[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_4345340
_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 H66 B2 N14 S U'
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_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'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 95.817(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8815(5)
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_cell_length_c                   21.5167(5)
_cell_measurement_reflns_used    76391
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.066
_cell_measurement_theta_min      5.601
_cell_volume                     5317.1(3)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
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_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 0.981
_diffrn_measured_fraction_theta_max 0.975
_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  0.0943
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76391
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.066
_diffrn_reflns_theta_min         5.601
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    9.363
_exptl_absorpt_correction_T_max  0.376
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
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_exptl_crystal_description       block
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         9854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1979
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_reflns_number_gt                7903
_reflns_number_total             9854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02547_si_006.cif
_cod_data_source_block           CT997
_cod_database_code               4345340
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.159
_shelx_estimated_absorpt_t_max   0.376
_shelx_res_checksum              75579
_shelx_hkl_checksum              158