# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2432
_database_code_depnum_ccdc_archive 'CCDC 1039383'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H39 N2 O6 P W'
_chemical_formula_sum            'C28 H39 N2 O6 P W'
_chemical_formula_weight         714.43

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'
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 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9216(4)
_cell_length_b                   23.5529(11)
_cell_length_c                   14.5767(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.717(2)
_cell_angle_gamma                90.00
_cell_volume                     3005.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    6921
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      29.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_T_max  0.8584
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24433
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         28.00
_reflns_number_total             7162
_reflns_number_gt                4505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/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         7162
_refine_ls_number_parameters     348
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0545
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_restrained_S_all      0.845
_refine_ls_shift/su_max          0.003
_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 1.057901(18) -0.124637(9) 0.795399(13) 0.01688(6) Uani 1 1 d U . .
P P 0.77494(12) -0.14480(5) 0.69133(9) 0.0154(3) Uani 1 1 d . . .
O1 O 0.7229(3) -0.19770(13) 0.6170(2) 0.0192(7) Uani 1 1 d . . .
O2 O 1.4147(3) -0.12098(17) 0.9250(2) 0.0392(9) Uani 1 1 d . . .
O3 O 1.1052(3) -0.05213(14) 0.9981(2) 0.0303(8) Uani 1 1 d . . .
O4 O 1.0228(4) -0.01328(15) 0.6583(3) 0.0371(9) Uani 1 1 d . . .
O5 O 1.0100(3) -0.18914(14) 0.5836(2) 0.0280(8) Uani 1 1 d . . .
O6 O 1.0896(3) -0.24063(15) 0.9194(2) 0.0294(8) Uani 1 1 d . . .
N1 N 0.7764(3) -0.13160(16) 0.8842(2) 0.0162(8) Uani 1 1 d . . .
H1A H 0.7803 -0.0955 0.8706 0.019 Uiso 1 1 calc R . .
N2 N 0.7039(3) -0.21972(16) 0.7889(3) 0.0182(9) Uani 1 1 d . . .
H2 H 0.6937 -0.2362 0.7306 0.022 Uiso 1 1 calc R . .
C1 C 0.7446(4) -0.1665(2) 0.8021(3) 0.0160(10) Uani 1 1 d . . .
C2 C 0.8069(5) -0.14347(19) 0.9965(3) 0.0195(11) Uani 1 1 d . . .
H2A H 0.7309 -0.1720 0.9847 0.023 Uiso 1 1 calc R . .
C3 C 0.9662(4) -0.1677(2) 1.0803(3) 0.0208(11) Uani 1 1 d . . .
H3A H 1.0430 -0.1398 1.0934 0.025 Uiso 1 1 calc R . .
H3B H 0.9773 -0.2026 1.0481 0.025 Uiso 1 1 calc R . .
C4 C 0.9936(5) -0.1814(2) 1.1936(3) 0.0243(12) Uani 1 1 d . . .
H4A H 0.9219 -0.2115 1.1813 0.029 Uiso 1 1 calc R . .
H4B H 1.0989 -0.1960 1.2488 0.029 Uiso 1 1 calc R . .
C5 C 0.9713(5) -0.1292(2) 1.2430(3) 0.0255(11) Uani 1 1 d . . .
H5A H 1.0524 -0.1012 1.2653 0.031 Uiso 1 1 calc R . .
H5B H 0.9808 -0.1399 1.3126 0.031 Uiso 1 1 calc R . .
C6 C 0.8147(5) -0.1020(2) 1.1564(3) 0.0267(12) Uani 1 1 d . . .
H6A H 0.7339 -0.1281 1.1423 0.032 Uiso 1 1 calc R . .
H6B H 0.8073 -0.0664 1.1890 0.032 Uiso 1 1 calc R . .
C7 C 0.7880(5) -0.0890(2) 1.0437(3) 0.0236(11) Uani 1 1 d . . .
H7A H 0.8622 -0.0601 1.0558 0.028 Uiso 1 1 calc R . .
H7B H 0.6837 -0.0736 0.9883 0.028 Uiso 1 1 calc R . .
C8 C 0.6713(5) -0.25784(19) 0.8527(3) 0.0191(11) Uani 1 1 d . . .
H8A H 0.7532 -0.2526 0.9365 0.023 Uiso 1 1 calc R . .
C9 C 0.5173(4) -0.2443(2) 0.8281(3) 0.0205(11) Uani 1 1 d . . .
H9A H 0.5111 -0.2029 0.8367 0.025 Uiso 1 1 calc R . .
H9B H 0.5113 -0.2637 0.8855 0.025 Uiso 1 1 calc R . .
C10 C 0.3809(5) -0.2624(2) 0.7082(3) 0.0263(12) Uani 1 1 d . . .
H10A H 0.2853 -0.2559 0.6999 0.032 Uiso 1 1 calc R . .
H10B H 0.3775 -0.2388 0.6504 0.032 Uiso 1 1 calc R . .
C11 C 0.3911(5) -0.3243(2) 0.6861(4) 0.0256(12) Uani 1 1 d . . .
H11A H 0.3031 -0.3345 0.6073 0.031 Uiso 1 1 calc R . .
H11B H 0.3873 -0.3482 0.7402 0.031 Uiso 1 1 calc R . .
C12 C 0.5400(5) -0.3354(2) 0.7011(3) 0.0256(12) Uani 1 1 d . . .
H12A H 0.5406 -0.3132 0.6437 0.031 Uiso 1 1 calc R . .
H12B H 0.5468 -0.3761 0.6881 0.031 Uiso 1 1 calc R . .
C13 C 0.6781(5) -0.3187(2) 0.8213(3) 0.0229(11) Uani 1 1 d . . .
H13A H 0.6846 -0.3446 0.8776 0.027 Uiso 1 1 calc R . .
H13B H 0.7721 -0.3237 0.8266 0.027 Uiso 1 1 calc R . .
C14 C 0.6217(4) -0.08861(19) 0.6111(3) 0.0146(10) Uani 1 1 d . . .
C15 C 0.6437(5) -0.03941(19) 0.6871(3) 0.0164(10) Uani 1 1 d . . .
C16 C 0.5286(5) -0.0391(2) 0.6969(3) 0.0183(10) Uani 1 1 d . . .
C17 C 0.4220(4) -0.0858(2) 0.6270(3) 0.0178(10) Uani 1 1 d . . .
C18 C 0.4705(4) -0.11361(19) 0.5744(3) 0.0166(10) Uani 1 1 d . . .
C19 C 0.6212(5) -0.0711(2) 0.5097(3) 0.0216(11) Uani 1 1 d . . .
H19A H 0.5472 -0.0404 0.4673 0.032 Uiso 1 1 calc R . .
H19B H 0.5927 -0.1037 0.4589 0.032 Uiso 1 1 calc R . .
H19C H 0.7232 -0.0579 0.5379 0.032 Uiso 1 1 calc R . .
