# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1412494'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H36 N O3 P3 W'
_chemical_formula_sum            'C42 H36 N O3 P3 W'
_chemical_formula_weight         879.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   10.23450(11)
_cell_length_b                   19.2654(3)
_cell_length_c                   18.46010(20)
_cell_angle_alpha                90
_cell_angle_beta                 94.9551(9)
_cell_angle_gamma                90
_cell_volume                     3626.21(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    6109
_cell_measurement_theta_min      4.5970
_cell_measurement_theta_max      73.5960

_exptl_crystal_description       needles
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             1752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    7.482
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            12470
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.322
_diffrn_reflns_theta_max         73.735
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             6984
_reflns_number_gt                6205
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0194P)²+0.3093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6984
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0492
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.005
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.55901(2) 0.24001(2) 0.63288(2) 0.02142(4) Uani 1 1 d . . . . .
N1 N 0.4031(2) 0.34095(12) 0.48455(12) 0.0282(5) Uani 1 1 d . . . . .
C2 C 0.4283(3) 0.27563(15) 0.44824(14) 0.0295(5) Uani 1 1 d . . . . .
H2A H 0.5065 0.2814 0.4208 0.035 Uiso 1 1 calc R U . . .
H2B H 0.3528 0.2652 0.4127 0.035 Uiso 1 1 calc R U . . .
P3 P 0.45586(6) 0.20013(3) 0.51141(3) 0.02451(13) Uani 1 1 d . . . . .
C4 C 0.5162(3) 0.38343(15) 0.50535(15) 0.0302(6) Uani 1 1 d . . . . .
H4A H 0.4857 0.4258 0.5292 0.036 Uiso 1 1 calc R U . . .
H4B H 0.5547 0.3983 0.4605 0.036 Uiso 1 1 calc R U . . .
P5 P 0.65136(6) 0.34275(4) 0.56826(3) 0.02588(13) Uani 1 1 d . . . . .
C6 C 0.3013(2) 0.33905(15) 0.53502(13) 0.0273(5) Uani 1 1 d . . . . .
H6A H 0.2355 0.3036 0.5182 0.033 Uiso 1 1 calc R U . . .
H6B H 0.2563 0.3846 0.5339 0.033 Uiso 1 1 calc R U . . .
P7 P 0.36335(6) 0.31892(3) 0.63201(3) 0.02351(13) Uani 1 1 d . . . . .
C8 C 0.2940(3) 0.15808(14) 0.50277(14) 0.0286(5) Uani 1 1 d . . . . .
C9 C 0.2220(3) 0.14740(14) 0.56224(15) 0.0300(5) Uani 1 1 d . . . . .
H9A H 0.2566 0.1622 0.6091 0.036 Uiso 1 1 calc R U . . .
C10 C 0.0993(3) 0.11510(16) 0.55404(18) 0.0378(6) Uani 1 1 d . . . . .
H10A H 0.0514 0.1080 0.5952 0.045 Uiso 1 1 calc R U . . .
C11 C 0.0478(3) 0.09350(19) 0.4862(2) 0.0462(8) Uani 1 1 d . . . . .
H11A H -0.0357 0.0716 0.4807 0.055 Uiso 1 1 calc R U . . .
C12 C 0.1180(3) 0.1038(2) 0.42655(18) 0.0485(8) Uani 1 1 d . . . . .
H12A H 0.0825 0.0887 0.3799 0.058 Uiso 1 1 calc R U . . .
C13 C 0.2400(3) 0.13599(18) 0.43406(17) 0.0405(7) Uani 1 1 d . . . . .
H13A H 0.2872 0.1431 0.3925 0.049 Uiso 1 1 calc R U . . .
C14 C 0.5472(3) 0.13830(15) 0.46033(14) 0.0285(5) Uani 1 1 d . . . . .
C15 C 0.5946(3) 0.07882(15) 0.49588(16) 0.0323(6) Uani 1 1 d . . . . .
H15A H 0.5787 0.0717 0.5453 0.039 Uiso 1 1 calc R U . . .
C16 C 0.6648(3) 0.02966(17) 0.46055(18) 0.0394(7) Uani 1 1 d . . . . .
H16A H 0.6957 -0.0110 0.4856 0.047 Uiso 1 1 calc R U . . .
C17 C 0.6898(3) 0.03983(18) 0.38880(19) 0.0453(8) Uani 1 1 d . . . . .
H17A H 0.7393 0.0066 0.3647 0.054 Uiso 1 1 calc R U . . .
C18 C 0.6429(4) 0.09825(19) 0.35256(18) 0.0480(8) Uani 1 1 d . . . . .
H18A H 0.6596 0.1051 0.3033 0.058 Uiso 1 1 calc R U . . .
C19 C 0.5711(3) 0.14729(17) 0.38747(16) 0.0417(7) Uani 1 1 d . . . . .
H19A H 0.5381 0.1872 0.3617 0.050 Uiso 1 1 calc R U . . .
C20 C 0.7821(3) 0.33115(16) 0.50661(15) 0.0319(6) Uani 1 1 d . . . . .
C21 C 0.8087(3) 0.26561(19) 0.48082(16) 0.0404(7) Uani 1 1 d . . . . .
H21A H 0.7616 0.2266 0.4962 0.048 Uiso 1 1 calc R U . . .
C22 C 0.9053(4) 0.2569(2) 0.43206(18) 0.0509(9) Uani 1 1 d . . . . .
H22A H 0.9222 0.2119 0.4140 0.061 Uiso 1 1 calc R U . . .
C23 C 0.9753(3) 0.3124(3) 0.41025(18) 0.0533(10) Uani 1 1 d . . . . .
H23A H 1.0407 0.3060 0.3774 0.064 Uiso 1 1 calc R U . . .
C24 C 0.9505(4) 0.3772(2) 0.4362(2) 0.0545(9) Uani 1 1 d . . . . .
H24A H 0.9992 0.4159 0.4212 0.065 Uiso 1 1 calc R U . . .
C25 C 0.8552(3) 0.3870(2) 0.48400(19) 0.0466(8) Uani 1 1 d . . . . .
H25A H 0.8394 0.4323 0.5017 0.056 Uiso 1 1 calc R U . . .
C26 C 0.7159(3) 0.41868(15) 0.62087(15) 0.0301(6) Uani 1 1 d . . . . .
C27 C 0.6893(3) 0.48699(16) 0.59897(17) 0.0369(6) Uani 1 1 d . . . . .
H27A H 0.6366 0.4954 0.5549 0.044 Uiso 1 1 calc R U . . .
C28 C 0.7381(3) 0.54262(18) 0.6400(2) 0.0463(8) Uani 1 1 d . . . . .
H28A H 0.7179 0.5887 0.6245 0.056 Uiso 1 1 calc R U . . .
C29 C 0.8163(4) 0.53127(19) 0.7039(2) 0.0507(9) Uani 1 1 d . . . . .
H29A H 0.8495 0.5694 0.7325 0.061 Uiso 1 1 calc R U . . .
C30 C 0.8459(3) 0.4637(2) 0.7258(2) 0.0501(8) Uani 1 1 d . . . . .
H30A H 0.9005 0.4557 0.7693 0.060 Uiso 1 1 calc R U . . .
C31 C 0.7962(3) 0.40797(17) 0.68457(17) 0.0383(7) Uani 1 1 d . . . . .
H31A H 0.8173 0.3620 0.7000 0.046 Uiso 1 1 calc R U . . .
C32 C 0.3700(3) 0.40558(14) 0.67403(14) 0.0287(5) Uani 1 1 d . . . . .
C33 C 0.2657(3) 0.45189(18) 0.66145(17) 0.0415(7) Uani 1 1 d . . . . .
H33A H 0.1914 0.4391 0.6298 0.050 Uiso 1 1 calc R U . . .
C34 C 0.2697(4) 0.51661(18) 0.69500(19) 0.0504(9) Uani 1 1 d . . . . .
H34A H 0.1988 0.5481 0.6856 0.060 Uiso 1 1 calc R U . . .
C35 C 0.3760(4) 0.53524(17) 0.74178(18) 0.0469(8) Uani 1 1 d . . . . .
H35A H 0.3785 0.5796 0.7644 0.056 Uiso 1 1 calc R U . . .
C36 C 0.4789(4) 0.48944(17) 0.75574(17) 0.0426(7) Uani 1 1 d . . . . .
H36A H 0.5524 0.5024 0.7879 0.051 Uiso 1 1 calc R U . . .
C37 C 0.4752(3) 0.42428(15) 0.72281(15) 0.0321(6) Uani 1 1 d . . . . .
H37A H 0.5450 0.3924 0.7338 0.039 Uiso 1 1 calc R U . . .
C38 C 0.2206(3) 0.28452(14) 0.67292(14) 0.0264(5) Uani 1 1 d . . . . .
C39 C 0.2434(3) 0.25130(15) 0.73986(15) 0.0303(6) Uani 1 1 d . . . . .
H39A H 0.3296 0.2500 0.7635 0.036 Uiso 1 1 calc R U . . .
C40 C 0.1411(3) 0.22015(16) 0.77230(16) 0.0343(6) Uani 1 1 d . . . . .
H40A H 0.1577 0.1972 0.8177 0.041 Uiso 1 1 calc R U . . .
C41 C 0.0145(3) 0.22240(17) 0.73850(18) 0.0396(7) Uani 1 1 d . . . . .
H41A H -0.0553 0.2003 0.7602 0.048 Uiso 1 1 calc R U . . .
C42 C -0.0089(3) 0.25691(17) 0.67341(18) 0.0390(7) Uani 1 1 d . . . . .
H42A H -0.0959 0.2594 0.6510 0.047 Uiso 1 1 calc R U . . .
C43 C 0.0926(3) 0.28827(16) 0.63989(16) 0.0344(6) Uani 1 1 d . . . . .
H43A H 0.0750 0.3120 0.5950 0.041 Uiso 1 1 calc R U . . .
C44 C 0.6401(3) 0.26450(15) 0.73092(14) 0.0293(5) Uani 1 1 d . . . . .
O44 O 0.6878(2) 0.27155(14) 0.78938(11) 0.0474(6) Uani 1 1 d . . . . .
C45 C 0.4748(3) 0.16325(15) 0.68242(14) 0.0296(6) Uani 1 1 d . . . . .
O45 O 0.4311(2) 0.11821(12) 0.71353(13) 0.0454(5) Uani 1 1 d . . . . .
C46 C 0.7075(3) 0.17380(15) 0.62669(14) 0.0291(6) Uani 1 1 d . . . . .
O46 O 0.7899(2) 0.13360(12) 0.62734(13) 0.0439(5) 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
W1 C45 1.975(3) . ?
W1 C44 1.982(3) . ?
W1 C46 1.995(3) . ?
W1 P7 2.5131(6) . ?
W1 P3 2.5148(6) . ?
W1 P5 2.5354(7) . ?
N1 C4 1.442(4) . ?
N1 C6 1.457(3) . ?
N1 C2 1.459(4) . ?
C2 P3 1.870(3) . ?
P3 C14 1.826(3) . ?
P3 C8 1.839(3) . ?
C4 P5 1.897(3) . ?
P5 C20 1.844(3) . ?
P5 C26 1.846(3) . ?
C6 P7 1.888(3) . ?
P7 C38 1.826(3) . ?
P7 C32 1.840(3) . ?
C8 C9 1.389(4) . ?
C8 C13 1.405(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.380(5) . ?
C11 C12 1.381(5) . ?
C12 C13 1.391(5) . ?
C14 C15 1.387(4) . ?
C14 C19 1.399(4) . ?
C15 C16 1.385(4) . ?
C16 C17 1.385(5) . ?
C17 C18 1.375(5) . ?
C18 C19 1.389(5) . ?
C20 C21 1.385(5) . ?
C20 C25 1.395(5) . ?
C21 C22 1.403(4) . ?
C22 C23 1.367(6) . ?
C23 C24 1.369(6) . ?
C24 C25 1.384(5) . ?
C26 C31 1.391(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.381(5) . ?
C28 C29 1.384(5) . ?
C29 C30 1.388(5) . ?
C30 C31 1.388(5) . ?
C32 C37 1.390(4) . ?
C32 C33 1.396(4) . ?
C33 C34 1.391(5) . ?
C34 C35 1.377(5) . ?
C35 C36 1.381(5) . ?
C36 C37 1.394(4) . ?
C38 C39 1.393(4) . ?
C38 C43 1.399(4) . ?
C39 C40 1.386(4) . ?
C40 C41 1.389(4) . ?
C41 C42 1.376(5) . ?
C42 C43 1.392(4) . ?
C44 O44 1.154(4) . ?
C45 O45 1.152(4) . ?
C46 O46 1.145(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C45 W1 C44 85.44(12) . . ?
C45 W1 C46 84.99(11) . . ?
C44 W1 C46 86.76(11) . . ?
C45 W1 P7 94.39(8) . . ?
C44 W1 P7 97.62(8) . . ?
C46 W1 P7 175.53(8) . . ?
C45 W1 P3 91.02(8) . . ?
C44 W1 P3 175.94(8) . . ?
C46 W1 P3 90.96(8) . . ?
P7 W1 P3 84.62(2) . . ?
C45 W1 P5 175.94(8) . . ?
C44 W1 P5 95.74(8) . . ?
C46 W1 P5 98.95(8) . . ?
P7 W1 P5 81.60(2) . . ?
P3 W1 P5 87.93(2) . . ?
C4 N1 C6 116.5(2) . . ?
C4 N1 C2 116.2(2) . . ?
C6 N1 C2 115.9(2) . . ?
N1 C2 P3 114.04(17) . . ?
C14 P3 C8 99.53(13) . . ?
C14 P3 C2 104.00(12) . . ?
C8 P3 C2 101.67(13) . . ?
C14 P3 W1 117.74(9) . . ?
C8 P3 W1 121.17(9) . . ?
C2 P3 W1 110.33(9) . . ?
N1 C4 P5 117.04(19) . . ?
C20 P5 C26 100.08(13) . . ?
C20 P5 C4 101.65(12) . . ?
C26 P5 C4 101.74(13) . . ?
C20 P5 W1 121.05(10) . . ?
C26 P5 W1 120.14(9) . . ?
C4 P5 W1 109.19(9) . . ?
N1 C6 P7 114.26(17) . . ?
C38 P7 C32 99.03(12) . . ?
C38 P7 C6 104.55(12) . . ?
C32 P7 C6 102.16(12) . . ?
C38 P7 W1 116.31(9) . . ?
C32 P7 W1 123.07(9) . . ?
C6 P7 W1 109.46(8) . . ?
C9 C8 C13 118.4(3) . . ?
C9 C8 P3 122.1(2) . . ?
C13 C8 P3 119.5(2) . . ?
C8 C9 C10 120.9(3) . . ?
C11 C10 C9 120.1(3) . . ?
C10 C11 C12 119.7(3) . . ?
C11 C12 C13 120.6(3) . . ?
C12 C13 C8 120.3(3) . . ?
C15 C14 C19 118.3(3) . . ?
C15 C14 P3 117.9(2) . . ?
C19 C14 P3 123.8(2) . . ?
C16 C15 C14 121.1(3) . . ?
C17 C16 C15 120.0(3) . . ?
C18 C17 C16 119.7(3) . . ?
C17 C18 C19 120.5(3) . . ?
C18 C19 C14 120.4(3) . . ?
C21 C20 C25 118.3(3) . . ?
C21 C20 P5 119.8(2) . . ?
C25 C20 P5 121.9(3) . . ?
C20 C21 C22 120.0(3) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C24 119.6(3) . . ?
C23 C24 C25 120.6(4) . . ?
C24 C25 C20 120.8(4) . . ?
C31 C26 C27 118.1(3) . . ?
C31 C26 P5 119.1(2) . . ?
C27 C26 P5 122.9(2) . . ?
C28 C27 C26 121.3(3) . . ?
C27 C28 C29 120.0(3) . . ?
C28 C29 C30 119.5(3) . . ?
C31 C30 C29 120.4(3) . . ?
C30 C31 C26 120.7(3) . . ?
C37 C32 C33 118.7(3) . . ?
C37 C32 P7 120.5(2) . . ?
C33 C32 P7 120.7(2) . . ?
C34 C33 C32 120.4(3) . . ?
C35 C34 C33 120.3(3) . . ?
C34 C35 C36 119.9(3) . . ?
C35 C36 C37 120.1(3) . . ?
C32 C37 C36 120.4(3) . . ?
C39 C38 C43 119.3(3) . . ?
C39 C38 P7 117.1(2) . . ?
C43 C38 P7 123.6(2) . . ?
C40 C39 C38 120.5(3) . . ?
C39 C40 C41 120.1(3) . . ?
C42 C41 C40 119.5(3) . . ?
C41 C42 C43 121.1(3) . . ?
C42 C43 C38 119.4(3) . . ?
O44 C44 W1 173.0(3) . . ?
O45 C45 W1 176.7(2) . . ?
O46 C46 W1 175.3(2) . . ?

