# Copyright The Royal Society of Chemistry, 1998.

data_buwf4 


_publ_contact_author               'Fabrice Guyon'
_publ_contact_author_email         
'fabrice.guyon@univ-fcomte.fr'

loop_
_publ_author_name
'Jourdain, Isabelle V.; Fourmigu\'e, Marc; Guyon, Fabrice; Amaudrut, Jacques'

_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'



 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Bis
(\h^5^-tert-butylcyclopentadienyl)(4,5-disulfanyl-1,3-dithiole-2-
thionato) tungsten (V)
tetrafluoro-7,7,8,8-tetracyanoquinodimethane salt, acetonitrile
solvate  
; 
_chemical_name_common           
'[(\h^5^C~5~H~4~CMe~3~)~2~W(C~3~S~5~)][tcnqf~4~], CH~3~CN' 
_chemical_formula_moiety          'C21 H26 S5 W, C12 F4 N4, C2 H3 N' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C35 H29 F4 N5 S5 W' 
_chemical_formula_weight          939.78 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 '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' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 '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' 
 'W'  'W'  -0.8490   6.8722 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 2~1~/n' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    7.9560(13) 
_cell_length_b                    21.020(3) 
_cell_length_c                    21.722(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.390(14) 
_cell_angle_gamma                 90.00 
_cell_volume                      3610.1(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     2000 
_cell_measurement_theta_min       1.45 
_cell_measurement_theta_max       24.2 
 
