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

data_7133065
_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 H20 O25 Tc U4, 0.75(O)'
_chemical_formula_sum            'C8 H20 O25.75 Tc U4'
_chemical_formula_weight         1578.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3710(3)
_cell_length_b                   13.8231(3)
_cell_length_c                   14.8033(3)
_cell_measurement_reflns_used    16660
_cell_measurement_temperature    222.99(10)
_cell_measurement_theta_max      76.5190
_cell_measurement_theta_min      2.9920
_cell_volume                     2940.70(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      222.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -58.00  21.00   0.50    5.00    --  -47.14  57.00-150.00  158
  2  \w   -119.00 -89.00   0.50    5.00    --  -47.14 -77.00 -30.00   60
  3  \w    -61.00  24.00   0.50    5.00    --  -47.14  57.00  90.00  170
  4  \w   -119.00 -92.00   0.50    5.00    --  -47.14 -77.00   0.00   54
  5  \w    -25.00  22.00   0.50    5.00    --   47.14 -19.00   0.00   94
  6  \w     88.00 115.00   0.50    5.00    --   47.14  77.00  60.00   54
  7  \w    -25.00 119.00   0.50    5.00    --   47.14   0.00  30.00  288
  8  \w    -80.00 -38.00   0.50    8.00    --  -86.25 125.00 -60.00   84
  9  \w     99.00 171.00   0.50    8.00    --  107.75  30.00  30.00  144
 10  \w     50.00 106.00   0.50    8.00    --  107.75 -94.00 120.00  112
 11  \w     35.00  70.00   0.50    8.00    --  107.75 -61.00 150.00   70
 12  \w     99.00 170.00   0.50    8.00    --  107.75  15.00  90.00  142
 13  \w     59.00 105.00   0.50    8.00    --  107.75 -94.00-180.00   92
 14  \w     35.00  69.00   0.50    8.00    --  107.75 -77.00 -90.00   68
 15  \w     35.00  73.00   0.50    8.00    --  107.75 -87.00-110.33   76
 16  \w     39.00  64.00   0.50    8.00    --  107.75 -61.00-180.00   50
 17  \w    130.00 162.00   0.50    8.00    --  107.75  45.00-120.00   64
 18  \w     41.00  97.00   0.50    8.00    --  107.75 -77.00  30.00  112
 19  \w     43.00  69.00   0.50    8.00    --  107.75 -61.00  30.00   52
 20  \w     42.00  70.00   0.50    8.00    --  107.75 -77.00 120.00   56
 21  \w     38.00  63.00   0.50    8.00    --  107.75 -61.00 -90.00   50
 22  \w    110.00 178.00   0.50    8.00    --  107.75  30.00   0.00  136
 23  \w     95.00 167.00   0.50    8.00    --  107.75  45.00 -30.00  144
 24  \w     49.00  92.00   0.50    8.00    --  107.75-125.00 -90.00   86
 25  \w    103.00 131.00   0.50    8.00    --  107.75  45.00  90.00   56
 26  \w    144.00 178.00   0.50    8.00    --  107.75  45.00  90.00   68
 27  \w     35.00  60.00   0.50    8.00    --  107.75 -61.00-120.00   50
 28  \w     40.00  65.00   0.50    8.00    --  107.75 -61.00   0.00   50
 29  \w     40.00  71.00   0.50    8.00    --  107.75 -61.00 120.00   62
 30  \w     71.00 105.00   0.50    8.00    --  107.75 -77.00 -90.00   68
 31  \w    145.00 172.00   0.50    8.00    --  107.75 125.00  90.00   54
 32  \w     95.00 122.00   0.50    8.00    --  107.75 125.00  90.00   54
 33  \w     77.00 103.00   0.50    8.00    --  107.75 -94.00  90.00   52
 34  \w     41.00  71.00   0.50    8.00    --  107.75 -94.00  90.00   60
 35  \w     36.00 105.00   0.50    8.00    --  107.75 -94.00-150.00  138
 36  \w     37.00  62.00   0.50    8.00    --  107.75-125.00-120.00   50
 37  \w    108.00 175.00   0.50    8.00    --  107.75  30.00 120.00  134
 38  \w     97.00 123.00   0.50    8.00    --  107.75  45.00-120.00   52
 39  \w     88.00 115.00   0.50    8.00    --  107.75 -87.00-110.33   54
 40  \w     67.00 106.00   0.50    8.00    --  107.75 -94.00 150.00   78
 41  \w     55.00 105.00   0.50    8.00    --  107.75 -77.00 -30.00  100
 42  \w     68.00  95.00   0.50    8.00    --  107.75 -77.00  60.00   54
 43  \w     74.00 122.00   0.50    8.00    --  107.75 -87.00 -10.88   96
 44  \w     81.00 106.00   0.50    8.00    --  107.75 -77.00-120.00   50
 45  \w     76.00 105.00   0.50    8.00    --  107.75 -94.00-120.00   58
 46  \w     92.00 134.00   0.50    8.00    --  107.75 -88.00 -65.47   84
;
_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      -0.0140774000
_diffrn_orient_matrix_UB_12      0.0590811000
_diffrn_orient_matrix_UB_13      -0.0872043000
_diffrn_orient_matrix_UB_21      -0.1043525000
_diffrn_orient_matrix_UB_22      -0.0256910000
_diffrn_orient_matrix_UB_23      0.0007717000
_diffrn_orient_matrix_UB_31      -0.0202587000
_diffrn_orient_matrix_UB_32      0.0909364000
_diffrn_orient_matrix_UB_33      0.0567442000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36295
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         4.438
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    65.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26414
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.565
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.393
_refine_diff_density_min         -2.572
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.000061(8)
_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   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0529P)^2^+40.1766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2488
_reflns_number_total             2695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           utc_3_rod_131414_cu_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133065
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U Tc O C'
_shelx_estimated_absorpt_t_max   0.559
_shelx_estimated_absorpt_t_min   0.077
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O21(0.25) O22(0.125)
3.a Rotating group:
 O14(H14A,H14B), O12(H12A,H12B)
3.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              17857
_shelx_hkl_checksum              61556
_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 3.566
_oxdiff_exptl_absorpt_empirical_full_min 0.405