# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010

data_global
_journal_name_full               'New J.Chem.'

_journal_coden_Cambridge         0440
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Rainer Streubel'
_publ_contact_author_email       r.streubel@uni-bonn.de

_publ_section_title              
;
Extended pi conjugation in 2H-1,4,2-diazaphosphole complexes
;
loop_
_publ_author_name
'Rainer Streubel'
'Helten Holger'

# Attachment '- 3a.cif'

data_str010_m
_database_code_depnum_ccdc_archive 'CCDC 767169'
#TrackingRef '- 3a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
[2-Bis(trimethylsilyl)methyl-3,5,-di(2-thienyl)-2H-1,4,2-diazaphosphole-
kappaP]pentacarbonyltungsten(0)
;
_chemical_name_common            
;
(2-Bis(trimethylsilyl)methyl-3,5,-di(2-thienyl)-2H-1,4,2-
diazaphosphole-kappaP)pentacarbonyltungsten(0)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H25 N2 O5 P S2 Si2 W'
_chemical_formula_sum            'C22 H25 N2 O5 P S2 Si2 W'
_chemical_formula_weight         732.56

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
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                   9.5035(3)
_cell_length_b                   10.9580(4)
_cell_length_c                   15.4221(7)
_cell_angle_alpha                75.868(2)
_cell_angle_beta                 84.937(2)
_cell_angle_gamma                65.551(2)
_cell_volume                     1417.64(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    3746
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plates
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_absorpt_coefficient_mu    4.397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36309
_exptl_absorpt_correction_T_max  0.53875
_exptl_absorpt_process_details   'MULABS (Platon, cf. Blessing, 1995)'

_exptl_special_details           
;
dx = 40 mm, 20 sec./deg., 2 deg., 5 sets, 197 frames, mos.= 0.539(2) deg.
;

