A Uranium(IV) Triamide Species with Brønsted Basic Ligand Character: Metal‒Ligand Cooperativity in the f Block
Kiernicki, John J.; Staun, Selena L.; Zeller, Matthias; Bart, Suzanne C.; Organometallics 36 (2017) 665–; doi:10.1021/acs.organomet.6b00861

data_4087130
_publ_section_title
;
 A Uranium(IV) Triamide Species with Br\/onsted Basic Ligand Character:
 Metal--Ligand Cooperativity in the f Block
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              665
_journal_paper_doi               10.1021/acs.organomet.6b00861
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C40 H61 Cl Li N3 O2 U'
_chemical_formula_sum            'C40 H61 Cl Li N3 O2 U'
_chemical_formula_weight         896.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.952(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5441(3)
_cell_length_b                   16.7176(5)
_cell_length_c                   17.3618(4)
_cell_measurement_reflns_used    27651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.751
_cell_measurement_theta_min      1.505
_cell_volume                     3925.93(17)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'Encifer (Allen et al., 2004)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27651
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.751
_diffrn_reflns_theta_min         1.505
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    4.239
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.480
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         10419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0656P)^2^+31.2320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7695
_reflns_number_total             10419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00861_si_007.cif
_cod_data_source_block           ss1190
_cod_database_code               4087130
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.226
_shelx_estimated_absorpt_t_max   0.677
_shelx_res_checksum              93623
_shelx_hkl_checksum              53988