#------------------------------------------------------------------------------
#$Date: 2023-11-21 14:36:55 +0100 (Tue 21 de Nov de 2023) $
#$Revision: 287703 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/72/2237277.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2237277
loop_
_publ_author_name
'Schumer, Benjamin N.'
'Downs, Robert T.'
'Domanik, Kenneth J.'
'Andrade, Marcelo B.'
'Origlieri, Marcus J.'
_publ_section_title
;
 Pirquitasite, Ag₂ZnSnS₄
;
_journal_coeditor_code           BR2219
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i8
_journal_page_last               i9
_journal_paper_doi               10.1107/S1600536813001013
_journal_volume                  69
_journal_year                    2013
_chemical_compound_source        'Pirquitas, Jujuy Province, Argentina'
_chemical_formula_iupac
'(Ag1.87 Cu0.13) (Zn0.61 Fe0.36 Cd0.03) Sn S4'
_chemical_formula_structural     'Ag1.87 Cu0.13 Zn0.61 Fe0.36 Cd.03 Sn S4'
_chemical_formula_sum            'Ag1.87 Cd0.03 Cu0.13 Fe0.36 S4 Sn Zn0.61'
_chemical_formula_weight         520.26
_chemical_name_common            Pirquitasite
_chemical_name_mineral           Pirquitasite
_chemical_name_systematic
;
Disilver zinc tin tetrasulfide
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.7757(12)
_cell_length_b                   5.7757(12)
_cell_length_c                   10.870(2)
_cell_measurement_reflns_used    527
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      6.25
_cell_volume                     362.61(13)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XtalDraw (Downs & Hall-Wallace, 2003)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0131
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1312
_diffrn_reflns_theta_full        32.02
_diffrn_reflns_theta_max         32.02
_diffrn_reflns_theta_min         3.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.575
_exptl_absorpt_correction_T_max  0.6332
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2005)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    4.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.868
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.91(6)
_refine_ls_extinction_coef       0.0061(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         575
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0272P)²+2.1498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                570
_reflns_number_total             575
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            br2219.cif
_cod_data_source_block           I
_cod_original_cell_volume        362.60(13)
_cod_original_formula_sum        'Ag1.87 Cd.03 Cu0.13 Fe0.36 S4 Sn Zn0.61'
_cod_database_code               2237277
_cod_database_fobs_code          2237277
_database_code_amcsd             0019767
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ag Ag1 0.0000 0.0000 0.0000 0.0364(4) Uani d S 1 4
Ag Ag2 0.0000 0.5000 0.2500 0.0301(6) Uani d SP 0.87 4
Cu Cu 0.0000 0.5000 0.2500 0.0301(6) Uani d SP 0.13 4
Zn Zn 0.5000 0.0000 0.2500 0.0220(6) Uani d SP 0.61 4
Fe Fe 0.5000 0.0000 0.2500 0.0220(6) Uani d SP 0.36 4
Cd Cd 0.5000 0.0000 0.2500 0.0220(6) Uani d SP 0.03 4
Sn Sn 0.5000 0.5000 0.0000 0.01176(18) Uani d S 1 4
S S 0.7325(3) 0.2526(4) 0.12847(11) 0.0214(3) Uani d . 1 1
loop_
_atom_site_aniso_label
_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 0.0360(5) 0.0360(5) 0.0372(4) 0.000 0.000 0.000
Ag2 0.0274(7) 0.0274(7) 0.0355(9) 0.000 0.000 0.000
Cu 0.0274(7) 0.0274(7) 0.0355(9) 0.000 0.000 0.000
Zn 0.0248(8) 0.0248(8) 0.0163(9) 0.000 0.000 0.000
Fe 0.0248(8) 0.0248(8) 0.0163(9) 0.000 0.000 0.000
Cd 0.0248(8) 0.0248(8) 0.0163(9) 0.000 0.000 0.000
Sn 0.0114(2) 0.0114(2) 0.0125(3) 0.000 0.000 0.000
S 0.0250(6) 0.0212(6) 0.0181(6) 0.0053(5) -0.0023(5) 0.0044(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 '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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Cd Cd -0.8075 1.2024 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
S Ag1 S 4_545 3_565 113.39(6)
S Ag1 S 4_545 1_455 107.55(3)
S Ag1 S 3_565 1_455 107.55(3)
S Ag1 S 4_545 2_655 107.55(3)
S Ag1 S 3_565 2_655 107.55(3)
S Ag1 S 1_455 2_655 113.39(6)
S Ag2 S 1_455 2_665 115.77(7)
S Ag2 S 1_455 7_465 106.42(3)
S Ag2 S 2_665 7_465 106.42(3)
S Ag2 S 1_455 8_545 106.42(3)
S Ag2 S 2_665 8_545 106.42(3)
S Ag2 S 7_465 8_545 115.77(7)
S Zn S 2_655 7 107.90(4)
S Zn S 2_655 . 112.66(8)
S Zn S 7 . 107.90(4)
S Zn S 2_655 8_545 107.90(4)
S Zn S 7 8_545 112.66(8)
S Zn S . 8_545 107.90(4)
S Sn S 3_565 . 109.67(4)
S Sn S 3_565 2_665 109.67(4)
S Sn S . 2_665 109.08(7)
S Sn S 3_565 4_655 109.08(7)
S Sn S . 4_655 109.67(4)
S Sn S 2_665 4_655 109.67(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ag1 S 4_545 2.5430(17)
Ag1 S 3_565 2.5430(17)
Ag1 S 1_455 2.5430(17)
Ag1 S 2_655 2.5430(17)
Ag2 S 1_455 2.485(2)
Ag2 S 2_665 2.485(2)
Ag2 S 7_465 2.485(2)
Ag2 S 8_545 2.485(2)
Zn S 2_655 2.383(2)
Zn S 7 2.383(2)
Zn S . 2.383(2)
Zn S 8_545 2.383(2)
Sn S 3_565 2.4070(16)
Sn S . 2.4070(16)
Sn S 2_665 2.4070(16)
Sn S 4_655 2.4070(16)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
_cod_related_entry_description
1 AMCSD 0019767 .
2 Wikidata Q425727 pirquitasite
