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_7241877
_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 Mn O15 S2 U'
_chemical_formula_sum            'H10 Mn O15 S2 U'
_chemical_formula_weight         607.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 90.773(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.51140(10)
_cell_length_b                   11.3829(2)
_cell_length_c                   8.3439(2)
_cell_measurement_reflns_used    10264
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.5390
_cell_measurement_theta_min      1.7820
_cell_volume                     618.38(2)
_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 (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      296(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  \w      8.21 192.21   0.50   60.00    --   34.00  73.86 -25.79  368
  2  \w      8.21 192.21   0.50   60.00    --   34.00  73.86  64.21  368
  3  \w      8.21 192.21   0.50   60.00    --   34.00  73.86 154.21  368
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1085739000
_diffrn_orient_matrix_UB_12      -0.0049776000
_diffrn_orient_matrix_UB_13      -0.0032756000
_diffrn_orient_matrix_UB_21      0.0067559000
_diffrn_orient_matrix_UB_22      -0.0306072000
_diffrn_orient_matrix_UB_23      -0.0737062000
_diffrn_orient_matrix_UB_31      0.0062680000
_diffrn_orient_matrix_UB_32      -0.0541021000
_diffrn_orient_matrix_UB_33      0.0420813000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8215
_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         29.988
_diffrn_reflns_theta_min         2.441
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_refine_ls_extinction_coef       0.0075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3600
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0163
_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^)+(0.0283P)^2^+0.1753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3495
_reflns_number_total             3600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_14
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241877
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Mn1 U1 S2 O15'
_shelx_estimated_absorpt_t_max   0.275
_shelx_estimated_absorpt_t_min   0.061
_reflns_odcompleteness_completeness 96.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.27
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 H3A-H3B
 1.54 with sigma of 0.02
 O3-H3B
 0.98 with sigma of 0.02
 O3-H3A
 0.98 with sigma of 0.02
 O6_$1-H3B
 1.65 with sigma of 0.02
 O14_$1-H14B_$1 = O14_$1-H14A_$1
 0.98 with sigma of 0.02
 H14B_$1-H14A_$1
 1.54 with sigma of 0.02
 O5_$2-H14B_$1
 2.1 with sigma of 0.02
 H14A_$1-O7_$3
 2.1 with sigma of 0.02
 O15-H15B = O15-H15A
 0.9 with sigma of 0.02
 H15A-H15B
 1.45 with sigma of 0.02
 H15A-O7_$4
 2.1 with sigma of 0.02
 H15B-O6
 2.1 with sigma of 0.02
 O13-H13A = O13-H13B
 0.9 with sigma of 0.02
 H13A-H13B
 1.45 with sigma of 0.02
 H13A-O1_$2
 2.1 with sigma of 0.02
 O13-H13B
 0.9 with sigma of 0.02
 H13B-H13A
 1.54 with sigma of 0.02
 H13B-O3_$3
 2.2 with sigma of 0.02
 O2_$3-H12A
 2.5 with sigma of 0.02
 O12-H12A
 0.9 with sigma of 0.02
 H12B-H12A
 1.54 with sigma of 0.02
 O12-H12B
 0.9 with sigma of 0.02
 H12A-O2_$3
 2.41 with sigma of 0.02
 H12B-O1
 2.2 with sigma of 0.02
;
_shelx_res_checksum              25137
_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 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.680