_refine_diff_density_max         0.595
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.069

_shelxl_version_number           2013-4
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1412495'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H37 N O3 P3 W, B F4, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C43.50 H40 B Cl3 F4 N O3 P3 W'
_chemical_formula_weight         1094.68

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.1122(4)
_cell_length_b                   35.0113(8)
_cell_length_c                   13.3447(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8462.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173
_cell_measurement_reflns_used    5760
_cell_measurement_theta_min      2.8450
_cell_measurement_theta_max      28.3830

_exptl_crystal_description       blocks
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_F_000             4344
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.093
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            18835
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.577
_diffrn_reflns_theta_max         28.212
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             8710
_reflns_number_gt                6893
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0143P)²+210.7588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8710
_refine_ls_number_parameters     510
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0761
_refine_ls_wR_factor_ref         0.1669
_refine_ls_wR_factor_gt          0.1602
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.137
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.28735(2) 0.42801(2) 0.48697(3) 0.01584(12) Uani 1 1 d . . . . .
N1 N 0.3751(4) 0.3343(2) 0.4639(6) 0.0168(17) Uani 1 1 d D . . . .
H1 H 0.395(3) 0.3116(9) 0.448(7) 0.03(3) Uiso 1 1 d D . . . .
C2 C 0.2975(6) 0.3279(3) 0.4251(7) 0.021(2) Uani 1 1 d . . . . .
H2A H 0.2679 0.3159 0.4788 0.025 Uiso 1 1 calc R U . . .
H2B H 0.2998 0.3098 0.3684 0.025 Uiso 1 1 calc R U . . .
P3 P 0.24875(15) 0.37202(7) 0.3823(2) 0.0186(5) Uani 1 1 d D . . . .
C4 C 0.3787(5) 0.3419(3) 0.5746(7) 0.017(2) Uani 1 1 d . . . . .
H4A H 0.4302 0.3485 0.5924 0.020 Uiso 1 1 calc R U . . .
H4B H 0.3660 0.3180 0.6105 0.020 Uiso 1 1 calc R U . . .
P5 P 0.31650(14) 0.38095(7) 0.62095(19) 0.0164(5) Uani 1 1 d . . . . .
C6 C 0.4228(6) 0.3609(3) 0.4006(8) 0.022(2) Uani 1 1 d . . . . .
H6A H 0.4081 0.3582 0.3295 0.026 Uiso 1 1 calc R U . . .
H6B H 0.4749 0.3527 0.4064 0.026 Uiso 1 1 calc R U . . .
P7 P 0.41683(14) 0.41199(7) 0.43526(19) 0.0151(5) Uani 1 1 d . . . . .
C8 C 0.2637(5) 0.3741(3) 0.2462(8) 0.019(2) Uani 1 1 d . . . . .
C9 C 0.2308(6) 0.4041(3) 0.1954(8) 0.026(2) Uani 1 1 d . . . . .
H9A H 0.2034 0.4225 0.2320 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2372(6) 0.4078(3) 0.0918(9) 0.030(3) Uani 1 1 d . . . . .
H10A H 0.2133 0.4282 0.0579 0.036 Uiso 1 1 calc R U . . .
C11 C 0.2786(7) 0.3816(4) 0.0390(9) 0.037(3) Uani 1 1 d . . . . .
H11A H 0.2849 0.3846 -0.0312 0.045 Uiso 1 1 calc R U . . .
C12 C 0.3113(6) 0.3508(4) 0.0876(8) 0.031(3) Uani 1 1 d . . . . .
H12A H 0.3388 0.3325 0.0504 0.037 Uiso 1 1 calc R U . . .
C13 C 0.3035(6) 0.3468(3) 0.1911(8) 0.025(2) Uani 1 1 d . . . . .
H13A H 0.3252 0.3256 0.2243 0.030 Uiso 1 1 calc R U . . .
C14 C 0.1524(6) 0.3551(5) 0.3761(15) 0.019(5) Uani 0.52(3) 1 d DG U P A 1
C15 C 0.0948(9) 0.3779(4) 0.4101(17) 0.024(5) Uani 0.52(3) 1 d G U P A 1
H15A H 0.1050 0.4018 0.4408 0.029 Uiso 0.52(3) 1 calc R U P A 1
C16 C 0.0222(8) 0.3657(4) 0.3991(15) 0.029(6) Uani 0.52(3) 1 d G U P A 1
H16A H -0.0172 0.3813 0.4223 0.035 Uiso 0.52(3) 1 calc R U P A 1
C17 C 0.0072(5) 0.3308(4) 0.3542(14) 0.019(4) Uani 0.52(3) 1 d G U P A 1
H17A H -0.0424 0.3225 0.3467 0.023 Uiso 0.52(3) 1 calc R U P A 1
C18 C 0.0648(7) 0.3080(4) 0.3202(17) 0.032(6) Uani 0.52(3) 1 d G U P A 1
H18A H 0.0546 0.2841 0.2895 0.038 Uiso 0.52(3) 1 calc R U P A 1
C19 C 0.1374(6) 0.3201(5) 0.3312(17) 0.032(6) Uani 0.52(3) 1 d G U P A 1
H19A H 0.1768 0.3046 0.3079 0.038 Uiso 0.52(3) 1 calc R U P A 1
C14' C 0.1552(8) 0.3513(6) 0.3871(19) 0.022(6) Uiso 0.48(3) 1 d DG U P A 2
C15' C 0.0967(12) 0.3770(5) 0.389(2) 0.020(6) Uiso 0.48(3) 1 d G U P A 2
H15B H 0.1061 0.4037 0.3918 0.024 Uiso 0.48(3) 1 calc R U P A 2
C16' C 0.0245(10) 0.3636(5) 0.3868(19) 0.025(6) Uiso 0.48(3) 1 d G U P A 2
H16B H -0.0155 0.3812 0.3881 0.030 Uiso 0.48(3) 1 calc R U P A 2
C17' C 0.0107(6) 0.3246(6) 0.3827(16) 0.024(6) Uiso 0.48(3) 1 d G U P A 2
H17B H -0.0387 0.3155 0.3811 0.028 Uiso 0.48(3) 1 calc R U P A 2
C18' C 0.0692(9) 0.2989(4) 0.3808(19) 0.035(6) Uiso 0.48(3) 1 d G U P A 2
H18B H 0.0598 0.2723 0.3780 0.042 Uiso 0.48(3) 1 calc R U P A 2
C19' C 0.1415(7) 0.3123(6) 0.3830(18) 0.034(6) Uiso 0.48(3) 1 d G U P A 2
H19B H 0.1815 0.2947 0.3817 0.041 Uiso 0.48(3) 1 calc R U P A 2
C20 C 0.2452(6) 0.3520(3) 0.6838(8) 0.022(2) Uani 1 1 d . . . . .
C21 C 0.1740(7) 0.3507(3) 0.6430(9) 0.027(2) Uani 1 1 d . . . . .
H21A H 0.1616 0.3659 0.5864 0.033 Uiso 1 1 calc R U . . .
C22 C 0.1211(7) 0.3266(4) 0.6874(11) 0.040(3) Uani 1 1 d . . . . .
H22A H 0.0729 0.3249 0.6599 0.048 Uiso 1 1 calc R U . . .
C23 C 0.1398(8) 0.3051(4) 0.7725(11) 0.045(4) Uani 1 1 d . . . . .
H23A H 0.1041 0.2890 0.8028 0.054 Uiso 1 1 calc R U . . .
C24 C 0.2101(9) 0.3073(4) 0.8124(12) 0.055(4) Uani 1 1 d . . . . .
H24A H 0.2222 0.2933 0.8712 0.066 Uiso 1 1 calc R U . . .
C25 C 0.2625(7) 0.3297(4) 0.7671(10) 0.040(3) Uani 1 1 d . . . . .
H25A H 0.3114 0.3301 0.7929 0.048 Uiso 1 1 calc R U . . .
C26 C 0.3696(6) 0.3983(3) 0.7285(7) 0.017(2) Uani 1 1 d . . . . .
C27 C 0.4352(7) 0.3839(3) 0.7640(9) 0.033(3) Uani 1 1 d . . . . .
H27A H 0.4567 0.3623 0.7319 0.040 Uiso 1 1 calc R U . . .
C28 C 0.4705(7) 0.3999(4) 0.8451(9) 0.031(3) Uani 1 1 d . . . . .
H28A H 0.5162 0.3897 0.8674 0.037 Uiso 1 1 calc R U . . .
C29 C 0.4399(7) 0.4307(3) 0.8940(8) 0.031(3) Uani 1 1 d . . . . .
H29A H 0.4649 0.4419 0.9492 0.037 Uiso 1 1 calc R U . . .
C30 C 0.3730(7) 0.4451(3) 0.8628(9) 0.028(3) Uani 1 1 d . . . . .
H30A H 0.3507 0.4657 0.8979 0.034 Uiso 1 1 calc R U . . .
C31 C 0.3386(6) 0.4295(3) 0.7804(7) 0.022(2) Uani 1 1 d . . . . .
H31A H 0.2930 0.4399 0.7581 0.026 Uiso 1 1 calc R U . . .
C32 C 0.4927(5) 0.4181(3) 0.5260(7) 0.0136(19) Uani 1 1 d . . . . .
C33 C 0.5479(6) 0.3919(3) 0.5432(9) 0.026(2) Uani 1 1 d . . . . .
H33A H 0.5471 0.3681 0.5089 0.031 Uiso 1 1 calc R U . . .
C34 C 0.6045(6) 0.3997(4) 0.6099(9) 0.029(3) Uani 1 1 d . . . . .
H34A H 0.6415 0.3811 0.6224 0.035 Uiso 1 1 calc R U . . .
C35 C 0.6071(6) 0.4349(4) 0.6586(8) 0.030(3) Uani 1 1 d . . . . .
H35A H 0.6459 0.4403 0.7045 0.036 Uiso 1 1 calc R U . . .
C36 C 0.5543(6) 0.4615(3) 0.6403(9) 0.032(3) Uani 1 1 d . . . . .
H36A H 0.5566 0.4856 0.6729 0.039 Uiso 1 1 calc R U . . .
C37 C 0.4969(6) 0.4536(3) 0.5740(8) 0.023(2) Uani 1 1 d . . . . .
H37A H 0.4603 0.4725 0.5613 0.028 Uiso 1 1 calc R U . . .
C38 C 0.4553(5) 0.4332(3) 0.3219(7) 0.0162(19) Uani 1 1 d . . . . .
C39 C 0.5307(6) 0.4444(3) 0.3141(8) 0.021(2) Uani 1 1 d . . . . .
H39A H 0.5643 0.4393 0.3671 0.025 Uiso 1 1 calc R U . . .
C40 C 0.5542(6) 0.4629(3) 0.2281(8) 0.025(2) Uani 1 1 d . . . . .
H40A H 0.6043 0.4707 0.2232 0.030 Uiso 1 1 calc R U . . .
C41 C 0.5074(7) 0.4703(3) 0.1502(8) 0.028(3) Uani 1 1 d . . . . .
H41A H 0.5251 0.4829 0.0918 0.033 Uiso 1 1 calc R U . . .
C42 C 0.4343(6) 0.4594(3) 0.1566(8) 0.026(2) Uani 1 1 d . . . . .
H42A H 0.4018 0.4646 0.1025 0.032 Uiso 1 1 calc R U . . .
C43 C 0.4080(6) 0.4409(3) 0.2417(8) 0.019(2) Uani 1 1 d . . . . .
H43A H 0.3576 0.4335 0.2453 0.022 Uiso 1 1 calc R U . . .
C44 C 0.3180(5) 0.4733(3) 0.5667(8) 0.019(2) Uani 1 1 d . . . . .
O44 O 0.3304(5) 0.5008(2) 0.6100(6) 0.0329(19) Uani 1 1 d . . . . .
C45 C 0.2706(6) 0.4663(3) 0.3795(8) 0.020(2) Uani 1 1 d . . . . .
O45 O 0.2606(5) 0.4901(2) 0.3201(6) 0.038(2) Uani 1 1 d . . . . .
C46 C 0.1861(5) 0.4400(3) 0.5384(8) 0.019(2) Uani 1 1 d . . . . .
O46 O 0.1315(5) 0.4504(2) 0.5687(7) 0.040(2) Uani 1 1 d . . . . .
B10 B 0.3918(11) 0.2500 0.2722(14) 0.027(4) Uani 1 2 d S T P . .
F11 F 0.4038(7) 0.2500 0.1700(8) 0.047(3) Uani 1 2 d S T P . .
F12 F 0.3157(6) 0.2500 0.2942(8) 0.040(3) Uani 1 2 d S T P . .
F13 F 0.4228(4) 0.28237(17) 0.3165(5) 0.0341(16) Uani 1 1 d . . . . .
B20 B 0.4557(11) 0.2500 0.5708(16) 0.029(4) Uani 1 2 d S T P . .
F21 F 0.4621(11) 0.2500 0.6704(11) 0.098(6) Uani 1 2 d S T P . .
F22 F 0.3831(6) 0.2500 0.5385(9) 0.044(3) Uani 1 2 d S T P . .
F23 F 0.4902(4) 0.28304(19) 0.5309(7) 0.050(2) 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
W1 C45 1.985(10) . ?
W1 C44 1.988(10) . ?
W1 C46 2.003(10) . ?
W1 P5 2.488(3) . ?
W1 P3 2.507(3) . ?
W1 P7 2.508(3) . ?
N1 C4 1.502(12) . ?
N1 C2 1.514(13) . ?
N1 C6 1.526(13) . ?
C2 P3 1.867(10) . ?
P3 C8 1.838(11) . ?
P3 C14' 1.844(11) . ?
P3 C14 1.844(9) . ?
C4 P5 1.877(9) . ?
P5 C26 1.831(10) . ?
P5 C20 1.845(11) . ?
C6 P7 1.849(11) . ?
P7 C38 1.824(10) . ?
P7 C32 1.845(9) . ?
C8 C9 1.384(15) . ?
C8 C13 1.405(14) . ?
C9 C10 1.393(16) . ?
C10 C11 1.379(17) . ?
C11 C12 1.391(17) . ?
C12 C13 1.395(15) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C14' C15' 1.3900 . ?
C14' C19' 1.3900 . ?
C15' C16' 1.3900 . ?
C16' C17' 1.3900 . ?
C17' C18' 1.3900 . ?
C18' C19' 1.3900 . ?
C20 C25 1.392(16) . ?
C20 C21 1.400(15) . ?
C21 C22 1.407(16) . ?
C22 C23 1.403(19) . ?
C23 C24 1.38(2) . ?
C24 C25 1.372(18) . ?
C26 C27 1.376(15) . ?
C26 C31 1.410(13) . ?
C27 C28 1.375(15) . ?
C28 C29 1.375(16) . ?
C29 C30 1.378(16) . ?
C30 C31 1.378(15) . ?
C32 C33 1.376(14) . ?
C32 C37 1.402(13) . ?
C33 C34 1.385(15) . ?
C34 C35 1.394(17) . ?
C35 C36 1.357(17) . ?
C36 C37 1.394(14) . ?
C38 C43 1.397(13) . ?
C38 C39 1.424(14) . ?
C39 C40 1.384(14) . ?
C40 C41 1.366(15) . ?
C41 C42 1.380(16) . ?
C42 C43 1.391(14) . ?
C44 O44 1.146(12) . ?
C45 O45 1.166(12) . ?
C46 O46 1.128(12) . ?
B10 F11 1.38(2) . ?
B10 F13 1.396(14) 7_565 ?
B10 F13 1.396(14) . ?
B10 F12 1.41(2) . ?
B20 F21 1.33(2) . ?
B20 F22 1.38(2) . ?
B20 F23 1.419(14) . ?
B20 F23 1.419(14) 7_565 ?

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
C45 W1 C44 83.8(4) . . ?
C45 W1 C46 88.0(4) . . ?
C44 W1 C46 84.6(4) . . ?
C45 W1 P5 176.5(3) . . ?
C44 W1 P5 94.8(3) . . ?
C46 W1 P5 95.0(3) . . ?
C45 W1 P3 94.7(3) . . ?
C44 W1 P3 178.4(3) . . ?
C46 W1 P3 95.7(3) . . ?
P5 W1 P3 86.66(9) . . ?
C45 W1 P7 95.4(3) . . ?
C44 W1 P7 93.7(3) . . ?
C46 W1 P7 175.9(3) . . ?
P5 W1 P7 81.45(8) . . ?
P3 W1 P7 86.13(8) . . ?
C4 N1 C2 113.8(8) . . ?
C4 N1 C6 114.4(8) . . ?
C2 N1 C6 115.2(8) . . ?
N1 C2 P3 114.9(6) . . ?
C8 P3 C14' 100.7(8) . . ?
C8 P3 C14 96.2(7) . . ?
C8 P3 C2 105.4(5) . . ?
C14' P3 C2 95.7(8) . . ?
C14 P3 C2 101.3(7) . . ?
C8 P3 W1 118.6(3) . . ?
C14' P3 W1 123.0(7) . . ?
C14 P3 W1 122.7(5) . . ?
C2 P3 W1 110.1(3) . . ?
N1 C4 P5 115.2(6) . . ?
C26 P5 C20 101.2(5) . . ?
C26 P5 C4 100.6(4) . . ?
C20 P5 C4 99.7(5) . . ?
C26 P5 W1 117.1(3) . . ?
C20 P5 W1 122.9(4) . . ?
C4 P5 W1 111.9(3) . . ?
N1 C6 P7 114.7(7) . . ?
C38 P7 C32 102.3(4) . . ?
C38 P7 C6 99.4(5) . . ?
C32 P7 C6 103.5(4) . . ?
C38 P7 W1 119.7(3) . . ?
C32 P7 W1 119.4(3) . . ?
C6 P7 W1 109.9(3) . . ?
C9 C8 C13 118.7(10) . . ?
C9 C8 P3 116.8(8) . . ?
C13 C8 P3 124.5(8) . . ?
C8 C9 C10 121.4(10) . . ?
C11 C10 C9 119.3(11) . . ?
C10 C11 C12 120.7(11) . . ?
C11 C12 C13 119.7(11) . . ?
C12 C13 C8 120.1(10) . . ?
C15 C14 C19 120.0 . . ?
C15 C14 P3 120.8(9) . . ?
C19 C14 P3 119.1(9) . . ?
C14 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C14 120.0 . . ?
C15' C14' C19' 120.0 . . ?
C15' C14' P3 116.5(13) . . ?
C19' C14' P3 123.4(13) . . ?
C16' C15' C14' 120.0 . . ?
C15' C16' C17' 120.0 . . ?
C18' C17' C16' 120.0 . . ?
C17' C18' C19' 120.0 . . ?
C18' C19' C14' 120.0 . . ?
C25 C20 C21 120.0(10) . . ?
C25 C20 P5 120.8(9) . . ?
C21 C20 P5 119.0(8) . . ?
C20 C21 C22 118.8(11) . . ?
C23 C22 C21 119.8(12) . . ?
C24 C23 C22 120.3(12) . . ?
C25 C24 C23 119.9(13) . . ?
C24 C25 C20 121.0(12) . . ?
C27 C26 C31 117.4(9) . . ?
C27 C26 P5 127.0(8) . . ?
C31 C26 P5 115.6(8) . . ?
C28 C27 C26 121.5(11) . . ?
C27 C28 C29 120.4(11) . . ?
C28 C29 C30 119.8(11) . . ?
C31 C30 C29 119.6(10) . . ?
C30 C31 C26 121.3(10) . . ?
C33 C32 C37 118.6(9) . . ?
C33 C32 P7 125.0(8) . . ?
C37 C32 P7 116.3(7) . . ?
C32 C33 C34 120.8(11) . . ?
C33 C34 C35 120.0(10) . . ?
C36 C35 C34 119.9(10) . . ?
C35 C36 C37 120.3(11) . . ?
C36 C37 C32 120.4(10) . . ?
C43 C38 C39 118.6(9) . . ?
C43 C38 P7 118.7(7) . . ?
C39 C38 P7 122.6(7) . . ?
C40 C39 C38 119.0(10) . . ?
C41 C40 C39 121.9(11) . . ?
C40 C41 C42 119.7(10) . . ?
C41 C42 C43 120.6(10) . . ?
C42 C43 C38 120.3(9) . . ?
O44 C44 W1 174.3(9) . . ?
O45 C45 W1 176.6(9) . . ?
O46 C46 W1 173.2(9) . . ?
F11 B10 F13 110.8(9) . 7_565 ?
F11 B10 F13 110.8(9) . . ?
F13 B10 F13 108.5(15) 7_565 . ?
F11 B10 F12 111.1(16) . . ?
F13 B10 F12 107.8(9) 7_565 . ?
F13 B10 F12 107.8(9) . . ?
F21 B20 F22 113.1(19) . . ?
F21 B20 F23 109.7(11) . . ?
F22 B20 F23 107.5(11) . . ?
F21 B20 F23 109.7(11) . 7_565 ?
F22 B20 F23 107.5(11) . 7_565 ?
F23 B20 F23 109.3(15) . 7_565 ?

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
N1 H1 F13 0.9000(11) 2.10(6) 2.816(10) 136(8) .
N1 H1 F22 0.9000(11) 2.48(6) 3.120(9) 128(6) .
N1 H1 F23 0.9000(11) 2.27(7) 2.893(11) 126(7) .

