#------------------------------------------------------------------------------
#$Date: 2021-02-05 16:53:33 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261800 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022291.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_2022291
loop_
_publ_author_name
'Stoyko, Stanislav S.'
'Craig, Andrew J.'
'Kotchey, Joshua W.'
'Aitken, Jennifer A.'
_publ_section_title
;
 Synthesis, crystal structure, and electronic structure of Li₂PbSiS₄:
 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 (Hübschle et al.,  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       'φ and ω 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/[σ²(Fo²)] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.294
_shelx_estimated_absorpt_t_max   0.583
loop_
_space_group_symop_operation_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+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'
'-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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li Li 0.000000 0.500000 0.250000 0.024(3) Uani d 1 . .
Pb Pb 0.000000 0.000000 0.500000 0.02611(17) Uani d 1 . .
Si Si 0.000000 0.000000 0.000000 0.0098(6) Uani d 1 . .
S S 0.19091(19) 0.19091(19) 0.1569(2) 0.0140(4) Uani d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Pb Pb -3.3944 10.1111 '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
_geom_angle_publ_flag
S Li S 12 11_455 145.91(8) ?
S Li S 12 2_565 94.93(2) ?
S Li S 11_455 2_565 94.93(2) ?
S Li S 12 . 94.93(2) ?
S Li S 11_455 . 94.93(2) ?
S Li S 2_565 . 145.91(8) ?
S Li Pb 12 9_454 148.05(4) ?
S Li Pb 11_455 9_454 56.80(4) ?
S Li Pb 2_565 9_454 54.44(4) ?
S Li Pb . 9_454 106.30(4) ?
S Li Pb 12 1_565 54.44(4) ?
S Li Pb 11_455 1_565 106.30(4) ?
S Li Pb 2_565 1_565 56.80(4) ?
S Li Pb . 1_565 148.05(4) ?
Pb Li Pb 9_454 1_565 105.2870(10) ?
S Li Pb 12 . 106.30(4) ?
S Li Pb 11_455 . 54.44(4) ?
S Li Pb 2_565 . 148.05(4) ?
S Li Pb . . 56.80(4) ?
Pb Li Pb 9_454 . 105.2870(10) ?
Pb Li Pb 1_565 . 118.209(2) ?
S Li Pb 12 9_554 56.80(4) ?
S Li Pb 11_455 9_554 148.05(4) ?
S Li Pb 2_565 9_554 106.30(4) ?
S Li Pb . 9_554 54.44(4) ?
Pb Li Pb 9_454 9_554 118.2090(10) ?
Pb Li Pb 1_565 9_554 105.2870(10) ?
Pb Li Pb . 9_554 105.2870(10) ?
S Pb S 10 9_445 133.49(6) ?
S Pb S 10 12_545 98.97(2) ?
S Pb S 9_445 12_545 98.97(2) ?
S Pb S 10 11_455 98.97(2) ?
S Pb S 9_445 11_455 98.97(2) ?
S Pb S 12_545 11_455 133.49(6) ?
S Pb S 10 2 146.58(6) ?
S Pb S 9_445 2 79.923(19) ?
S Pb S 12_545 2 70.74(2) ?
S Pb S 11_455 2 70.74(2) ?
S Pb S 10 4_556 70.74(2) ?
S Pb S 9_445 4_556 70.74(2) ?
S Pb S 12_545 4_556 146.58(6) ?
S Pb S 11_455 4_556 79.924(19) ?
S Pb S 2 4_556 134.28(4) ?
S Pb S 10 3_556 70.74(2) ?
S Pb S 9_445 3_556 70.74(2) ?
S Pb S 12_545 3_556 79.924(19) ?
S Pb S 11_455 3_556 146.58(6) ?
S Pb S 2 3_556 134.28(4) ?
S Pb S 4_556 3_556 66.66(6) ?
S Pb S 10 . 79.924(19) ?
S Pb S 9_445 . 146.58(6) ?
S Pb S 12_545 . 70.74(2) ?
S Pb S 11_455 . 70.74(2) ?
S Pb S 2 . 66.66(6) ?
S Pb S 4_556 . 134.28(4) ?
S Pb S 3_556 . 134.28(4) ?
S Si S . 4 109.03(5) ?
S Si S . 3 109.03(5) ?
S Si S 4 3 110.35(9) ?
S Si S . 2 110.35(9) ?
S Si S 4 2 109.03(5) ?
S Si S 3 2 109.03(5) ?
Si S Li . 13_545 110.36(4) ?
Si S Li . . 110.36(4) ?
Li S Li 13_545 . 137.01(7) ?
Si S Pb . 9_554 121.92(7) ?
Li S Pb 13_545 9_554 85.05(4) ?
Li S Pb . 9_554 85.05(4) ?
Si S Pb . . 91.50(6) ?
Li S Pb 13_545 . 82.87(4) ?
Li S Pb . . 82.87(4) ?
Pb S Pb 9_554 . 146.58(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li S 12 2.4554(6) yes
Li S 11_455 2.4554(6) yes
Li S 2_565 2.4554(6) yes
Li S . 2.4554(6) yes
Li Pb 9_454 3.76516(5) no
Li Pb 1_565 3.76516(5) no
Li Pb . 3.76516(5) no
Li Pb 9_554 3.76516(5) no
Pb S 10 3.0743(18) yes
Pb S 9_445 3.0743(18) yes
Pb S 12_545 3.0743(18) yes
Pb S 11_455 3.0743(18) yes
Pb S 2 3.1752(17) yes
Pb S 4_556 3.1752(17) yes
Pb S 3_556 3.1752(17) yes
Pb S . 3.1752(17) yes
Si S . 2.1252(17) yes
Si S 4 2.1253(17) yes
Si S 3 2.1253(17) yes
Si S 2 2.1253(17) yes
