uiso 1 1 calc R . . H3 H 0.4106 -0.0328 0.3561 0.044 Uiso 1 1 calc R . . C2 C 0.5147(4) 0.1781(4) 0.3569(2) 0.0229(11) Uani 1 1 d . . . H4 H 0.5151 0.1701 0.4106 0.028 Uiso 1 1 calc R . . H5 H 0.5676 0.1242 0.3407 0.028 Uiso 1 1 calc R . . C3 C 0.5492(4) 0.2948(3) 0.3394(2) 0.0210(11) Uani 1 1 d . . . C4 C 0.5253(4) 0.3824(4) 0.3844(2) 0.0256(12) Uani 1 1 d . . . H6 H 0.4846 0.3688 0.4243 0.031 Uiso 1 1 calc R . . C5 C 0.5604(4) 0.4894(4) 0.3714(2) 0.0259(11) Uani 1 1 d . . . H7 H 0.5436 0.5489 0.4022 0.031 Uiso 1 1 calc R . . C6 C 0.6199(4) 0.5088(4) 0.3136(2) 0.0292(12) Uani 1 1 d . . . H8 H 0.6442 0.5820 0.3046 0.035 Uiso 1 1 calc R . . C7 C 0.6442(4) 0.4220(4) 0.2686(2) 0.0265(11) Uani 1 1 d . . . H9 H 0.6857 0.4360 0.2292 0.032 Uiso 1 1 calc R . . C8 C 0.6086(4) 0.3148(4) 0.2806(2) 0.0234(11) Uani 1 1 d . . . C9 C 0.6372(4) 0.2231(4) 0.2303(2) 0.0250(11) Uani 1 1 d . . . H10 H 0.6551 0.1557 0.2602 0.030 Uiso 1 1 calc R . . H11 H 0.7039 0.2452 0.2088 0.030 Uiso 1 1 calc R . . C10 C 0.4970(4) 0.3216(4) 0.1193(3) 0.0339(13) Uani 1 1 d . . . H12 H 0.4397 0.3143 0.0780 0.051 Uiso 1 1 calc R . . H13 H 0.5612 0.3567 0.1025 0.051 Uiso 1 1 calc R . . H14 H 0.4704 0.3676 0.1575 0.051 Uiso 1 1 calc R . . C11 C 0.3730(4) -0.1480(3) 0.0824(2) 0.0271(12) Uani 1 1 d . . . H15 H 0.4288 -0.1786 0.1192 0.041 Uiso 1 1 calc R . . H16 H 0.3774 -0.1847 0.0352 0.041 Uiso 1 1 calc R . . H17 H 0.3007 -0.1605 0.0980 0.041 Uiso 1 1 calc R . . C12 C 0.2819(4) 0.0260(4) 0.0035(2) 0.0252(11) Uani 1 1 d . . . H18 H 0.2851 -0.0260 -0.0380 0.030 Uiso 1 1 calc R . . H19 H 0.2126 0.0132 0.0243 0.030 Uiso 1 1 calc R . . C13 C 0.2854(4) 0.1434(4) -0.0237(2) 0.0222(11) Uani 1 1 d . . . C14 C 0.3407(4) 0.1640(4) -0.0843(2) 0.0274(12) Uani 1 1 d . . . H20 H 0.3729 0.1041 -0.1078 0.033 Uiso 1 1 calc R . . C15 C 0.3491(4) 0.2715(4) -0.1103(2) 0.0325(13) Uani 1 1 d . . . H21 H 0.3882 0.2853 -0.1510 0.039 Uiso 1 1 calc R . . C16 C 0.3008(4) 0.3588(4) -0.0772(2) 0.0316(12) Uani 1 1 d . . . H22 H 0.3067 0.4325 -0.0949 0.038 Uiso 1 1 calc R . . C17 C 0.2441(4) 0.3378(4) -0.0184(2) 0.0274(12) Uani 1 1 d . . . H23 H 0.2098 0.3976 0.0038 0.033 Uiso 1 1 calc R . . C18 C 0.2360(4) 0.2307(4) 0.0091(2) 0.0242(11) Uani 1 1 d . . . C19 C 0.1726(4) 0.2122(4) 0.0733(2) 0.0284(12) Uani 1 1 d . . . H24 H 0.1430 0.1356 0.0712 0.034 Uiso 1 1 calc R . . H25 H 0.1104 0.2646 0.0701 0.034 Uiso 1 1 calc R . . C20 C 0.1495(4) 0.2232(4) 0.2190(2) 0.0272(12) Uani 1 1 d . . . H26 H 0.1803 0.2323 0.2703 0.041 Uiso 1 1 calc R . . H27 H 0.1140 0.1505 0.2126 0.041 Uiso 1 1 calc R . . H28 H 0.0958 0.2820 0.2059 0.041 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 Rh1 0.0192(2) 0.0199(2) 0.01749(19) -0.00143(16) 0.00244(14) -0.00031(18) Cl1 0.0232(7) 0.0250(6) 0.0209(6) -0.0007(5) 0.0023(5) 0.0039(5) Cl2 0.0228(7) 0.0244(6) 0.0306(7) -0.0022(5) 0.0026(5) -0.0037(5) S1 0.0226(7) 0.0235(7) 0.0177(6) -0.0023(5) 0.0049(5) -0.0029(5) S2 0.0243(7) 0.0292(7) 0.0182(6) -0.0020(5) 0.0034(5) -0.0055(6) S3 0.0240(7) 0.0220(6) 0.0193(6) -0.0027(5) -0.0002(5) 0.0019(6) S4 0.0236(7) 0.0216(6) 0.0206(6) -0.0023(5) 0.0035(5) 0.0013(6) P1 0.0252(8) 0.0246(7) 0.0211(6) 0.0003(5) 0.0050(6) -0.0021(6) F1 0.049(2) 0.060(2) 0.0392(17) -0.0177(15) 0.0222(15) -0.0036(17) F2 0.0343(17) 0.0321(16) 0.0298(15) 0.0013(12) 0.0073(13) -0.0105(14) F3 0.0323(18) 0.0372(17) 0.0435(17) 0.0038(14) -0.0087(14) 0.0076(15) F4 0.042(2) 0.0431(18) 0.0408(17) 0.0040(14) 0.0042(14) -0.0205(16) F5 0.042(2) 0.0413(17) 0.0382(17) 0.0102(14) -0.0111(14) -0.0052(16) F6 0.046(2) 0.0348(16) 0.0371(16) -0.0113(14) 0.0112(14) 0.0031(15) C1 0.039(3) 0.030(3) 0.019(2) 0.003(2) 0.008(2) -0.015(3) C2 0.026(3) 0.030(3) 0.013(2) 0.002(2) 0.003(2) 0.002(2) C3 0.024(3) 0.019(3) 0.020(2) 0.001(2) 0.002(2) -0.001(2) C4 0.025(3) 0.030(3) 0.022(3) -0.006(2) 0.003(2) 0.002(2) C5 0.025(3) 0.024(3) 0.028(3) -0.007(2) 0.000(2) 0.001(2) C6 0.029(3) 0.028(3) 0.030(3) 0.004(2) -0.001(2) -0.003(3) C7 0.024(3) 0.034(3) 0.023(3) -0.002(2) 0.005(2) -0.003(2) C8 0.019(3) 0.030(3) 0.020(2) -0.001(2) 0.000(2) -0.005(2) C9 0.021(3) 0.036(3) 0.018(2) 0.001(2) 0.003(2) -0.001(2) C10 0.029(3) 0.038(3) 0.033(3) 0.010(2) -0.005(2) -0.010(3) C11 0.035(3) 0.020(3) 0.025(3) -0.001(2) 0.002(2) 0.002(2) C12 0.029(3) 0.025(3) 0.019(2) -0.006(2) -0.003(2) -0.001(2) C13 0.022(3) 0.029(3) 0.014(2) 0.001(2) -0.003(2) 0.002(2) C14 0.031(3) 0.029(3) 0.021(3) -0.003(2) -0.002(2) 0.009(2) C15 0.026(3) 0.050(4) 0.023(3) 0.005(3) 0.006(2) 0.003(3) C16 0.033(3) 0.033(3) 0.027(3) 0.008(2) -0.002(2) -0.001(3) C17 0.031(3) 0.026(3) 0.023(3) -0.005(2) -0.006(2) 0.016(2) C18 0.023(3) 0.029(3) 0.020(2) 0.000(2) -0.001(2) 0.001(2) C19 0.020(3) 0.036(3) 0.028(3) -0.005(2) 0.000(2) 0.001(2) C20 0.025(3) 0.036(3) 0.021(2) 0.000(2) 0.006(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 Cl2 2.3474(12) . ? Rh1 S4 2.3529(12) . ? Rh1 S2 2.3587(12) . ? Rh1 Cl1 2.3601(12) . ? Rh1 S1 2.3756(12) . ? Rh1 S3 2.3933(12) . ? S1 C1 1.808(4) . ? S1 C2 1.822(5) . ? S2 C10 1.793(5) . ? S2 C9 1.823(4) . ? S3 C11 1.807(4) . ? S3 C12 1.810(4) . ? S4 C20 1.815(4) . ? S4 C19 1.825(4) . ? P1 F3 1.592(3) . ? P1 F6 1.594(3) . ? P1 F5 1.596(3) . ? P1 F4 1.599(3) . ? P1 F1 1.602(3) . ? P1 F2 1.609(3) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 C3 1.512(6) . ? C2 H4 0.9900 . ? C2 H5 0.9900 . ? C3 C4 1.392(6) . ? C3 C8 1.395(6) . ? C4 C5 1.387(6) . ? C4 H6 0.9500 . ? C5 C6 1.380(6) . ? C5 H7 0.9500 . ? C6 C7 1.386(6) . ? C6 H8 0.9500 . ? C7 C8 1.388(6) . ? C7 H9 0.9500 . ? C8 C9 1.506(6) . ? C9 H10 0.9900 . ? C9 H11 0.9900 . ? C10 H12 0.9800 . ? C10 H13 0.9800 . ? C10 H14 0.9800 . ? C11 H15 0.9800 . ? C11 H16 0.9800 . ? C11 H17 0.9800 . ? C12 C13 1.499(6) . ? C12 H18 0.9900 . ? C12 H19 0.9900 . ? C13 C18 1.387(6) . ? C13 C14 1.394(6) . ? C14 C15 1.387(6) . ? C14 H20 0.9500 . ? C15 C16 1.382(6) . ? C15 H21 0.9500 . ? C16 C17 1.377(6) . ? C16 H22 0.9500 . ? C17 C18 1.391(6) . ? C17 H23 0.9500 . ? C18 C19 1.505(6) . ? C19 H24 0.9900 . ? C19 H25 0.9900 . ? C20 H26 0.9800 . ? C20 H27 0.9800 . ? C20 H28 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 Cl2 Rh1 S4 88.82(4) . . ? Cl2 Rh1 S2 169.24(4) . . ? S4 Rh1 S2 94.39(4) . . ? Cl2 Rh1 Cl1 95.74(4) . . ? S4 Rh1 Cl1 171.67(4) . . ? S2 Rh1 Cl1 82.40(4) . . ? Cl2 Rh1 S1 89.72(4) . . ? S4 Rh1 S1 84.34(4) . . ? S2 Rh1 S1 100.81(4) . . ? Cl1 Rh1 S1 88.71(4) . . ? Cl2 Rh1 S3 87.53(4) . . ? S4 Rh1 S3 103.75(4) . . ? S2 Rh1 S3 81.73(4) . . ? Cl1 Rh1 S3 83.46(4) . . ? S1 Rh1 S3 171.39(4) . . ? C1 S1 C2 97.4(2) . . ? C1 S1 Rh1 105.45(15) . . ? C2 S1 Rh1 112.45(14) . . ? C10 S2 C9 100.7(2) . . ? C10 S2 Rh1 112.96(17) . . ? C9 S2 Rh1 116.13(14) . . ? C11 S3 C12 97.3(2) . . ? C11 S3 Rh1 108.40(15) . . ? C12 S3 Rh1 115.03(15) . . ? C20 S4 C19 97.1(2) . . ? C20 S4 Rh1 109.20(15) . . ? C19 S4 Rh1 112.99(16) . . ? F3 P1 F6 89.99(15) . . ? F3 P1 F5 179.85(19) . . ? F6 P1 F5 90.00(16) . . ? F3 P1 F4 90.33(16) . . ? F6 P1 F4 90.12(15) . . ? F5 P1 F4 89.82(15) . . ? F3 P1 F1 90.23(16) . . ? F6 P1 F1 179.54(18) . . ? F5 P1 F1 89.78(16) . . ? F4 P1 F1 90.28(15) . . ? F3 P1 F2 89.93(15) . . ? F6 P1 F2 89.96(14) . . ? F5 P1 F2 89.92(15) . . ? F4 P1 F2 179.73(18) . . ? F1 P1 F2 89.64(15) . . ? S1 C1 H1 109.5 . . ? S1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? S1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? C3 C2 S1 111.1(3) . . ? C3 C2 H4 109.4 . . ? S1 C2 H4 109.4 . . ? C3 C2 H5 109.4 . . ? S1 C2 H5 109.4 . . ? H4 C2 H5 108.0 . . ? C4 C3 C8 119.7(4) . . ? C4 C3 C2 119.5(4) . . ? C8 C3 C2 120.8(4) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H6 119.7 . . ? C3 C4 H6 119.7 . . ? C6 C5 C4 119.6(4) . . ? C6 C5 H7 120.2 . . ? C4 C5 H7 120.2 . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H8 119.9 . . ? C7 C6 H8 119.9 . . ? C6 C7 C8 120.8(4) . . ? C6 C7 H9 119.6 . . ? C8 C7 H9 119.6 . . ? C7 C8 C3 119.2(4) . . ? C7 C8 C9 118.9(4) . . ? C3 C8 C9 121.9(4) . . ? C8 C9 S2 116.2(3) . . ? C8 C9 H10 108.2 . . ? S2 C9 H10 108.2 . . ? C8 C9 H11 108.2 . . ? S2 C9 H11 108.2 . . ? H10 C9 H11 107.4 . . ? S2 C10 H12 109.5 . . ? S2 C10 H13 109.5 . . ? H12 C10 H13 109.5 . . ? S2 C10 H14 109.5 . . ? H12 C10 H14 109.5 . . ? H13 C10 H14 109.5 . . ? S3 C11 H15 109.5 . . ? S3 C11 H16 109.5 . . ? H15 C11 H16 109.5 . . ? S3 C11 H17 109.5 . . ? H15 C11 H17 109.5 . . ? H16 C11 H17 109.5 . . ? C13 C12 S3 110.5(3) . . ? C13 C12 H18 109.5 . . ? S3 C12 H18 109.5 . . ? C13 C12 H19 109.5 . . ? S3 C12 H19 109.5 . . ? H18 C12 H19 108.1 . . ? C18 C13 C14 119.5(4) . . ? C18 C13 C12 122.5(4) . . ? C14 C13 C12 117.9(4) . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H20 119.9 . . ? C13 C14 H20 119.9 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H21 119.9 . . ? C14 C15 H21 119.9 . . ? C17 C16 C15 119.3(4) . . ? C17 C16 H22 120.3 . . ? C15 C16 H22 120.3 . . ? C16 C17 C18 121.3(4) . . ? C16 C17 H23 119.4 . . ? C18 C17 H23 119.4 . . ? C13 C18 C17 119.3(4) . . ? C13 C18 C19 121.5(4) . . ? C17 C18 C19 119.1(4) . . ? C18 C19 S4 111.6(3) . . ? C18 C19 H24 109.3 . . ? S4 C19 H24 109.3 . . ? C18 C19 H25 109.3 . . ? S4 C19 H25 109.3 . . ? H24 C19 H25 108.0 . . ? S4 C20 H26 109.5 . . ? S4 C20 H27 109.5 . . ? H26 C20 H27 109.5 . . ? S4 C20 H28 109.5 . . ? H26 C20 H28 109.5 . . ? H27 C20 H28 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.675 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.143 #===END OF CIF ============================================================== # 06nts003 data_06nts003 _database_code_depnum_ccdc_archive 'CCDC 621500' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-03-16 _chemical_name_systematic ; trans-dichlorobis(1,2-bis(methylthiomethyl)benzene)ruthenium(II) ; _chemical_name_common ;trans-dichlorobis(1,2- bis(methylthiomethyl)benzene)ruthenium(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Cl2 Ru S4' _chemical_formula_sum 'C20 H28 Cl2 Ru S4' _chemical_formula_weight 568.63 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' 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' Ru Ru -1.2594 0.8363 '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_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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 8.401(2) _cell_length_b 9.182(2) _cell_length_c 15.308(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.282(10) _cell_angle_gamma 90.00 _cell_volume 1158.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2752 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8164 # 0.9391 _exptl_absorpt_correction_T_max 1.0000 # 0.9628 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' # damien _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11787 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2645 _reflns_number_gt 2311 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+1.0774P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2645 _refine_ls_number_parameters 126 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Ru1 Ru 0.5000 0.0000 0.0000 0.01691(8) Uani 1 2 d S . . Cl1 Cl 0.57648(7) -0.16067(6) 0.12635(4) 0.02492(14) Uani 1 1 d . . . S1 S 0.44748(7) 0.17250(6) 0.10477(4) 0.02265(14) Uani 1 1 d . . . S2 S 0.78103(7) 0.03633(6) 0.01123(4) 0.02040(13) Uani 1 1 d . . . C1 C 0.4108(3) 0.3516(3) 0.05715(18) 0.0316(6) Uani 1 1 d . . . H1A H 0.3879 0.4192 0.1026 0.047 Uiso 1 1 calc R . . H1B H 0.3176 0.3482 0.0074 0.047 Uiso 1 1 calc R . . H1C H 0.5070 0.3847 0.0355 0.047 Uiso 1 1 calc R . . C2 C 0.6157(3) 0.2092(3) 0.19740(15) 0.0266(5) Uani 1 1 d . . . H2A H 0.5710 0.2553 0.2459 0.032 Uiso 1 1 calc R . . H2B H 0.6637 0.1149 0.2202 0.032 Uiso 1 1 calc R . . C3 C 0.7498(3) 0.3049(3) 0.17733(14) 0.0242(5) Uani 1 1 d . . . C4 C 0.7451(3) 0.4542(3) 0.19398(17) 0.0321(6) Uani 1 1 d . . . H4 H 0.6566 0.4931 0.2167 0.038 Uiso 1 1 calc R . . C5 C 0.8663(3) 0.5469(3) 0.17814(18) 0.0356(6) Uani 1 1 d . . . H5 H 0.8596 0.6485 0.1886 0.043 Uiso 1 1 calc R . . C6 C 0.9973(3) 0.4904(3) 0.14687(18) 0.0341(6) Uani 1 1 d . . . H6 H 1.0819 0.5528 0.1365 0.041 Uiso 1 1 calc R . . C7 C 1.0045(3) 0.3419(3) 0.13065(16) 0.0291(6) Uani 1 1 d . . . H7 H 1.0955 0.3035 0.1101 0.035 Uiso 1 1 calc R . . C8 C 0.8810(3) 0.2483(3) 0.14386(14) 0.0234(5) Uani 1 1 d . . . C9 C 0.8941(3) 0.0903(3) 0.12114(14) 0.0230(5) Uani 1 1 d . . . H9A H 0.8551 0.0312 0.1668 0.028 Uiso 1 1 calc R . . H9B H 1.0101 0.0665 0.1245 0.028 Uiso 1 1 calc R . . C10 C 0.8248(3) 0.1865(3) -0.05627(15) 0.0264(5) Uani 1 1 d . . . H10A H 0.7754 0.2756 -0.0384 0.040 Uiso 1 1 calc R . . H10B H 0.7801 0.1659 -0.1191 0.040 Uiso 1 1 calc R . . H10C H 0.9426 0.1995 -0.0480 0.040 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 Ru1 0.01875(14) 0.01877(14) 0.01476(13) 0.00239(10) 0.00709(9) 0.00214(10) Cl1 0.0273(3) 0.0273(3) 0.0217(3) 0.0093(2) 0.0088(2) 0.0048(2) S1 0.0219(3) 0.0248(3) 0.0235(3) -0.0031(2) 0.0100(2) 0.0013(2) S2 0.0214(3) 0.0229(3) 0.0185(3) 0.0000(2) 0.0078(2) 0.0011(2) C1 0.0284(14) 0.0234(13) 0.0410(15) -0.0043(11) 0.0023(11) 0.0057(10) C2 0.0271(13) 0.0363(14) 0.0184(11) -0.0056(10) 0.0088(10) 0.0030(11) C3 0.0267(13) 0.0280(13) 0.0163(11) -0.0021(9) 0.0006(9) 0.0022(10) C4 0.0306(14) 0.0336(14) 0.0284(13) -0.0119(11) -0.0029(11) 0.0079(11) C5 0.0373(16) 0.0261(13) 0.0360(14) -0.0063(11) -0.0107(12) 0.0017(11) C6 0.0378(15) 0.0321(14) 0.0292(13) 0.0022(11) -0.0012(11) -0.0064(12) C7 0.0280(14) 0.0350(14) 0.0244(12) -0.0005(11) 0.0053(10) -0.0008(11) C8 0.0265(13) 0.0269(12) 0.0157(10) 0.0001(9) 0.0013(9) 0.0023(10) C9 0.0218(12) 0.0275(13) 0.0196(11) 0.0001(10) 0.0039(9) 0.0030(9) C10 0.0289(13) 0.0310(13) 0.0210(11) 0.0052(10) 0.0086(10) -0.0020(10) _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 Ru1 S1 2.3565(6) . ? Ru1 S1 2.3565(6) 3_655 ? Ru1 S2 2.3571(8) 3_655 ? Ru1 S2 2.3571(8) . ? Ru1 Cl1 2.4175(6) . ? Ru1 Cl1 2.4175(6) 3_655 ? S1 C1 1.801(3) . ? S1 C2 1.827(2) . ? S2 C10 1.803(2) . ? S2 C9 1.831(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.507(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.396(3) . ? C3 C8 1.403(3) . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.389(4) . ? C6 H6 0.9500 . ? C7 C8 1.392(3) . ? C7 H7 0.9500 . ? C8 C9 1.501(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 S1 Ru1 S1 180.00(3) . 3_655 ? S1 Ru1 S2 80.01(2) . 3_655 ? S1 Ru1 S2 99.99(2) 3_655 3_655 ? S1 Ru1 S2 99.99(2) . . ? S1 Ru1 S2 80.01(2) 3_655 . ? S2 Ru1 S2 180.00(3) 3_655 . ? S1 Ru1 Cl1 85.49(3) . . ? S1 Ru1 Cl1 94.51(3) 3_655 . ? S2 Ru1 Cl1 94.45(2) 3_655 . ? S2 Ru1 Cl1 85.55(2) . . ? S1 Ru1 Cl1 94.51(3) . 3_655 ? S1 Ru1 Cl1 85.49(3) 3_655 3_655 ? S2 Ru1 Cl1 85.55(2) 3_655 3_655 ? S2 Ru1 Cl1 94.45(2) . 3_655 ? Cl1 Ru1 Cl1 180.00(3) . 3_655 ? C1 S1 C2 101.00(12) . . ? C1 S1 Ru1 112.22(9) . . ? C2 S1 Ru1 115.66(8) . . ? C10 S2 C9 101.09(11) . . ? C10 S2 Ru1 112.33(8) . . ? C9 S2 Ru1 115.94(8) . . ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 116.42(16) . . ? C3 C2 H2A 108.2 . . ? S1 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? S1 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C8 118.8(2) . . ? C4 C3 C2 119.1(2) . . ? C8 C3 C2 122.1(2) . . ? C5 C4 C3 121.6(2) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 119.7(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 121.4(2) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C7 C8 C3 119.0(2) . . ? C7 C8 C9 118.2(2) . . ? C3 C8 C9 122.7(2) . . ? C8 C9 S2 115.22(16) . . ? C8 C9 H9A 108.5 . . ? S2 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? S2 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # S1 Ru1 S1 C1 -13(100) 3_655 . . . ? # S1 Ru1 S1 C2 -128(100) 3_655 . . . ? # S2 Ru1 S2 C10 52(100) 3_655 . . . ? # S2 Ru1 S2 C9 167(100) 3_655 . . . ? S2 Ru1 S1 C1 -94.77(10) 3_655 . . . ? S2 Ru1 S1 C1 85.23(10) . . . . ? Cl1 Ru1 S1 C1 169.90(10) . . . . ? Cl1 Ru1 S1 C1 -10.10(10) 3_655 . . . ? S2 Ru1 S1 C2 150.09(9) 3_655 . . . ? S2 Ru1 S1 C2 -29.91(9) . . . . ? Cl1 Ru1 S1 C2 54.76(9) . . . . ? Cl1 Ru1 S1 C2 -125.24(9) 3_655 . . . ? S1 Ru1 S2 C10 -83.48(9) . . . . ? S1 Ru1 S2 C10 96.52(9) 3_655 . . . ? Cl1 Ru1 S2 C10 -168.10(9) . . . . ? Cl1 Ru1 S2 C10 11.90(9) 3_655 . . . ? S1 Ru1 S2 C9 32.06(9) . . . . ? S1 Ru1 S2 C9 -147.94(9) 3_655 . . . ? Cl1 Ru1 S2 C9 -52.57(9) . . . . ? Cl1 Ru1 S2 C9 127.43(9) 3_655 . . . ? C1 S1 C2 C3 -44.8(2) . . . . ? Ru1 S1 C2 C3 76.63(19) . . . . ? S1 C2 C3 C4 94.5(2) . . . . ? S1 C2 C3 C8 -86.6(3) . . . . ? C8 C3 C4 C5 0.1(4) . . . . ? C2 C3 C4 C5 179.0(2) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? C4 C5 C6 C7 0.9(4) . . . . ? C5 C6 C7 C8 1.0(4) . . . . ? C6 C7 C8 C3 -2.4(4) . . . . ? C6 C7 C8 C9 177.4(2) . . . . ? C4 C3 C8 C7 1.8(3) . . . . ? C2 C3 C8 C7 -177.1(2) . . . . ? C4 C3 C8 C9 -178.0(2) . . . . ? C2 C3 C8 C9 3.2(3) . . . . ? C7 C8 C9 S2 -97.2(2) . . . . ? C3 C8 C9 S2 82.6(2) . . . . ? C10 S2 C9 C8 42.4(2) . . . . ? Ru1 S2 C9 C8 -79.35(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.655 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.078 #===END OF CIF ============================================================== # 06nts004 data_06nts004 _database_code_depnum_ccdc_archive 'CCDC 621501' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-03-16 _chemical_name_systematic ; cis-dichlorobis(1,2-bis(methylselenomethyl)benzene)rhodium(III) hexafluorophosphate ; _chemical_name_common ; cis-dichlorobis(1,2- bis(methylselenomethyl)benzene)rhodium(iii) hexafluorophosphate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Cl2 Rh Se4 1+, F6 P 1-' _chemical_formula_sum 'C20 H28 Cl2 F6 P Rh Se4' _chemical_formula_weight 903.04 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** 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 12.515(2) _cell_length_b 12.0649(16) _cell_length_c 18.630(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.422(8) _cell_angle_gamma 90.00 _cell_volume 2800.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10717 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 6.