C-H Bond Addition across a Transient Uranium-Nitrido Moiety and Formation of a Parent Uranium Imido Complex.
Mullane, Kimberly C.; Ryu, Ho; Cheisson, Thibault; Grant, Lauren N.; Park, Ji Young; Manor, Brian C.; Carroll, Patrick J.; Baik, Mu-Hyun; Mindiola, Daniel J.; Schelter, Eric J.; Journal of the American Chemical Society 140 (2018) 11335–11340; doi:10.1021/jacs.8b06090

data_4132763
_publ_section_title
;
 C-H Bond Addition across a Transient Uranium-Nitrido Moiety and Formation
 of a Parent Uranium Imido Complex.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11335
_journal_page_last               11340
_journal_paper_doi               10.1021/jacs.8b06090
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C56 H86 K N3 O3 P2 U, C3 H7'
_chemical_formula_sum            'C59 H93 K N3 O3 P2 U'
_chemical_formula_weight         1231.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.070(2)
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_cell_angle_gamma                98.501(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7487(5)
_cell_length_b                   13.6035(6)
_cell_length_c                   17.6124(7)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.49
_cell_volume                     2948.2(2)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker SAINT v8.34A'
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_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            104437
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.921
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/4'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.046
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13518
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0314P)^2^+6.1291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                12684
_reflns_number_total             13518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06090_si_001.cif
_cod_data_source_block           4921
_cod_database_code               4132763
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.474