# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  from this site to visualise CIF-encoded structures and 
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data_greg1752f

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H22 N O6 P W'
_chemical_formula_sum            'C21 H22 N O6 P W'
_chemical_formula_weight         599.22

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                   8.8600(4)
_cell_length_b                   10.8854(5)
_cell_length_c                   12.8306(5)
_cell_angle_alpha                86.595(2)
_cell_angle_beta                 78.246(2)
_cell_angle_gamma                66.290(2)
_cell_volume                     1108.89(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9951
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      30.15

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    5.317
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.1763
_exptl_absorpt_correction_T_max  0.3386
_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       '\f and \w 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            13781
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_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         3.24
_diffrn_reflns_theta_max         28.00
_reflns_number_total             5338
_reflns_number_gt                5130
_reflns_threshold_expression     I>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 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^)+(0.0093P)^2^+0.9685P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5338
_refine_ls_number_parameters     277
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0174
_refine_ls_wR_factor_ref         0.0410
_refine_ls_wR_factor_gt          0.0404
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.059
_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
C1 C 0.9638(3) 0.6465(2) 0.80163(17) 0.0160(4) Uani 1 1 d . . .
C2 C 1.1580(3) 0.6096(2) 0.77123(17) 0.0168(4) Uani 1 1 d . . .
C3 C 1.2001(3) 0.6383(2) 0.87485(18) 0.0174(4) Uani 1 1 d . . .
C4 C 1.0616(3) 0.7049(2) 0.94718(18) 0.0187(4) Uani 1 1 d . . .
C5 C 0.9064(3) 0.7197(2) 0.91066(17) 0.0174(4) Uani 1 1 d . . .
C6 C 1.2627(3) 0.4678(2) 0.72593(19) 0.0228(5) Uani 1 1 d . . .
H6A H 1.3814 0.4538 0.7074 0.034 Uiso 1 1 calc R . .
H6B H 1.2253 0.4553 0.6620 0.034 Uiso 1 1 calc R . .
H6C H 1.2488 0.4028 0.7792 0.034 Uiso 1 1 calc R . .
C7 C 1.3794(3) 0.6042(3) 0.8828(2) 0.0250(5) Uani 1 1 d . . .
H7A H 1.3820 0.6417 0.9496 0.037 Uiso 1 1 calc R . .
H7B H 1.4327 0.6421 0.8225 0.037 Uiso 1 1 calc R . .
H7C H 1.4403 0.5064 0.8813 0.037 Uiso 1 1 calc R . .
C8 C 1.0496(3) 0.7706(3) 1.05010(19) 0.0258(5) Uani 1 1 d . . .
H8A H 1.1619 0.7409 1.0667 0.039 Uiso 1 1 calc R . .
H8B H 0.9765 0.7455 1.1075 0.039 Uiso 1 1 calc R . .
H8C H 1.0024 0.8684 1.0431 0.039 Uiso 1 1 calc R . .
C9 C 0.7600(3) 0.7104(3) 0.98978(19) 0.0239(5) Uani 1 1 d . . .
H9A H 0.7938 0.6201 1.0189 0.036 Uiso 1 1 calc R . .
H9B H 0.6657 0.7283 0.9540 0.036 Uiso 1 1 calc R . .
H9C H 0.7255 0.7766 1.0477 0.036 Uiso 1 1 calc R . .
C10 C 1.1804(3) 0.7182(2) 0.69267(17) 0.0164(4) Uani 1 1 d . . .
H10 H 1.2878 0.7256 0.6972 0.020 Uiso 1 1 calc R . .
C11 C 1.0715(3) 0.9633(2) 0.7453(2) 0.0245(5) Uani 1 1 d . . .
H11A H 1.1340 0.9500 0.8028 0.037 Uiso 1 1 calc R . .
H11B H 0.9646 1.0416 0.7627 0.037 Uiso 1 1 calc R . .
H11C H 1.1381 0.9782 0.6786 0.037 Uiso 1 1 calc R . .
C12 C 1.1854(3) 0.6904(2) 0.57880(18) 0.0190(4) Uani 1 1 d . . .
C13 C 1.3073(3) 0.6578(3) 0.49041(19) 0.0241(5) Uani 1 1 d . . .
H13 H 1.4201 0.6480 0.4852 0.029 Uiso 1 1 calc R . .
C14 C 1.2330(3) 0.6407(3) 0.4060(2) 0.0301(6) Uani 1 1 d . . .
H14 H 1.2869 0.6177 0.3337 0.036 Uiso 1 1 calc R . .
C15 C 1.0729(3) 0.6637(3) 0.4489(2) 0.0311(6) Uani 1 1 d . . .
H15 H 0.9936 0.6595 0.4108 0.037 Uiso 1 1 calc R . .
C16 C 0.3934(3) 1.0997(3) 0.6805(2) 0.0255(5) Uani 1 1 d . . .
C17 C 0.6049(3) 1.1379(2) 0.80391(18) 0.0188(5) Uani 1 1 d . . .
C18 C 0.7457(3) 0.9981(3) 0.5979(2) 0.0246(5) Uani 1 1 d . . .
C19 C 0.5910(3) 0.8172(3) 0.6616(2) 0.0231(5) Uani 1 1 d . . .
C20 C 0.4439(3) 0.9521(2) 0.8718(2) 0.0213(5) Uani 1 1 d . . .
C27 C 0.8907(3) 0.5514(2) 0.7758(2) 0.0236(5) Uani 1 1 d . . .
H27A H 0.9432 0.4648 0.8085 0.035 Uiso 1 1 calc R . .
H27B H 0.9122 0.5384 0.6984 0.035 Uiso 1 1 calc R . .
H27C H 0.7692 0.5890 0.8036 0.035 Uiso 1 1 calc R . .
N N 1.0391(2) 0.84555(19) 0.73317(15) 0.0166(4) Uani 1 1 d . . .
O1 O 1.0392(2) 0.6942(2) 0.55566(13) 0.0269(4) Uani 1 1 d . . .
O2 O 0.2792(3) 1.1701(2) 0.64650(18) 0.0401(5) Uani 1 1 d U . .
O3 O 0.6080(2) 1.23048(18) 0.83898(14) 0.0252(4) Uani 1 1 d . . .
