# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr R Streubel'
_publ_contact_author_address     
;
Institut fur Anorganische Chemie
Bonn
D-53121
GERMANY
;

_publ_contact_author_email       R.STREUBEL@UNI-BONN.DE

_publ_section_title              
;
Electrophilic terminal phosphinidene complex-Lewis base adducts:
Chemistry in between carbon-halide activation and weak Lewis base adduct
formation
;

loop_
_publ_author_name
_publ_author_address
A.A.Khan
;     Institut fur Anorganische und Analytische Chemie
Technische Universitat Braunschweig
Postfach 3329
38023 Braunschweig
Germany
;
C.Wismach
;     Institut fur Anorganische und Analytische Chemie
Technische Universitat Braunschweig
Postfach 3329
38023 Braunschweig
Germany
;
P.G.Jones
;     Institut fur Anorganische und Analytische Chemie
Technische Universitat Braunschweig
Postfach 3329
38023 Braunschweig
Germany
;
R.Streubel
;     Institut fur Anorganische und Analytische Chemie
Technische Universitat Braunschweig
Postfach 3329
38023 Braunschweig
Germany
;

#=============================================================================
# cif data for "Gies" (compound 6)
#=============================================================================

data_gies
_database_code_CSD               215573

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H26 Br O5 P Si2 W'
_chemical_formula_weight         685.31

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'
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'
Br Br -0.2901 2.4595 '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                   9.0099(6)
_cell_length_b                   10.2351(6)
_cell_length_c                   14.4398(11)
_cell_angle_alpha                87.965(4)
_cell_angle_beta                 88.558(4)
_cell_angle_gamma                68.778(4)
_cell_volume                     1240.40(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6756
_cell_measurement_theta_min      2.588
_cell_measurement_theta_max      30.535

_exptl_crystal_description       tablet
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    6.454
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(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  'Bruker AXS Smart 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26263
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         30.03
_reflns_number_total             7239
_reflns_number_gt                6362
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Smart'
_computing_cell_refinement       'Bruker Saint'
_computing_data_reduction        'Bruker SAint'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  ?