C20 C 0.7633(5) 0.00576(19) 0.7266(3) 0.0214(11) Uani 1 1 d . . .
H20A H 0.8651 -0.0113 0.7770 0.032 Uiso 1 1 calc R . .
H20B H 0.7518 0.0352 0.7685 0.032 Uiso 1 1 calc R . .
H20C H 0.7507 0.0228 0.6601 0.032 Uiso 1 1 calc R . .
C21 C 0.4997(5) 0.0026(2) 0.7590(4) 0.0314(14) Uani 1 1 d . . .
H21A H 0.5875 0.0281 0.8040 0.047 Uiso 1 1 calc R . .
H21B H 0.4846 -0.0178 0.8102 0.047 Uiso 1 1 calc R . .
H21C H 0.4080 0.0247 0.7037 0.047 Uiso 1 1 calc R . .
C22 C 0.2765(5) -0.0955(2) 0.6153(4) 0.0331(13) Uani 1 1 d . . .
H22A H 0.3017 -0.1055 0.6900 0.050 Uiso 1 1 calc R . .
H22B H 0.2185 -0.1265 0.5611 0.050 Uiso 1 1 calc R . .
H22C H 0.2149 -0.0608 0.5871 0.050 Uiso 1 1 calc R . .
C23 C 0.3893(5) -0.1603(2) 0.4875(3) 0.0241(11) Uani 1 1 d . . .
H23A H 0.3704 -0.1484 0.4156 0.036 Uiso 1 1 calc R . .
H23B H 0.2917 -0.1683 0.4741 0.036 Uiso 1 1 calc R . .
H23C H 0.4527 -0.1946 0.5161 0.036 Uiso 1 1 calc R . .
C24 C 1.2834(5) -0.1228(2) 0.8779(3) 0.0266(11) Uani 1 1 d U . .
C25 C 1.0853(4) -0.0791(2) 0.9239(3) 0.0193(10) Uani 1 1 d U . .
C26 C 1.0333(5) -0.0529(2) 0.7083(4) 0.0221(10) Uani 1 1 d U . .
C27 C 1.0265(5) -0.1672(2) 0.6603(4) 0.0190(10) Uani 1 1 d U . .
C28 C 1.0797(5) -0.1989(2) 0.8766(3) 0.0206(10) Uani 1 1 d U . .


_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 C24 1.993(4) . ?
W C25 2.019(5) . ?
W C26 2.032(5) . ?
W C28 2.045(5) . ?
W C27 2.048(5) . ?
W P 2.5440(11) . ?
P O1 1.521(3) . ?
P C14 1.892(4) . ?
P C1 1.902(4) . ?
O2 C24 1.163(5) . ?
O3 C25 1.158(5) . ?
O4 C26 1.147(5) . ?
O5 C27 1.144(5) . ?
O6 C28 1.134(5) . ?
N1 C1 1.317(5) . ?
N1 C2 1.489(5) . ?
N1 H1A 0.8800 . ?
N2 C1 1.305(5) . ?
N2 C8 1.481(5) . ?
N2 H2 0.8800 . ?
C2 C3 1.518(5) . ?
C2 C7 1.528(6) . ?
C2 H2A 1.0000 . ?
C3 C4 1.527(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.517(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.532(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.519(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.520(6) . ?
C8 C9 1.529(6) . ?
C8 H8A 1.0000 . ?
C9 C10 1.531(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.511(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.528(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.529(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C18 1.517(6) . ?
C14 C15 1.520(6) . ?
C14 C19 1.531(5) . ?
C15 C16 1.348(6) . ?
C15 C20 1.507(6) . ?
C16 C17 1.478(6) . ?
C16 C21 1.492(6) . ?
C17 C18 1.335(6) . ?
C17 C22 1.511(6) . ?
C18 C23 1.502(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
C24 W C25 89.10(17) . . ?
C24 W C26 90.73(19) . . ?
C25 W C26 91.68(18) . . ?
C24 W C28 89.74(19) . . ?
C25 W C28 90.94(18) . . ?
C26 W C28 177.35(18) . . ?
C24 W C27 91.54(17) . . ?
C25 W C27 177.12(18) . . ?
C26 W C27 85.51(18) . . ?
C28 W C27 91.87(18) . . ?
C24 W P 170.50(16) . . ?
C25 W P 96.07(12) . . ?
C26 W P 97.06(12) . . ?
C28 W P 82.24(12) . . ?
C27 W P 83.69(12) . . ?
O1 P C14 108.48(17) . . ?
O1 P C1 101.76(19) . . ?
C14 P C1 100.04(18) . . ?
O1 P W 112.40(12) . . ?
C14 P W 123.25(14) . . ?
C1 P W 108.06(12) . . ?
C1 N1 C2 130.3(4) . . ?
C1 N1 H1A 114.9 . . ?
C2 N1 H1A 114.9 . . ?
C1 N2 C8 132.7(4) . . ?
C1 N2 H2 113.6 . . ?
C8 N2 H2 113.6 . . ?
N2 C1 N1 128.0(4) . . ?
N2 C1 P 110.5(3) . . ?
N1 C1 P 121.3(3) . . ?
N1 C2 C3 110.5(3) . . ?
N1 C2 C7 109.6(3) . . ?
C3 C2 C7 110.6(3) . . ?
N1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C7 C2 H2A 108.7 . . ?
C2 C3 C4 109.9(4) . . ?
C2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 C3 110.9(4) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 C6 111.4(3) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C7 C6 C5 111.9(4) . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C2 109.1(4) . . ?
C6 C7 H7A 109.9 . . ?
C2 C7 H7A 109.9 . . ?
C6 C7 H7B 109.9 . . ?
C2 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N2 C8 C13 108.0(4) . . ?
N2 C8 C9 111.7(3) . . ?
C13 C8 C9 111.8(4) . . ?
N2 C8 H8A 108.4 . . ?
C13 C8 H8A 108.4 . . ?
C9 C8 H8A 108.4 . . ?
C8 C9 C10 113.1(4) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C9 111.5(4) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 109.9(4) . . ?
C10 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C11 C12 C13 110.9(4) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C8 C13 C12 113.3(4) . . ?
C8 C13 H13A 108.9 . . ?
C12 C13 H13A 108.9 . . ?
C8 C13 H13B 108.9 . . ?
C12 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C18 C14 C15 102.6(3) . . ?
C18 C14 C19 112.9(3) . . ?
C15 C14 C19 113.9(4) . . ?
C18 C14 P 108.7(3) . . ?
C15 C14 P 112.7(3) . . ?
C19 C14 P 106.1(3) . . ?
C16 C15 C20 127.3(4) . . ?
C16 C15 C14 109.3(4) . . ?
C20 C15 C14 122.7(4) . . ?
C15 C16 C17 108.9(4) . . ?
C15 C16 C21 128.1(4) . . ?
C17 C16 C21 122.9(4) . . ?
