#------------------------------------------------------------------------------ #$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/16/4001657.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4001657 loop_ _publ_author_name 'Purdy, Andrew P.' _publ_section_title ; Ammonothermal Crystal Growth of Sulfide Materials ; _journal_issue 3 _journal_name_full 'Chemistry of Materials' _journal_page_first 692 _journal_paper_doi 10.1021/cm970674h _journal_volume 10 _journal_year 1998 _chemical_compound_source 'CaS + CuI + NH4I in NH3 at 365 C' _chemical_formula_analytical 'not determined' _chemical_formula_moiety '(NH4 +) (Cu4S3 -)' _chemical_formula_sum 'Cu4 H4 N S3' _chemical_formula_weight 368.38 _chemical_melting_point ? _chemical_name_common 'Ammonium tetracoppertrisulfide' _chemical_name_systematic ; ? ; _space_group_IT_number 123 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4 2' _symmetry_space_group_name_H-M 'P 4/m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 3.91010(10) _cell_length_b 3.91010(10) _cell_length_c 9.4758(6) _cell_measurement_reflns_used 47 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 17.32 _cell_measurement_theta_min 4.3 _cell_volume 144.874(11) _computing_cell_refinement 'Siemens XSCANS' _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_molecular_graphics 'SHELXL-94 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-94 (sheldrick, 1994)' _computing_structure_refinement 'SHELXL-94 (Sheldrick, 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 680 _diffrn_reflns_theta_max 34.98 _diffrn_reflns_theta_min 2.15 _diffrn_standards_decay_% 1.89 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 15.419 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_type integration _exptl_crystal_colour black _exptl_crystal_density_diffrn 4.222 _exptl_crystal_description 'square plate' _exptl_crystal_F_000 175 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.354 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.190 _refine_ls_extinction_coef 0.1146(90) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_matrix_type full _refine_ls_number_parameters 17 _refine_ls_number_reflns 239 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_restrained_S_obs 1.091 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_obs 0.0274 _refine_ls_shift/esd_max -0.021 _refine_ls_shift/esd_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0701 _refine_ls_wR_factor_obs 0.0661 _reflns_number_observed 207 _reflns_number_total 239 _reflns_observed_criterion >2sigma(I) _cod_data_source_file cm970674h.cif _cod_data_source_block pur66t _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value 'not determined' was changed to '?' - the value is undefined or not given. '_exptl_absorpt_correction_type' value 'Integration' changed to 'integration' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M P4/mmm _cod_original_formula_sum 'H4 Cu4 N S3' _cod_database_code 4001657 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' 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 0.0116(4) 0.0116(4) 0.0139(6) 0.000 0.000 0.000 S2 0.0126(5) 0.0126(5) 0.0102(7) 0.000 0.000 0.000 Cu1 0.0251(4) 0.0135(3) 0.0278(4) 0.000 0.000 0.000 N1 0.021(2) 0.021(2) 0.017(3) 0.000 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags S1 S 0.0000 0.0000 0.2121(2) 0.0124(3) Uani 1 d S S2 S -0.5000 -0.5000 0.5000 0.0118(4) Uani 1 d S Cu1 Cu 0.0000 -0.5000 0.34295(7) 0.0221(3) Uani 1 d S N1 N -0.5000 0.5000 0.0000 0.019(2) Uani 1 d S H1 H -0.6121(261) 0.3879(261) 0.0385(124) 0.011(53) Uiso 0.25(8) d SP loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cu1 S1 Cu1 73.34(3) . 