_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^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     heavy-atom
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7239
_refine_ls_number_parameters     268
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0502
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.000
_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 0.790725(12) 0.242041(11) 0.334215(7) 0.01549(3) Uani 1 1 d . . .
Br Br 0.54622(3) 0.41438(3) 0.123031(19) 0.02653(7) Uani 1 1 d . . .
P P 0.69403(8) 0.46004(7) 0.23356(5) 0.01709(13) Uani 1 1 d . . .
Si1 Si 0.37657(9) 0.74098(9) 0.22829(6) 0.02479(17) Uani 1 1 d U . .
Si2 Si 0.68587(9) 0.72116(8) 0.34275(5) 0.01963(15) Uani 1 1 d U . .
O1 O 0.8814(3) -0.0418(3) 0.44988(16) 0.0412(6) Uani 1 1 d . . .
O2 O 0.9123(3) 0.0632(2) 0.15257(15) 0.0342(5) Uani 1 1 d . . .
O3 O 0.6784(3) 0.4101(3) 0.51957(14) 0.0358(5) Uani 1 1 d . . .
O4 O 1.1335(2) 0.2462(2) 0.37677(15) 0.0325(5) Uani 1 1 d . . .
O5 O 0.4523(3) 0.2182(3) 0.30855(16) 0.0423(6) Uani 1 1 d . . .
C1 C 0.8508(3) 0.0620(3) 0.40913(19) 0.0258(6) Uani 1 1 d . . .
C2 C 0.8698(3) 0.1295(3) 0.21590(19) 0.0210(5) Uani 1 1 d . . .
C3 C 0.7165(3) 0.3508(3) 0.45211(19) 0.0232(6) Uani 1 1 d . . .
C4 C 1.0118(3) 0.2461(3) 0.35809(19) 0.0226(6) Uani 1 1 d . . .
C5 C 0.5723(3) 0.2297(3) 0.31778(19) 0.0252(6) Uani 1 1 d . . .
C6 C 0.5669(3) 0.6211(3) 0.28769(17) 0.0170(5) Uani 1 1 d U . .
H6 H 0.5241 0.5847 0.3434 0.020 Uiso 1 1 calc R . .
C7 C 0.2256(3) 0.6540(4) 0.2364(2) 0.0354(7) Uani 1 1 d U . .
H7A H 0.1184 0.7257 0.2400 0.042 Uiso 1 1 calc R . .
H7B H 0.2449 0.5928 0.2921 0.042 Uiso 1 1 calc R . .
H7C H 0.2345 0.5981 0.1814 0.042 Uiso 1 1 calc R . .
C8 C 0.2834(4) 0.9078(3) 0.2924(2) 0.0397(8) Uani 1 1 d U . .
H8A H 0.3595 0.9557 0.2955 0.048 Uiso 1 1 calc R . .
H8B H 0.2542 0.8861 0.3554 0.048 Uiso 1 1 calc R . .
H8C H 0.1878 0.9686 0.2600 0.048 Uiso 1 1 calc R . .
C9 C 0.4122(4) 0.7920(3) 0.1063(2) 0.0327(7) Uani 1 1 d U . .
H9A H 0.4613 0.7074 0.0702 0.039 Uiso 1 1 calc R . .
H9B H 0.4834 0.8452 0.1063 0.039 Uiso 1 1 calc R . .
H9C H 0.3106 0.8501 0.0785 0.039 Uiso 1 1 calc R . .
C10 C 0.5759(4) 0.8070(3) 0.4484(2) 0.0290(7) Uani 1 1 d U . .
H10A H 0.6414 0.8475 0.4820 0.035 Uiso 1 1 calc R . .
H10B H 0.5527 0.7373 0.4884 0.035 Uiso 1 1 calc R . .
H10C H 0.4760 0.8814 0.4303 0.035 Uiso 1 1 calc R . .
C11 C 0.7125(4) 0.8518(3) 0.2560(2) 0.0281(6) Uani 1 1 d U . .
H11A H 0.6081 0.9216 0.2400 0.034 Uiso 1 1 calc R . .
H11B H 0.7648 0.8034 0.2000 0.034 Uiso 1 1 calc R . .
H11C H 0.7783 0.8987 0.2825 0.034 Uiso 1 1 calc R . .
C12 C 0.8891(3) 0.6025(3) 0.3833(2) 0.0248(6) Uani 1 1 d U . .
H12A H 0.9479 0.6596 0.4047 0.030 Uiso 1 1 calc R . .
H12B H 0.9478 0.5453 0.3319 0.030 Uiso 1 1 calc R . .
H12C H 0.8773 0.5412 0.4343 0.030 Uiso 1 1 calc R . .
C13 C 0.8277(3) 0.5145(3) 0.15392(18) 0.0206(5) Uani 1 1 d U . .