C18 C17 C16 109.9(4) . . ?
C18 C17 C22 127.8(4) . . ?
C16 C17 C22 122.2(4) . . ?
C17 C18 C23 127.3(4) . . ?
C17 C18 C14 109.2(4) . . ?
C23 C18 C14 123.4(4) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 C24 W 179.0(5) . . ?
O3 C25 W 177.7(4) . . ?
O4 C26 W 177.6(4) . . ?
O5 C27 W 177.6(4) . . ?
O6 C28 W 178.6(4) . . ?

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
C24 W P O1 -33.4(8) . . . . ?
C25 W P O1 -156.10(18) . . . . ?
C26 W P O1 111.44(18) . . . . ?
C28 W P O1 -65.98(18) . . . . ?
C27 W P O1 26.79(18) . . . . ?
C24 W P C14 -166.3(7) . . . . ?
C25 W P C14 71.0(2) . . . . ?
C26 W P C14 -21.4(2) . . . . ?
C28 W P C14 161.2(2) . . . . ?
C27 W P C14 -106.1(2) . . . . ?
C24 W P C1 78.1(8) . . . . ?
C25 W P C1 -44.6(2) . . . . ?
C26 W P C1 -137.1(2) . . . . ?
C28 W P C1 45.5(2) . . . . ?
C27 W P C1 138.3(2) . . . . ?
C8 N2 C1 N1 3.8(7) . . . . ?
C8 N2 C1 P 177.8(3) . . . . ?
C2 N1 C1 N2 14.0(7) . . . . ?
C2 N1 C1 P -159.4(3) . . . . ?
O1 P C1 N2 5.8(3) . . . . ?
C14 P C1 N2 117.2(3) . . . . ?
W P C1 N2 -112.7(3) . . . . ?
O1 P C1 N1 -179.8(3) . . . . ?
C14 P C1 N1 -68.4(3) . . . . ?
W P C1 N1 61.7(3) . . . . ?
C1 N1 C2 C3 75.6(5) . . . . ?
C1 N1 C2 C7 -162.2(4) . . . . ?
N1 C2 C3 C4 -178.1(4) . . . . ?
C7 C2 C3 C4 60.3(5) . . . . ?
C2 C3 C4 C5 -57.1(5) . . . . ?
C3 C4 C5 C6 54.1(5) . . . . ?
C4 C5 C6 C7 -54.3(5) . . . . ?
C5 C6 C7 C2 56.2(5) . . . . ?
N1 C2 C7 C6 178.3(3) . . . . ?
C3 C2 C7 C6 -59.5(5) . . . . ?
C1 N2 C8 C13 -162.5(4) . . . . ?
C1 N2 C8 C9 74.2(5) . . . . ?
N2 C8 C9 C10 72.4(5) . . . . ?
C13 C8 C9 C10 -48.8(5) . . . . ?
C8 C9 C10 C11 53.8(5) . . . . ?
C9 C10 C11 C12 -57.8(5) . . . . ?
C10 C11 C12 C13 58.0(5) . . . . ?
N2 C8 C13 C12 -73.8(4) . . . . ?
C9 C8 C13 C12 49.5(5) . . . . ?
C11 C12 C13 C8 -54.6(5) . . . . ?
O1 P C14 C18 53.5(3) . . . . ?
C1 P C14 C18 -52.6(3) . . . . ?
W P C14 C18 -172.1(2) . . . . ?
O1 P C14 C15 166.5(3) . . . . ?
C1 P C14 C15 60.4(3) . . . . ?
W P C14 C15 -59.2(3) . . . . ?
O1 P C14 C19 -68.2(3) . . . . ?
C1 P C14 C19 -174.3(3) . . . . ?
W P C14 C19 66.2(3) . . . . ?
C18 C14 C15 C16 3.2(4) . . . . ?
C19 C14 C15 C16 125.6(4) . . . . ?
P C14 C15 C16 -113.5(3) . . . . ?
C18 C14 C15 C20 -167.9(3) . . . . ?
C19 C14 C15 C20 -45.6(5) . . . . ?
P C14 C15 C20 75.4(4) . . . . ?
C20 C15 C16 C17 168.9(4) . . . . ?
C14 C15 C16 C17 -1.7(5) . . . . ?
C20 C15 C16 C21 -6.8(7) . . . . ?
C14 C15 C16 C21 -177.4(4) . . . . ?
C15 C16 C17 C18 -0.8(5) . . . . ?
C21 C16 C17 C18 175.2(4) . . . . ?
C15 C16 C17 C22 -177.2(4) . . . . ?
C21 C16 C17 C22 -1.3(6) . . . . ?
C16 C17 C18 C23 -174.1(4) . . . . ?
C22 C17 C18 C23 2.1(8) . . . . ?
C16 C17 C18 C14 2.9(5) . . . . ?
C22 C17 C18 C14 179.1(4) . . . . ?
C15 C14 C18 C17 -3.7(4) . . . . ?
C19 C14 C18 C17 -126.7(4) . . . . ?
P C14 C18 C17 115.9(3) . . . . ?
C15 C14 C18 C23 173.4(4) . . . . ?
C19 C14 C18 C23 50.4(6) . . . . ?
P C14 C18 C23 -67.0(4) . . . . ?
C25 W C24 O2 -97(29) . . . . ?
C26 W C24 O2 -5(29) . . . . ?
C28 W C24 O2 172(100) . . . . ?
C27 W C24 O2 80(29) . . . . ?
P W C24 O2 140(29) . . . . ?
C24 W C25 O3 31(10) . . . . ?
C26 W C25 O3 -59(10) . . . . ?
C28 W C25 O3 121(10) . . . . ?
C27 W C25 O3 -72(11) . . . . ?
P W C25 O3 -157(10) . . . . ?
C24 W C26 O4 47(10) . . . . ?
C25 W C26 O4 136(10) . . . . ?
C28 W C26 O4 -53(12) . . . . ?
C27 W C26 O4 -45(10) . . . . ?
P W C26 O4 -128(10) . . . . ?
C24 W C27 O5 -75(9) . . . . ?
C25 W C27 O5 28(11) . . . . ?
C26 W C27 O5 16(9) . . . . ?
C28 W C27 O5 -165(9) . . . . ?
P W C27 O5 113(9) . . . . ?
C24 W C28 O6 -128(17) . . . . ?
C25 W C28 O6 143(17) . . . . ?
C26 W C28 O6 -28(20) . . . . ?
C27 W C28 O6 -36(17) . . . . ?
