Sterically Congested Uranyl Complexes with Seven-Coordination of the UO2 Unit: the Peculiar Ligation Mode of Nitrate in [UO2(NO3)2(Rbtp)] Complexes
Jean-Claude Berthet; Pierre Thuéry; Jean-Pierre Dognon; Denis Guillaneux; Michel Ephritikhine; Inorganic Chemistry 47 (2008) 6850–6862; doi:10.1021/ic8004486

data_4305461
_publ_contact_author_address
;
      CEA/Saclay, SCM (CNRS URA 331)
      B\^at. 125
      91191 Gif-sur-Yvette
      France
;
_publ_contact_author_email       jean-claude.berthet@cea.fr
_publ_contact_author_fax         '33 1 69 08 66 40'
_publ_contact_author_name        'J. C. Berthet'
_publ_contact_author_phone       '33 01 69 08 64 36'
_publ_section_title
;
Sterically Congested Uranyl Complexes with Seven-Coordination of the
UO2 Unit: the Peculiar Ligation Mode of Nitrate in [UO2(NO3)2(Rbtp)]
Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6850
_journal_page_last               6862
_journal_paper_doi               10.1021/ic8004486
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C36 H36 F6 N16 O8 S2 U'
_chemical_formula_weight         1236.96
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 111.379(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.543(2)
_cell_length_b                   6.2642(2)
_cell_length_c                   25.3392(17)
_cell_measurement_reflns_used    132752
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.15
_cell_volume                     4662.3(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and four \w scans with 2\% steps'
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            132752
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.662
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.005
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8867
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                4908
_reflns_number_total             8867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8004486.file003_3.cif
_cod_data_source_block           3.2MeCN
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4305461