# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1837
 
data_dw9958 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C16 H29 O4 P3 W' 
_chemical_formula_weight          562.15 
_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' 
 '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' 
 'W'  'W'  -0.8490   6.8722 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pnma 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, y+1/2, -z' 
 '-x+1/2, -y, z+1/2' 
 '-x, -y, -z' 
 '-x-1/2, y-1/2, z-1/2' 
 'x, -y-1/2, z' 
 'x-1/2, y, -z-1/2' 
 
_cell_length_a                    17.3386(7) 
_cell_length_b                    13.7599(5) 
_cell_length_c                    9.4610(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2257.2(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.09 
_exptl_crystal_size_mid           0.07 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.654 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1104 
_exptl_absorpt_coefficient_mu     5.345 
_exptl_absorpt_correction_type 'multiscan' 
_exptl_absorpt_correction_T_min  1.156
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details 
;
multi-scan from symmetry-related measurements (Blessing 1995)
;
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       180(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_measurement_device_type   'KappaCCD'
_diffrn_measurement_device        '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean  9
_diffrn_radiation_monochromator   'horizonally mounted graphite crystal'
_diffrn_measurement_method        'CCD'

_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             21678 
_diffrn_reflns_av_R_equivalents   0.0817 
_diffrn_reflns_av_sigmaI/netI     0.0396 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        20 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          2.35 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              2087 
_reflns_number_observed           1790 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection       'Collect (Nonius BV, 1997-2000)' 
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution     teXsan
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 7 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^)+(0.0363P)^2^+1.2068P] 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     ? 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0011(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          2080 
_refine_ls_number_parameters      135 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0436 
_refine_ls_R_factor_obs           0.0267 
_refine_ls_wR_factor_all          0.0664 
_refine_ls_wR_factor_obs          0.0616 
_refine_ls_goodness_of_fit_all    1.076 
_refine_ls_goodness_of_fit_obs    1.108 
_refine_ls_restrained_S_all       1.100 
_refine_ls_restrained_S_obs       1.107 
_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 0.597473(12) 0.2500 0.60409(2) 0.02918(13) Uani 1 d S . 
P1 P 0.58152(6) 0.35853(8) 0.39264(11) 0.0273(2) Uani 1 d . . 
H1 H 0.5194(22) 0.4064(27) 0.3830(35) 0.033 Uiso 1 d . . 
P2 P 0.57283(8) 0.2500 0.2205(2) 0.0286(3) Uani 1 d S . 
O1 O 0.4175(3) 0.2500 0.6659(6) 0.0560(13) Uani 1 d S . 
C1 C 0.4818(4) 0.2500 0.6386(6) 0.0343(13) Uani 1 d S . 
O2 O 0.6108(2) 0.0805(3) 0.8255(4) 0.0717(11) Uani 1 d . . 
C2 C 0.6053(2) 0.1431(3) 0.7451(5) 0.0452(11) Uani 1 d . . 
O3 O 0.7801(3) 0.2500 0.6155(5) 0.0603(14) Uani 1 d S . 
C3 C 0.7138(4) 0.2500 0.6036(6) 0.0387(14) Uani 1 d S . 
C4 C 0.6516(2) 0.4528(3) 0.3325(5) 0.0356(9) Uani 1 d . . 
C5 C 0.6576(3) 0.5263(3) 0.4530(5) 0.0567(13) Uani 1 d . . 
H5A H 0.6927(16) 0.5788(13) 0.4256(15) 0.085 Uiso 1 calc R . 
H5B H 0.6775(19) 0.4939(7) 0.5377(11) 0.085 Uiso 1 calc R . 
H5C H 0.6064(5) 0.5533(18) 0.4730(25) 0.085 Uiso 1 calc R . 
C6 C 0.7301(2) 0.4049(3) 0.3053(5) 0.0497(12) Uani 1 d . . 
H6A H 0.7681(5) 0.4549(4) 0.2812(33) 0.075 Uiso 1 calc R . 
H6B H 0.7255(5) 0.3588(17) 0.2268(23) 0.075 Uiso 1 calc R . 
H6C H 0.7468(9) 0.3703(19) 0.3906(12) 0.075 Uiso 1 calc R . 
C7 C 0.6237(3) 0.5019(3) 0.1984(5) 0.0501(11) Uani 1 d . . 
H7A H 0.6611(9) 0.5513(16) 0.1692(19) 0.075 Uiso 1 calc R . 
H7B H 0.5736(9) 0.5327(19) 0.2161(10) 0.075 Uiso 1 calc R . 
H7C H 0.6182(17) 0.4533(5) 0.1234(10) 0.075 Uiso 1 calc R . 
C8 C 0.4683(3) 0.2500 0.1611(6) 0.0335(13) Uani 1 d S . 
C9 C 0.4583(3) 0.3408(4) 0.0688(5) 0.0533(13) Uani 1 d . . 
H9A H 0.4070(8) 0.3401(12) 0.0254(28) 0.080 Uiso 1 calc R . 
H9B H 0.4978(12) 0.3411(12) -0.0054(21) 0.080 Uiso 1 calc R . 
H9C H 0.4638(18) 0.3990(4) 0.1275(8) 0.080 Uiso 1 calc R . 
C10 C 0.4089(3) 0.2500 0.2786(8) 0.042(2) Uani 1 d SD . 
H10A H 0.3606(27) 0.2500 0.2372(63) 0.063 Uiso 1 d SD . 
H10B H 0.4138(23) 0.1958(31) 0.3347(53) 0.063 Uiso 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 0.0331(2) 0.0329(2) 0.0216(2) 0.000 0.00233(10) 0.000 
P1 0.0298(5) 0.0263(5) 0.0257(6) 0.0000(4) 0.0014(4) 0.0002(4) 
P2 0.0314(7) 0.0296(7) 0.0249(8) 0.000 -0.0029(6) 0.000 
O1 0.039(3) 0.063(3) 0.066(4) 0.000 0.017(2) 0.000 
C1 0.044(4) 0.031(3) 0.027(3) 0.000 0.004(3) 0.000 
O2 0.090(3) 0.068(2) 0.057(2) 0.032(2) 0.016(2) 0.025(2) 
C2 0.048(3) 0.050(3) 0.038(3) 0.002(2) 0.009(2) 0.014(2) 
O3 0.036(3) 0.084(4) 0.061(3) 0.000 -0.010(2) 0.000 
C3 0.045(4) 0.042(3) 0.029(3) 0.000 -0.002(3) 0.000 
C4 0.039(2) 0.031(2) 0.037(2) 0.003(2) -0.001(2) -0.006(2) 
C5 0.077(3) 0.044(3) 0.049(3) -0.006(2) 0.003(3) -0.025(3) 
C6 0.035(2) 0.052(3) 0.061(3) 0.011(2) 0.006(2) -0.009(2) 
C7 0.060(3) 0.045(3) 0.046(3) 0.016(2) -0.003(3) -0.010(2) 
C8 0.029(3) 0.035(3) 0.036(3) 0.000 -0.008(3) 0.000 
C9 0.045(3) 0.063(3) 0.052(3) 0.015(2) -0.015(2) 0.000(2) 
C10 0.031(3) 0.050(4) 0.044(5) 0.000 -0.002(3) 0.000 
 