_diffrn_ambient_temperature      123(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_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13970
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.47
_reflns_number_total             6484
_reflns_number_gt                5969
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Collect
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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.
One 2-thienyl group is disordered (0.59(1):0.41(1)).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+2.0372P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6484
_refine_ls_number_parameters     309
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_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_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 0.141679(15) 0.723722(14) 0.378633(9) 0.01758(5) Uani 1 1 d . . .
C1A C -0.0036(4) 0.8331(4) 0.4613(3) 0.0277(8) Uani 1 1 d . . .
O1A O -0.0853(4) 0.8936(3) 0.5097(2) 0.0422(8) Uani 1 1 d . . .
C1B C 0.2600(5) 0.8448(4) 0.3701(3) 0.0291(9) Uani 1 1 d . . .
O1B O 0.3214(4) 0.9152(3) 0.3696(3) 0.0458(9) Uani 1 1 d . . .
C1C C 0.0173(4) 0.6062(4) 0.3879(2) 0.0227(7) Uani 1 1 d . . .
O1C O -0.0537(3) 0.5431(3) 0.3918(2) 0.0319(6) Uani 1 1 d . . .
C1D C 0.0106(4) 0.8609(4) 0.2710(3) 0.0228(7) Uani 1 1 d . . .
O1D O -0.0619(3) 0.9388(3) 0.2108(2) 0.0341(7) Uani 1 1 d . . .
C1E C 0.2749(4) 0.5980(4) 0.4887(3) 0.0235(8) Uani 1 1 d . . .
O1E O 0.3454(4) 0.5366(3) 0.5525(2) 0.0364(7) Uani 1 1 d . . .
P1 P 0.30444(10) 0.58986(9) 0.26622(6) 0.01651(17) Uani 1 1 d . . .
N1 N 0.1810(3) 0.5869(3) 0.1937(2) 0.0210(6) Uani 1 1 d . . .
C1 C 0.1678(4) 0.6827(4) 0.1225(2) 0.0190(7) Uani 1 1 d D A .
N2 N 0.2613(3) 0.7591(3) 0.1103(2) 0.0206(6) Uani 1 1 d . . .
C2 C 0.3533(4) 0.7160(4) 0.1788(2) 0.0191(7) Uani 1 1 d D . .
C3 C 0.4631(4) 0.4194(4) 0.2890(2) 0.0190(7) Uani 1 1 d . . .
H3 H 0.5273 0.4247 0.3348 0.023 Uiso 1 1 calc R . .
Si1 Si 0.40015(12) 0.27440(10) 0.35077(7) 0.0219(2) Uani 1 1 d . . .
C4 C 0.2426(5) 0.2692(5) 0.2905(3) 0.0344(10) Uani 1 1 d . . .
H4A H 0.2751 0.2603 0.2294 0.052 Uiso 1 1 calc R . .
H4B H 0.1497 0.3544 0.2885 0.052 Uiso 1 1 calc R . .
H4C H 0.2200 0.1902 0.3219 0.052 Uiso 1 1 calc R . .
C5 C 0.3379(5) 0.2902(4) 0.4670(3) 0.0304(9) Uani 1 1 d . . .
H5A H 0.4208 0.2927 0.4991 0.046 Uiso 1 1 calc R . .
H5B H 0.3153 0.2110 0.4979 0.046 Uiso 1 1 calc R . .
H5C H 0.2448 0.3753 0.4651 0.046 Uiso 1 1 calc R . .
C6 C 0.5692(5) 0.1031(4) 0.3686(3) 0.0358(10) Uani 1 1 d . . .
H6A H 0.6517 0.1061 0.4009 0.054 Uiso 1 1 calc R . .
H6B H 0.6074 0.0820 0.3106 0.054 Uiso 1 1 calc R . .
H6C H 0.5371 0.0318 0.4037 0.054 Uiso 1 1 calc R . .
Si2 Si 0.60870(12) 0.36171(11) 0.19660(7) 0.0234(2) Uani 1 1 d . . .
C7 C 0.5503(5) 0.2625(5) 0.1351(3) 0.0349(10) Uani 1 1 d . . .
H7A H 0.5337 0.1875 0.1780 0.052 Uiso 1 1 calc R . .
H7B H 0.6321 0.2240 0.0938 0.052 Uiso 1 1 calc R . .
H7C H 0.4544 0.3238 0.1013 0.052 Uiso 1 1 calc R . .
C8 C 0.6353(5) 0.4974(4) 0.1055(3) 0.0376(10) Uani 1 1 d . . .
H8A H 0.6667 0.5556 0.1314 0.056 Uiso 1 1 calc R . .
H8B H 0.5378 0.5540 0.0721 0.056 Uiso 1 1 calc R . .
H8C H 0.7154 0.4538 0.0649 0.056 Uiso 1 1 calc R . .
C9 C 0.7994(5) 0.2637(5) 0.2560(3) 0.0426(11) Uani 1 1 d . . .
H9A H 0.8205 0.3232 0.2865 0.064 Uiso 1 1 calc R . .
H9B H 0.8807 0.2332 0.2127 0.064 Uiso 1 1 calc R . .
H9C H 0.7970 0.1833 0.3001 0.064 Uiso 1 1 calc R . .
C10 C 0.0567(4) 0.7194(4) 0.0523(2) 0.0239(7) Uani 1 1 d DU . .
C11 C 0.0187(9) 0.8258(8) -0.0263(5) 0.0255(14) Uiso 0.590(4) 1 d PDU A 1
