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_7003947
_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            'C56 H40 B Cl4 F4 P3 S9 W2'
_chemical_formula_weight         1690.64
_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                72.088(12)
_cell_angle_beta                 81.358(13)
_cell_angle_gamma                74.814(12)
_cell_formula_units_Z            2
_cell_length_a                   14.2601(15)
_cell_length_b                   14.6295(15)
_cell_length_c                   15.1780(17)
_cell_measurement_reflns_used    5461
_cell_measurement_temperature    206(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      2.10
_cell_volume                     2899.3(6)
_computing_cell_refinement       'STOE IPDS software'
_computing_data_collection       'STOE IPDS software'
_computing_data_reduction        'STOE IPDS software, STOE X-RED'
_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
_diffrn_ambient_temperature      206(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Stoe IPDS area detector'
_diffrn_measurement_method       '\f 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  0.0929
_diffrn_reflns_av_sigmaI/netI    0.3006
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15937
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    4.609
_exptl_absorpt_correction_T_max  0.8858
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin rhombus '
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.762
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.636
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7890
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.636
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                3072
_reflns_number_total             7890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801531g.txt
_cod_data_source_block           s038_fin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2899.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003947