#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2000 Version : 08/11/2007' # 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 ; Petricek, V., Dusek, M. & Palatinus L. (2000). Jana2000. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. # enable this reference if Diamond ver. 2 was used for visualization #Brandenburg, K. (1999). DIAMOND. Version. 2.1c. #Crystal Impact GbR, Bonn, Germany. # enable this reference if Diamond ver. 3 was used for visualization #Brandenburg, K. & Putz, H. (2005). DIAMOND Version 3. #Crystal Impact GbR, Postfach 1251, D-53002 Bonn, Germany. # enable 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 SIR2002 was used for solving of the structure #Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., #Polidori, G., Spagna, R. #SIR2002: the program, J. Appl. Cryst, (2003). 36, 1103 # enable this reference if bond valences were calculated #Brown, I. D. (1996). J. Appl. Cryst. 29, 479-480. # enable this reference if Xshape wase used for crystal shape refinement #Stoe & Cie (1998). X-SHAPE. Stoe & Cie, Darmstadt, Germany. # enable this reference if Flack coefficient was refined #Flack, H. D. (1983). Acta Cryst. A39, 876-881. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_(I) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_mineral 'kurilite' _chemical_compound_source 'Prasolovskoe, Kuril islands' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Ag6.667 Se0.056 Te2.5' _chemical_formula_weight 1042.6 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -x,-y,-z 5 y,-x+y,-z 6 x-y,x,-z 7 2/3+x,1/3+y,1/3+z 8 2/3-y,1/3+x-y,1/3+z 9 2/3-x+y,1/3-x,1/3+z 10 2/3-x,1/3-y,1/3-z 11 2/3+y,1/3-x+y,1/3-z 12 2/3+x-y,1/3+x,1/3-z 13 1/3+x,2/3+y,2/3+z 14 1/3-y,2/3+x-y,2/3+z 15 1/3-x+y,2/3-x,2/3+z 16 1/3-x,2/3-y,2/3-z 17 1/3+y,2/3-x+y,2/3-z 18 1/3+x-y,2/3+x,2/3-z _cell_length_a 15.8135(18) _cell_length_b 15.8135(18) _cell_length_c 19.618(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 4248.6(9) _cell_formula_units_Z 18 _cell_measurement_reflns_used 16523 _cell_measurement_theta_min 9.84 _cell_measurement_theta_max 14.25 _cell_measurement_temperature 293(2) _cell_special_details ; ? ; _exptl_crystal_density_diffrn 7.3325 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10188 _exptl_absorpt_coefficient_mu 21.245 _exptl_crystal_description block _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.035 _exptl_crystal_colour black _exptl_absorpt_correction_type 'gaussian' _exptl_absorpt_process_details 'ABSPACK (Oxford Diffraction, 2006)' _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.268 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w scans' _diffrn_reflns_number 16568 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.06 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _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 16568 _reflns_number_gt 2513 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_gt 0.0365 _refine_ls_R_factor_all 0.0265 _refine_ls_wR_factor_ref 0.0492 _refine_ls_goodness_of_fit_ref 1.12 _refine_ls_goodness_of_fit_gt 1.23 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 2776 _refine_ls_number_parameters 193 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/\s^2^(F)' _refine_ls_hydrogen_treatment undef _refine_ls_shift/su_max 0.0080 _refine_ls_shift/su_mean 0.0062 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? 