Basicity of Uranyl Oxo Ligands upon Coordination of Alkoxides
Marianne P. Wilkerson; Carol J. Burns; Harry J. Dewey; Jerod M. Martin; David E. Morris; Robert T. Paine; Brian L. Scott; Inorganic Chemistry 39 (2000) 5277–5285; doi:10.1021/ic000142u

data_4321528
_publ_section_title
;
 Basicity of Uranyl Oxo Ligands upon Coordination of Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5277
_journal_page_last               5285
_journal_paper_doi               10.1021/ic000142u
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C56 H120 O16 U4'
_chemical_formula_weight         2001.64
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.8570(6)
_cell_length_b                   17.8570(6)
_cell_length_c                   11.4489(6)
_cell_measurement_temperature    203(2)
_cell_volume                     3650.7(3)
_computing_cell_refinement       'SAINT 4.051 (Bruker, 1996)'
_computing_data_collection       'SMART 4.210 (Bruker, 1996)'
_computing_data_reduction        'SAINT 4.051 (Bruker, 1996)'
_computing_molecular_graphics    'SHELXTL 5.1 (Bruker, 1997)'
_computing_publication_material  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_refinement  'SHELXTL 5.1 (Bruker, 1997)'
_computing_structure_solution    'SHELXTL 5.1 (Bruker, 1997)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4\CCD'
_diffrn_measurement_method       '\w  and \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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1981
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    8.899
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'watermelon red'
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.472(13)
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.940
_refine_ls_goodness_of_fit_obs   0.935
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         1981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.940
_refine_ls_restrained_S_obs      0.935
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_obs          0.0198
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0435
_refine_ls_wR_factor_obs         0.0421
_reflns_number_observed          1887
_reflns_number_total             1981
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000142u_3.cif
_cod_data_source_block           C56H120O16U4
_cod_database_code               4321528