P W C28 O6 47(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         2.838
_refine_diff_density_min         -2.320
_refine_diff_density_rms         0.189
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3299f
_database_code_depnum_ccdc_archive 'CCDC 1039384'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H29 N2 O5 P W'
_chemical_formula_sum            'C22 H29 N2 O5 P W'
_chemical_formula_weight         616.29

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'
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'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9909(5)
_cell_length_b                   11.0605(6)
_cell_length_c                   12.8740(10)
_cell_angle_alpha                108.084(4)
_cell_angle_beta                 95.194(4)
_cell_angle_gamma                118.186(2)
_cell_volume                     1257.68(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5171
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      29.22

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    4.688
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3753
_exptl_absorpt_correction_T_max  0.9121
_exptl_absorpt_process_details   'Sadabs 2008/2'

_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  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'φ and ω CCD rotation images, thin slices'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12812
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         28.00
_reflns_number_total             6035
_reflns_number_gt                5137
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0451P)²+5.0322P] where P=(Fo²+2Fc²)/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         6035
_refine_ls_number_parameters     289
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1026
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.054
_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
C1 C 0.5052(8) 0.1982(8) 0.2232(7) 0.0595(19) Uani 1 1 d U . .
C2 C 0.3921(9) 0.2994(10) 0.1081(6) 0.0555(19) Uani 1 1 d U . .
H2A H 0.2898 0.2716 0.0992 0.067 Uiso 1 1 calc R . .
C3 C 0.4773(12) 0.4556(12) 0.1893(9) 0.093(3) Uani 1 1 d U . .
H3A H 0.4527 0.5159 0.1605 0.111 Uiso 1 1 calc R . .
H3B H 0.5799 0.4927 0.1993 0.111 Uiso 1 1 calc R . .
H3C H 0.4565 0.4633 0.2627 0.111 Uiso 1 1 calc R . .
C4 C 0.4105(10) 0.2770(10) -0.0101(6) 0.059(2) Uani 1 1 d U . .
H4C H 0.3514 0.1701 -0.0602 0.070 Uiso 1 1 calc R . .
H4B H 0.5119 0.3135 -0.0066 0.070 Uiso 1 1 calc R . .
H4A H 0.3802 0.3327 -0.0402 0.070 Uiso 1 1 calc R . .
C5 C 0.7030(10) 0.2502(9) 0.3452(6) 0.060(2) Uani 1 1 d U . .
H5A H 0.6283 0.1856 0.3748 0.072 Uiso 1 1 calc R . .
C6 C 0.8059(13) 0.4105(12) 0.4320(9) 0.095(3) Uani 1 1 d U . .
H6A H 0.8855 0.4619 0.4023 0.114 Uiso 1 1 calc R . .
H6B H 0.8441 0.4095 0.5033 0.114 Uiso 1 1 calc R . .
H6C H 0.7544 0.4633 0.4463 0.114 Uiso 1 1 calc R . .
C7 C 0.7873(11) 0.1852(11) 0.2936(7) 0.067(2) Uani 1 1 d U . .
H7C H 0.7208 0.0816 0.2384 0.080 Uiso 1 1 calc R . .
H7B H 0.8499 0.1866 0.3538 0.080 Uiso 1 1 calc R . .
H7A H 0.8462 0.2449 0.2550 0.080 Uiso 1 1 calc R . .
C8 C 0.2642(6) -0.1225(5) 0.1273(4) 0.0242(10) Uani 1 1 d . . .
C9 C 0.1075(6) -0.1922(6) 0.0728(5) 0.0288(12) Uani 1 1 d . . .
C10 C 0.0297(6) -0.3034(6) 0.1058(5) 0.0338(13) Uani 1 1 d . . .
C11 C 0.1281(7) -0.3114(6) 0.1856(5) 0.0363(14) Uani 1 1 d . . .
C12 C 0.2648(6) -0.2088(6) 0.1988(5) 0.0287(11) Uani 1 1 d . . .
C13 C 0.3511(7) -0.1244(6) 0.0417(5) 0.0316(12) Uani 1 1 d . . .
H13A H 0.3479 -0.0641 0.0009 0.038 Uiso 1 1 calc R . .
H13B H 0.3101 -0.2278 -0.0128 0.038 Uiso 1 1 calc R . .
H13C H 0.4512 -0.0826 0.0820 0.038 Uiso 1 1 calc R . .
C14 C 0.0549(8) -0.1423(8) -0.0060(6) 0.0443(16) Uani 1 1 d . . .
H14A H 0.0936 -0.1545 -0.0716 0.053 Uiso 1 1 calc R . .
H14B H 0.0870 -0.0365 0.0340 0.053 Uiso 1 1 calc R . .
H14C H -0.0505 -0.2028 -0.0324 0.053 Uiso 1 1 calc R . .
C15 C -0.1304(7) -0.4062(7) 0.0697(8) 0.057(2) Uani 1 1 d . . .
H15A H -0.1564 -0.5076 0.0212 0.068 Uiso 1 1 calc R . .
H15B H -0.1750 -0.3708 0.0271 0.068 Uiso 1 1 calc R . .
H15C H -0.1647 -0.4074 0.1373 0.068 Uiso 1 1 calc R . .
C16 C 0.0734(10) -0.4242(8) 0.2374(8) 0.062(2) Uani 1 1 d . . .
H16A H 0.0100 -0.5248 0.1770 0.075 Uiso 1 1 calc R . .
H16B H 0.0195 -0.4018 0.2890 0.075 Uiso 1 1 calc R . .
H16C H 0.1548 -0.4198 0.2803 0.075 Uiso 1 1 calc R . .
C17 C 0.4005(8) -0.1797(8) 0.2671(6) 0.0437(15) Uani 1 1 d . . .
H17C H 0.3768 -0.2469 0.3069 0.052 Uiso 1 1 calc R . .
H17B H 0.4569 -0.0754 0.3229 0.052 Uiso 1 1 calc R . .
H17A H 0.4568 -0.1977 0.2162 0.052 Uiso 1 1 calc R . .
C18 C 0.1419(8) 0.1974(7) 0.5088(6) 0.0438(16) Uani 1 1 d . . .
C19 C 0.2339(7) -0.0122(7) 0.4400(5) 0.0397(14) Uani 1 1 d . . .
C20 C 0.4207(7) 0.2981(8) 0.4806(6) 0.0449(16) Uani 1 1 d . . .
C21 C 0.1969(6) 0.2745(6) 0.3209(5) 0.0317(12) Uani 1 1 d . . .
C22 C 0.0114(7) -0.0270(7) 0.2825(6) 0.0379(14) Uani 1 1 d . . .
N1 N 0.4031(8) 0.1817(8) 0.1501(6) 0.0583(15) Uani 1 1 d U . .
N2 N 0.6442(8) 0.2785(8) 0.2544(6) 0.0587(16) Uani 1 1 d U . .
O1 O 0.1017(7) 0.2374(6) 0.5827(5) 0.0698(19) Uani 1 1 d . . .
O2 O 0.2433(7) -0.0892(7) 0.4768(4) 0.0593(14) Uani 1 1 d . . .
O3 O 0.5339(6) 0.3901(7) 0.5394(5) 0.076(2) Uani 1 1 d . . .
O4 O 0.1790(5) 0.3500(5) 0.2878(4) 0.0458(11) Uani 1 1 d . . .
