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

data_7133064
_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         'C4 H6 O32 Tc2 U5'
_chemical_formula_sum            'C4 H6 O32 Tc2 U5'
_chemical_formula_weight         1952.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-06
_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                93.982(3)
_cell_angle_beta                 99.211(3)
_cell_angle_gamma                109.708(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7451(3)
_cell_length_b                   8.4501(2)
_cell_length_c                   12.7565(5)
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    172.97(10)
_cell_measurement_theta_max      76.8720
_cell_measurement_theta_min      3.5520
_cell_volume                     768.96(5)
_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      172.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -38.00   7.00   0.50    6.00    --  -47.14  36.00 -34.00   90
  2  \w   -116.00 -41.00   0.50    6.00    --  -47.14 -36.00 169.00  150
  3  \w     -7.00  33.00   0.50    6.00    --   47.14 -36.00 169.00   80
  4  \w     37.00 120.00   0.50    6.00    --   47.14  36.00 -34.00  166
  5  \w   -125.00-100.00   0.50    8.00    --  -86.25 -36.00 169.00   50
  6  \w    -41.00 -14.00   0.50    8.00    --  -86.25  36.00 -34.00   54
  7  \w    138.00 178.00   0.50    8.00    --  107.75  36.00 -34.00   80
  8  \w   -118.00 -89.00   0.50    6.00    --  -47.14 -77.00  60.00   58
  9  \w   -118.00 -93.00   0.50    6.00    --  -47.14 -77.00-180.00   50
 10  \w   -118.00 -79.00   0.50    6.00    --  -47.14-125.00 -60.00   78
 11  \w     42.00  78.00   0.50    6.00    --   47.14-125.00  30.00   72
 12  \w     85.00 115.00   0.50    6.00    --   47.14  77.00  30.00   60
 13  \w     65.00  93.00   0.50    6.00    --   47.14-125.00-150.00   56
 14  \w     42.00  74.00   0.50    6.00    --   47.14 -99.00-180.00   64
 15  \w     35.00  61.00   0.50    6.00    --   47.14-125.00-150.00   52
 16  \w     46.00 106.00   0.50    8.00    --  107.75 -77.00 -60.00  120
 17  \w     87.00 112.00   0.50    8.00    --  107.75-125.00   0.00   50
 18  \w     36.00  71.00   0.50    8.00    --  107.75 -61.00 120.00   70
 19  \w     49.00 105.00   0.50    8.00    --  107.75 -77.00  30.00  112
 20  \w     58.00 110.00   0.50    8.00    --  107.75-125.00-150.00  104
 21  \w     35.00  66.00   0.50    8.00    --  107.75 -85.00-148.01   62
 22  \w     35.00  70.00   0.50    8.00    --  107.75 -61.00 -30.00   70
 23  \w    100.00 136.00   0.50    8.00    --  107.75  30.00 -60.00   72
 24  \w    126.00 176.00   0.50    8.00    --  107.75  77.00 -90.00  100
 25  \w    100.00 125.00   0.50    8.00    --  107.75  61.00-180.00   50
 26  \w     59.00 100.00   0.50    8.00    --  107.75 -94.00 -90.00   82
 27  \w    102.00 156.00   0.50    8.00    --  107.75  45.00 120.00  108
 28  \w     95.00 160.00   0.50    8.00    --  107.75  15.00  60.00  130
 29  \w     38.00  71.00   0.50    8.00    --  107.75-125.00   0.00   66
 30  \w    104.00 148.00   0.50    8.00    --  107.75  45.00   0.00   88
 31  \w     73.00 129.00   0.50    8.00    --  107.75 -88.00 117.48  112
 32  \w     65.00 101.00   0.50    8.00    --  107.75 -94.00  90.00   72
 33  \w     35.00  80.00   0.50    8.00    --  107.75-125.00 150.00   90
 34  \w    107.00 132.00   0.50    8.00    --  107.75  45.00-180.00   50
 35  \w    139.00 167.00   0.50    8.00    --  107.75  45.00-180.00   56
 36  \w     66.00 117.00   0.50    8.00    --  107.75 -87.00  53.68  102
 37  \w     35.00  81.00   0.50    8.00    --  107.75 -77.00   0.00   92
 38  \w     35.00  62.00   0.50    8.00    --  107.75 -61.00  60.00   54
 39  \w     51.00  77.00   0.50    8.00    --  107.75 -94.00-120.00   52
 40  \w    101.00 155.00   0.50    8.00    --  107.75  45.00 150.00  108
 41  \w     44.00  69.00   0.50    8.00    --  107.75 -61.00 -90.00   50
 42  \w     88.00 132.00   0.50    8.00    --  107.75 -85.00-148.01   88
 43  \w     50.00 105.00   0.50    8.00    --  107.75 -94.00-150.00  110
 44  \w    100.00 126.00   0.50    8.00    --  107.75 125.00-150.00   52
 45  \w     94.00 163.00   0.50    8.00    --  107.75  15.00 -90.00  138
 46  \w     35.00  73.00   0.50    8.00    --  107.75 -94.00 120.00   76
 47  \w    107.00 150.00   0.50    8.00    --  107.75  45.00  60.00   86
 48  \w     38.00  64.00   0.50    8.00    --  107.75 -86.00-108.13   52
 49  \w     97.00 122.00   0.50    8.00    --  107.75 -86.00-108.13   50
 50  \w     49.00 101.00   0.50    8.00    --  107.75 -94.00  30.00  104
;
_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      0.1094387000
_diffrn_orient_matrix_UB_12      0.1924887000
_diffrn_orient_matrix_UB_13      0.0218605000
_diffrn_orient_matrix_UB_21      -0.1563367000
_diffrn_orient_matrix_UB_22      0.0257902000
_diffrn_orient_matrix_UB_23      0.0522167000
_diffrn_orient_matrix_UB_31      0.0999757000
_diffrn_orient_matrix_UB_32      -0.0214361000
_diffrn_orient_matrix_UB_33      0.1096929000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10031
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.170
_diffrn_reflns_theta_min         3.541
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    81.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55873
_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 orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.216
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.047
_refine_diff_density_min         -1.923
_refine_diff_density_rms         0.336
_refine_ls_extinction_coef       0.00033(3)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2797
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0404P)^2^+6.9353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2699
_reflns_number_total             2797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           utc_10_070812_ms_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U5 Tc2 O32 C4 H20'
_shelx_estimated_absorpt_t_max   0.294
_shelx_estimated_absorpt_t_min   0.140
_reflns_odcompleteness_completeness 99.86
_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
2.a Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              55915
_shelx_hkl_checksum              7652
_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 3.004
_oxdiff_exptl_absorpt_empirical_full_min 0.336