Solution and solid-state characterization of rare silyluranium(III) complexes.
Lin, Nathan J.; Zeller, Matthias; Bart, Suzanne C.; Chemical communications (Cambridge, England) 60 (2024) 3954–3957; doi:10.1039/d4cc00655k

data_7132780
_publ_section_title
;
 Solution and solid-state characterization of rare silyluranium(III)
 complexes.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3954
_journal_page_last               3957
_journal_paper_doi               10.1039/d4cc00655k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C20 H58 I2 O3 Si8 U, C16 H40 K O8'
_chemical_formula_sum            'C36 H98 I2 K O11 Si8 U'
_chemical_formula_weight         1462.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8717(5)
_cell_length_b                   15.8095(5)
_cell_length_c                   28.9025(9)
_cell_measurement_reflns_used    9865
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4090
_cell_measurement_theta_min      2.6315
_cell_volume                     6599.7(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex4 v2021.4-0 (Bruker, 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1275(H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            127091
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.247
_diffrn_reflns_theta_min         1.766
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.
(2015). J. Appl. Cryst. 48, 3-10.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.699
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         25260
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0445P)^2^+5.5493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1275
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12924
_reflns_number_total             25260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00655k2.cif
_cod_data_source_block           NL_3_99_UI3_t2_0m_a
_cod_depositor_comments
'Adding full bibliography for 7132779--7132781.cif.'
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7132780
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.964
_shelx_res_checksum              76368
_shelx_hkl_checksum              46037