#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003945.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7003945
loop_
_publ_author_name
'Hildebrand, Alexandra'
'Lönnecke, Peter'
'Silaghi-Dumitrescu, Luminita'
'Hey-Hawkins, Evamarie'
_publ_section_title
;
 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
;
_journal_issue                   34
_journal_name_full               'Dalton Transactions'
_journal_page_first              4639
_journal_paper_doi               10.1039/b801531g
_journal_year                    2008
_chemical_formula_sum            'C38 H30 Cl4 O2 P2 S4 W'
_chemical_formula_weight         1034.45
_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                91.291(1)
_cell_angle_beta                 102.895(1)
_cell_angle_gamma                110.232(1)
_cell_formula_units_Z            2
_cell_length_a                   12.1339(8)
_cell_length_b                   12.4984(8)
_cell_length_c                   13.9306(9)
_cell_measurement_reflns_used    4253
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.37
_cell_volume                     1920.8(2)
_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 0.989
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'Ω 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12323
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    3.622
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.979
_refine_diff_density_min         -1.985
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         8997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ2(Fo2)+(0.0550P)2+5.5439P] where P=(Fo2+2Fc2)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                8176
_reflns_number_total             8997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801531g.txt
_cod_data_source_block           c2147fin
_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_sg_symbol_H-M      P-1
_cod_database_code               7003945
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.787758(17) 0.640154(16) 0.719753(14) 0.01863(7) Uani 1 1 d . . .
S1 S 0.90415(12) 0.58658(11) 0.61388(9) 0.0233(2) Uani 1 1 d . . .
S2 S 0.79144(12) 0.71396(12) 0.88983(9) 0.0265(3) Uani 1 1 d . . .
S3 S 0.67399(12) 0.59407(11) 0.54065(9) 0.0256(3) Uani 1 1 d . . .
S4 S 0.59637(11) 0.68506(11) 0.71087(10) 0.0249(2) Uani 1 1 d . . .
P1 P 1.00552(12) 0.69931(11) 0.82731(9) 0.0207(2) Uani 1 1 d . . .
P2 P 0.78731(11) 0.88601(10) 0.64106(9) 0.0203(2) Uani 1 1 d . . .
O1 O 0.8570(3) 0.8092(3) 0.6822(2) 0.0199(7) Uani 1 1 d . . .
O2 O 0.7300(3) 0.5032(3) 0.7479(3) 0.0258(7) Uani 1 1 d . . .
C1 C 1.0932(5) 0.6307(4) 0.7794(4) 0.0248(10) Uani 1 1 d . . .
C2 C 1.0372(5) 0.5723(4) 0.6851(4) 0.0238(10) Uani 1 1 d . . .
C3 C 1.0959(5) 0.5122(5) 0.6425(4) 0.0300(11) Uani 1 1 d . . .
H3 H 1.0570 0.4674 0.5811 0.036 Uiso 1 1 calc R . .
C4 C 1.2107(5) 0.5187(5) 0.6906(4) 0.0332(12) Uani 1 1 d . . .
H4 H 1.2496 0.4782 0.6617 0.040 Uiso 1 1 calc R . .
C5 C 1.2693(5) 0.5842(5) 0.7811(5) 0.0331(12) Uani 1 1 d . . .
H5 H 1.3489 0.5905 0.8119 0.040 Uiso 1 1 calc R . .
C6 C 1.2108(5) 0.6405(5) 0.8263(4) 0.0302(11) Uani 1 1 d . . .
H6 H 1.2501 0.6848 0.8880 0.036 Uiso 1 1 calc R . .
C7 C 0.9997(5) 0.6664(4) 0.9513(4) 0.0237(10) Uani 1 1 d . . .
C8 C 0.9014(5) 0.6813(4) 0.9779(4) 0.0258(10) Uani 1 1 d . . .
C9 C 0.8923(5) 0.6734(5) 1.0757(4) 0.0320(12) Uani 1 1 d . . .
H9 H 0.8265 0.6836 1.0944 0.038 Uiso 1 1 calc R . .
C10 C 0.9804(6) 0.6504(5) 1.1455(4) 0.0350(13) Uani 1 1 d . . .
H10 H 0.9746 0.6465 1.2116 0.042 Uiso 1 1 calc R . .
C11 C 1.0770(6) 0.6333(5) 1.1183(4) 0.0339(12) Uani 1 1 d . . .
H11 H 1.1359 0.6170 1.1656 0.041 Uiso 1 1 calc R . .