_refine_diff_density_max         1.729
_refine_diff_density_min         -5.917
_refine_diff_density_rms         0.203

_shelxl_version_number           2013-4

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.179 0.250 -0.250 497 248 ' '
2 0.808 0.750 0.250 497 249 ' '
_platon_squeeze_details          
;
 SQUEEZE suggested 498 e/cell = 62.3 e/asu
 The solvents used were ether (C4H10O, 42e), dcm (CH2Cl2, 42e),
 water (H2O, 10e) and methanol (CH4O, 18e).
 Before the use of SQUEEZE the solvent most resembled dcm.
 1.5CH2Cl2 = 63e, so this was used as the solvent present.
 
 So, the atom list is low by 1.5(CH2Cl2) = C1.5 H3 Cl3 and the UNIT is
 low by C12 H24 Cl24, i.e. C336 H296 B8 N8 O24 F32 P24 W8 Cl0
 
 The missing 5 non-H atoms would have required 45 variables (5 x 9)
 if refined anisotropically.
 The L.S. instruction was adjusted appropriately.
;
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1412496'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H24 F12 N O3 P3 W'
_chemical_formula_sum            'C42 H24 F12 N O3 P3 W'
_chemical_formula_weight         1095.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   10.3366(2)
_cell_length_b                   8.3660(2)
_cell_length_c                   45.8955(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.650(2)
_cell_angle_gamma                90
_cell_volume                     3964.62(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    5278
_cell_measurement_theta_min      3.8380
_cell_measurement_theta_max      73.5960

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_F_000             2136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    7.445
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            12719
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         73.773
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             7582
_reflns_number_gt                6523
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+8.0987P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000297(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7582
_refine_ls_number_parameters     560
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_restrained_S_all      1.249
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.26926(2) 0.32848(3) 0.12962(2) 0.01857(9) Uani 1 1 d . . . . .
N1 N 0.4688(4) 0.6845(6) 0.12083(9) 0.0236(9) Uani 1 1 d . . . . .
C2 C 0.4072(5) 0.7232(7) 0.14792(12) 0.0240(11) Uani 1 1 d . . . . .
H2A H 0.3616 0.8266 0.1453 0.029 Uiso 1 1 calc R U . . .
H2B H 0.4760 0.7384 0.1634 0.029 Uiso 1 1 calc R U . . .
P3 P 0.28820(13) 0.57209(17) 0.16122(3) 0.0210(3) Uani 1 1 d . . . . .
C4 C 0.3861(5) 0.6901(7) 0.09444(11) 0.0244(11) Uani 1 1 d . . . . .
H4A H 0.4414 0.7096 0.0778 0.029 Uiso 1 1 calc R U . . .
H4B H 0.3273 0.7829 0.0958 0.029 Uiso 1 1 calc R U . . .
P5 P 0.28481(13) 0.50736(17) 0.08612(3) 0.0203(3) Uani 1 1 d . . . . .
C6 C 0.5673(5) 0.5590(7) 0.12275(12) 0.0248(11) Uani 1 1 d . . . . .
H6A H 0.6301 0.5867 0.1389 0.030 Uiso 1 1 calc R U . . .
H6B H 0.6147 0.5608 0.1045 0.030 Uiso 1 1 calc R U . . .
P7 P 0.51007(12) 0.34719(16) 0.12879(3) 0.0195(3) Uani 1 1 d . . . . .
C8 C 0.3373(5) 0.5688(8) 0.20023(12) 0.0284(12) Uani 1 1 d . . . . .
C9 C 0.3621(7) 0.4245(9) 0.21440(14) 0.0435(17) Uani 1 1 d . . . . .
H9A H 0.3500 0.3256 0.2045 0.052 Uiso 1 1 calc R U . . .
C10 C 0.4048(8) 0.4292(11) 0.24333(15) 0.053(2) Uani 1 1 d . . . . .
F10 F 0.4286(7) 0.2886(8) 0.25695(11) 0.094(2) Uani 1 1 d . . . . .
C11 C 0.4242(8) 0.5687(13) 0.25865(15) 0.060(2) Uani 1 1 d . . . . .
H11A H 0.4540 0.5680 0.2785 0.072 Uiso 1 1 calc R U . . .
C12 C 0.3988(7) 0.7087(11) 0.24414(15) 0.051(2) Uani 1 1 d . . . . .
F12 F 0.4170(6) 0.8472(8) 0.25831(11) 0.0818(18) Uani 1 1 d . . . . .
C13 C 0.3552(6) 0.7118(9) 0.21518(14) 0.0381(15) Uani 1 1 d . . . . .
H13A H 0.3378 0.8108 0.2056 0.046 Uiso 1 1 calc R U . . .
C14 C 0.1347(5) 0.6822(7) 0.16215(11) 0.0236(11) Uani 1 1 d . . . . .
C15 C 0.0489(6) 0.6429(8) 0.18361(12) 0.0324(14) Uani 1 1 d . . . . .
H15A H 0.0730 0.5693 0.1987 0.039 Uiso 1 1 calc R U . . .
C16 C -0.0712(6) 0.7127(9) 0.18247(14) 0.0390(16) Uani 1 1 d . . . . .
F16 F -0.1549(4) 0.6758(8) 0.20325(10) 0.0663(14) Uani 1 1 d . . . . .
C17 C -0.1113(6) 0.8189(10) 0.16131(16) 0.0454(17) Uani 1 1 d . . . . .
H17A H -0.1947 0.8667 0.1611 0.054 Uiso 1 1 calc R U . . .
C18 C -0.0248(7) 0.8532(9) 0.14025(15) 0.0412(16) Uani 1 1 d . . . . .
F18 F -0.0611(5) 0.9571(7) 0.11866(12) 0.0688(15) Uani 1 1 d . . . . .
C19 C 0.0969(6) 0.7891(8) 0.14022(13) 0.0341(14) Uani 1 1 d . . . . .
H19A H 0.1544 0.8170 0.1255 0.041 Uiso 1 1 calc R U . . .
C20 C 0.1454(6) 0.5930(7) 0.06544(12) 0.0269(12) Uani 1 1 d . . . . .
C21 C 0.1606(8) 0.6616(11) 0.03832(14) 0.053(2) Uani 1 1 d . . . . .
H21A H 0.2433 0.6659 0.0302 0.064 Uiso 1 1 calc R U . . .
C22 C 0.0524(9) 0.7238(12) 0.02335(15) 0.062(3) Uani 1 1 d . . . . .
F22 F 0.0680(7) 0.7890(11) -0.00309(11) 0.122(3) Uani 1 1 d . U . . .
C23 C -0.0696(8) 0.7177(10) 0.03364(16) 0.052(2) Uani 1 1 d . . . . .
H23A H -0.1430 0.7572 0.0227 0.063 Uiso 1 1 calc R U . . .
C24 C -0.0797(6) 0.6510(9) 0.06074(16) 0.0398(15) Uani 1 1 d . . . . .
F24 F -0.1988(4) 0.6471(7) 0.07210(13) 0.0703(16) Uani 1 1 d . . . . .
C25 C 0.0237(6) 0.5889(7) 0.07709(14) 0.0309(13) Uani 1 1 d . . . . .
H25A H 0.0121 0.5445 0.0958 0.037 Uiso 1 1 calc R U . . .
C26 C 0.3669(5) 0.4117(7) 0.05565(11) 0.0230(11) Uani 1 1 d . . . . .
C27 C 0.4903(5) 0.4528(7) 0.04747(11) 0.0250(11) Uani 1 1 d . . . . .
H27A H 0.5353 0.5398 0.0566 0.030 Uiso 1 1 calc R U . . .
C28 C 0.5465(6) 0.3656(8) 0.02597(12) 0.0295(13) Uani 1 1 d . . . . .
F28 F 0.6668(4) 0.4070(5) 0.01839(8) 0.0430(9) Uani 1 1 d . . . . .
C29 C 0.4866(6) 0.2375(8) 0.01207(12) 0.0331(14) Uani 1 1 d . . . . .
H29A H 0.5277 0.1774 -0.0024 0.040 Uiso 1 1 calc R U . . .
C30 C 0.3640(6) 0.2019(7) 0.02046(12) 0.0313(13) Uani 1 1 d . . . . .
F30 F 0.3019(4) 0.0761(5) 0.00735(8) 0.0422(9) Uani 1 1 d . . . . .
C31 C 0.3009(6) 0.2850(7) 0.04189(11) 0.0269(12) Uani 1 1 d . . . . .
H31A H 0.2159 0.2566 0.0470 0.032 Uiso 1 1 calc R U . . .
C32 C 0.6068(5) 0.2355(7) 0.10286(11) 0.0221(11) Uani 1 1 d . . . . .
C33 C 0.7332(6) 0.2804(7) 0.09837(12) 0.0272(12) Uani 1 1 d . . . . .
H33A H 0.7719 0.3671 0.1089 0.033 Uiso 1 1 calc R U . . .
C34 C 0.8023(5) 0.1967(7) 0.07827(12) 0.0267(12) Uani 1 1 d . . . . .
F34 F 0.9249(3) 0.2410(5) 0.07380(9) 0.0434(9) Uani 1 1 d . . . . .
C35 C 0.7527(5) 0.0694(7) 0.06274(12) 0.0260(12) Uani 1 1 d . . . . .
H35A H 0.8017 0.0141 0.0489 0.031 Uiso 1 1 calc R U . . .
C36 C 0.6271(6) 0.0260(7) 0.06829(12) 0.0263(12) Uani 1 1 d . . . . .
F36 F 0.5744(4) -0.0995(5) 0.05309(8) 0.0385(9) Uani 1 1 d . . . . .
C37 C 0.5524(5) 0.1048(7) 0.08786(11) 0.0232(11) Uani 1 1 d . . . . .
H37A H 0.4664 0.0712 0.0910 0.028 Uiso 1 1 calc R U . . .
C38 C 0.5926(5) 0.2809(7) 0.16322(11) 0.0238(11) Uani 1 1 d . . . . .
C39 C 0.5867(6) 0.1174(7) 0.16849(13) 0.0281(12) Uani 1 1 d . . . . .
H39A H 0.5519 0.0464 0.1540 0.034 Uiso 1 1 calc R U . . .
C40 C 0.6328(6) 0.0608(8) 0.19532(14) 0.0330(13) Uani 1 1 d . . . . .
F40 F 0.6259(4) -0.0991(5) 0.20020(9) 0.0497(10) Uani 1 1 d . . . . .
C41 C 0.6816(7) 0.1574(10) 0.21709(14) 0.0480(18) Uani 1 1 d . . . . .
H41A H 0.7110 0.1160 0.2355 0.058 Uiso 1 1 calc R U . . .
C42 C 0.6859(9) 0.3147(10) 0.21101(15) 0.058(2) Uani 1 1 d . . . . .
F42 F 0.7286(9) 0.4161(8) 0.23226(12) 0.118(3) Uani 1 1 d . U . . .
C43 C 0.6414(8) 0.3828(9) 0.18461(15) 0.0440(17) Uani 1 1 d . . . . .
H43A H 0.6447 0.4950 0.1815 0.053 Uiso 1 1 calc R U . . .
C44 C 0.2344(5) 0.1447(7) 0.10312(12) 0.0268(12) Uani 1 1 d . . . . .
O44 O 0.2084(4) 0.0335(5) 0.08880(9) 0.0322(9) Uani 1 1 d . . . . .
C45 C 0.2760(5) 0.1679(8) 0.16156(12) 0.0273(12) Uani 1 1 d . . . . .
O45 O 0.2766(5) 0.0678(6) 0.17882(10) 0.0411(11) Uani 1 1 d . . . . .
C46 C 0.0798(5) 0.3357(7) 0.13596(12) 0.0255(11) Uani 1 1 d . . . . .
O46 O -0.0273(4) 0.3378(7) 0.14146(10) 0.0413(11) 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
W1 C44 1.983(6) . ?
W1 C45 1.987(6) . ?
W1 C46 1.994(5) . ?
W1 P7 2.4961(13) . ?
W1 P3 2.5038(14) . ?
W1 P5 2.5059(13) . ?
N1 C4 1.450(7) . ?
N1 C2 1.459(6) . ?
N1 C6 1.463(7) . ?
C2 P3 1.885(6) . ?
P3 C14 1.837(6) . ?
P3 C8 1.839(6) . ?
C4 P5 1.882(6) . ?
P5 C20 1.834(6) . ?
P5 C26 1.851(5) . ?
C6 P7 1.892(6) . ?
P7 C32 1.844(6) . ?
P7 C38 1.846(5) . ?
C8 C13 1.387(9) . ?
C8 C9 1.389(10) . ?
C9 C10 1.380(10) . ?
C10 F10 1.349(10) . ?
C10 C11 1.373(13) . ?
C11 C12 1.366(13) . ?
C12 F12 1.338(10) . ?
C12 C13 1.384(9) . ?
C14 C19 1.389(9) . ?
C14 C15 1.395(8) . ?
C15 C16 1.371(9) . ?
C16 F16 1.352(8) . ?
C16 C17 1.366(11) . ?
C17 C18 1.377(10) . ?
C18 F18 1.358(8) . ?
C18 C19 1.368(9) . ?
C20 C21 1.386(9) . ?
C20 C25 1.390(9) . ?
C21 C22 1.386(10) . ?
C22 F22 1.347(9) . ?
C22 C23 1.368(12) . ?
C23 C24 1.371(11) . ?
C24 F24 1.359(8) . ?
C24 C25 1.379(9) . ?
C26 C27 1.390(8) . ?
C26 C31 1.395(8) . ?
C27 C28 1.377(8) . ?
C28 F28 1.352(7) . ?
C28 C29 1.379(9) . ?
C29 C30 1.374(9) . ?
C30 F30 1.359(7) . ?
C30 C31 1.391(8) . ?
C32 C33 1.384(8) . ?
C32 C37 1.397(8) . ?
C33 C34 1.383(8) . ?
C34 F34 1.345(7) . ?
C34 C35 1.367(9) . ?
C35 C36 1.384(8) . ?
C36 F36 1.360(7) . ?
C36 C37 1.379(8) . ?
C38 C43 1.379(9) . ?
C38 C39 1.390(9) . ?
C39 C40 1.383(8) . ?
C40 F40 1.359(8) . ?
C40 C41 1.363(10) . ?
C41 C42 1.347(12) . ?
C42 F42 1.351(9) . ?
C42 C43 1.397(10) . ?
C44 O44 1.163(7) . ?
C45 O45 1.153(8) . ?
C46 O46 1.147(7) . ?

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
C44 W1 C45 85.8(2) . . ?
C44 W1 C46 87.8(2) . . ?
C45 W1 C46 85.1(2) . . ?
C44 W1 P7 101.08(16) . . ?
C45 W1 P7 93.02(16) . . ?
C46 W1 P7 170.79(16) . . ?
C44 W1 P3 173.46(16) . . ?
C45 W1 P3 97.11(17) . . ?
C46 W1 P3 86.67(17) . . ?
P7 W1 P3 84.63(4) . . ?
C44 W1 P5 89.49(16) . . ?
C45 W1 P5 171.88(16) . . ?
C46 W1 P5 101.41(17) . . ?
P7 W1 P5 81.36(4) . . ?
P3 W1 P5 88.23(4) . . ?
C4 N1 C2 116.2(4) . . ?
C4 N1 C6 117.1(4) . . ?
C2 N1 C6 116.0(4) . . ?
N1 C2 P3 116.4(4) . . ?
C14 P3 C8 100.6(3) . . ?
C14 P3 C2 104.4(3) . . ?
C8 P3 C2 99.8(3) . . ?
C14 P3 W1 112.18(18) . . ?
C8 P3 W1 124.2(2) . . ?
C2 P3 W1 113.15(17) . . ?
N1 C4 P5 116.3(4) . . ?
C20 P5 C26 98.9(2) . . ?
C20 P5 C4 101.8(3) . . ?
C26 P5 C4 103.6(3) . . ?
C20 P5 W1 124.6(2) . . ?
C26 P5 W1 113.08(18) . . ?
C4 P5 W1 112.28(17) . . ?
N1 C6 P7 117.4(4) . . ?
C32 P7 C38 99.0(2) . . ?
C32 P7 C6 101.4(3) . . ?
C38 P7 C6 105.8(3) . . ?
C32 P7 W1 123.31(17) . . ?
C38 P7 W1 112.95(18) . . ?
C6 P7 W1 112.30(18) . . ?
C13 C8 C9 120.0(6) . . ?
C13 C8 P3 119.6(5) . . ?
C9 C8 P3 120.4(5) . . ?
C10 C9 C8 118.0(7) . . ?
F10 C10 C11 119.0(7) . . ?
F10 C10 C9 117.7(8) . . ?
C11 C10 C9 123.3(8) . . ?
C12 C11 C10 117.3(6) . . ?
F12 C12 C11 119.1(7) . . ?
F12 C12 C13 118.8(8) . . ?
C11 C12 C13 122.1(8) . . ?
C12 C13 C8 119.2(7) . . ?
C19 C14 C15 119.8(5) . . ?
C19 C14 P3 121.4(4) . . ?
C15 C14 P3 118.4(5) . . ?
C16 C15 C14 118.5(6) . . ?
F16 C16 C17 117.9(6) . . ?
F16 C16 C15 118.9(6) . . ?
C17 C16 C15 123.3(6) . . ?
C16 C17 C18 116.7(6) . . ?
F18 C18 C19 118.3(6) . . ?
F18 C18 C17 118.6(6) . . ?
C19 C18 C17 123.1(6) . . ?
C18 C19 C14 118.7(6) . . ?
C21 C20 C25 119.8(6) . . ?
C21 C20 P5 120.5(5) . . ?
C25 C20 P5 119.6(4) . . ?
C20 C21 C22 118.6(7) . . ?
F22 C22 C23 118.5(7) . . ?
F22 C22 C21 118.1(8) . . ?
C23 C22 C21 123.4(7) . . ?
C22 C23 C24 116.0(6) . . ?
F24 C24 C23 117.8(6) . . ?
F24 C24 C25 118.4(6) . . ?
C23 C24 C25 123.9(7) . . ?
C24 C25 C20 118.3(6) . . ?
C27 C26 C31 120.1(5) . . ?
C27 C26 P5 123.7(4) . . ?
C31 C26 P5 116.0(4) . . ?
C28 C27 C26 119.0(6) . . ?
F28 C28 C27 118.2(6) . . ?
F28 C28 C29 118.6(5) . . ?
C27 C28 C29 123.3(6) . . ?
C30 C29 C28 116.0(5) . . ?
F30 C30 C29 117.8(5) . . ?
F30 C30 C31 118.2(6) . . ?
C29 C30 C31 124.0(6) . . ?
C30 C31 C26 117.7(6) . . ?
C33 C32 C37 120.1(5) . . ?
C33 C32 P7 120.2(4) . . ?
C37 C32 P7 119.8(4) . . ?
C34 C33 C32 118.8(6) . . ?
F34 C34 C35 117.9(5) . . ?
F34 C34 C33 118.8(5) . . ?
C35 C34 C33 123.3(5) . . ?
C34 C35 C36 116.2(5) . . ?
F36 C36 C37 118.7(5) . . ?
F36 C36 C35 117.7(5) . . ?
C37 C36 C35 123.6(5) . . ?
C36 C37 C32 118.0(5) . . ?
C43 C38 C39 120.1(6) . . ?
C43 C38 P7 124.3(5) . . ?
C39 C38 P7 115.0(4) . . ?
C40 C39 C38 118.4(6) . . ?
F40 C40 C41 118.9(6) . . ?
F40 C40 C39 117.7(6) . . ?
C41 C40 C39 123.4(7) . . ?
C42 C41 C40 116.2(6) . . ?
C41 C42 F42 118.5(6) . . ?
C41 C42 C43 124.5(7) . . ?
F42 C42 C43 117.0(8) . . ?
C38 C43 C42 117.4(7) . . ?
O44 C44 W1 175.7(5) . . ?
O45 C45 W1 175.6(5) . . ?
O46 C46 W1 175.6(5) . . ?

