A trinuclear metallasilsesquioxane of uranium(III).
Tricoire, Maxime; Jori, Nadir; Fadaei Tirani, Farzaneh; Scopelliti, Rosario; Z Ivković, Ivica; Natrajan, Louise S.; Mazzanti, Marinella; Chemical communications (Cambridge, England) 60 (2023) 55–58; doi:10.1039/d3cc05390c

data_7132388
_publ_section_title
;
 A trinuclear metallasilsesquioxane of uranium(III).
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              55
_journal_page_last               58
_journal_paper_doi               10.1039/d3cc05390c
_journal_volume                  60
_journal_year                    2023
_chemical_formula_moiety         'C84 O36 Si21 U3, 1.5[C6H14]'
_chemical_formula_sum            'C93 H21 O36 Si21 U3'
_chemical_formula_weight         3018.08
_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_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-16 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                65.307(4)
_cell_angle_beta                 87.504(4)
_cell_angle_gamma                78.555(4)
_cell_formula_units_Z            2
_cell_length_a                   14.7163(7)
_cell_length_b                   22.3387(9)
_cell_length_c                   24.0090(11)
_cell_measurement_reflns_used    10580
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.0760
_cell_measurement_theta_min      3.6960
_cell_volume                     7021.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.94a 64-bit (release 20-10-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_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   -113.00 -88.00   1.00    5.00    --  -40.66-143.00  51.00   25
  2  \w    -88.00  -8.00   1.00    5.00    --  -40.66 127.00 -63.00   80
  3  \w    -82.00 -57.00   1.00    5.00    --  -40.66 143.00 105.00   25
  4  \w     61.00  86.00   1.00    5.00    --   40.66-127.00-139.00   25
  5  \w     48.00  73.00   1.00    5.00    --   40.66-143.00  51.00   25
  6  \w    108.00 135.00   1.00   20.00    --  105.15 143.00 105.00   27
  7  \w     49.00  75.00   1.00   20.00    --  105.15-127.00-139.00   26
  8  \w    119.00 144.00   1.00   20.00    --  105.15 127.00 -63.00   25
  9  \w     57.00  82.00   1.00   20.00    --  105.15-143.00  51.00   25
 10  \w   -115.00 -16.00   1.00    5.00    --  -40.66 -38.00  30.00   99
 11  \w    -64.00  31.00   1.00    5.00    --  -40.66  38.00-150.00   95
 12  \w     19.00 113.00   1.00    5.00    --   40.66  38.00 -60.00   94
 13  \w     12.00  39.00   1.00    5.00    --   40.66 -38.00 -90.00   27
 14  \w    115.00 145.00   1.00   20.00    --  105.15  77.00  90.00   30
 15  \w     97.00 137.00   1.00   20.00    --  105.15 -77.00  30.00   40
 16  \w    106.00 175.00   1.00   20.00    --  105.15 111.00   0.00   69
 17  \w     33.00 109.00   1.00   20.00    --  105.15-111.00 120.00   76
 18  \w    153.00 178.00   1.00   20.00    --  105.15  30.00 -30.00   25
 19  \w    106.00 176.00   1.00   20.00    --  105.15 111.00 -30.00   70
 20  \w     80.00 178.00   1.00   20.00    --  105.15  45.00 150.00   98
 21  \w     35.00 109.00   1.00   20.00    --  105.15-111.00 -60.00   74
 22  \w    119.00 144.00   1.00   20.00    --  105.15  30.00 -30.00   25
 23  \w     33.00 127.00   1.00   20.00    --  105.15 -61.00   0.00   94
 24  \w     23.00  98.00   1.00   20.00    --  105.15 -94.00 -30.00   75
 25  \w    134.00 160.00   1.00   20.00    --  105.15  77.00-120.00   26
 26  \w     68.00 109.00   1.00   20.00    --  105.15-111.00-150.00   41
 27  \w    103.00 130.00   1.00   20.00    --  105.15  77.00-180.00   27
 28  \w     78.00 106.00   1.00   20.00    --  105.15-111.00  30.00   28
 29  \w     85.00 172.00   1.00   20.00    --  105.15  45.00  60.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0743843000
_diffrn_orient_matrix_UB_12      0.0503063000
_diffrn_orient_matrix_UB_13      0.0141050000
_diffrn_orient_matrix_UB_21      0.0159195000
_diffrn_orient_matrix_UB_22      -0.0453663000
_diffrn_orient_matrix_UB_23      0.0691699000
_diffrn_orient_matrix_UB_31      0.0751247000
_diffrn_orient_matrix_UB_32      0.0375393000
_diffrn_orient_matrix_UB_33      0.0037532000
_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  0.0967
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56710
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.411
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.897
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.072
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2874
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.213
_refine_diff_density_max         3.331
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         24790
_refine_ls_number_restraints     2254
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1968
_refine_ls_R_factor_gt           0.1307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3490
_refine_ls_wR_factor_ref         0.3936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13031
_reflns_number_total             24790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05390c2.cif
_cod_data_source_block           nj1198-supa-3
_cod_depositor_comments
'Adding full bibliography for 7132387--7132389.cif.'
