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

data_7133063
_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 H18 O32 Re2 U5'
_chemical_formula_sum            'C4 H18 O32 Re2 U5'
_chemical_formula_weight         2140.73
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-03
_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                94.029(3)
_cell_angle_beta                 99.086(3)
_cell_angle_gamma                109.920(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7354(3)
_cell_length_b                   8.4717(3)
_cell_length_c                   12.7820(4)
_cell_measurement_reflns_used    6641
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      30.9270
_cell_measurement_theta_min      2.8480
_cell_volume                     770.66(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -66.00 -17.00   0.50   70.00    --    4.12 -64.00 -71.00   98
  2  \w     -4.00  72.00   0.50   70.00    --    4.12  64.00  65.00  152
  3  \w    -70.00   5.00   0.50   70.00    --    4.12 -19.00 150.00  150
  4  \w    -12.00  22.00   0.50   70.00    --    4.12 -64.00 -71.00   68
  5  \w    -14.00  25.00   0.50   70.00    --    4.12 -99.00 -90.00   78
  6  \w    -15.00  23.00   0.50   70.00    --    4.12 -99.00  60.00   76
  7  \w    -14.00  11.00   0.50   70.00    --   -6.08 -99.00 -60.00   50
  8  \w    -39.00  14.00   0.50   70.00    --   -6.08 -77.00-120.00  106
;
_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      0.0099248000
_diffrn_orient_matrix_UB_12      -0.0538909000
_diffrn_orient_matrix_UB_13      -0.0418572000
_diffrn_orient_matrix_UB_21      0.0926588000
_diffrn_orient_matrix_UB_22      0.0567269000
_diffrn_orient_matrix_UB_23      0.0019995000
_diffrn_orient_matrix_UB_31      0.0346377000
_diffrn_orient_matrix_UB_32      -0.0441894000
_diffrn_orient_matrix_UB_33      0.0382038000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       -15
_diffrn_reflns_number            9602
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.861
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    34.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    4.613
_exptl_crystal_description       cube
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0177P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2840
_reflns_number_total             3149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01726a2.cif
_cod_data_source_block           ui_36_ms_mo_auto
_cod_depositor_comments
'Adding full bibliography for 7133061--7133065.cif.'
_cod_database_code               7133063
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         UReO16C2
_reflns_odcompleteness_completeness 94.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 U3-H16A \\sim U3-H16B
 with sigma of 0.02
 U2-H12A \\sim U2-H12B
 with sigma of 0.02
3.a Free rotating group:
 O16(H16A,H16B), O12(H12A,H12B)
3.b Rotating group:
 O15(H15A,H15B)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              9588
_shelx_hkl_checksum              79365
_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 3.096
_oxdiff_exptl_absorpt_empirical_full_min 0.531