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_4108790
_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            'C84 H92 K2 O24 U2'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 73.031(9)
_cell_angle_gamma                87.072(6)
_cell_formula_units_Z            1
_cell_length_a                   12.657(5)
_cell_length_b                   12.883(5)
_cell_length_c                   14.939(7)
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_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.70
_cell_measurement_theta_min      2.22
_cell_volume                     2095.8(15)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10007
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    4.032
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.10
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_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.528
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0356P)^2^+5.9851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                6177
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804766r_si_001_2.cif
_cod_data_source_block           4
_cod_original_cell_volume        2095.7(15)
_cod_database_code               4108790