_exptl_crystal_description        'parallelepipedic' 
_exptl_crystal_colour             'black' 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.09 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.729 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1856 
_exptl_absorpt_coefficient_mu     3.544 
_exptl_absorpt_correction_type    ' Multi-scan (XPREP, SHELXTL 5.04) ' 
_exptl_absorpt_correction_T_min   0.203 
_exptl_absorpt_correction_T_max   0.277 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'STOE IPDS' 
_diffrn_measurement_method        'rotation' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             22608 
_diffrn_reflns_av_R_equivalents   0.0815 
_diffrn_reflns_av_sigmaI/netI     0.0915 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -23 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          24.22 
_reflns_number_total              5715 
_reflns_number_observed           3538 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'EXPOSE (STOE)' 
_computing_cell_refinement        'CELL (STOE)' 
_computing_data_reduction         'INTEGRATE (STOE)' 
_computing_structure_solution     'SHELXTL 5.04' 
_computing_structure_refinement   'SHELXTL 5.04' 
_computing_molecular_graphics     'ORTEP (XTAL 3.4)' 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very
negative F^2^ 
 or flagged by the user for potential systematic errors. 
Weighted R-factors 
 wR and all goodnesses of fit S are based on F^2^, conventional
R-factors R 
 are based on F, with F set to zero for negative F^2^. The
observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating
_R_factor_obs etc. and is 
 not relevant to the choice of reflections for refinement. 
R-factors based 
 on F^2^ are statistically about twice as large as those based on
F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     noref 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5715 
_refine_ls_number_parameters      458 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0776 
_refine_ls_R_factor_obs           0.0360 
_refine_ls_wR_factor_all          0.0797 
_refine_ls_wR_factor_obs          0.0690 
_refine_ls_goodness_of_fit_all    0.842 
_refine_ls_goodness_of_fit_obs    0.952 
_refine_ls_restrained_S_all       0.842 
_refine_ls_restrained_S_obs       0.952 
_refine_ls_shift/esd_max          0.094 
_refine_ls_shift/esd_mean         0.001 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
W1 W 0.73821(4) 0.86487(2) 0.137895(14) 0.03446(10) Uani 1 d . . 
S1 S 0.7050(2) 0.96577(10) 0.18976(9) 0.0415(5) Uani 1 d . . 
S2 S 0.7271(3) 0.93269(11) 0.04645(9) 0.0466(5) Uani 1 d . . 
S3 S 0.8650(3) 1.09172(11) 0.16563(11) 0.0556(6) Uani 1 d . . 
S4 S 0.8733(3) 1.06416(11) 0.03536(10) 0.0543(6) Uani 1 d . . 
S5 S 0.9929(4) 1.18979(13) 0.08430(15) 0.0812(8) Uani 1 d . . 
C1 C 0.7937(8) 1.0175(4) 0.1405(4) 0.040(2) Uani 1 d . . 
C2 C 0.7981(9) 1.0042(4) 0.0789(4) 0.040(2) Uani 1 d . . 
C3 C 0.9121(10) 1.1192(4) 0.0943(4) 0.054(2) Uani 1 d . . 
C4 C 0.4479(8) 0.8671(5) 0.1545(3) 0.046(2) Uani 1 d . . 
H4 H 0.3992(8) 0.9023(5) 0.1716(3) 0.055 Uiso 1 calc R . 
C5 C 0.4537(7) 0.8558(4) 0.0905(3) 0.045(2) Uani 1 d . . 
H5 H 0.4084(7) 0.8821(4) 0.0585(3) 0.054 Uiso 1 calc R . 
C6 C 0.5409(9) 0.7970(4) 0.0830(3) 0.040(2) Uani 1 d . . 
C7 C 0.5837(9) 0.7729(4) 0.1441(4) 0.043(2) Uani 1 d . . 
H7 H 0.6394(9) 0.7347(4) 0.1540(4) 0.052 Uiso 1 calc R . 
C8 C 0.5278(10) 0.8165(4) 0.1875(4) 0.051(2) Uani 1 d . . 
H8 H 0.5420(10) 0.8120(4) 0.2304(4) 0.062 Uiso 1 calc R . 
C9 C 1.0258(8) 0.8846(4) 0.1304(4) 0.047(2) Uani 1 d . . 
H9 H 1.0586(8) 0.9188(4) 0.1074(4) 0.056 Uiso 1 calc R . 
C10 C 1.0119(8) 0.8847(4) 0.1947(4) 0.044(2) Uani 1 d . . 
H10 H 1.0364(8) 0.9192(4) 0.2209(4) 0.052 Uiso 1 calc R . 
C11 C 0.9547(8) 0.8242(4) 0.2134(3) 0.038(2) Uani 1 d . . 
C12 C 0.9400(9) 0.7847(4) 0.1586(4) 0.046(2) Uani 1 d . . 
H12 H 0.9094(9) 0.7420(4) 0.1568(4) 0.055 Uiso 1 calc R . 
C13 C 0.9809(9) 0.8228(5) 0.1072(4) 0.052(2) Uani 1 d . . 
H13 H 0.9783(9) 0.8095(5) 0.0663(4) 0.062 Uiso 1 calc R . 
C14 C 0.9546(10) 0.8026(4) 0.2792(4) 0.049(2) Uani 1 d . . 
C15 C 0.8663(12) 0.7381(4) 0.2848(4) 0.066(3) Uani 1 d . . 
H15A H 0.7473(16) 0.7428(7) 0.2724(27) 0.098 Uiso 1 calc R . 
H15B H 0.8838(66) 0.7238(14) 0.3270(7) 0.098 Uiso 1 calc R . 
H15C H 0.9127(53) 0.7075(8) 0.2586(21) 0.098 Uiso 1 calc R . 
C16 C 1.1457(12) 0.7940(6) 0.3023(5) 0.084(3) Uani 1 d . . 
H16A H 1.1574(12) 0.7775(35) 0.3438(14) 0.126 Uiso 1 calc R . 
H16B H 1.2020(22) 0.8344(8) 0.3018(34) 0.126 Uiso 1 calc R . 
H16C H 1.1956(25) 0.7648(28) 0.2756(21) 0.126 Uiso 1 calc R . 
C17 C 0.8768(13) 0.8516(5) 0.3190(4) 0.075(3) Uani 1 d . . 
H17A H 0.8831(76) 0.8365(15) 0.3609(8) 0.112 Uiso 1 calc R . 
H17B H 0.7606(26) 0.8584(24) 0.3032(19) 0.112 Uiso 1 calc R . 
H17C H 0.9377(53) 0.8910(10) 0.3180(25) 0.112 Uiso 1 calc R . 
C18 C 0.5411(10) 0.7609(4) 0.0231(4) 0.053(2) Uani 1 d . . 
C19 C 0.3809(14) 0.7195(6) 0.0177(5) 0.096(4) Uani 1 d . . 
H19A H 0.3778(55) 0.6933(30) -0.0186(22) 0.143 Uiso 1 calc R . 
H19B H 0.2827(14) 0.7464(6) 0.0146(39) 0.143 Uiso 1 calc R . 
H19C H 0.3821(53) 0.6931(29) 0.0538(19) 0.143 Uiso 1 calc R . 
C20 C 0.5336(12) 0.8049(5) -0.0330(4) 0.070(3) Uani 1 d . . 
H20A H 0.5270(82) 0.7799(5) -0.0702(4) 0.104 Uiso 1 calc R . 
H20B H 0.6334(40) 0.8309(22) -0.0301(15) 0.104 Uiso 1 calc R . 
H20C H 0.4355(46) 0.8317(21) -0.0340(17) 0.104 Uiso 1 calc R . 
C21 C 0.6955(13) 0.7183(5) 0.0221(5) 0.081(3) Uani 1 d . . 
H21A H 0.6809(43) 0.6913(25) -0.0137(19) 0.121 Uiso 1 calc R . 
H21B H 0.7084(54) 0.6925(25) 0.0589(17) 0.121 Uiso 1 calc R . 
H21C H 0.7945(19) 0.7441(5) 0.0207(34) 0.121 Uiso 1 calc R . 
C22 C 0.2195(11) 0.6277(5) 0.1421(4) 0.057(2) Uani 1 d . . 
C23 C 0.3663(11) 0.5320(5) 0.1615(5) 0.059(2) Uani 1 d . . 
C24 C 0.2632(9) 0.5686(4) 0.1169(4) 0.047(2) Uani 1 d . . 
C25 C 0.2253(8) 0.5502(4) 0.0549(4) 0.040(2) Uani 1 d . . 
C26 C 0.1128(9) 0.5850(4) 0.0113(4) 0.045(2) Uani 1 d . . 
C27 C 0.0760(10) 0.5678(4) -0.0487(4) 0.047(2) Uani 1 d . . 
C28 C 0.1461(9) 0.5137(4) -0.0758(4) 0.042(2) Uani 1 d . . 
C29 C 1.0011(12) 0.4678(5) 0.1809(4) 0.057(2) Uani 1 d . . 
C30 C 0.8380(12) 0.5629(6) 0.1610(4) 0.068(3) Uani 1 d . . 
C31 C 0.2591(10) 0.4804(4) -0.0317(4) 0.049(2) Uani 1 d . . 
C32 C 0.2932(9) 0.4968(4) 0.0274(4) 0.046(2) Uani 1 d . . 
C33 C 0.8971(11) 0.5049(5) 0.1367(4) 0.054(2) Uani 1 d . . 
F1 F 0.0335(5) 0.6360(3) 0.0323(2) 0.0626(13) Uani 1 d . . 
F2 F -0.0364(6) 0.6041(3) -0.0836(2) 0.0681(14) Uani 1 d . . 
F3 F 0.3414(6) 0.4301(2) -0.0523(2) 0.0680(14) Uani 1 d . . 
F4 F 0.4050(6) 0.4603(2) 0.0641(2) 0.0611(13) Uani 1 d . . 
N1 N 0.1945(12) 0.6745(5) 0.1657(4) 0.086(3) Uani 1 d . . 
N2 N 0.4452(11) 0.5064(4) 0.2019(4) 0.084(3) Uani 1 d . . 
N3 N 0.7983(12) 0.6102(5) 0.1815(4) 0.091(3) Uani 1 d . . 
N4 N 1.0824(12) 0.4395(5) 0.2181(4) 0.079(3) Uani 1 d . . 
N5 N 0.2708(11) 0.0069(4) 0.1041(4) 0.083(3) Uani 1 d . . 
C34 C 0.3066(11) 0.0451(5) 0.1403(5) 0.064(3) Uani 1 d . . 
C35 C 0.3512(14) 0.0927(6) 0.1872(5) 0.094(4) Uani 1 d . . 
H35A H 0.2803(69) 0.0881(24) 0.2200(18) 0.141 Uiso 1 calc R . 
H35B H 0.3353(95) 0.1343(6) 0.1693(10) 0.141 Uiso 1 calc R . 
H35C H 0.4674(32) 0.0875(24) 0.2037(27) 0.141 Uiso 1 calc R . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
W1 0.03230(14) 0.0384(2) 0.03261(15) 0.0021(2) 0.00324(10)
0.0004(2) 
S1 0.0448(11) 0.0388(12) 0.0424(11) -0.0015(10) 0.0114(9)
-0.0009(9) 
S2 0.0546(12) 0.0487(13) 0.0358(11) 0.0082(10) 0.0016(9)
-0.0057(10) 
S3 0.0595(13) 0.0457(14) 0.0625(14) -0.0011(12) 0.0106(11)
-0.0061(11) 
S4 0.0557(13) 0.0511(14) 0.0559(13) 0.0160(11) 0.0047(10)
-0.0039(10) 
S5 0.083(2) 0.053(2) 0.108(2) 0.015(2) 0.013(2) -0.0160(14) 
C1 0.036(4) 0.035(5) 0.050(5) 0.002(4) 0.003(4) -0.001(3) 
C2 0.035(4) 0.038(5) 0.048(5) 0.011(4) 0.009(3) 0.001(3) 
C3 0.051(5) 0.041(6) 0.068(6) 0.015(4) 0.005(4) 0.006(4) 
C4 0.027(3) 0.063(5) 0.048(5) -0.005(5) 0.013(3) -0.010(4) 
C5 0.015(3) 0.067(6) 0.051(5) -0.003(5) -0.012(3) -0.004(4) 
C6 0.038(4) 0.037(5) 0.043(5) -0.007(4) -0.001(3) -0.011(4) 
C7 0.046(4) 0.034(5) 0.048(5) 0.007(4) 0.002(4) -0.011(4) 
C8 0.046(5) 0.071(7) 0.039(5) 0.012(5) 0.012(4) -0.024(4) 
C9 0.010(3) 0.065(6) 0.066(6) 0.011(5) 0.009(3) -0.008(3) 
C10 0.024(4) 0.054(6) 0.049(5) 0.002(4) -0.012(3) -0.002(3) 
C11 0.022(4) 0.045(5) 0.042(5) 0.017(4) -0.018(3) 0.006(3) 
C12 0.036(4) 0.038(5) 0.061(6) 0.001(5) -0.005(4) 0.020(4) 
C13 0.031(4) 0.074(7) 0.051(5) 0.002(5) 0.011(4) 0.013(4) 
C14 0.057(5) 0.043(5) 0.045(5) 0.012(4) -0.010(4) -0.003(4) 
C15 0.084(7) 0.050(6) 0.059(6) 0.021(5) -0.009(5) -0.008(5) 
C16 0.073(7) 0.103(9) 0.070(7) 0.032(6) -0.019(5) -0.011(6) 
C17 0.104(7) 0.071(8) 0.048(5) -0.002(5) 0.009(5) -0.011(6) 
C18 0.060(5) 0.048(5) 0.047(5) -0.009(4) -0.004(4) -0.010(4) 
C19 0.105(8) 0.114(10) 0.069(7) -0.033(7) 0.013(6) -0.058(8) 
C20 0.077(6) 0.084(8) 0.048(6) -0.015(5) 0.009(5) 0.000(6) 
C21 0.098(8) 0.063(7) 0.080(7) -0.018(6) 0.002(6) 0.015(6) 
C22 0.068(5) 0.063(6) 0.041(4) 0.008(5) 0.011(4) 0.015(6) 
C23 0.059(6) 0.051(6) 0.068(6) 0.009(5) 0.015(5) -0.006(5) 
C24 0.043(5) 0.044(5) 0.054(5) 0.007(4) 0.009(4) 0.009(4) 
C25 0.029(4) 0.045(5) 0.048(5) 0.009(4) 0.009(3) 0.002(3) 
C26 0.038(4) 0.037(5) 0.060(5) 0.002(4) 0.012(4) 0.000(4) 
C27 0.045(5) 0.045(5) 0.050(5) 0.010(4) 0.004(4) 0.000(4) 
C28 0.046(4) 0.033(5) 0.052(5) 0.006(4) 0.018(4) -0.004(4) 
C29 0.067(6) 0.065(7) 0.043(5) 0.001(5) 0.023(5) 0.001(5) 
C30 0.070(6) 0.080(8) 0.056(6) -0.004(6) 0.017(5) -0.011(6) 
C31 0.047(5) 0.039(5) 0.065(6) -0.004(5) 0.021(4) 0.002(4) 
C32 0.036(4) 0.041(5) 0.063(6) 0.010(5) 0.010(4) 0.005(4) 
C33 0.054(5) 0.060(6) 0.051(5) -0.003(5) 0.018(4) -0.008(5) 
F1 0.064(3) 0.062(3) 0.061(3) -0.006(3) 0.003(2) 0.028(3) 
F2 0.073(3) 0.076(4) 0.053(3) 0.012(3) -0.001(2) 0.029(3) 
F3 0.070(3) 0.057(3) 0.077(4) -0.011(3) 0.007(3) 0.015(3) 
F4 0.056(3) 0.055(3) 0.071(3) 0.008(3) 0.000(2) 0.013(2) 
N1 0.108(7) 0.078(7) 0.070(6) -0.013(5) 0.007(5) 0.042(6) 
N2 0.083(6) 0.080(6) 0.085(6) 0.006(5) -0.013(5) 0.017(5) 
N3 0.093(6) 0.088(8) 0.091(7) -0.029(6) 0.008(5) -0.001(5) 
N4 0.093(6) 0.092(7) 0.056(5) 0.017(5) 0.024(5) 0.006(5) 
N5 0.091(6) 0.064(6) 0.086(6) 0.001(5) -0.017(5) -0.004(5) 
C34 0.057(5) 0.059(7) 0.071(7) 0.011(6) -0.010(5) -0.003(5) 
C35 0.091(8) 0.086(8) 0.099(9) -0.016(7) -0.014(7) -0.001(7) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s.
planes) 
 are estimated using the full covariance matrix.  The cell esds
are taken 
 into account individually in the estimation of esds in
distances, angles 
 and torsion angles; correlations between esds in cell parameters
are only 
 used when they are defined by crystal symmetry.  An approximate
(isotropic) 
 treatment of cell esds is used for estimating esds involving
l.s. planes. 
; 
 