_cod_database_code               7132388
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C84 H189 Si21 O36 U3'
_shelx_estimated_absorpt_t_max   0.186
_shelx_estimated_absorpt_t_min   0.106
_olex2_refinement_description
;
1. Restrained distances
 C61-C62 = C62-C63
 1.54 with sigma of 0.02
 Si9-C33
 1.9 with sigma of 0.02
 Si4-C13
 1.9 with sigma of 0.02
 Si19-C73
 1.9 with sigma of 0.02
 Si16-C61
 1.9 with sigma of 0.02
 Si7-C25
 1.9 with sigma of 0.02
 Si18-C69
 1.9 with sigma of 0.02
 C69-C70 = C71-C70 = C72-C70
 1.54 with sigma of 0.02
 Si11-C41
 1.9 with sigma of 0.02
 Si3-C9
 1.9 with sigma of 0.02
 C11-Si3
 3.5 with sigma of 0.02
 Si3-C12
 4.2 with sigma of 0.02
 C10-C9 = C11-C10 = C12-C10
 1.54 with sigma of 0.02
 Si13-C49
 1.9 with sigma of 0.02
 C49-C50 = C51-C50 = C52-C50
 1.54 with sigma of 0.02
 C52-Si13
 3.5 with sigma of 0.02
 C51-Si13
 4.2 with sigma of 0.02
 Si12-C45
 1.9 with sigma of 0.02
 C45-C46 = C46-C48 = C47-C46
 1.54 with sigma of 0.02
 C48-Si12
 3.5 with sigma of 0.02
 Si17-C65
 1.9 with sigma of 0.02
 C65-C66 = C68-C66 = C67-C66
 1.54 with sigma of 0.02
 Si17-C67
 3.5 with sigma of 0.02
 C68-Si17
 4.2 with sigma of 0.02
 Si6-C21
 1.9 with sigma of 0.02
 C21-C22 = C23-C22 = C24-C22
 1.54 with sigma of 0.02
 C23-Si6
 3.5 with sigma of 0.02
 C24-Si6
 4.2 with sigma of 0.02
 Si2-C5
 1.9 with sigma of 0.02
 C6-C5 = C6-C8 = C7-C6
 1.54 with sigma of 0.02
 C8-Si2
 3.5 with sigma of 0.02
 C7-Si2
 4.2 with sigma of 0.02
 Si21-C81
 1.9 with sigma of 0.02
 C82-C81 = C83-C82 = C84-C82
 1.54 with sigma of 0.02
 C83-Si21
 4.2 with sigma of 0.02
 C84-Si21
 3.5 with sigma of 0.02
 Si5-C17
 1.9 with sigma of 0.02
 C18-C17 = C19-C18 = C20-C18
 1.54 with sigma of 0.02
 Si15-C57
 1.9 with sigma of 0.02
 C58-C57 = C59-C58 = C60-C58
 1.54 with sigma of 0.02
 C60-Si15
 3.5 with sigma of 0.02
 C59-Si15
 4.2 with sigma of 0.02
 Si10-C37
 1.9 with sigma of 0.02
 C38-C37 = C39-C38 = C38-C40
 1.54 with sigma of 0.02
 C39-C37 = C39-C40
 2.5 with sigma of 0.02
 C39-Si10
 3.5 with sigma of 0.02
 C40-Si10
 4.2 with sigma of 0.02
 Si20-C77
 1.9 with sigma of 0.02
 C78-C77 = C80-C78 = C79-C78
 1.54 with sigma of 0.02
 C80-Si20
 3.5 with sigma of 0.02
 C79-Si20
 4.2 with sigma of 0.02
 C79-C77 = C80-C79 = C80-C77
 2.5 with sigma of 0.02
 Si8-C29
 1.9 with sigma of 0.02
 C30-C29 = C31-C30 = C32-C30
 1.54 with sigma of 0.02
 Si18-C71
 3.5 with sigma of 0.02
 C72-Si18
 4.2 with sigma of 0.02
 C71-C70 = C70-C69 = C72-C70
 1.54 with sigma of 0.02
 C20-Si5
 3.5 with sigma of 0.02
 C19-Si5
 4.2 with sigma of 0.02
 C19-C20
 2.5 with sigma of 0.02
 C17-C19