_refine_diff_density_max         0.807
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.118

_shelxl_version_number           2013-4
####################################################################### 
# 
# 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_4'
_database_code_depnum_ccdc_archive 'CCDC 1412497'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H24 F12 N O3 P3 W'
_chemical_formula_sum            'C42 H24 F12 N O3 P3 W'
_chemical_formula_weight         1095.38

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'
F F 0.0171 0.0103 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.30064(15)
_cell_length_b                   10.2472(2)
_cell_length_c                   23.6539(5)
_cell_angle_alpha                101.9521(18)
_cell_angle_beta                 94.4676(17)
_cell_angle_gamma                90.3026(16)
_cell_volume                     1961.89(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173
_cell_measurement_reflns_used    13524
_cell_measurement_theta_min      2.6750
_cell_measurement_theta_max      28.6200

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_F_000             1068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.167
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.616
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            24942
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.462
_diffrn_reflns_theta_max         28.945
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8502
_reflns_number_gt                8104
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+15.9833P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8502
_refine_ls_number_parameters     559
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0431
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_restrained_S_all      1.329
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.39827(3) 0.37957(2) 0.26040(2) 0.01229(7) Uani 1 1 d . . . . .
N1 N 0.7474(6) 0.1677(5) 0.2388(2) 0.0182(10) Uani 1 1 d . . . . .
C2 C 0.8030(7) 0.2585(6) 0.2922(3) 0.0199(12) Uani 1 1 d . . . . .
H2A H 0.9041 0.3029 0.2857 0.024 Uiso 1 1 calc R U . . .
H2B H 0.8303 0.2052 0.3220 0.024 Uiso 1 1 calc R U . . .
P3 P 0.65868(18) 0.39164(15) 0.32242(6) 0.0150(3) Uani 1 1 d . . . . .
C4 C 0.7381(7) 0.2221(6) 0.1868(3) 0.0213(13) Uani 1 1 d . . . . .
H4A H 0.7484 0.1477 0.1532 0.026 Uiso 1 1 calc R U . . .
H4B H 0.8323 0.2832 0.1891 0.026 Uiso 1 1 calc R U . . .
P5 P 0.55164(18) 0.31410(15) 0.17209(6) 0.0154(3) Uani 1 1 d . . . . .
C6 C 0.6236(7) 0.0699(6) 0.2425(3) 0.0211(13) Uani 1 1 d . . . . .
H6A H 0.6616 0.0222 0.2732 0.025 Uiso 1 1 calc R U . . .
H6B H 0.6138 0.0036 0.2054 0.025 Uiso 1 1 calc R U . . .
P7 P 0.41448(18) 0.13430(14) 0.25809(6) 0.0147(3) Uani 1 1 d . . . . .
C8 C 0.6678(7) 0.3749(6) 0.3985(3) 0.0192(12) Uani 1 1 d . . . . .
C9 C 0.5287(8) 0.3531(6) 0.4236(3) 0.0207(13) Uani 1 1 d . . . . .
H9A H 0.4259 0.3504 0.4026 0.025 Uiso 1 1 calc R U . . .
C10 C 0.5430(8) 0.3351(7) 0.4809(3) 0.0254(14) Uani 1 1 d . . . . .
F10 F 0.4067(6) 0.3156(5) 0.50531(19) 0.0433(11) Uani 1 1 d . . . . .
C11 C 0.6895(10) 0.3365(7) 0.5120(3) 0.0324(16) Uani 1 1 d . . . . .
H11A H 0.6966 0.3237 0.5508 0.039 Uiso 1 1 calc R U . . .
C12 C 0.8253(9) 0.3571(7) 0.4854(3) 0.0309(16) Uani 1 1 d . . . . .
F12 F 0.9705(6) 0.3597(5) 0.5152(2) 0.0523(13) Uani 1 1 d . . . . .
C13 C 0.8188(8) 0.3764(7) 0.4289(3) 0.0252(14) Uani 1 1 d . . . . .
H13A H 0.9148 0.3903 0.4114 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7755(7) 0.5461(6) 0.3273(3) 0.0188(12) Uani 1 1 d . . . . .
C15 C 0.7812(8) 0.6467(6) 0.3772(3) 0.0243(14) Uani 1 1 d . . . . .
H15A H 0.7312 0.6338 0.4105 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8613(10) 0.7660(7) 0.3773(3) 0.0383(18) Uani 1 1 d . . . . .
F16 F 0.8714(8) 0.8611(5) 0.4258(2) 0.0661(17) Uani 1 1 d . . . . .
C17 C 0.9352(10) 0.7889(8) 0.3300(4) 0.044(2) Uani 1 1 d . . . . .
H17A H 0.9888 0.8714 0.3306 0.053 Uiso 1 1 calc R U . . .
C18 C 0.9278(10) 0.6866(8) 0.2821(3) 0.0387(18) Uani 1 1 d . . . . .
F18 F 0.9975(7) 0.7066(5) 0.2349(2) 0.0651(17) Uani 1 1 d . . . . .
C19 C 0.8493(8) 0.5674(7) 0.2793(3) 0.0270(14) Uani 1 1 d . . . . .
H19A H 0.8454 0.5001 0.2449 0.032 Uiso 1 1 calc R U . . .
C20 C 0.6268(7) 0.4308(6) 0.1302(3) 0.0212(13) Uani 1 1 d . . . . .
C21 C 0.6852(11) 0.3829(8) 0.0770(3) 0.043(2) Uani 1 1 d . . . . .
H21A H 0.6888 0.2895 0.0622 0.051 Uiso 1 1 calc R U . . .
C22 C 0.7378(12) 0.4708(9) 0.0458(3) 0.050(2) Uani 1 1 d . . . . .
F22 F 0.7939(10) 0.4248(7) -0.0065(2) 0.097(3) Uani 1 1 d . U . . .
C23 C 0.7341(10) 0.6072(8) 0.0651(3) 0.042(2) Uani 1 1 d . . . . .
H23A H 0.7681 0.6672 0.0424 0.051 Uiso 1 1 calc R U . . .
C24 C 0.6793(9) 0.6512(7) 0.1182(3) 0.0341(17) Uani 1 1 d . . . . .
F24 F 0.6775(7) 0.7843(4) 0.1395(3) 0.0618(16) Uani 1 1 d . . . . .
C25 C 0.6249(8) 0.5679(7) 0.1517(3) 0.0270(14) Uani 1 1 d . . . . .
H25A H 0.5871 0.6031 0.1886 0.032 Uiso 1 1 calc R U . . .
C26 C 0.4395(7) 0.1973(6) 0.1121(3) 0.0193(12) Uani 1 1 d . . . . .
C27 C 0.4764(8) 0.0629(6) 0.0945(3) 0.0211(13) Uani 1 1 d . . . . .
H27A H 0.5681 0.0268 0.1119 0.025 Uiso 1 1 calc R U . . .
C28 C 0.3769(9) -0.0165(6) 0.0513(3) 0.0267(14) Uani 1 1 d . . . . .
F28 F 0.4164(6) -0.1471(4) 0.03509(18) 0.0401(11) Uani 1 1 d . . . . .
C29 C 0.2435(9) 0.0268(7) 0.0245(3) 0.0292(15) Uani 1 1 d . . . . .
H29A H 0.1772 -0.0309 -0.0049 0.035 Uiso 1 1 calc R U . . .
C30 C 0.2104(8) 0.1606(7) 0.0428(3) 0.0265(14) Uani 1 1 d . . . . .
F30 F 0.0763(5) 0.2090(5) 0.01761(18) 0.0382(10) Uani 1 1 d . . . . .
C31 C 0.3036(8) 0.2471(6) 0.0848(3) 0.0226(13) Uani 1 1 d . . . . .
H31A H 0.2769 0.3385 0.0953 0.027 Uiso 1 1 calc R U . . .
C32 C 0.2865(7) 0.0084(6) 0.2060(3) 0.0175(12) Uani 1 1 d . . . . .
C33 C 0.3258(8) -0.1253(6) 0.1960(3) 0.0223(13) Uani 1 1 d . . . . .
H33A H 0.4175 -0.1535 0.2166 0.027 Uiso 1 1 calc R U . . .
C34 C 0.2329(8) -0.2162(6) 0.1567(3) 0.0250(14) Uani 1 1 d . . . . .
F34 F 0.2716(5) -0.3458(4) 0.14780(19) 0.0375(10) Uani 1 1 d . . . . .
C35 C 0.0998(7) -0.1804(6) 0.1250(3) 0.0227(13) Uani 1 1 d . . . . .
H35A H 0.0376 -0.2443 0.0967 0.027 Uiso 1 1 calc R U . . .
C36 C 0.0621(7) -0.0483(6) 0.1363(3) 0.0195(12) Uani 1 1 d . . . . .
F36 F -0.0682(5) -0.0108(4) 0.10570(17) 0.0319(9) Uani 1 1 d . . . . .
C37 C 0.1503(7) 0.0490(6) 0.1758(3) 0.0191(12) Uani 1 1 d . . . . .
H37A H 0.1199 0.1398 0.1823 0.023 Uiso 1 1 calc R U . . .
C38 C 0.3689(8) 0.0823(6) 0.3252(3) 0.0192(12) Uani 1 1 d . . . . .
C39 C 0.2155(8) 0.1143(6) 0.3435(3) 0.0219(13) Uani 1 1 d . . . . .
H39A H 0.1415 0.1577 0.3212 0.026 Uiso 1 1 calc R U . . .
C40 C 0.1725(9) 0.0828(6) 0.3938(3) 0.0284(15) Uani 1 1 d . . . . .
F40 F 0.0240(5) 0.1166(5) 0.4113(2) 0.0433(11) Uani 1 1 d . . . . .
C41 C 0.2738(11) 0.0199(8) 0.4280(3) 0.0387(18) Uani 1 1 d . . . . .
H41A H 0.2421 -0.0002 0.4630 0.046 Uiso 1 1 calc R U . . .
C42 C 0.4211(11) -0.0116(9) 0.4089(3) 0.045(2) Uani 1 1 d . . . . .
F42 F 0.5230(8) -0.0781(8) 0.4391(3) 0.087(2) Uani 1 1 d . . . . .
C43 C 0.4722(9) 0.0176(8) 0.3580(3) 0.0343(17) Uani 1 1 d . . . . .
H43A H 0.5766 -0.0068 0.3462 0.041 Uiso 1 1 calc R U . . .
C44 C 0.2001(7) 0.3885(6) 0.2098(3) 0.0180(12) Uani 1 1 d . . . . .
O44 O 0.0808(5) 0.4003(5) 0.1813(2) 0.0281(10) Uani 1 1 d . . . . .
C45 C 0.2527(8) 0.4165(6) 0.3240(3) 0.0204(13) Uani 1 1 d . . . . .
O45 O 0.1624(5) 0.4416(5) 0.3589(2) 0.0313(11) Uani 1 1 d . . . . .
C46 C 0.4195(8) 0.5770(6) 0.2734(3) 0.0212(13) Uani 1 1 d . . . . .
O46 O 0.4312(7) 0.6913(4) 0.2855(2) 0.0363(12) 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
W1 C44 1.972(6) . ?
W1 C45 1.980(6) . ?
W1 C46 1.987(6) . ?
W1 P3 2.5036(15) . ?
W1 P5 2.5054(15) . ?
W1 P7 2.5072(15) . ?
N1 C2 1.446(7) . ?
N1 C4 1.450(8) . ?
N1 C6 1.451(8) . ?
C2 P3 1.886(6) . ?
P3 C14 1.830(6) . ?
P3 C8 1.839(6) . ?
C4 P5 1.863(6) . ?
P5 C20 1.838(6) . ?
P5 C26 1.842(6) . ?
C6 P7 1.896(6) . ?
P7 C38 1.842(6) . ?
P7 C32 1.853(6) . ?
C8 C9 1.376(9) . ?
C8 C13 1.394(9) . ?
C9 C10 1.402(9) . ?
C10 F10 1.342(8) . ?
C10 C11 1.371(10) . ?
C11 C12 1.369(11) . ?
C12 F12 1.346(8) . ?
C12 C13 1.387(9) . ?
C14 C19 1.386(9) . ?
C14 C15 1.395(8) . ?
C15 C16 1.388(9) . ?
C16 F16 1.340(8) . ?
C16 C17 1.376(11) . ?
C17 C18 1.372(11) . ?
C18 F18 1.347(9) . ?
C18 C19 1.369(10) . ?
C20 C21 1.379(9) . ?
C20 C25 1.392(9) . ?
C21 C22 1.367(11) . ?
C22 F22 1.350(9) . ?
C22 C23 1.379(12) . ?
C23 C24 1.359(11) . ?
C24 F24 1.353(8) . ?
C24 C25 1.376(9) . ?
C26 C27 1.397(9) . ?
C26 C31 1.406(9) . ?
C27 C28 1.380(9) . ?
C28 C29 1.356(10) . ?
C28 F28 1.363(8) . ?
C29 C30 1.386(10) . ?
C30 F30 1.365(8) . ?
C30 C31 1.372(9) . ?
C32 C33 1.387(8) . ?
C32 C37 1.401(8) . ?
C33 C34 1.360(9) . ?
C34 F34 1.346(7) . ?
C34 C35 1.381(9) . ?
C35 C36 1.368(9) . ?
C36 F36 1.356(7) . ?
C36 C37 1.379(8) . ?
C38 C43 1.376(9) . ?
C38 C39 1.396(9) . ?
C39 C40 1.367(9) . ?
C40 F40 1.355(8) . ?
C40 C41 1.375(11) . ?
C41 C42 1.354(12) . ?
C42 F42 1.343(9) . ?
C42 C43 1.395(10) . ?
C44 O44 1.175(7) . ?
C45 O45 1.149(7) . ?
C46 O46 1.148(7) . ?

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
C44 W1 C45 84.6(2) . . ?
C44 W1 C46 88.6(2) . . ?
C45 W1 C46 84.4(3) . . ?
C44 W1 P3 173.89(17) . . ?
C45 W1 P3 97.30(18) . . ?
C46 W1 P3 85.80(18) . . ?
C44 W1 P5 89.26(18) . . ?
C45 W1 P5 172.27(18) . . ?
C46 W1 P5 100.11(19) . . ?
P3 W1 P5 89.32(5) . . ?
C44 W1 P7 101.95(17) . . ?
C45 W1 P7 95.14(18) . . ?
C46 W1 P7 169.36(19) . . ?
P3 W1 P7 83.71(5) . . ?
P5 W1 P7 81.57(5) . . ?
C2 N1 C4 116.3(5) . . ?
C2 N1 C6 116.8(5) . . ?
C4 N1 C6 116.8(5) . . ?
N1 C2 P3 116.5(4) . . ?
C14 P3 C8 102.3(3) . . ?
C14 P3 C2 102.9(3) . . ?
C8 P3 C2 100.6(3) . . ?
C14 P3 W1 113.5(2) . . ?
C8 P3 W1 122.6(2) . . ?
C2 P3 W1 112.47(19) . . ?
N1 C4 P5 116.5(4) . . ?
C20 P5 C26 98.4(3) . . ?
C20 P5 C4 101.6(3) . . ?
C26 P5 C4 103.4(3) . . ?
C20 P5 W1 124.9(2) . . ?
C26 P5 W1 113.81(19) . . ?
C4 P5 W1 112.0(2) . . ?
N1 C6 P7 117.1(4) . . ?
C38 P7 C32 98.2(3) . . ?
C38 P7 C6 105.5(3) . . ?
C32 P7 C6 100.9(3) . . ?
C38 P7 W1 115.66(19) . . ?
C32 P7 W1 122.7(2) . . ?
C6 P7 W1 111.6(2) . . ?
C9 C8 C13 120.9(6) . . ?
C9 C8 P3 120.4(5) . . ?
C13 C8 P3 118.7(5) . . ?
C8 C9 C10 118.1(6) . . ?
F10 C10 C11 119.8(6) . . ?
F10 C10 C9 117.8(6) . . ?
C11 C10 C9 122.4(6) . . ?
C12 C11 C10 117.7(6) . . ?
F12 C12 C11 118.8(6) . . ?
F12 C12 C13 118.7(7) . . ?
C11 C12 C13 122.5(6) . . ?
C12 C13 C8 118.4(6) . . ?
C19 C14 C15 119.5(6) . . ?
C19 C14 P3 119.5(5) . . ?
C15 C14 P3 120.8(5) . . ?
C16 C15 C14 118.7(6) . . ?
F16 C16 C17 118.6(7) . . ?
F16 C16 C15 118.8(7) . . ?
C17 C16 C15 122.6(7) . . ?
C18 C17 C16 116.6(7) . . ?
F18 C18 C19 118.5(7) . . ?
F18 C18 C17 118.1(7) . . ?
C19 C18 C17 123.4(7) . . ?
C18 C19 C14 119.1(6) . . ?
C21 C20 C25 119.4(6) . . ?
C21 C20 P5 120.1(5) . . ?
C25 C20 P5 120.5(5) . . ?
C22 C21 C20 119.5(7) . . ?
F22 C22 C21 119.9(8) . . ?
F22 C22 C23 117.4(7) . . ?
C21 C22 C23 122.7(7) . . ?
C24 C23 C22 116.4(7) . . ?
F24 C24 C23 118.4(7) . . ?
F24 C24 C25 117.9(7) . . ?
C23 C24 C25 123.7(7) . . ?
C24 C25 C20 118.3(7) . . ?
C27 C26 C31 119.0(6) . . ?
C27 C26 P5 124.1(5) . . ?
C31 C26 P5 116.8(5) . . ?
C28 C27 C26 118.6(6) . . ?
C29 C28 F28 118.4(6) . . ?
C29 C28 C27 124.4(6) . . ?
F28 C28 C27 117.2(6) . . ?
C28 C29 C30 115.6(6) . . ?
F30 C30 C31 118.1(6) . . ?
F30 C30 C29 118.0(6) . . ?
C31 C30 C29 123.9(6) . . ?
C30 C31 C26 118.5(6) . . ?
C33 C32 C37 119.7(5) . . ?
C33 C32 P7 120.6(5) . . ?
C37 C32 P7 119.7(4) . . ?
C34 C33 C32 119.9(6) . . ?
F34 C34 C33 119.3(6) . . ?
F34 C34 C35 118.3(6) . . ?
C33 C34 C35 122.4(6) . . ?
C36 C35 C34 116.6(6) . . ?
F36 C36 C35 117.6(5) . . ?
F36 C36 C37 118.3(5) . . ?
C35 C36 C37 124.1(6) . . ?
C36 C37 C32 117.3(6) . . ?
C43 C38 C39 118.8(6) . . ?
C43 C38 P7 125.8(5) . . ?
C39 C38 P7 115.4(5) . . ?
C40 C39 C38 119.5(6) . . ?
F40 C40 C39 118.6(6) . . ?
F40 C40 C41 118.3(6) . . ?
C39 C40 C41 123.2(7) . . ?
C42 C41 C40 116.2(7) . . ?
F42 C42 C41 119.1(7) . . ?
F42 C42 C43 117.5(8) . . ?
C41 C42 C43 123.5(7) . . ?
C38 C43 C42 118.9(7) . . ?
O44 C44 W1 176.5(5) . . ?
O45 C45 W1 176.0(6) . . ?
O46 C46 W1 174.7(6) . . ?

