Isolation of U(ii) compounds using strong donor ligands, C5Me4H and N(SiMe3)2, including a three-coordinate U(ii) complex
Ryan, Austin J.; Angadol, Mary A.; Ziller, Joseph W.; Evans, William J.; Chemical Communications  (2019) –; doi:10.1039/C8CC08767A

data_7122947
_publ_section_title
;
 Isolation of U(ii) compounds using strong donor ligands, C5Me4H and
 N(SiMe3)2, including a three-coordinate U(ii) complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08767A
_journal_year                    2019
_chemical_formula_sum            'C36 H90 K N5 O6 Si6 U'
_chemical_formula_weight         1134.79
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2019-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.4169(17)
_cell_length_b                   18.4169(17)
_cell_length_c                   18.1996(17)
_cell_measurement_reflns_used    7989
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.21
_cell_volume                     5346.0(9)
_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      88(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19702
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         1.698
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.468
_exptl_absorpt_correction_T_max  0.4296
_exptl_absorpt_correction_T_min  0.3334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.214
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.008(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2443
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0389P)^2^+0.5323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2317
_reflns_number_total             2443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08767a2.cif
_cod_data_source_block           ajr4
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5346.0(11)
_cod_database_code               7122947
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.447
_shelx_estimated_absorpt_t_max   0.620
_exptl_absorpt_special_details
; 
Reflections not merged 
19712 Corrected reflections written to file ajr4s.hkl 
Estimated minimum and maximum transmission:  0.3334  0.4296 
The ratio (0.7761) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              93
_shelx_fab_checksum              75406