H11 H 0.0725 0.8842 -0.0423 0.031 Uiso 0.590(4) 1 calc PR A 1
C12 C -0.0983(9) 0.8404(7) -0.0776(5) 0.0274(13) Uiso 0.590(4) 1 d PDU A 1
H12 H -0.1373 0.9085 -0.1313 0.033 Uiso 0.590(4) 1 calc PR A 1
C13 C -0.1503(9) 0.7427(8) -0.0400(5) 0.0317(14) Uiso 0.590(4) 1 d PDU A 1
H13 H -0.2320 0.7339 -0.0657 0.038 Uiso 0.590(4) 1 calc PR A 1
S1 S -0.0556(2) 0.6328(2) 0.06000(14) 0.0302(5) Uiso 0.590(4) 1 d PDU A 1
C11' C -0.0393(13) 0.6490(11) 0.0435(7) 0.0255(14) Uiso 0.41 1 d PDU A 2
H11' H -0.0350 0.5679 0.0854 0.031 Uiso 0.410(4) 1 calc PR A 2
C12' C -0.1356(12) 0.7070(11) -0.0287(7) 0.0274(13) Uiso 0.41 1 d PDU A 2
H12' H -0.2091 0.6761 -0.0422 0.033 Uiso 0.410(4) 1 calc PR A 2
C13' C -0.1107(13) 0.8147(11) -0.0779(7) 0.0317(14) Uiso 0.41 1 d PDU A 2
H13' H -0.1638 0.8669 -0.1329 0.038 Uiso 0.410(4) 1 calc PR A 2
S1' S 0.0270(4) 0.8538(3) -0.0342(2) 0.0302(5) Uiso 0.41 1 d PDU A 2
C14 C 0.4653(4) 0.7705(3) 0.1854(2) 0.0200(7) Uani 1 1 d D . .
C15 C 0.5719(4) 0.7320(4) 0.2536(3) 0.0241(8) Uani 1 1 d D . .
H15 H 0.5777 0.6665 0.3080 0.029 Uiso 1 1 calc R . .
C16 C 0.6701(4) 0.8019(4) 0.2326(3) 0.0301(9) Uani 1 1 d D . .
H16 H 0.7493 0.7896 0.2717 0.036 Uiso 1 1 calc R . .
C17 C 0.6397(5) 0.8890(4) 0.1504(3) 0.0313(9) Uani 1 1 d D . .
H17 H 0.6959 0.9433 0.1255 0.038 Uiso 1 1 calc R . .
S2 S 0.48916(11) 0.89014(10) 0.09673(7) 0.0286(2) Uani 1 1 d 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 0.01812(8) 0.01883(8) 0.01511(8) -0.00308(5) 0.00225(5) -0.00768(6)
C1A 0.0257(19) 0.028(2) 0.029(2) -0.0061(17) 0.0049(16) -0.0121(16)
O1A 0.0417(17) 0.0448(19) 0.041(2) -0.0221(16) 0.0169(15) -0.0147(15)
C1B 0.0292(19) 0.027(2) 0.033(2) -0.0136(18) 0.0085(17) -0.0108(17)
O1B 0.0470(18) 0.0389(18) 0.069(3) -0.0293(18) 0.0201(17) -0.0284(16)
C1C 0.0204(17) 0.0262(19) 0.0165(18) -0.0004(15) 0.0011(14) -0.0074(15)
O1C 0.0288(14) 0.0358(16) 0.0345(17) -0.0031(13) 0.0019(12) -0.0194(13)
C1D 0.0206(17) 0.0234(19) 0.0232(19) -0.0032(16) 0.0027(15) -0.0093(15)
O1D 0.0344(15) 0.0292(15) 0.0306(16) 0.0055(13) -0.0066(13) -0.0104(13)
C1E 0.0257(18) 0.0262(19) 0.0223(19) -0.0064(16) 0.0003(15) -0.0139(16)
O1E 0.0455(17) 0.0412(18) 0.0250(16) 0.0013(14) -0.0151(14) -0.0219(15)
P1 0.0182(4) 0.0183(4) 0.0129(4) -0.0016(3) 0.0002(3) -0.0084(3)
N1 0.0211(14) 0.0221(15) 0.0201(16) -0.0061(13) 0.0000(12) -0.0082(12)
C1 0.0195(16) 0.0205(17) 0.0166(17) -0.0084(14) 0.0010(13) -0.0055(14)
N2 0.0217(14) 0.0217(15) 0.0173(15) -0.0038(12) 0.0007(12) -0.0082(12)
C2 0.0207(16) 0.0159(16) 0.0189(18) -0.0047(14) 0.0025(14) -0.0057(13)
C3 0.0199(16) 0.0206(17) 0.0161(17) -0.0046(14) -0.0012(13) -0.0075(14)
Si1 0.0270(5) 0.0176(5) 0.0202(5) -0.0004(4) -0.0025(4) -0.0098(4)
C4 0.042(2) 0.036(2) 0.038(2) -0.006(2) -0.0025(19) -0.029(2)
C5 0.034(2) 0.027(2) 0.026(2) 0.0006(17) 0.0027(17) -0.0124(17)
C6 0.043(2) 0.022(2) 0.034(2) -0.0017(18) 0.0001(19) -0.0069(18)
Si2 0.0238(5) 0.0237(5) 0.0245(5) -0.0101(4) 0.0049(4) -0.0096(4)
C7 0.050(3) 0.037(2) 0.027(2) -0.0147(19) 0.0097(19) -0.025(2)
C8 0.046(2) 0.033(2) 0.037(3) -0.016(2) 0.024(2) -0.019(2)
C9 0.026(2) 0.052(3) 0.050(3) -0.026(3) 0.007(2) -0.010(2)
C10 0.0208(15) 0.0254(17) 0.0216(17) -0.0072(14) -0.0005(13) -0.0044(13)
C14 0.0287(18) 0.0147(16) 0.0136(17) 0.0010(13) 0.0004(14) -0.0082(14)
C15 0.0269(18) 0.0222(18) 0.024(2) -0.0033(15) 0.0004(15) -0.0119(15)
C16 0.0261(19) 0.029(2) 0.037(2) -0.0037(18) -0.0054(17) -0.0139(17)
C17 0.031(2) 0.026(2) 0.038(2) -0.0014(18) 0.0001(18) -0.0164(17)
S2 0.0289(5) 0.0277(5) 0.0267(5) 0.0052(4) -0.0003(4) -0.0153(4)

