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

data_7133061
_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 Na O14 Re U2'
_chemical_formula_sum            'C4 H6 Na O14 Re U2'
_chemical_formula_weight         963.34
_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                 113.798(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2417(5)
_cell_length_b                   8.1267(2)
_cell_length_c                   15.0583(5)
_cell_measurement_reflns_used    6401
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      77.1190
_cell_measurement_theta_min      3.2010
_cell_volume                     1706.60(10)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -68.00 -33.00   0.50    6.00    --  -47.14 125.00 120.00   70
  2  \w    -70.00   1.00   0.50    6.00    --  -47.14  77.00 -60.00  142
  3  \w   -119.00 -93.00   0.50    6.00    --  -47.14-125.00-180.00   52
  4  \w    -26.00  25.00   0.50    6.00    --  -47.14  19.00  60.00  102
  5  \w    -41.00  25.00   0.50    6.00    --  -47.14  37.00-180.00  132
  6  \w   -119.00 -79.00   0.50    6.00    --  -47.14-125.00 -30.00   80
  7  \w     48.00  84.00   0.50    6.00    --   47.14-125.00-180.00   72
  8  \w     84.00 114.00   0.50    6.00    --   47.14  57.00 -90.00   60
  9  \w     33.00  66.00   0.50    6.00    --   47.14  57.00 -90.00   66
 10  \w     94.00 119.00   0.50    6.00    --   47.14  77.00-150.00   50
 11  \w     89.00 117.00   0.50    6.00    --   47.14  77.00 150.00   56
 12  \w     41.00 105.00   0.50    8.00    --  107.75 -77.00  60.00  128
 13  \w     36.00  70.00   0.50    8.00    --  107.75 -88.00  58.18   68
 14  \w     95.00 131.00   0.50    8.00    --  107.75  45.00 120.00   72
 15  \w     99.00 178.00   0.50    8.00    --  107.75  15.00  60.00  158
 16  \w    124.00 177.00   0.50    8.00    --  107.75  15.00 150.00  106
 17  \w     87.00 134.00   0.50    8.00    --  107.75 -87.00 -43.15   94
 18  \w     35.00  70.00   0.50    8.00    --  107.75 -88.00 168.77   70
 19  \w     36.00  66.00   0.50    8.00    --  107.75 -61.00   0.00   60
 20  \w     94.00 120.00   0.50    8.00    --  107.75  15.00 150.00   52
 21  \w     45.00 103.00   0.50    8.00    --  107.75 -77.00 -90.00  116
 22  \w     65.00  91.00   0.50    8.00    --  107.75 -77.00   0.00   52
 23  \w     37.00  70.00   0.50    8.00    --  107.75 -61.00-180.00   66
 24  \w    103.00 175.00   0.50    8.00    --  107.75  45.00 -90.00  144
 25  \w     44.00  71.00   0.50    8.00    --  107.75 -61.00 150.00   54
 26  \w     39.00  65.00   0.50    8.00    --  107.75 -61.00 -90.00   52
 27  \w     38.00  64.00   0.50    8.00    --  107.75 -87.00 -43.15   52
 28  \w     95.00 151.00   0.50    8.00    --  107.75 125.00 120.00  112
 29  \w     37.00  68.00   0.50    8.00    --  107.75 -61.00 120.00   62
 30  \w    145.00 171.00   0.50    8.00    --  107.75  45.00 120.00   52
 31  \w     44.00  70.00   0.50    8.00    --  107.75 -61.00 -60.00   52
 32  \w     50.00 102.00   0.50    8.00    --  107.75 -77.00 120.00  104
 33  \w    143.00 169.00   0.50    8.00    --  107.75  15.00  90.00   52
 34  \w    107.00 133.00   0.50    8.00    --  107.75  15.00  90.00   52
 35  \w    101.00 177.00   0.50    8.00    --  107.75  45.00   0.00  152
 36  \w     37.00  62.00   0.50    8.00    --  107.75 -61.00  60.00   50
 37  \w     67.00 109.00   0.50    8.00    --  107.75-125.00-120.00   84
 38  \w     78.00 122.00   0.50    8.00    --  107.75 -88.00  58.18   88
 39  \w     85.00 130.00   0.50    8.00    --  107.75 -88.00 168.77   90
 40  \w     91.00 139.00   0.50    8.00    --  107.75  61.00-120.00   96
 41  \w     98.00 136.00   0.50    8.00    --  107.75 -88.00-124.15   76
 42  \w     50.00 103.00   0.50    8.00    --  107.75 -77.00 -30.00  106
 43  \w     49.00 108.00   0.50    8.00    --  107.75-125.00 -90.00  118
 44  \w     60.00  94.00   0.50    8.00    --  107.75 -88.00-124.15   68
;
_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      0.0718701000
_diffrn_orient_matrix_UB_12      0.0981859000
_diffrn_orient_matrix_UB_13      -0.0274936000
_diffrn_orient_matrix_UB_21      0.0045721000
_diffrn_orient_matrix_UB_22      -0.1430442000
_diffrn_orient_matrix_UB_23      -0.0651208000
_diffrn_orient_matrix_UB_31      -0.0837444000
_diffrn_orient_matrix_UB_32      0.0764085000
_diffrn_orient_matrix_UB_33      -0.0866439000
_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     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_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            1669
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    67.259
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29089
_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    3.749
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.709
_refine_diff_density_min         -8.171
_refine_diff_density_rms         0.618
_refine_ls_extinction_coef       0.00012(4)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0698
_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^)+(0.1277P)^2^+100.4844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1546
_reflns_number_total             1669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           ui_36_thinplate150816_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133061
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U Re2 O12'
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.174
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.514(6)
 0.486(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: Re4(0.25) O13(0.25) H16A(0.5) H16B(0.5) H16C(0.5) O12(0.5)
 Re3(0.25) H17A(0.5) H17B(0.5) H17C(0.5) O1(0.25)
4.a Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              36157
_shelx_hkl_checksum              20797
_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 3.008
_oxdiff_exptl_absorpt_empirical_full_min 0.507