O5 O -0.1060(5) -0.1065(6) 0.2322(5) 0.0595(15) Uani 1 1 d . . .
P P 0.33170(15) 0.07156(15) 0.23051(12) 0.0265(3) Uani 1 1 d . . .
W W 0.21888(2) 0.13295(2) 0.380445(19) 0.02919(9) Uani 1 1 d . . .


_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
C1 N2 1.291(10) . ?
C1 N1 1.299(11) . ?
C1 P 1.789(7) . ?
C2 C3 1.459(12) . ?
C2 C4 1.513(10) . ?
C2 N1 1.604(10) . ?
C2 H2A 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4C 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4A 0.9800 . ?
C5 N2 1.470(10) . ?
C5 C7 1.504(12) . ?
C5 C6 1.523(13) . ?
C5 H5A 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7C 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7A 0.9800 . ?
C8 C9 1.498(7) . ?
C8 C12 1.519(8) . ?
C8 C13 1.524(7) . ?
C8 P 1.863(5) . ?
C9 C10 1.349(8) . ?
C9 C14 1.488(9) . ?
C10 C11 1.476(9) . ?
C10 C15 1.496(8) . ?
C11 C12 1.340(9) . ?
C11 C16 1.499(9) . ?
C12 C17 1.495(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17C 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17A 0.9800 . ?
C18 O1 1.138(8) . ?
C18 W 2.012(7) . ?
C19 O2 1.134(8) . ?
C19 W 2.045(7) . ?
C20 O3 1.146(8) . ?
C20 W 2.027(7) . ?
C21 O4 1.131(8) . ?
C21 W 2.041(7) . ?
C22 O5 1.132(8) . ?
C22 W 2.050(6) . ?
N1 P 1.789(7) . ?
P W 2.4778(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
N2 C1 N1 135.6(9) . . ?
N2 C1 P 155.5(8) . . ?
N1 C1 P 68.7(4) . . ?
C3 C2 C4 113.5(8) . . ?
C3 C2 N1 115.8(8) . . ?
C4 C2 N1 111.9(6) . . ?
C3 C2 H2A 104.8 . . ?
C4 C2 H2A 104.8 . . ?
N1 C2 H2A 104.8 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4C 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4C C4 H4B 109.5 . . ?
C2 C4 H4A 109.5 . . ?
H4C C4 H4A 109.5 . . ?
H4B C4 H4A 109.5 . . ?
N2 C5 C7 104.2(7) . . ?
N2 C5 C6 100.0(8) . . ?
C7 C5 C6 109.7(9) . . ?
N2 C5 H5A 113.9 . . ?
C7 C5 H5A 113.9 . . ?
C6 C5 H5A 113.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7C 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7C C7 H7B 109.5 . . ?
C5 C7 H7A 109.5 . . ?
H7C C7 H7A 109.5 . . ?
H7B C7 H7A 109.5 . . ?
C9 C8 C12 103.7(4) . . ?
C9 C8 C13 113.3(5) . . ?
C12 C8 C13 114.4(4) . . ?
C9 C8 P 106.8(3) . . ?
C12 C8 P 105.9(3) . . ?
C13 C8 P 111.9(4) . . ?
C10 C9 C14 128.3(6) . . ?
C10 C9 C8 109.0(5) . . ?
C14 C9 C8 122.7(5) . . ?
C9 C10 C11 109.2(5) . . ?
C9 C10 C15 127.5(6) . . ?
C11 C10 C15 123.3(6) . . ?
C12 C11 C10 109.8(5) . . ?
C12 C11 C16 128.5(7) . . ?
C10 C11 C16 121.8(6) . . ?
C11 C12 C17 128.9(6) . . ?
C11 C12 C8 108.4(5) . . ?
C17 C12 C8 122.7(5) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17C 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17C C17 H17B 109.5 . . ?
C12 C17 H17A 109.5 . . ?
H17C C17 H17A 109.5 . . ?
H17B C17 H17A 109.5 . . ?
O1 C18 W 178.2(6) . . ?
O2 C19 W 177.6(6) . . ?
O3 C20 W 178.2(7) . . ?
O4 C21 W 177.2(5) . . ?
O5 C22 W 174.2(5) . . ?
C1 N1 C2 131.1(7) . . ?
C1 N1 P 68.7(5) . . ?
C2 N1 P 142.9(5) . . ?
C1 N2 C5 110.5(8) . . ?
N1 P C1 42.6(4) . . ?
N1 P C8 103.2(3) . . ?
C1 P C8 109.9(3) . . ?
N1 P W 123.5(2) . . ?
C1 P W 125.1(2) . . ?
C8 P W 123.90(17) . . ?
C18 W C20 88.8(3) . . ?
C18 W C21 88.5(3) . . ?
C20 W C21 91.5(3) . . ?
C18 W C19 90.4(3) . . ?
C20 W C19 90.0(3) . . ?
C21 W C19 178.1(2) . . ?
C18 W C22 88.9(3) . . ?
C20 W C22 177.2(2) . . ?
C21 W C22 86.7(2) . . ?
C19 W C22 91.7(3) . . ?
C18 W P 175.6(2) . . ?
C20 W P 86.91(18) . . ?
C21 W P 90.66(15) . . ?
C19 W P 90.56(18) . . ?
C22 W P 95.32(17) . . ?

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
C12 C8 C9 C10 -1.1(6) . . . . ?
C13 C8 C9 C10 123.6(5) . . . . ?
P C8 C9 C10 -112.7(4) . . . . ?
C12 C8 C9 C14 -180.0(5) . . . . ?
C13 C8 C9 C14 -55.3(7) . . . . ?
P C8 C9 C14 68.4(6) . . . . ?
C14 C9 C10 C11 -179.6(5) . . . . ?
C8 C9 C10 C11 1.6(6) . . . . ?
C14 C9 C10 C15 0.8(10) . . . . ?
C8 C9 C10 C15 -178.0(5) . . . . ?
C9 C10 C11 C12 -1.6(6) . . . . ?
C15 C10 C11 C12 178.1(5) . . . . ?
C9 C10 C11 C16 179.8(5) . . . . ?
C15 C10 C11 C16 -0.5(9) . . . . ?
C10 C11 C12 C17 -177.3(5) . . . . ?
C16 C11 C12 C17 1.1(10) . . . . ?
C10 C11 C12 C8 0.9(6) . . . . ?
C16 C11 C12 C8 179.3(6) . . . . ?
C9 C8 C12 C11 0.1(6) . . . . ?
C13 C8 C12 C11 -123.9(5) . . . . ?
P C8 C12 C11 112.4(4) . . . . ?
C9 C8 C12 C17 178.4(5) . . . . ?
C13 C8 C12 C17 54.4(7) . . . . ?
P C8 C12 C17 -69.3(6) . . . . ?
N2 C1 N1 C2 -34.0(13) . . . . ?
