Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ Ligand Synthesis versus Direct Assembly
Rowland, Clare E.; Belai, Nebebech; Knope, Karah E.; Cahill, Christopher L.; Crystal Growth & Design 10 (2010) 1390–; doi:10.1021/cg901390n

data_4502571
_publ_section_title
;
 Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds: In Situ
 Ligand Synthesis versus Direct Assembly
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1390
_journal_paper_doi               10.1021/cg901390n
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C28 H16 O12 S4 U2'
_chemical_formula_sum            'C28 H16 O12 S4 U2'
_chemical_formula_weight         1148.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.6010(10)
_cell_angle_beta                 84.4200(10)
_cell_angle_gamma                77.1690(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3354(4)
_cell_length_b                   10.9653(4)
_cell_length_c                   14.0982(5)
_cell_measurement_reflns_used    9904
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.5995
_cell_measurement_theta_min      2.3915
_cell_volume                     1550.47(10)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.918
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30641
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.32
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    10.764
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.286
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.486
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.8432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0486
_reflns_number_gt                7038
_reflns_number_total             8536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901390n_si_002.cif
_cod_data_source_block           3
_cod_database_code               4502571