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6234 # 0.5803 _exptl_absorpt_correction_T_max 1.0000 # 0.9415 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 45493 _diffrn_reflns_av_R_equivalents 0.1597 _diffrn_reflns_av_sigmaI/netI 0.1218 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.58 _reflns_number_total 6423 _reflns_number_gt 4051 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0043P)^2^+20.6816P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6423 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Rh1 Rh 0.88026(5) 0.08821(5) 0.19024(3) 0.02069(16) Uani 1 1 d . . . Cl1 Cl 1.01848(16) -0.03877(16) 0.22990(10) 0.0260(5) Uani 1 1 d . . . Cl2 Cl 0.73694(16) -0.03267(16) 0.20746(11) 0.0282(5) Uani 1 1 d . . . Se1 Se 1.03405(7) 0.19410(7) 0.15357(5) 0.0287(2) Uani 1 1 d . . . Se2 Se 0.87302(6) 0.15347(6) 0.31620(4) 0.02211(19) Uani 1 1 d . . . Se3 Se 0.89860(7) -0.00506(6) 0.07216(4) 0.0236(2) Uani 1 1 d . . . Se4 Se 0.75250(7) 0.23799(6) 0.16014(4) 0.0245(2) Uani 1 1 d . . . P1 P 0.83333(18) 0.17555(17) 0.56300(12) 0.0259(5) Uani 1 1 d . . . F1 F 0.7884(4) 0.1046(4) 0.6265(3) 0.0458(14) Uani 1 1 d . . . F2 F 0.7524(4) 0.2742(4) 0.5785(2) 0.0346(12) Uani 1 1 d . . . F3 F 0.9218(4) 0.2286(4) 0.6194(3) 0.0425(13) Uani 1 1 d . . . F4 F 0.9135(4) 0.0769(4) 0.5480(3) 0.0476(15) Uani 1 1 d . . . F5 F 0.7444(4) 0.1227(4) 0.5064(3) 0.0453(14) Uani 1 1 d . . . F6 F 0.8767(4) 0.2471(4) 0.5001(3) 0.0479(14) Uani 1 1 d . . . C1 C 0.9938(8) 0.3444(7) 0.1248(5) 0.050(3) Uani 1 1 d . . . H1A H 0.9726 0.3854 0.1666 0.075 Uiso 1 1 calc R . . H1B H 0.9335 0.3422 0.0872 0.075 Uiso 1 1 calc R . . H1C H 1.0550 0.3815 0.1060 0.075 Uiso 1 1 calc R . . C2 C 1.1428(6) 0.2308(7) 0.2341(4) 0.028(2) Uani 1 1 d . . . H2A H 1.1582 0.1630 0.2632 0.033 Uiso 1 1 calc R . . H2B H 1.2099 0.2523 0.2136 0.033 Uiso 1 1 calc R . . C3 C 1.1131(6) 0.3221(7) 0.2838(4) 0.028(2) Uani 1 1 d . . . C4 C 1.1457(7) 0.4307(6) 0.2714(5) 0.031(2) Uani 1 1 d . . . H4 H 1.1854 0.4462 0.2316 0.037 Uiso 1 1 calc R . . C5 C 1.1208(7) 0.5154(7) 0.3164(5) 0.032(2) Uani 1 1 d . . . H5 H 1.1445 0.5886 0.3079 0.039 Uiso 1 1 calc R . . C6 C 1.0618(7) 0.4948(7) 0.3734(5) 0.031(2) Uani 1 1 d . . . H6 H 1.0438 0.5540 0.4037 0.037 Uiso 1 1 calc R . . C7 C 1.0282(7) 0.3873(6) 0.3872(4) 0.028(2) Uani 1 1 d . . . H7 H 0.9883 0.3732 0.4271 0.034 Uiso 1 1 calc R . . C8 C 1.0532(6) 0.3007(6) 0.3424(4) 0.0215(18) Uani 1 1 d . . . C9 C 1.0187(6) 0.1848(6) 0.3597(4) 0.0241(19) Uani 1 1 d . . . H9A H 1.0212 0.1760 0.4127 0.029 Uiso 1 1 calc R . . H9B H 1.0693 0.1309 0.3416 0.029 Uiso 1 1 calc R . . C10 C 0.8591(7) 0.0156(6) 0.3679(4) 0.032(2) Uani 1 1 d . . . H10A H 0.9118 -0.0380 0.3534 0.048 Uiso 1 1 calc R . . H10B H 0.7866 -0.0142 0.3567 0.048 Uiso 1 1 calc R . . H10C H 0.8718 0.0292 0.4199 0.048 Uiso 1 1 calc R . . C11 C 0.8693(7) -0.1614(6) 0.0862(4) 0.029(2) Uani 1 1 d . . . H11A H 0.7963 -0.1702 0.1002 0.043 Uiso 1 1 calc R . . H11B H 0.9208 -0.1911 0.1243 0.043 Uiso 1 1 calc R . . H11C H 0.8762 -0.2017 0.0412 0.043 Uiso 1 1 calc R . . C12 C 0.7763(7) 0.0208(6) 0.0008(4) 0.027(2) Uani 1 1 d . . . H12A H 0.7777 -0.0330 -0.0393 0.033 Uiso 1 1 calc R . . H12B H 0.7084 0.0105 0.0233 0.033 Uiso 1 1 calc R . . C13 C 0.7821(7) 0.1368(6) -0.0278(4) 0.026(2) Uani 1 1 d . . . C14 C 0.8369(7) 0.1597(7) -0.0862(4) 0.031(2) Uani 1 1 d . . . H14 H 0.8693 0.1004 -0.1097 0.038 Uiso 1 1 calc R . . C15 C 0.8468(7) 0.2659(8) -0.1122(5) 0.036(2) Uani 1 1 d . . . H15 H 0.8858 0.2794 -0.1527 0.043 Uiso 1 1 calc R . . C16 C 0.7995(7) 0.3521(7) -0.0786(5) 0.035(2) Uani 1 1 d . . . H16 H 0.8069 0.4257 -0.0955 0.042 Uiso 1 1 calc R . . C17 C 0.7412(7) 0.3323(7) -0.0204(5) 0.033(2) Uani 1 1 d . . . H17 H 0.7076 0.3919 0.0020 0.039 Uiso 1 1 calc R . . C18 C 0.7322(6) 0.2249(7) 0.0051(4) 0.028(2) Uani 1 1 d . . . C19 C 0.6664(7) 0.2082(7) 0.0684(4) 0.033(2) Uani 1 1 d . . . H19A H 0.6396 0.1310 0.0682 0.039 Uiso 1 1 calc R . . H19B H 0.6036 0.2584 0.0635 0.039 Uiso 1 1 calc R . . C20 C 0.6339(6) 0.2183(7) 0.2192(4) 0.027(2) Uani 1 1 d . . . H20A H 0.5807 0.2770 0.2081 0.041 Uiso 1 1 calc R . . H20B H 0.6607 0.2222 0.2702 0.041 Uiso 1 1 calc R . . H20C H 0.6004 0.1459 0.2089 0.041 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 Rh1 0.0229(4) 0.0197(3) 0.0188(3) -0.0016(3) -0.0014(3) -0.0008(3) Cl1 0.0281(12) 0.0273(10) 0.0218(11) -0.0017(9) -0.0023(9) 0.0038(8) Cl2 0.0285(12) 0.0244(10) 0.0311(12) -0.0006(9) 0.0003(9) -0.0038(8) Se1 0.0297(5) 0.0345(5) 0.0215(5) -0.0024(4) 0.0006(4) -0.0085(4) Se2 0.0240(5) 0.0222(4) 0.0197(4) -0.0018(3) -0.0002(3) -0.0026(3) Se3 0.0275(5) 0.0219(4) 0.0203(4) -0.0012(3) -0.0032(4) 0.0028(3) Se4 0.0281(5) 0.0227(4) 0.0220(4) -0.0010(4) -0.0008(4) 0.0028(4) P1 0.0285(13) 0.0236(11) 0.0251(12) -0.0016(9) -0.0004(10) 0.0024(9) F1 0.067(4) 0.031(3) 0.040(3) 0.009(2) 0.009(3) -0.009(3) F2 0.036(3) 0.032(3) 0.036(3) 0.002(2) 0.004(2) 0.011(2) F3 0.038(3) 0.042(3) 0.045(3) -0.006(2) -0.013(3) -0.005(2) F4 0.051(4) 0.050(3) 0.041(3) -0.010(3) -0.003(3) 0.028(3) F5 0.049(4) 0.042(3) 0.041(3) -0.010(2) -0.017(3) 0.003(2) F6 0.053(4) 0.058(3) 0.036(3) 0.016(3) 0.016(3) 0.001(3) C1 0.049(7) 0.047(6) 0.049(6) 0.033(5) -0.021(5) -0.023(5) C2 0.026(5) 0.039(5) 0.017(4) 0.001(4) 0.000(4) -0.004(4) C3 0.022(5) 0.032(5) 0.028(5) -0.003(4) -0.007(4) -0.004(4) C4 0.026(5) 0.028(5) 0.039(5) 0.004(4) -0.003(4) 0.003(4) C5 0.037(6) 0.019(4) 0.040(5) 0.000(4) -0.001(4) -0.007(4) C6 0.030(5) 0.030(5) 0.034(5) -0.004(4) 0.006(4) 0.000(4) C7 0.034(5) 0.031(5) 0.019(4) -0.001(4) 0.000(4) -0.001(4) C8 0.017(4) 0.023(4) 0.023(4) -0.002(3) -0.005(4) 0.001(3) C9 0.021(5) 0.033(5) 0.017(4) -0.005(4) -0.007(3) -0.003(4) C10 0.049(6) 0.031(5) 0.016(4) 0.002(4) 0.005(4) -0.018(4) C11 0.036(5) 0.023(4) 0.026(5) 0.002(4) -0.003(4) 0.005(4) C12 0.030(5) 0.022(4) 0.026(5) -0.001(4) -0.018(4) 0.003(4) C13 0.032(5) 0.025(4) 0.017(4) 0.000(4) -0.013(4) 0.002(4) C14 0.029(5) 0.042(5) 0.022(5) 0.003(4) -0.005(4) 0.012(4) C15 0.027(5) 0.051(6) 0.030(5) 0.005(5) 0.000(4) 0.007(4) C16 0.035(6) 0.030(5) 0.037(6) 0.009(4) -0.010(4) 0.005(4) C17 0.039(6) 0.033(5) 0.026(5) -0.006(4) -0.002(4) 0.004(4) C18 0.024(5) 0.032(5) 0.025(5) 0.001(4) -0.010(4) 0.001(4) C19 0.035(5) 0.037(5) 0.025(5) -0.011(4) -0.001(4) 0.004(4) C20 0.018(5) 0.031(5) 0.033(5) -0.004(4) 0.002(4) 0.006(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 Rh1 Cl2 2.357(2) . ? Rh1 Cl1 2.376(2) . ? Rh1 Se4 2.4427(10) . ? Rh1 Se1 2.4601(11) . ? Rh1 Se2 2.4849(11) . ? Rh1 Se3 2.5005(11) . ? Se1 C1 1.944(9) . ? Se1 C2 1.978(7) . ? Se2 C10 1.939(7) . ? Se2 C9 1.961(7) . ? Se3 C11 1.944(7) . ? Se3 C12 1.956(7) . ? Se4 C20 1.944(8) . ? Se4 C19 1.966(8) . ? P1 F3 1.587(5) . ? P1 F6 1.591(5) . ? P1 F5 1.592(5) . ? P1 F4 1.599(5) . ? P1 F1 1.604(5) . ? P1 F2 1.607(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.508(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.399(11) . ? C3 C8 1.404(11) . ? C4 C5 1.376(11) . ? C4 H4 0.9500 . ? C5 C6 1.372(12) . ? C5 H5 0.9500 . ? C6 C7 1.395(11) . ? C6 H6 0.9500 . ? C7 C8 1.390(11) . ? C7 H7 0.9500 . ? C8 C9 1.507(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.501(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.369(12) . ? C13 C18 1.403(11) . ? C14 C15 1.379(12) . ? C14 H14 0.9500 . ? C15 C16 1.375(12) . ? C15 H15 0.9500 . ? C16 C17 1.384(12) . ? C16 H16 0.9500 . ? C17 C18 1.388(11) . ? C17 H17 0.9500 . ? C18 C19 1.513(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 Cl2 Rh1 Cl1 95.72(7) . . ? Cl2 Rh1 Se4 89.94(6) . . ? Cl1 Rh1 Se4 171.90(6) . . ? Cl2 Rh1 Se1 169.91(6) . . ? Cl1 Rh1 Se1 81.69(6) . . ? Se4 Rh1 Se1 93.69(4) . . ? Cl2 Rh1 Se2 88.36(6) . . ? Cl1 Rh1 Se2 90.06(5) . . ? Se4 Rh1 Se2 84.31(3) . . ? Se1 Rh1 Se2 101.36(4) . . ? Cl2 Rh1 Se3 88.60(6) . . ? Cl1 Rh1 Se3 81.88(5) . . ? Se4 Rh1 Se3 104.09(3) . . ? Se1 Rh1 Se3 81.38(3) . . ? Se2 Rh1 Se3 171.06(4) . . ? C1 Se1 C2 98.2(4) . . ? C1 Se1 Rh1 111.8(3) . . ? C2 Se1 Rh1 113.9(2) . . ? C10 Se2 C9 94.8(3) . . ? C10 Se2 Rh1 102.2(2) . . ? C9 Se2 Rh1 109.7(2) . . ? C11 Se3 C12 95.8(3) . . ? C11 Se3 Rh1 106.5(2) . . ? C12 Se3 Rh1 113.3(3) . . ? C20 Se4 C19 94.9(4) . . ? C20 Se4 Rh1 107.4(2) . . ? C19 Se4 Rh1 110.9(3) . . ? F3 P1 F6 90.2(3) . . ? F3 P1 F5 179.8(3) . . ? F6 P1 F5 89.8(3) . . ? F3 P1 F4 90.3(3) . . ? F6 P1 F4 90.7(3) . . ? F5 P1 F4 89.8(3) . . ? F3 P1 F1 89.9(3) . . ? F6 P1 F1 179.2(3) . . ? F5 P1 F1 90.1(3) . . ? F4 P1 F1 90.1(3) . . ? F3 P1 F2 89.7(3) . . ? F6 P1 F2 89.7(3) . . ? F5 P1 F2 90.1(3) . . ? F4 P1 F2 179.6(3) . . ? F1 P1 F2 89.5(3) . . ? Se1 C1 H1A 109.5 . . ? Se1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Se1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Se1 116.0(5) . . ? C3 C2 H2A 108.3 . . ? Se1 C2 H2A 108.3 . . ? C3 C2 H2B 108.3 . . ? Se1 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C8 119.1(8) . . ? C4 C3 C2 119.3(8) . . ? C8 C3 C2 121.6(7) . . ? C5 C4 C3 120.6(9) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.4(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.3(8) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.0(8) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C3 119.6(7) . . ? C7 C8 C9 118.9(7) . . ? C3 C8 C9 121.4(7) . . ? C8 C9 Se2 111.4(5) . . ? C8 C9 H9A 109.4 . . ? Se2 C9 H9A 109.4 . . ? C8 C9 H9B 109.4 . . ? Se2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? Se2 C10 H10A 109.5 . . ? Se2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Se2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Se3 C11 H11A 109.5 . . ? Se3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Se3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 Se3 109.2(5) . . ? C13 C12 H12A 109.8 . . ? Se3 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? Se3 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C14 C13 C18 118.2(8) . . ? C14 C13 C12 121.0(8) . . ? C18 C13 C12 120.9(8) . . ? C13 C14 C15 122.3(8) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C16 