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 C13 2.289(7) . ? 
W1 C7 2.303(7) . ? 
W1 C8 2.324(7) . ? 
W1 C12 2.336(7) . ? 
W1 C6 2.347(7) . ? 
W1 C9 2.349(6) . ? 
W1 C4 2.378(6) . ? 
W1 C5 2.388(6) . ? 
W1 C11 2.400(6) . ? 
W1 C10 2.416(6) . ? 
W1 S1 2.430(2) . ? 
W1 S2 2.439(2) . ? 
S1 C1 1.729(8) . ? 
S2 C2 1.727(8) . ? 
S3 C1 1.728(8) . ? 
S3 C3 1.734(9) . ? 
S4 C2 1.722(8) . ? 
S4 C3 1.727(9) . ? 
S5 C3 1.641(8) . ? 
C1 C2 1.372(10) . ? 
C4 C8 1.397(12) . ? 
C4 C5 1.417(10) . ? 
C5 C6 1.435(11) . ? 
C6 C7 1.426(10) . ? 
C6 C18 1.506(11) . ? 
C7 C8 1.421(11) . ? 
C9 C10 1.412(11) . ? 
C9 C13 1.423(12) . ? 
C10 C11 1.425(10) . ? 
C11 C12 1.444(11) . ? 
C11 C14 1.500(11) . ? 
C12 C13 1.440(11) . ? 
C14 C17 1.521(12) . ? 
C14 C15 1.537(12) . ? 
C14 C16 1.558(11) . ? 
C18 C21 1.522(12) . ? 
C18 C20 1.525(12) . ? 
C18 C19 1.538(12) . ? 
C22 N1 1.136(11) . ? 
C22 C24 1.417(13) . ? 
C23 N2 1.154(11) . ? 
C23 C24 1.423(12) . ? 
C24 C25 1.400(11) . ? 
C25 C32 1.406(11) . ? 
C25 C26 1.431(10) . ? 
C26 F1 1.349(9) . ? 
C26 C27 1.352(11) . ? 
C27 F2 1.344(8) . ? 
C27 C28 1.423(11) . ? 
C28 C33 1.386(11) 3_665 ? 
C28 C31 1.423(11) . ? 
C29 N4 1.145(11) . ? 
C29 C33 1.426(13) . ? 
C30 N3 1.148(12) . ? 
C30 C33 1.428(15) . ? 
C31 C32 1.328(11) . ? 
C31 F3 1.345(9) . ? 
C32 F4 1.363(8) . ? 
C33 C28 1.386(11) 3_665 ? 
N5 C34 1.138(12) . ? 
C34 C35 1.444(14) . ? 
 
