Sulfonate Complexes of Actinide Ions: Structural Diversity in Uranyl Complexes with 2-Sulfobenzoate
Pierre Thuéry; Inorganic Chemistry 52 (2013) 435–447; doi:10.1021/ic3022744

data_4331757
_publ_section_title
;
 Sulfonate Complexes of Actinide Ions: Structural Diversity in Uranyl
 Complexes with 2-Sulfobenzoate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              435
_journal_page_last               447
_journal_paper_doi               10.1021/ic3022744
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C41 H40 N4 O24 S3 U2'
_chemical_formula_weight         1545.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.324(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.743(4)
_cell_length_b                   32.178(2)
_cell_length_c                   14.3508(10)
_cell_measurement_reflns_used    66867
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.91
_cell_volume                     4880.6(19)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two \f and two \w scans with 2\% steps (359 frames)'
_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  0.1275
_diffrn_reflns_av_sigmaI/netI    0.1998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66867
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.847
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.431
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12563
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1916
_reflns_number_gt                6022
_reflns_number_total             12563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3022744_si_002_05.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4331757