Synthesis, X-ray crystal structures, thermal and electrochemical properties of thiosemicarbazidatodioxouranium(VI) complexes.
Sahin, Musa; Koca, Atıf; Ozdemir, Namık; Dinçer, Muharrem; Büyükgüngör, Orhan; Bal-Demirci, Tülay; Ulküseven, Bahri; Dalton transactions (Cambridge, England : 2003) 39 (2010) 10228–10237; doi:10.1039/c0dt00265h

data_7026202
_publ_section_title
;
 Synthesis, X-ray crystal structures, thermal and electrochemical
 properties of thiosemicarbazidatodioxouranium(VI) complexes.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10228
_journal_page_last               10237
_journal_paper_doi               10.1039/c0dt00265h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C27 H35 Cl2 N3 O5 S U'
_chemical_formula_sum            'C27 H35 Cl2 N3 O5 S U'
_chemical_formula_weight         822.57
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                68.857(4)
_cell_angle_beta                 86.466(4)
_cell_angle_gamma                78.133(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7379(5)
_cell_length_b                   12.8908(6)
_cell_length_c                   13.8735(8)
_cell_measurement_reflns_used    109807
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      1.57
_cell_volume                     1589.43(15)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        X-RED32
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'w scans'
_diffrn_radiation_collimation    '0.8 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35703
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.378
_exptl_absorpt_correction_T_max  0.4547
_exptl_absorpt_correction_T_min  0.0448
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED32 (Stoe & Cie, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.688
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6236
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0392P)^2^+1.0304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                5593
_reflns_number_total             6236
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0dt00265h.txt
_cod_data_source_block           muh73
_cod_original_cell_volume        1589.43(14)
_cod_database_code               7026202