_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 C1A 2.009(4) . ?
W1 C1D 2.041(4) . ?
W1 C1B 2.041(4) . ?
W1 C1E 2.044(4) . ?
W1 C1C 2.054(4) . ?
W1 P1 2.5377(9) . ?
C1A O1A 1.145(5) . ?
C1B O1B 1.142(5) . ?
C1C O1C 1.138(4) . ?
C1D O1D 1.141(5) . ?
C1E O1E 1.135(5) . ?
P1 N1 1.705(3) . ?
P1 C3 1.824(4) . ?
P1 C2 1.858(4) . ?
N1 C1 1.294(5) . ?
C1 N2 1.426(4) . ?
C1 C10 1.445(5) . ?
N2 C2 1.296(5) . ?
C2 C14 1.441(5) . ?
C3 Si2 1.927(4) . ?
C3 Si1 1.933(4) . ?
C3 H3 1.0000 . ?
Si1 C4 1.857(4) . ?
Si1 C5 1.863(4) . ?
Si1 C6 1.873(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Si2 C8 1.865(4) . ?
Si2 C9 1.865(5) . ?
Si2 C7 1.867(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.413(8) . ?
C10 C11' 1.450(9) . ?
C10 S1' 1.671(5) . ?
C10 S1 1.677(4) . ?
C11 C12 1.355(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.346(9) . ?
C12 H12 0.9500 . ?
C13 S1 1.756(8) . ?
C13 H13 0.9500 . ?
C11' C12' 1.354(12) . ?
C11' H11' 0.9500 . ?
C12' C13' 1.336(11) . ?
C12' H12' 0.9500 . ?
C13' S1' 1.764(10) . ?
C13' H13' 0.9500 . ?
C14 C15 1.389(5) . ?
C14 S2 1.719(3) . ?
C15 C16 1.407(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.359(6) . ?
C16 H16 0.9500 . ?
C17 S2 1.709(4) . ?
C17 H17 0.9500 . ?