_refine_diff_density_max         2.065
_refine_diff_density_min         -3.068
_refine_diff_density_rms         0.154

_shelxl_version_number           2013-4
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1412498'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H48 N O4 P3 W'
_chemical_formula_sum            'C25 H48 N O4 P3 W'
_chemical_formula_weight         703.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   15.45700(18)
_cell_length_b                   12.41049(15)
_cell_length_c                   32.2167(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3745(14)
_cell_angle_gamma                90.00
_cell_volume                     6152.93(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    173
_cell_measurement_reflns_used    17780
_cell_measurement_theta_min      2.7530
_cell_measurement_theta_max      72.3485

_exptl_crystal_description       plates
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848
_exptl_absorpt_coefficient_mu    8.660
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19350
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         72.37
_reflns_number_total             19350
_reflns_number_gt                17023
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.1567P)²+64.9382P] 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         19350
_refine_ls_number_parameters     627
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0797
_refine_ls_wR_factor_ref         0.2588
_refine_ls_wR_factor_gt          0.2534
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1A W 0.36106(3) 0.11280(4) 0.173139(12) 0.02852(14) Uani 1 1 d . . .
N1A N 0.5100(5) 0.3561(6) 0.1314(2) 0.0300(16) Uani 1 1 d . . .
C2A C 0.4202(6) 0.3416(8) 0.1113(3) 0.033(2) Uani 1 1 d . . .
H2AA H 0.4165 0.3765 0.0836 0.039 Uiso 1 1 calc R . .
H2AB H 0.3799 0.3803 0.1283 0.039 Uiso 1 1 calc R . .
P3A P 0.38211(15) 0.20284(19) 0.10440(7) 0.0286(5) Uani 1 1 d . . .
C4A C 0.5141(9) 0.3396(9) 0.1766(3) 0.045(3) Uani 1 1 d . . .
H4AA H 0.4653 0.3793 0.1874 0.053 Uiso 1 1 calc R . .
H4AB H 0.5687 0.3719 0.1895 0.053 Uiso 1 1 calc R . .
P5A P 0.50929(17) 0.1963(2) 0.19419(7) 0.0320(5) Uani 1 1 d . . .
C6A C 0.5376(7) 0.4692(9) 0.1252(3) 0.039(2) Uani 1 1 d . . .
H6AA H 0.5950 0.4805 0.1409 0.046 Uiso 1 1 calc R . .
H6AB H 0.4957 0.5181 0.1370 0.046 Uiso 1 1 calc R . .
P7A P 0.54545(17) 0.5066(2) 0.06946(8) 0.0345(5) Uani 1 1 d . . .
C8A C 0.4627(6) 0.1498(9) 0.0698(3) 0.037(2) Uani 1 1 d . . .
H8AA H 0.5210 0.1682 0.0841 0.044 Uiso 1 1 calc R . .
C9A C 0.4615(8) 0.0280(11) 0.0661(4) 0.050(3) Uani 1 1 d . . .
H9AA H 0.5053 0.0051 0.0478 0.075 Uiso 1 1 calc R . .
H9AB H 0.4039 0.0043 0.0543 0.075 Uiso 1 1 calc R . .
H9AC H 0.4746 -0.0042 0.0937 0.075 Uiso 1 1 calc R . .
C10A C 0.4596(7) 0.2032(9) 0.0270(3) 0.042(2) Uani 1 1 d . . .
H10A H 0.5041 0.1711 0.0111 0.063 Uiso 1 1 calc R . .
H10B H 0.4707 0.2806 0.0304 0.063 Uiso 1 1 calc R . .
H10C H 0.4021 0.1921 0.0120 0.063 Uiso 1 1 calc R . .
C11A C 0.2835(6) 0.2308(10) 0.0682(3) 0.039(2) Uani 1 1 d . . .
H11A H 0.3015 0.2738 0.0442 0.047 Uiso 1 1 calc R . .
C12A C 0.2412(7) 0.1265(8) 0.0510(4) 0.042(2) Uani 1 1 d . . .
H12A H 0.1896 0.1440 0.0321 0.063 Uiso 1 1 calc R . .
H12B H 0.2243 0.0823 0.0741 0.063 Uiso 1 1 calc R . .
H12C H 0.2827 0.0866 0.0356 0.063 Uiso 1 1 calc R . .
C13A C 0.2164(7) 0.2967(10) 0.0897(4) 0.046(3) Uani 1 1 d . . .
H13A H 0.1654 0.3101 0.0700 0.068 Uiso 1 1 calc R . .
H13B H 0.2422 0.3656 0.0992 0.068 Uiso 1 1 calc R . .
H13C H 0.1989 0.2565 0.1137 0.068 Uiso 1 1 calc R . .
C14A C 0.6103(6) 0.1441(9) 0.1746(3) 0.039(2) Uani 1 1 d . . .
H14A H 0.6055 0.1615 0.1442 0.046 Uiso 1 1 calc R . .
C15A C 0.6175(7) 0.0218(11) 0.1774(4) 0.047(3) Uani 1 1 d . . .
H15A H 0.6718 -0.0015 0.1667 0.071 Uiso 1 1 calc R . .
H15B H 0.5681 -0.0110 0.1607 0.071 Uiso 1 1 calc R . .
H15C H 0.6172 -0.0007 0.2065 0.071 Uiso 1 1 calc R . .
C16A C 0.6956(8) 0.1997(11) 0.1934(4) 0.051(3) Uani 1 1 d . . .
H16A H 0.7455 0.1673 0.1815 0.076 Uiso 1 1 calc R . .
H16B H 0.7018 0.1898 0.2237 0.076 Uiso 1 1 calc R . .
H16C H 0.6930 0.2768 0.1869 0.076 Uiso 1 1 calc R . .
C17A C 0.5380(8) 0.2199(9) 0.2507(3) 0.042(3) Uani 1 1 d . . .
H17A H 0.5896 0.2688 0.2535 0.050 Uiso 1 1 calc R . .
C18A C 0.5631(8) 0.1175(10) 0.2745(4) 0.050(3) Uani 1 1 d . . .
H18A H 0.5779 0.1347 0.3040 0.074 Uiso 1 1 calc R . .
H18B H 0.6135 0.0846 0.2631 0.074 Uiso 1 1 calc R . .
H18C H 0.5142 0.0669 0.2719 0.074 Uiso 1 1 calc R . .
C19A C 0.4629(8) 0.2785(9) 0.2704(3) 0.043(2) Uani 1 1 d . . .
H19A H 0.4791 0.2899 0.3002 0.065 Uiso 1 1 calc R . .
H19B H 0.4102 0.2343 0.2667 0.065 Uiso 1 1 calc R . .
H19C H 0.4519 0.3482 0.2566 0.065 Uiso 1 1 calc R . .
C20A C 0.6649(8) 0.5005(10) 0.0670(4) 0.049(3) Uani 1 1 d . . .
H20A H 0.6948 0.5369 0.0921 0.059 Uiso 1 1 calc R . .
C21A C 0.6913(11) 0.3801(11) 0.0669(6) 0.074(5) Uani 1 1 d . . .
H21A H 0.7543 0.3743 0.0659 0.111 Uiso 1 1 calc R . .
H21B H 0.6615 0.3444 0.0425 0.111 Uiso 1 1 calc R . .
H21C H 0.6749 0.3454 0.0924 0.111 Uiso 1 1 calc R . .
C22A C 0.6883(8) 0.5577(11) 0.0275(4) 0.056(3) Uani 1 1 d . . .
H22A H 0.7513 0.5554 0.0263 0.084 Uiso 1 1 calc R . .
H22B H 0.6690 0.6329 0.0280 0.084 Uiso 1 1 calc R . .
H22C H 0.6594 0.5215 0.0030 0.084 Uiso 1 1 calc R . .
C23A C 0.5235(8) 0.6533(10) 0.0725(4) 0.047(3) Uani 1 1 d . . .
H23A H 0.5439 0.6859 0.0468 0.057 Uiso 1 1 calc R . .
C24A C 0.4295(9) 0.6759(11) 0.0710(5) 0.064(4) Uani 1 1 d . . .
H24A H 0.4203 0.7539 0.0726 0.095 Uiso 1 1 calc R . .
H24B H 0.4054 0.6405 0.0945 0.095 Uiso 1 1 calc R . .
H24C H 0.4005 0.6484 0.0447 0.095 Uiso 1 1 calc R . .
C25A C 0.5738(10) 0.7122(11) 0.1100(4) 0.059(3) Uani 1 1 d . . .
H25A H 0.5591 0.7890 0.1090 0.089 Uiso 1 1 calc R . .
H25B H 0.6365 0.7035 0.1084 0.089 Uiso 1 1 calc R . .
H25C H 0.5577 0.6811 0.1361 0.089 Uiso 1 1 calc R . .
C26A C 0.3060(7) 0.2522(9) 0.1921(3) 0.038(2) Uani 1 1 d . . .
O26A O 0.2702(6) 0.3231(7) 0.2032(3) 0.054(2) Uani 1 1 d . . .
C27A C 0.3490(7) 0.0464(9) 0.2295(3) 0.040(2) Uani 1 1 d . . .
O27A O 0.3406(6) 0.0074(7) 0.2607(2) 0.051(2) Uani 1 1 d . . .
C28A C 0.2386(7) 0.0689(9) 0.1564(3) 0.038(2) Uani 1 1 d . . .
O28A O 0.1694(5) 0.0420(6) 0.1491(3) 0.0475(19) Uani 1 1 d . . .
C29A C 0.3939(7) -0.0391(8) 0.1562(3) 0.034(2) Uani 1 1 d . . .
O29A O 0.4006(6) -0.1289(6) 0.1484(3) 0.052(2) Uani 1 1 d . . .
W1B W 0.10812(3) 0.61544(4) 0.170560(12) 0.02870(14) Uani 1 1 d . . .
N1B N -0.0568(6) 0.8603(7) 0.1310(3) 0.0355(18) Uani 1 1 d . . .
C2B C 0.0226(6) 0.8461(9) 0.1091(3) 0.037(2) Uani 1 1 d . . .
H2BA H 0.0709 0.8850 0.1250 0.044 Uiso 1 1 calc R . .
H2BB H 0.0128 0.8804 0.0814 0.044 Uiso 1 1 calc R . .
P3B P 0.05669(15) 0.7053(2) 0.10197(7) 0.0308(5) Uani 1 1 d . . .
C4B C -0.0396(8) 0.8454(8) 0.1759(3) 0.039(2) Uani 1 1 d . . .
H4BA H -0.0872 0.8794 0.1897 0.046 Uiso 1 1 calc R . .
H4BB H 0.0148 0.8840 0.1855 0.046 Uiso 1 1 calc R . .
P5B P -0.02892(16) 0.7022(2) 0.19359(7) 0.0306(5) Uani 1 1 d . . .
C6B C -0.0854(7) 0.9727(9) 0.1250(3) 0.039(2) Uani 1 1 d . A .
H6BA H -0.0365 1.0206 0.1349 0.046 Uiso 1 1 calc R . .
H6BB H -0.1332 0.9863 0.1427 0.046 Uiso 1 1 calc R . .
P7B P -0.12340(18) 1.0108(2) 0.07016(8) 0.0373(6) Uani 1 1 d D . .
C8B C -0.0396(7) 0.6493(9) 0.0695(3) 0.038(2) Uani 1 1 d . . .
H8BA H -0.0905 0.6672 0.0852 0.045 Uiso 1 1 calc R . .
C9B C -0.0421(9) 0.5314(11) 0.0649(4) 0.058(3) Uani 1 1 d . . .
H9BA H -0.0950 0.5106 0.0476 0.087 Uiso 1 1 calc R . .
H9BB H -0.0420 0.4979 0.0924 0.087 Uiso 1 1 calc R . .
H9BC H 0.0089 0.5073 0.0515 0.087 Uiso 1 1 calc R . .
C10B C -0.0587(10) 0.7053(11) 0.0266(4) 0.057(3) Uani 1 1 d . . .
H10D H -0.1098 0.6722 0.0114 0.086 Uiso 1 1 calc R . .
H10E H -0.0084 0.6971 0.0104 0.086 Uiso 1 1 calc R . .
H10F H -0.0697 0.7821 0.0308 0.086 Uiso 1 1 calc R . .
C11B C 0.1406(7) 0.7306(8) 0.0643(3) 0.038(2) Uani 1 1 d . . .
H11B H 0.1118 0.7749 0.0410 0.046 Uiso 1 1 calc R . .
C12B C 0.1710(8) 0.6299(10) 0.0453(4) 0.047(3) Uani 1 1 d . . .
H12D H 0.2143 0.6477 0.0260 0.071 Uiso 1 1 calc R . .
H12E H 0.1215 0.5934 0.0300 0.071 Uiso 1 1 calc R . .
H12F H 0.1971 0.5823 0.0673 0.071 Uiso 1 1 calc R . .
C13B C 0.2150(7) 0.7964(10) 0.0842(4) 0.047(3) Uani 1 1 d . . .
H13D H 0.2574 0.8086 0.0639 0.071 Uiso 1 1 calc R . .
H13E H 0.2429 0.7576 0.1083 0.071 Uiso 1 1 calc R . .
H13F H 0.1932 0.8658 0.0932 0.071 Uiso 1 1 calc R . .
C14B C -0.1414(7) 0.6549(11) 0.1747(4) 0.046(3) Uani 1 1 d . . .
H14B H -0.1508 0.6759 0.1446 0.055 Uiso 1 1 calc R . .
C15B C -0.1495(7) 0.5310(11) 0.1759(4) 0.051(3) Uani 1 1 d . . .
H15D H -0.2090 0.5100 0.1659 0.076 Uiso 1 1 calc R . .
H15E H -0.1360 0.5056 0.2045 0.076 Uiso 1 1 calc R . .
H15F H -0.1088 0.4988 0.1579 0.076 Uiso 1 1 calc R . .
C16B C -0.2146(7) 0.7095(13) 0.1963(4) 0.058(4) Uani 1 1 d . . .
H16D H -0.2709 0.6806 0.1849 0.087 Uiso 1 1 calc R . .
H16E H -0.2132 0.7874 0.1915 0.087 Uiso 1 1 calc R . .
H16F H -0.2063 0.6951 0.2264 0.087 Uiso 1 1 calc R . .
C17B C -0.0312(8) 0.7266(9) 0.2508(3) 0.040(2) Uani 1 1 d . . .
H17B H -0.0807 0.7764 0.2546 0.048 Uiso 1 1 calc R . .
C18B C -0.0469(9) 0.6223(11) 0.2744(4) 0.053(3) Uani 1 1 d . . .
H18D H -0.0484 0.6382 0.3041 0.079 Uiso 1 1 calc R . .
H18E H 0.0001 0.5711 0.2707 0.079 Uiso 1 1 calc R . .
H18F H -0.1025 0.5907 0.2634 0.079 Uiso 1 1 calc R . .
C19B C 0.0518(9) 0.7811(10) 0.2691(3) 0.049(3) Uani 1 1 d . . .
H19D H 0.0484 0.7938 0.2990 0.074 Uiso 1 1 calc R . .
H19E H 0.0587 0.8500 0.2550 0.074 Uiso 1 1 calc R . .
H19F H 0.1016 0.7346 0.2653 0.074 Uiso 1 1 calc R . .
C20B C -0.2408(7) 1.0187(10) 0.0730(4) 0.045(3) Uani 1 1 d . A .
H20B H -0.2522 1.0556 0.0995 0.054 Uiso 1 1 calc R . .
C21B C -0.2744(11) 0.9030(12) 0.0741(5) 0.074(5) Uani 1 1 d . . .
H21D H -0.3373 0.9038 0.0758 0.111 Uiso 1 1 calc R A .
H21E H -0.2459 0.8658 0.0985 0.111 Uiso 1 1 calc R . .
H21F H -0.2614 0.8652 0.0487 0.111 Uiso 1 1 calc R . .
C22B C -0.2870(7) 1.0807(10) 0.0363(4) 0.053(3) Uani 1 1 d . . .
H22D H -0.3495 1.0833 0.0394 0.080 Uiso 1 1 calc R A .
H22E H -0.2772 1.0444 0.0102 0.080 Uiso 1 1 calc R . .
H22F H -0.2640 1.1542 0.0360 0.080 Uiso 1 1 calc R . .
C23B C -0.0946(8) 1.1579(11) 0.0730(6) 0.036(4) Uani 0.80(4) 1 d PDU A 1
H23B H -0.1223 1.1919 0.0469 0.043 Uiso 0.80(4) 1 calc PR A 1
C24B C 0.0039(10) 1.168(2) 0.0715(7) 0.063(6) Uani 0.80(4) 1 d PDU A 1
H24D H 0.0208 1.2436 0.0734 0.094 Uiso 0.80(4) 1 calc PR A 1
H24E H 0.0202 1.1373 0.0452 0.094 Uiso 0.80(4) 1 calc PR A 1
H24F H 0.0337 1.1278 0.0949 0.094 Uiso 0.80(4) 1 calc PR A 1
C25B C -0.1227(13) 1.2248(12) 0.1096(6) 0.047(4) Uani 0.80(4) 1 d PDU A 1
H25D H -0.1031 1.2994 0.1070 0.070 Uiso 0.80(4) 1 calc PR A 1
H25E H -0.0966 1.1943 0.1359 0.070 Uiso 0.80(4) 1 calc PR A 1
H25F H -0.1861 1.2232 0.1092 0.070 Uiso 0.80(4) 1 calc PR A 1
C23" C -0.081(3) 1.147(3) 0.0582(18) 0.034(9) Uiso 0.20(4) 1 d PDU A 2
H23C H -0.1103 1.1776 0.0320 0.041 Uiso 0.20(4) 1 calc PR A 2
C24" C 0.016(3) 1.126(7) 0.055(2) 0.053(10) Uiso 0.20(4) 1 d PDU A 2
H24G H 0.0450 1.1947 0.0498 0.080 Uiso 0.20(4) 1 calc PR A 2
H24H H 0.0232 1.0763 0.0321 0.080 Uiso 0.20(4) 1 calc PR A 2
H24I H 0.0422 1.0953 0.0812 0.080 Uiso 0.20(4) 1 calc PR A 2
C25" C -0.094(4) 1.216(5) 0.096(2) 0.043(10) Uiso 0.20(4) 1 d PDU A 2
H25G H -0.0733 1.2890 0.0919 0.064 Uiso 0.20(4) 1 calc PR A 2
H25H H -0.0613 1.1846 0.1210 0.064 Uiso 0.20(4) 1 calc PR A 2
H25I H -0.1559 1.2178 0.1006 0.064 Uiso 0.20(4) 1 calc PR A 2
C26B C 0.1727(7) 0.7514(11) 0.1894(4) 0.045(3) Uani 1 1 d . . .
O26B O 0.2172(6) 0.8218(7) 0.2011(3) 0.052(2) Uani 1 1 d . . .
C27B C 0.1445(7) 0.5503(8) 0.2262(3) 0.036(2) Uani 1 1 d . . .
O27B O 0.1650(6) 0.5082(7) 0.2573(2) 0.051(2) Uani 1 1 d . . .
C28B C 0.2222(7) 0.5679(9) 0.1522(4) 0.042(2) Uani 1 1 d . . .
O28B O 0.2894(5) 0.5453(6) 0.1430(3) 0.0480(19) Uani 1 1 d . . .
C29B C 0.0671(6) 0.4658(9) 0.1558(3) 0.037(2) Uani 1 1 d . . .
O29B O 0.0546(5) 0.3735(6) 0.1484(3) 0.0480(19) 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
W1A C28A 1.994(11) . ?
W1A C27A 2.019(11) . ?
W1A C29A 2.041(10) . ?
W1A C26A 2.047(12) . ?
W1A P3A 2.529(2) . ?
W1A P5A 2.548(3) . ?
N1A C4A 1.468(12) . ?
N1A C2A 1.486(12) . ?
N1A C6A 1.486(12) . ?
C2A P3A 1.826(10) . ?
P3A C11A 1.863(10) . ?
P3A C8A 1.867(10) . ?
C4A P5A 1.869(11) . ?
P5A C14A 1.855(11) . ?
P5A C17A 1.857(11) . ?
C6A P7A 1.870(10) . ?
P7A C23A 1.856(12) . ?
P7A C20A 1.857(12) . ?
C8A C9A 1.517(17) . ?
C8A C10A 1.527(15) . ?
C11A C12A 1.530(15) . ?
C11A C13A 1.536(15) . ?
C14A C15A 1.524(18) . ?
C14A C16A 1.559(15) . ?
C17A C18A 1.516(16) . ?
C17A C19A 1.555(16) . ?
C20A C22A 1.528(17) . ?
C20A C21A 1.549(18) . ?
C23A C24A 1.476(17) . ?
C23A C25A 1.555(19) . ?
C26A O26A 1.116(13) . ?
C27A O27A 1.134(13) . ?
C28A O28A 1.124(13) . ?
C29A O29A 1.149(13) . ?
W1B C27B 1.999(10) . ?
W1B C28B 2.000(12) . ?
W1B C29B 2.006(12) . ?
W1B C26B 2.025(13) . ?
W1B P3B 2.536(2) . ?
W1B P5B 2.548(3) . ?
N1B C4B 1.460(13) . ?
N1B C6B 1.470(13) . ?
N1B C2B 1.482(13) . ?
C2B P3B 1.845(11) . ?
P3B C8B 1.871(11) . ?
P3B C11B 1.883(11) . ?
C4B P5B 1.868(10) . ?
P5B C17B 1.871(10) . ?
P5B C14B 1.882(11) . ?
C6B P7B 1.869(11) . ?
P7B C20B 1.827(12) . ?
P7B C23" 1.86(2) . ?
P7B C23B 1.880(13) . ?
C8B C9B 1.470(17) . ?
C8B C10B 1.551(15) . ?
C11B C12B 1.487(15) . ?
C11B C13B 1.504(17) . ?
C14B C16B 1.542(16) . ?
C14B C15B 1.544(19) . ?
C17B C19B 1.519(17) . ?
C17B C18B 1.532(16) . ?
C20B C21B 1.529(18) . ?
C20B C22B 1.529(16) . ?
C23B C24B 1.533(14) . ?
C23B C25B 1.536(15) . ?
C23" C25" 1.53(2) . ?
C23" C24" 1.53(2) . ?
C26B O26B 1.153(15) . ?
C27B O27B 1.147(13) . ?
C28B O28B 1.141(14) . ?
C29B O29B 1.182(13) . ?

