Investigation of the Dithiolene Ligand Conformation in Analogous U(IV)/U(V) Complexes: X-ray Diffraction and Density Functional Theory Analysis of the U···(CC) Interaction
Belkhiri, Lotfi; Arliguie, Thérèse; Thuéry, Pierre; Fourmigué, Marc; Boucekkine, Abdou; Ephritikhine, Michel; Organometallics 25 (2006) 2782–; doi:10.1021/om060083d

data_4075171
_publ_section_title
;
 Investigation of the Dithiolene Ligand Conformation in Analogous
 U(IV)/U(V) Complexes:&#x00A0; X-ray Diffraction and Density Functional
 Theory Analysis of the U&#x00B7;&#x00B7;&#x00B7;(CC) Interaction
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2782
_journal_paper_doi               10.1021/om060083d
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C64 H112 Na2 O18 S8 U'
_chemical_formula_weight         1710.03
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.720(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3620(10)
_cell_length_b                   17.2660(10)
_cell_length_c                   25.3040(15)
_cell_measurement_reflns_used    13130
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.81
_cell_volume                     7582.0(8)
_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 0.931
_diffrn_measured_fraction_theta_max 0.931
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13130
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.436
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent light red'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6701
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0517P)^2^+56.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                5340
_reflns_number_total             6701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060083dsi20060126_040052.cif
_cod_data_source_block           1.2thf
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4075171