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 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 Te -0.531 1.675 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 19.964399 4.81742 19.0138 0.420885 6.14487 28.5284 2.5239 70.840302 4.352 Se -0.093 2.226 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 17.000601 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.816299 2.8409 _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2000)' _computing_molecular_graphics ? _computing_publication_material 'Jana2006 (Petricek, Dusek & Palatinus, 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 Ag1 Ag 0 0 0 Uani 0.0536(3) 3 1 d . . . Ag2 Ag 0.36595(6) 0.41067(5) 0.00402(4) Uani 0.0584(2) 18 1 d . . . Ag3 Ag 0.37191(5) 0.43480(6) 0.24452(4) Uani 0.04574(17) 18 1 d . . . Ag4 Ag 0.37626(4) 0.41219(3) 0.45583(2) Uani 0.0673(2) 18 1 d . . . Ag5 Ag 0.16988(6) 0.16995(6) 0.04757(5) Uani 0.0636(2) 18 1 d . . . Ag6 Ag 0.05963(5) 0.19591(5) 0.15858(4) Uani 0.0553(2) 18 1 d . . . Ag7 Ag 0.17553(13) 0.16098(13) 0.21296(8) Uani 0.0477(4) 18 0.5 d . . . Ag8 Ag 0.11496(6) 0.17985(6) 0.45043(4) Uani 0.0567(2) 18 1 d . . . Ag9 Ag 0 0 0.35585(8) Uani 0.0635(3) 6 1 d . . . Ag10 Ag 0.27091(6) 0.45108(6) -0.01333(5) Uani 0.0699(3) 18 1 d . . . Te1 Te 0.24878(2) 0.35741(2) 0.129872(15) Uani 0.04055(15) 18 1 d . . . Te2 Te 0.04143(2) 0.17647(3) 0.304592(16) Uani 0.04251(16) 18 1 d . . . Te3 Te -0.08333(2) 0.20283(3) 0.076750(16) Uani 0.05182(18) 18 1 d . . . Se1 Se 0 0 0.13168(5) Uani 0.0466(3) 6 1 d . . . Se2 Se 0 0 0.5 Uani 0.0382(3) 3 1 d . . . Se3 Se 0.19294(10) 0.16114(11) 0.17202(7) Uani 0.0390(5) 18 0.5 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 Ag1 Ag 0.0545(4) 0.0545(4) 0.0518(7) 0.0273(2) 0 0 Ag2 Ag 0.0629(3) 0.0613(3) 0.0523(2) 0.0319(2) 0.0007(2) 0.0006(2) Ag3 Ag 0.0488(2) 0.0474(2) 0.0408(2) 0.02392(19) -0.00004(18) 0.00005(17) Ag4 Ag 0.0718(3) 0.0681(3) 0.0613(3) 0.0345(3) 0.0004(3) 0.0009(3) Ag5 Ag 0.0658(3) 0.0670(3) 0.0573(3) 0.0327(2) -0.0006(2) 0.0006(2) Ag6 Ag 0.0582(3) 0.0555(2) 0.0520(3) 0.0282(2) -0.0003(2) 0.0002(2) Ag7 Ag 0.0467(5) 0.0528(5) 0.0443(6) 0.0254(5) -0.0004(5) 0.0010(5) Ag8 Ag 0.0596(3) 0.0593(3) 0.0514(2) 0.0299(2) -0.0001(2) 0.0001(2) Ag9 Ag 0.0657(3) 0.0657(3) 0.0590(5) 0.03287(15) 0 0 Ag10 Ag 0.0698(3) 0.0721(3) 0.0662(3) 0.0343(3) -0.0008(3) -0.0001(2) Te1 Te 0.04190(19) 0.0424(2) 0.0372(2) 0.02097(15) 0.00005(13) -0.00022(13) Te2 Te 0.0445(2) 0.0440(2) 0.0392(2) 0.02229(15) 0.00030(14) 0.00010(15) Te3 Te 0.0543(2) 0.0534(2) 0.0469(2) 0.02630(18) 0.00019(17) 0.00010(16) Se1 Se 0.0471(3) 0.0471(3) 0.0456(6) 0.02353(17) 0 0 Se2 Se 0.0401(4) 0.0401(4) 0.0342(7) 0.0201(2) 0 0 Se3 Se 0.0373(7) 0.0427(7) 0.0379(7) 0.0208(5) -0.0013(6) 0.0022(7) #======================================================================= # 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 Ag1 Ag5 . . 2.8444(7) yes Ag1 Ag5 . 4_555 2.8444(7) yes Ag1 Ag5 . 2_555 2.8444(11) yes Ag1 Ag5 . 5_555 2.8444(11) yes Ag1 Ag5 . 3_555 2.8444(11) yes Ag1 Ag5 . 6_555 2.8444(11) yes Ag1 Se1 . . 2.5833(9) yes Ag1 Se1 . 4_555 2.5833(9) yes Ag2 Ag3 . 15_554 2.7898(13) yes Ag2 Ag10 . . 1.9348(16) yes Ag2 Te1 . . 2.9459(9) yes Ag2 Te2 . 12_555 2.9849(12) yes Ag2 Te3 . 5_555 2.8217(8) yes Ag3 Ag8 . 16_555 2.9793(15) yes Ag3 Te1 . . 2.8222(8) yes Ag3 Te1 . 12_555 2.8074(7) yes Ag3 Te2 . 16_555 2.9656(9) yes Ag4 Ag6 . 16_555 2.4578(12) yes Ag4 Te1 . 8_555 2.6063(7) yes Ag4 Te2 . 16_555 2.8862(7) yes Ag4 Te3 . 7_555 2.9920(5) yes Ag4 Te3 . 16_555 2.7336(6) yes Ag4 Se3 . 8_555 2.683(2) yes Ag5 Ag6 . . 2.9440(13) yes Ag5 Te3 . 5_555 2.9393(10) yes Ag5 Te3 . 3_555 2.8466(12) yes Ag5 Se3 . . 2.4827(16) yes Ag6 Ag7 . . 2.411(3) yes Ag6 Te1 . . 2.8544(7) yes Ag6 Te2 . . 2.8799(9) yes Ag6 Te3 . . 2.8191(10) yes Ag6 Se1 . . 2.8007(9) yes Ag6 Se3 . . 2.444(2) yes Ag7 Ag10 . 8_555 2.2147(19) yes Ag7 Te2 . . 2.882(2) yes Ag7 Te3 . 12_555 2.9424(18) yes Ag7 Se3 . . 0.849(2) yes Ag8 Te1 . 16_555 2.8763(10) yes Ag8 Te1 . 8_555 2.7976(10) yes Ag8 Se2 . . 2.6775(7) yes Ag9 Te2 . . 2.7202(7) yes Ag9 Te2 . 2_555 2.7202(7) yes Ag9 Te2 . 3_555 2.7202(8) yes Ag9 Se2 . . 2.8279(16) yes Ag10 Te2 . 14_554 2.6952(13) yes Ag10 Te2 . 15_554 2.9709(8) yes Ag10 Te3 . 5_555 2.5886(10) yes Ag10 Se3 . 15_554 2.9356(16) yes Te1 Se3 . . 2.8907(17) yes Te3 Se3 . 2_555 2.9989(19) yes Se1 Se3 . . 2.9417(12) yes Se1 Se3 . 2_555 2.942(2) yes Se1 Se3 . 3_555 2.9417(18) yes #=======================================================================