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_7132781
_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         'C36 H88 I2 K O9 Si8 U, C4 H10 O'
_chemical_formula_sum            'C40 H98 I2 K O10 Si8 U'
_chemical_formula_weight         1494.83
_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_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-02-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.054(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   49.049(13)
_cell_length_b                   13.108(5)
_cell_length_c                   21.124(7)
_cell_measurement_reflns_used    9729
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4964
_cell_measurement_theta_min      2.2121
_cell_volume                     13581(8)
_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-2019/3 (Sheldrick, 2015, 2019), 
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 0.995
_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  0.1004
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            179769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.599
_diffrn_reflns_theta_min         2.491
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    3.542
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             5976
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.586
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         20794
_refine_ls_number_restraints     300
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0451P)^2^+40.3862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13797
_reflns_number_total             20794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00655k2.cif
_cod_data_source_block           NLguest3_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

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

 Adding full bibliography for 7132779--7132781.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7132781
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.484
_shelx_estimated_absorpt_t_max   0.871
_shelx_res_checksum              70590
_shelx_hkl_checksum              35268