Dimensional Evolution in Hydrated K±bearing Uranyl Sulfates: From 2D-sheet to 3D-framework
Kornyakov, Ilya V.; Tyumentseva, Olga S.; Gurzhiy, Vladislav V.; Krivovichev, Sergey V.; CrystEngComm  (2020) –; doi:10.1039/D0CE00673D

data_7240664
_publ_section_title
;
 Dimensional Evolution in Hydrated K+-bearing Uranyl Sulfates: From
 2D-sheet to 3D-framework
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00673D
_journal_year                    2020
_chemical_formula_moiety         '0.25(O72 S12 U8), 2(K), 3(O)'
_chemical_formula_sum            'K2 O21 S3 U2'
_chemical_formula_weight         986.44
_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'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-13 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3051(2)
_cell_length_b                   12.56130(10)
_cell_length_c                   17.3240(2)
_cell_measurement_reflns_used    38615
_cell_measurement_temperature    293(3)
_cell_measurement_theta_max      38.7500
_cell_measurement_theta_min      1.7780
_cell_volume                     3741.01(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_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      293(3)
_diffrn_detector                 'CCD plate'
_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  \f   -357.95  -5.95   0.50   60.01 -28.41 -40.00  37.99    --   704
  2  \w    -65.16   3.84   0.50   60.00    --  -38.00  96.00 -80.00  138
  3  \w    -96.81 -21.81   0.50   60.00    --  -34.00 147.98 -65.99  150
  4  \w    283.03 320.53   0.50   60.00    --  -34.00 102.00 134.00   75
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291474000
_diffrn_orient_matrix_UB_12      0.0156649000
_diffrn_orient_matrix_UB_13      0.0233380000
_diffrn_orient_matrix_UB_21      0.0014101000
_diffrn_orient_matrix_UB_22      -0.0511111000
_diffrn_orient_matrix_UB_23      0.0174825000
_diffrn_orient_matrix_UB_31      0.0291760000
_diffrn_orient_matrix_UB_32      0.0181284000
_diffrn_orient_matrix_UB_33      0.0291366000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    18.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.503
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0272P)^2^+8.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7674
_reflns_number_total             8580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00673d2.cif
_cod_data_source_block           Compound_5
_cod_database_code               7240664
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'U24 S60 K6 O68'
_shelx_estimated_absorpt_t_max   0.464
_shelx_estimated_absorpt_t_min   0.115
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5584(6)
 0.4416(6)
;
_shelx_res_checksum              57683
_shelx_hkl_checksum              52035
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.885
_oxdiff_exptl_absorpt_empirical_full_min 0.430