H13A H 0.7619 0.5813 0.1065 0.025 Uiso 1 1 calc R . .
H13B H 0.8814 0.5649 0.1898 0.025 Uiso 1 1 calc R . .
C14 C 0.9528(3) 0.3957(3) 0.10534(18) 0.0217(5) Uani 1 1 d U . .
C15 C 1.1031(3) 0.3333(3) 0.1430(2) 0.0267(6) Uani 1 1 d U . .
H15 H 1.1263 0.3674 0.1991 0.032 Uiso 1 1 calc R . .
C16 C 1.2205(4) 0.2221(3) 0.1008(2) 0.0324(7) Uani 1 1 d U . .
H16 H 1.3229 0.1808 0.1276 0.039 Uiso 1 1 calc R . .
C17 C 1.1861(4) 0.1719(3) 0.0187(2) 0.0328(7) Uani 1 1 d U . .
H17 H 1.2648 0.0953 -0.0106 0.039 Uiso 1 1 calc R . .
C18 C 1.0368(4) 0.2340(3) -0.0202(2) 0.0307(7) Uani 1 1 d U . .
H18 H 1.0134 0.1998 -0.0762 0.037 Uiso 1 1 calc R . .
C19 C 0.9215(4) 0.3460(3) 0.02245(19) 0.0263(6) Uani 1 1 d U . .
H19 H 0.8202 0.3891 -0.0053 0.032 Uiso 1 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
W 0.01627(5) 0.01567(5) 0.01499(5) 0.00090(4) -0.00002(3) -0.00646(4)
Br 0.03388(15) 0.02560(15) 0.01987(13) -0.00282(11) -0.00708(11) -0.00981(11)
P 0.0199(3) 0.0157(3) 0.0152(3) -0.0012(3) 0.0006(2) -0.0059(2)
Si1 0.0226(4) 0.0233(4) 0.0234(4) -0.0018(3) -0.0034(3) -0.0019(3)
Si2 0.0220(4) 0.0191(4) 0.0185(3) -0.0041(3) 0.0022(3) -0.0080(3)
O1 0.0606(15) 0.0324(14) 0.0393(13) 0.0181(11) -0.0228(11) -0.0277(12)
O2 0.0477(13) 0.0258(12) 0.0296(11) -0.0095(10) 0.0088(10) -0.0136(10)
O3 0.0418(13) 0.0458(15) 0.0234(11) -0.0098(10) 0.0089(9) -0.0201(11)
O4 0.0201(10) 0.0429(14) 0.0365(12) 0.0012(10) -0.0019(9) -0.0139(9)
O5 0.0318(12) 0.0663(18) 0.0388(13) 0.0016(12) -0.0006(10) -0.0299(12)
C1 0.0316(15) 0.0279(16) 0.0228(14) 0.0029(12) -0.0073(11) -0.0165(12)
C2 0.0248(13) 0.0171(14) 0.0230(13) 0.0026(11) -0.0005(10) -0.0102(10)
C3 0.0221(13) 0.0255(15) 0.0232(13) 0.0037(12) 0.0000(10) -0.0103(11)
C4 0.0243(14) 0.0196(14) 0.0218(13) -0.0017(11) 0.0033(10) -0.0057(10)
C5 0.0269(14) 0.0312(17) 0.0202(13) 0.0010(12) 0.0006(11) -0.0139(12)
C6 0.0179(11) 0.0178(13) 0.0145(11) -0.0027(10) 0.0008(9) -0.0051(9)
C7 0.0228(14) 0.052(2) 0.0305(16) -0.0025(15) -0.0034(12) -0.0122(14)
C8 0.0293(16) 0.0315(18) 0.0434(19) -0.0089(15) -0.0056(14) 0.0081(13)
C9 0.0396(17) 0.0275(17) 0.0254(14) 0.0051(13) -0.0068(13) -0.0052(13)
C10 0.0316(15) 0.0334(17) 0.0242(14) -0.0125(13) 0.0057(12) -0.0135(13)
C11 0.0402(16) 0.0225(15) 0.0245(14) -0.0031(12) 0.0042(12) -0.0150(12)
C12 0.0204(13) 0.0283(16) 0.0326(15) 0.0117(12) -0.0114(11) -0.0174(11)
C13 0.0280(13) 0.0180(13) 0.0166(12) -0.0008(10) 0.0065(10) -0.0097(10)
C14 0.0286(14) 0.0167(13) 0.0200(12) -0.0003(10) 0.0081(10) -0.0091(10)
C15 0.0303(15) 0.0293(16) 0.0220(13) -0.0026(12) 0.0062(11) -0.0129(12)
C16 0.0262(15) 0.0342(18) 0.0318(16) 0.0013(14) 0.0056(12) -0.0056(12)
C17 0.0407(17) 0.0220(16) 0.0298(16) -0.0028(13) 0.0136(13) -0.0049(13)
C18 0.0416(17) 0.0273(16) 0.0216(14) -0.0075(12) 0.0102(12) -0.0105(13)
C19 0.0328(15) 0.0242(15) 0.0195(13) -0.0010(11) 0.0038(11) -0.0075(12)