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
C28A W1A C27A 88.0(4) . . ?
C28A W1A C29A 85.9(4) . . ?
C27A W1A C29A 84.8(4) . . ?
C28A W1A C26A 84.3(4) . . ?
C27A W1A C26A 90.0(4) . . ?
C29A W1A C26A 169.1(4) . . ?
C28A W1A P3A 94.7(3) . . ?
C27A W1A P3A 177.0(3) . . ?
C29A W1A P3A 96.8(3) . . ?
C26A W1A P3A 88.8(3) . . ?
C28A W1A P5A 171.8(3) . . ?
C27A W1A P5A 94.8(3) . . ?
C29A W1A P5A 101.9(3) . . ?
C26A W1A P5A 88.0(3) . . ?
P3A W1A P5A 82.36(8) . . ?
C4A N1A C2A 111.5(8) . . ?
C4A N1A C6A 106.1(8) . . ?
C2A N1A C6A 109.0(7) . . ?
N1A C2A P3A 116.4(7) . . ?
C2A P3A C11A 97.8(5) . . ?
C2A P3A C8A 100.4(5) . . ?
C11A P3A C8A 104.1(5) . . ?
C2A P3A W1A 112.1(3) . . ?
C11A P3A W1A 117.8(4) . . ?
C8A P3A W1A 121.0(4) . . ?
N1A C4A P5A 115.7(7) . . ?
C14A P5A C17A 104.9(5) . . ?
C14A P5A C4A 99.8(5) . . ?
C17A P5A C4A 97.7(5) . . ?
C14A P5A W1A 122.1(4) . . ?
C17A P5A W1A 116.8(4) . . ?
C4A P5A W1A 111.5(4) . . ?
N1A C6A P7A 114.1(7) . . ?
C23A P7A C20A 103.3(6) . . ?
C23A P7A C6A 99.4(5) . . ?
C20A P7A C6A 100.7(5) . . ?
C9A C8A C10A 111.2(9) . . ?
C9A C8A P3A 113.3(8) . . ?
C10A C8A P3A 114.9(7) . . ?
C12A C11A C13A 109.3(9) . . ?
C12A C11A P3A 111.5(8) . . ?
C13A C11A P3A 111.3(7) . . ?
C15A C14A C16A 111.3(9) . . ?
C15A C14A P5A 112.8(7) . . ?
C16A C14A P5A 114.9(9) . . ?
C18A C17A C19A 110.6(9) . . ?
C18A C17A P5A 113.0(8) . . ?
C19A C17A P5A 110.7(8) . . ?
C22A C20A C21A 111.3(12) . . ?
C22A C20A P7A 109.3(8) . . ?
C21A C20A P7A 107.6(9) . . ?
C24A C23A C25A 110.9(12) . . ?
C24A C23A P7A 111.6(9) . . ?
C25A C23A P7A 114.9(9) . . ?
O26A C26A W1A 174.1(10) . . ?
O27A C27A W1A 178.3(10) . . ?
O28A C28A W1A 176.3(10) . . ?
O29A C29A W1A 169.8(9) . . ?
C27B W1B C28B 88.0(5) . . ?
C27B W1B C29B 84.0(4) . . ?
C28B W1B C29B 85.7(4) . . ?
C27B W1B C26B 88.8(4) . . ?
C28B W1B C26B 84.9(5) . . ?
C29B W1B C26B 168.3(4) . . ?
C27B W1B P3B 176.8(3) . . ?
C28B W1B P3B 94.9(3) . . ?
C29B W1B P3B 97.7(3) . . ?
C26B W1B P3B 90.0(3) . . ?
C27B W1B P5B 94.7(3) . . ?
C28B W1B P5B 172.1(3) . . ?
C29B W1B P5B 102.0(3) . . ?
C26B W1B P5B 87.7(3) . . ?
P3B W1B P5B 82.33(8) . . ?
C4B N1B C6B 106.0(8) . . ?
C4B N1B C2B 112.0(8) . . ?
C6B N1B C2B 107.6(8) . . ?
N1B C2B P3B 115.6(7) . . ?
C2B P3B C8B 101.6(5) . . ?
C2B P3B C11B 98.3(5) . . ?
C8B P3B C11B 105.1(5) . . ?
C2B P3B W1B 112.2(3) . . ?
C8B P3B W1B 119.5(4) . . ?
C11B P3B W1B 117.1(3) . . ?
N1B C4B P5B 115.2(7) . . ?
C4B P5B C17B 97.9(5) . . ?
C4B P5B C14B 98.4(6) . . ?
C17B P5B C14B 105.5(5) . . ?
C4B P5B W1B 111.4(4) . . ?
C17B P5B W1B 116.6(4) . . ?
C14B P5B W1B 122.8(4) . . ?
N1B C6B P7B 115.4(7) . . ?
C20B P7B C23" 109.5(16) . . ?
C20B P7B C6B 101.1(5) . . ?
C23" P7B C6B 109.7(17) . . ?
C20B P7B C23B 100.2(6) . . ?
C6B P7B C23B 98.5(6) . . ?
C9B C8B C10B 110.8(10) . . ?
C9B C8B P3B 116.0(8) . . ?
C10B C8B P3B 114.0(8) . . ?
C12B C11B C13B 111.9(9) . . ?
C12B C11B P3B 112.9(8) . . ?
C13B C11B P3B 111.2(7) . . ?
C16B C14B C15B 111.2(11) . . ?
C16B C14B P5B 114.3(9) . . ?
C15B C14B P5B 112.2(8) . . ?
C19B C17B C18B 110.6(9) . . ?
C19B C17B P5B 111.2(8) . . ?
C18B C17B P5B 111.8(8) . . ?
C21B C20B C22B 110.9(10) . . ?
C21B C20B P7B 107.0(10) . . ?
C22B C20B P7B 112.6(9) . . ?
C24B C23B C25B 109.6(13) . . ?
C24B C23B P7B 107.8(11) . . ?
C25B C23B P7B 118.6(10) . . ?
C25" C23" C24" 111(2) . . ?
C25" C23" P7B 105(3) . . ?
C24" C23" P7B 103(4) . . ?
O26B C26B W1B 172.5(10) . . ?
O27B C27B W1B 176.7(9) . . ?
O28B C28B W1B 176.2(10) . . ?
O29B C29B W1B 170.8(9) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        72.37
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.294
_refine_diff_density_min         -1.957
_refine_diff_density_rms         0.230
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1412499'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H60 N O4 P3 W'
_chemical_formula_sum            'C37 H60 N O4 P3 W'
_chemical_formula_weight         859.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   21.077(2)
_cell_length_b                   20.1866(18)
_cell_length_c                   8.8990(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3786.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    2021
_cell_measurement_theta_min      3.0210
_cell_measurement_theta_max      73.3900

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    7.152
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) 
(compiled Aug  2 2013,16:46:58) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            8136
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0146
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.031
_diffrn_reflns_theta_max         73.489
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_point_group_measured_fraction_full 0.708
_reflns_number_total             5188
_reflns_number_gt                5108
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.330
_reflns_Friedel_fraction_max     0.362
_reflns_Friedel_fraction_full    0.391

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       CrysAlisPro,
_computing_cell_refinement       CrysAlisPro,
_computing_data_reduction        CrysAlisPro,
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+1.3435P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1251 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   -0.009(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5188
_refine_ls_number_parameters     437
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0464
_refine_ls_wR_factor_gt          0.0462
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.72727(2) 0.46454(2) 0.44844(3) 0.02273(6) Uani 1 1 d . . . . .
N1 N 0.80039(13) 0.39407(14) 0.0911(3) 0.0220(6) Uani 1 1 d . . . . .
C2 C 0.83558(17) 0.45615(16) 0.1081(4) 0.0231(7) Uani 1 1 d . . . . .
H2A H 0.8258 0.4850 0.0212 0.028 Uiso 1 1 calc R U . . .
H2B H 0.8815 0.4462 0.1051 0.028 Uiso 1 1 calc R U . . .
P3 P 0.81806(4) 0.50280(4) 0.28455(10) 0.02101(17) Uani 1 1 d . . . . .
C4 C 0.73368(16) 0.40675(18) 0.0546(5) 0.0240(7) Uani 1 1 d . . . . .
H4A H 0.7189 0.3737 -0.0198 0.029 Uiso 1 1 calc R U . . .
H4B H 0.7296 0.4513 0.0088 0.029 Uiso 1 1 calc R U . . .
P5 P 0.68327(4) 0.40215(4) 0.22522(10) 0.02184(17) Uani 1 1 d D . . . .
C6 C 0.83045(15) 0.35120(17) -0.0215(4) 0.0272(9) Uani 1 1 d . . . . .
H6A H 0.8382 0.3770 -0.1143 0.033 Uiso 1 1 calc R U . . .
H6B H 0.8014 0.3143 -0.0466 0.033 Uiso 1 1 calc R U . . .
P7 P 0.90713(4) 0.31691(4) 0.04881(12) 0.02639(19) Uani 1 1 d . . . . .
C8 C 0.81600(17) 0.58880(16) 0.2132(4) 0.0249(7) Uani 1 1 d . . . . .
H8A H 0.8558 0.5967 0.1548 0.030 Uiso 1 1 calc R U . . .
C9 C 0.7590(2) 0.60396(18) 0.1088(5) 0.0317(8) Uani 1 1 d . . . . .
H9A H 0.7711 0.5984 0.0021 0.038 Uiso 1 1 calc R U . . .
H9B H 0.7230 0.5740 0.1313 0.038 Uiso 1 1 calc R U . . .
C10 C 0.7409(2) 0.6768(2) 0.1417(6) 0.0420(10) Uani 1 1 d . . . . .
H10A H 0.7412 0.7032 0.0479 0.050 Uiso 1 1 calc R U . . .
H10B H 0.6980 0.6794 0.1870 0.050 Uiso 1 1 calc R U . . .
C11 C 0.7909(2) 0.70256(19) 0.2514(5) 0.0390(9) Uani 1 1 d . . . . .
H11A H 0.8269 0.7229 0.1969 0.047 Uiso 1 1 calc R U . . .
H11B H 0.7724 0.7358 0.3204 0.047 Uiso 1 1 calc R U . . .
C12 C 0.8123(2) 0.64112(18) 0.3376(5) 0.0301(8) Uani 1 1 d . . . . .
H12A H 0.7811 0.6285 0.4156 0.036 Uiso 1 1 calc R U . . .
H12B H 0.8542 0.6481 0.3853 0.036 Uiso 1 1 calc R U . . .
C13 C 0.89576(17) 0.50220(17) 0.3818(5) 0.0263(7) Uani 1 1 d . . . . .
H13A H 0.8901 0.5267 0.4785 0.032 Uiso 1 1 calc R U . . .
C14 C 0.95134(19) 0.53525(18) 0.2976(6) 0.0347(9) Uani 1 1 d . . . . .
H14A H 0.9490 0.5262 0.1884 0.042 Uiso 1 1 calc R U . . .
H14B H 0.9514 0.5838 0.3137 0.042 Uiso 1 1 calc R U . . .
C15 C 1.0098(2) 0.5034(2) 0.3666(6) 0.0443(11) Uani 1 1 d . . . . .
H15A H 1.0198 0.5232 0.4656 0.053 Uiso 1 1 calc R U . . .
H15B H 1.0471 0.5082 0.2998 0.053 Uiso 1 1 calc R U . . .
C16 C 0.9904(2) 0.4307(2) 0.3825(7) 0.0472(11) Uani 1 1 d . . . . .
H16A H 0.9976 0.4065 0.2871 0.057 Uiso 1 1 calc R U . . .
H16B H 1.0153 0.4089 0.4630 0.057 Uiso 1 1 calc R U . . .
C17 C 0.92001(18) 0.43157(17) 0.4222(5) 0.0343(10) Uani 1 1 d . . . . .
H17A H 0.9139 0.4225 0.5305 0.041 Uiso 1 1 calc R U . . .
H17B H 0.8968 0.3976 0.3636 0.041 Uiso 1 1 calc R U . . .
C18 C 0.68008(17) 0.31150(17) 0.2554(4) 0.0265(7) Uani 1 1 d . . . . .
H18A H 0.7249 0.2971 0.2727 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6426(2) 0.28970(18) 0.3953(5) 0.0339(8) Uani 1 1 d . . . . .
H19A H 0.6690 0.2934 0.4869 0.041 Uiso 1 1 calc R U . . .
H19B H 0.6041 0.3172 0.4083 0.041 Uiso 1 1 calc R U . . .
C20 C 0.6249(3) 0.2173(2) 0.3643(5) 0.0539(14) Uani 1 1 d . . . . .
H20A H 0.6525 0.1874 0.4232 0.065 Uiso 1 1 calc R U . . .
H20B H 0.5803 0.2091 0.3937 0.065 Uiso 1 1 calc R U . . .
C21 C 0.6333(4) 0.2050(2) 0.2024(6) 0.0635(16) Uani 1 1 d . . . . .
H21A H 0.5927 0.1900 0.1578 0.076 Uiso 1 1 calc R U . . .
H21B H 0.6654 0.1699 0.1868 0.076 Uiso 1 1 calc R U . . .
C22 C 0.6545(2) 0.2675(2) 0.1285(5) 0.0402(10) Uani 1 1 d . . . . .
H22A H 0.6185 0.2894 0.0769 0.048 Uiso 1 1 calc R U . . .
H22B H 0.6882 0.2583 0.0537 0.048 Uiso 1 1 calc R U . . .
C23 C 0.6068(3) 0.4251(5) 0.1348(13) 0.026(2) Uani 0.667(16) 1 d D U P A 1
H23A H 0.6001 0.3943 0.0481 0.031 Uiso 0.667(16) 1 calc R U P A 1
C24 C 0.5492(3) 0.4176(4) 0.2409(13) 0.0318(19) Uani 0.667(16) 1 d D U P A 1
H24A H 0.5342 0.3711 0.2444 0.038 Uiso 0.667(16) 1 calc R U P A 1
H24B H 0.5597 0.4324 0.3441 0.038 Uiso 0.667(16) 1 calc R U P A 1
C25 C 0.4991(3) 0.4631(4) 0.1688(11) 0.039(2) Uani 0.667(16) 1 d D U P A 1
H25A H 0.4785 0.4413 0.0819 0.047 Uiso 0.667(16) 1 calc R U P A 1
H25B H 0.4662 0.4760 0.2425 0.047 Uiso 0.667(16) 1 calc R U P A 1
C26 C 0.5377(3) 0.5224(4) 0.1197(13) 0.043(2) Uani 0.667(16) 1 d D U P A 1
H26A H 0.5418 0.5545 0.2033 0.052 Uiso 0.667(16) 1 calc R U P A 1
H26B H 0.5169 0.5449 0.0338 0.052 Uiso 0.667(16) 1 calc R U P A 1
C27 C 0.6028(3) 0.4965(5) 0.0739(12) 0.030(2) Uani 0.667(16) 1 d D U P A 1
H27A H 0.6367 0.5243 0.1179 0.036 Uiso 0.667(16) 1 calc R U P A 1
H27B H 0.6073 0.4968 -0.0368 0.036 Uiso 0.667(16) 1 calc R U P A 1
C23' C 0.6018(7) 0.4194(10) 0.159(2) 0.024(5) Uiso 0.333(16) 1 d D U P A 2
H23B H 0.5883 0.3814 0.0945 0.029 Uiso 0.333(16) 1 calc R U P A 2
C24' C 0.5511(9) 0.4293(8) 0.2788(18) 0.032(5) Uiso 0.333(16) 1 d D U P A 2
H24C H 0.5257 0.3884 0.2911 0.038 Uiso 0.333(16) 1 calc R U P A 2
H24D H 0.5709 0.4403 0.3765 0.038 Uiso 0.333(16) 1 calc R U P A 2
C25' C 0.5090(7) 0.4860(8) 0.2264(16) 0.039(4) Uiso 0.333(16) 1 d D U P A 2
H25C H 0.5160 0.5258 0.2893 0.047 Uiso 0.333(16) 1 calc R U P A 2
H25D H 0.4637 0.4734 0.2324 0.047 Uiso 0.333(16) 1 calc R U P A 2
C26' C 0.5281(7) 0.4996(9) 0.0641(15) 0.038(4) Uiso 0.333(16) 1 d D U P A 2
H26C H 0.5208 0.5465 0.0371 0.045 Uiso 0.333(16) 1 calc R U P A 2
H26D H 0.5042 0.4709 -0.0063 0.045 Uiso 0.333(16) 1 calc R U P A 2
C27' C 0.5995(8) 0.4827(11) 0.062(3) 0.036(6) Uiso 0.333(16) 1 d D U P A 2
H27C H 0.6251 0.5188 0.1071 0.043 Uiso 0.333(16) 1 calc R U P A 2
H27D H 0.6147 0.4741 -0.0414 0.043 Uiso 0.333(16) 1 calc R U P A 2
C28 C 0.8762(2) 0.26316(19) 0.2013(5) 0.0345(9) Uani 1 1 d . . . . .
H28A H 0.8487 0.2923 0.2647 0.041 Uiso 1 1 calc R U . . .
C29 C 0.9293(2) 0.2384(2) 0.3057(6) 0.0465(11) Uani 1 1 d . . . . .
H29A H 0.9670 0.2245 0.2472 0.056 Uiso 1 1 calc R U . . .
H29B H 0.9420 0.2732 0.3779 0.056 Uiso 1 1 calc R U . . .
C30 C 0.8994(3) 0.1792(3) 0.3871(6) 0.0571(13) Uani 1 1 d . . . . .
H30A H 0.9323 0.1477 0.4216 0.069 Uiso 1 1 calc R U . . .
H30B H 0.8741 0.1939 0.4747 0.069 Uiso 1 1 calc R U . . .
C31 C 0.8579(4) 0.1486(3) 0.2694(8) 0.082(2) Uani 1 1 d . . . . .
H31A H 0.8210 0.1268 0.3172 0.098 Uiso 1 1 calc R U . . .
H31B H 0.8820 0.1146 0.2130 0.098 Uiso 1 1 calc R U . . .
C32 C 0.8357(2) 0.2021(2) 0.1640(7) 0.0482(12) Uani 1 1 d . . . . .
H32A H 0.7901 0.2116 0.1800 0.058 Uiso 1 1 calc R U . . .
H32B H 0.8421 0.1885 0.0582 0.058 Uiso 1 1 calc R U . . .
C33 C 0.92504(17) 0.26077(18) -0.1094(5) 0.0310(8) Uani 1 1 d . . . . .
H33A H 0.8864 0.2340 -0.1334 0.037 Uiso 1 1 calc R U . . .
C34 C 0.9454(2) 0.3002(2) -0.2511(5) 0.0388(9) Uani 1 1 d . . . . .
H34A H 0.9132 0.2959 -0.3315 0.047 Uiso 1 1 calc R U . . .
H34B H 0.9507 0.3478 -0.2268 0.047 Uiso 1 1 calc R U . . .
C35 C 1.0086(3) 0.2701(3) -0.3009(7) 0.0601(14) Uani 1 1 d . . . . .
H35A H 1.0100 0.2657 -0.4117 0.072 Uiso 1 1 calc R U . . .
H35B H 1.0445 0.2982 -0.2680 0.072 Uiso 1 1 calc R U . . .
C36 C 1.0117(3) 0.2041(3) -0.2284(8) 0.0710(18) Uani 1 1 d . . . . .
H36A H 1.0563 0.1895 -0.2170 0.085 Uiso 1 1 calc R U . . .
H36B H 0.9884 0.1707 -0.2884 0.085 Uiso 1 1 calc R U . . .
C37 C 0.9808(2) 0.2136(2) -0.0765(6) 0.0442(12) Uani 1 1 d . . . . .
H37A H 1.0108 0.2336 -0.0040 0.053 Uiso 1 1 calc R U . . .
H37B H 0.9654 0.1709 -0.0356 0.053 Uiso 1 1 calc R U . . .
C38 C 0.76887(19) 0.5114(2) 0.6194(5) 0.0345(9) Uani 1 1 d . . . . .
O38 O 0.7931(2) 0.53764(17) 0.7192(4) 0.0556(10) Uani 1 1 d . . . . .
C39 C 0.77484(16) 0.38163(19) 0.5071(5) 0.0299(8) Uani 1 1 d . . . . .
O39 O 0.79895(15) 0.33360(14) 0.5485(4) 0.0453(8) Uani 1 1 d . . . . .
C40 C 0.6607(2) 0.4338(2) 0.5924(5) 0.0355(9) Uani 1 1 d . . . . .
O40 O 0.62467(18) 0.41759(18) 0.6821(4) 0.0555(9) Uani 1 1 d . . . . .
C41 C 0.67083(19) 0.54395(18) 0.4078(5) 0.0316(9) Uani 1 1 d . . . . .
O41 O 0.63629(16) 0.58741(15) 0.3929(4) 0.0496(8) 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
W1 C38 1.995(5) . ?
W1 C40 1.999(4) . ?
W1 C39 2.020(4) . ?
W1 C41 2.029(4) . ?
W1 P3 2.5269(9) . ?
W1 P5 2.5283(9) . ?
N1 C2 1.464(4) . ?
N1 C4 1.466(4) . ?
N1 C6 1.468(4) . ?
C2 P3 1.868(4) . ?
P3 C8 1.849(3) . ?
P3 C13 1.852(4) . ?
C4 P5 1.856(4) . ?
P5 C23' 1.847(14) . ?
P5 C18 1.851(4) . ?
P5 C23 1.860(7) . ?
C6 P7 1.866(3) . ?
P7 C33 1.846(4) . ?
P7 C28 1.856(4) . ?
C8 C12 1.532(5) . ?
C8 C9 1.550(5) . ?
C9 C10 1.547(5) . ?
C10 C11 1.528(7) . ?
C11 C12 1.527(5) . ?
C13 C14 1.542(5) . ?
C13 C17 1.557(5) . ?
C14 C15 1.520(6) . ?
C15 C16 1.530(6) . ?
C16 C17 1.526(6) . ?
C18 C22 1.535(5) . ?
C18 C19 1.539(6) . ?
C19 C20 1.533(6) . ?
C20 C21 1.473(7) . ?
C21 C22 1.491(6) . ?
C23 C27 1.543(10) . ?
C23 C24 1.546(10) . ?
C24 C25 1.539(8) . ?
C25 C26 1.512(9) . ?
C26 C27 1.524(8) . ?
C23' C24' 1.523(14) . ?
C23' C27' 1.545(14) . ?
C24' C25' 1.521(13) . ?
C25' C26' 1.524(13) . ?
C26' C27' 1.543(14) . ?
C28 C32 1.536(6) . ?
C28 C29 1.538(6) . ?
C29 C30 1.532(7) . ?
C30 C31 1.499(9) . ?
C31 C32 1.505(8) . ?
C33 C37 1.541(5) . ?
C33 C34 1.553(6) . ?
C34 C35 1.529(6) . ?
C35 C36 1.482(9) . ?
C36 C37 1.513(8) . ?
C38 O38 1.153(6) . ?
C39 O39 1.155(5) . ?
C40 O40 1.149(5) . ?
C41 O41 1.148(5) . ?