C12 C 1.0861(5) 0.6404(5) 1.0214(4) 0.0288(11) Uani 1 1 d . . .
H12 H 1.1506 0.6276 1.0026 0.035 Uiso 1 1 calc R . .
C13 C 1.0974(5) 0.8519(4) 0.8431(4) 0.0263(10) Uani 1 1 d . . .
C14 C 1.1733(6) 0.8944(5) 0.7810(5) 0.0371(13) Uani 1 1 d . . .
H14 H 1.1725 0.8462 0.7278 0.045 Uiso 1 1 calc R . .
C15 C 1.2504(6) 1.0079(6) 0.7972(6) 0.0482(17) Uani 1 1 d . . .
H15 H 1.3026 1.0365 0.7555 0.058 Uiso 1 1 calc R . .
C16 C 1.2509(6) 1.0785(6) 0.8735(6) 0.0537(19) Uani 1 1 d . . .
H16 H 1.3040 1.1554 0.8845 0.064 Uiso 1 1 calc R . .
C17 C 1.1739(6) 1.0379(5) 0.9348(5) 0.0470(16) Uani 1 1 d . . .
H17 H 1.1740 1.0872 0.9868 0.056 Uiso 1 1 calc R . .
C18 C 1.0965(6) 0.9242(5) 0.9193(4) 0.0342(12) Uani 1 1 d . . .
H18 H 1.0436 0.8963 0.9605 0.041 Uiso 1 1 calc R . .
C19 C 0.6705(4) 0.8212(4) 0.5311(4) 0.0233(10) Uani 1 1 d . . .
C20 C 0.6315(5) 0.7060(4) 0.4906(4) 0.0243(10) Uani 1 1 d . . .
C21 C 0.5463(5) 0.6725(5) 0.3981(4) 0.0303(11) Uani 1 1 d . . .
H21 H 0.5213 0.5970 0.3683 0.036 Uiso 1 1 calc R . .
C22 C 0.4986(5) 0.7480(5) 0.3502(4) 0.0348(13) Uani 1 1 d . . .
H22 H 0.4431 0.7237 0.2880 0.042 Uiso 1 1 calc R . .
C23 C 0.5316(5) 0.8596(5) 0.3929(4) 0.0356(13) Uani 1 1 d . . .
H23 H 0.4966 0.9100 0.3614 0.043 Uiso 1 1 calc R . .
C24 C 0.6166(5) 0.8950(5) 0.4823(4) 0.0289(11) Uani 1 1 d . . .
H24 H 0.6394 0.9704 0.5115 0.035 Uiso 1 1 calc R . .
C25 C 0.7166(5) 0.9206(4) 0.7314(4) 0.0254(10) Uani 1 1 d . . .
C26 C 0.6340(5) 0.8271(5) 0.7628(4) 0.0249(10) Uani 1 1 d . . .
C27 C 0.5735(5) 0.8495(6) 0.8307(5) 0.0359(13) Uani 1 1 d . . .
H27 H 0.5192 0.7882 0.8540 0.043 Uiso 1 1 calc R . .
C28 C 0.5930(6) 0.9615(6) 0.8641(5) 0.0396(14) Uani 1 1 d . . .
H28 H 0.5490 0.9752 0.9076 0.048 Uiso 1 1 calc R . .
C29 C 0.6756(6) 1.0529(6) 0.8347(5) 0.0412(14) Uani 1 1 d . . .
H29 H 0.6898 1.1283 0.8596 0.049 Uiso 1 1 calc R . .
C30 C 0.7382(5) 1.0329(5) 0.7676(4) 0.0309(11) Uani 1 1 d . . .
H30 H 0.7946 1.0948 0.7468 0.037 Uiso 1 1 calc R . .
C31 C 0.8950(5) 1.0151(4) 0.6138(4) 0.0236(10) Uani 1 1 d . . .
C32 C 0.8897(5) 1.0488(4) 0.5186(4) 0.0269(10) Uani 1 1 d . . .
H32 H 0.8248 1.0063 0.4655 0.032 Uiso 1 1 calc R . .
C33 C 0.9803(5) 1.1452(5) 0.5029(5) 0.0341(12) Uani 1 1 d . . .
H33 H 0.9767 1.1680 0.4388 0.041 Uiso 1 1 calc R . .
C34 C 1.0764(5) 1.2086(5) 0.5807(5) 0.0336(12) Uani 1 1 d . . .
