#====================================================================== data_global _publ_requested_journal Inorg.Chem. #============================================================================= # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Akiko Kobayashi' _publ_contact_author_address # Address of author for ;Department of Chemistry, College of Humanities and Sciences, Nihon University, Sakurajosui 3-25-40, Setagaya-Ku, Tokyo 156-8550, Japan, ; _publ_contact_author_email akoba@chs.nihon-u.ac.jp _publ_contact_author_phone ? _publ_contact_author_fax ? #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================== _publ_section_title ; Title (type here to add) ; _publ_section_title_footnote . loop_ _publ_author_footnote ; ? ; #============================================================================== # 4. TEXT (For Acta Cryst. C and E, include the text of your paper in the CIF) #============================================================================== _publ_section_synopsis . _publ_section_abstract ; (type here to add abstract) ; _publ_section_comment ; (type here to add) ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; (type here to add preparation details) ; _publ_section_exptl_refinement ; (type here to add refinement details) ; _publ_section_references ; ? ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; #============================================================================== # If more than one structure is reported, sections 5-10 should be completed # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== data_Au(tmdt)2_9K # by a unique identifier. #============================================================================== # 5. CHEMICAL DATA #============================================================================== _chemical_name_systematic '[Au(tmdt)2]' _chemical_name_common '[Au(tmdt)2]' _chemical_formula_moiety 'C18 H12 Au S12' _chemical_formula_sum 'C18 H12 Au S12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 810.1 #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA #============================================================================== _space_group_crystal_system Triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z #------------------------------------------------------------------------------ _cell_length_a 6.35584(5) _cell_length_b 7.35278(5) _cell_length_c 12.08905(8) _cell_angle_alpha 89.7445(9) _cell_angle_beta 96.4578(7) _cell_angle_gamma 103.0535(9) _cell_volume 546.74(1) _cell_formula_units_Z 1 _cell_measurement_temperature 9 _cell_special_details ; ; #------------------------------------------------------------------------------ _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 391 _exptl_crystal_colour Black #------------------------------------------------------------------------------ _diffrn_ambient_temperature 9 #------------------------------------------------------------------------------ # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection #------------------------------------------------------------------------------ # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions #------------------------------------------------------------------------------ # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? #------------------------------------------------------------------------------ # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA #============================================================================== _exptl_special_details ; ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ; _diffrn_radiation_probe x-ray #------------------------------------------------------------------------------ _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.50247 _diffrn_source synchrotron _diffrn_source_type 'SPring-8 BL02B2' _diffrn_source_target ? _diffrn_measurement_device_type ? _diffrn_detector 'Imaging Plate' _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ; _diffrn_radiation_monochromator Si(111) _pd_meas_2theta_range_min 0.006 _pd_meas_2theta_range_max 37.634 _pd_meas_2theta_range_inc ? _pd_meas_number_of_points 7860 #============================================================================== # 8. REFINEMENT DATA #============================================================================== # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function pseudo-Voigt _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; _pd_proc_ls_prof_R_factor ? _pd_proc_ls_prof_wR_factor 0.017 _refine_ls_R_I_factor 0.024 _refine_special_details ; rigid-body refinement. ; #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? # options are 'sigma' (based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? #------------------------------------------------------------------------------ _refine_ls_number_parameters ? _refine_ls_number_constraints ? _refine_ls_number_restraints 0 #------------------------------------------------------------------------------ # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all ? _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? #------------------------------------------------------------------------------ _pd_proc_2theta_range_min 1.9 _pd_proc_2theta_range_max 37.45 _pd_proc_2theta_range_inc ? _pd_proc_wavelength 0.50247 _pd_block_diffractogram_id ? #------------------------------------------------------------------------------ # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement 'Synchrotron Powder(Eiji Nishibori,2007)' _computing_data_reduction 'Synchrotron Powder' _computing_structure_solution ? _computing_structure_refinement 'Synchrotron Powder' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS #============================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Au1 Au Uani 0.00000 0.00000 0.00000 1.000 . d G S1 S Uani 0.3513(3) 0.0601(4) 0.0909(2) 1.000 . d G S2 S Uani -0.1376(3) 0.0656(4) 0.1615(2) 1.000 . d G C1 C Uani 0.303(1) 0.118(1) 0.2252(6) 1.000 . d G C2 C Uani 0.103(1) 0.121(1) 0.2542(6) 1.000 . d G S3 S Uani 0.5221(3) 0.1765(4) 0.3279(2) 1.000 . d G S4 S Uani 0.0865(3) 0.1815(3) 0.3909(2) 1.000 . d G C3 C Uiso 0.366(1) 0.215(1) 0.4319(6) 1.000 0.010(3) d G C4 C Uiso 0.454(1) 0.267(1) 0.5364(6) 1.000 0.010(3) d G S5 S Uani 0.7352(3) 0.3014(4) 0.5786(2) 1.000 . d G S6 S Uani 0.2981(3) 0.3064(4) 0.6418(2) 1.000 . d G C5 C Uiso 0.716(1) 0.362(1) 0.7141(7) 1.000 0.013(3) d G C6 C Uiso 0.518(1) 0.364(1) 0.7427(7) 1.000 0.013(3) d G C7 C Uiso 0.894(1) 0.414(1) 0.8094(7) 1.000 0.008(3) d G C8 C Uiso 0.522(1) 0.419(2) 0.8632(7) 1.000 0.008(3) d G C9 C Uiso 0.768(1) 0.452(1) 0.9067(6) 1.000 0.005(3) d G H1 H Uiso 0.99(2) 0.31(1) 0.828(8) 1.000 0.048 d G H2 H Uiso 1.02(2) 0.54(1) 0.793(8) 1.000 0.048 d G H3 H Uiso 0.42(2) 0.31(1) 0.910(8) 1.000 0.048 d G H4 H Uiso 0.46(2) 0.54(1) 0.874(8) 1.000 0.048 d G H5 H Uiso 0.79(2) 0.36(1) 0.974(8) 1.000 0.048 d G H6 H Uiso 0.83(2) 0.60(1) 0.937(8) 1.000 0.048 d G 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 Au1 0.0115(3) 0.0142(4) 0.0029(3) -0.0033(3) -0.0004(3) 0.0028(3) S1 0.007(1) 0.008(2) 0.004(1) -0.003(1) -0.0003(8) 0.001(1) S2 0.007(1) 0.008(2) 0.004(1) -0.003(1) -0.0003(9) 0.001(1) C1 0.006(4) 0.008(7) 0.003(5) -0.003(4) -0.000(3) 0.001(4) C2 0.006(5) 0.008(6) 0.003(4) -0.003(5) -0.000(4) 0.001(5) S3 0.006(1) 0.016(2) 0.004(1) -0.003(1) -0.0003(8) 0.003(1) S4 0.006(1) 0.016(2) 0.004(1) -0.003(1) -0.000(1) 0.003(1) S5 0.009(1) 0.015(2) 0.002(1) -0.003(1) -0.001(1) 0.003(1) S6 0.009(1) 0.015(2) 0.002(1) -0.003(1) -0.0005(9) 0.003(1) # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================== # 10. MOLECULAR GEOMETRY #============================================================================== _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Au1 S1 2.32272 Au1 S2 2.32267 S1 C1 1.75749 S2 C2 1.75753 C1 C2 1.36420 C1 S3 1.73391 C2 S4 1.73392 S3 C3 1.74957 S4 C3 1.74964 C3 C4 1.34335 C4 S5 1.76269 C4 S6 1.76274 S5 C5 1.72374 S6 C6 1.72362 C5 C6 1.34637 C5 C7 1.50806 C6 C8 1.50805 C7 C9 1.55395 C8 C9 1.55394 C7 H1 1.09049 C7 H2 1.09051 C8 H3 1.09056 C8 H4 1.09056 C9 H5 1.09212 C9 H6 1.09212 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle S1 Au1 S2 91.33423 Au1 S1 C1 100.46950 Au1 S2 C2 100.46975 S1 C1 C2 123.86335 S2 C2 C1 123.86317 S1 C1 S3 118.72103 S2 C2 S4 118.72226 C2 C1 S3 117.41562 C1 C2 S4 117.41457 C1 S3 C3 94.78874 C2 S4 C3 94.78719 S3 C3 S4 115.59388 S3 C3 C4 122.20301 S4 C3 C4 122.20311 C3 C4 S5 122.57162 C3 C4 S6 122.57247 S5 C4 S6 114.85590 C4 S5 C5 94.45610 C4 S6 C6 94.45713 S5 C5 C6 118.11296 S6 C6 C5 118.11791 S5 C5 C7 128.85796 S6 C6 C8 128.85691 C6 C5 C7 113.02908 C5 C6 C8 113.02518 C5 C7 C9 102.59902 C6 C8 C9 102.60144 C7 C9 C8 108.74528 C5 C7 H1 113.33426 C5 C7 H2 113.33549 C6 C8 H3 113.33367 C6 C8 H4 113.33891 H1 C7 H2 102.41811 H3 C8 H4 102.41615 