A fresh view on the structure and twinning of owyheeite, a rod-polytype and twofold superstructure.
Stöger, Berthold; Göb, Christian; Topa, Dan; Acta crystallographica Section B, Structural science, crystal engineering and materials 79 (2023) –; doi:10.1107/S2052520623004523

data_2312140
_publ_section_title
;
 A fresh view on the structure and twinning of owyheeite, a rod-polytype
 and twofold superstructure.
;
_journal_coeditor_code           RA5131
_journal_issue                   4
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_paper_doi               10.1107/S2052520623004523
_journal_volume                  79
_journal_year                    2023
_chemical_formula_moiety         'Ag2.802 Cu0.198 Pb9.773 S28 Sb11.227'
_chemical_formula_sum            'Ag2.8 Cu0.2 Pb9.77 S28 Sb11.23'
_chemical_formula_weight         4604.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_creation_date             2023-03-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.283(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1882(3)
_cell_length_b                   27.2641(7)
_cell_length_c                   22.8679(7)
_cell_measurement_reflns_used    10665
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.3410
_cell_measurement_theta_min      2.5920
_cell_volume                     5105.1(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-6000 HE'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40130
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         30.477
_diffrn_reflns_theta_min         2.597
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    40.200
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.991
_exptl_crystal_description       needle
_exptl_crystal_F_000             7838
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.017
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.219
_refine_diff_density_min         -4.447
_refine_diff_density_rms         0.476
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         22895
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+282.6104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15639
_reflns_number_total             22895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ra5131sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5105.0(3)
_cod_original_formula_sum        'Ag2.80 Cu0.20 Pb9.77 S28 Sb11.23'
_cod_database_code               2312140
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6672(10)
 0.3328(10)
2. Shared sites
{Sb5A, Pb5A}
{Sb5B, Pb5B}
{Sb6A, Pb6A}
{Pb6B, Sb6B}
{SbAA, PbAA}
{SbAB, PbAB}
{SbBA, PbBA}
3. Uiso/Uaniso restraints and constraints
Uanis(Pb4A) = Uanis(Sb4A)
Uanis(Sb5A) = Uanis(Pb5A)
Uanis(Sb5B) = Uanis(Pb5B)
Uanis(Sb6A) = Uanis(Pb6A)
Uanis(Pb6B) = Uanis(Sb6B)
Uanis(SbAA) = Uanis(PbAA)
Uanis(SbAB) = Uanis(PbAB)
Uanis(SbBA) = Uanis(PbBA)
Uanis(SbBB) = Uanis(PbBB)
Uiso(Cu4B) = Uiso(Ag4C)
4. Others
 1*[Sof(Ag4B)]+1*[Sof(Cu4B)]+1*[Sof(Ag4C)]=1 with esd of 0.00001
 Sof(Sb6B)=1-FVAR(1)
 Sof(Pb6B)=FVAR(1)
 Sof(Sb4A)=1-FVAR(2)
 Sof(Pb4A)=FVAR(2)
 Sof(Pb5B)=1-FVAR(3)
 Sof(Sb5B)=FVAR(3)
 Sof(PbAA)=1-FVAR(4)
 Sof(SbAA)=FVAR(4)
 Sof(Pb5A)=1-FVAR(5)
 Sof(Sb5A)=FVAR(5)
 Sof(PbAB)=1-FVAR(6)
 Sof(SbAB)=FVAR(6)
 Sof(Pb6A)=1-FVAR(7)
 Sof(Sb6A)=FVAR(7)
 Sof(PbBA)=1-FVAR(8)
 Sof(SbBA)=FVAR(8)
 Sof(PbBB)=1-FVAR(9)
 Sof(SbBB)=FVAR(9)
;
_shelx_res_checksum              64373
_shelx_hkl_checksum              84631
_olex2_submission_special_instructions 'No special instructions were received'
_cod_database_fobs_code 2312140