O4 O 0.8267(3) 1.0091(2) 0.52021(16) 0.0401(5) Uani 1 1 d . . .
O5 O 0.5883(3) 0.7311(2) 0.61657(16) 0.0344(4) Uani 1 1 d . . .
O6 O 0.3548(2) 0.9407(2) 0.94644(15) 0.0294(4) Uani 1 1 d . . .
P P 0.86286(7) 0.82674(6) 0.79081(4) 0.01448(11) Uani 1 1 d . . .
W W 0.595085(10) 0.976461(9) 0.736346(7) 0.01560(3) 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
C1 0.0155(10) 0.0127(10) 0.0187(10) -0.0001(8) -0.0038(8) -0.0043(8)
C2 0.0148(10) 0.0155(11) 0.0183(10) -0.0020(8) -0.0047(8) -0.0031(8)
C3 0.0173(10) 0.0147(11) 0.0196(10) 0.0015(9) -0.0078(8) -0.0040(9)
C4 0.0209(11) 0.0155(11) 0.0198(11) 0.0015(9) -0.0079(9) -0.0056(9)
C5 0.0178(10) 0.0160(11) 0.0172(10) 0.0020(9) -0.0037(8) -0.0054(9)
C6 0.0213(11) 0.0165(12) 0.0247(12) -0.0032(9) -0.0058(9) -0.0003(9)
C7 0.0176(11) 0.0284(14) 0.0266(12) -0.0009(10) -0.0096(9) -0.0042(10)
C8 0.0284(12) 0.0244(13) 0.0207(11) -0.0045(10) -0.0063(9) -0.0053(11)
C9 0.0221(11) 0.0211(12) 0.0244(12) 0.0001(10) 0.0002(9) -0.0066(10)
C10 0.0104(9) 0.0179(11) 0.0189(10) -0.0014(9) -0.0024(8) -0.0035(8)
C11 0.0226(11) 0.0222(13) 0.0312(13) -0.0077(10) 0.0012(10) -0.0136(10)
C12 0.0158(10) 0.0181(11) 0.0201(11) 0.0006(9) -0.0055(8) -0.0029(9)
C13 0.0241(12) 0.0248(13) 0.0204(11) -0.0016(10) -0.0017(9) -0.0077(10)
C14 0.0355(14) 0.0299(15) 0.0181(11) -0.0020(10) -0.0053(10) -0.0058(12)
C15 0.0313(13) 0.0336(15) 0.0228(12) -0.0079(11) -0.0131(10) -0.0025(12)
C16 0.0252(12) 0.0207(13) 0.0349(13) 0.0038(10) -0.0125(10) -0.0110(10)
C17 0.0120(9) 0.0208(12) 0.0218(11) 0.0026(9) -0.0050(8) -0.0043(9)
C18 0.0262(12) 0.0218(13) 0.0271(12) 0.0019(10) -0.0082(10) -0.0097(10)
C19 0.0182(11) 0.0241(13) 0.0274(12) 0.0038(10) -0.0071(9) -0.0080(10)
C20 0.0167(10) 0.0162(12) 0.0281(12) -0.0019(9) -0.0043(9) -0.0034(9)
C27 0.0236(12) 0.0167(11) 0.0336(13) -0.0009(10) -0.0084(10) -0.0096(10)
N 0.0129(8) 0.0145(9) 0.0221(9) -0.0025(7) -0.0019(7) -0.0056(7)
O1 0.0169(8) 0.0361(11) 0.0229(8) -0.0090(8) -0.0066(6) -0.0030(8)
O2 0.0360(10) 0.0297(10) 0.0612(12) 0.0095(9) -0.0283(9) -0.0119(8)
O3 0.0243(8) 0.0201(9) 0.0317(9) -0.0021(7) -0.0076(7) -0.0079(7)
O4 0.0474(12) 0.0370(12) 0.0309(10) 0.0033(9) 0.0054(9) -0.0182(10)
O5 0.0379(11) 0.0307(11) 0.0414(11) -0.0062(9) -0.0126(9) -0.0175(9)
O6 0.0225(9) 0.0296(10) 0.0308(10) 0.0037(8) 0.0004(7) -0.0080(8)
P 0.0119(2) 0.0124(3) 0.0182(3) -0.0003(2) -0.00334(19) -0.0037(2)
W 0.01240(5) 0.01394(5) 0.02022(5) 0.00073(3) -0.00507(3) -0.00418(4)

_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C27 1.506(3) . ?
C1 C5 1.539(3) . ?
C1 C2 1.569(3) . ?
C1 P 1.810(2) . ?
C2 C6 1.522(3) . ?
C2 C3 1.533(3) . ?
C2 C10 1.555(3) . ?
C3 C4 1.339(3) . ?
C3 C7 1.502(3) . ?
C4 C5 1.487(3) . ?
C4 C8 1.503(3) . ?
C5 C9 1.510(3) . ?
C5 P 1.881(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 N 1.478(3) . ?
C10 C12 1.498(3) . ?
C10 H10 1.0000 . ?
C11 N 1.445(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.349(3) . ?
C12 O1 1.371(3) . ?
C13 C14 1.433(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.339(4) . ?
C14 H14 0.9500 . ?
C15 O1 1.372(3) . ?
C15 H15 0.9500 . ?
C16 O2 1.148(3) . ?
C16 W 1.997(3) . ?
C17 O3 1.140(3) . ?
C17 W 2.045(2) . ?
C18 O4 1.135(3) . ?
C18 W 2.056(3) . ?
C19 O5 1.140(3) . ?
C19 W 2.047(3) . ?
C20 O6 1.146(3) . ?
C20 W 2.041(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N P 1.6723(18) . ?
P W 2.4907(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
C27 C1 C5 121.40(19) . . ?
C27 C1 C2 120.88(19) . . ?
C5 C1 C2 105.09(17) . . ?
C27 C1 P 123.28(16) . . ?
C5 C1 P 67.79(12) . . ?
C2 C1 P 106.17(15) . . ?
C6 C2 C3 114.04(19) . . ?
C6 C2 C10 112.34(18) . . ?
C3 C2 C10 105.60(18) . . ?
C6 C2 C1 114.69(19) . . ?
C3 C2 C1 103.24(17) . . ?
