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_7003944
_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            'C50 H42 P2 S4 W'
_chemical_formula_weight         1016.87
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 129.831(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.255(3)
_cell_length_b                   10.7671(10)
_cell_length_c                   20.444(2)
_cell_measurement_reflns_used    4683
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.23
_cell_measurement_theta_min      2.14
_cell_volume                     4438.2(8)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'ccd area detector (Briker 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  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13749
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    2.897
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0265
_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/[\s2(Fo2)+(0.0204P)2+5.3230P] where P=(Fo2+2Fc2)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0512
_reflns_number_gt                4981
_reflns_number_total             5467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801531g.txt
_cod_data_source_block           c2050fin
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        4438.3(8)
_cod_original_sg_symbol_H-M      'C2/c '
_cod_database_code               7003944