C15 C14 119.1(9) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 120.5(8) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 119.7(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C13 120.2(8) . . ? C17 C18 C19 117.3(8) . . ? C13 C18 C19 122.4(7) . . ? C18 C19 Se4 111.0(6) . . ? C18 C19 H19A 109.4 . . ? Se4 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? Se4 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? Se4 C20 H20A 109.5 . . ? Se4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Se4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # Se3 Rh1 Se2 C10 -25.8(4) . . . . ? # Se3 Rh1 Se2 C9 73.9(4) . . . . ? # Se2 Rh1 Se3 C11 33.3(4) . . . . ? # Se2 Rh1 Se3 C12 137.4(4) . . . . ? # Cl1 Rh1 Se4 C20 -99.7(5) . . . . ? # Cl1 Rh1 Se4 C19 157.9(5) . . . . ? Cl2 Rh1 Se1 C1 114.7(5) . . . . ? Cl1 Rh1 Se1 C1 -169.5(3) . . . . ? Se4 Rh1 Se1 C1 3.8(3) . . . . ? Se2 Rh1 Se1 C1 -81.2(3) . . . . ? Se3 Rh1 Se1 C1 107.5(3) . . . . ? Cl2 Rh1 Se1 C2 -135.1(4) . . . . ? Cl1 Rh1 Se1 C2 -59.3(3) . . . . ? Se4 Rh1 Se1 C2 114.0(3) . . . . ? Se2 Rh1 Se1 C2 29.0(3) . . . . ? Se3 Rh1 Se1 C2 -142.3(3) . . . . ? Cl2 Rh1 Se2 C10 44.4(3) . . . . ? Cl1 Rh1 Se2 C10 -51.3(3) . . . . ? Se4 Rh1 Se2 C10 134.5(3) . . . . ? Se1 Rh1 Se2 C10 -132.8(3) . . . . ? Cl2 Rh1 Se2 C9 144.1(2) . . . . ? Cl1 Rh1 Se2 C9 48.4(2) . . . . ? Se4 Rh1 Se2 C9 -125.8(2) . . . . ? Se1 Rh1 Se2 C9 -33.2(2) . . . . ? Cl2 Rh1 Se3 C11 -36.8(3) . . . . ? Cl1 Rh1 Se3 C11 59.2(3) . . . . ? Se4 Rh1 Se3 C11 -126.4(3) . . . . ? Se1 Rh1 Se3 C11 141.9(3) . . . . ? Cl2 Rh1 Se3 C12 67.2(3) . . . . ? Cl1 Rh1 Se3 C12 163.2(3) . . . . ? Se4 Rh1 Se3 C12 -22.4(3) . . . . ? Se1 Rh1 Se3 C12 -114.1(3) . . . . ? Cl2 Rh1 Se4 C20 34.8(3) . . . . ? Se1 Rh1 Se4 C20 -154.6(2) . . . . ? Se2 Rh1 Se4 C20 -53.6(2) . . . . ? Se3 Rh1 Se4 C20 123.3(2) . . . . ? Cl2 Rh1 Se4 C19 -67.6(3) . . . . ? Se1 Rh1 Se4 C19 103.0(3) . . . . ? Se2 Rh1 Se4 C19 -156.0(3) . . . . ? Se3 Rh1 Se4 C19 20.9(3) . . . . ? C1 Se1 C2 C3 43.4(7) . . . . ? Rh1 Se1 C2 C3 -74.9(6) . . . . ? Se1 C2 C3 C4 -94.4(8) . . . . ? Se1 C2 C3 C8 85.5(8) . . . . ? C8 C3 C4 C5 0.8(12) . . . . ? C2 C3 C4 C5 -179.3(7) . . . . ? C3 C4 C5 C6 -1.2(13) . . . . ? C4 C5 C6 C7 1.2(13) . . . . ? C5 C6 C7 C8 -0.9(12) . . . . ? C6 C7 C8 C3 0.6(11) . . . . ? C6 C7 C8 C9 178.2(7) . . . . ? C4 C3 C8 C7 -0.5(11) . . . . ? C2 C3 C8 C7 179.6(7) . . . . ? C4 C3 C8 C9 -178.1(7) . . . . ? C2 C3 C8 C9 2.0(11) . . . . ? C7 C8 C9 Se2 87.5(7) . . . . ? C3 C8 C9 Se2 -94.9(8) . . . . ? C10 Se2 C9 C8 -169.7(6) . . . . ? Rh1 Se2 C9 C8 85.6(6) . . . . ? C11 Se3 C12 C13 -174.4(6) . . . . ? Rh1 Se3 C12 C13 74.9(6) . . . . ? Se3 C12 C13 C14 88.9(8) . . . . ? Se3 C12 C13 C18 -90.5(8) . . . . ? C18 C13 C14 C15 1.7(12) . . . . ? C12 C13 C14 C15 -177.7(7) . . . . ? C13 C14 C15 C16 -0.4(13) . . . . ? C14 C15 C16 C17 -1.1(13) . . . . ? C15 C16 C17 C18 1.2(12) . . . . ? C16 C17 C18 C13 0.2(12) . . . . ? C16 C17 C18 C19 -179.3(7) . . . . ? C14 C13 C18 C17 -1.6(11) . . . . ? C12 C13 C18 C17 177.9(7) . . . . ? C14 C13 C18 C19 177.9(7) . . . . ? C12 C13 C18 C19 -2.7(11) . . . . ? C17 C18 C19 Se4 -83.5(8) . . . . ? C13 C18 C19 Se4 97.0(8) . . . . ? C20 Se4 C19 C18 175.5(6) . . . . ? Rh1 Se4 C19 C18 -73.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.798 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.200 #===END OF CIF ============================================================== # 05nts005 data_05nts005 _database_code_depnum_ccdc_archive 'CCDC 621502' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-03-17 _chemical_name_systematic ; bis(1,2-bis(methylthiomethyl)benzene)copper(I) tetrafluoroborate ; _chemical_name_common ;bis(1,2-bis(methylthiomethyl)benzene)copper(i) tetrafluoroborate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 CU S4 1+, B F4 1-' _chemical_formula_sum 'C20 H28 B Cu F4 S4' _chemical_formula_weight 547.01 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 '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 2/n' _symmetry_Int_Tables_number 13 # Superceded ** _symmetry_space_group_name_Hall '-P 2yac' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 10.111(3) _cell_length_b 7.746(2) _cell_length_c 15.129(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.987(12) _cell_angle_gamma 90.00 _cell_volume 1154.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2740 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 # 0.21 +/- 0.02 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5873 # 0.7653 _exptl_absorpt_correction_T_max 1.0000 # 0.9607 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10037 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2637 _reflns_number_gt 1799 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.2726P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2637 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Cu1 Cu 0.7500 0.38791(6) 0.7500 0.02223(15) Uani 1 2 d S . . S1 S 0.76612(8) 0.18536(9) 0.63916(5) 0.02399(19) Uani 1 1 d . . . S2 S 0.94988(7) 0.53487(9) 0.79417(5) 0.02396(19) Uani 1 1 d . . . B1 B 0.2500 0.9989(6) 0.7500 0.0273(11) Uani 1 2 d S . . F1 F 0.1341(2) 1.1011(2) 0.73506(12) 0.0457(5) Uani 1 1 d . . . F2 F 0.25323(19) 0.8942(2) 0.82556(11) 0.0401(5) Uani 1 1 d . . . C1 C 0.6053(3) 0.1943(4) 0.5581(2) 0.0335(8) Uani 1 1 d . . . H1A H 0.5862 0.3137 0.5378 0.050 Uiso 1 1 calc R . . H1B H 0.5333 0.1529 0.5866 0.050 Uiso 1 1 calc R . . H1C H 0.6091 0.1212 0.5059 0.050 Uiso 1 1 calc R . . C2 C 0.8805(3) 0.2698(3) 0.57181(18) 0.0234(7) Uani 1 1 d . . . H2A H 0.9753 0.2492 0.6050 0.028 Uiso 1 1 calc R . . H2B H 0.8656 0.2050 0.5140 0.028 Uiso 1 1 calc R . . C3 C 0.8626(3) 0.4588(4) 0.55091(18) 0.0206(6) Uani 1 1 d . . . C4 C 0.7760(3) 0.5063(4) 0.46889(18) 0.0239(7) Uani 1 1 d . . . H4 H 0.7295 0.4191 0.4297 0.029 Uiso 1 1 calc R . . C5 C 0.7565(3) 0.6783(4) 0.44362(19) 0.0251(7) Uani 1 1 d . . . H5 H 0.6968 0.7085 0.3878 0.030 Uiso 1 1 calc R . . C6 C 0.8245(3) 0.8052(4) 0.49998(19) 0.0253(7) Uani 1 1 d . . . H6 H 0.8114 0.9231 0.4830 0.030 Uiso 1 1 calc R . . C7 C 0.9121(3) 0.7612(4) 0.58155(18) 0.0235(6) Uani 1 1 d . . . H7 H 0.9592 0.8495 0.6196 0.028 Uiso 1 1 calc R . . C8 C 0.9315(3) 0.5889(3) 0.60828(18) 0.0207(6) Uani 1 1 d . . . C9 C 1.0289(3) 0.5476(4) 0.69672(18) 0.0241(7) Uani 1 1 d . . . H9A H 1.1004 0.6373 0.7089 0.029 Uiso 1 1 calc R . . H9B H 1.0734 0.4359 0.6904 0.029 Uiso 1 1 calc R . . C10 C 0.9204(3) 0.7601(4) 0.81274(19) 0.0312(7) Uani 1 1 d . . . H10A H 1.0076 0.8201 0.8311 0.047 Uiso 1 1 calc R . . H10B H 0.8698 0.7714 0.8606 0.047 Uiso 1 1 calc R . . H10C H 0.8678 0.8114 0.7565 0.047 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 Cu1 0.0215(3) 0.0224(3) 0.0226(3) 0.000 0.0046(2) 0.000 S1 0.0275(4) 0.0185(4) 0.0272(4) -0.0023(3) 0.0088(3) -0.0013(3) S2 0.0228(4) 0.0261(4) 0.0212(4) 0.0005(3) 0.0012(3) -0.0020(3) B1 0.030(3) 0.023(3) 0.026(3) 0.000 0.002(2) 0.000 F1 0.0439(13) 0.0417(11) 0.0463(11) 0.0024(9) -0.0007(9) 0.0187(10) F2 0.0410(12) 0.0386(11) 0.0381(11) 0.0099(9) 0.0032(9) 0.0037(9) C1 0.0257(18) 0.0364(18) 0.0381(18) -0.0129(15) 0.0070(14) -0.0084(15) C2 0.0229(17) 0.0226(16) 0.0251(15) -0.0038(12) 0.0066(12) -0.0001(13) C3 0.0202(15) 0.0205(15) 0.0227(14) -0.0019(12) 0.0084(12) 0.0025(13) C4 0.0243(17) 0.0246(16) 0.0228(15) -0.0045(13) 0.0054(12) -0.0033(13) C5 0.0219(17) 0.0280(16) 0.0244(15) 0.0021(13) 0.0029(12) -0.0008(13) C6 0.0291(18) 0.0176(14) 0.0317(16) 0.0016(13) 0.0119(13) 0.0019(13) C7 0.0258(17) 0.0217(15) 0.0249(15) -0.0047(13) 0.0102(13) -0.0042(13) C8 0.0179(15) 0.0237(15) 0.0223(14) -0.0019(13) 0.0086(12) 0.0015(12) C9 0.0209(16) 0.0250(15) 0.0255(15) -0.0023(13) 0.0031(12) -0.0024(13) C10 0.0299(18) 0.0339(18) 0.0291(16) -0.0099(14) 0.0053(13) -0.0050(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 Cu1 S2 2.2846(9) . ? Cu1 S2 2.2846(9) 2_656 ? Cu1 S1 2.3288(8) . ? Cu1 S1 2.3288(8) 2_656 ? S1 C1 1.804(3) . ? S1 C2 1.826(3) . ? S2 C10 1.803(3) . ? S2 C9 1.830(3) . ? B1 F1 1.390(3) 2_556 ? B1 F1 1.390(3) . ? B1 F2 1.396(3) . ? B1 F2 1.396(3) 2_556 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.500(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.398(4) . ? C3 C8 1.408(4) . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.379(4) . ? C5 H5 0.9500 . ? C6 C7 1.390(4) . ? C6 H6 0.9500 . ? C7 C8 1.396(4) . ? C7 H7 0.9500 . ? C8 C9 1.506(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 S2 Cu1 S2 120.23(5) . 2_656 ? S2 Cu1 S1 110.24(3) . . ? S2 Cu1 S1 109.00(3) 2_656 . ? S2 Cu1 S1 109.00(3) . 2_656 ? S2 Cu1 S1 110.24(3) 2_656 2_656 ? S1 Cu1 S1 95.29(4) . 2_656 ? C1 S1 C2 101.17(14) . . ? C1 S1 Cu1 105.39(10) . . ? C2 S1 Cu1 108.42(9) . . ? C10 S2 C9 100.99(14) . . ? C10 S2 Cu1 111.19(10) . . ? C9 S2 Cu1 107.97(9) . . ? F1 B1 F1 110.5(4) 2_556 . ? F1 B1 F2 109.51(11) 2_556 . ? F1 B1 F2 109.14(11) . . ? F1 B1 F2 109.14(11) 2_556 2_556 ? F1 B1 F2 109.51(11) . 2_556 ? F2 B1 F2 109.0(3) . 