Tracing electron density changes in langbeinite under pressure
Gajda, Roman; Zhang, Dongzhou; Parafiniuk, Jan; Dera, Przemysław; Woźniak, Krzysztof; IUCrJ 9 (2022) 146–162; doi:10.1107/S2052252521012628

data_1565826
_publ_section_title
;
 Tracing electron density changes in langbeinite under pressure
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              146
_journal_page_last               162
_journal_paper_doi               10.1107/S2052252521012628
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'K2 Mg2 O12 S3'
_chemical_formula_sum            'K2 Mg2 O12 S3'
_chemical_formula_weight         415.00
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.91895(2)
_cell_length_b                   9.91895(2)
_cell_length_c                   9.91895(2)
_cell_measurement_reflns_used    80569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      44.3910
_cell_measurement_theta_min      2.7870
_cell_volume                     975.882(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0128
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -20.00  30.00   1.00   15.00    --  -24.72 -99.00 -30.00   50
  2  \w   -101.00  13.00   1.00   15.00    --  -24.72 -57.00  30.00  114
  3  \w   -101.00  13.00   1.00   15.00    --  -24.72 -57.00 120.00  114
  4  \w    -51.00  63.00   1.00   15.00    --   24.72 -57.00 150.00  114
  5  \w    -51.00  63.00   1.00   15.00    --   24.72 -57.00   0.00  114
  6  \w    -13.00 101.00   1.00   15.00    --   24.72  57.00 -60.00  114
  7  \w    -20.00  80.00   1.00   15.00    --   24.72 -99.00 -90.00  100
  8  \w    -21.00 107.00   1.00   60.00    --   64.14 -77.00  30.00  128
  9  \w     21.00 149.00   1.00   60.00    --   64.14  77.00  60.00  128
 10  \w     21.00 149.00   1.00   60.00    --   64.14  77.00 120.00  128
 11  \w     21.00 149.00   1.00   60.00    --   64.14  77.00  90.00  128
 12  \w     21.00 149.00   1.00   60.00    --   64.14  77.00 -30.00  128
 13  \w    -12.00 101.00   1.00   60.00    --   64.14 -61.00  90.00  113
 14  \w     21.00 149.00   1.00   60.00    --   64.14  77.00 -60.00  128
 15  \w     21.00 149.00   1.00   60.00    --   64.14  77.00 -90.00  128
 16  \w     49.00 155.00   1.00   60.00    --   64.14 160.00 120.00  106
 17  \w     21.00 149.00   1.00   60.00    --   64.14  77.00  30.00  128
 18  \w     21.00 149.00   1.00   60.00    --   64.14  77.00   0.00  128
 19  \w     21.00 149.00   1.00   60.00    --   64.14  77.00-120.00  128
 20  \w     21.00 149.00   1.00   60.00    --   64.14  77.00 150.00  128
 21  \w     21.00 149.00   1.00   60.00    --   64.14  77.00-180.00  128
 22  \w     49.00 155.00   1.00   60.00    --   64.14 160.00 -30.00  106
 23  \w     21.00 149.00   1.00   60.00    --   64.14  77.00-180.00  128
 24  \w    -12.00 101.00   1.00   60.00    --   64.14 -61.00-150.00  113
 25  \w     21.00 149.00   1.00   60.00    --   64.14  77.00-153.77  128
 26  \w    -20.00  30.00   1.00   15.00    --  -24.72 -99.00   0.00   50
 27  \w     21.00  66.00   1.00   15.00    --  -24.72-160.00  60.00   45
 28  \w    -20.00  30.00   1.00   15.00    --  -24.72 -99.00-180.00   50
 29  \w    -20.00  30.00   1.00   15.00    --  -24.72 -99.00 150.00   50
 30  \w    -66.00 -21.00   1.00   15.00    --   24.72 160.00-150.00   45
 31  \w    -60.00  68.00   1.00   15.00    --   24.72 -77.00  30.00  128
 32  \w    -30.00  17.00   1.00   15.00    --   24.72 101.00 134.00   47
 33  \w    -66.00 -21.00   1.00   15.00    --   24.72 160.00  30.00   45
 34  \w     49.00 155.00   1.00   60.00    --   64.14 160.00  90.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0070729000
_diffrn_orient_matrix_UB_12      0.0299470000
_diffrn_orient_matrix_UB_13      0.0472484000
_diffrn_orient_matrix_UB_21      0.0532028000
_diffrn_orient_matrix_UB_22      0.0111576000
_diffrn_orient_matrix_UB_23      -0.0150405000
_diffrn_orient_matrix_UB_31      -0.0173462000
_diffrn_orient_matrix_UB_32      0.0464711000
_diffrn_orient_matrix_UB_33      -0.0268551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0070
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            168589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         44.610
_diffrn_reflns_theta_min         2.292
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'pale grey'
_exptl_crystal_density_diffrn    2.825
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.425
_exptl_crystal_size_min          0.279
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 2346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         5360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0221
_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^)+(0.0284P)^2^+0.1847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5292
_reflns_number_total             5360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ti5023.cif
_cod_data_source_block           Langbeinite_silver_source_structural
_cod_depositor_comments
'Adding full bibliography for 1565826--1565831.cif.'
_cod_original_cell_volume        975.880(5)
_cod_database_code               1565826
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K2 Mg2 S3 O12'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.37
_olex2_refinement_description
;
;
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.937