#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/78/2217893.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2217893
loop_
_publ_author_name
'Leyva Bailen, Patricia'
'Powell, Anthony V.'
'Vaqueiro, Paz'
_publ_section_title
;
 Bis(tetraphenylphosphonium) tetrasulfidotungstate(VI)
;
_journal_coeditor_code           CS2070
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m574
_journal_paper_doi               10.1107/S1600536808007472
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C24 H20 P)2 [W S4]'
_chemical_formula_moiety         '2(C24 H20 P +), S4 W 2-'
_chemical_formula_sum            'C48 H40 P2 S4 W'
_chemical_formula_weight         990.86
_chemical_name_systematic
;
Bis(tetraphenylphosphonium) tetrasulfidotungstate
;
_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
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 91.242(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1069(4)
_cell_length_b                   19.4557(6)
_cell_length_c                   20.2373(6)
_cell_measurement_reflns_used    6646
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.5077
_cell_measurement_theta_min      2.0131
_cell_volume                     4372.1(2)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker--Nonius APEXII CCD area-detector diffractometer
;
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26702
_diffrn_reflns_theta_full        30.508
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  0.4141
_exptl_absorpt_correction_T_min  0.3514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.47
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.002621
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial,
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting
 W = [weight] * [1-(deltaF/6*sigmaF)²]²
 Ai are:
 2.09 -0.539 1.80
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0377
_refine_ls_wR_factor_gt          0.0312
_refine_ls_wR_factor_ref         0.0312
_reflns_number_gt                4008
_reflns_number_total             6646
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            cs2070.cif
_cod_data_source_block           I
_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 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2217893
_cod_database_fobs_code          2217893
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_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
W W1 0.0000 0.543792(10) 0.7500 0.0336 Uani 1.0000
S S2 0.10243(10) 0.60787(6) 0.82067(6) 0.0600 Uani 1.0000
S S3 0.12468(8) 0.47920(5) 0.69500(5) 0.0484 Uani 1.0000
P P4 0.40710(8) 0.63367(4) 0.57674(4) 0.0388 Uani 1.0000
C C5 0.3781(3) 0.70067(18) 0.63526(17) 0.0437 Uani 1.0000
C C6 0.3089(5) 0.6844(2) 0.6898(2) 0.0563 Uani 1.0000
C C7 0.2841(6) 0.7352(3) 0.7362(2) 0.0707 Uani 1.0000
