Identification of the U(v) complex (C5Me5)2UVI(NSiMe3) in the reaction of (C5Me5)2UIIII(THF) with N3SiMe3
Wedal, Justin C.; Ziller, Joseph W.; Evans, William J.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01926D

data_7711020
_publ_section_title
;
 Identification of the U(v) complex (C5Me5)2UVI(&#xE001;NSiMe3) in the
 reaction of (C5Me5)2UIIII(THF) with N3SiMe3
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01926D
_journal_year                    2022
_chemical_formula_sum            'C23 H39 I N Si U'
_chemical_formula_weight         722.57
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-13 deposited with the CCDC.	2022-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6286(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0187(12)
_cell_length_b                   15.8538(19)
_cell_length_c                   19.991(2)
_cell_measurement_reflns_used    8089
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.44
_cell_volume                     3110.1(6)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35670
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.740
_diffrn_reflns_theta_min         1.040
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.257
_exptl_absorpt_correction_T_max  0.2594
_exptl_absorpt_correction_T_min  0.1951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1372
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.934
_refine_diff_density_min         -2.413
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         6170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0812P)^2^+35.5263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4634
_reflns_number_total             6170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01926d2.cif
_cod_data_source_block           jcw104
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3110.2(6)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7711020
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.349
_shelx_estimated_absorpt_t_max   0.709
_exptl_absorpt_special_details
; 
Reflections not merged 
35703 Corrected reflections written to file jcw104s.hkl 
Estimated minimum and maximum transmission:  0.1951  0.2594 
The ratio (0.7521) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  1.0000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              90070
_shelx_hkl_checksum              66941
_shelx_fab_checksum              70530