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 
C13 W1 C7 99.6(3) . . ? 
C13 W1 C8 129.8(3) . . ? 
C7 W1 C8 35.8(3) . . ? 
C13 W1 C12 36.3(3) . . ? 
C7 W1 C12 75.1(3) . . ? 
C8 W1 C12 96.3(3) . . ? 
C13 W1 C6 99.0(3) . . ? 
C7 W1 C6 35.7(3) . . ? 
C8 W1 C6 59.6(3) . . ? 
C12 W1 C6 93.8(3) . . ? 
C13 W1 C9 35.7(3) . . ? 
C7 W1 C9 133.0(3) . . ? 
C8 W1 C9 150.1(3) . . ? 
C12 W1 C9 59.1(3) . . ? 
C6 W1 C9 132.4(3) . . ? 
C13 W1 C4 156.5(3) . . ? 
C7 W1 C4 58.3(3) . . ? 
C8 W1 C4 34.5(3) . . ? 
C12 W1 C4 130.1(3) . . ? 
C6 W1 C4 58.9(3) . . ? 
C9 W1 C4 167.8(3) . . ? 
C13 W1 C5 129.3(3) . . ? 
C7 W1 C5 58.1(3) . . ? 
C8 W1 C5 57.8(3) . . ? 
C12 W1 C5 128.6(3) . . ? 
C6 W1 C5 35.3(3) . . ? 
C9 W1 C5 150.3(3) . . ? 
C4 W1 C5 34.6(2) . . ? 
C13 W1 C11 59.8(3) . . ? 
C7 W1 C11 90.5(3) . . ? 
C8 W1 C11 91.5(3) . . ? 
C12 W1 C11 35.5(3) . . ? 
C6 W1 C11 121.3(3) . . ? 
C9 W1 C11 58.6(3) . . ? 
C4 W1 C11 122.6(3) . . ? 
C5 W1 C11 147.1(3) . . ? 
C13 W1 C10 58.3(3) . . ? 
C7 W1 C10 124.9(3) . . ? 
C8 W1 C10 119.6(3) . . ? 
C12 W1 C10 57.7(3) . . ? 
C6 W1 C10 151.4(3) . . ? 
C9 W1 C10 34.4(3) . . ? 
C4 W1 C10 139.0(3) . . ? 
C5 W1 C10 172.3(3) . . ? 
C11 W1 C10 34.4(2) . . ? 
C13 W1 S1 127.6(2) . . ? 
C7 W1 S1 128.3(2) . . ? 
C8 W1 S1 92.6(2) . . ? 
C12 W1 S1 130.4(2) . . ? 
C6 W1 S1 131.7(2) . . ? 
C9 W1 S1 92.0(2) . . ? 
C4 W1 S1 75.8(2) . . ? 
C5 W1 S1 97.1(2) . . ? 
C11 W1 S1 95.8(2) . . ? 
C10 W1 S1 75.6(2) . . ? 
C13 W1 S2 86.8(2) . . ? 
C7 W1 S2 124.6(2) . . ? 
C8 W1 S2 132.1(2) . . ? 
C12 W1 S2 122.7(2) . . ? 
C6 W1 S2 88.9(2) . . ? 
C9 W1 S2 77.8(2) . . ? 
C4 W1 S2 99.5(2) . . ? 
C5 W1 S2 75.5(2) . . ? 
C11 W1 S2 136.3(2) . . ? 
C10 W1 S2 105.3(2) . . ? 
S1 W1 S2 82.61(7) . . ? 
C1 S1 W1 100.9(3) . . ? 
C2 S2 W1 101.3(3) . . ? 
C1 S3 C3 96.6(4) . . ? 
C2 S4 C3 97.4(4) . . ? 
C2 C1 S3 116.7(6) . . ? 
C2 C1 S1 122.2(6) . . ? 
S3 C1 S1 121.0(5) . . ? 
C1 C2 S4 115.8(6) . . ? 
C1 C2 S2 122.1(6) . . ? 
S4 C2 S2 122.1(5) . . ? 
S5 C3 S4 123.2(5) . . ? 
S5 C3 S3 123.1(5) . . ? 
S4 C3 S3 113.6(5) . . ? 
C8 C4 C5 108.2(8) . . ? 
C8 C4 W1 70.6(4) . . ? 
C5 C4 W1 73.1(4) . . ? 
C4 C5 C6 109.0(7) . . ? 
C4 C5 W1 72.3(3) . . ? 
C6 C5 W1 70.8(4) . . ? 
C7 C6 C5 105.5(7) . . ? 
C7 C6 C18 127.1(7) . . ? 
C5 C6 C18 125.4(7) . . ? 
C7 C6 W1 70.5(4) . . ? 
C5 C6 W1 73.9(4) . . ? 
C18 C6 W1 132.8(5) . . ? 
C8 C7 C6 109.2(7) . . ? 
C8 C7 W1 72.9(4) . . ? 
C6 C7 W1 73.8(4) . . ? 
C4 C8 C7 108.0(7) . . ? 
C4 C8 W1 74.9(4) . . ? 
C7 C8 W1 71.3(4) . . ? 
C10 C9 C13 107.9(7) . . ? 
C10 C9 W1 75.4(4) . . ? 
C13 C9 W1 69.8(4) . . ? 
C9 C10 C11 110.0(7) . . ? 
C9 C10 W1 70.1(4) . . ? 
C11 C10 W1 72.2(4) . . ? 
C10 C11 C12 106.1(7) . . ? 
C10 C11 C14 125.2(7) . . ? 
C12 C11 C14 127.0(7) . . ? 
C10 C11 W1 73.4(4) . . ? 
C12 C11 W1 69.8(4) . . ? 
C14 C11 W1 133.0(5) . . ? 
C13 C12 C11 108.3(7) . . ? 
C13 C12 W1 70.1(4) . . ? 
C11 C12 W1 74.7(4) . . ? 
C9 C13 C12 107.6(7) . . ? 
C9 C13 W1 74.4(4) . . ? 
C12 C13 W1 73.7(4) . . ? 
C11 C14 C17 112.3(7) . . ? 
C11 C14 C15 113.1(7) . . ? 
C17 C14 C15 109.5(8) . . ? 
C11 C14 C16 103.8(7) . . ? 
C17 C14 C16 109.8(8) . . ? 
C15 C14 C16 108.1(7) . . ? 
C6 C18 C21 112.7(7) . . ? 
C6 C18 C20 112.4(7) . . ? 
C21 C18 C20 107.9(8) . . ? 
C6 C18 C19 105.6(7) . . ? 
C21 C18 C19 109.2(8) . . ? 
C20 C18 C19 108.9(8) . . ? 
N1 C22 C24 174.8(10) . . ? 
N2 C23 C24 173.3(10) . . ? 
C25 C24 C22 125.3(7) . . ? 
C25 C24 C23 123.4(8) . . ? 
C22 C24 C23 111.0(8) . . ? 
C24 C25 C32 125.3(7) . . ? 
C24 C25 C26 123.2(7) . . ? 
C32 C25 C26 111.6(7) . . ? 
F1 C26 C27 118.6(7) . . ? 
F1 C26 C25 117.6(7) . . ? 
C27 C26 C25 123.7(8) . . ? 
F2 C27 C26 116.8(7) . . ? 
F2 C27 C28 119.2(7) . . ? 
C26 C27 C28 124.0(7) . . ? 
C33 C28 C31 125.1(8) 3_665 . ? 
C33 C28 C27 123.6(8) 3_665 . ? 
C31 C28 C27 111.2(7) . . ? 
N4 C29 C33 177.4(10) . . ? 
N3 C30 C33 176.7(11) . . ? 
C32 C31 F3 118.2(8) . . ? 
C32 C31 C28 124.7(8) . . ? 
F3 C31 C28 117.1(7) . . ? 
C31 C32 F4 117.9(7) . . ? 
C31 C32 C25 124.9(7) . . ? 
F4 C32 C25 117.3(7) . . ? 
C28 C33 C30 122.4(9) 3_665 . ? 
C28 C33 C29 123.5(9) 3_665 . ? 
C30 C33 C29 114.1(8) . . ? 
N5 C34 C35 178.9(12) . . ? 
 
