Hydrothermal Synthesis of Uranyl Squarates and Squarate-Oxalates: Hydrolysis Trends and in Situ Oxalate Formation
Clare E. Rowland; Christopher L. Cahill; Inorganic Chemistry 49 (2010) 6716–6724; doi:10.1021/ic100887c

data_4316096
_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
;
 Hydrothermal Synthesis of Uranyl Squarates and Squarate-Oxalates:
 Hydrolysis Trends and in Situ Oxalate Formation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6716
_journal_page_last               6724
_journal_paper_doi               10.1021/ic100887c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C10 O12 U, 2(H2O), 3(NH4)'
_chemical_formula_sum            'C10 H16 N3 O14 U'
_chemical_formula_weight         640.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.294(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.731(17)
_cell_length_b                   7.280(8)
_cell_length_c                   15.872(16)
_cell_measurement_reflns_used    8828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5675
_cell_measurement_theta_min      2.5735
_cell_volume                     1776(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 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker Smart 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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31998
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    9.222
_exptl_absorpt_correction_T_max  0.692
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1204
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0238
_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^)+(0.0198P)^2^+7.1937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                4108
_reflns_number_total             4855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100887c_si_002_2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316096