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_7240663
_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         'O27 S5 U3, 3.5(K), 2(O)'
_chemical_formula_sum            'K3.5 O29 S5 U3'
_chemical_formula_weight         1475.24
_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                 98.038(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8901(3)
_cell_length_b                   16.1105(5)
_cell_length_c                   17.2862(5)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    296(3)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.25
_cell_volume                     2727.23(14)
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0616
_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       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26393
_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         27.492
_diffrn_reflns_theta_min         1.736
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.800
_exptl_absorpt_correction_T_max  0.3382
_exptl_absorpt_correction_T_min  0.1961
_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    3.593
_exptl_crystal_description       needle
_exptl_crystal_F_000             2618
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.729
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       0.00035(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   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6259
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0290P)^2^+13.5932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4615
_reflns_number_total             6259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00673d2.cif
_cod_data_source_block           Compound_3
_cod_original_formula_sum        'K3.50 O29 S5 U3'
_cod_database_code               7240663
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O29A) \\sim Ueq, Uanis(O29B) \\sim Ueq, Uanis(O29C) \\sim Ueq,
Uanis(O29D) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(K4B) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.012
Uanis(O28A) = Uanis(O28B)
Uanis(O29A) = Uanis(O29C) = Uanis(O24)
Uanis(O29B) = Uanis(O29D) = Uanis(O24)
2. Others
 Sof(O28A)=1-FVAR(1)
 Sof(O28B)=FVAR(1)
 Fixed Sof: K3(0.5) K4A(0.2) K4B(0.2) K4C(0.6) O29A(0.25) O29B(0.25)
 O29C(0.25) O29D(0.25)
;
_shelx_res_checksum              60922
_shelx_hkl_checksum              28842
_olex2_submission_special_instructions 'No special instructions were received'