Crystal chemistry of the M2+[(UO2)(T6+O4)2(H2O)](H2O)4 (M2+ = Mg, Mn, Fe, Co, Ni and Zn; T6+ = S, Se) compounds: the interplay between chemical composition, pH and structural architecture
Kornyakov, Ilya V.; Tyumentseva, Olga S.; Krivovichev, Sergey V.; Tananaev, Ivan G.; Gurzhiy, Vladislav V.; CrystEngComm 23 (2021) 1140–1148; doi:10.1039/D0CE01587C

data_7241879
_publ_section_title
;
 Crystal chemistry of the M2+[(UO2)(T6+O4)2(H2O)](H2O)4 (M2+ = Mg, Mn, Fe,
 Co, Ni and Zn; T6+ = S, Se) compounds: the interplay between chemical
 composition, pH and structural architecture
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1140
_journal_page_last               1148
_journal_paper_doi               10.1039/D0CE01587C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'H10 Ni O15 S1.85 Se0.15 U'
_chemical_formula_sum            'H10 Ni O15 S1.85 Se0.15 U'
_chemical_formula_weight         617.86
_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
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7808(3)
_cell_length_b                   8.2806(2)
_cell_length_c                   11.3074(3)
_cell_measurement_reflns_used    8702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2650
_cell_measurement_theta_min      2.3910
_cell_volume                     1196.69(5)
_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 (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      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      0.10 332.60   0.50   70.01 -98.65 -34.00 -40.00    --   665
  2  \w   -100.38 -20.38   0.50   70.00    --  -34.00 147.98 -65.98  160
  3  \w    -77.02  -1.52   0.50   70.00    --  -34.00 102.00 134.00  151
  4  \w    241.02 268.02   0.50   70.00    --  -34.00 -89.99 -60.00   54
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0427600000
_diffrn_orient_matrix_UB_12      -0.0541046000
_diffrn_orient_matrix_UB_13      -0.0051994000
_diffrn_orient_matrix_UB_21      -0.0313512000
_diffrn_orient_matrix_UB_22      -0.0631903000
_diffrn_orient_matrix_UB_23      0.0231901000
_diffrn_orient_matrix_UB_31      -0.0164210000
_diffrn_orient_matrix_UB_32      -0.0205022000
_diffrn_orient_matrix_UB_33      -0.0580261000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10729
_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         27.498
_diffrn_reflns_theta_min         2.405
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37498
_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            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             1139
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.430
_refine_diff_density_min         -1.619
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.068(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2756
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+2.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2575
_reflns_number_total             2756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241879
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni2 U2 S3 O12'
_shelx_estimated_absorpt_t_max   0.568
_shelx_estimated_absorpt_t_min   0.127
_reflns_odcompleteness_completeness 96.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.19
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.932(12)
 0.068(12)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
3. Shared sites
{S1, Se1}
{S2, Se2}
4. Restrained distances
 O12-H12_$1
 0.98 with sigma of 0.02
 H12-H12_$1
 1.54 with sigma of 0.02
 H12_$1-O4_$10
 2 with sigma of 0.02
 O10_$1-H14_$10
 2.1 with sigma of 0.02
 O14-H14_$1
 0.98 with sigma of 0.02
 H14-H14_$1
 1.54 with sigma of 0.02
 H14_$11-O10_$10
 1.9 with sigma of 0.02
 O10_$10-H10B_$10
 0.98 with sigma of 0.02
 H10B_$10-O7_$2
 1.8 with sigma of 0.02
 O10_$10-H10A_$10
 0.98 with sigma of 0.02
 H10B_$10-H10A_$10
 1.54 with sigma of 0.02
 H10A_$10-O4_$3
 1.8 with sigma of 0.02
 O16_$11-H16_$4
 0.98 with sigma of 0.02
 H16_$11-H16_$4
 1.54 with sigma of 0.02
 H16_$11-O3_$3
 1.9 with sigma of 0.02
 O15_$2-H15_$5
 0.98 with sigma of 0.02
 H15_$2-H15_$5
 1.54 with sigma of 0.02
 H15_$5-O5_$6
 1.9 with sigma of 0.02
 H12_$2-O4_$3
 1.8 with sigma of 0.02
 O13-H13_$1
 0.98 with sigma of 0.02
 O19-H19
 0.98 with sigma of 0.02
 H19_$9-H19
 1.54 with sigma of 0.02
 H19-O5_$8
 1.75 with sigma of 0.02
 O17-H17
 0.98 with sigma of 0.02
 H17-H17_$9
 1.54 with sigma of 0.02
 H17-O11_$7
 2.3 with sigma of 0.02
 H13-H13_$1
 1.54 with sigma of 0.02
 O18-H18
 0.98 with sigma of 0.02
 H18-H18_$9
 1.54 with sigma of 0.02
 O3_$9-H18_$9
 2.4 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(Se1)
Uanis(S2) = Uanis(Se2)
6. Others
 Sof(Se1)=1-FVAR(1)
 Sof(S1)=FVAR(1)
 Sof(Se2)=1-FVAR(2)
 Sof(S2)=FVAR(2)
;
_shelx_res_checksum              65438
_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 2.409
_oxdiff_exptl_absorpt_empirical_full_min 0.579