#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2000 Version : 17/02/2006' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _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_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Acta Crystallographica Section C' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Acta Crystallographica Section C' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ? # name ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. Petricek, V., Dusek, M. & Palatinus L. (2000). Jana2000. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. # use this reference if Diamond ver. 2 was used for visualization Brandenburg, K. (1999). DIAMOND. Version. 2.1c. Crystal Impact GbR, Bonn, Germany. # use this reference if Diamond ver. 3 was used for visualization in preparation # use this reference if SIR97 was used for solving of the structure Altomare, A., Burla, M. C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G., Spagna, R. (1997). SIR97. A Package for Crystal Structure Solution by Direct Methods and Refinement, Bari, Rome, Italy. # use this reference if bond valences were calculated Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # use this reference if Xshape wase used for crystal shape refinement Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_(I) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common stephanite _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ag2.5 S2 Sb0.5' _chemical_formula_weight 394.7 _chemical_melting_point ? _chemical_compound_source ? #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2zc;-2x' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 -x,y,z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2-y,1/2+z 7 1/2-x,1/2+y,z 8 1/2+x,1/2-y,1/2+z _cell_length_a 7.8329(6) _cell_length_b 12.4576(12) _cell_length_c 8.5272(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 832.08(12) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 298(2) _cell_special_details ; ? ; _exptl_crystal_density_diffrn 6.2990 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 15.647 _exptl_crystal_description ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details 'ABSPACK (Oxford Diffraction, 2006)' _exptl_absorpt_correction_T_min 0.486 _exptl_absorpt_correction_T_max 0.710 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_reflns_number 5362 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 1041 _reflns_number_gt 998 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_gt 0.1106 _refine_ls_R_factor_all 0.0466 _refine_ls_wR_factor_ref 0.1125 _refine_ls_goodness_of_fit_ref 1.53 _refine_ls_goodness_of_fit_gt 1.54 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 1041 _refine_ls_number_parameters 62 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0036I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0002 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 6.9053 1.4679 5.2034 22.215099 1.4379 0.2536 1.5863 56.172001 0.8669 Ag -0.897 1.102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 19.2808 0.6446 16.688499 7.4726 4.8045 24.6605 1.0463 99.815598 5.179 Sb -0.587 1.546 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.282501 4.5909 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0 -0.16905(7) -0.485736 Uani 0.0305(2) 4 1 d . . . Ag1 Ag 0.18557(12) 0.12312(9) -0.39887(16) Uani 0.0508(3) 8 1 d . . . Ag2 Ag 0.3139(4) 0.0648(3) -0.7151(3) Uani 0.0676(4) 8 1 d . . . Ag3 Ag 0.5 -0.14506(14) -0.5544(3) Uani 0.0587(5) 4 1 d . . . S1 S 0.5 0.0276(3) -0.4083(4) Uani 0.0335(8) 4 1 d . . . S2 S 0 0.0142(3) -0.5905(4) Uani 0.0305(8) 4 1 d . . . S3 S -0.2294(3) -0.23297(19) -0.6536(3) Uani 0.0326(6) 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb1 Sb 0.0323(4) 0.0323(4) 0.0268(4) 0 0 0.0009(3) Ag1 Ag 0.0559(5) 0.0576(6) 0.0389(5) -0.0102(4) -0.0004(3) -0.0109(4) Ag2 Ag 0.0670(7) 0.0750(8) 0.0609(7) 0.0197(6) 0.0101(5) -0.0239(6) Ag3 Ag 0.0512(7) 0.0577(8) 0.0673(11) 0 0 -0.0184(7) S1 S 0.0331(12) 0.0381(16) 0.0295(15) 0 0 0.0046(14) S2 S 0.0305(11) 0.0300(13) 0.0311(15) 0 0 0.0007(12) S3 S 0.0324(9) 0.0313(10) 0.0340(10) -0.0050(8) -0.0029(9) 0.0020(9) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sb1 S2 . . 