Preparation and Isolation of Dithiolene Thiophosphoryl Molecules as Stable, Protected Forms of Dithiolene Ligands
Kuppuswamy Arumugam; James E. Bollinger; Mark Fink; James P. Donahue; Inorganic Chemistry 46 (2007) 3283–3288; doi:10.1021/ic0700203

data_4308057
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
Preparation and Isolation of Dithiolene Thiophosphoryl Molecules as Stable,
Protected Forms of Dithiolene Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3283
_journal_page_last               3288
_journal_paper_doi               10.1021/ic0700203
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C32 H28 O4 S'
_chemical_formula_weight         508.60
_chemical_name_common            tetra(p-anisyl)thiophene
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.476(3)
_cell_length_b                   10.329(3)
_cell_length_c                   25.685(7)
_cell_measurement_reflns_used    5579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.014
_cell_measurement_theta_min      2.291
_cell_volume                     2514.0(13)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21801
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.167
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1140P)^2^+0.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1817
_reflns_number_gt                5152
_reflns_number_total             5986
_reflns_threshold_expression     >2/s(I)
_cod_data_source_file            ic0700203si20070105_024028_4.cif
_cod_data_source_block           (H3CO-p-C6H4)4C4S_3
_cod_original_cell_volume        2514.1(12)
_cod_database_code               4308057