C10 C2 C1 106.00(17) . . ?
C4 C3 C7 127.3(2) . . ?
C4 C3 C2 112.03(19) . . ?
C7 C3 C2 120.40(19) . . ?
C3 C4 C5 111.6(2) . . ?
C3 C4 C8 127.9(2) . . ?
C5 C4 C8 120.2(2) . . ?
C4 C5 C9 119.8(2) . . ?
C4 C5 C1 106.60(18) . . ?
C9 C5 C1 120.2(2) . . ?
C4 C5 P 115.17(16) . . ?
C9 C5 P 118.72(16) . . ?
C1 C5 P 62.98(12) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N C10 C12 111.44(18) . . ?
N C10 C2 105.50(17) . . ?
C12 C10 C2 114.56(19) . . ?
N C10 H10 108.4 . . ?
C12 C10 H10 108.4 . . ?
C2 C10 H10 108.4 . . ?
N C11 H11A 109.5 . . ?
N C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 O1 110.1(2) . . ?
C13 C12 C10 133.6(2) . . ?
O1 C12 C10 116.20(18) . . ?
C12 C13 C14 106.4(2) . . ?
C12 C13 H13 126.8 . . ?
C14 C13 H13 126.8 . . ?
C15 C14 C13 106.6(2) . . ?
C15 C14 H14 126.7 . . ?
C13 C14 H14 126.7 . . ?
C14 C15 O1 110.5(2) . . ?
C14 C15 H15 124.7 . . ?
O1 C15 H15 124.7 . . ?
O2 C16 W 178.7(2) . . ?
O3 C17 W 177.7(2) . . ?
O4 C18 W 178.3(2) . . ?
O5 C19 W 177.5(2) . . ?
O6 C20 W 177.9(2) . . ?
C1 C27 H27A 109.5 . . ?
C1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C11 N C10 119.66(18) . . ?
C11 N P 124.73(15) . . ?
C10 N P 113.57(15) . . ?
C12 O1 C15 106.35(19) . . ?
N P C1 95.09(10) . . ?
N P C5 108.00(10) . . ?
C1 P C5 49.23(10) . . ?
N P W 118.25(7) . . ?
C1 P W 132.72(7) . . ?
C5 P W 131.84(7) . . ?
C16 W C20 90.37(10) . . ?
C16 W C17 89.57(10) . . ?
C20 W C17 90.95(9) . . ?
C16 W C19 89.92(10) . . ?
C20 W C19 91.87(10) . . ?
C17 W C19 177.13(9) . . ?
C16 W C18 89.24(10) . . ?
C20 W C18 178.62(9) . . ?
C17 W C18 90.36(10) . . ?
C19 W C18 86.81(10) . . ?
C16 W P 174.69(8) . . ?
C20 W P 94.94(7) . . ?
C17 W P 90.14(6) . . ?
C19 W P 90.11(7) . . ?
C18 W P 85.47(7) . . ?

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
C27 C1 C2 C6 -6.1(3) . . . . ?
C5 C1 C2 C6 136.0(2) . . . . ?
P C1 C2 C6 -153.19(16) . . . . ?
C27 C1 C2 C3 -130.8(2) . . . . ?
C5 C1 C2 C3 11.4(2) . . . . ?
P C1 C2 C3 82.14(18) . . . . ?
C27 C1 C2 C10 118.4(2) . . . . ?
C5 C1 C2 C10 -99.41(19) . . . . ?
P C1 C2 C10 -28.64(19) . . . . ?
C6 C2 C3 C4 -136.1(2) . . . . ?
C10 C2 C3 C4 100.1(2) . . . . ?
C1 C2 C3 C4 -11.0(3) . . . . ?
C6 C2 C3 C7 49.5(3) . . . . ?
C10 C2 C3 C7 -74.3(3) . . . . ?
C1 C2 C3 C7 174.6(2) . . . . ?
C7 C3 C4 C5 179.8(2) . . . . ?
C2 C3 C4 C5 5.9(3) . . . . ?
C7 C3 C4 C8 4.9(4) . . . . ?
C2 C3 C4 C8 -169.1(2) . . . . ?
C3 C4 C5 C9 142.9(2) . . . . ?
C8 C4 C5 C9 -41.8(3) . . . . ?
C3 C4 C5 C1 2.0(3) . . . . ?
C8 C4 C5 C1 177.4(2) . . . . ?
C3 C4 C5 P -65.4(2) . . . . ?
C8 C4 C5 P 110.0(2) . . . . ?
C27 C1 C5 C4 133.3(2) . . . . ?
C2 C1 C5 C4 -8.6(2) . . . . ?
P C1 C5 C4 -110.26(17) . . . . ?
C27 C1 C5 C9 -7.3(3) . . . . ?
C2 C1 C5 C9 -149.3(2) . . . . ?
P C1 C5 C9 109.1(2) . . . . ?
C27 C1 C5 P -116.4(2) . . . . ?
C2 C1 C5 P 101.63(16) . . . . ?
C6 C2 C10 N 164.30(18) . . . . ?
C3 C2 C10 N -70.8(2) . . . . ?
C1 C2 C10 N 38.3(2) . . . . ?
C6 C2 C10 C12 41.3(2) . . . . ?
C3 C2 C10 C12 166.24(18) . . . . ?
C1 C2 C10 C12 -84.6(2) . . . . ?
N C10 C12 C13 129.4(3) . . . . ?
C2 C10 C12 C13 -111.0(3) . . . . ?
N C10 C12 O1 -52.8(3) . . . . ?
C2 C10 C12 O1 66.9(3) . . . . ?
O1 C12 C13 C14 0.4(3) . . . . ?
C10 C12 C13 C14 178.4(3) . . . . ?
C12 C13 C14 C15 -0.2(3) . . . . ?
C13 C14 C15 O1 -0.1(3) . . . . ?
C12 C10 N C11 -103.9(2) . . . . ?
C2 C10 N C11 131.2(2) . . . . ?
C12 C10 N P 91.6(2) . . . . ?
C2 C10 N P -33.3(2) . . . . ?
C13 C12 O1 C15 -0.5(3) . . . . ?
C10 C12 O1 C15 -178.9(2) . . . . ?
C14 C15 O1 C12 0.4(3) . . . . ?