_refine_diff_density_max    0.542 
_refine_diff_density_min   -1.630 
_refine_diff_density_rms    0.128

# = END

data_wtcnq 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
Bis
(\h^5^-cyclopentadienyl)(5,6-dihydro-1,4-dithiine-2,3-dithiolato)
tungsten (V) tetracyanoquinodimethane salt  
; 
_chemical_name_common            
'[(\h^5^-C~5~H~5~)~2~W(dddt)][tcnq]'
_chemical_formula_moiety          'C14 H14 S4 W, C12 H4 N4' 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C26 H18 N4 S4 W' 
_chemical_formula_weight          698.53 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 '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' 
 'N'  'N'   0.0061   0.0033 
 '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' 
 'W'  'W'  -0.8490   6.8722 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'triclinic' 
_symmetry_space_group_name_H-M    'P -1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    9.5090(14) 
_cell_length_b                    10.5400(14) 
_cell_length_c                    12.385(2) 
_cell_angle_alpha                 84.310(14) 
_cell_angle_beta                  81.450(15) 
_cell_angle_gamma                 89.320(15) 
_cell_volume                      1221.4(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used     5000 
_cell_measurement_theta_min       1.45 
_cell_measurement_theta_max       24.2 
 
_exptl_crystal_description        'parallelepipedic' 
_exptl_crystal_colour             'black' 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.024 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.899 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              680 
_exptl_absorpt_coefficient_mu     5.095 
_exptl_absorpt_correction_type    'numerical (FACEIT, STOE)' 
_exptl_absorpt_correction_T_min   0.44 
_exptl_absorpt_correction_T_max   0.86 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'STOE IPDS' 
_diffrn_measurement_method        'rotation' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             3624 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0572 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.67 
_diffrn_reflns_theta_max          24.09 
_reflns_number_total              3624 
_reflns_number_observed           3084 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'EXPOSE (STOE)' 
_computing_cell_refinement        'CELL (STOE)' 
_computing_data_reduction         'INTEGRATE (STOE)' 
_computing_structure_solution     'SHELXTL 5.04' 
_computing_structure_refinement   'SHELXTL 5.04' 
_computing_molecular_graphics     'ORTEP (XTAL 3.4)' 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very
negative F^2^ 
 or flagged by the user for potential systematic errors. 
Weighted R-factors 
 wR and all goodnesses of fit S are based on F^2^, conventional
R-factors R 
 are based on F, with F set to zero for negative F^2^. The
observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating
_R_factor_obs etc. and is 
 not relevant to the choice of reflections for refinement. 
R-factors based 
 on F^2^ are statistically about twice as large as those based on
F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     'noref' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3624 
_refine_ls_number_parameters      316 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0366 
_refine_ls_R_factor_obs           0.0246 
_refine_ls_wR_factor_all          0.0552 
_refine_ls_wR_factor_obs          0.0503 
_refine_ls_goodness_of_fit_all    0.970 
_refine_ls_goodness_of_fit_obs    0.965 
_refine_ls_restrained_S_all       0.970 
_refine_ls_restrained_S_obs       0.965 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_mean         0.000 
 
