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_7241873
_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 S0.43 Se1.57 U'
_chemical_formula_sum            'H10 Ni O15 S0.43 Se1.57 U'
_chemical_formula_weight         684.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-17 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.103(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3752(2)
_cell_length_b                   11.5330(3)
_cell_length_c                   13.0328(3)
_cell_measurement_reflns_used    10517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.1650
_cell_measurement_theta_min      2.3490
_cell_volume                     1257.01(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   -360.00   9.50   0.50  125.04 -98.65 -34.00 -40.00    --   739
  2  \w    -90.34 -28.84   0.50  125.00    --  -34.00 133.99 116.00  123
  3  \f    117.27 255.77   0.50  125.08-112.09 -34.00 -51.99    --   277
;
_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      -0.0747669000
_diffrn_orient_matrix_UB_12      0.0283672000
_diffrn_orient_matrix_UB_13      -0.0077166000
_diffrn_orient_matrix_UB_21      -0.0003665000
_diffrn_orient_matrix_UB_22      -0.0127846000
_diffrn_orient_matrix_UB_23      -0.0532202000
_diffrn_orient_matrix_UB_31      -0.0400817000
_diffrn_orient_matrix_UB_32      -0.0530818000
_diffrn_orient_matrix_UB_33      0.0086480000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12242
_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         27.500
_diffrn_reflns_theta_min         2.360
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77521
_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    3.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             1241
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0192P)^2^+3.0687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2380
_reflns_number_total             2882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_9
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241873
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Ni4  O60  S1  Se7  U4  H1  '
_shelx_estimated_absorpt_t_max   0.252
_shelx_estimated_absorpt_t_min   0.064
_reflns_odcompleteness_completeness 95.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.16
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Shared sites
{S2, Se2}
{S1, Se1}
3. Restrained distances
 H10A-H10B
 1.5 with sigma of 0.02
 O10-H10A
 0.98 with sigma of 0.02
 O10-H10B
 0.98 with sigma of 0.02
 O12-H12A
 0.98 with sigma of 0.02
 O12-H12B
 0.98 with sigma of 0.02
 H12B-H12A
 1.5 with sigma of 0.02
 H14B-O14
 0.98 with sigma of 0.02
 O14-H14A
 0.98 with sigma of 0.02
 H14A-H14B
 1.5 with sigma of 0.02
 O13_$1-H13A_$1
 0.98 with sigma of 0.02
 O13_$1-H13B_$1
 0.98 with sigma of 0.02
 H13A_$1-H13B_$1
 1.5 with sigma of 0.02
 H13A_$1-O5_$3
 1.9 with sigma of 0.02
 H13B_$1-O9_$2
 2.3 with sigma of 0.02
 O15-H15B
 0.98 with sigma of 0.02
 O15-H15A
 0.98 with sigma of 0.02
 H15B-H15A
 1.5 with sigma of 0.02
 H15B-O2_$4
 2.1 with sigma of 0.02
 H15A-O11
 1.86 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(S2) = Uanis(Se2)
Uanis(S1) = Uanis(Se1)
5. Others
 Sof(Se2)=1-FVAR(1)
 Sof(S2)=FVAR(1)
 Sof(Se1)=1-FVAR(2)
 Sof(S1)=FVAR(2)
;
_shelx_res_checksum              91139
_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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.769