C11 N P C1 -149.3(2) . . . . ?
C10 N P C1 14.29(17) . . . . ?
C11 N P C5 -100.6(2) . . . . ?
C10 N P C5 62.96(17) . . . . ?
C11 N P W 65.5(2) . . . . ?
C10 N P W -130.91(13) . . . . ?
C27 C1 P N -136.66(19) . . . . ?
C5 C1 P N 109.43(13) . . . . ?
C2 C1 P N 9.39(15) . . . . ?
C27 C1 P C5 113.9(2) . . . . ?
C2 C1 P C5 -100.04(18) . . . . ?
C27 C1 P W 0.2(2) . . . . ?
C5 C1 P W -113.75(12) . . . . ?
C2 C1 P W 146.21(11) . . . . ?
C4 C5 P N 15.6(2) . . . . ?
C9 C5 P N 167.66(18) . . . . ?
C1 C5 P N -80.98(13) . . . . ?
C4 C5 P C1 96.6(2) . . . . ?
C9 C5 P C1 -111.4(2) . . . . ?
C4 C5 P W -147.93(13) . . . . ?
C9 C5 P W 4.1(2) . . . . ?
C1 C5 P W 115.49(12) . . . . ?
O2 C16 W C20 -161(10) . . . . ?
O2 C16 W C17 108(10) . . . . ?
O2 C16 W C19 -69(10) . . . . ?
O2 C16 W C18 18(10) . . . . ?
O2 C16 W P 21(11) . . . . ?
O6 C20 W C16 6(6) . . . . ?
O6 C20 W C17 95(6) . . . . ?
O6 C20 W C19 -84(6) . . . . ?
O6 C20 W C18 -68(8) . . . . ?
O6 C20 W P -175(6) . . . . ?
O3 C17 W C16 -29(5) . . . . ?
O3 C17 W C20 -120(5) . . . . ?
O3 C17 W C19 50(6) . . . . ?
O3 C17 W C18 60(5) . . . . ?
O3 C17 W P 145(5) . . . . ?
O5 C19 W C16 50(5) . . . . ?
O5 C19 W C20 140(5) . . . . ?
O5 C19 W C17 -30(6) . . . . ?
O5 C19 W C18 -39(5) . . . . ?
O5 C19 W P -125(5) . . . . ?
O4 C18 W C16 -56(9) . . . . ?
O4 C18 W C20 18(11) . . . . ?
O4 C18 W C17 -145(9) . . . . ?
O4 C18 W C19 34(9) . . . . ?
O4 C18 W P 125(9) . . . . ?
N P W C16 19.6(8) . . . . ?
C1 P W C16 -109.7(8) . . . . ?
C5 P W C16 -178.2(8) . . . . ?
N P W C20 -158.21(10) . . . . ?
C1 P W C20 72.48(12) . . . . ?
C5 P W C20 3.97(12) . . . . ?
N P W C17 -67.24(10) . . . . ?
C1 P W C17 163.45(12) . . . . ?
C5 P W C17 94.94(12) . . . . ?
N P W C19 109.90(10) . . . . ?
C1 P W C19 -19.41(12) . . . . ?
C5 P W C19 -87.92(12) . . . . ?
N P W C18 23.11(11) . . . . ?
C1 P W C18 -106.20(12) . . . . ?
C5 P W C18 -174.71(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 936605'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2252

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H28 N O6 P W'
_chemical_formula_sum            'C29 H28 N O6 P W'
_chemical_formula_weight         701.34

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/n'
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.32930(10)
_cell_length_b                   18.8398(3)
_cell_length_c                   16.1143(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8670(8)
_cell_angle_gamma                90.00
_cell_volume                     2771.75(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    7558
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      29.13

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.2612
_exptl_absorpt_correction_T_max  0.6749
_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 \k-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            52522
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         28.00
_reflns_number_total             6681
_reflns_number_gt                5883
_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 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^)+(0.0208P)^2^+5.0102P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6681
_refine_ls_number_parameters     349
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0594
_refine_ls_wR_factor_gt          0.0576
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_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 0.3538(3) 0.74079(15) -0.08788(18) 0.0154(6) Uani 1 1 d . . .
C2 C 0.4892(3) 0.79036(16) -0.07356(18) 0.0164(6) Uani 1 1 d . . .
H2 H 0.5608 0.7859 -0.0183 0.020 Uiso 1 1 calc R . .
C3 C 0.5506(3) 0.78405(16) -0.15562(18) 0.0176(6) Uani 1 1 d . . .
C4 C 0.6021(3) 0.70608(17) -0.15184(19) 0.0195(6) Uani 1 1 d . . .
C5 C 0.4830(3) 0.66448(17) -0.16715(19) 0.0198(6) Uani 1 1 d . . .
C6 C 0.3483(3) 0.71352(16) -0.18091(18) 0.0174(6) Uani 1 1 d . . .
C7 C 0.4083(3) 0.77783(16) -0.22561(18) 0.0183(6) Uani 1 1 d . . .
C8 C 0.2993(3) 0.84114(18) -0.24251(19) 0.0209(6) Uani 1 1 d . . .
H8A H 0.2058 0.8209 -0.2756 0.025 Uiso 1 1 calc R . .
C9 C 0.3271(3) 0.68754(16) -0.02389(19) 0.0170(6) Uani 1 1 d . . .
C10 C 0.4410(3) 0.64965(17) 0.0263(2) 0.0211(6) Uani 1 1 d . . .
H10A H 0.5391 0.6580 0.0210 0.025 Uiso 1 1 calc R . .
C11 C 0.4123(4) 0.59951(18) 0.0845(2) 0.0268(7) Uani 1 1 d . . .
H11A H 0.4908 0.5737 0.1181 0.032 Uiso 1 1 calc R . .
C12 C 0.2698(4) 0.58711(18) 0.0934(2) 0.0275(7) Uani 1 1 d . . .
H12A H 0.2505 0.5532 0.1334 0.033 Uiso 1 1 calc R . .
C13 C 0.1555(4) 0.62458(18) 0.0438(2) 0.0249(7) Uani 1 1 d . . .
H13A H 0.0577 0.6163 0.0497 0.030 Uiso 1 1 calc R . .
C14 C 0.1839(3) 0.67420(17) -0.01452(19) 0.0201(6) Uani 1 1 d . . .
