Synthesis, crystal structure, and electronic structure of Li~2~PbSiS~4~: a quaternary thiosilicate with a compressed chalcopyrite-like structure
Stoyko, Stanislav S.; Craig, Andrew J.; Kotchey, Joshua W.; Aitken, Jennifer A.; Acta Crystallographica Section C 77 (2021) 1–10; doi:10.1107/S2053229620015338

data_2022291
_publ_section_title
;
 Synthesis, crystal structure, and electronic structure of Li~2~PbSiS~4~:
 a quaternary thiosilicate with a compressed chalcopyrite-like structure
;
_journal_coeditor_code           KU3266
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1
_journal_page_last               10
_journal_paper_doi               10.1107/S2053229620015338
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'Li2 Pb Si S4'
_chemical_formula_sum            'Li2 Pb S4 Si'
_chemical_formula_weight         377.40
_chemical_name_common            'lithium lead silicon sulfide'
_chemical_name_systematic
;
Dilithium lead silicon tetrasulfide
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.46180(10)
_cell_length_b                   6.46180(10)
_cell_length_c                   7.7333(2)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.4165
_cell_measurement_theta_min      4.0915
_cell_volume                     322.903(11)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
shelXle (H\"ubschle <i>et al.</i>,  2011) and CrystalMaker (Palmer,
2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1559
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.486
_diffrn_reflns_theta_min         4.110
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    27.465
_exptl_absorpt_correction_T_max  0.4352
_exptl_absorpt_correction_T_min  0.2948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.457
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.062(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         236
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0157
_refine_ls_R_factor_gt           0.0155
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0278
_refine_ls_wR_factor_ref         0.0278
_reflns_number_gt                235
_reflns_number_total             236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ku3266sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022291.cif.'
_cod_original_cell_volume        322.903(13)
_cod_database_code               2022291
_cod_database_fobs_code          2022291
_shelx_estimated_absorpt_t_min   0.294
_shelx_estimated_absorpt_t_max   0.583
_shelx_hkl_checksum              30925
_shelx_res_checksum              90975