[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_4345341
_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_moiety         'C42 H59 B2 N13 U, C4 H10 O'
_chemical_formula_sum            'C46 H69 B2 N13 O U'
_chemical_formula_weight         1079.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 115.484(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0622(4)
_cell_length_b                   20.1994(12)
_cell_length_c                   17.3817(9)
_cell_measurement_reflns_used    24929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.778
_cell_measurement_theta_min      2.499
_cell_volume                     5090.8(4)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect (Nonius, 1998)'
_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_full 0.998
_diffrn_measured_fraction_theta_max 0.830
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24929
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.778
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'fine focus X-ray tube'
_exptl_absorpt_coefficient_mu    3.235
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       needle
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.240
_refine_diff_density_max         2.202
_refine_diff_density_min         -2.781
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.00175(13)
_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   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6602
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0385P)^2^+66.2343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4833
_reflns_number_total             6602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02547_si_004.cif
_cod_data_source_block           cjt76_pl
_cod_database_code               4345341
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.247
_shelx_estimated_absorpt_t_max   0.511
_shelx_res_checksum              13670
_shelx_hkl_checksum              38629