H14A H 0.1049 0.6994 -0.0485 0.024 Uiso 1 1 calc R . .
C15 C 0.6634(3) 0.83999(18) -0.1649(2) 0.0242(7) Uani 1 1 d . . .
H15A H 0.7502 0.8343 -0.1194 0.029 Uiso 1 1 calc R . .
H15B H 0.6215 0.8873 -0.1612 0.029 Uiso 1 1 calc R . .
H15C H 0.6911 0.8345 -0.2200 0.029 Uiso 1 1 calc R . .
C16 C 0.7599(4) 0.68492(19) -0.1249(2) 0.0269(7) Uani 1 1 d . . .
H16A H 0.7976 0.7008 -0.0666 0.032 Uiso 1 1 calc R . .
H16B H 0.8170 0.7070 -0.1627 0.032 Uiso 1 1 calc R . .
H16C H 0.7683 0.6332 -0.1279 0.032 Uiso 1 1 calc R . .
C17 C 0.4705(4) 0.58542(18) -0.1674(2) 0.0297(8) Uani 1 1 d . . .
H17A H 0.5684 0.5644 -0.1512 0.036 Uiso 1 1 calc R . .
H17B H 0.4238 0.5692 -0.2243 0.036 Uiso 1 1 calc R . .
H17C H 0.4111 0.5708 -0.1268 0.036 Uiso 1 1 calc R . .
C18 C 0.2027(4) 0.68185(19) -0.2244(2) 0.0261(7) Uani 1 1 d . . .
H18A H 0.1253 0.7175 -0.2272 0.031 Uiso 1 1 calc R . .
H18B H 0.1806 0.6406 -0.1922 0.031 Uiso 1 1 calc R . .
H18C H 0.2082 0.6670 -0.2820 0.031 Uiso 1 1 calc R . .
C19 C 0.4382(4) 0.75730(18) -0.31281(19) 0.0247(7) Uani 1 1 d . . .
H19A H 0.4922 0.7124 -0.3081 0.030 Uiso 1 1 calc R . .
H19B H 0.4965 0.7946 -0.3325 0.030 Uiso 1 1 calc R . .
H19C H 0.3450 0.7519 -0.3534 0.030 Uiso 1 1 calc R . .
C20 C 0.3395(4) 0.90057(18) -0.29651(19) 0.0229(7) Uani 1 1 d . . .
C21 C 0.3207(4) 0.9561(2) -0.4182(2) 0.0333(8) Uani 1 1 d U . .
H21A H 0.2937 0.9670 -0.4769 0.040 Uiso 1 1 calc R . .
C22 C 0.4033(4) 0.9970(2) -0.3606(2) 0.0342(8) Uani 1 1 d U . .
H22A H 0.4459 1.0413 -0.3703 0.041 Uiso 1 1 calc R . .
C23 C 0.4158(5) 0.96132(19) -0.2805(2) 0.0358(9) Uani 1 1 d . . .
H23A H 0.4676 0.9775 -0.2268 0.043 Uiso 1 1 calc R . .
C24 C 0.1138(4) 0.9055(2) -0.1855(3) 0.0392(9) Uani 1 1 d U . .
H24C H 0.0848 0.9191 -0.1326 0.047 Uiso 1 1 calc R . .
H24B H 0.0436 0.8710 -0.2159 0.047 Uiso 1 1 calc R . .
H24A H 0.1151 0.9477 -0.2209 0.047 Uiso 1 1 calc R . .
C25 C 0.2358(4) 0.9333(2) 0.1674(2) 0.0343(8) Uani 1 1 d U . .
C26 C 0.3306(4) 0.79824(19) 0.1326(2) 0.0244(7) Uani 1 1 d . . .
C27 C 0.0611(4) 0.84396(17) 0.0312(2) 0.0228(6) Uani 1 1 d U . .
C28 C 0.1940(4) 0.9806(2) 0.0066(3) 0.0370(8) Uani 1 1 d U . .
C29 C 0.4778(4) 0.9231(2) 0.0819(2) 0.0314(8) Uani 1 1 d U . .
N N 0.2615(3) 0.87342(15) -0.16588(17) 0.0252(6) Uani 1 1 d . . .
O1 O 0.2795(3) 0.89590(14) -0.38149(15) 0.0300(5) Uani 1 1 d U . .
O2 O 0.2199(4) 0.96211(18) 0.2281(2) 0.0546(8) Uani 1 1 d U . .
O3 O 0.3620(3) 0.75173(14) 0.17784(15) 0.0324(6) Uani 1 1 d . . .
O4 O -0.0506(3) 0.81768(14) 0.01324(16) 0.0312(5) Uani 1 1 d . . .
O5 O 0.1495(4) 1.03466(18) -0.0191(3) 0.0604(9) Uani 1 1 d U . .
O6 O 0.5956(3) 0.94210(18) 0.0928(2) 0.0493(7) Uani 1 1 d U . .
P P 0.31823(9) 0.83448(4) -0.07208(5) 0.01762(15) Uani 1 1 d . . .
W W 0.266929(14) 0.887090(7) 0.061094(8) 0.02129(5) Uani 1 1 d U . .