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
C38 W1 C40 88.08(18) . . ?
C38 W1 C39 88.71(17) . . ?
C40 W1 C39 85.75(16) . . ?
C38 W1 C41 91.11(17) . . ?
C40 W1 C41 87.00(17) . . ?
C39 W1 C41 172.75(16) . . ?
C38 W1 P3 87.86(12) . . ?
C40 W1 P3 175.15(13) . . ?
C39 W1 P3 91.52(11) . . ?
C41 W1 P3 95.71(12) . . ?
C38 W1 P5 175.42(12) . . ?
C40 W1 P5 95.26(13) . . ?
C39 W1 P5 88.41(12) . . ?
C41 W1 P5 92.19(11) . . ?
P3 W1 P5 88.66(3) . . ?
C2 N1 C4 111.1(3) . . ?
C2 N1 C6 110.9(3) . . ?
C4 N1 C6 111.4(3) . . ?
N1 C2 P3 114.7(2) . . ?
C8 P3 C13 100.80(16) . . ?
C8 P3 C2 100.91(17) . . ?
C13 P3 C2 102.40(17) . . ?
C8 P3 W1 117.87(12) . . ?
C13 P3 W1 113.44(13) . . ?
C2 P3 W1 118.74(11) . . ?
N1 C4 P5 111.0(3) . . ?
C23' P5 C18 101.4(7) . . ?
C23' P5 C4 105.2(6) . . ?
C18 P5 C4 100.89(17) . . ?
C18 P5 C23 106.1(3) . . ?
C4 P5 C23 97.5(4) . . ?
C23' P5 W1 119.8(7) . . ?
C18 P5 W1 113.08(13) . . ?
C4 P5 W1 114.08(12) . . ?
C23 P5 W1 122.3(3) . . ?
N1 C6 P7 111.3(2) . . ?
C33 P7 C28 105.69(18) . . ?
C33 P7 C6 98.59(17) . . ?
C28 P7 C6 99.08(18) . . ?
C12 C8 C9 104.9(3) . . ?
C12 C8 P3 113.6(3) . . ?
C9 C8 P3 114.2(2) . . ?
C10 C9 C8 105.4(3) . . ?
C11 C10 C9 105.9(3) . . ?
C12 C11 C10 104.4(3) . . ?
C11 C12 C8 102.3(3) . . ?
C14 C13 C17 105.0(3) . . ?
C14 C13 P3 116.2(3) . . ?
C17 C13 P3 113.8(2) . . ?
C15 C14 C13 103.7(3) . . ?
C14 C15 C16 103.1(3) . . ?
C17 C16 C15 105.6(3) . . ?
C16 C17 C13 106.1(3) . . ?
C22 C18 C19 104.4(3) . . ?
C22 C18 P5 118.6(3) . . ?
C19 C18 P5 114.7(2) . . ?
C20 C19 C18 104.6(3) . . ?
C21 C20 C19 107.9(4) . . ?
C20 C21 C22 109.0(4) . . ?
C21 C22 C18 105.7(4) . . ?
C27 C23 C24 105.2(5) . . ?
C27 C23 P5 115.6(7) . . ?
C24 C23 P5 113.1(7) . . ?
C25 C24 C23 103.0(5) . . ?
C26 C25 C24 103.0(5) . . ?
C25 C26 C27 106.8(5) . . ?
C26 C27 C23 106.1(5) . . ?
C24' C23' C27' 105.0(9) . . ?
C24' C23' P5 117.1(14) . . ?
C27' C23' P5 111.3(14) . . ?
C25' C24' C23' 107.1(8) . . ?
C24' C25' C26' 105.8(8) . . ?
C25' C26' C27' 103.2(9) . . ?
C26' C27' C23' 102.0(9) . . ?
C32 C28 C29 105.8(4) . . ?
C32 C28 P7 120.5(3) . . ?
C29 C28 P7 112.1(3) . . ?
C30 C29 C28 103.9(4) . . ?
C31 C30 C29 103.3(4) . . ?
C30 C31 C32 108.7(4) . . ?
C31 C32 C28 105.6(4) . . ?
C37 C33 C34 105.1(3) . . ?
C37 C33 P7 113.0(3) . . ?
C34 C33 P7 111.2(3) . . ?
C35 C34 C33 105.8(4) . . ?
C36 C35 C34 105.7(4) . . ?
C35 C36 C37 104.8(4) . . ?
C36 C37 C33 103.7(4) . . ?
O38 C38 W1 179.1(4) . . ?
O39 C39 W1 175.2(4) . . ?
O40 C40 W1 175.9(4) . . ?
O41 C41 W1 175.2(4) . . ?

_refine_diff_density_max         0.519
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.055

_shelxl_version_number           2013-4
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1412500'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H60 N O5 P3 W'
_chemical_formula_sum            'C37 H60 N O5 P3 W'
_chemical_formula_weight         875.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   20.9984(5)
_cell_length_b                   20.2089(4)
_cell_length_c                   8.90858(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3780.39(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173
_cell_measurement_reflns_used    3683
_cell_measurement_theta_min      3.0110
_cell_measurement_theta_max      73.4030

_exptl_crystal_description       'brown plates'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    7.195
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.220
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            7841
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         3.035
_diffrn_reflns_theta_max         73.826
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.572
_diffrn_reflns_point_group_measured_fraction_full 0.596
_reflns_number_total             4377
_reflns_number_gt                3938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.121
_reflns_Friedel_fraction_max     0.132
_reflns_Friedel_fraction_full    0.147

