Thermal behavior of uranyl selenite minerals derriksite and demesmaekerite
Vladislav V. Gurzhiy; Alina R. Izatulina; Maria G. Krzhizhanovskaya; Mikhail N. Murashko; Dar-ya V. Spiridonova; Vladimir V. Shilovskikh; Sergey V. Krivovichev; Journal of GeoSciences 65 (2020) 249–259; doi:10.3190/jgeosci.315

data_1566217
_publ_section_title
;
 Thermal behavior of uranyl selenite minerals derriksite and
 demesmaekerite
;
_journal_name_full               'Journal of GeoSciences'
_journal_page_first              249
_journal_page_last               259
_journal_paper_doi               10.3190/jgeosci.315
_journal_volume                  65
_journal_year                    2020
_chemical_formula_moiety         'Cu5 H10 O30 Pb2 Se6 U2'
_chemical_formula_sum            'Cu5 H10 O30 Pb2 Se6 U2'
_chemical_formula_weight         2171.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                88.622(3)
_cell_angle_beta                 79.572(4)
_cell_angle_gamma                89.699(4)
_cell_formula_units_Z            1
_cell_length_a                   5.6320(4)
_cell_length_b                   10.0417(3)
_cell_length_c                   11.9844(4)
_cell_measurement_reflns_used    2912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7290
_cell_measurement_theta_min      3.6750
_cell_volume                     666.39(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -26.00   1.00   1.00   22.50    --  -15.14 -77.00-150.00   27
  2  \w    -40.00  17.00   1.00   22.50    --  -15.14 -77.00 -30.00   57
  3  \w     39.00 102.00   1.00   22.50    --   16.86 178.00  60.00   63
  4  \w     -2.00  93.00   1.00   22.50    --   16.86  38.00-120.00   95
  5  \w    -57.00  41.00   1.00   22.50    --   16.86 -57.00  90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0856349000
_diffrn_orient_matrix_UB_12      -0.0271059000
_diffrn_orient_matrix_UB_13      -0.0298610000
_diffrn_orient_matrix_UB_21      0.0825721000
_diffrn_orient_matrix_UB_22      0.0088741000
_diffrn_orient_matrix_UB_23      -0.0518098000
_diffrn_orient_matrix_UB_31      0.0473988000
_diffrn_orient_matrix_UB_32      -0.0646415000
_diffrn_orient_matrix_UB_33      0.0068844000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5475
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    36.907
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    5.412
_exptl_crystal_description       prism
_exptl_crystal_F_000             947
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.055
_refine_diff_density_max         3.021
_refine_diff_density_min         -2.491
_refine_diff_density_rms         0.416
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         3053
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2611
_reflns_number_total             3053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Demesmaekerite_SN_-173C_last.cif
_cod_data_source_block           demesmaekerite_sn_-173C
_cod_database_code               1566217
_chemical_oxdiff_formula         'Pb2 Cu5 U2 Se6 O30'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O14-H14
 0.95 with sigma of 0.02
 O13-H13
 0.95 with sigma of 0.02
 O12-H12
 0.95 with sigma of 0.02
 H15A-O5_$3
 2 with sigma of 0.02
 H13-O9_$2
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) = Uanis(O3) = Uanis(O10)
Uanis(O5) = Uanis(O4)
Uanis(O12) = Uanis(O14) = Uanis(O13)
Uanis(O7) = Uanis(O8)
4.a Rotating group:
 O15(H15A,H15B)
;
_shelx_res_checksum              18136
_shelx_hkl_checksum              40807
_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 1.721
_oxdiff_exptl_absorpt_empirical_full_min 0.552