_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 C2 1.990(5) 7_565 ? 
W1 C2 1.990(5) . ? 
W1 C3 2.017(7) . ? 
W1 C1 2.032(6) . ? 
W1 P1 2.5117(11) 7_565 ? 
W1 P1 2.5117(11) . ? 
P1 C4 1.866(4) . ? 
P1 P2 2.2151(15) . ? 
P2 C8 1.897(5) . ? 
P2 P1 2.2151(15) 7_565 ? 
O1 C1 1.145(7) . ? 
O2 C2 1.153(6) . ? 
O3 C3 1.155(8) . ? 
C4 C7 1.516(6) . ? 
C4 C5 1.528(6) . ? 
C4 C6 1.534(5) . ? 
C8 C10 1.515(8) . ? 
C8 C9 1.533(6) 7_565 ? 
C8 C9 1.533(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 
C2 W1 C2 95.3(3) 7_565 . ? 
C2 W1 C3 86.2(2) 7_565 . ? 
C2 W1 C3 86.2(2) . . ? 
C2 W1 C1 87.7(2) 7_565 . ? 
C2 W1 C1 87.7(2) . . ? 
C3 W1 C1 170.9(2) . . ? 
C2 W1 P1 168.75(14) 7_565 7_565 ? 
C2 W1 P1 95.87(14) . 7_565 ? 
C3 W1 P1 96.21(13) . 7_565 ? 
C1 W1 P1 91.10(13) . 7_565 ? 
C2 W1 P1 95.87(14) 7_565 . ? 
C2 W1 P1 168.75(14) . . ? 
C3 W1 P1 96.21(13) . . ? 
C1 W1 P1 91.10(13) . . ? 
P1 W1 P1 72.96(5) 7_565 . ? 
C4 P1 P2 106.76(14) . . ? 
C4 P1 W1 125.77(13) . . ? 
P2 P1 W1 101.09(5) . . ? 
C8 P2 P1 106.42(15) . . ? 
C8 P2 P1 106.42(14) . 7_565 ? 
P1 P2 P1 84.78(7) . 7_565 ? 
O1 C1 W1 176.2(5) . . ? 
O2 C2 W1 178.9(4) . . ? 
O3 C3 W1 174.2(5) . . ? 
C7 C4 C5 110.6(4) . . ? 
C7 C4 C6 109.6(4) . . ? 
C5 C4 C6 110.4(4) . . ? 
C7 C4 P1 110.9(3) . . ? 
C5 C4 P1 106.0(3) . . ? 
C6 C4 P1 109.3(3) . . ? 
C10 C8 C9 109.9(3) . 7_565 ? 
C10 C8 C9 109.9(3) . . ? 
C9 C8 C9 109.1(5) 7_565 . ? 
C10 C8 P2 115.6(4) . . ? 
C9 C8 P2 106.0(3) 7_565 . ? 
C9 C8 P2 106.0(3) . . ? 
 
_refine_diff_density_max    0.903 
_refine_diff_density_min   -1.675 
_refine_diff_density_rms    0.114