A Bimetallic Aluminum(salen) Complex for the Synthesis of 1,3-Oxathiolane-2-thiones and 1,3-Dithiolane-2-thiones
William Clegg; Ross W. Harrington; Michael North; Pedro Villuendas; Journal of Organic Chemistry 75 (2010) 6201–6207; doi:10.1021/jo101121h

data_4025681
_publ_section_title
;
 A Bimetallic Aluminum(salen) Complex for the Synthesis of
 1,3-Oxathiolane-2-thiones and 1,3-Dithiolane-2-thiones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6201
_journal_page_last               6207
_journal_paper_doi               10.1021/jo101121h
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C7 H10 S3'
_chemical_formula_sum            'C7 H10 S3'
_chemical_formula_weight         190.33
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.759(7)
_cell_length_b                   10.142(5)
_cell_length_c                   6.664(3)
_cell_measurement_reflns_used    564
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      3.1
_cell_volume                     862.3(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Crystal Logic diffractometer and Rigaku Saturn 724+ detector'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond Light Source beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1227
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6324
_diffrn_reflns_theta_full        24.18
_diffrn_reflns_theta_max         24.18
_diffrn_reflns_theta_min         3.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         805
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0571P)^2^+0.1532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1246
_reflns_number_gt                487
_reflns_number_total             805
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo101121h_si_001_2.cif
_cod_data_source_block           mn32_compound_4i
_cod_database_code               4025681