2_556 ? S1 C1 H1A 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 S1 113.96(19) . . ? C3 C2 H2A 108.8 . . ? S1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? S1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C8 118.9(2) . . ? C4 C3 C2 117.7(2) . . ? C8 C3 C2 123.3(2) . . ? C5 C4 C3 121.2(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C3 119.2(2) . . ? C7 C8 C9 118.8(2) . . ? C3 C8 C9 122.0(2) . . ? C8 C9 S2 114.3(2) . . ? C8 C9 H9A 108.7 . . ? S2 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? S2 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Cu1 S1 C1 -139.76(11) . . . . ? S2 Cu1 S1 C1 -5.78(11) 2_656 . . . ? S1 Cu1 S1 C1 107.75(11) 2_656 . . . ? S2 Cu1 S1 C2 -32.09(10) . . . . ? S2 Cu1 S1 C2 101.89(10) 2_656 . . . ? S1 Cu1 S1 C2 -144.58(10) 2_656 . . . ? S2 Cu1 S2 C10 12.97(10) 2_656 . . . ? S1 Cu1 S2 C10 141.02(10) . . . . ? S1 Cu1 S2 C10 -115.64(11) 2_656 . . . ? S2 Cu1 S2 C9 -96.96(10) 2_656 . . . ? S1 Cu1 S2 C9 31.09(10) . . . . ? S1 Cu1 S2 C9 134.44(10) 2_656 . . . ? C1 S1 C2 C3 70.0(2) . . . . ? Cu1 S1 C2 C3 -40.6(2) . . . . ? S1 C2 C3 C4 -93.6(3) . . . . ? S1 C2 C3 C8 88.3(3) . . . . ? C8 C3 C4 C5 -0.3(4) . . . . ? C2 C3 C4 C5 -178.5(3) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C5 C6 C7 C8 -0.7(4) . . . . ? C6 C7 C8 C3 0.9(4) . . . . ? C6 C7 C8 C9 179.2(3) . . . . ? C4 C3 C8 C7 -0.3(4) . . . . ? C2 C3 C8 C7 177.7(2) . . . . ? C4 C3 C8 C9 -178.6(3) . . . . ? C2 C3 C8 C9 -0.6(4) . . . . ? C7 C8 C9 S2 92.0(3) . . . . ? C3 C8 C9 S2 -89.7(3) . . . . ? C10 S2 C9 C8 -74.2(2) . . . . ? Cu1 S2 C9 C8 42.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.398 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.088 #===END OF CIF ============================================================== # 06mnh001 data_06mnh001 _database_code_depnum_ccdc_archive 'CCDC 621503' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-10-25 _audit_update_record ; 2006-10-25 Set sof C30 to 21, added C30A with sof -21 Rerefined. No H on C30A. ; _chemical_name_systematic ; bis(1,2-bis(methyltelluromethyl)benzene)silver(I) tetrafluoroborate ; _chemical_name_common ;bis(1,2-bis(methyltelluromethyl)benzene)silver(i) tetrafluoroborate ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Ag Te4 1+, B F4 1-' _chemical_formula_sum 'C20 H28 Ag B F4 Te4' _chemical_formula_weight 973.50 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' Ag Ag -0.8971 1.1015 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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/a' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yab' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _cell_length_a 15.8366(10) _cell_length_b 20.3931(15) _cell_length_c 16.5289(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.405(4) _cell_angle_gamma 90.00 _cell_volume 5266.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12442 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 5.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8417 # 0.4933 _exptl_absorpt_correction_T_max 1.0000 # 0.8207 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 101652 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.51 _reflns_number_total 12089 _reflns_number_gt 9316 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 'w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+16.0567P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12089 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ag1 Ag 0.82326(2) 0.453137(19) 0.56049(2) 0.01949(9) Uani 1 1 d . . . Ag2 Ag 0.68783(2) 0.549100(19) 0.97499(2) 0.02094(9) Uani 1 1 d . . . Te1 Te 0.91114(2) 0.546743(16) 0.481853(19) 0.01668(7) Uani 1 1 d . . . Te2 Te 0.74694(2) 0.532119(17) 0.66351(2) 0.01994(8) Uani 1 1 d . . . Te3 Te 0.73505(2) 0.384773(18) 0.42920(2) 0.02319(8) Uani 1 1 d . . . Te4 Te 0.93901(2) 0.364366(17) 0.64251(2) 0.02166(8) Uani 1 1 d . . . Te5 Te 0.58053(2) 0.647426(16) 0.90334(2) 0.01965(8) Uani 1 1 d . . . Te6 Te 0.84456(2) 0.599489(18) 1.04940(2) 0.02141(13) Uani 0.9395(14) 1 d P . . Te6A Te 0.8019(4) 0.6101(3) 1.0839(3) 0.0194(19) Uiso 0.0605(14) 1 d P . . Te7 Te 0.71939(2) 0.458562(17) 0.85689(2) 0.02021(8) Uani 1 1 d . . . Te8 Te 0.59981(2) 0.473291(17) 1.07604(2) 0.02057(8) Uani 1 1 d . . . C1 C 0.8876(3) 0.5022(3) 0.3631(3) 0.0253(12) Uani 1 1 d . . . H1A H 0.9202 0.4613 0.3641 0.038 Uiso 1 1 calc R . . H1B H 0.9054 0.5322 0.3227 0.038 Uiso 1 1 calc R . . H1C H 0.8264 0.4927 0.3480 0.038 Uiso 1 1 calc R . . C2 C 0.8286(3) 0.6306(2) 0.4476(3) 0.0196(11) Uani 1 1 d . . . H2A H 0.8448 0.6659 0.4883 0.024 Uiso 1 1 calc R . . H2B H 0.8392 0.6471 0.3938 0.024 Uiso 1 1 calc R . . C3 C 0.7354(3) 0.6175(2) 0.4420(3) 0.0192(11) Uani 1 1 d . . . C4 C 0.6865(3) 0.6097(2) 0.3642(3) 0.0201(11) Uani 1 1 d . . . H4 H 0.7136 0.6115 0.3170 0.024 Uiso 1 1 calc R . . C5 C 0.5988(3) 0.5994(3) 0.3550(3) 0.0277(13) Uani 1 1 d . . . H5 H 0.5665 0.5936 0.3018 0.033 Uiso 1 1 calc R . . C6 C 0.5582(3) 0.5975(3) 0.4231(3) 0.0287(13) Uani 1 1 d . . . H6 H 0.4981 0.5909 0.4168 0.034 Uiso 1 1 calc R . . C7 C 0.6059(3) 0.6053(3) 0.5000(3) 0.0247(12) Uani 1 1 d . . . H7 H 0.5781 0.6038 0.5467 0.030 Uiso 1 1 calc R . . C8 C 0.6944(3) 0.6153(2) 0.5109(3) 0.0202(11) Uani 1 1 d . . . C9 C 0.7413(3) 0.6240(3) 0.5964(3) 0.0227(11) Uani 1 1 d . . . H9A H 0.7119 0.6575 0.6250 0.027 Uiso 1 1 calc R . . H9B H 0.8001 0.6397 0.5945 0.027 Uiso 1 1 calc R . . C10 C 0.8599(4) 0.5588(3) 0.7461(4) 0.0323(14) Uani 1 1 d . . . H10A H 0.8762 0.5229 0.7850 0.048 Uiso 1 1 calc R . . H10B H 0.8487 0.5985 0.7762 0.048 Uiso 1 1 calc R . . H10C H 0.9064 0.5672 0.7151 0.048 Uiso 1 1 calc R . . C11 C 0.6073(4) 0.4138(3) 0.4325(4) 0.0400(15) Uani 1 1 d . . . H11A H 0.5980 0.4582 0.4102 0.060 Uiso 1 1 calc R . . H11B H 0.5968 0.4132 0.4893 0.060 Uiso 1 1 calc R . . H11C H 0.5679 0.3834 0.3996 0.060 Uiso 1 1 calc R . . C12 C 0.7234(3) 0.2886(2) 0.4831(3) 0.0229(11) Uani 1 1 d . . . H12A H 0.6751 0.2651 0.4496 0.028 Uiso 1 1 calc R . . H12B H 0.7762 0.2634 0.4798 0.028 Uiso 1 1 calc R . . C13 C 0.7090(3) 0.2887(2) 0.5709(3) 0.0186(11) Uani 1 1 d . . . C14 C 0.6254(3) 0.2930(2) 0.5856(3) 0.0234(12) Uani 1 1 d . . . H14 H 0.5803 0.2986 0.5406 0.028 Uiso 1 1 calc R . . C15 C 0.6059(3) 0.2892(3) 0.6643(3) 0.0241(12) Uani 1 1 d . . . H15 H 0.5483 0.2931 0.6732 0.029 Uiso 1 1 calc R . . C16 C 0.6717(3) 0.2797(3) 0.7299(3) 0.0247(12) Uani 1 1 d . . . H16 H 0.6594 0.2767 0.7841 0.030 Uiso 1 1 calc R . . C17 C 0.7556(3) 0.2747(3) 0.7160(3) 0.0243(12) Uani 1 1 d . . . H17 H 0.8001 0.2672 0.7610 0.029 Uiso 1 1 calc R . . C18 C 0.7759(3) 0.2803(2) 0.6372(3) 0.0200(11) Uani 1 1 d . . . C19 C 0.8673(3) 0.2728(3) 0.6281(3) 0.0230(11) Uani 1 1 d . . . H19A H 0.8702 0.2545 0.5732 0.028 Uiso 1 1 calc R . . H19B H 0.8948 0.2410 0.6694 0.028 Uiso 1 1 calc R . . C20 C 0.9272(4) 0.3772(3) 0.7688(3) 0.0295(13) Uani 1 1 d . . . H20A H 0.9561 0.4178 0.7895 0.044 Uiso 1 1 calc R . . H20B H 0.9537 0.3399 0.8008 0.044 Uiso 1 1 calc R . . H20C H 0.8665 0.3797 0.7739 0.044 Uiso 1 1 calc R . . C21 C 0.5693(4) 0.6269(3) 0.7749(3) 0.0340(14) Uani 1 1 d . . . H21A H 0.5349 0.5872 0.7618 0.051 Uiso 1 1 calc R . . H21B H 0.6264 0.6202 0.7607 0.051 Uiso 1 1 calc R . . H21C H 0.5415 0.6640 0.7434 0.051 Uiso 1 1 calc R . . C22 C 0.6583(3) 0.7344(3) 0.8973(3) 0.0252(12) Uani 1 1 d . . . H22A H 0.6253 0.7652 0.8579 0.030 Uiso 1 1 calc R . . H22B H 0.6663 0.7557 0.9518 0.030 Uiso 1 1 calc R . . C23 C 0.7451(3) 0.7261(2) 0.8731(3) 0.0223(11) Uani 1 1 d . . . C24 C 0.7529(3) 0.7366(3) 0.7907(3) 0.0260(12) Uani 1 1 d . . . H24 H 0.7032 0.7456 0.7518 0.031 Uiso 1 1 calc R . . C25 C 0.8318(4) 0.7341(3) 0.7652(3) 0.0269(12) Uani 1 1 d . . . H25 H 0.8357 0.7412 0.7091 0.032 Uiso 1 1 calc R . . C26 C 0.9049(3) 0.7212(3) 0.8211(3) 0.0272(12) Uani 1 1 d . . . H26 H 0.9591 0.7194 0.8037 0.033 Uiso 1 1 calc R . . C27 C 0.8984(4) 0.7109(3) 0.9021(3) 0.0279(13) Uani 1 1 d . . . H27 H 0.9487 0.7025 0.9405 0.033 Uiso 1 1 calc R . . C28 C 0.8186(3) 0.7126(2) 0.9292(3) 0.0204(11) Uani 1 1 d . . . C29 C 0.8183(4) 0.7021(3) 1.0189(3) 0.0263(12) Uani 1 1 d . . . H29A H 0.7618 0.7145 1.0326 0.032 Uiso 1 1 calc R . . H29B H 0.8624 0.7301 1.0514 0.032 Uiso 1 1 calc R . . C30 C 0.8305(4) 0.6143(3) 1.1742(3) 0.0357(15) Uani 0.9395(14) 1 d P . . H30A H 0.8396 0.5727 1.2040 0.054 Uiso 0.9395(14) 1 calc PR . . H30B H 0.7727 0.6305 1.1766 0.054 Uiso 0.9395(14) 1 calc PR . . H30C H 0.8727 0.6465 1.1993 0.054 Uiso 0.9395(14) 1 calc PR . . C30A C 0.9197 0.5731 1.0554 0.030 Uiso 0.0605(14) 1 d P . . C31 C 0.5928(3) 0.4368(3) 0.7970(4) 0.0328(14) Uani 1 1 d . . . H31A H 0.5722 0.4724 0.7590 0.049 Uiso 1 1 calc R . . H31B H 0.5549 0.4324 0.8380 0.049 Uiso 1 1 calc R . . H31C H 0.5931 0.3957 0.7664 0.049 Uiso 1 1 calc R . . C32 C 0.7405(4) 0.3712(3) 0.9321(3) 0.0262(12) Uani 1 1 d . . . H32A H 0.6850 0.3537 0.9424 0.031 Uiso 1 1 calc R . . H32B H 0.7687 0.3372 0.9031 0.031 Uiso 1 1 calc R . . C33 C 0.7957(3) 0.3874(2) 1.0118(3) 0.0215(11) Uani 1 1 d . . . C34 C 0.8835(3) 0.3989(3) 1.0144(3) 0.0273(12) Uani 1 1 d . . . H34 H 0.9065 0.3965 0.9649 0.033 Uiso 1 1 calc R . . C35 C 0.9372(4) 0.4134(3) 1.0859(3) 0.0322(14) Uani 1 1 d . . . H35 H 0.9960 0.4224 1.0852 0.039 Uiso 1 1 calc R . . C36 C 0.9055(4) 0.4149(3) 1.1593(3) 0.0323(14) Uani 1 1 d . . . H36 H 0.9425 0.4241 1.2092 0.039 Uiso 1 1 calc R . . C37 C 0.8196(3) 0.4028(3) 1.1589(3) 0.0280(13) Uani 1 1 d . . . H37 H 0.7985 0.4025 1.2095 0.034 Uiso 1 1 calc R . . C38 C 0.7629(3) 0.3911(2) 1.0866(3) 0.0210(11) Uani 1 1 d . . . C39 C 0.6698(3) 0.3810(2) 1.0903(3) 0.0220(11) Uani 1 1 d . . . H39A H 0.6638 0.3610 1.1437 0.026 Uiso 1 