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_7132389
_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         'C112 O48 Si28 U4'
_chemical_formula_sum            'C112 O48 Si28 U4'
_chemical_formula_weight         3851.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-30 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.864(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.7165(7)
_cell_length_b                   33.7274(5)
_cell_length_c                   35.2400(9)
_cell_measurement_reflns_used    34537
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      29.0860
_cell_measurement_theta_min      2.9250
_cell_volume                     39217.8(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (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    'SHELXT (Shedlrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5633
_diffrn_detector_type            AtlasS2
_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    -52.00  31.00   1.00   22.50    --   11.66 -68.00-131.00   83
  2  \w    -19.00  84.00   1.00   22.50    --   11.66  68.00   2.00  103
  3  \w     42.00  69.00   1.00   22.50    --   11.66 178.00-150.00   27
  4  \w     73.00  98.00   1.00   22.50    --   11.66 178.00 -90.00   25
  5  \w     -5.00  21.00   1.00   22.50    --  -11.81  77.00 120.00   26
  6  \w     -4.00  21.00   1.00   22.50    --  -11.81 -77.00 -30.00   25
  7  \w    -14.00  15.00   1.00   22.50    --  -11.81  77.00 150.00   29
  8  \w    -34.00  -9.00   1.00   22.50    --  -11.81  57.00-120.00   25
  9  \w    -33.00  18.00   1.00   22.50    --  -11.81 -77.00  90.00   51
;
_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      0.0085824000
_diffrn_orient_matrix_UB_12      -0.0069761000
_diffrn_orient_matrix_UB_13      -0.0155128000
_diffrn_orient_matrix_UB_21      -0.0109366000
_diffrn_orient_matrix_UB_22      0.0146186000
_diffrn_orient_matrix_UB_23      -0.0123673000
_diffrn_orient_matrix_UB_31      0.0163944000
_diffrn_orient_matrix_UB_32      0.0134171000
_diffrn_orient_matrix_UB_33      0.0054185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            77282
_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         26.372
_diffrn_reflns_theta_min         2.685
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.523
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (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            'lustrous dark black'
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       irregular
_exptl_crystal_F_000             14528
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.222
_refine_diff_density_max         3.264
_refine_diff_density_min         -6.528
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1718
_refine_ls_number_reflns         77282
_refine_ls_number_restraints     2761
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.1234
_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^)+(0.1550P)^2^+3774.9341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3271
_refine_ls_wR_factor_ref         0.3366
_reflns_Friedel_coverage         0.000
_reflns_number_gt                55856
_reflns_number_total             77282
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9968\% 
around [-0.70 0.70 0.15] (reciprocal) or [-0.71 0.71 -0.00] (direct)
;
_cod_data_source_file            d3cc05390c2.cif
_cod_data_source_block           mt-246_sq
_cod_depositor_comments
'Adding full bibliography for 7132387--7132389.cif.'
_cod_original_cell_volume        39218.0(15)
_cod_database_code               7132389
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C50 H100 O20 Si21 U3'
_shelx_estimated_absorpt_t_max   0.508
_shelx_estimated_absorpt_t_min   0.322
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.549(2)
 0.451(2)
2. Restrained distances
 C97-C51 = C51-C103 = C99-C51
 1.54 with sigma of 0.02
 C51-Si3
 2.9 with sigma of 0.02
 C97-Si3
 3.5 with sigma of 0.02
 C99-Si3
 4.2 with sigma of 0.02
 C97-C103
 2.5 with sigma of 0.02
 C99-C97
 2.5 with sigma of 0.02
 C99-C103
 2.5 with sigma of 0.02
 C94-C104 = C94-C83 = C94-C92
 1.54 with sigma of 0.02
 C104-C92
 2.5 with sigma of 0.02
 C104-C83
 2.5 with sigma of 0.02
 C83-C92
 2.5 with sigma of 0.02
 Si13-C48 \\sim Si7-C65 \\sim Si20-C30 \\sim Si24-C20 \\sim Si28-C59 \\sim
Si22-C98 \\sim Si6-C12
 with sigma of 0.02
 C58-C48 \\sim C58-C39 \\sim C77-C58
 with sigma of 0.02
 C39-C48 \\sim C48-C77 \\sim C39-C77