_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 C1 2.006(3) . ?
W C3 2.030(3) . ?
W C5 2.038(3) . ?
W C4 2.046(3) . ?
W C2 2.058(3) . ?
W P 2.5052(7) . ?
Br P 2.2693(7) . ?
P C6 1.822(2) . ?
P C13 1.859(3) . ?
Si1 C9 1.872(3) . ?
Si1 C8 1.874(3) . ?
Si1 C7 1.875(3) . ?
Si1 C6 1.912(3) . ?
Si2 C10 1.863(3) . ?
Si2 C11 1.875(3) . ?
Si2 C12 1.888(3) . ?
Si2 C6 1.931(3) . ?
O1 C1 1.142(4) . ?
O2 C2 1.132(3) . ?
O3 C3 1.144(3) . ?
O4 C4 1.136(3) . ?
O5 C5 1.140(3) . ?
C13 C14 1.507(4) . ?
C14 C15 1.387(4) . ?
C14 C19 1.391(4) . ?
C15 C16 1.390(4) . ?
C16 C17 1.394(4) . ?
C17 C18 1.386(4) . ?
C18 C19 1.389(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 W C3 89.59(12) . . ?
C1 W C5 87.88(12) . . ?
C3 W C5 91.22(11) . . ?
C1 W C4 88.71(11) . . ?
C3 W C4 87.38(10) . . ?
C5 W C4 176.32(11) . . ?
C1 W C2 89.70(11) . . ?
C3 W C2 178.94(11) . . ?
C5 W C2 89.53(11) . . ?
C4 W C2 91.82(10) . . ?
C1 W P 174.18(8) . . ?
C3 W P 92.65(8) . . ?
C5 W P 86.70(9) . . ?
C4 W P 96.76(8) . . ?
C2 W P 88.14(8) . . ?
C6 P C13 104.84(12) . . ?
C6 P Br 106.57(8) . . ?
C13 P Br 97.13(9) . . ?
C6 P W 117.34(9) . . ?
C13 P W 122.83(9) . . ?
Br P W 105.20(3) . . ?
C9 Si1 C8 106.82(16) . . ?
C9 Si1 C7 112.60(15) . . ?
C8 Si1 C7 104.75(16) . . ?
C9 Si1 C6 112.95(13) . . ?
C8 Si1 C6 110.82(13) . . ?
C7 Si1 C6 108.60(14) . . ?
C10 Si2 C11 111.93(14) . . ?
C10 Si2 C12 105.86(14) . . ?
C11 Si2 C12 108.27(13) . . ?
C10 Si2 C6 108.26(12) . . ?
C11 Si2 C6 109.39(12) . . ?
C12 Si2 C6 113.15(12) . . ?
O1 C1 W 177.5(2) . . ?
O2 C2 W 177.2(2) . . ?
O3 C3 W 178.2(3) . . ?
O4 C4 W 175.9(2) . . ?
O5 C5 W 177.8(3) . . ?
P C6 Si1 120.34(13) . . ?
P C6 Si2 112.91(12) . . ?
Si1 C6 Si2 113.57(13) . . ?
C14 C13 P 114.60(19) . . ?
C15 C14 C19 118.5(3) . . ?
C15 C14 C13 120.1(2) . . ?
C19 C14 C13 121.4(3) . . ?
C14 C15 C16 121.7(3) . . ?
C15 C16 C17 119.1(3) . . ?
C18 C17 C16 119.9(3) . . ?
C17 C18 C19 120.2(3) . . ?
C18 C19 C14 120.7(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
C1 W P C6 101.0(8) . . . . ?
C3 W P C6 -11.45(12) . . . . ?
C5 W P C6 79.62(12) . . . . ?
C4 W P C6 -99.12(12) . . . . ?