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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
W1 W 0.23067(2) 0.99856(2) 0.19948(2) 0.01952(8) Uani 1 d . . 
S1 S 0.39689(14) 0.82821(13) 0.16294(12) 0.0264(3) Uani 1 d . . 
S2 S 0.1888(2) 0.96551(13) 0.01632(12) 0.0275(3) Uani 1 d . . 
S3 S 0.3665(2) 0.58493(14) 0.0810(2) 0.0473(5) Uani 1 d . . 
S4 S 0.1444(2) 0.7383(2) -0.0882(2) 0.0503(5) Uani 1 d . . 
C1 C 0.3144(5) 0.7430(5) 0.0756(5) 0.0242(13) Uani 1 d . . 
C2 C 0.2260(6) 0.8035(5) 0.0107(5) 0.0268(13) Uani 1 d . . 
C3 C 0.2487(11) 0.5953(7) -0.1080(7) 0.071(3) Uani 1 d . . 
H3A H 0.2056(11) 0.5450(7) -0.1559(7) 0.085 Uiso 1 calc R . 
H3B H 0.3434(11) 0.6194(7) -0.1444(7) 0.085 Uiso 1 calc R . 
C4 C 0.2601(10) 0.5184(6) -0.0078(7) 0.068(3) Uani 1 d . . 
H4A H 0.2999(10) 0.4366(6) -0.0256(7) 0.081 Uiso 1 calc R . 
H4B H 0.1651(10) 0.5028(6) 0.0322(7) 0.081 Uiso 1 calc R . 
C5 C 0.0525(6) 0.8441(6) 0.2484(6) 0.040(2) Uani 1 d . . 
H5 H 0.0406(6) 0.7827(6) 0.2015(6) 0.048 Uiso 1 calc R . 
C6 C 0.1364(7) 0.8323(10) 0.3301(8) 0.069(3) Uani 1 d . . 
H6 H 0.1897(7) 0.7610(10) 0.3484(8) 0.082 Uiso 1 calc R . 
C7 C 0.1288(10) 0.9414(14) 0.3798(7) 0.088(4) Uani 1 d . . 
H7 H 0.1782(10) 0.9586(14) 0.4361(7) 0.106 Uiso 1 calc R . 
C8 C 0.0343(9) 1.0237(8) 0.3320(8) 0.065(3) Uani 1 d . . 
H8 H 0.0070(9) 1.1039(8) 0.3526(8) 0.079 Uiso 1 calc R . 
C9 C -0.0121(6) 0.9642(6) 0.2479(6) 0.040(2) Uani 1 d . . 
H9 H -0.0738(6) 0.9976(6) 0.2008(6) 0.048 Uiso 1 calc R . 
C10 C 0.3164(6) 1.1650(6) 0.2815(5) 0.037(2) Uani 1 d . . 
H10 H 0.2942(6) 1.1691(6) 0.3568(5) 0.045 Uiso 1 calc R . 
C11 C 0.2384(7) 1.2204(6) 0.2041(7) 0.049(2) Uani 1 d . . 
H11 H 0.1564(7) 1.2687(6) 0.2177(7) 0.059 Uiso 1 calc R . 
C12 C 0.3054(10) 1.1905(6) 0.1013(6) 0.061(2) Uani 1 d . . 
H12 H 0.2745(10) 1.2142(6) 0.0344(6) 0.073 Uiso 1 calc R . 
C13 C 0.4264(8) 1.1192(6) 0.1166(7) 0.052(2) Uani 1 d . . 
H13 H 0.4915(8) 1.0882(6) 0.0617(7) 0.062 Uiso 1 calc R . 
C14 C 0.4324(6) 1.1025(6) 0.2306(6) 0.043(2) Uani 1 d . . 
H14 H 0.5013(6) 1.0579(6) 0.2647(6) 0.051 Uiso 1 calc R . 
C15 C 0.4197(6) 0.7215(5) 0.5034(5) 0.0238(12) Uani 1 d . . 
H15 H 0.4407(6) 0.7955(5) 0.5330(5) 0.029 Uiso 1 calc R . 
C16 C 0.5078(5) 0.6869(4) 0.4067(4) 0.0199(12) Uani 1 d . . 
C17 C 0.4690(5) 0.5744(5) 0.3642(4) 0.0214(12) Uani 1 d . . 
H17 H 0.5217(5) 0.5497(5) 0.3003(4) 0.026 Uiso 1 calc R . 
C18 C 0.3563(5) 0.5019(5) 0.4148(4) 0.0206(12) Uani 1 d . . 
H18 H 0.3353(5) 0.4279(5) 0.3852(4) 0.025 Uiso 1 calc R . 
C19 C 0.2697(6) 0.5354(5) 0.5114(5) 0.0235(12) Uani 1 d . . 
C20 C 0.3063(6) 0.6495(5) 0.5531(5) 0.0253(13) Uani 1 d . . 
H20 H 0.2515(6) 0.6754(5) 0.6157(5) 0.030 Uiso 1 calc R . 
C21 C 0.6255(5) 0.7626(5) 0.3529(5) 0.0225(12) Uani 1 d . . 
C22 C 0.7038(5) 0.7340(5) 0.2510(5) 0.0238(13) Uani 1 d . . 
C23 C 0.6599(6) 0.8773(5) 0.3933(5) 0.0250(13) Uani 1 d . . 
C24 C 0.1526(5) 0.4582(5) 0.5632(4) 0.0200(12) Uani 1 d . . 
C25 C 0.0652(6) 0.4883(5) 0.6607(5) 0.0281(13) Uani 1 d . . 
C26 C 0.1126(5) 0.3497(5) 0.5144(5) 0.0236(13) Uani 1 d . . 
N1 N 0.7630(5) 0.7119(4) 0.1671(4) 0.0313(12) Uani 1 d . . 
N2 N 0.6857(5) 0.9711(5) 0.4273(5) 0.0402(14) Uani 1 d . . 
N3 N -0.0032(6) 0.5155(5) 0.7387(5) 0.0423(14) Uani 1 d . . 
N4 N 0.0818(5) 0.2641(5) 0.4722(4) 0.0331(12) Uani 1 d . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
W1 0.01848(12) 0.02299(12) 0.01635(13) -0.00209(9) 0.00007(8)
-0.00186(8) 
S1 0.0259(8) 0.0280(7) 0.0280(9) -0.0064(7) -0.0112(6) 0.0063(6) 
S2 0.0361(8) 0.0280(7) 0.0196(8) -0.0020(6) -0.0084(6) 0.0065(6) 
S3 0.0739(13) 0.0260(8) 0.0508(12) -0.0113(8) -0.0346(10)
0.0138(8) 
S4 0.0690(12) 0.0437(9) 0.0504(12) -0.0194(9) -0.0396(10)
0.0126(9) 
C1 0.020(3) 0.027(3) 0.025(3) -0.006(3) -0.001(2) -0.003(2) 
C2 0.030(3) 0.031(3) 0.020(3) -0.006(3) -0.005(2) 0.003(2) 
C3 0.120(8) 0.042(4) 0.064(6) -0.027(4) -0.043(5) 0.009(4) 
C4 0.118(7) 0.031(4) 0.066(6) -0.016(4) -0.045(5) -0.003(4) 
C5 0.035(4) 0.037(4) 0.042(4) -0.012(3) 0.021(3) -0.021(3) 
C6 0.028(4) 0.103(7) 0.058(6) 0.060(6) 0.006(4) -0.006(4) 
C7 0.062(6) 0.175(11) 0.024(5) -0.010(6) 0.008(4) -0.078(7) 
C8 0.052(5) 0.057(5) 0.074(6) -0.035(5) 0.053(5) -0.026(4) 
C9 0.018(3) 0.058(4) 0.041(4) 0.006(4) 0.002(3) -0.007(3) 
C10 0.038(4) 0.038(3) 0.036(4) -0.020(3) 0.004(3) -0.010(3) 
C11 0.048(4) 0.019(3) 0.082(6) -0.014(4) -0.012(4) 0.001(3) 
C12 0.128(8) 0.023(3) 0.034(5) 0.011(3) -0.031(5) -0.035(4) 
C13 0.056(5) 0.031(4) 0.058(6) -0.015(4) 0.034(4) -0.023(3) 
C14 0.026(3) 0.032(3) 0.073(6) -0.006(4) -0.018(3) -0.011(3) 
C15 0.029(3) 0.020(3) 0.025(3) -0.007(3) -0.008(2) -0.001(2) 
C16 0.024(3) 0.015(2) 0.022(3) 0.000(2) -0.011(2) 0.003(2) 
C17 0.024(3) 0.022(3) 0.019(3) -0.007(2) -0.003(2) 0.005(2) 
C18 0.025(3) 0.018(3) 0.020(3) -0.002(2) -0.008(2) 0.003(2) 
C19 0.023(3) 0.024(3) 0.024(3) -0.001(3) -0.010(2) 0.005(2) 
C20 0.027(3) 0.024(3) 0.024(3) -0.005(3) 0.000(2) 0.007(2) 
C21 0.024(3) 0.021(3) 0.024(3) -0.004(3) -0.008(2) -0.002(2) 
C22 0.018(3) 0.022(3) 0.034(4) -0.002(3) -0.012(3) 0.000(2) 
C23 0.023(3) 0.027(3) 0.024(3) -0.001(3) 0.002(2) 0.001(2) 
C24 0.018(3) 0.024(3) 0.017(3) 0.002(2) -0.002(2) -0.001(2) 
C25 0.026(3) 0.036(3) 0.024(4) -0.005(3) -0.007(3) 0.000(2) 
C26 0.017(3) 0.031(3) 0.020(3) 0.003(3) 0.002(2) 0.003(2) 
N1 0.031(3) 0.034(3) 0.028(3) -0.006(2) 0.000(2) -0.003(2) 
N2 0.038(3) 0.034(3) 0.049(4) -0.013(3) -0.001(3) -0.006(2) 
N3 0.039(3) 0.057(3) 0.031(3) -0.011(3) 0.000(3) 0.005(3) 
N4 0.037(3) 0.030(3) 0.031(3) -0.005(3) 0.002(2) -0.007(2) 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s.
planes) 
 are estimated using the full covariance matrix.  The cell esds
are taken 
 into account individually in the estimation of esds in
distances, angles 
 and torsion angles; correlations between esds in cell parameters
are only 
 used when they are defined by crystal symmetry.  An approximate
(isotropic) 
 treatment of cell esds is used for estimating esds involving
l.s. planes. 
; 
 
