Tungsten phosphanylarylthiolato complexes [W{PhP(2-SC6H4)2-κ3S,S′,P}2] and [W{P(2-SC6H4)3-κ4S,S′,S″,P}2]: Synthesis, structures and redox chemistry
Hildebrand, Alexandra; Lönnecke, Peter; Silaghi-Dumitrescu, Luminita; Hey-Hawkins, Evamarie; Dalton Transactions  (2008) 4639–; doi:10.1039/b801531g

data_7003948
_publ_section_title
;
 Tungsten phosphanylarylthiolato complexes
 [W{PhP(2-SC6H4)2-\k3S,S&#x2032;,P}2] and
 [W{P(2-SC6H4)3-\k4S,S&#x2032;,S&#x2033;,P}2]: Synthesis, structures
 and redox chemistry
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              4639
_journal_paper_doi               10.1039/b801531g
_journal_year                    2008
_chemical_formula_sum            'C18 H15 P S2'
_chemical_formula_weight         326.39
_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                 97.533(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7251(8)
_cell_length_b                   8.0946(8)
_cell_length_c                   26.725(3)
_cell_measurement_reflns_used    4724
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      28.61
_cell_measurement_theta_min      2.30
_cell_volume                     1656.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (L. J. Farrugia,1997)'
_computing_publication_material  'WINGX (L.J. Farrugia,1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick,1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'ccd area detector (Bruker AXS)'
_diffrn_measurement_method       \w-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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            9751
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.354
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.354
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0800
_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/[\s2(Fo2)+(0.0340P)2+1.6832P] where P=(Fo2+2Fc2)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3664
_reflns_number_total             4021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801531g.txt
_cod_data_source_block           c2061fin
_cod_original_sg_symbol_H-M      p21/n
_cod_database_code               7003948