C2 W P C6 169.26(12) . . . . ?
C1 W P C13 -126.4(8) . . . . ?
C3 W P C13 121.15(13) . . . . ?
C5 W P C13 -147.78(13) . . . . ?
C4 W P C13 33.47(13) . . . . ?
C2 W P C13 -58.14(12) . . . . ?
C1 W P Br -17.2(8) . . . . ?
C3 W P Br -129.68(8) . . . . ?
C5 W P Br -38.61(8) . . . . ?
C4 W P Br 142.64(8) . . . . ?
C2 W P Br 51.03(8) . . . . ?
C3 W C1 O1 122(7) . . . . ?
C5 W C1 O1 31(7) . . . . ?
C4 W C1 O1 -151(7) . . . . ?
C2 W C1 O1 -59(7) . . . . ?
P W C1 O1 9(7) . . . . ?
C1 W C2 O2 24(5) . . . . ?
C3 W C2 O2 71(9) . . . . ?
C5 W C2 O2 -64(5) . . . . ?
C4 W C2 O2 113(5) . . . . ?
P W C2 O2 -151(5) . . . . ?
C1 W C3 O3 51(8) . . . . ?
C5 W C3 O3 139(8) . . . . ?
C4 W C3 O3 -38(8) . . . . ?
C2 W C3 O3 4(13) . . . . ?
P W C3 O3 -134(8) . . . . ?
C1 W C4 O4 -44(3) . . . . ?
C3 W C4 O4 45(3) . . . . ?
C5 W C4 O4 -22(5) . . . . ?
C2 W C4 O4 -134(3) . . . . ?
P W C4 O4 138(3) . . . . ?
C1 W C5 O5 -34(6) . . . . ?
C3 W C5 O5 -124(6) . . . . ?
C4 W C5 O5 -56(7) . . . . ?
C2 W C5 O5 56(6) . . . . ?
P W C5 O5 144(6) . . . . ?
C13 P C6 Si1 85.91(17) . . . . ?
Br P C6 Si1 -16.38(17) . . . . ?
W P C6 Si1 -133.88(12) . . . . ?
C13 P C6 Si2 -52.71(16) . . . . ?
Br P C6 Si2 -155.00(10) . . . . ?
W P C6 Si2 87.50(14) . . . . ?
C9 Si1 C6 P -53.5(2) . . . . ?
C8 Si1 C6 P -173.31(18) . . . . ?
C7 Si1 C6 P 72.14(19) . . . . ?
C9 Si1 C6 Si2 84.86(17) . . . . ?
C8 Si1 C6 Si2 -34.9(2) . . . . ?
C7 Si1 C6 Si2 -149.49(14) . . . . ?
C10 Si2 C6 P -145.84(15) . . . . ?
C11 Si2 C6 P 91.96(16) . . . . ?
C12 Si2 C6 P -28.83(18) . . . . ?
C10 Si2 C6 Si1 72.66(17) . . . . ?
C11 Si2 C6 Si1 -49.54(17) . . . . ?
C12 Si2 C6 Si1 -170.33(13) . . . . ?
C6 P C13 C14 176.06(19) . . . . ?
Br P C13 C14 -74.6(2) . . . . ?
W P C13 C14 38.6(2) . . . . ?
P C13 C14 C15 -93.4(3) . . . . ?
P C13 C14 C19 86.7(3) . . . . ?
C19 C14 C15 C16 -1.0(4) . . . . ?
C13 C14 C15 C16 179.0(3) . . . . ?
C14 C15 C16 C17 -0.2(5) . . . . ?
C15 C16 C17 C18 0.7(5) . . . . ?
C16 C17 C18 C19 0.0(5) . . . . ?
C17 C18 C19 C14 -1.2(5) . . . . ?
C15 C14 C19 C18 1.7(4) . . . . ?
C13 C14 C19 C18 -178.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.119