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
C1A W1 C1D 90.40(16) . . ?
C1A W1 C1B 87.37(15) . . ?
C1D W1 C1B 88.76(16) . . ?
C1A W1 C1E 87.41(16) . . ?
C1D W1 C1E 175.82(14) . . ?
C1B W1 C1E 87.58(16) . . ?
C1A W1 C1C 91.26(15) . . ?
C1D W1 C1C 90.54(14) . . ?
C1B W1 C1C 178.46(14) . . ?
C1E W1 C1C 93.07(14) . . ?
C1A W1 P1 174.96(11) . . ?
C1D W1 P1 85.71(10) . . ?
C1B W1 P1 95.74(11) . . ?
C1E W1 P1 96.66(11) . . ?
C1C W1 P1 85.57(10) . . ?
O1A C1A W1 178.8(4) . . ?
O1B C1B W1 176.0(4) . . ?
O1C C1C W1 178.6(3) . . ?
O1D C1D W1 179.1(3) . . ?
O1E C1E W1 174.9(3) . . ?
N1 P1 C3 106.68(15) . . ?
N1 P1 C2 90.55(16) . . ?
C3 P1 C2 112.25(16) . . ?
N1 P1 W1 107.55(11) . . ?
C3 P1 W1 127.74(12) . . ?
C2 P1 W1 105.67(11) . . ?
C1 N1 P1 108.0(2) . . ?
N1 C1 N2 121.4(3) . . ?
N1 C1 C10 122.0(3) . . ?
N2 C1 C10 116.6(3) . . ?
C2 N2 C1 109.5(3) . . ?
N2 C2 C14 122.8(3) . . ?
N2 C2 P1 109.7(2) . . ?
C14 C2 P1 127.3(3) . . ?
P1 C3 Si2 119.88(19) . . ?
P1 C3 Si1 113.56(17) . . ?
Si2 C3 Si1 111.02(17) . . ?
P1 C3 H3 103.3 . . ?
Si2 C3 H3 103.3 . . ?
Si1 C3 H3 103.3 . . ?
C4 Si1 C5 109.1(2) . . ?
C4 Si1 C6 109.8(2) . . ?
C5 Si1 C6 102.9(2) . . ?
C4 Si1 C3 112.42(18) . . ?
C5 Si1 C3 111.71(17) . . ?
C6 Si1 C3 110.50(18) . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 Si2 C9 105.5(2) . . ?
C8 Si2 C7 103.3(2) . . ?
C9 Si2 C7 114.9(2) . . ?
C8 Si2 C3 118.14(17) . . ?
C9 Si2 C3 104.62(19) . . ?
C7 Si2 C3 110.70(17) . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C1 130.0(4) . . ?
C11 C10 C11' 102.4(6) . . ?
C1 C10 C11' 127.5(5) . . ?
C11 C10 S1' 8.3(3) . . ?
C1 C10 S1' 121.9(3) . . ?
C11' C10 S1' 110.6(4) . . ?
C11 C10 S1 110.1(4) . . ?
C1 C10 S1 119.9(3) . . ?
C11' C10 S1 9.2(4) . . ?
S1' C10 S1 118.1(3) . . ?
C12 C11 C10 116.6(6) . . ?
C12 C11 H11 121.7 . . ?
C10 C11 H11 121.7 . . ?
C13 C12 C11 108.8(6) . . ?
C13 C12 H12 125.6 . . ?
C11 C12 H12 125.6 . . ?
C12 C13 S1 114.8(6) . . ?
C12 C13 H13 122.6 . . ?
S1 C13 H13 122.6 . . ?
C10 S1 C13 89.7(3) . . ?
C12' C11' C10 115.2(7) . . ?
C12' C11' H11' 122.4 . . ?
C10 C11' H11' 122.4 . . ?
C13' C12' C11' 109.1(8) . . ?
C13' C12' H12' 125.4 . . ?
C11' C12' H12' 125.4 . . ?
C12' C13' S1' 115.8(8) . . ?
C12' C13' H13' 122.1 . . ?
S1' C13' H13' 122.1 . . ?
C10 S1' C13' 89.1(4) . . ?
C15 C14 C2 128.6(3) . . ?
C15 C14 S2 111.5(3) . . ?
C2 C14 S2 119.7(3) . . ?
C14 C15 C16 111.9(3) . . ?
C14 C15 H15 124.1 . . ?
C16 C15 H15 124.1 . . ?
C17 C16 C15 112.7(4) . . ?
C17 C16 H16 123.6 . . ?
C15 C16 H16 123.6 . . ?
C16 C17 S2 112.6(3) . . ?
C16 C17 H17 123.7 . . ?
S2 C17 H17 123.7 . . ?
C17 S2 C14 91.26(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1D W1 C1A O1A 165(17) . . . . ?
C1B W1 C1A O1A -106(17) . . . . ?
C1E W1 C1A O1A -19(17) . . . . ?
C1C W1 C1A O1A 74(17) . . . . ?
P1 W1 C1A O1A 125(17) . . . . ?
C1A W1 C1B O1B 13(6) . . . . ?
C1D W1 C1B O1B 104(6) . . . . ?
C1E W1 C1B O1B -74(6) . . . . ?
C1C W1 C1B O1B 41(10) . . . . ?
P1 W1 C1B O1B -171(6) . . . . ?
C1A W1 C1C O1C 79(15) . . . . ?
C1D W1 C1C O1C -11(15) . . . . ?
C1B W1 C1C O1C 51(18) . . . . ?
C1E W1 C1C O1C 166(15) . . . . ?
P1 W1 C1C O1C -97(15) . . . . ?
C1A W1 C1D O1D 78(23) . . . . ?
C1B W1 C1D O1D -9(23) . . . . ?
C1E W1 C1D O1D 20(24) . . . . ?
C1C W1 C1D O1D 169(100) . . . . ?
