[2π+2π] Cycloaddition of Isocyanates to Uranium(IV) Imido Complexes for the Synthesis of U(IV) κ(2)-Ureato Compounds.
Tatebe, Caleb J.; Zeller, Matthias; Bart, Suzanne C.; Inorganic chemistry 56 (2017) 1956–1965; doi:10.1021/acs.inorgchem.6b02547

data_4345339
_publ_section_title
;
 [2\p+2\p] Cycloaddition of Isocyanates to Uranium(IV) Imido Complexes for
 the Synthesis of U(IV) \k(2)-Ureato Compounds.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1956
_journal_page_last               1965
_journal_paper_doi               10.1021/acs.inorgchem.6b02547
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C37 H51 B2 N13 U'
_chemical_formula_weight         937.55
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                87.040(5)
_cell_angle_beta                 77.226(4)
_cell_angle_gamma                84.309(5)
_cell_formula_units_Z            2
_cell_length_a                   11.0487(6)
_cell_length_b                   13.1053(7)
_cell_length_c                   14.2827(7)
_cell_measurement_reflns_used    65073
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.907
_cell_measurement_theta_min      3.391
_cell_volume                     2006.02(19)
_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_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
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_diffrn_measured_fraction_theta_max 0.915
_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  0.1121
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            65073
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.907
_diffrn_reflns_theta_min         3.391
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    11.734
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_correction_T_min  0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         3.113
_refine_diff_density_min         -2.238
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       0.00033(12)
_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   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0955P)^2^+25.2868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.1842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6853
_reflns_number_total             7332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02547_si_007.cif
_cod_data_source_block           ct998
_cod_database_code               4345339
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.227
_shelx_estimated_absorpt_t_max   0.454
_shelx_res_checksum              33852
_shelx_hkl_checksum              44879