Evolution of Chernobyl Corium in Water: Formation of Secondary Uranyl Phases
Gurzhiy, Vladislav V.; Burakov, Boris E.; Zubekhina, Bella Yu.; Kasatkin, Anatoly V.; Materials 16 (2023) 4533–; doi:10.3390/ma16134533

data_1569467
_publ_section_title
;
 Evolution of Chernobyl Corium in Water: Formation of Secondary Uranyl
 Phases
;
_journal_issue                   13
_journal_name_full               Materials
_journal_page_first              4533
_journal_paper_doi               10.3390/ma16134533
_journal_volume                  16
_journal_year                    2023
_chemical_formula_moiety         'Ca H6 O22 U6, 8(H2 O)'
_chemical_formula_sum            'Ca H22 O30 U6'
_chemical_formula_weight         1970.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2022-07-31
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9073(6)
_cell_length_b                   15.0023(6)
_cell_length_c                   12.4269(6)
_cell_measurement_reflns_used    8928
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1700
_cell_measurement_theta_min      3.3360
_cell_volume                     2592.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_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    -91.00 -26.00   0.50   12.00    --  -20.20 129.00   4.00  130
  2  \w   -106.00 -16.00   0.50   12.00    --  -20.20 -12.00 136.00  180
  3  \w    -23.00  14.00   0.50   12.00    --  -20.20  19.00 -60.00   74
  4  \w    -19.00  43.00   0.50   12.00    --  -20.20  19.00 -30.00  124
  5  \w    -17.00  34.00   0.50   12.00    --  -20.20 -99.00-120.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0220462000
_diffrn_orient_matrix_UB_12      0.0056372000
_diffrn_orient_matrix_UB_13      0.0509944000
_diffrn_orient_matrix_UB_21      0.0452730000
_diffrn_orient_matrix_UB_22      0.0052628000
_diffrn_orient_matrix_UB_23      -0.0254945000
_diffrn_orient_matrix_UB_31      -0.0078215000
_diffrn_orient_matrix_UB_32      0.0466565000
_diffrn_orient_matrix_UB_33      -0.0033959000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14077
_diffrn_reflns_point_group_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    37.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    5.048
_exptl_crystal_description       prism
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.442
_refine_diff_density_min         -2.203
_refine_diff_density_rms         0.319
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+18.8016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0801
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.774
_reflns_Friedel_fraction_max     0.704
_reflns_number_gt                4284
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Bqr_2_last.cif
_cod_data_source_block           Bqr_2_chern_yelllow_prism_new
_cod_database_code               1569467
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(3)
 0.46(3)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 OH17-HH17 = OH18-HH18 = OH19-HH19
 0.9 with sigma of 0.02
 OH20-HH20 = OH21-HH21 = OH22-HH22
 0.9 with sigma of 0.02
 OW29-HW2N
 0.9 with sigma of 0.02
 O11_$4-HW2J = O8_$1-HW2A = HW2K-O7_$3
 2 with sigma of 0.02
 OW27_$1-HH20 = O3-HW2B = HW2D-O10_$3
 2.1 with sigma of 0.02
 HW2H-O4_$2 = HH19-OW26 = HW2G-O9
 2.1 with sigma of 0.02
 HW2I-O2 = HW2N-O11_$4 = HW2L-OW29
 2.15 with sigma of 0.02
 HW3B-O4 = HW3A-O10
 2.17 with sigma of 0.02
 U6-HH20 = U2-HH21 = U3-HH18
 2.65 with sigma of 0.02
 U2-HH17 = U4-HH22
 2.65 with sigma of 0.02
 U2-HH20
 2.9 with sigma of 0.02
 U1-HH17
 3 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(OW28) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O16) = Uanis(OH22) = Uanis(OH18)
Uanis(OH19) = Uanis(O13) = Uanis(OH20) = Uanis(O15) = Uanis(OH21)
Uanis(O9) = Uanis(O10)
Uanis(O14) = Uanis(OH18)
Uanis(O4) = Uanis(O3)
Uanis(O11) = Uanis(O12)
Uanis(OW26) = Uanis(OW30)
5.a Everything fixed:
 HW2M, HW2N
5.b Rotating group:
 OW23(HW2A,HW2B), OW24(HW2C,HW2D), OW25(HW2E,HW2F), OW26(HW2G,HW2H), OW27(HW2I,
 HW2J), OW28(HW2K,HW2L), OW30(HW3A,HW3B)
;
_shelx_res_checksum              9806
_shelx_hkl_checksum              38572
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.836