2.451(3) yes Sb1 S3 . . 2.431(2) yes Sb1 S3 . 3_555 2.431(2) yes Ag1 Ag1 . 3_555 2.9071(13) yes Ag1 Ag2 . . 2.968(3) yes Ag1 Ag2 . 4_555 2.991(3) yes Ag1 S1 . . 2.7364(18) yes Ag1 S2 . . 2.574(3) yes Ag1 S3 . 5_555 2.894(3) yes Ag1 S3 . 2_555 2.523(3) yes Ag2 Ag2 . 3_655 2.916(4) yes Ag2 S1 . 2_654 2.483(4) yes Ag2 S2 . . 2.751(3) yes Ag2 S3 . 5_555 2.596(4) yes Ag3 S1 . . 2.486(4) yes Ag3 S3 . 1_655 2.532(3) yes Ag3 S3 . 3_555 2.532(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S2 Sb1 S3 . . . 95.19(8) yes S2 Sb1 S3 . . 3_555 95.19(8) yes S3 Sb1 S3 . . 3_555 95.28(8) yes S3 Sb1 S3 3_555 . . 95.28(8) yes Ag1 Ag1 Ag2 3_555 . . 109.79(8) yes Ag1 Ag1 Ag2 3_555 . 4_555 109.63(7) yes Ag1 Ag1 S1 3_555 . . 154.16(8) yes Ag1 Ag1 S2 3_555 . . 55.61(5) yes Ag1 Ag1 S3 3_555 . 5_555 103.31(6) yes Ag1 Ag1 S3 3_555 . 2_555 97.82(7) yes Ag2 Ag1 Ag2 . . 4_555 99.82(9) yes Ag2 Ag1 S1 . . . 64.02(10) yes Ag2 Ag1 S2 . . . 59.03(9) yes Ag2 Ag1 S3 . . 5_555 52.54(8) yes Ag2 Ag1 S3 . . 2_555 147.13(9) yes Ag2 Ag1 Ag2 4_555 . . 99.82(9) yes Ag2 Ag1 S1 4_555 . . 51.15(10) yes Ag2 Ag1 S2 4_555 . . 96.30(10) yes Ag2 Ag1 S3 4_555 . 5_555 143.20(8) yes Ag2 Ag1 S3 4_555 . 2_555 86.82(9) yes S1 Ag1 S2 . . . 105.09(9) yes S1 Ag1 S3 . . 5_555 92.29(9) yes S1 Ag1 S3 . . 2_555 97.93(10) yes S2 Ag1 S3 . . 5_555 88.86(10) yes S2 Ag1 S3 . . 2_555 152.76(8) yes S3 Ag1 S3 5_555 . 2_555 104.76(8) yes S3 Ag1 S3 2_555 . 5_555 104.76(8) yes Ag1 Ag2 Ag1 . . 4_554 123.64(11) yes Ag1 Ag2 Ag2 . . 3_655 109.79(11) yes Ag1 Ag2 S1 . . 2_654 156.24(15) yes Ag1 Ag2 S2 . . . 53.32(9) yes Ag1 Ag2 S3 . . 5_555 62.27(9) yes Ag1 Ag2 Ag1 4_554 . . 123.64(11) yes Ag1 Ag2 Ag2 4_554 . 3_655 109.63(12) yes Ag1 Ag2 S1 4_554 . 2_654 59.12(9) yes Ag1 Ag2 S2 4_554 . . 73.91(11) yes Ag1 Ag2 S3 4_554 . 5_555 145.25(13) yes Ag2 Ag2 S1 3_655 . 2_654 54.04(10) yes Ag2 Ag2 S2 3_655 . . 153.32(14) yes Ag2 Ag2 S3 3_655 . 5_555 97.49(13) yes S1 Ag2 S2 2_654 . . 132.44(16) yes S1 Ag2 S3 2_654 . 5_555 131.34(16) yes S2 Ag2 S3 . . 5_555 91.59(13) yes S1 Ag3 S3 . . 1_655 122.81(6) yes S1 Ag3 S3 . . 3_555 122.81(6) yes S3 Ag3 S3 1_655 . 3_555 113.73(11) yes S3 Ag3 S3 3_555 . 1_655 113.73(11) yes Ag1 S1 Ag1 . . 3_655 128.33(14) yes Ag1 S1 Ag2 . . 2_655 135.27(16) yes Ag1 S1 Ag2 . . 4_555 69.72(9) yes Ag1 S1 Ag3 . . . 113.02(8) yes Ag1 S1 Ag1 3_655 . . 128.33(14) yes Ag1 S1 Ag2 3_655 . 2_655 69.72(9) yes Ag1 S1 Ag2 3_655 . 4_555 135.27(16) yes Ag1 S1 Ag3 3_655 . . 113.02(8) yes Ag2 S1 Ag2 2_655 . 4_555 71.91(14) yes Ag2 S1 Ag3 2_655 . . 86.07(13) yes Ag2 S1 Ag2 4_555 . 2_655 71.91(14) yes Ag2 S1 Ag3 4_555 . . 86.07(13) yes Sb1 S2 Ag1 . . . 105.06(11) yes Sb1 S2 Ag1 . . 3_555 105.06(11) yes Sb1 S2 Ag2 . . . 110.73(10) yes Sb1 S2 Ag2 . . 3_555 110.73(10) yes Ag1 S2 Ag1 . . 3_555 68.78(9) yes Ag1 S2 Ag2 . . . 67.65(7) yes Ag1 S2 Ag2 . . 3_555 128.98(13) yes Ag1 S2 Ag1 3_555 . . 68.78(9) yes Ag1 S2 Ag2 3_555 . . 128.98(13) yes Ag1 S2 Ag2 3_555 . 3_555 67.65(7) yes Ag2 S2 Ag2 . . 3_555 126.63(15) yes Ag2 S2 Ag2 3_555 . . 126.63(15) yes Sb1 S3 Ag1 . . 5_445 86.04(8) yes Sb1 S3 Ag1 . . 2_554 102.12(9) yes Sb1 S3 Ag2 . . 5_445 109.90(11) yes Sb1 S3 Ag3 . . 1_455 106.28(10) yes Ag1 S3 Ag1 5_445 . 2_554 171.70(11) yes Ag1 S3 Ag2 5_445 . 5_445 65.19(9) yes Ag1 S3 Ag3 5_445 . 1_455 79.88(8) yes Ag1 S3 Ag1 2_554 . 5_445 171.70(11) yes Ag1 S3 Ag2 2_554 . 5_445 109.97(11) yes Ag1 S3 Ag3 2_554 . 1_455 98.99(10) yes Ag2 S3 Ag3 5_445 . 1_455 126.63(12) yes #=======================================================================