1 calc R . . H39B H 0.6449 0.3504 1.0464 0.026 Uiso 1 1 calc R . . C40 C 0.6539(4) 0.5068(3) 1.1948(3) 0.0409(16) Uani 1 1 d . . . H40A H 0.6313 0.5504 1.2040 0.061 Uiso 1 1 calc R . . H40B H 0.7163 0.5092 1.1991 0.061 Uiso 1 1 calc R . . H40C H 0.6391 0.4763 1.2361 0.061 Uiso 1 1 calc R . . B1 B 0.5439(4) 0.6957(3) 0.1196(4) 0.0275(14) Uani 1 1 d . . . B2 B 0.9736(4) 0.2973(4) 0.3822(4) 0.0320(16) Uani 1 1 d . . . F1 F 0.4857(3) 0.6569(3) 0.0731(2) 0.112(2) Uani 1 1 d . . . F2 F 0.6043(4) 0.6592(4) 0.1563(6) 0.182(4) Uani 1 1 d . . . F3 F 0.5797(4) 0.7412(3) 0.0782(3) 0.113(2) Uani 1 1 d . . . F4 F 0.5121(5) 0.7209(3) 0.1828(4) 0.145(3) Uani 1 1 d . . . F5 F 0.9334(3) 0.3117(2) 0.4472(3) 0.0744(14) Uani 1 1 d . . . F6 F 0.9235(3) 0.3011(3) 0.3091(3) 0.0883(17) Uani 1 1 d . . . F7 F 1.0101(5) 0.2373(3) 0.3900(3) 0.119(2) Uani 1 1 d . . . F8 F 1.0399(3) 0.3411(3) 0.3817(3) 0.0925(19) 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 Ag1 0.0219(2) 0.0160(2) 0.0210(2) 0.00097(15) 0.00452(15) -0.00057(16) Ag2 0.0254(2) 0.0155(2) 0.0207(2) 0.00109(15) 0.00011(15) -0.00045(16) Te1 0.01535(15) 0.01545(17) 0.01941(16) 0.00152(13) 0.00333(12) 0.00026(13) Te2 0.02118(17) 0.02108(19) 0.01818(17) 0.00159(14) 0.00502(13) 0.00124(14) Te3 0.02678(18) 0.02182(19) 0.02140(18) -0.00025(14) 0.00529(14) -0.00629(15) Te4 0.01662(16) 0.01876(19) 0.03018(19) 0.00538(15) 0.00557(14) 0.00022(14) Te5 0.01900(17) 0.01498(18) 0.02470(18) 0.00137(14) 0.00275(13) 0.00093(13) Te6 0.0211(2) 0.0187(2) 0.0231(2) 0.00155(15) -0.00023(15) -0.00071(15) Te7 0.02251(17) 0.02059(19) 0.01732(17) 0.00145(14) 0.00266(13) 0.00138(14) Te8 0.01883(17) 0.01851(18) 0.02430(18) 0.00256(14) 0.00329(13) 0.00120(14) C1 0.029(3) 0.026(3) 0.021(3) 0.001(2) 0.007(2) -0.005(2) C2 0.021(3) 0.016(3) 0.023(3) 0.003(2) 0.006(2) 0.002(2) C3 0.023(3) 0.009(2) 0.026(3) 0.001(2) 0.007(2) 0.005(2) C4 0.023(3) 0.019(3) 0.017(3) 0.002(2) 0.002(2) 0.005(2) C5 0.027(3) 0.029(3) 0.025(3) -0.006(2) -0.001(2) 0.007(2) C6 0.014(3) 0.031(3) 0.041(3) -0.001(3) 0.002(2) 0.007(2) C7 0.027(3) 0.021(3) 0.027(3) 0.001(2) 0.007(2) 0.003(2) C8 0.023(3) 0.014(3) 0.024(3) 0.004(2) 0.006(2) 0.003(2) C9 0.032(3) 0.017(3) 0.019(3) 0.005(2) 0.005(2) 0.007(2) C10 0.029(3) 0.028(3) 0.036(3) 0.006(3) -0.008(2) -0.008(3) C11 0.043(4) 0.031(4) 0.047(4) 0.014(3) 0.010(3) -0.003(3) C12 0.033(3) 0.010(3) 0.027(3) 0.000(2) 0.011(2) -0.001(2) C13 0.024(3) 0.007(2) 0.025(3) 0.000(2) 0.003(2) -0.001(2) C14 0.023(3) 0.016(3) 0.030(3) -0.001(2) 0.002(2) -0.004(2) C15 0.019(3) 0.024(3) 0.031(3) -0.004(2) 0.011(2) -0.001(2) C16 0.027(3) 0.019(3) 0.029(3) -0.001(2) 0.007(2) -0.005(2) C17 0.025(3) 0.018(3) 0.029(3) 0.005(2) 0.003(2) -0.002(2) C18 0.019(3) 0.015(3) 0.027(3) 0.004(2) 0.007(2) 0.002(2) C19 0.021(3) 0.017(3) 0.033(3) 0.000(2) 0.009(2) 0.000(2) C20 0.028(3) 0.032(3) 0.027(3) 0.003(3) 0.000(2) 0.000(3) C21 0.047(4) 0.032(3) 0.021(3) -0.003(2) -0.003(3) 0.004(3) C22 0.025(3) 0.013(3) 0.037(3) 0.004(2) 0.004(2) 0.000(2) C23 0.023(3) 0.011(3) 0.031(3) 0.001(2) 0.000(2) -0.003(2) C24 0.027(3) 0.021(3) 0.027(3) -0.001(2) -0.003(2) -0.002(2) C25 0.039(3) 0.018(3) 0.025(3) -0.005(2) 0.010(2) -0.005(2) C26 0.024(3) 0.022(3) 0.037(3) -0.006(2) 0.007(2) -0.008(2) C27 0.031(3) 0.013(3) 0.038(3) -0.001(2) -0.001(2) -0.003(2) C28 0.025(3) 0.008(2) 0.028(3) 0.000(2) 0.004(2) -0.002(2) C29 0.033(3) 0.015(3) 0.029(3) 0.001(2) 0.000(2) -0.004(2) C30 0.041(4) 0.042(4) 0.023(3) 0.001(3) 0.000(3) -0.002(3) C31 0.030(3) 0.026(3) 0.038(3) -0.008(3) -0.009(3) -0.002(3) C32 0.037(3) 0.015(3) 0.025(3) -0.001(2) -0.001(2) 0.001(2) C33 0.031(3) 0.011(3) 0.022(3) 0.003(2) 0.000(2) 0.005(2) C34 0.030(3) 0.026(3) 0.027(3) 0.003(2) 0.007(2) 0.012(2) C35 0.021(3) 0.035(4) 0.039(3) 0.000(3) 0.003(2) 0.009(3) C36 0.029(3) 0.037(4) 0.027(3) -0.005(3) -0.008(2) 0.008(3) C37 0.026(3) 0.030(3) 0.027(3) -0.003(2) 0.001(2) 0.007(2) C38 0.021(3) 0.013(3) 0.028(3) 0.004(2) 0.001(2) 0.005(2) C39 0.030(3) 0.013(3) 0.022(3) 0.002(2) 0.002(2) 0.004(2) C40 0.051(4) 0.046(4) 0.026(3) -0.017(3) 0.004(3) -0.006(3) B1 0.027(3) 0.034(4) 0.021(3) -0.002(3) 0.003(3) -0.002(3) B2 0.030(4) 0.040(4) 0.023(3) -0.002(3) -0.004(3) 0.002(3) F1 0.114(4) 0.194(6) 0.030(2) -0.024(3) 0.015(2) -0.115(4) F2 0.092(5) 0.106(6) 0.315(11) 0.058(6) -0.065(6) 0.027(4) F3 0.165(6) 0.135(5) 0.044(3) 0.000(3) 0.028(3) -0.104(5) F4 0.194(7) 0.124(5) 0.153(6) -0.083(5) 0.137(6) -0.105(5) F5 0.081(3) 0.080(3) 0.077(3) -0.027(3) 0.056(3) -0.027(3) F6 0.059(3) 0.130(5) 0.063(3) 0.026(3) -0.029(2) -0.024(3) F7 0.196(7) 0.080(4) 0.082(4) 0.011(3) 0.025(4) 0.077(4) F8 0.066(3) 0.153(5) 0.067(3) -0.064(3) 0.035(2) -0.070(3) _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 Ag1 Te3 2.7593(5) . ? Ag1 Te2 2.7617(5) . ? Ag1 Te4 2.7682(5) . ? Ag1 Te1 2.8039(5) . ? Ag2 Te6A 2.643(6) . ? Ag2 Te5 2.7664(5) . ? Ag2 Te6 2.7805(5) . ? Ag2 Te7 2.7908(5) . ? Ag2 Te8 2.8078(5) . ? Te1 C1 2.140(5) . ? Te1 C2 2.171(5) . ? Te2 C10 2.136(5) . ? Te2 C9 2.172(5) . ? Te3 C11 2.117(6) . ? Te3 C12 2.175(5) . ? Te4 C20 2.141(5) . ? Te4 C19 2.177(5) . ? Te5 C21 2.143(5) . ? Te5 C22 2.172(5) . ? Te6 Te6A 0.977(6) . ? Te6 C30A 1.2950(4) . ? Te6 C30 2.132(6) . ? Te6 C29 2.176(5) . ? Te6A C30A 2.135(6) . ? Te7 C31 2.133(5) . ? Te7 C32 2.167(5) . ? Te8 C40 2.123(5) . ? Te8 C39 2.177(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.488(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.397(7) . ? C3 C8 1.401(7) . ? C4 C5 1.388(7) . ? C4 H4 0.9500 . ? C5 C6 1.384(8) . ? C5 H5 0.9500 . ? C6 C7 1.378(7) . ? C6 H6 0.9500 . ? C7 C8 1.398(7) . ? C7 H7 0.9500 . ? C8 C9 1.494(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.505(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.387(7) . ? C13 C18 1.405(7) . ? C14 C15 1.387(7) . ? C14 H14 0.9500 . ? C15 C16 1.390(7) . ? C15 H15 0.9500 . ? C16 C17 1.388(7) . ? C16 H16 0.9500 . ? C17 C18 1.395(7) . ? C17 H17 0.9500 . ? C18 C19 1.488(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.502(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.392(7) . ? C23 C24 1.403(7) . ? C24 C25 1.383(7) . ? C24 H24 0.9500 . ? C25 C26 1.383(8) . ? C25 H25 0.9500 . ? C26 C27 1.376(8) . ? C26 H26 0.9500 . ? C27 C28 1.408(7) . ? C27 H27 0.9500 . ? C28 C29 1.500(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.493(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.404(7) . ? C33 C38 1.419(7) . ? C34 C35 1.371(8) . ? C34 H34 0.9500 . ? C35 C36 1.386(8) . ? C35 H35 0.9500 . ? C36 C37 1.382(8) . ? C36 H36 0.9500 . ? C37 C38 1.393(7) . ? C37 H37 0.9500 . ? C38 C39 1.501(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? B1 F2 1.284(8) . ? B1 F4 1.333(8) . ? B1 F3 1.334(8) . ? B1 F1 1.355(7) . ? B2 F6 1.335(7) . ? B2 F7 1.350(8) . ? B2 F5 1.367(8) . ? B2 F8 1.380(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # Te6A Ag2 Te6 20.55(14) . . ? # Te6A Te6 C30A 139.6(3) . . ? # Te6A Te6 C30 38.1(4) . . ? # C30A Te6 C30 103.00(18) . . ? # Te6A Te6 C29 78.4(4) . . ? # C30A Te6 C29 123.76(15) . . ? # Te6A Te6 Ag2 71.7(3) . . ? # Te6 Te6A C30A 23.1(2) . . ? # Te6 Te6A Ag2 87.7(3) . . ? # Te6 C30A Te6A 17.24(15) . . ? Te3 Ag1 Te2 124.283(17) . . ? Te3 Ag1 Te4 105.328(17) . . ? Te2 Ag1 Te4 113.639(17) . . ? Te3 Ag1 Te1 101.844(16) . . ? Te2 Ag1 Te1 100.903(16) . . ? Te4 Ag1 Te1 109.458(16) . . ? Te6A Ag2 Te5 104.73(13) . . ? Te5 Ag2 Te6 111.281(17) . . ? Te6A Ag2 Te7 127.38(14) . . ? Te5 Ag2 Te7 110.351(17) . . ? Te6 Ag2 Te7 107.757(17) . . ? Te6A Ag2 Te8 101.79(13) . . ? Te5 Ag2 Te8 108.893(17) . . ? Te6 Ag2 Te8 115.748(17) . . ? Te7 Ag2 Te8 102.409(17) . . ? C1 Te1 C2 95.0(2) . . ? C1 Te1 Ag1 96.38(14) . . ? C2 Te1 Ag1 109.50(13) . . ? C10 Te2 C9 93.9(2) . . ? C10 Te2 Ag1 97.92(17) . . ? C9 Te2 Ag1 100.00(14) . . ? C11 Te3 C12 95.5(2) . . ? C11 Te3 Ag1 101.62(18) . . ? C12 Te3 Ag1 101.51(14) . . ? C20 Te4 C19 94.8(2) . . ? C20 Te4 Ag1 103.96(15) . . ? C19 Te4 Ag1 102.42(14) . . ? C21 Te5 C22 94.0(2) . . ? C21 Te5 Ag2 103.21(16) . . ? C22 Te5 Ag2 107.37(14) . . ? C30 Te6 C29 92.4(2) . . ? C30A Te6 Ag2 128.53(2) . . ? C30 Te6 Ag2 104.68(18) . . ? C29 Te6 Ag2 97.47(15) . . ? C30A Te6A Ag2 102.0(2) . . ? C31 Te7 C32 98.1(2) . . ? C31 Te7 Ag2 101.55(16) . . ? C32 Te7 Ag2 99.83(14) . . ? C40 Te8 C39 93.2(2) . . ? C40 Te8 Ag2 102.01(18) . . ? C39 Te8 Ag2 104.30(14) . . ? Te1 C1 H1A 109.5 . . ? Te1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Te1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Te1 115.0(3) . . ? C3 C2 H2A 108.5 . . ? Te1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? Te1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C4 C3 C8 119.0(5) . . ? C4 C3 C2 118.2(4) . . ? C8 C3 C2 122.8(5) . . ? C5 C4 C3 120.8(5) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.3(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 119.3(5) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 121.5(5) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C3 119.2(5) . . ? C7 C8 C9 118.2(5) . . ? C3 C8 C9 122.7(5) . . ? C8 C9 Te2 110.7(4) . . ? C8 C9 H9A 109.5 . . ? Te2 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? Te2 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? Te2 C10 H10A 109.5 . . ? Te2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Te2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Te3 