Li6SiO4Cl2: A Hexagonal Argyrodite Based on Antiperovskite Layer Stacking
Morscher, Alexandra; Dyer, Matthew S.; Duff, Benjamin B.; Han, Guopeng; Gamon, Jacinthe; Daniels, Luke M.; Dang, Yun; Surta, T. Wesley; Robertson, Craig M.; Blanc, Frédéric; Claridge, John B.; Rosseinsky, Matthew J.; Chemistry of Materials 33 (2021) 2206–2217; doi:10.1021/acs.chemmater.1c00157

data_4003883
_publ_section_title
;
 Li6SiO4Cl2: A Hexagonal Argyrodite Based on Antiperovskite Layer Stacking
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2206
_journal_page_last               2217
_journal_paper_doi               10.1021/acs.chemmater.1c00157
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety         'Cl2 Li6 O4 Si'
_chemical_formula_sum            'Cl2 Li6 O4 Si'
_chemical_formula_weight         204.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5204(8)
_cell_length_b                   6.0756(4)
_cell_length_c                   9.9530(7)
_cell_measurement_reflns_used    3392
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.3210
_cell_measurement_theta_min      3.8440
_cell_volume                     636.17(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -110.00  15.00   1.00    2.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    2.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    2.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    2.00    --  -20.00 -30.00  90.00  125
  5  \w    -90.00  90.00   1.00    2.00    --    0.00   0.00   0.00  180
  6  \w    -90.00  90.00   1.00    2.00    --    0.00   0.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0337886000
_diffrn_orient_matrix_UB_12      0.0320991000
_diffrn_orient_matrix_UB_13      0.0584472000
_diffrn_orient_matrix_UB_21      -0.0101343000
_diffrn_orient_matrix_UB_22      0.1057615000
_diffrn_orient_matrix_UB_23      -0.0282204000
_diffrn_orient_matrix_UB_31      -0.0574565000
_diffrn_orient_matrix_UB_32      -0.0376022000
_diffrn_orient_matrix_UB_33      -0.0294319000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12264
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.391
_diffrn_reflns_theta_min         3.873
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 294 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1232
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0475P)^2^+2.9842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                894
_reflns_number_total             1232
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 92.6144\% 
 around [-0.59 0.37 -0.72] (reciprocal) or [-0.39 0.75 -0.53] (direct)
;
_cod_data_source_file            cm1c00157_si_002.cif
_cod_data_source_block           alex_li6sio4cl2_11_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 4003883.cif.'
_cod_database_code               4003883
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Li6SiO4Cl2
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Li2) \\sim Ueq, Uanis(Li1) \\sim Ueq, Uanis(Li5) \\sim Ueq, Uanis(Li4)
\\sim Ueq, Uanis(Li3) \\sim Ueq, Uanis(Li6) \\sim Ueq, Uanis(O4) \\sim Ueq,
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.002 and
sigma for terminal atoms of 3
;
_shelx_res_checksum              75597
_shelx_hkl_checksum              51905
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.862
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2