 2.5 with sigma of 0.02
 C20-C17
 2.5 with sigma of 0.02
 C54-C53 = C55-C54 = C56-C54
 1.54 with sigma of 0.02
 C2-C1 = C4-C2 = C3-C2
 1.54 with sigma of 0.02
 C26-C25 = C28-C26 = C27-C26
 1.54 with sigma of 0.02
 C25-C28
 2.5 with sigma of 0.02
 C25-C27
 2.5 with sigma of 0.02
 C27-C28
 2.5 with sigma of 0.02
 C8-C5
 2.5 with sigma of 0.02
 C5-C7
 2.5 with sigma of 0.02
 C7-C8
 2.5 with sigma of 0.02
 C34-C33 \\sim C35-C34 \\sim C36-C34
 with sigma of 0.01
 C33-C35 \\sim C35-C36 \\sim C33-C36
 with sigma of 0.01
 C14-C13 \\sim C14-C15 \\sim C16-C14
 with sigma of 0.01
 C13-C15 \\sim C15-C16 \\sim C13-C16
 with sigma of 0.01
 C74-C73 \\sim C76-C74 \\sim C75-C74
 with sigma of 0.01
 C75-C73 \\sim C73-C76 \\sim C75-C76
 with sigma of 0.01
 C61-C62 \\sim C62-C63 \\sim C62-C64
 with sigma of 0.01
 C63-C61 \\sim C61-C64 \\sim C63-C64
 with sigma of 0.01
 C25-C26 \\sim C27-C26 \\sim C28-C26
 with sigma of 0.01
 C25-C27 \\sim C27-C28 \\sim C25-C28
 with sigma of 0.01
 C69-C70 \\sim C71-C70 \\sim C72-C70
 with sigma of 0.01
 C71-C69 \\sim C69-C72 \\sim C71-C72
 with sigma of 0.01
 C42-C41 \\sim C43-C42 \\sim C44-C42
 with sigma of 0.01
 C41-C43 \\sim C43-C44 \\sim C41-C44
 with sigma of 0.01
 C10-C9 \\sim C11-C10 \\sim C12-C10
 with sigma of 0.01
 C11-C12 \\sim C12-C9 \\sim C9-C11
 with sigma of 0.01
 C49-C51 \\sim C51-C52 \\sim C49-C52
 with sigma of 0.01
 C48-C45 \\sim C45-C47 \\sim C47-C48
 with sigma of 0.01
 C65-C68 \\sim C68-C67 \\sim C65-C67
 with sigma of 0.01
 C21-C23 \\sim C23-C24 \\sim C21-C24
 with sigma of 0.01
 C5-C7 \\sim C7-C8 \\sim C5-C8
 with sigma of 0.01
 C81-C84 \\sim C84-C83 \\sim C81-C83
 with sigma of 0.01
 C19-C17 \\sim C17-C20 \\sim C19-C20
 with sigma of 0.01
 C45-C48 \\sim C48-C47 \\sim C45-C47
 with sigma of 0.01
 C57-C59 \\sim C59-C60 \\sim C57-C60
 with sigma of 0.01
 C37-C39 \\sim C39-C40 \\sim C37-C40
 with sigma of 0.01
 C77-C79 \\sim C79-C80 \\sim C77-C80
 with sigma of 0.01
 C69-C71 \\sim C71-C72 \\sim C69-C72
 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(U4)=Sof(U5)=Sof(U6)=1-FVAR(1)
 Sof(U1)=Sof(U2)=Sof(U3)=FVAR(1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 149 electrons were 
found in a volume of 905\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
1.5[C6H14] per Asymmetric Unit 
which account for 150 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              53006
_shelx_hkl_checksum              34955
_shelx_fab_checksum              92307
_olex2_date_sample_data_collection 2023-10-30
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.583
_oxdiff_exptl_absorpt_empirical_full_min 0.230