P1 W1 C1D O1D -105(23) . . . . ?
C1A W1 C1E O1E -33(4) . . . . ?
C1D W1 C1E O1E 26(5) . . . . ?
C1B W1 C1E O1E 55(4) . . . . ?
C1C W1 C1E O1E -124(4) . . . . ?
P1 W1 C1E O1E 150(4) . . . . ?
C1A W1 P1 N1 -4.5(13) . . . . ?
C1D W1 P1 N1 -44.11(15) . . . . ?
C1B W1 P1 N1 -132.43(17) . . . . ?
C1E W1 P1 N1 139.34(15) . . . . ?
C1C W1 P1 N1 46.76(16) . . . . ?
C1A W1 P1 C3 -133.2(13) . . . . ?
C1D W1 P1 C3 -172.82(17) . . . . ?
C1B W1 P1 C3 98.86(19) . . . . ?
C1E W1 P1 C3 10.64(17) . . . . ?
C1C W1 P1 C3 -81.95(17) . . . . ?
C1A W1 P1 C2 91.2(13) . . . . ?
C1D W1 P1 C2 51.58(15) . . . . ?
C1B W1 P1 C2 -36.74(17) . . . . ?
C1E W1 P1 C2 -124.96(15) . . . . ?
C1C W1 P1 C2 142.46(15) . . . . ?
C3 P1 N1 C1 -121.8(2) . . . . ?
C2 P1 N1 C1 -8.4(3) . . . . ?
W1 P1 N1 C1 98.3(2) . . . . ?
P1 N1 C1 N2 6.9(4) . . . . ?
P1 N1 C1 C10 -172.1(3) . . . . ?
N1 C1 N2 C2 0.2(4) . . . . ?
C10 C1 N2 C2 179.2(3) . . . . ?
C1 N2 C2 C14 178.3(3) . . . . ?
C1 N2 C2 P1 -6.6(3) . . . . ?
N1 P1 C2 N2 9.0(3) . . . . ?
C3 P1 C2 N2 117.3(3) . . . . ?
W1 P1 C2 N2 -99.4(2) . . . . ?
N1 P1 C2 C14 -176.2(3) . . . . ?
C3 P1 C2 C14 -67.9(3) . . . . ?
W1 P1 C2 C14 75.4(3) . . . . ?
N1 P1 C3 Si2 69.8(2) . . . . ?
C2 P1 C3 Si2 -27.9(2) . . . . ?
W1 P1 C3 Si2 -161.20(11) . . . . ?
N1 P1 C3 Si1 -64.8(2) . . . . ?
C2 P1 C3 Si1 -162.49(17) . . . . ?
W1 P1 C3 Si1 64.2(2) . . . . ?
P1 C3 Si1 C4 55.6(3) . . . . ?
Si2 C3 Si1 C4 -83.0(2) . . . . ?
P1 C3 Si1 C5 -67.6(2) . . . . ?
Si2 C3 Si1 C5 153.87(19) . . . . ?
P1 C3 Si1 C6 178.6(2) . . . . ?
Si2 C3 Si1 C6 40.0(2) . . . . ?
P1 C3 Si2 C8 24.5(3) . . . . ?
Si1 C3 Si2 C8 160.1(2) . . . . ?
P1 C3 Si2 C9 141.3(2) . . . . ?
Si1 C3 Si2 C9 -83.0(2) . . . . ?
P1 C3 Si2 C7 -94.3(2) . . . . ?
Si1 C3 Si2 C7 41.3(3) . . . . ?
N1 C1 C10 C11 175.2(6) . . . . ?
N2 C1 C10 C11 -3.8(7) . . . . ?
N1 C1 C10 C11' -8.3(8) . . . . ?
N2 C1 C10 C11' 172.7(7) . . . . ?
N1 C1 C10 S1' 173.4(3) . . . . ?
N2 C1 C10 S1' -5.6(5) . . . . ?
N1 C1 C10 S1 -2.2(5) . . . . ?
N2 C1 C10 S1 178.7(3) . . . . ?
C1 C10 C11 C12 -176.1(6) . . . . ?
C11' C10 C11 C12 6.8(10) . . . . ?
S1' C10 C11 C12 -165(4) . . . . ?
S1 C10 C11 C12 1.6(9) . . . . ?
C10 C11 C12 C13 -1.4(11) . . . . ?
C11 C12 C13 S1 0.6(10) . . . . ?
C11 C10 S1 C13 -0.9(5) . . . . ?
C1 C10 S1 C13 177.0(4) . . . . ?
C11' C10 S1 C13 -35(3) . . . . ?
S1' C10 S1 C13 1.2(4) . . . . ?
C12 C13 S1 C10 0.2(7) . . . . ?
C11 C10 C11' C12' -3.7(12) . . . . ?
C1 C10 C11' C12' 179.1(8) . . . . ?
S1' C10 C11' C12' -2.5(12) . . . . ?
S1 C10 C11' C12' 144(4) . . . . ?
C10 C11' C12' C13' 3.3(15) . . . . ?
C11' C12' C13' S1' -2.8(15) . . . . ?
C11 C10 S1' C13' 9(3) . . . . ?
C1 C10 S1' C13' 179.2(5) . . . . ?
C11' C10 S1' C13' 0.7(7) . . . . ?
S1 C10 S1' C13' -5.1(5) . . . . ?
C12' C13' S1' C10 1.3(10) . . . . ?
N2 C2 C14 C15 -178.7(4) . . . . ?
P1 C2 C14 C15 7.1(6) . . . . ?
N2 C2 C14 S2 -4.3(5) . . . . ?
P1 C2 C14 S2 -178.47(19) . . . . ?
C2 C14 C15 C16 175.3(4) . . . . ?
S2 C14 C15 C16 0.5(4) . . . . ?
C14 C15 C16 C17 -0.8(5) . . . . ?
C15 C16 C17 S2 0.7(5) . . . . ?
C16 C17 S2 C14 -0.4(3) . . . . ?
C15 C14 S2 C17 -0.1(3) . . . . ?
C2 C14 S2 C17 -175.4(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3 O1E 1.00 2.41 3.407(4) 172.8 2_666
C15 H15 O1E 0.95 2.59 3.525(5) 167.9 2_666

