Isolation of a Tetrameric Cation-Cation Complex of Pentavalent Uranyl
Fabien Burdet; Jacques Pécaut; Marinella Mazzanti; Journal of the American Chemical Society 128 (2006) 16512–16513; doi:10.1021/ja067445t

data_4111316
_publ_section_title
;
 Isolation of a Tetrameric Cation-Cation Complex of Pentavalent Uranyl
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16512
_journal_page_last               16513
_journal_paper_doi               10.1021/ja067445t
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C180 H148 I2 K6 N12 O24 U4'
_chemical_formula_weight         4303.62
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 87.800(11)
_cell_angle_gamma                77.837(14)
_cell_formula_units_Z            1
_cell_length_a                   16.674(5)
_cell_length_b                   16.969(6)
_cell_length_c                   17.087(6)
_cell_measurement_reflns_used    736
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      2.90
_cell_volume                     4208(2)
_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 0.592
_diffrn_measured_fraction_theta_max 0.592
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_theta_full        28.62
_diffrn_reflns_theta_max         28.62
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    4.424
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.662
_refine_diff_density_min         -4.366
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         12761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1940
_refine_ls_wR_factor_ref         0.2267
_reflns_number_gt                8643
_reflns_number_total             12761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067445tsi20061122_073216.cif
_cod_data_source_block           struc_{[UO2(dbm)2]4[K6py10]}.I2.Py2_(3)
_cod_database_code               4111316