C C8 0.3290(5) 0.8004(2) 0.7288(2) 0.0686 Uani 1.0000
C C9 0.3984(5) 0.8169(2) 0.6756(3) 0.0689 Uani 1.0000
C C10 0.4229(4) 0.7669(2) 0.6283(2) 0.0573 Uani 1.0000
C C11 0.5148(4) 0.66260(19) 0.5171(2) 0.0487 Uani 1.0000
C C12 0.4796(5) 0.7113(2) 0.4705(2) 0.0628 Uani 1.0000
C C13 0.5591(6) 0.7353(3) 0.4247(3) 0.0736 Uani 1.0000
C C14 0.6755(6) 0.7104(3) 0.4251(2) 0.0784 Uani 1.0000
C C15 0.7125(4) 0.6610(3) 0.4694(3) 0.0736 Uani 1.0000
C C16 0.6318(4) 0.6367(3) 0.5169(2) 0.0587 Uani 1.0000
C C17 0.4672(3) 0.56172(17) 0.62141(17) 0.0385 Uani 1.0000
C C18 0.5678(4) 0.5713(2) 0.6630(2) 0.0510 Uani 1.0000
C C19 0.6220(4) 0.5167(3) 0.6945(2) 0.0565 Uani 1.0000
C C20 0.5746(4) 0.4515(3) 0.68513(19) 0.0595 Uani 1.0000
C C21 0.4726(4) 0.44106(19) 0.6465(2) 0.0550 Uani 1.0000
C C22 0.4181(3) 0.49626(19) 0.61360(18) 0.0445 Uani 1.0000
C C23 0.2728(3) 0.60850(18) 0.53184(17) 0.0396 Uani 1.0000
C C24 0.2857(4) 0.5749(2) 0.4718(2) 0.0528 Uani 1.0000
C C25 0.1833(4) 0.5528(2) 0.43687(19) 0.0583 Uani 1.0000
C C26 0.0705(4) 0.5641(2) 0.4617(2) 0.0538 Uani 1.0000
C C27 0.0588(4) 0.5965(2) 0.5217(2) 0.0542 Uani 1.0000
C C28 0.1588(3) 0.6183(2) 0.55694(18) 0.0471 Uani 1.0000
H H61 0.2773 0.6368 0.6957 0.0679 Uiso 1.0000
H H71 0.2337 0.7241 0.7750 0.0853 Uiso 1.0000
H H81 0.3108 0.8363 0.7624 0.0823 Uiso 1.0000
H H91 0.4312 0.8644 0.6708 0.0827 Uiso 1.0000
H H101 0.4725 0.7788 0.5893 0.0687 Uiso 1.0000
H H121 0.3955 0.7294 0.4702 0.0758 Uiso 1.0000
H H131 0.5329 0.7706 0.3915 0.0887 Uiso 1.0000
H H141 0.7338 0.7287 0.3926 0.0950 Uiso 1.0000
H H151 0.7961 0.6423 0.4681 0.0883 Uiso 1.0000
H H161 0.6583 0.6014 0.5500 0.0706 Uiso 1.0000
H H181 0.6007 0.6186 0.6700 0.0612 Uiso 1.0000
H H191 0.6946 0.5237 0.7237 0.0677 Uiso 1.0000
H H201 0.6152 0.4114 0.7068 0.0719 Uiso 1.0000
H H211 0.4376 0.3940 0.6421 0.0663 Uiso 1.0000
H H221 0.3450 0.4889 0.5848 0.0533 Uiso 1.0000
H H241 0.3675 0.5666 0.4538 0.0636 Uiso 1.0000
H H251 0.1918 0.5287 0.3936 0.0699 Uiso 1.0000
H H261 -0.0027 0.5489 0.4362 0.0647 Uiso 1.0000
H H271 -0.0231 0.6043 0.5398 0.0652 Uiso 1.0000
H H281 0.1494 0.6412 0.6007 0.0565 Uiso 1.0000
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 'International Tables Vol C 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 W1 S3 5_556 5_556 109.40(4) yes
S2 W1 S2 5_556 . 110.82(7) yes
S3 W1 S2 5_556 . 108.59(4) yes
S2 W1 S3 5_556 . 108.59(4) yes
S3 W1 S3 5_556 . 110.02(6) yes
S2 W1 S3 . . 109.40(4) yes
C5 P4 C11 . . 110.19(17) no
C5 P4 C17 . . 107.77(16) no
C11 P4 C17 . . 109.65(17) no
C5 P4 C23 . . 111.88(17) no
C11 P4 C23 . . 107.53(18) no
C17 P4 C23 . . 109.81(16) no
P4 C5 C6 . . 117.8(3) no
P4 C5 C10 . . 122.5(3) no
C6 C5 C10 . . 119.7(4) no
C5 C6 C7 . . 119.5(4) no
C5 C6 H61 . . 120.3 no
C7 C6 H61 . . 120.2 no
C6 C7 C8 . . 120.2(4) no
C6 C7 H71 . . 120.0 no
C8 C7 H71 . . 119.8 no