#=============================================================================
# end  of cif data for "Gies" (compound 6)
#=============================================================================

#=============================================================================
# cif data for "Kanti" (compound 7)
#=============================================================================

data_kanti
_database_code_CSD               215574

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Br O5 P Si2 W'
_chemical_formula_weight         595.19

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'
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'
Br Br -0.2901 2.4595 '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                   6.9656(2)
_cell_length_b                   9.4476(3)
_cell_length_c                   16.0750(5)
_cell_angle_alpha                74.9900(10)
_cell_angle_beta                 88.9010(10)
_cell_angle_gamma                82.8530(10)
_cell_volume                     1013.74(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    5879
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      30.5

_exptl_crystal_description       tablet
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             568
_exptl_absorpt_coefficient_mu    7.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_T_max  0.494
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      133(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  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20897
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         30.03
_reflns_number_total             5896
_reflns_number_gt                5660
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97

_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^)+(0.0306P)^2^+0.7156P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'PH free, rigid methyls, others riding'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5896
_refine_ls_number_parameters     209
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0192
_refine_ls_wR_factor_ref         0.0510
_refine_ls_wR_factor_gt          0.0506
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.059
_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
W W 0.256503(11) 0.165923(8) 0.114591(5) 0.01776(3) Uani 1 1 d . . .
Br Br 0.62096(4) 0.32889(3) 0.243753(18) 0.03201(6) Uani 1 1 d . . .
P P 0.31810(8) 0.34485(6) 0.19482(4) 0.01736(10) Uani 1 1 d . . .
H1 H 0.313(5) 0.481(4) 0.143(2) 0.034(9) Uiso 1 1 d . . .
Si1 Si 0.10255(10) 0.58007(7) 0.27419(4) 0.02084(12) Uani 1 1 d U . .
Si2 Si 0.23070(10) 0.24742(7) 0.39561(4) 0.02210(12) Uani 1 1 d U . .
C1 C 0.2212(4) 0.0251(3) 0.04232(18) 0.0284(5) Uani 1 1 d . . .
C2 C 0.4981(4) 0.0271(3) 0.16815(18) 0.0281(5) Uani 1 1 d . . .
C3 C 0.4079(4) 0.2814(3) 0.01450(17) 0.0268(5) Uani 1 1 d . . .
C4 C 0.0100(4) 0.3004(3) 0.06541(15) 0.0228(4) Uani 1 1 d . . .
C5 C 0.0886(3) 0.0614(3) 0.21032(16) 0.0238(4) Uani 1 1 d . . .
C6 C 0.1659(3) 0.3737(2) 0.28355(14) 0.0182(4) Uani 1 1 d U . .
H6 H 0.0401 0.3434 0.2700 0.022 Uiso 1 1 calc R . .
C7 C -0.0218(5) 0.6673(3) 0.16783(17) 0.0334(6) Uani 1 1 d U . .