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
C1 0.0171(13) 0.0145(14) 0.0150(13) 0.0007(11) 0.0040(11) 0.0009(11)
C2 0.0200(14) 0.0154(14) 0.0137(13) 0.0005(11) 0.0035(11) -0.0008(11)
C3 0.0207(14) 0.0172(15) 0.0165(14) 0.0018(12) 0.0071(11) 0.0001(11)
C4 0.0238(15) 0.0189(15) 0.0180(14) 0.0023(12) 0.0094(12) 0.0047(12)
C5 0.0267(15) 0.0172(15) 0.0174(14) -0.0006(12) 0.0090(12) 0.0030(12)
C6 0.0211(14) 0.0160(14) 0.0154(13) -0.0019(11) 0.0046(11) -0.0007(11)
C7 0.0225(14) 0.0177(15) 0.0156(14) 0.0009(12) 0.0060(11) 0.0031(12)
C8 0.0255(15) 0.0233(16) 0.0151(14) 0.0036(12) 0.0066(12) 0.0048(13)
C9 0.0226(14) 0.0133(14) 0.0164(14) -0.0005(11) 0.0070(11) -0.0007(11)
C10 0.0232(15) 0.0195(16) 0.0213(15) 0.0024(12) 0.0058(12) 0.0021(12)
C11 0.0347(18) 0.0219(17) 0.0237(16) 0.0057(13) 0.0057(14) 0.0030(14)
C12 0.045(2) 0.0185(16) 0.0224(16) 0.0038(13) 0.0139(14) -0.0042(14)
C13 0.0290(17) 0.0238(17) 0.0258(17) -0.0039(13) 0.0145(14) -0.0064(13)
C14 0.0219(14) 0.0190(16) 0.0201(15) -0.0027(12) 0.0061(12) -0.0016(12)
C15 0.0249(15) 0.0217(16) 0.0274(17) 0.0031(14) 0.0089(13) -0.0046(13)
C16 0.0247(16) 0.0293(18) 0.0287(17) 0.0043(14) 0.0102(14) 0.0064(14)
C17 0.0393(19) 0.0175(16) 0.0364(19) -0.0005(15) 0.0176(16) 0.0027(14)
C18 0.0268(16) 0.0272(18) 0.0233(16) -0.0031(14) 0.0028(13) -0.0066(14)
C19 0.0315(17) 0.0261(17) 0.0180(15) 0.0008(13) 0.0087(13) 0.0037(14)
C20 0.0294(16) 0.0261(17) 0.0144(14) 0.0047(12) 0.0076(12) 0.0093(13)
C21 0.0363(15) 0.0370(16) 0.0294(14) 0.0136(13) 0.0134(12) 0.0082(13)
C22 0.0423(16) 0.0280(15) 0.0360(16) 0.0081(13) 0.0164(13) 0.0064(13)
C23 0.060(3) 0.0211(18) 0.0271(18) 0.0017(15) 0.0120(17) 0.0015(17)
C24 0.0405(16) 0.0427(17) 0.0360(16) 0.0090(14) 0.0116(13) 0.0206(14)
C25 0.0396(15) 0.0341(16) 0.0348(15) -0.0113(13) 0.0208(13) -0.0094(13)
C26 0.0271(16) 0.0286(18) 0.0181(15) -0.0062(14) 0.0055(13) -0.0050(14)
C27 0.0318(15) 0.0190(16) 0.0196(15) 0.0010(13) 0.0095(13) 0.0027(12)
C28 0.0371(15) 0.0286(14) 0.0504(17) 0.0035(13) 0.0211(14) 0.0038(13)
C29 0.0367(15) 0.0320(15) 0.0287(14) -0.0061(13) 0.0147(12) -0.0075(13)
N 0.0352(15) 0.0242(15) 0.0182(13) 0.0089(11) 0.0099(12) 0.0124(12)
O1 0.0311(11) 0.0373(12) 0.0209(10) 0.0109(9) 0.0036(9) 0.0007(10)
O2 0.0658(16) 0.0569(16) 0.0500(15) -0.0226(13) 0.0330(13) -0.0141(13)
O3 0.0419(14) 0.0326(14) 0.0206(12) 0.0003(11) 0.0018(10) -0.0022(12)
O4 0.0311(13) 0.0304(14) 0.0314(13) 0.0015(11) 0.0046(10) -0.0007(11)
O5 0.0528(15) 0.0417(15) 0.0935(19) 0.0135(14) 0.0309(14) 0.0103(12)
O6 0.0437(14) 0.0560(15) 0.0515(14) -0.0045(13) 0.0176(12) -0.0169(12)
P 0.0245(4) 0.0144(4) 0.0157(4) 0.0019(3) 0.0080(3) 0.0035(3)
W 0.02931(8) 0.01674(7) 0.02185(8) -0.00380(5) 0.01464(5) -0.00273(5)

_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 C9 1.495(4) . ?
C1 C2 1.550(4) . ?
C1 C6 1.576(4) . ?
C1 P 1.824(3) . ?
C2 C3 1.550(4) . ?
C2 P 1.803(3) . ?
C2 H2 1.0000 . ?
C3 C15 1.518(4) . ?
C3 C4 1.543(4) . ?
C3 C7 1.560(4) . ?
C4 C5 1.340(4) . ?
C4 C16 1.501(4) . ?
C5 C17 1.494(5) . ?
C5 C6 1.538(4) . ?
C6 C18 1.517(4) . ?
C6 C7 1.570(4) . ?
C7 C19 1.537(4) . ?
C7 C8 1.555(4) . ?
C8 N 1.483(4) . ?
C8 C20 1.512(4) . ?
C8 H8A 1.0000 . ?
C9 C10 1.393(4) . ?
C9 C14 1.398(4) . ?
C10 C11 1.394(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.387(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.389(5) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
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 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C23 1.344(5) . ?
C20 O1 1.371(4) . ?
C21 C22 1.325(6) . ?
C21 O1 1.370(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.440(5) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 N 1.479(5) . ?
C24 H24C 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24A 0.9800 . ?
C25 O2 1.155(4) . ?
C25 W 1.995(4) . ?
C26 O3 1.139(4) . ?
C26 W 2.050(4) . ?
C27 O4 1.136(4) . ?
C27 W 2.049(3) . ?
C28 O5 1.145(5) . ?
C28 W 2.023(4) . ?
C29 O6 1.135(4) . ?
C29 W 2.043(4) . ?
N P 1.666(3) . ?
P W 2.4978(8) . ?

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
C9 C1 C2 123.2(2) . . ?
C9 C1 C6 117.4(2) . . ?
C2 C1 C6 101.8(2) . . ?
C9 C1 P 119.5(2) . . ?
C2 C1 P 64.03(15) . . ?
C6 C1 P 118.5(2) . . ?
C3 C2 C1 105.1(2) . . ?
C3 C2 P 122.0(2) . . ?
C1 C2 P 65.37(15) . . ?
C3 C2 H2 117.2 . . ?
C1 C2 H2 117.2 . . ?
P C2 H2 117.2 . . ?
C15 C3 C4 116.7(3) . . ?
C15 C3 C2 114.6(3) . . ?
C4 C3 C2 101.9(2) . . ?
C15 C3 C7 119.0(3) . . ?
C4 C3 C7 99.7(2) . . ?
