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_1566226
_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         'Cu4 H6 O14 Se2 U'
_chemical_formula_sum            'Cu4 H6 O14 Se2 U'
_chemical_formula_weight         880.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.9679(3)
_cell_length_b                   5.5501(3)
_cell_length_c                   19.0613(9)
_cell_measurement_reflns_used    2726
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8570
_cell_measurement_theta_min      4.2470
_cell_volume                     631.36(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 0.998
_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  \w    -47.00   3.00   1.00   22.50    --  -14.99  77.00-180.00   50
  2  \w    -27.00  19.00   1.00   22.50    --  -14.99 -77.00-150.00   46
  3  \w     42.00  83.00   1.00   22.50    --   16.86 178.00 -30.00   41
  4  \w     31.00  59.00   1.00   22.50    --   16.86 -99.00 120.00   28
  5  \w     -4.00  93.00   1.00   22.50    --   16.86  38.00 120.00   97
  6  \w     -8.00  93.00   1.00   22.50    --   16.86  38.00  30.00  101
;
_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      0.1107012000
_diffrn_orient_matrix_UB_12      0.0330414000
_diffrn_orient_matrix_UB_13      0.0095566000
_diffrn_orient_matrix_UB_21      -0.0239061000
_diffrn_orient_matrix_UB_22      0.1216467000
_diffrn_orient_matrix_UB_23      -0.0085407000
_diffrn_orient_matrix_UB_31      -0.0361605000
_diffrn_orient_matrix_UB_32      0.0206627000
_diffrn_orient_matrix_UB_33      0.0349146000
_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  0.0451
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5132
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         3.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.247
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.990
_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            green
_exptl_crystal_density_diffrn    4.630
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.041
_refine_diff_density_max         1.491
_refine_diff_density_min         -1.845
_refine_diff_density_rms         0.255
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1538
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0681P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.882
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                1502
_reflns_number_total             1538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Derriksite_SN_-173C_last.cif
_cod_data_source_block           derriksite_sn_-173C
_cod_original_cell_volume        631.35(5)
_cod_database_code               1566226
_chemical_oxdiff_formula         'Cu4 U Se2 O14'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O9-H9
 1 with sigma of 0.02
 H9-O5_$5
 2.15 with sigma of 0.02
 O7-H7
 0.9 with sigma of 0.02
 O10-H10
 0.9 with sigma of 0.02
 O8-H8
 0.95 with sigma of 0.02
 H8-O1_$3
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O10) = Uanis(O4)
Uanis(O8) = Uanis(O4)
4. Others
 Fixed Sof: H9(0.5)
;
_shelx_res_checksum              34458
_shelx_hkl_checksum              12553
_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 2.336
_oxdiff_exptl_absorpt_empirical_full_min 0.645