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_4087131
_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 H46 Cl2 N3 O P U, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H62 Cl2 N3 O3 P U'
_chemical_formula_weight         1068.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.3236(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4818(2)
_cell_length_b                   11.9095(2)
_cell_length_c                   29.3157(5)
_cell_measurement_reflns_used    61896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.912
_cell_measurement_theta_min      2.628
_cell_volume                     4699.06(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.914
_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  0.0527
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            61896
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.912
_diffrn_reflns_theta_min         2.628
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    3.644
_exptl_absorpt_correction_T_max  0.529
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       rod
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00128(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         12433
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+2.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9692
_reflns_number_total             12433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00861_si_003.cif
_cod_data_source_block           SS1199
_cod_database_code               4087131
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.263
_shelx_estimated_absorpt_t_max   0.529
_shelx_res_checksum              30913
_shelx_hkl_checksum              37327