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.268
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.154

#==============================================================================
# _eof # End of Crystallographic Information File

# Attachment '- 3b.cif'

data_joerg143
_database_code_depnum_ccdc_archive 'CCDC 767316'
#TrackingRef '- 3b.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            "joerg143 H.Helten ''HHE-298F1'' 100K 13.02.08"
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H28 N3 O5 P S Si2 W'
_chemical_formula_sum            'C20 H28 N3 O5 P S Si2 W'
_chemical_formula_weight         693.51

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'
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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   P21/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                   11.8239(2)
_cell_length_b                   20.2887(5)
_cell_length_c                   11.9270(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.5180(10)
_cell_angle_gamma                90.00
_cell_volume                     2769.83(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43773
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    4.423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3949
_exptl_absorpt_correction_T_max  0.8787
_exptl_absorpt_process_details   'MULABS (Platon, cf. Blessing, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 2 deg.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44556
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6333
_reflns_number_gt                4956
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6333
_refine_ls_number_parameters     306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0541
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_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_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
W W 0.714875(10) 0.269319(6) 0.613676(11) 0.01505(5) Uani 1 1 d . . .
P P 0.69703(7) 0.35997(4) 0.75347(7) 0.01407(17) Uani 1 1 d . . .
S S 0.92408(7) 0.51443(4) 0.64013(7) 0.02071(18) Uani 1 1 d . . .
Si1 Si 0.58729(7) 0.30748(5) 0.94479(8) 0.0204(2) Uani 1 1 d . . .
Si2 Si 0.80501(7) 0.40428(4) 1.01758(8) 0.0185(2) Uani 1 1 d . . .
N1 N 0.6952(2) 0.48214(12) 0.6816(2) 0.0168(6) Uani 1 1 d . . .
N2 N 0.5688(2) 0.40051(12) 0.7254(2) 0.0163(6) Uani 1 1 d . . .
N3 N 0.4953(2) 0.50345(13) 0.6555(3) 0.0244(7) Uani 1 1 d . . .
O1 O 0.7105(2) 0.16561(12) 0.4158(2) 0.0334(6) Uani 1 1 d . . .
O2 O 0.6799(2) 0.15414(12) 0.7827(2) 0.0388(7) Uani 1 1 d . . .
O3 O 0.44134(19) 0.28852(12) 0.5042(2) 0.0282(6) Uani 1 1 d . . .
O4 O 0.7937(2) 0.37408(12) 0.4495(2) 0.0279(6) Uani 1 1 d . . .
O5 O 0.9772(2) 0.23456(11) 0.7443(2) 0.0273(6) Uani 1 1 d . . .
C1 C 0.7716(3) 0.43633(15) 0.7190(3) 0.0159(7) Uani 1 1 d . . .
C2 C 0.5830(3) 0.46008(15) 0.6900(3) 0.0178(7) Uani 1 1 d . . .
C3 C 0.7263(2) 0.34069(14) 0.9069(3) 0.0148(7) Uani 1 1 d . . .
H3 H 0.7806 0.3021 0.9178 0.018 Uiso 1 1 calc R . .
C4 C 0.4738(3) 0.27082(17) 0.8221(3) 0.0282(8) Uani 1 1 d . . .
H4A H 0.5073 0.2332 0.7901 0.042 Uiso 1 1 calc R . .
H4B H 0.4477 0.3041 0.7617 0.042 Uiso 1 1 calc R . .
H4C H 0.4072 0.2560 0.8505 0.042 Uiso 1 1 calc R . .
C5 C 0.6362(3) 0.23865(17) 1.0510(3) 0.0319(9) Uani 1 1 d . . .
H5A H 0.6806 0.2568 1.1251 0.048 Uiso 1 1 calc R . .
H5B H 0.6858 0.2082 1.0209 0.048 Uiso 1 1 calc R . .
H5C H 0.5678 0.2150 1.0625 0.048 Uiso 1 1 calc R . .
C6 C 0.5093(3) 0.37438(17) 1.0038(3) 0.0287(8) Uani 1 1 d . . .
H6A H 0.4440 0.3553 1.0297 0.043 Uiso 1 1 calc R . .
H6B H 0.4795 0.4071 0.9431 0.043 Uiso 1 1 calc R . .
H6C H 0.5637 0.3957 1.0694 0.043 Uiso 1 1 calc R . .
C7 C 0.8052(3) 0.37444(18) 1.1656(3) 0.0298(9) Uani 1 1 d . . .
H7A H 0.8345 0.3291 1.1753 0.045 Uiso 1 1 calc R . .
H7B H 0.7255 0.3757 1.1756 0.045 Uiso 1 1 calc R . .
H7C H 0.8558 0.4028 1.2236 0.045 Uiso 1 1 calc R . .
C8 C 0.9627(3) 0.40969(17) 1.0191(3) 0.0251(8) Uani 1 1 d . . .
H8A H 1.0052 0.4327 1.0893 0.038 Uiso 1 1 calc R . .
H8B H 0.9713 0.4341 0.9507 0.038 Uiso 1 1 calc R . .
H8C H 0.9946 0.3652 1.0179 0.038 Uiso 1 1 calc R . .
C9 C 0.7379(3) 0.48783(16) 0.9899(3) 0.0271(8) Uani 1 1 d . . .
H9A H 0.7693 0.5163 1.0569 0.041 Uiso 1 1 calc R . .
H9B H 0.6530 0.4842 0.9774 0.041 Uiso 1 1 calc R . .
H9C H 0.7561 0.5069 0.9210 0.041 Uiso 1 1 calc R . .
C10 C 0.5112(3) 0.57139(16) 0.6253(3) 0.0285(8) Uani 1 1 d . . .
H10A H 0.5937 0.5791 0.6281 0.043 Uiso 1 1 calc R . .
H10B H 0.4873 0.6007 0.6805 0.043 Uiso 1 1 calc R . .
H10C H 0.4635 0.5803 0.5470 0.043 Uiso 1 1 calc R . .
C11 C 0.3765(3) 0.48334(18) 0.6557(4) 0.0349(10) Uani 1 1 d . . .
H11A H 0.3746 0.4356 0.6679 0.052 Uiso 1 1 calc R . .
H11B H 0.3232 0.4947 0.5812 0.052 Uiso 1 1 calc R . .
H11C H 0.3522 0.5062 0.7182 0.052 Uiso 1 1 calc R . .
C12 C 0.8899(3) 0.44450(15) 0.7077(3) 0.0160(7) Uani 1 1 d . . .
C13 C 0.9844(2) 0.40232(16) 0.7385(3) 0.0180(7) Uani 1 1 d . . .
H13 H 0.9831 0.3615 0.7771 0.022 Uiso 1 1 calc R . .
C14 C 1.0835(3) 0.42718(16) 0.7059(3) 0.0203(7) Uani 1 1 d . . .
H14 H 1.1564 0.4049 0.7203 0.024 Uiso 1 1 calc R . .
C15 C 1.0624(3) 0.48657(16) 0.6515(3) 0.0219(7) Uani 1 1 d . . .
H15 H 1.1189 0.5100 0.6229 0.026 Uiso 1 1 calc R . .
C16 C 0.7145(3) 0.20247(17) 0.4898(3) 0.0230(8) Uani 1 1 d . . .
C17 C 0.6867(3) 0.19623(17) 0.7218(3) 0.0248(8) Uani 1 1 d . . .
C18 C 0.5392(3) 0.28257(15) 0.5430(3) 0.0212(7) Uani 1 1 d . . .
C19 C 0.7632(3) 0.33776(16) 0.5088(3) 0.0198(7) Uani 1 1 d . . .
C20 C 0.8846(3) 0.24945(15) 0.6948(3) 0.0195(7) Uani 1 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
W 0.01551(7) 0.01407(7) 0.01561(7) -0.00061(5) 0.00400(5) -0.00097(5)
P 0.0132(4) 0.0133(4) 0.0156(4) 0.0011(3) 0.0034(3) -0.0007(3)
S 0.0206(4) 0.0194(4) 0.0235(5) 0.0031(3) 0.0081(4) -0.0019(3)
Si1 0.0209(5) 0.0216(5) 0.0211(5) 0.0009(4) 0.0095(4) -0.0028(4)
Si2 0.0191(4) 0.0189(5) 0.0162(5) -0.0016(4) 0.0022(4) 0.0006(4)
N1 0.0151(13) 0.0148(13) 0.0212(15) 0.0010(11) 0.0055(12) -0.0014(11)
N2 0.0131(12) 0.0162(13) 0.0196(15) 0.0019(11) 0.0041(11) 0.0004(10)
N3 0.0159(13) 0.0208(15) 0.0361(18) 0.0076(13) 0.0060(13) 0.0050(11)
O1 0.0295(14) 0.0364(15) 0.0348(15) -0.0190(13) 0.0093(12) -0.0047(11)
O2 0.0488(17) 0.0255(14) 0.0451(17) 0.0120(13) 0.0171(14) -0.0029(12)
O3 0.0178(12) 0.0314(14) 0.0330(15) -0.0026(11) 0.0019(11) -0.0016(10)
O4 0.0347(14) 0.0287(14) 0.0223(14) 0.0048(11) 0.0108(11) -0.0031(11)
O5 0.0217(13) 0.0308(14) 0.0272(14) 0.0034(11) 0.0022(11) 0.0075(11)
C1 0.0163(15) 0.0168(16) 0.0135(16) -0.0039(13) 0.0019(13) -0.0033(13)
C2 0.0169(16) 0.0187(17) 0.0178(17) -0.0014(13) 0.0041(14) 0.0010(13)
C3 0.0153(15) 0.0141(15) 0.0164(17) 0.0033(12) 0.0066(13) 0.0025(12)
C4 0.0226(18) 0.032(2) 0.033(2) -0.0038(17) 0.0125(16) -0.0089(15)
C5 0.039(2) 0.028(2) 0.034(2) 0.0071(17) 0.0189(19) -0.0003(17)
C6 0.0235(18) 0.032(2) 0.033(2) -0.0017(16) 0.0124(17) 0.0005(15)
C7 0.032(2) 0.035(2) 0.0192(19) -0.0014(16) 0.0006(16) -0.0041(16)
C8 0.0218(17) 0.0268(19) 0.0245(19) -0.0010(15) 0.0013(15) 0.0002(14)
C9 0.0265(18) 0.0229(18) 0.030(2) -0.0068(15) 0.0037(16) 0.0029(15)
C10 0.0276(18) 0.0194(18) 0.038(2) 0.0069(16) 0.0074(17) 0.0062(14)
C11 0.0158(17) 0.034(2) 0.055(3) 0.0102(19) 0.0081(18) 0.0067(15)
C12 0.0185(15) 0.0154(16) 0.0135(16) -0.0019(12) 0.0029(13) -0.0024(12)
C13 0.0129(15) 0.0223(17) 0.0182(17) 0.0029(13) 0.0025(13) -0.0033(13)
C14 0.0153(15) 0.0260(18) 0.0199(18) -0.0027(14) 0.0053(14) -0.0017(13)
C15 0.0203(16) 0.0272(18) 0.0201(18) -0.0015(14) 0.0090(15) -0.0071(14)
C16 0.0147(16) 0.0228(18) 0.030(2) -0.0024(16) 0.0036(15) -0.0037(14)
C17 0.0233(17) 0.0205(18) 0.030(2) -0.0047(16) 0.0063(16) -0.0021(14)
C18 0.0274(19) 0.0170(17) 0.0200(18) -0.0011(13) 0.0078(15) -0.0049(14)
C19 0.0178(16) 0.0210(17) 0.0187(18) -0.0044(14) 0.0009(14) 0.0017(13)
C20 0.0284(19) 0.0161(16) 0.0165(17) -0.0002(13) 0.0101(16) -0.0028(13)

