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_7240665
_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(K8 O84 S12 U8)'
_chemical_formula_sum            'K2 O21 S3 U2'
_chemical_formula_weight         986.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.465(7)
_cell_length_b                   12.605(7)
_cell_length_c                   12.944(8)
_cell_measurement_reflns_used    2826
_cell_measurement_temperature    296(3)
_cell_measurement_theta_max      31.40
_cell_measurement_theta_min      3.15
_cell_volume                     1870.6(19)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0532
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14744
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.255
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.171
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1627 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.8172.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.503
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0141P)^2^+10.1750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1713
_reflns_number_total             2237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00673d2.cif
_cod_data_source_block           Compound_6
_cod_original_cell_volume        1870.7(19)
_cod_database_code               7240665
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.264
_shelx_estimated_absorpt_t_min   0.115
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O8B) = Uanis(O8A)
Uanis(O7S) = Uanis(O7W)
2. Others
 Fixed Sof: S2(0.5) O7S(0.5) O7W(0.5) O8A(0.5) O8B(0.5)
;
_shelx_res_checksum              32934
_shelx_hkl_checksum              2256
_olex2_submission_special_instructions 'No special instructions were received'