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_4308488
_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            'C48 H80 Na4 O8 S16 U'
_chemical_formula_weight         1628.07
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_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.0956(8)
_cell_length_b                   15.9080(4)
_cell_length_c                   14.3610(4)
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_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.65
_cell_volume                     6647.0(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      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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
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_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44816
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    3.017
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.609
_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    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3296
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_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         12603
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0435
_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^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0791
_reflns_number_gt                9641
_reflns_number_total             12603
_reflns_threshold_expression     >2sigma(I)
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