P C1 N1 C2 142.7(8) . . . . ?
N2 C1 N1 P -176.7(10) . . . . ?
C3 C2 N1 C1 -27.0(11) . . . . ?
C4 C2 N1 C1 105.1(9) . . . . ?
C3 C2 N1 P 83.8(11) . . . . ?
C4 C2 N1 P -144.1(8) . . . . ?
N1 C1 N2 C5 178.9(8) . . . . ?
P C1 N2 C5 6.4(18) . . . . ?
C7 C5 N2 C1 117.1(8) . . . . ?
C6 C5 N2 C1 -129.5(8) . . . . ?
C2 N1 P C1 -130.9(11) . . . . ?
C1 N1 P C8 -105.1(4) . . . . ?
C2 N1 P C8 124.0(9) . . . . ?
C1 N1 P W 107.4(4) . . . . ?
C2 N1 P W -23.5(10) . . . . ?
N2 C1 P N1 174.4(17) . . . . ?
N2 C1 P C8 -97.5(14) . . . . ?
N1 C1 P C8 88.1(5) . . . . ?
N2 C1 P W 71.0(16) . . . . ?
N1 C1 P W -103.4(4) . . . . ?
C9 C8 P N1 -94.7(4) . . . . ?
C12 C8 P N1 155.2(4) . . . . ?
C13 C8 P N1 29.9(5) . . . . ?
C9 C8 P C1 -138.7(5) . . . . ?
C12 C8 P C1 111.2(5) . . . . ?
C13 C8 P C1 -14.1(6) . . . . ?
C9 C8 P W 52.6(4) . . . . ?
C12 C8 P W -57.5(4) . . . . ?
C13 C8 P W 177.2(3) . . . . ?
O1 C18 W C20 19(23) . . . . ?
O1 C18 W C21 -73(23) . . . . ?
O1 C18 W C19 109(23) . . . . ?
O1 C18 W C22 -160(23) . . . . ?
O1 C18 W P 7(26) . . . . ?
O3 C20 W C18 50(21) . . . . ?
O3 C20 W C21 139(21) . . . . ?
O3 C20 W C19 -40(21) . . . . ?
O3 C20 W C22 88(23) . . . . ?
O3 C20 W P -131(21) . . . . ?
O4 C21 W C18 -56(10) . . . . ?
O4 C21 W C20 -145(10) . . . . ?
O4 C21 W C19 -2(14) . . . . ?
O4 C21 W C22 33(10) . . . . ?
O4 C21 W P 128(10) . . . . ?
O2 C19 W C18 -33(15) . . . . ?
O2 C19 W C20 55(15) . . . . ?
O2 C19 W C21 -88(17) . . . . ?
O2 C19 W C22 -122(15) . . . . ?
O2 C19 W P 142(15) . . . . ?
O5 C22 W C18 41(7) . . . . ?
O5 C22 W C20 4(11) . . . . ?
O5 C22 W C21 -47(7) . . . . ?
O5 C22 W C19 132(7) . . . . ?
O5 C22 W P -138(7) . . . . ?
N1 P W C18 -63(3) . . . . ?
C1 P W C18 -11(3) . . . . ?
C8 P W C18 156(3) . . . . ?
N1 P W C20 -74.9(4) . . . . ?
C1 P W C20 -22.8(5) . . . . ?
C8 P W C20 144.2(3) . . . . ?
N1 P W C21 16.5(3) . . . . ?
C1 P W C21 68.6(5) . . . . ?
C8 P W C21 -124.4(3) . . . . ?
N1 P W C19 -164.9(4) . . . . ?
C1 P W C19 -112.8(5) . . . . ?
C8 P W C19 54.2(3) . . . . ?
N1 P W C22 103.3(4) . . . . ?
C1 P W C22 155.4(5) . . . . ?
C8 P W C22 -37.6(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.699
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.154
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3677f
_database_code_depnum_ccdc_archive 'CCDC 1039385'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_audit_creation_date             2014-09-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C22 H31 N2 O6 P W'
_chemical_formula_sum            'C22 H31 N2 O6 P W'
_chemical_formula_weight         634.31
_chemical_melting_point          ?
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.5748(5)
_cell_length_b                   27.7242(13)
_cell_length_c                   10.5851(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.3400(10)
_cell_angle_gamma                90.00
_cell_volume                     2539.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.35
_exptl_absorpt_coefficient_mu    4.649
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5227
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.7007.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19281
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.77
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'φ and ω CCD rotation images, thin slices'
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_reflns_number_gt                5448
_reflns_number_total             6102
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         6102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0204P)²+1.3296P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0476
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2A), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
W W 0.529531(10) 0.877994(3) 0.161747(9) 0.01238(4) Uani 1 d . . .
P P 0.24115(7) 0.86259(2) 0.03282(6) 0.01103(11) Uani 1 d . . .
O1 O 0.18821(19) 0.82082(6) 0.09465(16) 0.0149(3) Uani 1 d . . .
O2 O 0.8890(2) 0.88539(7) 0.3426(2) 0.0277(4) Uani 1 d . . .
O3 O 0.5211(3) 0.97874(7) 0.3032(2) 0.0352(5) Uani 1 d . . .
O4 O 0.5433(2) 0.92383(7) -0.10733(18) 0.0245(4) Uani 1 d . . .
O5 O 0.5685(3) 0.77593(7) 0.0443(2) 0.0334(5) Uani 1 d . . .
O6 O 0.4838(2) 0.82316(7) 0.40625(19) 0.0295(5) Uani 1 d . . .
N1 N 0.2193(2) 0.86284(7) -0.24293(19) 0.0138(4) Uani 1 d . . .
H1 H 0.2327 0.8941 -0.2282 0.017 Uiso 1 calc . . R
N2 N 0.1309(2) 0.79535(7) -0.1631(2) 0.0141(4) Uani 1 d . . .
H2 H 0.1475 0.7817 -0.0828 0.017 Uiso 1 calc . . R
C1 C 0.1888(3) 0.83889(8) -0.1500(2) 0.0128(4) Uani 1 d . . .
C2 C 0.2343(3) 0.84493(9) -0.3687(2) 0.0166(5) Uani 1 d . . .
H2A H 0.1366 0.8281 -0.4314 0.020 Uiso 1 calc . . R
C3 C 0.2582(3) 0.88836(9) -0.4445(3) 0.0215(5) Uani 1 d . . .
H3A H 0.1704 0.9104 -0.4698 0.032 Uiso 1 calc . . GR
H3B H 0.2662 0.8777 -0.5294 0.032 Uiso 1 calc . . GR
H3C H 0.3535 0.9050 -0.3832 0.032 Uiso 1 calc . . GR
C4 C 0.3686(3) 0.80952(10) -0.3251(3) 0.0231(6) Uani 1 d . . .