 with sigma of 0.02
 C65-C31 \\sim C33-C31 \\sim C67-C31
 with sigma of 0.02
 C65-C33 \\sim C33-C67 \\sim C65-C67
 with sigma of 0.02
 C30-C15 \\sim C81-C15 \\sim C37-C15
 with sigma of 0.02
 C30-C37 \\sim C37-C81 \\sim C30-C81
 with sigma of 0.02
 C98-C25 \\sim C25-C11 \\sim C29-C25
 with sigma of 0.02
 C11-C98 \\sim C98-C29 \\sim C11-C29
 with sigma of 0.02
 C16-C12 \\sim C80-C16 \\sim C22-C16
 with sigma of 0.02
 C12-C80 \\sim C80-C22 \\sim C12-C22
 with sigma of 0.02
 C95-C59 \\sim C95-C61 \\sim C95-C45
 with sigma of 0.02
 C59-C61 \\sim C61-C45 \\sim C59-C45
 with sigma of 0.02
 C20-C14 \\sim C82-C14 \\sim C7-C14
 with sigma of 0.02
 C82-C20 \\sim C20-C7 \\sim C82-C7
 with sigma of 0.02
 Si1-C108 \\sim Si26-C38 \\sim Si2-C47 \\sim Si27-C56 \\sim Si12-C60 \\sim
Si5-C104 \\sim Si15-C4
 with sigma of 0.02
 C5-C108 \\sim C63-C5 \\sim C5-C2
 with sigma of 0.02
 C108-C63 \\sim C63-C2 \\sim C108-C2
 with sigma of 0.02
 C44-C38 \\sim C55-C44 \\sim C44-C111
 with sigma of 0.02
 C38-C55 \\sim C55-C111 \\sim C38-C111
 with sigma of 0.02
 C87-C47 \\sim C87-C101 \\sim C87-C107
 with sigma of 0.02
 C101-C47 \\sim C47-C107 \\sim C101-C107
 with sigma of 0.02
 C66-C60 \\sim C66-C109 \\sim C66-C64
 with sigma of 0.02
 C60-C109 \\sim C109-C64 \\sim C60-C64
 with sigma of 0.02
 C56-C102 \\sim C72-C102 \\sim C70-C102
 with sigma of 0.02
 C72-C56 \\sim C56-C70 \\sim C72-C70
 with sigma of 0.02
 C94-C104 \\sim C94-C83 \\sim C94-C92
 with sigma of 0.02
 C104-C83 \\sim C83-C92 \\sim C104-C92
 with sigma of 0.02
 C93-C4 \\sim C93-C89 \\sim C93-C49
 with sigma of 0.02
 C4-C89 \\sim C89-C49 \\sim C4-C49
 with sigma of 0.02
 Si11-C46 \\sim Si21-C42 \\sim Si17-C110 \\sim Si25-C57 \\sim Si23-C18 \\sim
Si3-C103 \\sim Si8-C32
 with sigma of 0.02
 C42-C10 \\sim C52-C10 \\sim C62-C10
 with sigma of 0.02
 C52-C42 \\sim C42-C62 \\sim C52-C62
 with sigma of 0.02
 C54-C46 \\sim C54-C27 \\sim C78-C54
 with sigma of 0.02
 C27-C46 \\sim C46-C78 \\sim C27-C78
 with sigma of 0.02
 C57-C112 \\sim C53-C112 \\sim C112-C105
 with sigma of 0.02
 C57-C53 \\sim C53-C105 \\sim C57-C105
 with sigma of 0.02
 C84-C110 \\sim C84-C106 \\sim C91-C84
 with sigma of 0.02
 C110-C106 \\sim C106-C91 \\sim C110-C91
 with sigma of 0.02
 C19-C18 \\sim C75-C19 \\sim C3-C19
 with sigma of 0.02
 C18-C3 \\sim C3-C75 \\sim C18-C75
 with sigma of 0.02
 C51-C103 \\sim C99-C51 \\sim C97-C51
 with sigma of 0.02
 C103-C99 \\sim C99-C97 \\sim C103-C97
 with sigma of 0.02
 C71-C32 \\sim C71-C68 \\sim C76-C71
 with sigma of 0.02
 C32-C68 \\sim C68-C76 \\sim C32-C76
 with sigma of 0.02
 Si19-C34 \\sim Si4-C26 \\sim Si18-C6 \\sim Si14-C1 \\sim Si9-C100 \\sim
Si16-C8 \\sim Si10-C50
 with sigma of 0.02
 C26-C24 \\sim C28-C24 \\sim C24-C23
 with sigma of 0.02
 C26-C28 \\sim C28-C23 \\sim C26-C23
 with sigma of 0.02
 C86-C6 \\sim C86-C43 \\sim C96-C86
 with sigma of 0.02
 C6-C43 \\sim C43-C96 \\sim C6-C96
 with sigma of 0.02
 C34-C21 \\sim C9-C21 \\sim C41-C21
 with sigma of 0.02
 C34-C41 \\sim C41-C9 \\sim C34-C9
 with sigma of 0.02
 C69-C1 \\sim C69-C17 \\sim C69-C35
 with sigma of 0.02
 C1-C17 \\sim C17-C35 \\sim C1-C35
 with sigma of 0.02
 C79-C100 \\sim C90-C79 \\sim C88-C79
 with sigma of 0.02
 C100-C90 \\sim C90-C88 \\sim C100-C88
 with sigma of 0.02
 C73-C50 \\sim C85-C73 \\sim C73-C13
 with sigma of 0.02
 C50-C85 \\sim C85-C13 \\sim C50-C13
 with sigma of 0.02
 C8-C40 \\sim C74-C40 \\sim C40-C36
 with sigma of 0.02
 C8-C74 \\sim C74-C36 \\sim C8-C36
 with sigma of 0.02
3. 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 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(C104) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C92)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C98) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C109) = Uanis(C64)
Uanis(C12) = Uanis(C20)
4. 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
;
_shelx_res_checksum              54054
_shelx_hkl_checksum              93193
_shelx_fab_checksum              70670
_platon_squeeze_special_details
;
A solvent mask was calculated and 2252 electrons were 
found in a volume of 9232\%A^3^ in 11 voids per unit cell. 
This is consistent with the presence of 
2.5[C6H14], 0.5[], 0.5[], 3[C6H14], 0.75[], 0.25[], 0.25[], 0.25[], 0.5[], 0.5[], 0.5[] per Asymmetric Unit 
which account for 2200 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 3.115
_oxdiff_exptl_absorpt_empirical_full_min 0.516
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2