Polynuclear Cation-Cation Complexes of Pentavalent Uranyl: Relating Stability and Magnetic Properties to Structure
Grégory Nocton; Pawel Horeglad; Jacques Pécaut; Marinella Mazzanti; Journal of the American Chemical Society 130 (2008) 16633–16645; doi:10.1021/ja804766r

data_4108789
_publ_contact_author
;
      Dr Marinella Mazzanti
      LCIB (UMR-E 3 CEA-UJF)
      DRFMC, CEA Grenoble
      17, rue des Martyrs
      38054 Grenoble cedex 9
;
_publ_section_title
;
 Polynuclear Cation-Cation Complexes of Pentavalent Uranyl: Relating
 Stability and Magnetic Properties to Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16633
_journal_page_last               16645
_journal_paper_doi               10.1021/ja804766r
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C138 H115 K4 N9 O24 U4'
_chemical_formula_weight         3391.91
_chemical_name_systematic
; 
 ? 
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.202(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.537(17)
_cell_length_b                   14.227(8)
_cell_length_c                   31.856(18)
_cell_measurement_reflns_used    971
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.41
_cell_volume                     13576(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28159
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             6568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.295
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         10701
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0528P)^2^+1137.1892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                8866
_reflns_number_total             10701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804766r_si_001_1.cif
_cod_data_source_block           3
_cod_database_code               4108789