H4A H 0.4654 0.8263 -0.2682 0.035 Uiso 1 calc . . GR
H4B H 0.3740 0.7962 -0.4086 0.035 Uiso 1 calc . . GR
H4C H 0.3529 0.7833 -0.2704 0.035 Uiso 1 calc . . GR
C5 C 0.0435(3) 0.76448(9) -0.2855(2) 0.0181(5) Uani 1 d . . .
H5 H 0.1076 0.7583 -0.3376 0.022 Uiso 1 calc . . R
C6 C -0.1065(3) 0.78952(10) -0.3822(3) 0.0245(6) Uani 1 d . . .
H6A H -0.1727 0.7935 -0.3335 0.037 Uiso 1 calc . . GR
H6B H -0.1603 0.7698 -0.4662 0.037 Uiso 1 calc . . GR
H6C H -0.0827 0.8212 -0.4090 0.037 Uiso 1 calc . . GR
C7 C 0.0145(4) 0.71740(9) -0.2286(3) 0.0258(6) Uani 1 d . . .
H7A H 0.1136 0.7022 -0.1697 0.039 Uiso 1 calc . . GR
H7B H -0.0457 0.6959 -0.3064 0.039 Uiso 1 calc . . GR
H7C H -0.0431 0.7236 -0.1729 0.039 Uiso 1 calc . . GR
C8 C 0.0907(3) 0.91206(8) -0.0131(2) 0.0133(4) Uani 1 d . . .
C9 C 0.1149(3) 0.95166(8) -0.1008(2) 0.0155(5) Uani 1 d . . .
C10 C -0.0061(3) 0.95151(8) -0.2284(2) 0.0159(5) Uani 1 d . . .
C11 C -0.1181(3) 0.91493(8) -0.2332(2) 0.0157(5) Uani 1 d . . .
C12 C -0.0658(3) 0.89199(8) -0.1091(2) 0.0139(5) Uani 1 d . . .
C13 C 0.0998(3) 0.92973(9) 0.1279(2) 0.0183(5) Uani 1 d . . .
H13A H 0.0774 0.9029 0.1766 0.027 Uiso 1 calc . . GR
H13B H 0.0240 0.9555 0.1118 0.027 Uiso 1 calc . . GR
H13C H 0.2038 0.9421 0.1853 0.027 Uiso 1 calc . . GR
C14 C 0.2425(3) 0.98810(9) -0.0454(3) 0.0207(5) Uani 1 d . . .
H14A H 0.2388 1.0049 0.0345 0.031 Uiso 1 calc . . GR
H14B H 0.2300 1.0115 -0.1189 0.031 Uiso 1 calc . . GR
H14C H 0.3423 0.9717 -0.0156 0.031 Uiso 1 calc . . GR
C15 C -0.0329(3) 0.98375(9) -0.3509(2) 0.0233(6) Uani 1 d . . .
H15A H -0.0407 0.9641 -0.4306 0.035 Uiso 1 calc . . GR
H15B H 0.0537 1.0063 -0.3258 0.035 Uiso 1 calc . . GR
H15C H -0.1290 1.0019 -0.3761 0.035 Uiso 1 calc . . GR
C16 C -0.2700(3) 0.90832(10) -0.3585(3) 0.0240(6) Uani 1 d . . .
H16A H -0.3260 0.8812 -0.3422 0.036 Uiso 1 calc . . GR
H16B H -0.2514 0.9016 -0.4410 0.036 Uiso 1 calc . . GR
H16C H -0.3318 0.9378 -0.3742 0.036 Uiso 1 calc . . GR
C17 C -0.1490(3) 0.85415(9) -0.0657(3) 0.0201(5) Uani 1 d . . .
H17A H -0.1638 0.8657 0.0153 0.030 Uiso 1 calc . . GR
H17B H -0.0876 0.8245 -0.0407 0.030 Uiso 1 calc . . GR
H17C H -0.2499 0.8477 -0.1432 0.030 Uiso 1 calc . . GR
C18 C 0.7580(3) 0.88238(9) 0.2752(3) 0.0188(5) Uani 1 d . . .
C19 C 0.5180(3) 0.94299(9) 0.2486(3) 0.0209(5) Uani 1 d . . .
C20 C 0.5408(3) 0.90850(8) -0.0078(2) 0.0163(5) Uani 1 d . . .
C21 C 0.5533(3) 0.81245(9) 0.0861(3) 0.0197(5) Uani 1 d . . .
C22 C 0.5003(3) 0.84314(9) 0.3205(2) 0.0183(5) Uani 1 d . . .


_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 P 2.5384(6) . ?
W C18 1.998(3) . ?
W C19 2.047(3) . ?
W C20 2.028(2) . ?
W C21 2.037(3) . ?
W C22 2.058(3) . ?
P O1 1.5201(16) . ?
P C1 1.897(2) . ?
P C8 1.896(2) . ?
O2 C18 1.151(3) . ?
O3 C19 1.141(3) . ?
O4 C20 1.146(3) . ?
O5 C21 1.139(3) . ?
O6 C22 1.131(3) . ?
N1 H1 0.8800 . ?
N1 C1 1.319(3) . ?
N1 C2 1.485(3) . ?
N2 H2 0.8800 . ?
N2 C1 1.311(3) . ?
N2 C5 1.477(3) . ?
C2 H2A 1.0000 . ?
C2 C3 1.517(3) . ?
C2 C4 1.524(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 1.0000 . ?
C5 C6 1.528(4) . ?
C5 C7 1.512(3) . ?
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 C9 1.518(3) . ?
C8 C12 1.511(3) . ?
C8 C13 1.538(3) . ?
C9 C10 1.352(3) . ?
C9 C14 1.498(3) . ?
C10 C11 1.461(3) . ?
C10 C15 1.504(3) . ?
C11 C12 1.348(3) . ?
C11 C16 1.502(3) . ?
C12 C17 1.503(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

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
C18 W P 172.93(7) . . ?
C18 W C19 86.11(10) . . ?
C18 W C20 92.71(10) . . ?
C18 W C21 90.73(10) . . ?
C18 W C22 91.97(10) . . ?
C19 W P 97.71(8) . . ?
C19 W C22 89.68(10) . . ?
C20 W P 92.97(7) . . ?
C20 W C19 93.66(10) . . ?
C20 W C21 88.11(10) . . ?
C20 W C22 174.43(9) . . ?
C21 W P 85.27(8) . . ?
C21 W C19 176.44(10) . . ?
C21 W C22 88.80(10) . . ?
C22 W P 82.14(7) . . ?
O1 P W 112.53(7) . . ?
O1 P C1 100.61(10) . . ?
O1 P C8 107.75(10) . . ?
C1 P W 111.01(8) . . ?
C8 P W 123.28(8) . . ?
C8 P C1 98.56(10) . . ?
C1 N1 H1 115.2 . . ?
C1 N1 C2 129.6(2) . . ?
C2 N1 H1 115.2 . . ?
C1 N2 H2 113.5 . . ?