H34 H 1.1369 1.2749 0.5697 0.040 Uiso 1 1 calc R . .
C35 C 1.0827(6) 1.1734(5) 0.6748(5) 0.0375(13) Uani 1 1 d . . .
H35 H 1.1488 1.2150 0.7275 0.045 Uiso 1 1 calc R . .
C36 C 0.9926(5) 1.0778(5) 0.6917(4) 0.0311(11) Uani 1 1 d . . .
H36 H 0.9970 1.0550 0.7558 0.037 Uiso 1 1 calc R . .
Cl1 Cl 0.21680(18) 0.73512(17) 0.39578(15) 0.0547(4) Uani 1 1 d . . .
Cl2 Cl 0.3406(2) 0.81301(17) 0.60342(15) 0.0596(5) Uani 1 1 d . . .
C37 C 0.2991(7) 0.7056(6) 0.5063(5) 0.0486(17) Uani 1 1 d . . .
H37A H 0.2498 0.6328 0.5253 0.058 Uiso 1 1 calc R . .
H37B H 0.3723 0.6967 0.4946 0.058 Uiso 1 1 calc R . .
Cl3 Cl 0.4344(3) 0.4147(3) 0.8650(2) 0.0930(9) Uani 1 1 d . . .
Cl4 Cl 0.57276(18) 0.2729(2) 0.93341(16) 0.0645(5) Uani 1 1 d . . .
C38 C 0.5806(8) 0.4133(8) 0.9147(7) 0.068(2) Uani 1 1 d . . .
H38A H 0.6321 0.4437 0.8692 0.082 Uiso 1 1 calc R . .
H38B H 0.6170 0.4624 0.9779 0.082 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 W1 O1 178.89(15) . . ?
O2 W1 S1 92.06(13) . . ?
O1 W1 S1 87.72(10) . . ?
O2 W1 S2 89.77(12) . . ?
O1 W1 S2 91.02(10) . . ?
S1 W1 S2 145.91(4) . . ?
O2 W1 S3 94.57(12) . . ?
O1 W1 S3 84.34(9) . . ?
S1 W1 S3 67.83(4) . . ?
S2 W1 S3 145.90(4) . . ?
O2 W1 S4 95.91(13) . . ?
O1 W1 S4 83.61(9) . . ?
S1 W1 S4 142.12(4) . . ?
S2 W1 S4 71.26(4) . . ?
S3 W1 S4 74.65(4) . . ?
O2 W1 P1 99.64(13) . . ?
O1 W1 P1 81.34(9) . . ?
S1 W1 P1 74.33(4) . . ?
S2 W1 P1 71.80(4) . . ?
S3 W1 P1 139.90(4) . . ?
S4 W1 P1 139.64(4) . . ?
C2 S1 W1 111.81(17) . . ?
C8 S2 W1 109.09(18) . . ?
C20 S3 W1 113.76(17) . . ?
C26 S4 W1 110.39(17) . . ?
C7 P1 C1 110.7(2) . . ?
C7 P1 C13 103.7(2) . . ?
C1 P1 C13 104.4(2) . . ?
C7 P1 W1 108.72(18) . . ?
C1 P1 W1 112.48(18) . . ?
C13 P1 W1 116.44(17) . . ?
O1 P2 C19 113.4(2) . . ?
O1 P2 C25 110.0(2) . . ?
C19 P2 C25 107.2(2) . . ?
O1 P2 C31 107.4(2) . . ?
C19 P2 C31 108.9(2) . . ?
C25 P2 C31 109.9(2) . . ?
P2 O1 W1 128.4(2) . . ?
C6 C1 C2 121.0(5) . . ?
C6 C1 P1 124.8(4) . . ?
C2 C1 P1 114.1(4) . . ?
C1 C2 C3 118.7(5) . . ?
C1 C2 S1 121.1(4) . . ?
C3 C2 S1 119.8(4) . . ?
C4 C3 C2 120.0(5) . . ?
C3 C4 C5 120.7(5) . . ?
C4 C5 C6 120.1(5) . . ?
C5 C6 C1 119.2(5) . . ?
C8 C7 C12 120.1(5) . . ?
C8 C7 P1 112.2(4) . . ?
C12 C7 P1 127.3(4) . . ?
C9 C8 C7 119.3(5) . . ?
C9 C8 S2 120.1(4) . . ?
C7 C8 S2 120.5(4) . . ?
C10 C9 C8 120.1(5) . . ?