C2 C3 C7 102.3(2) . . ?
C5 C4 C16 128.7(3) . . ?
C5 C4 C3 108.1(3) . . ?
C16 C4 C3 122.9(3) . . ?
C4 C5 C17 130.1(3) . . ?
C4 C5 C6 107.3(3) . . ?
C17 C5 C6 122.5(3) . . ?
C18 C6 C5 117.2(3) . . ?
C18 C6 C7 117.5(3) . . ?
C5 C6 C7 99.9(2) . . ?
C18 C6 C1 114.7(2) . . ?
C5 C6 C1 101.1(2) . . ?
C7 C6 C1 103.9(2) . . ?
C19 C7 C8 105.5(2) . . ?
C19 C7 C3 113.1(2) . . ?
C8 C7 C3 119.9(3) . . ?
C19 C7 C6 112.0(3) . . ?
C8 C7 C6 113.0(2) . . ?
C3 C7 C6 93.3(2) . . ?
N C8 C20 107.8(3) . . ?
N C8 C7 115.3(2) . . ?
C20 C8 C7 116.0(3) . . ?
N C8 H8A 105.6 . . ?
C20 C8 H8A 105.6 . . ?
C7 C8 H8A 105.6 . . ?
C10 C9 C14 118.5(3) . . ?
C10 C9 C1 122.0(3) . . ?
C14 C9 C1 119.5(3) . . ?
C9 C10 C11 120.6(3) . . ?
C9 C10 H10A 119.7 . . ?
C11 C10 H10A 119.7 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C13 C14 C9 120.9(3) . . ?
C13 C14 H14A 119.6 . . ?
C9 C14 H14A 119.6 . . ?
C3 C15 H15A 109.5 . . ?
C3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C16 H16A 109.5 . . ?
C4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C5 C17 H17A 109.5 . . ?
C5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C6 C18 H18A 109.5 . . ?
C6 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C6 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C7 C19 H19A 109.5 . . ?
C7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C23 C20 O1 109.8(3) . . ?
C23 C20 C8 134.7(3) . . ?
O1 C20 C8 115.4(3) . . ?
C22 C21 O1 110.8(3) . . ?
C22 C21 H21A 124.6 . . ?
O1 C21 H21A 124.6 . . ?
C21 C22 C23 106.5(3) . . ?
C21 C22 H22A 126.8 . . ?
C23 C22 H22A 126.8 . . ?
C20 C23 C22 106.5(3) . . ?
C20 C23 H23A 126.8 . . ?
C22 C23 H23A 126.8 . . ?
N C24 H24C 109.5 . . ?
N C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
N C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
O2 C25 W 177.7(3) . . ?
O3 C26 W 174.2(3) . . ?
O4 C27 W 177.2(3) . . ?
O5 C28 W 175.2(4) . . ?
O6 C29 W 178.8(4) . . ?
C24 N C8 111.2(3) . . ?
C24 N P 118.8(2) . . ?
C8 N P 119.3(2) . . ?
C21 O1 C20 106.5(3) . . ?
N P C2 107.92(14) . . ?
N P C1 109.42(14) . . ?
C2 P C1 50.60(13) . . ?
N P W 121.58(10) . . ?
C2 P W 121.37(10) . . ?
C1 P W 125.21(10) . . ?
C25 W C28 84.09(17) . . ?
C25 W C29 91.12(15) . . ?
C28 W C29 90.51(16) . . ?
C25 W C27 94.61(14) . . ?
C28 W C27 91.60(15) . . ?
C29 W C27 174.07(13) . . ?
C25 W C26 87.13(15) . . ?
C28 W C26 171.09(14) . . ?
C29 W C26 91.18(14) . . ?
C27 W C26 87.58(13) . . ?
C25 W P 176.52(11) . . ?
C28 W P 94.57(12) . . ?
C29 W P 85.67(10) . . ?
C27 W P 88.64(9) . . ?
C26 W P 94.28(9) . . ?

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
C9 C1 C2 C3 131.7(3) . . . . ?
C6 C1 C2 C3 -2.5(3) . . . . ?
P C1 C2 C3 -118.7(2) . . . . ?
C9 C1 C2 P -109.6(3) . . . . ?
C6 C1 C2 P 116.2(2) . . . . ?
C1 C2 C3 C15 167.1(2) . . . . ?
P C2 C3 C15 97.0(3) . . . . ?
C1 C2 C3 C4 -66.0(3) . . . . ?
P C2 C3 C4 -136.1(2) . . . . ?
C1 C2 C3 C7 36.8(3) . . . . ?
P C2 C3 C7 -33.3(3) . . . . ?
C15 C3 C4 C5 -163.3(3) . . . . ?
C2 C3 C4 C5 71.2(3) . . . . ?
C7 C3 C4 C5 -33.7(3) . . . . ?
C15 C3 C4 C16 23.2(4) . . . . ?
C2 C3 C4 C16 -102.3(3) . . . . ?
C7 C3 C4 C16 152.8(3) . . . . ?
C16 C4 C5 C17 -4.1(6) . . . . ?
C3 C4 C5 C17 -177.1(3) . . . . ?
C16 C4 C5 C6 172.6(3) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C4 C5 C6 C18 162.3(3) . . . . ?
C17 C5 C6 C18 -20.8(4) . . . . ?
C4 C5 C6 C7 34.2(3) . . . . ?
C17 C5 C6 C7 -148.8(3) . . . . ?
C4 C5 C6 C1 -72.2(3) . . . . ?
C17 C5 C6 C1 104.8(3) . . . . ?
C9 C1 C6 C18 60.5(4) . . . . ?
C2 C1 C6 C18 -162.0(3) . . . . ?
P C1 C6 C18 -95.3(3) . . . . ?
C9 C1 C6 C5 -66.7(3) . . . . ?
C2 C1 C6 C5 70.8(3) . . . . ?
P C1 C6 C5 137.5(2) . . . . ?
C9 C1 C6 C7 -170.0(2) . . . . ?
C2 C1 C6 C7 -32.4(3) . . . . ?
P C1 C6 C7 34.2(3) . . . . ?
C15 C3 C7 C19 63.0(4) . . . . ?
C4 C3 C7 C19 -65.0(3) . . . . ?
