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_4086935
_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         'C38 H51 N3 S U'
_chemical_formula_sum            'C38 H51 N3 S U'
_chemical_formula_weight         819.90
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   9.3331(2)
_cell_length_b                   16.9164(3)
_cell_length_c                   22.2563(3)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.110
_cell_measurement_theta_min      3.972
_cell_volume                     3513.88(11)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.110
_diffrn_reflns_theta_min         3.972
_diffrn_source                   'microfocus X-ray tube'
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_exptl_absorpt_correction_T_max  0.169
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
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_exptl_crystal_description       block
_exptl_crystal_F_000             1632
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_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.726
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.030(8)
_refine_ls_extinction_coef       0.00023(3)
_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   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6807
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0236P)^2^+9.8555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6801
_reflns_number_total             6807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00861_si_005.cif
_cod_data_source_block           jk1017
_cod_depositor_comments
'Adding full bibliography for 4086932--4086937.cif.'
_cod_database_code               4086935
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.073
_shelx_estimated_absorpt_t_max   0.169
_shelx_res_checksum              76008
_shelx_hkl_checksum              22449