One of Nature’s Puzzles Is Assembled: Analog of the Earth’s Most Complex Mineral, Ewingite, Synthesized in a Laboratory
Tyumentseva, Olga S.; Kornyakov, Ilya V.; Kasatkin, Anatoly V.; Plášil, Jakub; Krzhizhanovskaya, Maria G.; Krivovichev, Sergey V.; Burns, Peter C.; Gurzhiy, Vladislav V.; Materials 15 (2022) 6643–; doi:10.3390/ma15196643

data_1567747
_publ_section_title
;
 One of Nature&#x2019;s Puzzles Is Assembled: Analog of the Earth&#x2019;s
 Most Complex Mineral, Ewingite, Synthesized in a Laboratory
;
_journal_issue                   19
_journal_name_full               Materials
_journal_page_first              6643
_journal_paper_doi               10.3390/ma15196643
_journal_volume                  15
_journal_year                    2022
_chemical_formula_moiety         'C36 O172 U24, 21(Ca), 4(C O3), 94(O)'
_chemical_formula_sum            'C40 Ca21 O278 U24'
_chemical_formula_weight         11482.80
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_audit_creation_date             2022-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.6098(2)
_cell_length_b                   24.6098(2)
_cell_length_c                   24.6246(4)
_cell_measurement_reflns_used    56126
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.3370
_cell_measurement_theta_min      1.6290
_cell_volume                     14913.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    143.91 340.41   0.50  360.26 -98.65 -34.00 -40.00    --   393
  2  \f     75.39 190.89   0.50  360.01 -72.49 -34.00 137.99    --   231
  3  \w    -91.73 -20.73   0.50  360.03    --  -34.00 147.98 -65.99  142
  4  \w    -76.26 -15.26   0.50  360.03    --  -34.00 102.00 134.00  122
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0098894000
_diffrn_orient_matrix_UB_12      0.0253358000
_diffrn_orient_matrix_UB_13      0.0095265000
_diffrn_orient_matrix_UB_21      0.0107039000
_diffrn_orient_matrix_UB_22      -0.0129520000
_diffrn_orient_matrix_UB_23      0.0234115000
_diffrn_orient_matrix_UB_31      0.0248540000
_diffrn_orient_matrix_UB_32      -0.0044833000
_diffrn_orient_matrix_UB_33      -0.0138618000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            111547
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         1.655
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    2.557
_exptl_crystal_description       prism
_exptl_crystal_F_000             10184
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.021
_refine_diff_density_max         2.872
_refine_diff_density_min         -1.317
_refine_diff_density_rms         0.266
_refine_ls_abs_structure_details
;
 Flack x determined using 5860 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         17137
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0541P)^2^+319.7196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                14963
_reflns_number_total             17137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            materials-1907186-supplementary.cif
_cod_data_source_block           Synthetic_ewingite_mo_orc2
_cod_database_code               1567747
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.541
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.514(14)
 0.486(14)
2. Restrained distances
 C2-O22
 1.23 with sigma of 0.02
 O44-C10
 1.3 with sigma of 0.05
 C2-O21
 1.23 with sigma of 0.02
 C2-O20
 1.23 with sigma of 0.02
 U5-O9
 1.7 with sigma of 0.02
3. Restrained planarity
 O20, O21, O22, C2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O47) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O71W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(O49W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.016
Uanis(O65W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O72W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.014
Uanis(Ca2B) \\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.01
Uanis(O75W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O56W) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.006
Uanis(O9) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O68W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O73W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.014
Uanis(O44) = Uanis(C10) = Uanis(O46) = Uanis(O45)
Uanis(Ca2A) = Uanis(Ca2B)
Uanis(C2) = Uanis(O22) = Uanis(O21) = Uanis(O20)
Uanis(O50W) = Uanis(Ca4)
Uanis(O69W) = Uanis(O70W)
Uanis(O60W) = Uanis(O74W)
5. Others
 Fixed Sof: Ca2A(0.0975) Ca2B(0.1525) Ca4(0.5) O47(0.5) O48W(0.75) O50W(0.5)
 O54W(0.85) O56W(0.5) O60W(0.5) O63W(0.75) O66W(0.65) O69W(0.5) O70W(0.5)
 O72W(0.25) O73W(0.25) O74W(0.5) O76W(0.75) O77W(0.75) O78W(0.75)
;
_shelx_res_checksum              28828
_shelx_hkl_checksum              70276
_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 1.515
_oxdiff_exptl_absorpt_empirical_full_min 0.559