Synthesis and Structural Characterization of Hydrolysis Products within the Uranyl Iminodiacetate and Malate Systems
Daniel K. Unruh; Kyle Gojdas; Erin Flores; Anna Libo; Tori Z. Forbes; Inorganic Chemistry 52 (2013) 10191–10198; doi:10.1021/ic401705j

data_4335924
_publ_contact_author_address
;Department of Chemistry
W374 Chemistry Building
The University of Iowa
Iowa City, IA 52242-1294
USA
;
_publ_contact_author_fax         1-319-335-1270
_publ_contact_author_name        'Forbes, Tori M.'
_publ_contact_author_phone       1-319-384-1908
_publ_section_title
;
 Synthesis and Structural Characterization of Hydrolysis Products within
 the Uranyl Iminodiacetate and Malate Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10191
_journal_page_last               10198
_journal_paper_doi               10.1021/ic401705j
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_sum            'C12 H34 N3 Na3 O29 U3'
_chemical_formula_weight         1467.48
_space_group_IT_number           160
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-04T15:47:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   16.5975(6)
_cell_length_b                   16.5975(6)
_cell_length_c                   10.6852(5)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.37
_cell_volume                     2549.17(18)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CrystalMaker v2.5.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11457
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    14.406
_exptl_absorpt_correction_T_max  0.3572
_exptl_absorpt_correction_T_min  0.2768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.868
_exptl_crystal_description       blocky
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1148
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0088
_refine_ls_R_factor_gt           0.0088
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.023
_refine_ls_wR_factor_ref         0.023
_reflns_number_gt                1148
_reflns_number_total             1148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401705j_si_002.cif
_cod_data_source_block           final
_cod_original_sg_symbol_Hall     R3-2"
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4335924