_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
W C16 2.005(4) . ?
W C20 2.038(3) . ?
W C19 2.044(4) . ?
W C17 2.046(4) . ?
W C18 2.054(3) . ?
W P 2.5266(8) . ?
P N2 1.683(2) . ?
P C3 1.818(3) . ?
P C1 1.879(3) . ?
S C15 1.704(3) . ?
S C12 1.729(3) . ?
Si1 C4 1.873(3) . ?
Si1 C6 1.874(3) . ?
Si1 C5 1.877(4) . ?
Si1 C3 1.932(3) . ?
Si2 C8 1.864(3) . ?
Si2 C7 1.866(3) . ?
Si2 C9 1.866(3) . ?
Si2 C3 1.913(3) . ?
N1 C1 1.295(4) . ?
N1 C2 1.428(4) . ?
N2 C2 1.305(4) . ?
N3 C2 1.343(4) . ?
N3 C10 1.449(4) . ?
N3 C11 1.463(4) . ?
O1 C16 1.148(4) . ?
O2 C17 1.137(4) . ?
O3 C18 1.140(4) . ?
O4 C19 1.141(4) . ?
O5 C20 1.146(4) . ?
C1 C12 1.448(4) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.382(4) . ?
C13 C14 1.416(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.361(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?

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
C16 W C20 92.07(13) . . ?
C16 W C19 87.58(13) . . ?
C20 W C19 91.83(12) . . ?
C16 W C17 90.20(14) . . ?
C20 W C17 81.60(13) . . ?
C19 W C17 172.98(12) . . ?
C16 W C18 88.34(13) . . ?
C20 W C18 174.21(13) . . ?
C19 W C18 93.96(12) . . ?
C17 W C18 92.63(13) . . ?
C16 W P 173.56(9) . . ?
C20 W P 93.77(9) . . ?
C19 W P 89.53(9) . . ?
C17 W P 93.33(10) . . ?
C18 W P 86.13(9) . . ?
N2 P C3 103.88(13) . . ?
N2 P C1 90.14(13) . . ?
C3 P C1 114.62(13) . . ?
N2 P W 116.40(9) . . ?
C3 P W 118.77(10) . . ?
C1 P W 109.53(10) . . ?
C15 S C12 91.28(15) . . ?
C4 Si1 C6 104.91(16) . . ?
C4 Si1 C5 105.72(17) . . ?
C6 Si1 C5 112.52(17) . . ?
C4 Si1 C3 116.14(15) . . ?
C6 Si1 C3 111.26(15) . . ?
C5 Si1 C3 106.32(15) . . ?
C8 Si2 C7 104.25(16) . . ?
C8 Si2 C9 109.18(16) . . ?
C7 Si2 C9 111.20(17) . . ?
C8 Si2 C3 111.03(14) . . ?
C7 Si2 C3 108.62(15) . . ?
C9 Si2 C3 112.28(14) . . ?
C1 N1 C2 109.4(3) . . ?
C2 N2 P 109.5(2) . . ?
C2 N3 C10 124.1(3) . . ?
C2 N3 C11 119.0(3) . . ?
C10 N3 C11 116.7(3) . . ?
N1 C1 C12 119.5(3) . . ?
N1 C1 P 110.0(2) . . ?
C12 C1 P 129.2(2) . . ?
N2 C2 N3 123.6(3) . . ?
N2 C2 N1 120.7(3) . . ?
N3 C2 N1 115.6(3) . . ?
P C3 Si2 119.12(16) . . ?
P C3 Si1 110.62(15) . . ?
Si2 C3 Si1 111.66(16) . . ?
P C3 H3 104.7 . . ?
Si2 C3 H3 104.7 . . ?
Si1 C3 H3 104.7 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C1 129.8(3) . . ?
C13 C12 S 111.4(2) . . ?
C1 C12 S 118.8(2) . . ?
C12 C13 C14 112.0(3) . . ?
C12 C13 H13 124.0 . . ?
C14 C13 H13 124.0 . . ?
C15 C14 C13 112.4(3) . . ?
C15 C14 H14 123.8 . . ?
C13 C14 H14 123.8 . . ?
C14 C15 S 112.9(2) . . ?
C14 C15 H15 123.6 . . ?
S C15 H15 123.6 . . ?
O1 C16 W 177.1(3) . . ?
O2 C17 W 174.6(3) . . ?
O3 C18 W 178.5(3) . . ?
O4 C19 W 177.1(3) . . ?
O5 C20 W 175.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 W P N2 22.0(9) . . . . ?
C20 W P N2 177.07(14) . . . . ?
C19 W P N2 85.27(13) . . . . ?
C17 W P N2 -101.14(14) . . . . ?
C18 W P N2 -8.73(14) . . . . ?
C16 W P C3 147.4(9) . . . . ?
C20 W P C3 -57.60(14) . . . . ?
C19 W P C3 -149.40(14) . . . . ?
C17 W P C3 24.19(14) . . . . ?
C18 W P C3 116.60(14) . . . . ?
C16 W P C1 -78.3(9) . . . . ?
C20 W P C1 76.76(13) . . . . ?
C19 W P C1 -15.04(13) . . . . ?
C17 W P C1 158.55(13) . . . . ?
C18 W P C1 -109.04(13) . . . . ?
C3 P N2 C2 118.6(2) . . . . ?
C1 P N2 C2 3.1(2) . . . . ?
W P N2 C2 -108.9(2) . . . . ?
C2 N1 C1 C12 173.5(3) . . . . ?
C2 N1 C1 P 5.2(3) . . . . ?
N2 P C1 N1 -5.1(2) . . . . ?
C3 P C1 N1 -110.5(2) . . . . ?
W P C1 N1 113.1(2) . . . . ?
N2 P C1 C12 -172.0(3) . . . . ?
C3 P C1 C12 82.7(3) . . . . ?
W P C1 C12 -53.7(3) . . . . ?
P N2 C2 N3 176.7(3) . . . . ?
P N2 C2 N1 -0.9(4) . . . . ?
C10 N3 C2 N2 174.6(3) . . . . ?
C11 N3 C2 N2 -0.8(5) . . . . ?
C10 N3 C2 N1 -7.8(5) . . . . ?
C11 N3 C2 N1 176.8(3) . . . . ?
C1 N1 C2 N2 -3.2(4) . . . . ?
C1 N1 C2 N3 179.0(3) . . . . ?
N2 P C3 Si2 -86.55(18) . . . . ?
C1 P C3 Si2 10.1(2) . . . . ?
W P C3 Si2 142.28(12) . . . . ?
N2 P C3 Si1 44.83(18) . . . . ?
C1 P C3 Si1 141.49(15) . . . . ?
W P C3 Si1 -86.34(15) . . . . ?
C8 Si2 C3 P -72.9(2) . . . . ?
C7 Si2 C3 P 173.07(17) . . . . ?
C9 Si2 C3 P 49.7(2) . . . . ?
C8 Si2 C3 Si1 156.22(15) . . . . ?
C7 Si2 C3 Si1 42.2(2) . . . . ?
C9 Si2 C3 Si1 -81.24(19) . . . . ?
C4 Si1 C3 P 22.9(2) . . . . ?
C6 Si1 C3 P -97.03(19) . . . . ?
C5 Si1 C3 P 140.14(17) . . . . ?
C4 Si1 C3 Si2 158.01(16) . . . . ?
C6 Si1 C3 Si2 38.1(2) . . . . ?
C5 Si1 C3 Si2 -84.72(19) . . . . ?
N1 C1 C12 C13 -178.5(3) . . . . ?
P C1 C12 C13 -12.7(5) . . . . ?
N1 C1 C12 S -2.0(4) . . . . ?
P C1 C12 S 163.74(18) . . . . ?
C15 S C12 C13 0.8(3) . . . . ?
C15 S C12 C1 -176.2(3) . . . . ?
C1 C12 C13 C14 176.2(3) . . . . ?
S C12 C13 C14 -0.5(4) . . . . ?
C12 C13 C14 C15 -0.2(4) . . . . ?
C13 C14 C15 S 0.9(4) . . . . ?
C12 S C15 C14 -1.0(3) . . . . ?
C20 W C16 O1 -157(6) . . . . ?
C19 W C16 O1 -65(6) . . . . ?
C17 W C16 O1 122(6) . . . . ?
C18 W C16 O1 29(6) . . . . ?
P W C16 O1 -2(7) . . . . ?
C16 W C17 O2 73(3) . . . . ?
C20 W C17 O2 -19(3) . . . . ?
C19 W C17 O2 1(4) . . . . ?
C18 W C17 O2 161(3) . . . . ?
P W C17 O2 -113(3) . . . . ?
C16 W C18 O3 59(12) . . . . ?
C20 W C18 O3 -35(13) . . . . ?
C19 W C18 O3 147(12) . . . . ?
C17 W C18 O3 -31(12) . . . . ?
P W C18 O3 -124(12) . . . . ?
C16 W C19 O4 -46(5) . . . . ?
C20 W C19 O4 46(5) . . . . ?
C17 W C19 O4 25(6) . . . . ?
C18 W C19 O4 -135(5) . . . . ?
P W C19 O4 139(5) . . . . ?
C16 W C20 O5 -83(3) . . . . ?
C19 W C20 O5 -171(3) . . . . ?
C17 W C20 O5 6(3) . . . . ?
C18 W C20 O5 10(4) . . . . ?
P W C20 O5 99(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.148

#==============================================================================
# _eof # End of Crystallographic Information File