[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_4345184
_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            'C55 H65 B2 N14 Se U'
_chemical_formula_weight         1260.82
_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                 95.8560(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8344(2)
_cell_length_b                   19.4119(3)
_cell_length_c                   21.6097(3)
_cell_measurement_reflns_used    103780
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.286
_cell_measurement_theta_min      3.842
_cell_volume                     5355.75(14)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103780
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.286
_diffrn_reflns_theta_min         3.842
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    9.709
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             2516
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.00038(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   1.246
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         10315
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0559P)^2^+53.5327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10223
_reflns_number_total             10315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02547_si_002.cif
_cod_data_source_block           ct992d-2
_cod_depositor_comments
'Adding full bibliography for 4345183--4345186.cif.'
_cod_database_code               4345184
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.324
_shelx_estimated_absorpt_t_max   0.444
_shelx_res_checksum              86133
_shelx_hkl_checksum              15537