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 C13 2.316(6) . ? 
W1 C12 2.316(6) . ? 
W1 C14 2.320(5) . ? 
W1 C9 2.321(6) . ? 
W1 C7 2.322(8) . ? 
W1 C10 2.325(5) . ? 
W1 C8 2.327(6) . ? 
W1 C5 2.336(5) . ? 
W1 C11 2.347(6) . ? 
W1 C6 2.353(8) . ? 
W1 S1 2.4099(14) . ? 
W1 S2 2.4198(14) . ? 
S1 C1 1.748(5) . ? 
S2 C2 1.745(5) . ? 
S3 C1 1.730(5) . ? 
S3 C4 1.796(7) . ? 
S4 C2 1.743(5) . ? 
S4 C3 1.811(8) . ? 
C1 C2 1.359(8) . ? 
C3 C4 1.431(11) . ? 
C5 C6 1.375(11) . ? 
C5 C9 1.400(9) . ? 
C6 C7 1.352(13) . ? 
C7 C8 1.396(14) . ? 
C8 C9 1.394(11) . ? 
C10 C11 1.378(10) . ? 
C10 C14 1.381(9) . ? 
C11 C12 1.400(11) . ? 
C12 C13 1.393(11) . ? 
C13 C14 1.415(10) . ? 
C15 C20 1.359(8) . ? 
C15 C16 1.432(7) . ? 
C16 C17 1.418(7) . ? 
C16 C21 1.424(8) . ? 
C17 C18 1.359(7) . ? 
C18 C19 1.421(8) . ? 
C19 C24 1.421(8) . ? 
C19 C20 1.422(7) . ? 
C21 C23 1.412(7) . ? 
C21 C22 1.424(8) . ? 
C22 N1 1.150(7) . ? 
C23 N2 1.155(7) . ? 
C24 C25 1.422(8) . ? 
C24 C26 1.426(7) . ? 
C25 N3 1.142(7) . ? 
C26 N4 1.148(6) . ? 
 
