Homoleptic Tris(dithiolene) and Tetrakis(dithiolene) Complexes of Uranium(IV)
Mathieu Roger; Thérèse Arliguie; Pierre Thuéry; Marc Fourmigué; Michel Ephritikhine; Inorganic Chemistry 44 (2005) 594–600; doi:10.1021/ic049054q

data_4308487
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       arliguie@drecam.cea.fr
_publ_contact_author_fax         '33 (0) 1 69 08 66 40'
_publ_contact_author_name        'T. Arliguie'
_publ_contact_author_phone       '33 (0) 1 69 08 60 42'
_publ_section_title
;
Homoleptic Tris(dithiolene) and Tetrakis(dithiolene) Complexes of
Uranium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              594
_journal_page_last               600
_journal_paper_doi               10.1021/ic049054q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C90 H126 N6 Na4 O18 S24 U2'
_chemical_formula_weight         2917.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.530(4)
_cell_angle_beta                 104.101(5)
_cell_angle_gamma                102.537(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4359(5)
_cell_length_b                   16.2555(8)
_cell_length_c                   18.9962(10)
_cell_measurement_reflns_used    20231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.78
_cell_volume                     2940.2(3)
_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 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.1039
_diffrn_reflns_av_sigmaI/netI    0.1536
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            20231
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    3.253
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_correction_T_min  0.537
_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    1.648
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10294
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                6525
_reflns_number_total             10294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049054qsi20040716_091518_1.cif
_cod_data_source_block           3
_cod_database_code               4308487