3 Cu1 S1 Cu1 115.24(7) . 1_565 Cu1 S1 Cu1 73.34(3) 3 1_565 Cu1 S1 Cu1 73.34(3) . 3_455 Cu1 S1 Cu1 115.24(7) 3 3_455 Cu1 S1 Cu1 73.34(3) 1_565 3_455 Cu1 S1 N1 142.931(9) . . Cu1 S1 N1 142.931(8) 3 . Cu1 S1 N1 80.321(15) 1_565 . Cu1 S1 N1 80.321(15) 3_455 . Cu1 S2 Cu1 180.0 11_556 3_445 Cu1 S2 Cu1 111.521(13) 11_556 1_455 Cu1 S2 Cu1 68.479(13) 3_445 1_455 Cu1 S2 Cu1 68.479(13) 11_556 9_546 Cu1 S2 Cu1 111.521(13) 3_445 9_546 Cu1 S2 Cu1 180.0 1_455 9_546 Cu1 S2 Cu1 105.44(3) 11_556 11_546 Cu1 S2 Cu1 74.56(3) 3_445 11_546 Cu1 S2 Cu1 111.521(13) 1_455 11_546 Cu1 S2 Cu1 68.479(13) 9_546 11_546 Cu1 S2 Cu1 68.479(13) 11_556 9_446 Cu1 S2 Cu1 111.521(13) 3_445 9_446 Cu1 S2 Cu1 74.56(3) 1_455 9_446 Cu1 S2 Cu1 105.44(3) 9_546 9_446 Cu1 S2 Cu1 68.479(13) 11_546 9_446 Cu1 S2 Cu1 74.56(3) 11_556 3_455 Cu1 S2 Cu1 105.44(3) 3_445 3_455 Cu1 S2 Cu1 68.479(13) 1_455 3_455 Cu1 S2 Cu1 111.521(13) 9_546 3_455 Cu1 S2 Cu1 180.0 11_546 3_455 Cu1 S2 Cu1 111.521(13) 9_446 3_455 Cu1 S2 Cu1 111.521(13) 11_556 . Cu1 S2 Cu1 68.479(13) 3_445 . Cu1 S2 Cu1 105.44(3) 1_455 . Cu1 S2 Cu1 74.56(3) 9_546 . Cu1 S2 Cu1 111.521(13) 11_546 . Cu1 S2 Cu1 180.0 9_446 . Cu1 S2 Cu1 68.479(13) 3_455 . S1 Cu1 S1 115.24(7) . 1_545 S1 Cu1 S2 108.93(2) . 1_655 S1 Cu1 S2 108.93(2) 1_545 1_655 S1 Cu1 S2 108.93(2) . . S1 Cu1 S2 108.93(2) 1_545 . S2 Cu1 S2 105.44(3) 1_655 . S1 Cu1 Cu1 53.33(2) . 3 S1 Cu1 Cu1 126.67(2) 1_545 3 S2 Cu1 Cu1 55.760(7) 1_655 3 S2 Cu1 Cu1 124.239(6) . 3 S1 Cu1 Cu1 126.67(2) . 3_445 S1 Cu1 Cu1 53.33(2) 1_545 3_445 S2 Cu1 Cu1 124.239(7) 1_655 3_445 S2 Cu1 Cu1 55.760(7) . 3_445 Cu1 Cu1 Cu1 180.00(6) 3 3_445 S1 Cu1 Cu1 53.33(2) . 3_455 S1 Cu1 Cu1 126.67(2) 1_545 3_455 S2 Cu1 Cu1 124.239(6) 1_655 3_455 S2 Cu1 Cu1 55.760(7) . 3_455 Cu1 Cu1 Cu1 90.0 3 3_455 Cu1 Cu1 Cu1 90.0 3_445 3_455 S1 Cu1 Cu1 126.67(2) . 3_545 S1 Cu1 Cu1 53.33(2) 1_545 3_545 S2 Cu1 Cu1 55.760(7) 1_655 3_545 S2 Cu1 Cu1 124.239(7) . 3_545 Cu1 Cu1 Cu1 90.0 3 3_545 Cu1 Cu1 Cu1 90.0 3_445 3_545 Cu1 Cu1 Cu1 180.00(6) 3_455 3_545 S1 Cu1 Cu1 122.38(3) . 9_546 S1 Cu1 Cu1 122.38(3) 1_545 9_546 S2 Cu1 Cu1 52.722(13) 1_655 9_546 S2 Cu1 Cu1 52.722(13) . 9_546 Cu1 Cu1 Cu1 90.0 3 9_546 Cu1 Cu1 Cu1 90.0 3_445 9_546 Cu1 Cu1 Cu1 90.0 3_455 9_546 Cu1 Cu1 Cu1 90.0 3_545 9_546 S1 N1 N1 55.115(11) . 1_545 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 S1 Cu1 2.3149(9) . S1 Cu1 2.3149(9) 3 S1 Cu1 2.3149(9) 1_565 S1 Cu1 2.3149(9) 3_455 S1 N1 3.4183(9) . S2 Cu1 2.4570(4) 11_556 S2 Cu1 2.4570(4) 3_445 S2 Cu1 2.4570(4) 1_455 S2 Cu1 2.4570(4) 9_546 S2 Cu1 2.4570(4) 11_546 S2 Cu1 2.4570(4) 9_446 S2 Cu1 2.4570(4) 3_455 S2 Cu1 2.4570(4) . Cu1 S1 2.3149(9) 1_545 Cu1 S2 2.4570(4) 1_655 Cu1 Cu1 2.7649(1) 3 Cu1 Cu1 2.7649(1) 3_445 Cu1 Cu1 2.7649(1) 3_455 Cu1 Cu1 2.7649(1) 3_545 Cu1 Cu1 2.9763(14) 9_546 N1 N1 3.9101(1) 1_545