Capturing Hydrolysis Products in the Solid State: Effects of pH on Uranyl Squarates under Ambient Conditions
Clare E. Rowland; Christopher L. Cahill; Inorganic Chemistry 49 (2010) 8668–8673; doi:10.1021/ic1000792

data_4316567
_publ_contact_author_address
;
Department of Chemistry
George Washington University
725 21st Street, NW
Washington, DC 20052
;
_publ_contact_author_email       cahill@gwu.edu
_publ_contact_author_fax         202-994-5873
_publ_contact_author_name        'Christopher L. Cahill'
_publ_contact_author_phone       202-994-6959
_publ_section_title
;
 Capturing Hydrolysis Products in the Solid State: Effects of pH on Uranyl
 Squarates under Ambient Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8668
_journal_page_last               8673
_journal_paper_doi               10.1021/ic1000792
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C12 H6 O32 U6, 9(H2O), 4(NH4)'
_chemical_formula_sum            'C12 H40 N4 O41 U6'
_chemical_formula_weight         2324.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6897(7)
_cell_length_b                   16.6897(7)
_cell_length_c                   16.6897(7)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.184
_cell_measurement_theta_min      2.436
_cell_volume                     4648.9(3)
_computing_cell_refinement       'ApexII software suite (Bruker AXS)'
_computing_data_collection       'SMART v5.05 (Bruker AXS)'
_computing_data_reduction        'ApexII software suite (Bruker AXS)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45874
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    20.906
_exptl_absorpt_correction_T_max  0.142
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.199
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.319
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0397P)^2^+74.2339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2253
_reflns_number_total             2302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1000792_si_002_2.cif
_cod_data_source_block           1
_cod_database_code               4316567