A General and Modular Synthesis of Monoimidouranium(IV) Dihalides
Robert E. Jilek; Liam P. Spencer; David L. Kuiper; Brian L. Scott; Ursula J. Williams; James M. Kikkawa; Eric J. Schelter; James M. Boncella; Inorganic Chemistry 50 (2011) 4235–4237; doi:10.1021/ic200377b

data_4325107
_publ_contact_author_address
;Materials Physics and Applications Division
Los Alamos National Laboratory
MS J514
Los Alamos, NM 87545
;
_publ_contact_author_email       boncella@lanl.gov
_publ_contact_author_name        'Dr. James M. Boncella'
_publ_contact_author_phone       505-665-0795
_publ_section_title
;
 A General and Modular Synthesis of Monoimidouranium(IV) Dihalides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4235
_journal_page_last               4237
_journal_paper_doi               10.1021/ic200377b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H66 Cl4 N2 O4 U2'
_chemical_formula_weight         1256.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.288(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.386(4)
_cell_length_b                   15.896(4)
_cell_length_c                   17.234(4)
_cell_measurement_temperature    140(1)
_cell_volume                     4462.0(19)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39602
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.529
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.2270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       needle
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.948
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8202
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                5001
_reflns_number_total             8202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200377b_si_002_2.cif
_cod_data_source_block           apx1052_2
_cod_original_cell_volume        4461.8(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4325107