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 
C13 W1 C12 35.0(3) . . ? 
C13 W1 C14 35.6(3) . . ? 
C12 W1 C14 58.5(3) . . ? 
C13 W1 C9 152.9(3) . . ? 
C12 W1 C9 117.9(3) . . ? 
C14 W1 C9 147.5(2) . . ? 
C13 W1 C7 134.7(3) . . ? 
C12 W1 C7 133.7(4) . . ? 
C14 W1 C7 99.4(3) . . ? 
C9 W1 C7 58.1(3) . . ? 
C13 W1 C10 57.9(2) . . ? 
C12 W1 C10 57.7(2) . . ? 
C14 W1 C10 34.6(2) . . ? 
C9 W1 C10 113.7(2) . . ? 
C7 W1 C10 81.0(3) . . ? 
C13 W1 C8 136.8(2) . . ? 
C12 W1 C8 112.0(3) . . ? 
C14 W1 C8 113.2(3) . . ? 
C9 W1 C8 34.9(3) . . ? 
C7 W1 C8 35.0(3) . . ? 
C10 W1 C8 81.5(2) . . ? 
C13 W1 C5 165.6(2) . . ? 
C12 W1 C5 148.3(3) . . ? 
C14 W1 C5 151.9(3) . . ? 
C9 W1 C5 35.0(2) . . ? 
C7 W1 C5 56.9(3) . . ? 
C10 W1 C5 136.1(2) . . ? 
C8 W1 C5 57.4(2) . . ? 
C13 W1 C11 58.0(2) . . ? 
C12 W1 C11 34.9(3) . . ? 
C14 W1 C11 57.9(2) . . ? 
C9 W1 C11 99.8(2) . . ? 
C7 W1 C11 99.0(4) . . ? 
C10 W1 C11 34.3(2) . . ? 
C8 W1 C11 80.4(3) . . ? 
C5 W1 C11 134.2(2) . . ? 
C13 W1 C6 148.4(3) . . ? 
C12 W1 C6 167.3(3) . . ? 
C14 W1 C6 117.8(3) . . ? 
C9 W1 C6 57.6(3) . . ? 
C7 W1 C6 33.6(3) . . ? 
C10 W1 C6 111.8(3) . . ? 
C8 W1 C6 56.9(3) . . ? 
C5 W1 C6 34.1(3) . . ? 
C11 W1 C6 132.4(3) . . ? 
C13 W1 S1 81.1(2) . . ? 
C12 W1 S1 112.6(2) . . ? 
C14 W1 S1 82.7(2) . . ? 
C9 W1 S1 122.7(2) . . ? 
C7 W1 S1 102.7(4) . . ? 
C10 W1 S1 115.1(2) . . ? 
C8 W1 S1 134.3(3) . . ? 
C5 W1 S1 88.0(2) . . ? 
C11 W1 S1 137.5(2) . . ? 
C6 W1 S1 77.6(2) . . ? 
C13 W1 S2 86.8(2) . . ? 
C12 W1 S2 77.9(2) . . ? 
C14 W1 S2 121.9(2) . . ? 
C9 W1 S2 84.9(2) . . ? 
C7 W1 S2 138.5(2) . . ? 
C10 W1 S2 135.5(2) . . ? 
C8 W1 S2 118.0(3) . . ? 
C5 W1 S2 82.2(2) . . ? 
C11 W1 S2 105.7(2) . . ? 
C6 W1 S2 112.2(3) . . ? 
S1 W1 S2 80.75(5) . . ? 
C1 S1 W1 102.2(2) . . ? 
C2 S2 W1 102.1(2) . . ? 
C1 S3 C4 102.9(3) . . ? 
C2 S4 C3 101.4(3) . . ? 
C2 C1 S3 127.9(4) . . ? 
C2 C1 S1 120.1(4) . . ? 
S3 C1 S1 112.0(3) . . ? 
C1 C2 S4 126.9(4) . . ? 
C1 C2 S2 120.8(4) . . ? 
S4 C2 S2 112.3(3) . . ? 
C4 C3 S4 113.3(6) . . ? 
C3 C4 S3 115.3(6) . . ? 
C6 C5 C9 108.4(7) . . ? 
C6 C5 W1 73.6(4) . . ? 
C9 C5 W1 71.9(3) . . ? 
C7 C6 C5 108.9(8) . . ? 
C7 C6 W1 71.9(5) . . ? 
C5 C6 W1 72.3(4) . . ? 
C6 C7 C8 108.3(7) . . ? 
C6 C7 W1 74.5(4) . . ? 
C8 C7 W1 72.7(5) . . ? 
C9 C8 C7 107.8(7) . . ? 
C9 C8 W1 72.3(4) . . ? 
C7 C8 W1 72.3(4) . . ? 
C8 C9 C5 106.5(7) . . ? 
C8 C9 W1 72.8(4) . . ? 
C5 C9 W1 73.1(3) . . ? 
C11 C10 C14 109.8(6) . . ? 
C11 C10 W1 73.7(3) . . ? 
C14 C10 W1 72.5(3) . . ? 
C10 C11 C12 107.4(6) . . ? 
C10 C11 W1 72.0(3) . . ? 
C12 C11 W1 71.4(3) . . ? 
C13 C12 C11 108.2(7) . . ? 
C13 C12 W1 72.5(4) . . ? 
C11 C12 W1 73.7(4) . . ? 
C12 C13 C14 107.6(6) . . ? 
C12 C13 W1 72.5(4) . . ? 
C14 C13 W1 72.4(3) . . ? 
C10 C14 C13 107.0(6) . . ? 
C10 C14 W1 72.9(3) . . ? 
C13 C14 W1 72.1(3) . . ? 
C20 C15 C16 122.0(4) . . ? 
C17 C16 C21 121.1(5) . . ? 
C17 C16 C15 116.4(5) . . ? 
C21 C16 C15 122.4(4) . . ? 
C18 C17 C16 121.4(5) . . ? 
C17 C18 C19 122.2(4) . . ? 
C18 C19 C24 121.3(4) . . ? 
C18 C19 C20 116.7(5) . . ? 
C24 C19 C20 122.0(5) . . ? 
C15 C20 C19 121.3(5) . . ? 
C23 C21 C16 120.7(5) . . ?
C23 C21 C22 117.0(5) . . ? 
C16 C21 C22 121.9(4) . . ? 
N1 C22 C21 177.7(6) . . ? 
N2 C23 C21 178.8(6) . . ? 
C19 C24 C25 122.6(5) . . ? 
C19 C24 C26 120.4(5) . . ? 
C25 C24 C26 116.9(4) . . ? 
N3 C25 C24 178.2(6) . . ? 
N4 C26 C24 178.0(6) . . ? 
 
_refine_diff_density_max    0.957 
_refine_diff_density_min   -1.090 
_refine_diff_density_rms    0.169