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_7132387
_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         'C102 H225 N2 O42 Si21 U3, 1.25[C6H14]'
_chemical_formula_sum            'C102 H225 N2 O42 Si21 U3'
_chemical_formula_weight         3455.81
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                98.4318(18)
_cell_angle_beta                 90.6353(18)
_cell_angle_gamma                110.969(2)
_cell_formula_units_Z            2
_cell_length_a                   18.0726(4)
_cell_length_b                   19.3200(4)
_cell_length_c                   25.3604(5)
_cell_measurement_reflns_used    25036
_cell_measurement_temperature    139.98(11)
_cell_measurement_theta_max      72.5200
_cell_measurement_theta_min      2.8090
_cell_volume                     8159.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      139.98(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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   -115.00 -32.00   1.00    2.50    --  -43.01 -52.00 -93.00   83
  2  \w    -70.00  28.00   1.00    2.50    --  -43.01  52.00  52.00   98
  3  \w     -4.00  21.00   1.00    2.50    --   43.01 -52.00 -93.00   25
  4  \w     54.00 110.00   1.00    2.50    --   43.01  52.00  52.00   56
  5  \w     90.00 173.00   1.00   10.00    --  103.80  52.00  52.00   83
  6  \w     43.00 128.00   1.00   10.00    --  103.80 -52.00 -93.00   85
  7  \w    -86.00  -9.00   1.00    2.50    --  -43.01 125.00 120.00   77
  8  \w    -23.00   2.00   1.00    2.50    --   43.01 -37.00  90.00   25
  9  \w     60.00  87.00   1.00    2.50    --   43.01-125.00-180.00   27
 10  \w     18.00  64.00   1.00    2.50    --   43.01 -37.00  90.00   46
 11  \w     62.00 106.00   1.00   10.00    --  103.80 178.00-180.00   44
 12  \w     62.00 134.00   1.00   10.00    --  103.80 178.00 -60.00   72
 13  \w    119.00 171.00   1.00   10.00    --  103.80 111.00   0.00   52
 14  \w    106.00 132.00   1.00   10.00    --  103.80  77.00   0.00   26
 15  \w     67.00 107.00   1.00   10.00    --  103.80-102.00 -24.94   40
 16  \w     61.00  86.00   1.00   10.00    --  103.80-111.00  30.00   25
 17  \w    107.00 170.00   1.00   10.00    --  103.80  77.00 -90.00   63
 18  \w     48.00 108.00   1.00   10.00    --  103.80-105.00  79.63   60
 19  \w     60.00 127.00   1.00   10.00    --  103.80-144.00 -22.90   67
 20  \w     31.00  57.00   1.00   10.00    --  103.80-111.00  30.00   26
 21  \w     51.00 108.00   1.00   10.00    --  103.80-111.00-180.00   57
 22  \w     76.00 177.00   1.00   10.00    --  103.80  30.00 -30.00  101
 23  \w     88.00 124.00   1.00   10.00    --  103.80 178.00-150.00   36
 24  \w    127.00 156.00   1.00   10.00    --  103.80 111.00 -60.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0565490000
_diffrn_orient_matrix_UB_12      -0.0188880000
_diffrn_orient_matrix_UB_13      0.0363749000
_diffrn_orient_matrix_UB_21      -0.0520532000
_diffrn_orient_matrix_UB_22      -0.0840023000
_diffrn_orient_matrix_UB_23      -0.0135163000
_diffrn_orient_matrix_UB_31      0.0496586000
_diffrn_orient_matrix_UB_32      -0.0085957000
_diffrn_orient_matrix_UB_33      -0.0477847000
_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  0.0475
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67579
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.657
_diffrn_reflns_theta_min         2.804
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.314
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       prism
_exptl_crystal_F_000             3514
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.067
_refine_diff_density_max         5.045
_refine_diff_density_min         -2.632
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1573
_refine_ls_number_reflns         31473
_refine_ls_number_restraints     2719
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0965P)^2^+24.4474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22680
_reflns_number_total             31473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05390c2.cif
_cod_data_source_block           mt-045
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7132387--7132389.cif.
;
_cod_database_code               7132387
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C102 H225 N2 O42 Si21 U3'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C23-C22 = C14-C13 = C20-C18
 1.54 with sigma of 0.01
 C8-C5 \\sim C5-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C2(H2), C6(H6), C10(H10), C14(H14), C18(H18), C22(H22), C26(H26), C30(H30),
 C34(H34), C38(H38), C42(H42), C46(H46), C50(H50), C54(H54), C58(H58), C62(H62),
  C66(H66), C70(H70), C74(H74), C78(H78), C82(H82)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C9(H9A,H9B), C13(H13A,H13B), C17(H17A,H17B),
 C21(H21A,H21B), C25(H25A,H25B), C29(H29A,H29B), C33(H33A,H33B), C37(H37A,H37B),
  C41(H41A,H41B), C45(H45A,H45B), C49(H49A,H49B), C53(H53A,H53B), C57(H57A,
 H57B), C61(H61A,H61B), C65(H65A,H65B), C69(H69A,H69B), C73(H73A,H73B),
 C77(H77A,H77B), C81(H81A,H81B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
  C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,
 H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C96(H96A,H96B),
 C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B), C101(H10C,
 H10D), C102(H10E,H10F)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,
 H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C55(H55A,
 H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C76(H76A,
 H76B,H76C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25005
_shelx_hkl_checksum              795
_shelx_fab_checksum              38685
_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 2.168
_oxdiff_exptl_absorpt_empirical_full_min 0.620