New Efficient Synthesis of [UI4(MeCN)4]. X-ray Crystal Structures of [UI2(MeCN)7][UI6], [UI4(py)3], and [U(dmf)9]I4
Jean-Claude Berthet; Pierre Thuéry; Michel Ephritikhine; Inorganic Chemistry 44 (2005) 1142–1146; doi:10.1021/ic048603p

data_4308551
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       ephri@drecam.cea.fr
_publ_contact_author_fax         '33 (1) 69 08 66 40'
_publ_contact_author_name        'M. Ephritikhine'
_publ_contact_author_phone       '33 (1) 69 08 64 36'
_publ_section_title
;
New Efficient Synthesis of [UI4(MeCN)4]. X-ray Crystal Structures of
[UI2(MeCN)7][UI6], [UI4(py)3], and [U(dmf)9]I4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1142
_journal_page_last               1146
_journal_paper_doi               10.1021/ic048603p
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C15 H15 I4 N3 U'
_chemical_formula_weight         982.93
_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     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.094(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3294(3)
_cell_length_b                   13.1236(5)
_cell_length_c                   15.4734(6)
_cell_measurement_reflns_used    14135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.06
_cell_volume                     2198.99(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f 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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14135
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    12.999
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_correction_T_min  0.168
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    2.969
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0255
_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^)+6.7946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                3558
_reflns_number_total             3741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048603psi20041007_101646_3.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4308551