C11 H11A 109.5 . . ? Te3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Te3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 Te3 115.4(3) . . ? C13 C12 H12A 108.4 . . ? Te3 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? Te3 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C18 119.4(5) . . ? C14 C13 C12 117.9(5) . . ? C18 C13 C12 122.6(4) . . ? C15 C14 C13 121.7(5) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 119.1(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 118.6(5) . . ? C17 C18 C19 117.5(5) . . ? C13 C18 C19 123.7(4) . . ? C18 C19 Te4 113.6(3) . . ? C18 C19 H19A 108.8 . . ? Te4 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? Te4 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? Te4 C20 H20A 109.5 . . ? Te4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Te4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Te5 C21 H21A 109.5 . . ? Te5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Te5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 Te5 118.1(3) . . ? C23 C22 H22A 107.8 . . ? Te5 C22 H22A 107.8 . . ? C23 C22 H22B 107.8 . . ? Te5 C22 H22B 107.8 . . ? H22A C22 H22B 107.1 . . ? C28 C23 C24 118.6(5) . . ? C28 C23 C22 123.1(5) . . ? C24 C23 C22 118.1(5) . . ? C25 C24 C23 121.2(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.4(5) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 121.3(5) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C23 C28 C27 119.3(5) . . ? C23 C28 C29 123.3(5) . . ? C27 C28 C29 117.4(5) . . ? C28 C29 Te6 109.6(3) . . ? C28 C29 H29A 109.8 . . ? Te6 C29 H29A 109.8 . . ? C28 C29 H29B 109.8 . . ? Te6 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? Te6 C30 H30A 109.5 . . ? Te6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Te6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Te7 C31 H31A 109.5 . . ? Te7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Te7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 Te7 109.7(3) . . ? C33 C32 H32A 109.7 . . ? Te7 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? Te7 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C38 117.7(5) . . ? C34 C33 C32 119.9(5) . . ? C38 C33 C32 122.4(5) . . ? C35 C34 C33 122.4(5) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C34 C35 C36 119.7(5) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 119.3(5) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 122.0(5) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C37 C38 C33 118.8(5) . . ? C37 C38 C39 119.2(5) . . ? C33 C38 C39 122.1(5) . . ? C38 C39 Te8 111.3(3) . . ? C38 C39 H39A 109.4 . . ? Te8 C39 H39A 109.4 . . ? C38 C39 H39B 109.4 . . ? Te8 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? Te8 C40 H40A 109.5 . . ? Te8 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Te8 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? F2 B1 F4 101.6(7) . . ? F2 B1 F3 107.4(7) . . ? F4 B1 F3 112.4(6) . . ? F2 B1 F1 108.3(7) . . ? F4 B1 F1 111.1(6) . . ? F3 B1 F1 115.0(5) . . ? F6 B2 F7 108.7(6) . . ? F6 B2 F5 114.5(6) . . ? F7 B2 F5 111.5(6) . . ? F6 B2 F8 107.3(6) . . ? F7 B2 F8 105.9(6) . . ? F5 B2 F8 108.5(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.376 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.184 #===END OF CIF ============================================================== # 06nts017 data_06nts017 _database_code_depnum_ccdc_archive 'CCDC 621504' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-09-08 _chemical_name_systematic ; Bis{dichloro(p-cymene)ruthenium}(mu2-1,2-bis(methylthiomethyl)benzene) ; _chemical_name_common ;Bis(dichloro(p-cymene)ruthenium)(mu2-1,2- bis(methylthiomethyl)benzene) ; _chemical_melting_point ? _chemical_formula_moiety 'C30 H42 Cl4 Ru2 S2' _chemical_formula_sum 'C30 H42 Cl4 Ru2 S2' _chemical_formula_weight 810.70 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 # Superceded ** _symmetry_space_group_name_Hall '-C 2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.604(3) _cell_length_b 13.415(2) _cell_length_c 13.5021(12) _cell_angle_alpha 90.00 _cell_angle_beta 124.612(8) _cell_angle_gamma 90.00 _cell_volume 3220.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3855 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7566 # 0.7270 _exptl_absorpt_correction_T_max 1.0000 # 0.9587 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 31058 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _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 3.02 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3705 _reflns_number_gt 2921 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (Ferrugia, 1997)' _computing_publication_material ? _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. There is disorder in the i-propyl group at C7A/B, C9A/B AND C10A/B. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+13.1193P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3705 _refine_ls_number_parameters 197 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ru1 Ru 0.172193(15) 0.08562(2) 0.02482(2) 0.02629(10) Uani 1 1 d . A . Cl1 Cl 0.11761(6) 0.12331(7) -0.18390(8) 0.0360(2) Uani 1 1 d . . . Cl2 Cl 0.26442(6) -0.00945(10) 0.01879(11) 0.0548(3) Uani 1 1 d . . . S1 S 0.09566(7) -0.06183(7) -0.03933(10) 0.0393(2) Uani 1 1 d . . . C1 C 0.2567(2) 0.1888(3) 0.1584(4) 0.0423(10) Uani 1 1 d . . . H1 H 0.3044 0.2063 0.1750 0.051 Uiso 1 1 calc R . . C2 C 0.2514(2) 0.1062(3) 0.2198(3) 0.0417(10) Uani 1 1 d . . . C3 C 0.1802(2) 0.0821(3) 0.1931(3) 0.0342(8) Uani 1 1 d . . . H3 H 0.1750 0.0281 0.2333 0.041 Uiso 1 1 calc R . . C4 C 0.1162(2) 0.1378(3) 0.1068(3) 0.0304(8) Uani 1 1 d . A . H4 H 0.0686 0.1194 0.0895 0.036 Uiso 1 1 calc R . . C5 C 0.1206(2) 0.2195(3) 0.0454(3) 0.0322(8) Uani 1 1 d . . . C6 C 0.1936(2) 0.2445(3) 0.0746(3) 0.0355(9) Uani 1 1 d . A . H6 H 0.1991 0.2998 0.0362 0.043 Uiso 1 1 calc R . . C7A C 0.0507(2) 0.2766(3) -0.0484(4) 0.0397(9) Uani 0.562(7) 1 d P A 1 H7A H 0.0119 0.2263 -0.1030 0.048 Uiso 0.562(7) 1 calc PR A 1 C7B C 0.0507(2) 0.2766(3) -0.0484(4) 0.0397(9) Uani 0.438(7) 1 d P A 2 H7B H 0.0431 0.2666 -0.1281 0.048 Uiso 0.438(7) 1 calc PR A 2 C8 C 0.3189(3) 0.0429(4) 0.3062(4) 0.0619(14) Uani 1 1 d . . . H8A H 0.3485 0.0759 0.3848 0.093 Uiso 1 1 calc R . . H8B H 0.3500 0.0341 0.2752 0.093 Uiso 1 1 calc R . . H8C H 0.3021 -0.0224 0.3148 0.093 Uiso 1 1 calc R . . C9A C 0.0204(6) 0.3325(7) 0.0163(9) 0.064(3) Uani 0.562(7) 1 d P A 1 H9AA H 0.0579 0.3810 0.0729 0.097 Uiso 0.562(7) 1 calc PR A 1 H9AB H 0.0103 0.2845 0.0602 0.097 Uiso 0.562(7) 1 calc PR A 1 H9AC H -0.0262 0.3674 -0.0434 0.097 Uiso 0.562(7) 1 calc PR A 1 C10A C 0.0606(5) 0.3448(6) -0.1252(7) 0.053(2) Uani 0.562(7) 1 d P A 1 H10A H 0.0986 0.3952 -0.0746 0.079 Uiso 0.562(7) 1 calc PR A 1 H10B H 0.0127 0.3777 -0.1836 0.079 Uiso 0.562(7) 1 calc PR A 1 H10C H 0.0771 0.3064 -0.1681 0.079 Uiso 0.562(7) 1 calc PR A 1 C9B C -0.0181(6) 0.2481(8) -0.0609(9) 0.049(3) Uani 0.438(7) 1 d P A 2 H9BA H -0.0294 0.1781 -0.0855 0.073 Uiso 0.438(7) 1 calc PR A 2 H9BB H -0.0596 0.2901 -0.1219 0.073 Uiso 0.438(7) 1 calc PR A 2 H9BC H -0.0119 0.2569 0.0164 0.073 Uiso 0.438(7) 1 calc PR A 2 C10B C 0.0640(8) 0.3938(9) -0.0172(12) 0.064(4) Uani 0.438(7) 1 d P A 2 H10D H 0.0161 0.4294 -0.0676 0.096 Uiso 0.438(7) 1 calc PR A 2 H10E H 0.1001 0.4196 -0.0328 0.096 Uiso 0.438(7) 1 calc PR A 2 H10F H 0.0838 0.4037 0.0678 0.096 Uiso 0.438(7) 1 calc PR A 2 C11 C 0.1546(4) -0.1563(3) 0.0702(5) 0.0712(17) Uani 1 1 d . . . H11A H 0.1301 -0.2215 0.0419 0.107 Uiso 1 1 calc R . . H11B H 0.1623 -0.1406 0.1473 0.107 Uiso 1 1 calc R . . H11C H 0.2033 -0.1581 0.0805 0.107 Uiso 1 1 calc R . . C12 C 0.0853(3) -0.1135(3) -0.1735(4) 0.0384(9) Uani 1 1 d . . . H12A H 0.0605 -0.0636 -0.2391 0.046 Uiso 1 1 calc R . . H12B H 0.1357 -0.1274 -0.1555 0.046 Uiso 1 1 calc R . . C13 C 0.0395(2) -0.2083(3) -0.2155(4) 0.0333(8) Uani 1 1 d . . . C14 C 0.0772(2) -0.2994(3) -0.1838(4) 0.0398(9) Uani 1 1 d . . . H14 H 0.1306 -0.3001 -0.1378 0.048 Uiso 1 1 calc R . . C15 C 0.0387(2) -0.3884(3) -0.2175(4) 0.0458(11) Uani 1 1 d . . . H15 H 0.0654 -0.4496 -0.1962 0.055 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 Ru1 0.02607(15) 0.02981(17) 0.02945(16) -0.00068(12) 0.01962(12) -0.00307(12) Cl1 0.0547(6) 0.0285(5) 0.0337(5) -0.0029(4) 0.0304(5) -0.0082(4) Cl2 0.0459(6) 0.0767(8) 0.0580(7) 0.0103(6) 0.0392(6) 0.0209(6) S1 0.0631(7) 0.0283(5) 0.0493(6) -0.0062(4) 0.0456(6) -0.0110(4) C1 0.032(2) 0.053(3) 0.043(2) -0.015(2) 0.0227(19) -0.0196(19) C2 0.032(2) 0.055(3) 0.0282(19) -0.0043(18) 0.0111(16) -0.0091(18) C3 0.040(2) 0.042(2) 0.0255(17) -0.0049(16) 0.0221(16) -0.0072(18) C4 0.0354(19) 0.034(2) 0.0355(19) -0.0082(16) 0.0282(17) -0.0075(16) C5 0.039(2) 0.031(2) 0.0366(19) -0.0084(16) 0.0281(17) -0.0060(16) C6 0.046(2) 0.031(2) 0.041(2) -0.0092(17) 0.0319(19) -0.0143(18) C7A 0.047(2) 0.033(2) 0.046(2) -0.0014(18) 0.030(2) 0.0027(18) C7B 0.047(2) 0.033(2) 0.046(2) -0.0014(18) 0.030(2) 0.0027(18) C8 0.036(2) 0.084(4) 0.045(3) 0.005(3) 0.010(2) -0.002(2) C9A 0.079(7) 0.055(6) 0.084(7) 0.016(5) 0.061(6) 0.019(5) C10A 0.063(5) 0.046(5) 0.057(5) -0.003(4) 0.039(4) 0.000(4) C9B 0.050(6) 0.045(6) 0.043(6) 0.003(5) 0.021(5) 0.001(5) C10B 0.079(9) 0.053(7) 0.081(9) -0.004(6) 0.057(8) -0.008(6) C11 0.145(6) 0.030(2) 0.064(3) 0.013(2) 