C1 N2 C5 132.99(19) . . ?
C5 N2 H2 113.5 . . ?
N1 C1 P 122.71(17) . . ?
N2 C1 P 110.03(16) . . ?
N2 C1 N1 127.1(2) . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 C3 107.65(19) . . ?
N1 C2 C4 109.67(19) . . ?
C3 C2 H2A 109.2 . . ?
C3 C2 C4 111.9(2) . . ?
C4 C2 H2A 109.2 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5 109.4 . . ?
N2 C5 C6 110.0(2) . . ?
N2 C5 C7 106.43(19) . . ?
C6 C5 H5 109.4 . . ?
C7 C5 H5 109.4 . . ?
C7 C5 C6 112.3(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 P 112.45(16) . . ?
C9 C8 C13 113.75(19) . . ?
C12 C8 P 109.40(15) . . ?
C12 C8 C9 102.87(18) . . ?
C12 C8 C13 113.5(2) . . ?
C13 C8 P 105.07(15) . . ?
C10 C9 C8 108.6(2) . . ?
C10 C9 C14 126.9(2) . . ?
C14 C9 C8 124.1(2) . . ?
C9 C10 C11 109.8(2) . . ?
C9 C10 C15 128.1(2) . . ?
C11 C10 C15 122.1(2) . . ?
C10 C11 C16 122.3(2) . . ?
C12 C11 C10 109.4(2) . . ?
C12 C11 C16 128.2(2) . . ?
C11 C12 C8 109.2(2) . . ?
C11 C12 C17 127.0(2) . . ?
C17 C12 C8 123.7(2) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 W 178.6(2) . . ?
O3 C19 W 175.6(2) . . ?
O4 C20 W 176.7(2) . . ?
O5 C21 W 179.1(2) . . ?
O6 C22 W 178.7(2) . . ?

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
N2 H2 O1 0.88 2.06 2.639(2) 122.8 .

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
W P C1 N1 -58.2(2) . . . . ?
W P C1 N2 117.31(16) . . . . ?
W P C8 C9 57.21(18) . . . . ?
W P C8 C12 170.85(12) . . . . ?
W P C8 C13 -67.02(17) . . . . ?
P W C18 O2 -90(10) . . . . ?
P W C19 O3 159(3) . . . . ?
P W C20 O4 -50(4) . . . . ?
P W C21 O5 168(100) . . . . ?
P W C22 O6 71(10) . . . . ?
P C8 C9 C10 114.60(19) . . . . ?
P C8 C9 C14 -72.5(3) . . . . ?
P C8 C12 C11 -117.17(19) . . . . ?
P C8 C12 C17 65.7(3) . . . . ?
O1 P C1 N1 -177.5(2) . . . . ?
O1 P C1 N2 -2.00(19) . . . . ?
O1 P C8 C9 -169.06(16) . . . . ?
O1 P C8 C12 -55.42(17) . . . . ?
O1 P C8 C13 66.71(17) . . . . ?
C1 P C8 C9 -64.96(18) . . . . ?
C1 P C8 C12 48.68(17) . . . . ?
C1 P C8 C13 170.81(16) . . . . ?
C1 N1 C2 C3 175.8(2) . . . . ?
C1 N1 C2 C4 -62.3(3) . . . . ?
C1 N2 C5 C6 -59.7(3) . . . . ?
C1 N2 C5 C7 178.5(3) . . . . ?
C2 N1 C1 P 158.16(19) . . . . ?
C2 N1 C1 N2 -16.5(4) . . . . ?
C5 N2 C1 P 165.3(2) . . . . ?
C5 N2 C1 N1 -19.5(4) . . . . ?
C8 P C1 N1 72.6(2) . . . . ?
C8 P C1 N2 -111.99(18) . . . . ?
C8 C9 C10 C11 2.4(3) . . . . ?
C8 C9 C10 C15 -179.4(2) . . . . ?
C9 C8 C12 C11 2.5(2) . . . . ?
C9 C8 C12 C17 -174.6(2) . . . . ?
C9 C10 C11 C12 -0.7(3) . . . . ?
C9 C10 C11 C16 175.9(2) . . . . ?
C10 C11 C12 C8 -1.3(3) . . . . ?
C10 C11 C12 C17 175.8(2) . . . . ?
C12 C8 C9 C10 -3.0(2) . . . . ?
C12 C8 C9 C14 169.9(2) . . . . ?
C13 C8 C9 C10 -126.1(2) . . . . ?
C13 C8 C9 C14 46.8(3) . . . . ?
C13 C8 C12 C11 125.9(2) . . . . ?
C13 C8 C12 C17 -51.3(3) . . . . ?
C14 C9 C10 C11 -170.3(2) . . . . ?
C14 C9 C10 C15 7.9(4) . . . . ?
C15 C10 C11 C12 -179.0(2) . . . . ?
C15 C10 C11 C16 -2.3(4) . . . . ?
C16 C11 C12 C8 -177.7(2) . . . . ?
C16 C11 C12 C17 -0.7(4) . . . . ?
C18 W P O1 11.0(6) . . . . ?
C18 W P C1 -100.9(6) . . . . ?
C18 W P C8 142.9(6) . . . . ?
C18 W C19 O3 -15(3) . . . . ?
C18 W C20 O4 126(4) . . . . ?
C18 W C21 O5 -18(15) . . . . ?
C18 W C22 O6 -105(10) . . . . ?
C19 W P O1 -111.39(10) . . . . ?
C19 W P C1 136.72(10) . . . . ?
C19 W P C8 20.45(11) . . . . ?
C19 W C18 O2 33(10) . . . . ?
C19 W C20 O4 -148(4) . . . . ?
C19 W C21 O5 -45(16) . . . . ?
C19 W C22 O6 169(10) . . . . ?
C20 W P O1 154.51(10) . . . . ?
C20 W P C1 42.63(10) . . . . ?
C20 W P C8 -73.65(11) . . . . ?
C20 W C18 O2 126(10) . . . . ?
C20 W C19 O3 -107(3) . . . . ?
C20 W C21 O5 75(15) . . . . ?
C20 W C22 O6 42(10) . . . . ?
C21 W P O1 66.65(10) . . . . ?
C21 W P C1 -45.23(10) . . . . ?
C21 W P C8 -161.51(11) . . . . ?
C21 W C18 O2 -145(10) . . . . ?
C21 W C19 O3 13(4) . . . . ?
C21 W C20 O4 35(4) . . . . ?
C21 W C22 O6 -14(10) . . . . ?
C22 W P O1 -22.79(10) . . . . ?
C22 W P C1 -134.67(10) . . . . ?
C22 W P C8 109.05(11) . . . . ?
C22 W C18 O2 -57(10) . . . . ?
C22 W C19 O3 77(3) . . . . ?
C22 W C20 O4 -22(5) . . . . ?
C22 W C21 O5 -110(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

#END---------------------------------------------------------------------------

