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_7240662
_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         'H2 K O17 S3 U2, H3 O, H2 O'
_chemical_formula_sum            'H7 K O19 S3 U2'
_chemical_formula_weight         922.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-04
_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                 101.280(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1337(15)
_cell_length_b                   10.0463(13)
_cell_length_c                   14.697(2)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    296(3)
_cell_measurement_theta_max      38.09
_cell_measurement_theta_min      2.47
_cell_volume                     1612.1(4)
_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      296(3)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28887
_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         27.499
_diffrn_reflns_theta_min         1.865
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.809
_exptl_absorpt_correction_T_max  0.3641
_exptl_absorpt_correction_T_min  0.2097
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.800
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00048(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3707
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0139
_refine_ls_R_factor_gt           0.0126
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+2.3873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0298
_refine_ls_wR_factor_ref         0.0302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3514
_reflns_number_total             3707
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00673d2.cif
_cod_data_source_block           Compound_8
_cod_original_cell_volume        1612.2(4)
_cod_database_code               7240662
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.189
_shelx_estimated_absorpt_t_min   0.126
_olex2_refinement_description
;
1. Restrained distances
 H18A-O18W
 0.98 with sigma of 0.02
 H18B-O18W
 0.98 with sigma of 0.02
 O17W-H17A
 0.98 with sigma of 0.02
 H17B-O17W
 0.98 with sigma of 0.02
 H18C_$1-O18W_$1
 0.98 with sigma of 0.02
 H17A-H17B
 1.45 with sigma of 0.02
 H19A-O19W
 0.98 with sigma of 0.02
 H19B-O19W
 0.98 with sigma of 0.02
 H19A-H19B
 1.45 with sigma of 0.02
2. Restrained angles
 H18C-O18W-H18B
 fixed at 120 with sigma of 0.02
;
_shelx_res_checksum              75159
_shelx_hkl_checksum              6793
_olex2_submission_special_instructions 'No special instructions were received'