H7A H -0.0678 0.7711 0.1642 0.040 Uiso 1 1 calc R . .
H7B H -0.1320 0.6151 0.1623 0.040 Uiso 1 1 calc R . .
H7C H 0.0693 0.6614 0.1213 0.040 Uiso 1 1 calc R . .
C8 C 0.3264(4) 0.6665(3) 0.2813(2) 0.0340(6) Uani 1 1 d U . .
H8A H 0.2913 0.7708 0.2798 0.041 Uiso 1 1 calc R . .
H8B H 0.4098 0.6586 0.2324 0.041 Uiso 1 1 calc R . .
H8C H 0.3958 0.6154 0.3352 0.041 Uiso 1 1 calc R . .
C9 C -0.0712(4) 0.6093(3) 0.35971(17) 0.0316(5) Uani 1 1 d U . .
H9A H -0.0148 0.5573 0.4164 0.038 Uiso 1 1 calc R . .
H9B H -0.1920 0.5710 0.3517 0.038 Uiso 1 1 calc R . .
H9C H -0.0979 0.7152 0.3559 0.038 Uiso 1 1 calc R . .
C10 C -0.0056(4) 0.2146(3) 0.45014(18) 0.0340(6) Uani 1 1 d U . .
H10A H 0.0185 0.1575 0.5100 0.041 Uiso 1 1 calc R . .
H10B H -0.0772 0.1594 0.4200 0.041 Uiso 1 1 calc R . .
H10C H -0.0818 0.3096 0.4490 0.041 Uiso 1 1 calc R . .
C11 C 0.3827(4) 0.3331(3) 0.45896(17) 0.0305(5) Uani 1 1 d U . .
H11A H 0.3191 0.4313 0.4597 0.037 Uiso 1 1 calc R . .
H11B H 0.5098 0.3422 0.4323 0.037 Uiso 1 1 calc R . .
H11C H 0.3989 0.2709 0.5181 0.037 Uiso 1 1 calc R . .
C12 C 0.3612(5) 0.0630(3) 0.39231(18) 0.0332(6) Uani 1 1 d U . .
H12A H 0.4926 0.0750 0.3711 0.040 Uiso 1 1 calc R . .
H12B H 0.2915 0.0214 0.3537 0.040 Uiso 1 1 calc R . .
H12C H 0.3676 -0.0037 0.4504 0.040 Uiso 1 1 calc R . .
O1 O 0.2116(3) -0.0546(3) 0.00044(16) 0.0429(5) Uani 1 1 d . . .
O2 O 0.6281(3) -0.0522(3) 0.19922(18) 0.0443(5) Uani 1 1 d . . .
O3 O 0.4839(3) 0.3461(3) -0.04357(14) 0.0408(5) Uani 1 1 d . . .
O4 O -0.1298(3) 0.3743(2) 0.03967(13) 0.0319(4) Uani 1 1 d . . .
O5 O -0.0074(3) 0.0060(2) 0.26424(14) 0.0360(4) 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 0.01552(5) 0.01669(5) 0.02218(5) -0.00757(3) -0.00043(3) -0.00064(3)
Br 0.01935(11) 0.03995(14) 0.04165(14) -0.01843(11) 0.00119(10) -0.00570(10)
P 0.0170(2) 0.0153(2) 0.0201(2) -0.00501(18) 0.00116(19) -0.00242(19)
Si1 0.0233(3) 0.0172(3) 0.0214(3) -0.0055(2) 0.0009(2) 0.0008(2)
Si2 0.0251(3) 0.0201(3) 0.0196(3) -0.0026(2) -0.0014(2) -0.0018(2)
C1 0.0210(11) 0.0295(12) 0.0387(13) -0.0171(10) -0.0003(9) -0.0009(9)
C2 0.0228(11) 0.0242(11) 0.0392(13) -0.0120(10) -0.0009(10) -0.0017(9)
C3 0.0212(11) 0.0316(12) 0.0291(11) -0.0111(10) 0.0000(9) -0.0022(9)
C4 0.0235(11) 0.0240(10) 0.0216(10) -0.0069(8) 0.0009(8) -0.0036(9)
C5 0.0204(10) 0.0181(9) 0.0322(11) -0.0058(8) -0.0030(9) -0.0005(8)
C6 0.0170(9) 0.0177(9) 0.0196(9) -0.0046(7) 0.0008(7) -0.0012(7)
C7 0.0415(15) 0.0269(12) 0.0265(11) -0.0037(9) -0.0028(10) 0.0097(11)
C8 0.0357(14) 0.0211(11) 0.0470(15) -0.0105(10) 0.0018(12) -0.0066(10)
C9 0.0370(14) 0.0293(12) 0.0287(12) -0.0115(10) 0.0064(10) 0.0028(10)
C10 0.0375(14) 0.0330(13) 0.0290(12) -0.0009(10) 0.0065(10) -0.0112(11)
C11 0.0323(13) 0.0338(13) 0.0264(11) -0.0099(10) -0.0036(9) -0.0030(10)
C12 0.0429(15) 0.0224(11) 0.0302(12) -0.0026(9) -0.0097(11) 0.0038(10)
O1 0.0317(11) 0.0478(12) 0.0631(14) -0.0402(11) -0.0021(10) -0.0021(9)
O2 0.0270(10) 0.0349(11) 0.0688(15) -0.0153(10) -0.0118(10) 0.0096(9)
O3 0.0336(11) 0.0514(13) 0.0337(10) -0.0017(9) 0.0080(8) -0.0116(10)
O4 0.0242(9) 0.0337(10) 0.0348(10) -0.0068(8) -0.0031(7) 0.0046(8)
O5 0.0297(10) 0.0336(10) 0.0410(11) -0.0007(8) 0.0046(8) -0.0102(8)