C9 C10 C11 120.4(5) . . ?
C12 C11 C10 119.7(5) . . ?
C11 C12 C7 120.2(5) . . ?
C18 C13 C14 119.7(5) . . ?
C18 C13 P1 120.7(4) . . ?
C14 C13 P1 119.5(4) . . ?
C15 C14 C13 119.9(6) . . ?
C16 C15 C14 120.2(7) . . ?
C15 C16 C17 120.5(6) . . ?
C16 C17 C18 119.7(7) . . ?
C13 C18 C17 119.9(6) . . ?
C24 C19 C20 119.3(5) . . ?
C24 C19 P2 115.2(4) . . ?
C20 C19 P2 125.5(4) . . ?
C21 C20 C19 117.6(5) . . ?
C21 C20 S3 113.7(4) . . ?
C19 C20 S3 128.6(4) . . ?
C22 C21 C20 121.6(5) . . ?
C21 C22 C23 120.8(5) . . ?
C24 C23 C22 118.7(5) . . ?
C23 C24 C19 121.8(5) . . ?
C30 C25 C26 120.8(5) . . ?
C30 C25 P2 123.2(4) . . ?
C26 C25 P2 115.9(4) . . ?
C27 C26 C25 118.2(5) . . ?
C27 C26 S4 120.0(4) . . ?
C25 C26 S4 121.6(4) . . ?
C28 C27 C26 120.5(6) . . ?
C29 C28 C27 121.1(6) . . ?
C28 C29 C30 119.5(6) . . ?
C25 C30 C29 119.8(6) . . ?
C36 C31 C32 119.6(5) . . ?
C36 C31 P2 116.9(4) . . ?
C32 C31 P2 123.3(4) . . ?
C33 C32 C31 119.7(5) . . ?
C32 C33 C34 120.7(6) . . ?
C33 C34 C35 119.4(5) . . ?
C36 C35 C34 120.5(6) . . ?
C35 C36 C31 120.1(5) . . ?
Cl2 C37 Cl1 112.7(4) . . ?
Cl4 C38 Cl3 110.0(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 O2 1.702(4) . ?
W1 O1 2.112(3) . ?
W1 S1 2.4814(12) . ?
W1 S2 2.5084(12) . ?
W1 S3 2.5121(12) . ?
W1 S4 2.5494(13) . ?
W1 P1 2.5701(13) . ?
S1 C2 1.765(5) . ?
S2 C8 1.766(5) . ?
S3 C20 1.758(5) . ?
S4 C26 1.765(5) . ?
P1 C7 1.795(5) . ?
P1 C1 1.798(5) . ?
P1 C13 1.825(5) . ?
P2 O1 1.528(3) . ?
P2 C19 1.787(5) . ?
P2 C25 1.794(5) . ?
P2 C31 1.801(5) . ?
C1 C6 1.392(7) . ?
C1 C2 1.392(7) . ?
C2 C3 1.400(7) . ?
C3 C4 1.378(8) . ?
C4 C5 1.384(9) . ?
C5 C6 1.387(8) . ?
C7 C8 1.394(7) . ?
C7 C12 1.398(7) . ?
C8 C9 1.393(7) . ?
C9 C10 1.390(8) . ?
C10 C11 1.391(9) . ?
C11 C12 1.380(8) . ?
C13 C18 1.383(8) . ?
C13 C14 1.385(8) . ?
C14 C15 1.382(9) . ?
C15 C16 1.364(11) . ?
C16 C17 1.380(11) . ?
C17 C18 1.386(9) . ?
C19 C24 1.409(7) . ?
C19 C20 1.411(7) . ?
C20 C21 1.410(7) . ?
C21 C22 1.380(8) . ?
C22 C23 1.389(9) . ?
C23 C24 1.377(8) . ?
C25 C30 1.395(7) . ?
C25 C26 1.404(7) . ?
C26 C27 1.397(8) . ?
C27 C28 1.387(9) . ?
C28 C29 1.374(9) . ?
C29 C30 1.398(8) . ?
C31 C36 1.393(7) . ?
C31 C32 1.395(7) . ?
C32 C33 1.382(8) . ?
C33 C34 1.385(9) . ?
C34 C35 1.387(9) . ?
C35 C36 1.379(8) . ?
Cl1 C37 1.760(8) . ?
Cl2 C37 1.742(8) . ?
Cl3 C38 1.761(10) . ?
Cl4 C38 1.752(10) . ?