C2 C3 C7 C19 -169.6(2) . . . . ?
C15 C3 C7 C8 -62.5(4) . . . . ?
C4 C3 C7 C8 169.5(3) . . . . ?
C2 C3 C7 C8 64.9(3) . . . . ?
C15 C3 C7 C6 178.6(3) . . . . ?
C4 C3 C7 C6 50.6(2) . . . . ?
C2 C3 C7 C6 -54.0(2) . . . . ?
C18 C6 C7 C19 -62.5(3) . . . . ?
C5 C6 C7 C19 65.4(3) . . . . ?
C1 C6 C7 C19 169.6(2) . . . . ?
C18 C6 C7 C8 56.5(4) . . . . ?
C5 C6 C7 C8 -175.6(2) . . . . ?
C1 C6 C7 C8 -71.4(3) . . . . ?
C18 C6 C7 C3 -179.0(3) . . . . ?
C5 C6 C7 C3 -51.1(2) . . . . ?
C1 C6 C7 C3 53.1(2) . . . . ?
C19 C7 C8 N -176.2(3) . . . . ?
C3 C7 C8 N -47.1(4) . . . . ?
C6 C7 C8 N 61.2(4) . . . . ?
C19 C7 C8 C20 -48.8(4) . . . . ?
C3 C7 C8 C20 80.2(3) . . . . ?
C6 C7 C8 C20 -171.5(3) . . . . ?
C2 C1 C9 C10 -36.8(4) . . . . ?
C6 C1 C9 C10 91.0(3) . . . . ?
P C1 C9 C10 -113.4(3) . . . . ?
C2 C1 C9 C14 144.2(3) . . . . ?
C6 C1 C9 C14 -88.0(3) . . . . ?
P C1 C9 C14 67.6(3) . . . . ?
C14 C9 C10 C11 0.1(5) . . . . ?
C1 C9 C10 C11 -178.9(3) . . . . ?
C9 C10 C11 C12 -0.5(5) . . . . ?
C10 C11 C12 C13 0.4(5) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C9 -0.4(5) . . . . ?
C10 C9 C14 C13 0.3(5) . . . . ?
C1 C9 C14 C13 179.4(3) . . . . ?
N C8 C20 C23 40.1(5) . . . . ?
C7 C8 C20 C23 -90.9(5) . . . . ?
N C8 C20 O1 -135.0(3) . . . . ?
C7 C8 C20 O1 94.0(3) . . . . ?
O1 C21 C22 C23 -0.6(4) . . . . ?
O1 C20 C23 C22 -0.2(4) . . . . ?
C8 C20 C23 C22 -175.6(3) . . . . ?
C21 C22 C23 C20 0.5(4) . . . . ?
C20 C8 N C24 76.6(3) . . . . ?
C7 C8 N C24 -152.0(3) . . . . ?
C20 C8 N P -139.3(2) . . . . ?
C7 C8 N P -7.9(4) . . . . ?
C22 C21 O1 C20 0.5(4) . . . . ?
C23 C20 O1 C21 -0.1(4) . . . . ?
C8 C20 O1 C21 176.2(3) . . . . ?
C24 N P C2 172.1(3) . . . . ?
C8 N P C2 30.7(3) . . . . ?
C24 N P C1 118.5(3) . . . . ?
C8 N P C1 -22.9(3) . . . . ?
C24 N P W -40.7(3) . . . . ?
C8 N P W 178.0(2) . . . . ?
C3 C2 P N -7.9(3) . . . . ?
C1 C2 P N -100.76(18) . . . . ?
C3 C2 P C1 92.9(3) . . . . ?
C3 C2 P W -155.19(19) . . . . ?
C1 C2 P W 111.91(14) . . . . ?
C9 C1 P N -147.3(2) . . . . ?
C2 C1 P N 97.62(18) . . . . ?
C6 C1 P N 8.0(3) . . . . ?
C9 C1 P C2 115.1(3) . . . . ?
C6 C1 P C2 -89.6(2) . . . . ?
C9 C1 P W 10.9(3) . . . . ?
C2 C1 P W -104.17(15) . . . . ?
C6 C1 P W 166.21(16) . . . . ?
O2 C25 W C28 -43(10) . . . . ?
O2 C25 W C29 47(10) . . . . ?
O2 C25 W C27 -134(10) . . . . ?
O2 C25 W C26 138(10) . . . . ?
O2 C25 W P 25(11) . . . . ?
O5 C28 W C25 -13(5) . . . . ?
O5 C28 W C29 -104(5) . . . . ?
O5 C28 W C27 81(5) . . . . ?
O5 C28 W C26 -3(5) . . . . ?
O5 C28 W P 170(5) . . . . ?
O6 C29 W C25 151(20) . . . . ?
O6 C29 W C28 -125(20) . . . . ?
O6 C29 W C27 -14(21) . . . . ?
O6 C29 W C26 63(20) . . . . ?
O6 C29 W P -31(20) . . . . ?
O4 C27 W C25 -145(6) . . . . ?
O4 C27 W C28 131(6) . . . . ?
O4 C27 W C29 20(7) . . . . ?
O4 C27 W C26 -58(6) . . . . ?
O4 C27 W P 36(6) . . . . ?
O3 C26 W C25 9(3) . . . . ?
O3 C26 W C28 -1(3) . . . . ?
O3 C26 W C29 100(3) . . . . ?
O3 C26 W C27 -86(3) . . . . ?
O3 C26 W P -174(3) . . . . ?
N P W C25 -78(2) . . . . ?
C2 P W C25 65(2) . . . . ?
C1 P W C25 126(2) . . . . ?
N P W C28 -10.53(18) . . . . ?
C2 P W C28 132.39(16) . . . . ?
C1 P W C28 -166.27(16) . . . . ?
N P W C29 -100.70(17) . . . . ?
C2 P W C29 42.23(16) . . . . ?
C1 P W C29 103.57(16) . . . . ?
N P W C27 80.96(16) . . . . ?
C2 P W C27 -136.12(15) . . . . ?
C1 P W C27 -74.77(15) . . . . ?
N P W C26 168.44(16) . . . . ?
C2 P W C26 -48.64(15) . . . . ?
C1 P W C26 12.70(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.382
_refine_diff_density_min         -2.255
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 949202'