_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 C1 2.018(3) . ?
W C5 2.035(3) . ?
W C4 2.044(2) . ?
W C3 2.050(3) . ?
W C2 2.053(3) . ?
W P 2.4568(6) . ?
Br P 2.2394(6) . ?
P C6 1.818(2) . ?
Si1 C9 1.866(3) . ?
Si1 C8 1.866(3) . ?
Si1 C7 1.871(3) . ?
Si1 C6 1.912(2) . ?
Si2 C11 1.870(3) . ?
Si2 C10 1.872(3) . ?
Si2 C12 1.875(3) . ?
Si2 C6 1.912(2) . ?
C1 O1 1.140(3) . ?
C2 O2 1.134(3) . ?
C3 O3 1.137(3) . ?
C4 O4 1.142(3) . ?
C5 O5 1.141(3) . ?

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
C1 W C5 92.47(10) . . ?
C1 W C4 92.41(10) . . ?
C5 W C4 86.71(9) . . ?
C1 W C3 87.76(11) . . ?
C5 W C3 175.82(9) . . ?
C4 W C3 89.10(10) . . ?
C1 W C2 87.93(10) . . ?
C5 W C2 91.06(10) . . ?
C4 W C2 177.76(9) . . ?
C3 W C2 93.13(10) . . ?
C1 W P 175.66(8) . . ?
C5 W P 91.81(7) . . ?
C4 W P 88.54(7) . . ?
C3 W P 88.02(7) . . ?
C2 W P 91.29(7) . . ?
C6 P Br 104.54(7) . . ?
C6 P W 121.57(7) . . ?
Br P W 116.48(2) . . ?
C9 Si1 C8 110.81(14) . . ?
C9 Si1 C7 107.35(13) . . ?
C8 Si1 C7 109.93(14) . . ?
C9 Si1 C6 110.23(11) . . ?
C8 Si1 C6 110.33(11) . . ?
C7 Si1 C6 108.11(11) . . ?
C11 Si2 C10 110.41(13) . . ?
C11 Si2 C12 108.19(13) . . ?
C10 Si2 C12 107.47(14) . . ?
C11 Si2 C6 112.06(11) . . ?
C10 Si2 C6 105.70(11) . . ?
C12 Si2 C6 112.90(11) . . ?
O1 C1 W 176.3(2) . . ?
O2 C2 W 178.0(3) . . ?
O3 C3 W 176.6(2) . . ?
O4 C4 W 178.4(2) . . ?
O5 C5 W 178.4(2) . . ?
P C6 Si2 117.43(11) . . ?
P C6 Si1 110.44(11) . . ?
Si2 C6 Si1 117.39(11) . . ?

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
C6 H6 Br 1.00 2.98 3.954(2) 164.0 1_455
P H1 O3 1.34(3) 2.52(3) 3.679(2) 143(2) 2_665

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.555
_refine_diff_density_rms         0.149

#=============================================================================
# end  of cif data for "Kanti" (compound 7)
#=============================================================================

#=============================================================================
# end  of combined cif
#=============================================================================