0.074(4) 0.010(3) C12 0.060(3) 0.028(2) 0.049(2) -0.0079(17) 0.044(2) -0.0096(18) C13 0.049(2) 0.0212(18) 0.049(2) -0.0050(16) 0.040(2) -0.0082(16) C14 0.040(2) 0.030(2) 0.060(3) -0.0034(18) 0.034(2) 0.0007(17) C15 0.048(2) 0.023(2) 0.072(3) -0.0003(19) 0.037(2) 0.0040(17) _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 Ru1 C4 2.167(3) . ? Ru1 C3 2.179(3) . ? Ru1 C1 2.183(4) . ? Ru1 C2 2.195(4) . ? Ru1 C6 2.203(4) . ? Ru1 C5 2.213(4) . ? Ru1 S1 2.4020(11) . ? Ru1 Cl2 2.4057(11) . ? Ru1 Cl1 2.4111(10) . ? S1 C11 1.809(5) . ? S1 C12 1.831(4) . ? C1 C6 1.394(6) . ? C1 C2 1.428(6) . ? C1 H1 0.9500 . ? C2 C3 1.404(5) . ? C2 C8 1.509(6) . ? C3 C4 1.412(5) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 H4 0.9500 . ? C5 C6 1.432(5) . ? C5 C7A 1.516(6) . ? C6 H6 0.9500 . ? C7A C10A 1.486(9) . ? C7A C9A 1.551(10) . ? C7A H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.509(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.394(5) . ? C13 C13 1.405(8) 2_554 ? C14 C15 1.375(6) . ? C14 H14 0.9500 . ? C15 C15 1.379(9) 2_554 ? C15 H15 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 C4 Ru1 C3 37.93(14) . . ? C4 Ru1 C1 79.69(14) . . ? C3 Ru1 C1 67.58(15) . . ? C4 Ru1 C2 68.15(15) . . ? C3 Ru1 C2 37.44(15) . . ? C1 Ru1 C2 38.09(16) . . ? C4 Ru1 C6 67.25(13) . . ? C3 Ru1 C6 79.87(14) . . ? C1 Ru1 C6 37.07(15) . . ? C2 Ru1 C6 68.11(16) . . ? C4 Ru1 C5 37.51(13) . . ? C3 Ru1 C5 68.49(14) . . ? C1 Ru1 C5 68.05(15) . . ? C2 Ru1 C5 81.52(15) . . ? C6 Ru1 C5 37.84(13) . . ? C4 Ru1 S1 88.88(10) . . ? C3 Ru1 S1 89.37(10) . . ? C1 Ru1 S1 154.42(12) . . ? C2 Ru1 S1 116.36(12) . . ? C6 Ru1 S1 152.72(10) . . ? C5 Ru1 S1 114.88(10) . . ? C4 Ru1 Cl2 154.35(10) . . ? C3 Ru1 Cl2 116.57(11) . . ? C1 Ru1 Cl2 92.52(12) . . ? C2 Ru1 Cl2 90.62(12) . . ? C6 Ru1 Cl2 119.26(10) . . ? C5 Ru1 Cl2 157.01(10) . . ? S1 Ru1 Cl2 87.99(4) . . ? C4 Ru1 Cl1 119.01(10) . . ? C3 Ru1 Cl1 156.89(11) . . ? C1 Ru1 Cl1 117.18(12) . . ? C2 Ru1 Cl1 154.98(12) . . ? C6 Ru1 Cl1 91.84(10) . . ? C5 Ru1 Cl1 91.72(10) . . ? S1 Ru1 Cl1 88.38(3) . . ? Cl2 Ru1 Cl1 86.34(4) . . ? C11 S1 C12 100.2(2) . . ? C11 S1 Ru1 105.2(2) . . ? C12 S1 Ru1 109.95(13) . . ? C6 C1 C2 121.5(4) . . ? C6 C1 Ru1 72.3(2) . . ? C2 C1 Ru1 71.4(2) . . ? C6 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? Ru1 C1 H1 129.6 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 C8 120.4(4) . . ? C1 C2 C8 121.6(4) . . ? C3 C2 Ru1 70.7(2) . . ? C1 C2 Ru1 70.5(2) . . ? C8 C2 Ru1 127.6(3) . . ? C2 C3 C4 120.4(4) . . ? C2 C3 Ru1 71.9(2) . . ? C4 C3 Ru1 70.57(19) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? Ru1 C3 H3 130.4 . . ? C5 C4 C3 122.4(3) . . ? C5 C4 Ru1 73.0(2) . . ? C3 C4 Ru1 71.5(2) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? Ru1 C4 H4 129.2 . . ? C4 C5 C6 116.8(4) . . ? C4 C5 C7A 121.2(3) . . ? C6 C5 C7A 122.0(3) . . ? C4 C5 Ru1 69.5(2) . . ? C6 C5 Ru1 70.7(2) . . ? C7A C5 Ru1 129.7(3) . . ? C1 C6 C5 121.0(4) . . ? C1 C6 Ru1 70.7(2) . . ? C5 C6 Ru1 71.5(2) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? Ru1 C6 H6 131.2 . . ? C10A C7A C5 115.2(5) . . ? C10A C7A C9A 111.7(6) . . ? C5 C7A C9A 108.2(5) . . ? C10A C7A H7A 107.2 . . ? C5 C7A H7A 107.2 . . ? C9A C7A H7A 107.2 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H9BA C9B H9BB 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? H10D C10B H10E 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 S1 112.1(3) . . ? C13 C12 H12A 109.2 . . ? S1 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? S1 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C13 118.8(2) . 2_554 ? C14 C13 C12 118.6(4) . . ? C13 C13 C12 122.6(2) 2_554 . ? C15 C14 C13 121.4(4) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C15 119.8(2) . 2_554 ? C14 C15 H15 120.1 . . ? C15 C15 H15 120.1 2_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Ru1 S1 C11 -99.0(2) . . . . ? C3 Ru1 S1 C11 -61.1(2) . . . . ? C1 Ru1 S1 C11 -36.1(3) . . . . ? C2 Ru1 S1 C11 -34.2(2) . . . . ? C6 Ru1 S1 C11 -127.2(3) . . . . ? C5 Ru1 S1 C11 -126.9(2) . . . . ? Cl2 Ru1 S1 C11 55.51(18) . . . . ? Cl1 Ru1 S1 C11 141.90(18) . . . . ? C4 Ru1 S1 C12 153.89(19) . . . . ? C3 Ru1 S1 C12 -168.19(19) . . . . ? C1 Ru1 S1 C12 -143.2(3) . . . . ? C2 Ru1 S1 C12 -141.3(2) . . . . ? C6 Ru1 S1 C12 125.7(3) . . . . ? C5 Ru1 S1 C12 125.97(19) . . . . ? Cl2 Ru1 S1 C12 -51.57(16) . . . . ? Cl1 Ru1 S1 C12 34.82(16) . . . . ? C4 Ru1 C1 C6 -65.7(2) . . . . ? C3 Ru1 C1 C6 -103.3(3) . . . . ? C2 Ru1 C1 C6 -133.3(4) . . . . ? C5 Ru1 C1 C6 -28.5(2) . . . . ? S1 Ru1 C1 C6 -130.5(3) . . . . ? Cl2 Ru1 C1 C6 138.9(2) . . . . ? Cl1 Ru1 C1 C6 51.7(2) . . . . ? C4 Ru1 C1 C2 67.6(3) . . . . ? C3 Ru1 C1 C2 30.0(2) . . . . ? C6 Ru1 C1 C2 133.3(4) . . . . ? C5 Ru1 C1 C2 104.9(3) . . . . ? S1 Ru1 C1 C2 2.8(4) . . . . ? Cl2 Ru1 C1 C2 -87.8(2) . . . . ? Cl1 Ru1 C1 C2 -175.0(2) . . . . ? C6 C1 C2 C3 0.1(6) . . . . ? Ru1 C1 C2 C3 -54.2(3) . . . . ? C6 C1 C2 C8 177.1(4) . . . . ? Ru1 C1 C2 C8 122.8(4) . . . . ? C6 C1 C2 Ru1 54.3(4) . . . . ? C4 Ru1 C2 C3 29.0(2) . . . . ? C1 Ru1 C2 C3 130.5(4) . . . . ? C6 Ru1 C2 C3 102.3(3) . . . . ? C5 Ru1 C2 C3 65.5(3) . . . . ? S1 Ru1 C2 C3 -48.1(3) . . . . ? Cl2 Ru1 C2 C3 -136.2(2) . . . . ? Cl1 Ru1 C2 C3 141.1(2) . . . . ? C4 Ru1 C2 C1 -101.5(3) . . . . ? C3 Ru1 C2 C1 -130.5(4) . . . . ? C6 Ru1 C2 C1 -28.2(2) . . . . ? C5 Ru1 C2 C1 -65.0(3) . . . . ? S1 Ru1 C2 C1 -178.6(2) . . . . ? Cl2 Ru1 C2 C1 93.3(2) . . . . ? Cl1 Ru1 C2 C1 10.6(5) . . . . ? C4 Ru1 C2 C8 143.1(4) . . . . ? C3 Ru1 C2 C8 114.0(5) . . . . ? C1 Ru1 C2 C8 -115.4(5) . . . . ? C6 Ru1 C2 C8 -143.7(4) . . . . ? C5 Ru1 C2 C8 179.5(4) . . . . ? S1 Ru1 C2 C8 65.9(4) . . . . ? Cl2 Ru1 C2 C8 -22.2(4) . . . . ? Cl1 Ru1 C2 C8 -104.8(4) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? C8 C2 C3 C4 -176.2(4) . . . . ? Ru1 C2 C3 C4 -53.3(3) . . . . ? C1 C2 C3 Ru1 54.2(3) . . . . ? C8 C2 C3 Ru1 -122.9(4) . . . . ? C4 Ru1 C3 C2 -132.9(4) . . . . ? C1 Ru1 C3 C2 -30.5(3) . . . . ? C6 Ru1 C3 C2 -67.1(3) . . . . ? C5 Ru1 C3 C2 -104.7(3) . . . . ? S1 Ru1 C3 C2 138.1(2) . . . . ? Cl2 Ru1 C3 C2 50.7(3) . . . . ? Cl1 Ru1 C3 C2 -137.5(3) . . . . ? C1 Ru1 C3 C4 102.4(3) . . . . ? C2 Ru1 C3 C4 132.9(4) . . . . ? C6 Ru1 C3 C4 65.8(2) . . . . ? C5 Ru1 C3 C4 28.2(2) . . . . ? S1 Ru1 C3 C4 -89.0(2) . . . . ? Cl2 Ru1 C3 C4 -176.43(18) . . . . ? Cl1 Ru1 C3 C4 -4.6(4) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? Ru1 C3 C4 C5 -54.8(3) . . . . ? C2 C3 C4 Ru1 53.9(3) . . . . ? C3 Ru1 C4 C5 133.8(3) . . . . ? C1 Ru1 C4 C5 67.2(2) . . . . ? C2 Ru1 C4 C5 105.1(2) . . . . ? C6 Ru1 C4 C5 30.7(2) . . . . ? S1 Ru1 C4 C5 -135.8(2) . . . . ? Cl2 Ru1 C4 C5 141.2(2) . . . . ? Cl1 Ru1 C4 C5 -48.2(2) . . . . ? C1 Ru1 C4 C3 -66.6(2) . . . . ? C2 Ru1 C4 C3 -28.7(2) . . . . ? C6 Ru1 C4 C3 -103.2(2) . . . . ? C5 Ru1 C4 C3 -133.8(3) . . . . ? S1 Ru1 C4 C3 90.4(2) . . . . ? Cl2 Ru1 C4 C3 7.4(4) . . . . ? Cl1 Ru1 C4 C3 177.93(18) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? Ru1 C4 C5 C6 -54.2(3) . . . . ? C3 C4 C5 C7A 178.9(3) . . . . ? Ru1 C4 C5 C7A 124.8(3) . . . . ? C3 C4 C5 Ru1 54.1(3) . . . . ? C3 Ru1 C5 C4 -28.5(2) . . . . ? C1 Ru1 C5 C4 -102.0(2) . . . . ? C2 Ru1 C5 C4 -64.9(2) . . . . ? C6 Ru1 C5 C4 -129.9(3) . . . . ? S1 Ru1 C5 C4 50.2(2) . . . . ? Cl2 Ru1 C5 C4 -136.0(2) . . . . ? Cl1 Ru1 C5 C4 139.3(2) . . . . ? C4 Ru1 C5 C6 129.9(3) . . . . ? C3 Ru1 C5 C6 101.5(2) . . . . ? C1 Ru1 C5 C6 27.9(2) . . . . ? C2 Ru1 C5 C6 65.0(2) . . . . ? S1 Ru1 C5 C6 -179.80(19) . . . . ? Cl2 Ru1 C5 C6 -6.1(4) . . . . ? Cl1 Ru1 C5 C6 -90.8(2) . . . . ? C4 Ru1 C5 C7A -114.1(4) . . . . ? C3 Ru1 C5 C7A -142.5(4) . . . . ? C1 Ru1 C5 C7A 143.9(4) . . . . ? C2 Ru1 C5 C7A -179.0(4) . . . . ? C6 Ru1 C5 C7A 116.0(4) . . . . ? S1 Ru1 C5 C7A -63.8(3) . . . . ? Cl2 Ru1 C5 C7A 109.9(4) . . . . ? Cl1 Ru1 C5 C7A 25.2(3) . . . . ? C2 C1 C6 C5 -1.1(6) . . . . ? Ru1 C1 C6 C5 52.9(3) . . . . ? C2 C1 C6 Ru1 -54.0(4) . . . . ? C4 C5 C6 C1 1.1(5) . . . . ? C7A C5 C6 C1 -177.9(4) . . . . ? Ru1 C5 C6 C1 -52.5(3) . . . . ? C4 C5 C6 Ru1 53.6(3) . . . . ? C7A C5 C6 Ru1 -125.4(3) . . . . ? C4 Ru1 C6 C1 103.5(3) . . . . ? C3 Ru1 C6 C1 66.0(2) . . . . ? C2 Ru1 C6 C1 28.9(2) . . . . ? C5 Ru1 C6 C1 133.9(3) . . . . ? S1 Ru1 C6 C1 134.3(2) . . . . ? Cl2 Ru1 C6 C1 -48.8(2) . . . . ? Cl1 Ru1 C6 C1 -135.7(2) . . . . ? C4 Ru1 C6 C5 -30.4(2) . . . . ? C3 Ru1 C6 C5 -67.8(2) . . . . ? C1 Ru1 C6 C5 -133.9(3) . . . . ? C2 Ru1 C6 C5 -105.0(2) . . . . ? S1 Ru1 C6 C5 0.4(4) . . . . ? Cl2 Ru1 C6 C5 177.27(18) . . . . ? Cl1 Ru1 C6 C5 90.4(2) . . . . ? C4 C5 C7A C10A -166.5(5) . . . . ? C6 C5 C7A C10A 12.4(6) . . . . ? Ru1 C5 C7A C10A -78.2(5) . . . . ? C4 C5 C7A C9A 67.8(6) . . . . ? C6 C5 C7A C9A -113.3(5) . . . . ? Ru1 C5 C7A C9A 156.1(5) . . . . ? C11 S1 C12 C13 67.9(4) . . . . ? Ru1 S1 C12 C13 178.2(3) . . . . ? S1 C12 C13 C14 -98.9(4) . . . . ? S1 C12 C13 C13 80.7(5) . . . 2_554 ? C13 C13 C14 C15 -0.7(7) 2_554 . . . ? C12 C13 C14 C15 178.9(4) . . . . ? C13 C14 C15 C15 -1.1(8) . . . 2_554 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.155 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.106 #===END OF CIF ============================================================== # # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # #===END OF FILE =============================================================