UI4(1,4-dioxane)2, [UCl4(1,4-dioxane)]2, and UI3(1,4-dioxane)1.5: Stable and Versatile Starting Materials for Low- and High-Valent Uranium Chemistry
Monreal, Marisa J.; Thomson, Robert K.; Cantat, Thibault; Travia, Nicholas E.; Scott, Brian L.; Kiplinger, Jaqueline L.; Organometallics 30 (2011) 2031–; doi:10.1021/om200093q

data_4064422
_publ_section_title
;
 UI4(1,4-dioxane)2, [UCl4(1,4-dioxane)]2, and UI3(1,4-dioxane)1.5: Stable
 and Versatile Starting Materials for Low- and High-Valent Uranium
 Chemistry
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2031
_journal_paper_doi               10.1021/om200093q
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C8 H16 I4 O4 U'
_chemical_formula_weight         921.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.518(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.358(4)
_cell_length_b                   8.738(4)
_cell_length_c                   12.857(6)
_cell_measurement_temperature    140(1)
_cell_volume                     938.9(8)
_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 0.951
_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  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9937
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.220
_exptl_absorpt_correction_T_max  0.3756
_exptl_absorpt_correction_T_min  0.3114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2228
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0658P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                1769
_reflns_number_total             2228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200093q_si_001.cif
_cod_data_source_block           apx1148
_cod_original_cell_volume        938.9(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064422