Uranyl-Tc(VII)/Tc(V) hybrid clusters.
Shohel, Mohammad; Nyman, May; Chemical communications (Cambridge, England) 60 (2024) 5820–5823; doi:10.1039/d4cc01726a

data_7133062
_publ_section_title
;
 Uranyl-Tc(VII)/Tc(V) hybrid clusters.
;
_journal_issue                   45
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5820
_journal_page_last               5823
_journal_paper_doi               10.1039/d4cc01726a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C8 H12 Na2 O30 Tc2 U4'
_chemical_formula_sum            'C8 H12 Na2 O30 Tc2 U4'
_chemical_formula_weight         1782.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-02-11 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.061(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2356(8)
_cell_length_b                   8.1216(3)
_cell_length_c                   15.0053(7)
_cell_measurement_reflns_used    5109
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      76.8850
_cell_measurement_theta_min      3.2210
_cell_volume                     1695.39(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -23.00  28.00   0.50    8.00    --  -47.14  19.00-180.00  102
  2  \w   -120.00 -52.00   0.50    8.00    --  -47.14 -19.00   0.00  136
  3  \w   -119.00 -85.00   0.50    8.00    --  -47.14 -77.00  90.00   68
  4  \w    -70.00  25.00   0.50    8.00    --  -47.14  77.00 120.00  190
  5  \w    -10.00  24.00   0.50    8.00    --  -47.14  19.00  30.00   68
  6  \w   -119.00 -93.00   0.50    8.00    --  -47.14 -77.00  60.00   52
  7  \w    -27.00  -2.00   0.50    8.00    --   47.14 -19.00 -90.00   50
  8  \w     55.00  94.00   0.50    8.00    --   47.14-125.00-150.00   78
  9  \w   -157.00-116.00   0.50   10.50    --  -86.25-125.00-120.00   82
 10  \w   -157.00-102.00   0.50   10.50    --  -86.25 -45.00 120.00  110
 11  \w     35.00 105.00   0.50   10.50    --  107.75 -77.00 150.00  140
 12  \w     98.00 177.00   0.50   10.50    --  107.75  15.00  30.00  158
 13  \w    100.00 178.00   0.50   10.50    --  107.75  30.00-150.00  156
 14  \w     80.00 105.00   0.50   10.50    --  107.75 -77.00 -90.00   50
 15  \w     40.00  67.00   0.50   10.50    --  107.75 -61.00-120.00   54
 16  \w     73.00 105.00   0.50   10.50    --  107.75 -77.00  30.00   64
 17  \w    135.00 178.00   0.50   10.50    --  107.75  30.00  60.00   86
 18  \w     38.00  66.00   0.50   10.50    --  107.75 -61.00  60.00   56
 19  \w     36.00  70.00   0.50   10.50    --  107.75 -61.00-150.00   68
 20  \w     36.00  77.00   0.50   10.50    --  107.75 -77.00 -30.00   82
 21  \w     77.00 105.00   0.50   10.50    --  107.75 -94.00-120.00   56
 22  \w     36.00  66.00   0.50   10.50    --  107.75 -77.00  30.00   60
 23  \w     79.00 106.00   0.50   10.50    --  107.75 -94.00 -30.00   54
 24  \w     35.00  66.00   0.50   10.50    --  107.75 -61.00 -90.00   62
 25  \w     42.00  75.00   0.50   10.50    --  107.75 -94.00 -30.00   66
 26  \w    111.00 175.00   0.50   10.50    --  107.75  15.00 -30.00  128
 27  \w     43.00  70.00   0.50   10.50    --  107.75 -61.00-180.00   54
 28  \w     46.00  76.00   0.50   10.50    --  107.75 -77.00 -90.00   60
 29  \w     45.00  72.00   0.50   10.50    --  107.75 -77.00-120.00   54
 30  \w    116.00 176.00   0.50   10.50    --  107.75  15.00 -90.00  120
 31  \w     60.00  86.00   0.50   10.50    --  107.75 -77.00-180.00   52
 32  \w     84.00 131.00   0.50   10.50    --  107.75 -88.00 139.01   94
 33  \w     37.00  99.00   0.50   10.50    --  107.75 -77.00  90.00  124
 34  \w     38.00  71.00   0.50   10.50    --  107.75 -61.00 150.00   66
 35  \w     74.00 105.00   0.50   10.50    --  107.75 -94.00 -90.00   62
 36  \w     41.00  78.00   0.50   10.50    --  107.75 -87.00  21.89   74
 37  \w     86.00 122.00   0.50   10.50    --  107.75 -87.00  21.89   72
 38  \w     37.00  64.00   0.50   10.50    --  107.75 -61.00 120.00   54
 39  \w     35.00  69.00   0.50   10.50    --  107.75 -61.00  30.00   68
 40  \w     67.00 105.00   0.50   10.50    --  107.75 -94.00 120.00   76
 41  \w    110.00 161.00   0.50   10.50    --  107.75  45.00 120.00  102
 42  \w    127.00 167.00   0.50   10.50    --  107.75  45.00-180.00   80
 43  \w     85.00 112.00   0.50   10.50    --  107.75 -88.00   4.91   54
 44  \w     76.00 106.00   0.50   10.50    --  107.75 -94.00   0.00   60
 45  \w     39.00  64.00   0.50   10.50    --  107.75 -88.00   4.91   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0935481000
_diffrn_orient_matrix_UB_12      0.0445351000
_diffrn_orient_matrix_UB_13      0.0105937000
_diffrn_orient_matrix_UB_21      -0.0122421000
_diffrn_orient_matrix_UB_22      0.1523208000
_diffrn_orient_matrix_UB_23      -0.0652621000
_diffrn_orient_matrix_UB_31      -0.0579356000
_diffrn_orient_matrix_UB_32      -0.1040059000
_diffrn_orient_matrix_UB_33      -0.0909437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1678
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    60.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         9.150
_refine_diff_density_min         -5.439
_refine_diff_density_rms         0.667
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1341P)^2^+30.9071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1538
_reflns_number_total             1678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           utc_3_thinplate_150815_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_original_cell_volume        1695.39(15)
_cod_database_code               7133062
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U2 Tc O15 C4 Na H6'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.485(6)
 0.515(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) O00G(0.375) H1A(0.5) H1B(0.5) H1C(0.5)
 O2(0.125)
4.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              95963
_shelx_hkl_checksum              79012
_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 2.201
_oxdiff_exptl_absorpt_empirical_full_min 0.465