C9 C7 H1 112.78632 C9 C7 H2 112.78399 C9 C8 H3 112.78365 C9 C8 H4 112.78329 C7 C9 H5 109.59465 C7 C9 H6 109.59341 C8 C9 H5 109.59317 C8 C9 H6 109.59125 H5 C9 H6 109.70584 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== #===END #=============================================================================== data_Au(tmdt)2_300K #============================================================================== # 5. CHEMICAL DATA #============================================================================== _chemical_name_systematic ; Endohedral metallofullerene ; _chemical_name_common ? _chemical_formula_moiety 'C18 H12 Au S12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H12 Au S12' _chemical_formula_weight 810.09 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.009 0.004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -11.631 4.032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.223 0.272 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA #============================================================================== _space_group_crystal_system Triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 'x,y,z' 2 '-x,-y,-z' #------------------------------------------------------------------------------ _cell_length_a 6.40300(2) _cell_length_b 7.48729(3) _cell_length_c 12.13353(4) _cell_angle_alpha 90.2312(4) _cell_angle_beta 96.6760(3) _cell_angle_gamma 103.1443(5) _cell_volume 562.335(7) _cell_formula_units_Z 1 _cell_measurement_temperature 300 _cell_special_details ; ; #------------------------------------------------------------------------------ _exptl_crystal_density_diffrn 2.392 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 391 _exptl_crystal_colour 'Black' #------------------------------------------------------------------------------ # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection #------------------------------------------------------------------------------ # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions #------------------------------------------------------------------------------ # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? #------------------------------------------------------------------------------ # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu 27.039 _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA #============================================================================== _exptl_special_details ; ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ; #------------------------------------------------------------------------------ _diffrn_ambient_temperature 300 _diffrn_source 'synchrotron' _diffrn_source_target ? _diffrn_source_type 'SPring-8 BL02B2' _diffrn_measurement_device_type '?' _diffrn_detector 'Imaging Plate' _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ; #------------------------------------------------------------------------------ _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 1.04890 _diffrn_radiation_monochromator Si(111) _pd_meas_2theta_range_min 0.010 _pd_meas_2theta_range_max 75.140 _pd_meas_2theta_range_inc 0.010 _pd_meas_number_of_points 7514 #============================================================================== # 8. REFINEMENT DATA #============================================================================== # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function 'pseudo-Voigt' _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; _pd_proc_ls_prof_R_factor 0.015 _pd_proc_ls_prof_wR_factor 0.021 _refine_ls_R_I_factor 0.032 _refine_special_details ; rigid-body refinement. ; #------------------------------------------------------------------------------ _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type ? _refine_ls_weighting_scheme ? # options are 'sigma' (based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? #------------------------------------------------------------------------------ _refine_ls_number_parameters 105 _refine_ls_number_constraints ? _refine_ls_number_restraints 0 #------------------------------------------------------------------------------ # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all ? _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? #------------------------------------------------------------------------------ _pd_proc_2theta_range_min 4.000 _pd_proc_2theta_range_max 74.000 _pd_proc_2theta_range_inc 0.010 _pd_proc_wavelength 1.04890 _pd_block_diffractogram_id ? #------------------------------------------------------------------------------ # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement 'Synchrotron Powder(Eiji Nishibori,2007)' _computing_data_reduction 'Synchrotron Powder' _computing_structure_solution ? _computing_structure_refinement 'Synchrotron Powder' _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS #============================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Au31 Au Uani 1.00000 1.00000 1.00000 1.000 0.02639(19) d G S2 S Uani 0.6525(2) 0.9394(3) 0.91007(9) 1.000 0.0260(7) d G S3 S Uani 1.1359(2) 0.9364(3) 0.84014(9) 1.000 0.0260(7) d G S6 S Uani 0.4805(2) 0.8230(3) 0.67238(9) 1.000 0.0278(8) d G S7 S Uani 0.9117(2) 0.8203(3) 0.61002(9) 1.000 0.0278(8) d G S10 S Uani 0.2695(2) 0.6993(3) 0.4236(1) 1.000 0.0297(7) d G S11 S Uani 0.7012(2) 0.6966(3) 0.3611(1) 1.000 0.0297(7) d G C4 C Uani 0.6986(2) 0.8820(7) 0.7758(1) 1.000 0.011(2) d G C5 C Uani 0.8972(2) 0.8808(7) 0.7470(1) 1.000 0.011(2) d G C8 C Uiso 0.6357(2) 0.7862(8) 0.5699(1) 1.000 0.0204(18) d G C9 C Uiso 0.5476(2) 0.7345(7) 0.4659(1) 1.000 0.0204(18) d G C12 C Uiso 0.2854(3) 0.6389(8) 0.2866(2) 1.000 0.0269(18) d G C13 C Uiso 0.4820(3) 0.6377(8) 0.2581(2) 1.000 0.0269(18) d G C14 C Uiso 0.1116(3) 0.5876(8) 0.1946(2) 1.000 0.0244(17) d G C15 C Uiso 0.4791(4) 0.5854(8) 0.1415(2) 1.000 0.0244(17) d G C20 C Uiso 0.2340(4) 0.5505(8) 0.0956(2) 1.000 0.0284(19) d G H16 H Uiso 0.0210(3) 0.6928(8) 0.1765(2) 1.000 0.0751(17) d G H17 H Uiso 0.0136(3) 0.4690(8) 0.2109(2) 1.000 0.0751(17) d G H18 H Uiso 0.5793(4) 0.6894(8) 0.0957(2) 1.000 0.0751(17) d G H19 H Uiso 0.5448(4) 0.4655(8) 0.1301(2) 1.000 0.0751(17) d G H21 H Uiso 0.2108(4) 0.6438(8) 0.0288(2) 1.000 0.0790(18) d G H22 H Uiso 0.1745(4) 0.4086(8) 0.0649(2) 1.000 0.0790(18) d G 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 Au31 0.0244(3) 0.0393(4) 0.0137(3) -0.0091(3) -0.0045(2) 0.0072(3) S2 0.0173(9) 0.0484(17) 0.0124(9) -0.0078(10) -0.0020(8) 0.010(1) S3 0.0173(9) 0.0484(17) 0.0124(9) -0.0078(10) -0.0020(7) 0.010(1) S6 0.0203(10) 0.0561(21) 0.0082(8) -0.0040(9) 0.0000(7) 0.0122(12) S7 0.0203(10) 0.0561(21) 0.0082(8) -0.0040(9) 0.0000(7) 0.0122(12) S10 0.0243(11) 0.0557(17) 0.0094(9) -0.0088(10) -0.0010(7) 0.0116(11) S11 0.0243(11) 0.0557(17) 0.0094(9) -0.0088(10) -0.0010(7) 0.0116(11) C4 0.0080(34) 0.0180(54) 0.0077(30) -0.0040(28) 0.0000(24) 0.0036(34) C5 0.0080(34) 0.0180(54) 0.0077(30) -0.0040(28) 0.0000(24) 0.0036(34) _atom_site_special_details ; ; # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================== # 10. MOLECULAR GEOMETRY #============================================================================== _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Au31 S2 2.3064 Au31 S3 2.3064 S2 C4 1.7578 S3 C5 1.7583 S6 C4 1.7400 S6 C8 1.7374 S7 C5 1.7393 S7 C8 1.7375 S10 C9 1.7540 S10 C12 1.7414 S11 C9 1.7549 S11 C13 1.7414 C4 C5 1.3593 C8 C9 1.3385 C12 C13 1.3456 C12 C14 1.4647 C13 C15 1.4633 C14 C20 1.5651 C15 C20 1.5654 C14 H16 1.0900 C14 H17 1.0000 C15 H18 1.0900 C15 H19 1.0900 C20 H21 1.0900 C20 H22 1.0900 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle S2 Au31 S3 91.63 Au31 S2 C4 100.52 Au31 S3 C5 100.53 C4 S6 C8 94.67 C5 S7 C8 94.65 C9 S10 C12 95.13 C9 S11 C13 95.14 S2 C4 S6 119.13 S2 C4 C5 123.70 S6 C4 C5 117.18 S3 C5 S7 119.12 S3 C5 C4 123.62 S7 C5 C4 117.26 S6 C8 S7 116.24 S6 C8 C9 121.88 S7 C8 C9 121.88 S10 C9 S11 114.70 S10 C9 C8 122.65 S11 C9 C8 122.65 S10 C12 C13 117.54 S10 C12 C14 128.97 C13 C12 C14 113.49 S11 C13 C12 117.49 S11 C13 C15 128.95 C12 C13 C15 113.56 C12 C14 C20 103.03 C13 C15 C20 103.04 C14 C20 C15 106.88 C12 C14 H16 114.00 C12 C14 H17 109.00 C20 C14 H16 112.00 C20 C14 H17 108.00 H16 C14 H17 111.00 C13 C15 H18 114.00 C13 C15 H19 114.00 C20 C15 H18 112.00 C20 C15 H19 112.00 H18 C15 H19 103.00 C14 C20 H21 110.00 C14 C20 H22 110.00 C15 C20 H21 110.00 C15 C20 H22 110.00 H21 C20 H22 110.00 #============================================================================== # Additional structures (sections 5-10 and associated data_? identifiers) # may be added at this point. #============================================================================== # 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 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ #======================================================================