C7 C8 C9 . . 120.8(4) no
C7 C8 H81 . . 119.6 no
C9 C8 H81 . . 119.7 no
C8 C9 C10 . . 119.7(4) no
C8 C9 H91 . . 120.1 no
C10 C9 H91 . . 120.2 no
C9 C10 C5 . . 120.1(4) no
C9 C10 H101 . . 119.9 no
C5 C10 H101 . . 120.0 no
P4 C11 C12 . . 119.1(3) no
P4 C11 C16 . . 121.3(3) no
C12 C11 C16 . . 119.5(4) no
C11 C12 C13 . . 121.0(5) no
C11 C12 H121 . . 119.6 no
C13 C12 H121 . . 119.5 no
C12 C13 C14 . . 119.4(5) no
C12 C13 H131 . . 120.3 no
C14 C13 H131 . . 120.3 no
C13 C14 C15 . . 121.2(4) no
C13 C14 H141 . . 119.4 no
C15 C14 H141 . . 119.4 no
C14 C15 C16 . . 119.6(5) no
C14 C15 H151 . . 120.2 no
C16 C15 H151 . . 120.2 no
C15 C16 C11 . . 119.2(4) no
C15 C16 H161 . . 120.4 no
C11 C16 H161 . . 120.4 no
P4 C17 C18 . . 119.1(3) no
P4 C17 C22 . . 121.2(3) no
C18 C17 C22 . . 119.7(3) no
C17 C18 C19 . . 121.0(4) no
C17 C18 H181 . . 119.6 no
C19 C18 H181 . . 119.5 no
C18 C19 C20 . . 119.0(4) no
C18 C19 H191 . . 120.6 no
C20 C19 H191 . . 120.4 no
C19 C20 C21 . . 121.2(4) no
C19 C20 H201 . . 119.3 no
C21 C20 H201 . . 119.5 no
C20 C21 C22 . . 120.0(4) no
C20 C21 H211 . . 120.0 no
C22 C21 H211 . . 120.0 no
C21 C22 C17 . . 119.0(4) no
C21 C22 H221 . . 120.4 no
C17 C22 H221 . . 120.6 no
P4 C23 C24 . . 118.0(3) no
P4 C23 C28 . . 122.1(3) no
C24 C23 C28 . . 119.8(3) no
C23 C24 C25 . . 119.3(4) no
C23 C24 H241 . . 120.3 no
C25 C24 H241 . . 120.3 no
C24 C25 C26 . . 120.3(4) no
C24 C25 H251 . . 119.8 no
C26 C25 H251 . . 119.9 no
C25 C26 C27 . . 119.9(4) no
C25 C26 H261 . . 120.0 no
C27 C26 H261 . . 120.0 no
C26 C27 C28 . . 120.5(4) no
C26 C27 H271 . . 119.7 no
C28 C27 H271 . . 119.8 no
C23 C28 C27 . . 120.1(3) no
C23 C28 H281 . . 120.0 no
C27 C28 H281 . . 119.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 S2 5_556 2.1962(10) yes
W1 S3 5_556 2.1915(9) yes
W1 S2 . 2.1962(10) yes
W1 S3 . 2.1915(9) yes
P4 C5 . 1.795(4) no
P4 C11 . 1.807(4) no
P4 C17 . 1.788(3) no
P4 C23 . 1.797(4) no
C5 C6 . 1.395(5) no
C5 C10 . 1.390(5) no
C6 C7 . 1.394(6) no
C6 H61 . 0.998 no
C7 C8 . 1.374(7) no
C7 H71 . 0.997 no
C8 C9 . 1.376(8) no
C8 H81 . 0.998 no
C9 C10 . 1.394(7) no
C9 H91 . 0.999 no
C10 H101 . 0.999 no
C11 C12 . 1.388(6) no
C11 C16 . 1.394(6) no
C12 C13 . 1.375(7) no
C12 H121 . 0.999 no
C13 C14 . 1.380(9) no
C13 H131 . 0.999 no
C14 C15 . 1.371(9) no
C14 H141 . 0.999 no
C15 C16 . 1.409(6) no
C15 H151 . 0.998 no
C16 H161 . 0.999 no
C17 C18 . 1.396(5) no
C17 C22 . 1.393(5) no
C18 C19 . 1.371(6) no
C18 H181 . 0.999 no
C19 C20 . 1.384(7) no
C19 H191 . 0.999 no
C20 C21 . 1.378(7) no
C20 H201 . 0.998 no
C21 C22 . 1.395(6) no
C21 H211 . 0.999 no
C22 H221 . 0.999 no
C23 C24 . 1.390(5) no
C23 C28 . 1.388(5) no
C24 C25 . 1.393(6) no
C24 H241 . 0.999 no
C25 C26 . 1.378(6) no
C25 H251 . 1.000 no
C26 C27 . 1.377(6) no
C26 H261 . 0.998 no
C27 C28 . 1.374(6) no
C27 H271 . 0.999 no
C28 H281 . 0.999 no