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0705P)²+3.7556P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.023(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4377
_refine_ls_number_parameters     425
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1200
_refine_ls_wR_factor_gt          0.1128
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.27215(2) 0.53732(2) 0.55104(8) 0.02835(13) Uani 1 1 d . . . . .
N1 N 0.1992(4) 0.6080(4) 0.9104(9) 0.0302(16) Uani 1 1 d . . . . .
C2 C 0.1618(5) 0.5462(5) 0.8892(12) 0.033(2) Uani 1 1 d . . . . .
H2A H 0.1159 0.5576 0.8891 0.039 Uiso 1 1 calc R U . . .
H2B H 0.1696 0.5167 0.9760 0.039 Uiso 1 1 calc R U . . .
P3 P 0.18025(11) 0.49979(10) 0.7133(3) 0.0273(4) Uani 1 1 d . . . . .
C4 C 0.2662(5) 0.5930(5) 0.9441(13) 0.037(2) Uani 1 1 d . . . . .
H4A H 0.2692 0.5478 0.9864 0.044 Uiso 1 1 calc R U . . .
H4B H 0.2821 0.6244 1.0207 0.044 Uiso 1 1 calc R U . . .
P5 P 0.31666(10) 0.59857(11) 0.7752(3) 0.0286(4) Uani 1 1 d . . . . .
C6 C 0.1695(4) 0.6488(4) 1.0282(13) 0.033(2) Uani 1 1 d . . . . .
H6A H 0.2006 0.6822 1.0635 0.040 Uiso 1 1 calc R U . . .
H6B H 0.1582 0.6203 1.1146 0.040 Uiso 1 1 calc R U . . .
P7 P 0.09731(12) 0.69130(12) 0.9599(3) 0.0350(5) Uani 1 1 d . . . . .
O7 O 0.0441(4) 0.6464(4) 0.9210(9) 0.0437(17) Uani 1 1 d . . . . .
C8 C 0.1824(5) 0.4140(4) 0.7879(11) 0.0333(19) Uani 1 1 d . . . . .
H8A H 0.1421 0.4066 0.8452 0.040 Uiso 1 1 calc R U . . .
C9 C 0.2375(5) 0.3986(5) 0.8922(13) 0.039(2) Uani 1 1 d . . . . .
H9A H 0.2243 0.4040 0.9981 0.047 Uiso 1 1 calc R U . . .
H9B H 0.2736 0.4289 0.8721 0.047 Uiso 1 1 calc R U . . .
C10 C 0.2571(7) 0.3265(6) 0.8616(16) 0.051(3) Uani 1 1 d . . . . .
H10A H 0.3001 0.3245 0.8161 0.061 Uiso 1 1 calc R U . . .
H10B H 0.2573 0.3005 0.9558 0.061 Uiso 1 1 calc R U . . .
C11 C 0.2068(7) 0.3000(5) 0.7525(15) 0.052(3) Uani 1 1 d . . . . .
H11A H 0.2252 0.2659 0.6856 0.062 Uiso 1 1 calc R U . . .
H11B H 0.1704 0.2806 0.8076 0.062 Uiso 1 1 calc R U . . .
C12 C 0.1861(6) 0.3607(4) 0.6629(12) 0.038(2) Uani 1 1 d . . . . .
H12A H 0.1441 0.3538 0.6146 0.046 Uiso 1 1 calc R U . . .
H12B H 0.2179 0.3726 0.5854 0.046 Uiso 1 1 calc R U . . .
C13 C 0.1032(4) 0.4997(5) 0.6183(11) 0.0308(18) Uani 1 1 d . . . . .
H13A H 0.1089 0.4730 0.5248 0.037 Uiso 1 1 calc R U . . .
C14 C 0.0469(5) 0.4693(5) 0.7015(14) 0.043(2) Uani 1 1 d . . . . .
H14A H 0.0483 0.4810 0.8093 0.051 Uiso 1 1 calc R U . . .
H14B H 0.0474 0.4205 0.6919 0.051 Uiso 1 1 calc R U . . .
C15 C -0.0124(5) 0.4982(6) 0.6274(16) 0.050(3) Uani 1 1 d . . . . .
H15A H -0.0495 0.4964 0.6958 0.060 Uiso 1 1 calc R U . . .
H15B H -0.0229 0.4746 0.5333 0.060 Uiso 1 1 calc R U . . .
C16 C 0.0078(5) 0.5707(6) 0.5957(16) 0.055(3) Uani 1 1 d . . . . .
H16A H -0.0149 0.5882 0.5068 0.066 Uiso 1 1 calc R U . . .
H16B H -0.0020 0.5992 0.6830 0.066 Uiso 1 1 calc R U . . .
C17 C 0.0792(5) 0.5688(5) 0.5672(15) 0.045(3) Uani 1 1 d . . . . .
H17A H 0.1008 0.6041 0.6249 0.054 Uiso 1 1 calc R U . . .
H17B H 0.0882 0.5755 0.4592 0.054 Uiso 1 1 calc R U . . .
C18 C 0.3218(4) 0.6895(4) 0.7472(11) 0.0319(19) Uani 1 1 d . . . . .
H18A H 0.2771 0.7047 0.7299 0.038 Uiso 1 1 calc R U . . .
C19 C 0.3593(6) 0.7111(4) 0.6080(13) 0.042(2) Uani 1 1 d . . . . .
H19A H 0.3323 0.7089 0.5169 0.050 Uiso 1 1 calc R U . . .
H19B H 0.3972 0.6827 0.5932 0.050 Uiso 1 1 calc R U . . .
C20 C 0.3792(8) 0.7835(6) 0.6415(15) 0.063(4) Uani 1 1 d . . . . .
H20A H 0.4246 0.7903 0.6163 0.076 Uiso 1 1 calc R U . . .
H20B H 0.3533 0.8146 0.5813 0.076 Uiso 1 1 calc R U . . .
C21 C 0.3685(8) 0.7947(6) 0.8019(19) 0.065(4) Uani 1 1 d . . . . .
H21A H 0.3357 0.8293 0.8155 0.078 Uiso 1 1 calc R U . . .
H21B H 0.4084 0.8105 0.8491 0.078 Uiso 1 1 calc R U . . .
C22 C 0.3475(7) 0.7326(6) 0.8760(14) 0.050(3) Uani 1 1 d . . . . .
H22A H 0.3137 0.7416 0.9508 0.060 Uiso 1 1 calc R U . . .
H22B H 0.3836 0.7105 0.9269 0.060 Uiso 1 1 calc R U . . .
C23 C 0.3942(5) 0.5767(5) 0.8561(14) 0.038(2) Uani 1 1 d . . . . .
H23A H 0.4037 0.6098 0.9366 0.046 Uiso 1 1 calc R U . . .
C24 C 0.4494(5) 0.5775(7) 0.7478(18) 0.059(4) Uani 1 1 d . . . . .
H24A H 0.4679 0.6224 0.7396 0.070 Uiso 1 1 calc R U . . .
H24B H 0.4360 0.5625 0.6468 0.070 Uiso 1 1 calc R U . . .
C25 C 0.4974(7) 0.5290(10) 0.817(3) 0.090(7) Uani 1 1 d . . . . .
H25A H 0.5227 0.5073 0.7375 0.108 Uiso 1 1 calc R U . . .
H25B H 0.5270 0.5529 0.8847 0.108 Uiso 1 1 calc R U . . .
C26 C 0.4640(7) 0.4830(10) 0.896(3) 0.101(8) Uani 1 1 d . . . . .
H26A H 0.4865 0.4735 0.9915 0.121 Uiso 1 1 calc R U . . .
H26B H 0.4621 0.4414 0.8377 0.121 Uiso 1 1 calc R U . . .
C27 C 0.3971(6) 0.5057(6) 0.9308(15) 0.051(3) Uani 1 1 d . . . . .
H27A H 0.3898 0.5083 1.0404 0.061 Uiso 1 1 calc R U . . .
H27B H 0.3651 0.4756 0.8858 0.061 Uiso 1 1 calc R U . . .
C28 C 0.1261(5) 0.7392(5) 0.8022(15) 0.046(2) Uani 1 1 d . . . . .
H28A H 0.1522 0.7081 0.7403 0.055 Uiso 1 1 calc R U . . .
C29 C 0.0711(6) 0.7637(7) 0.6973(16) 0.056(3) Uani 1 1 d . . . . .
H29A H 0.0582 0.7286 0.6259 0.067 Uiso 1 1 calc R U . . .
H29B H 0.0335 0.7775 0.7565 0.067 Uiso 1 1 calc R U . . .
C30 C 0.1007(8) 0.8226(7) 0.6151(19) 0.069(4) Uani 1 1 d . . . . .
H30A H 0.1262 0.8076 0.5279 0.083 Uiso 1 1 calc R U . . .
H30B H 0.0675 0.8536 0.5798 0.083 Uiso 1 1 calc R U . . .
C31 C 0.1422(11) 0.8542(8) 0.731(2) 0.087(6) Uani 1 1 d . . . . .
H31A H 0.1172 0.8859 0.7920 0.104 Uiso 1 1 calc R U . . .
H31B H 0.1776 0.8784 0.6826 0.104 Uiso 1 1 calc R U . . .
C32 C 0.1681(6) 0.7994(6) 0.8301(19) 0.058(3) Uani 1 1 d . . . . .
H32A H 0.1663 0.8125 0.9370 0.069 Uiso 1 1 calc R U . . .
H32B H 0.2129 0.7895 0.8035 0.069 Uiso 1 1 calc R U . . .
C33 C 0.0772(5) 0.7455(5) 1.1150(14) 0.043(2) Uani 1 1 d . . . . .
H33A H 0.1149 0.7733 1.1415 0.051 Uiso 1 1 calc R U . . .
C34 C 0.0561(6) 0.7051(7) 1.2535(15) 0.055(3) Uani 1 1 d . . . . .
H34A H 0.0522 0.6576 1.2281 0.066 Uiso 1 1 calc R U . . .
H34B H 0.0872 0.7100 1.3364 0.066 Uiso 1 1 calc R U . . .
C35 C -0.0086(8) 0.7340(10) 1.298(2) 0.086(6) Uani 1 1 d . . . . .
H35A H -0.0434 0.7050 1.2616 0.104 Uiso 1 1 calc R U . . .
H35B H -0.0119 0.7380 1.4080 0.104 Uiso 1 1 calc R U . . .
C36 C -0.0129(10) 0.7979(11) 1.229(2) 0.099(7) Uani 1 1 d . . . . .
H36A H 0.0087 0.8317 1.2908 0.119 Uiso 1 1 calc R U . . .
H36B H -0.0580 0.8109 1.2147 0.119 Uiso 1 1 calc R U . . .
C37 C 0.0194(6) 0.7906(6) 1.0817(16) 0.055(4) Uani 1 1 d . . . . .
H37A H 0.0335 0.8341 1.0430 0.066 Uiso 1 1 calc R U . . .
H37B H -0.0093 0.7699 1.0071 0.066 Uiso 1 1 calc R U . . .
C38 C 0.2297(5) 0.4904(6) 0.3791(15) 0.043(3) Uani 1 1 d . . . . .
O38 O 0.2059(6) 0.4649(5) 0.2803(11) 0.069(3) Uani 1 1 d . . . . .
C39 C 0.2248(4) 0.6229(5) 0.4935(13) 0.035(2) Uani 1 1 d . . . . .
O39 O 0.2021(4) 0.6695(4) 0.4539(12) 0.056(2) Uani 1 1 d . . . . .
C40 C 0.3391(6) 0.5671(5) 0.4106(16) 0.049(3) Uani 1 1 d . . . . .
O40 O 0.3757(5) 0.5838(5) 0.3179(12) 0.065(3) Uani 1 1 d . . . . .
C41 C 0.3294(5) 0.4573(5) 0.5932(14) 0.044(3) Uani 1 1 d . . . . .
O41 O 0.3622(4) 0.4135(4) 0.6068(12) 0.057(2) 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
W1 C40 1.976(14) . ?
W1 C38 2.010(14) . ?
W1 C41 2.050(11) . ?
W1 C39 2.061(10) . ?
W1 P3 2.527(2) . ?
W1 P5 2.528(2) . ?
N1 C4 1.470(13) . ?
N1 C6 1.473(12) . ?
N1 C2 1.488(11) . ?
C2 P3 1.867(10) . ?
P3 C13 1.825(10) . ?
P3 C8 1.857(9) . ?
C4 P5 1.844(11) . ?
P5 C23 1.834(10) . ?
P5 C18 1.858(9) . ?
C6 P7 1.845(9) . ?
P7 O7 1.480(8) . ?
P7 C28 1.811(13) . ?
P7 C33 1.813(11) . ?
C8 C9 1.516(14) . ?
C8 C12 1.551(13) . ?
C9 C10 1.539(15) . ?
C10 C11 1.532(19) . ?
C11 C12 1.527(15) . ?
C13 C14 1.524(13) . ?
C13 C17 1.552(14) . ?
C14 C15 1.526(16) . ?
C15 C16 1.550(18) . ?
C16 C17 1.521(16) . ?
C18 C19 1.532(15) . ?
C18 C22 1.538(15) . ?
C19 C20 1.549(15) . ?
C20 C21 1.46(2) . ?
C21 C22 1.486(17) . ?
C23 C24 1.509(17) . ?
C23 C27 1.582(16) . ?
C24 C25 1.536(19) . ?
C25 C26 1.36(2) . ?
C26 C27 1.510(17) . ?
C28 C32 1.522(17) . ?
C28 C29 1.566(18) . ?
C29 C30 1.529(19) . ?
C30 C31 1.50(3) . ?
C31 C32 1.52(2) . ?
C33 C34 1.544(18) . ?
C33 C37 1.546(15) . ?
C34 C35 1.531(18) . ?
C35 C36 1.43(3) . ?
C36 C37 1.48(2) . ?
C38 O38 1.136(17) . ?
C39 O39 1.113(13) . ?
C40 O40 1.178(16) . ?
C41 O41 1.128(13) . ?

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
C40 W1 C38 88.7(5) . . ?
C40 W1 C41 86.5(5) . . ?
C38 W1 C41 91.6(5) . . ?
C40 W1 C39 86.0(4) . . ?
C38 W1 C39 89.5(4) . . ?
C41 W1 C39 172.4(4) . . ?
C40 W1 P3 175.4(4) . . ?
C38 W1 P3 87.5(3) . . ?
C41 W1 P3 96.1(3) . . ?
C39 W1 P3 91.5(3) . . ?
C40 W1 P5 95.0(3) . . ?
C38 W1 P5 175.4(3) . . ?
C41 W1 P5 91.4(3) . . ?
C39 W1 P5 87.9(3) . . ?
P3 W1 P5 88.71(7) . . ?
C4 N1 C6 112.0(8) . . ?
C4 N1 C2 111.0(7) . . ?
C6 N1 C2 109.7(7) . . ?
N1 C2 P3 114.8(7) . . ?
C13 P3 C8 100.7(4) . . ?
C13 P3 C2 101.9(5) . . ?
C8 P3 C2 100.0(5) . . ?
C13 P3 W1 114.3(3) . . ?
C8 P3 W1 117.8(3) . . ?
C2 P3 W1 119.2(3) . . ?
N1 C4 P5 111.8(7) . . ?
C23 P5 C4 100.0(5) . . ?
C23 P5 C18 103.9(5) . . ?
C4 P5 C18 101.7(5) . . ?
C23 P5 W1 121.4(4) . . ?
C4 P5 W1 113.7(3) . . ?
C18 P5 W1 113.5(3) . . ?
N1 C6 P7 111.9(7) . . ?
O7 P7 C28 113.5(5) . . ?
O7 P7 C33 111.9(5) . . ?
C28 P7 C33 110.3(6) . . ?
O7 P7 C6 114.4(4) . . ?
C28 P7 C6 103.3(5) . . ?
C33 P7 C6 102.8(5) . . ?
C9 C8 C12 105.0(8) . . ?
C9 C8 P3 115.4(7) . . ?
C12 C8 P3 113.1(7) . . ?
C8 C9 C10 106.9(9) . . ?
C11 C10 C9 105.0(9) . . ?
C12 C11 C10 104.3(9) . . ?
C11 C12 C8 101.4(8) . . ?
C14 C13 C17 104.6(8) . . ?
C14 C13 P3 117.5(7) . . ?
C17 C13 P3 115.0(7) . . ?
C13 C14 C15 105.6(9) . . ?
C14 C15 C16 102.5(9) . . ?
C17 C16 C15 106.0(9) . . ?
C16 C17 C13 107.1(9) . . ?
C19 C18 C22 105.2(8) . . ?
C19 C18 P5 114.9(6) . . ?
C22 C18 P5 118.7(8) . . ?
C18 C19 C20 104.5(9) . . ?
C21 C20 C19 107.1(11) . . ?
C20 C21 C22 110.3(11) . . ?
C21 C22 C18 104.5(11) . . ?
C24 C23 C27 104.4(9) . . ?
C24 C23 P5 115.3(9) . . ?
C27 C23 P5 114.7(7) . . ?
C23 C24 C25 103.8(12) . . ?
C26 C25 C24 107.8(12) . . ?
C25 C26 C27 112.2(12) . . ?
C26 C27 C23 103.1(10) . . ?
C32 C28 C29 105.8(10) . . ?
C32 C28 P7 119.6(10) . . ?
C29 C28 P7 112.7(8) . . ?
C30 C29 C28 103.4(11) . . ?
C31 C30 C29 103.8(13) . . ?
C30 C31 C32 107.3(12) . . ?
C31 C32 C28 106.3(13) . . ?
C34 C33 C37 103.9(10) . . ?
C34 C33 P7 110.9(8) . . ?
C37 C33 P7 113.2(8) . . ?
C35 C34 C33 104.9(11) . . ?
C36 C35 C34 106.8(13) . . ?
C35 C36 C37 105.1(13) . . ?
C36 C37 C33 104.4(12) . . ?
O38 C38 W1 178.7(11) . . ?
O39 C39 W1 175.0(10) . . ?
O40 C40 W1 174.7(11) . . ?
O41 C41 W1 175.5(11) . . ?

_refine_diff_density_max         2.277
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.138

_shelxl_version_number           2013-4
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1412501'
_audit_update_record             
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H52 N2 O4 P2 W, 0.5(C7 H8)'
_chemical_formula_sum            'C38.50 H56 N2 O4 P2 W'
_chemical_formula_weight         856.64

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   P2(1)/c

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                   37.9478(5)
_cell_length_b                   10.57997(15)
_cell_length_c                   19.1922(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3336(14)
_cell_angle_gamma                90.00
_cell_volume                     7580.43(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    173
_cell_measurement_reflns_used    24342
_cell_measurement_theta_min      2.9045
_cell_measurement_theta_max      32.7112

_exptl_crystal_description       blocks
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3496
_exptl_absorpt_coefficient_mu    3.173
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 15.9825
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81655
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         32.79
_reflns_number_total             25641
_reflns_number_gt                15781
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0000P)²+18.3223P] 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         25641
_refine_ls_number_parameters     867
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0817
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.0978
_refine_ls_goodness_of_fit_ref   1.511
_refine_ls_restrained_S_all      1.508
_refine_ls_shift/su_max          0.005
_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
W1A W 0.385384(7) 0.59623(2) 0.481225(16) 0.01444(5) Uani 1 1 d . A .
N1A N 0.35017(13) 0.3241(5) 0.3411(3) 0.0164(10) Uani 1 1 d D . .
C2A C 0.32445(15) 0.3664(6) 0.3836(3) 0.0159(12) Uani 1 1 d . A .
H2AA H 0.3064 0.2990 0.3838 0.019 Uiso 1 1 calc R . .
H2AB H 0.3119 0.4416 0.3607 0.019 Uiso 1 1 calc R . .
P3A P 0.34371(4) 0.40724(14) 0.47724(9) 0.0122(3) Uani 1 1 d . . .
C4A C 0.37178(16) 0.4219(5) 0.3142(3) 0.0159(12) Uani 1 1 d . A .
H4AA H 0.3561 0.4942 0.2966 0.019 Uiso 1 1 calc R . .
H4AB H 0.3816 0.3872 0.2738 0.019 Uiso 1 1 calc R . .
P5A P 0.40942(4) 0.47930(13) 0.38277(8) 0.0111(3) Uani 1 1 d . . .
C6A C 0.3473(3) 0.2043(6) 0.3126(7) 0.018(2) Uani 0.68(4) 1 d PGDU A 1
N7A N 0.3734(2) 0.1778(10) 0.2723(6) 0.022(2) Uani 0.68(4) 1 d PGU A 1
C8A C 0.3758(3) 0.0574(12) 0.2445(5) 0.028(2) Uani 0.68(4) 1 d PGU A 1
H8AA H 0.3936 0.0393 0.2170 0.034 Uiso 0.68(4) 1 calc PR A 1
C9A C 0.3521(4) -0.0366(6) 0.2572(5) 0.022(2) Uani 0.68(4) 1 d PGU A 1
H9AA H 0.3537 -0.1189 0.2382 0.027 Uiso 0.68(4) 1 calc PR A 1
C10A C 0.3260(4) -0.0101(8) 0.2975(6) 0.030(2) Uani 0.68(4) 1 d PGU A 1
H10A H 0.3098 -0.0743 0.3061 0.037 Uiso 0.68(4) 1 calc PR A 1
C11A C 0.3236(3) 0.1103(11) 0.3252(7) 0.027(2) Uani 0.68(4) 1 d PGU A 1
H11A H 0.3058 0.1284 0.3528 0.033 Uiso 0.68(4) 1 calc PR A 1
C6' C 0.3517(7) 0.2028(14) 0.3101(15) 0.011(3) Uiso 0.32(4) 1 d PGDU A 2
N7' N 0.3229(6) 0.132(2) 0.3239(14) 0.026(4) Uiso 0.32(4) 1 d PGU A 2
C8' C 0.3179(6) 0.009(2) 0.2981(13) 0.030(4) Uiso 0.32(4) 1 d PGU A 2
H8'A H 0.2982 -0.0396 0.3075 0.036 Uiso 0.32(4) 1 calc PR A 2
C9' C 0.3416(7) -0.0426(13) 0.2586(12) 0.024(4) Uiso 0.32(4) 1 d PGU A 2
H9'A H 0.3382 -0.1265 0.2410 0.029 Uiso 0.32(4) 1 calc PR A 2
C10' C 0.3704(6) 0.029(2) 0.2448(12) 0.028(4) Uiso 0.32(4) 1 d PGU A 2
H10C H 0.3866 -0.0068 0.2178 0.033 Uiso 0.32(4) 1 calc PR A 2
C11' C 0.3754(6) 0.151(2) 0.2706(14) 0.020(4) Uiso 0.32(4) 1 d PGU A 2
H11C H 0.3951 0.1998 0.2611 0.024 Uiso 0.32(4) 1 calc PR A 2
C12A C 0.36239(14) 0.2488(5) 0.5121(4) 0.0144(12) Uani 1 1 d . A .
H12A H 0.3782 0.2186 0.4791 0.017 Uiso 1 1 calc R . .
C13A C 0.38616(17) 0.2603(6) 0.5856(4) 0.0214(14) Uani 1 1 d . . .
H13A H 0.3713 0.2835 0.6211 0.026 Uiso 1 1 calc R A .
H13B H 0.4042 0.3277 0.5849 0.026 Uiso 1 1 calc R . .
C14A C 0.40523(18) 0.1337(6) 0.6065(4) 0.0255(16) Uani 1 1 d . A .
H14A H 0.4218 0.1146 0.5734 0.031 Uiso 1 1 calc R . .
H14B H 0.4195 0.1404 0.6548 0.031 Uiso 1 1 calc R . .
C15A C 0.3780(2) 0.0261(6) 0.6042(4) 0.0279(16) Uani 1 1 d U . .
H15A H 0.3634 0.0399 0.6415 0.033 Uiso 1 1 calc R A .
H15B H 0.3909 -0.0551 0.6142 0.033 Uiso 1 1 calc R . .
C16A C 0.35326(18) 0.0186(6) 0.5318(4) 0.0257(15) Uani 1 1 d . A .
H16A H 0.3353 -0.0489 0.5328 0.031 Uiso 1 1 calc R . .
H16B H 0.3675 -0.0034 0.4951 0.031 Uiso 1 1 calc R . .
C17A C 0.33376(16) 0.1475(5) 0.5127(4) 0.0171(12) Uani 1 1 d . . .
H17A H 0.3181 0.1421 0.4656 0.020 Uiso 1 1 calc R A .
H17B H 0.3187 0.1688 0.5482 0.020 Uiso 1 1 calc R . .
C18A C 0.30005(15) 0.4281(5) 0.5079(4) 0.0157(12) Uani 1 1 d . A .
H18A H 0.2846 0.3541 0.4900 0.019 Uiso 1 1 calc R . .
C19A C 0.30285(17) 0.4317(6) 0.5882(4) 0.0199(13) Uani 1 1 d . . .
H19A H 0.3181 0.5039 0.6078 0.024 Uiso 1 1 calc R A .
H19B H 0.3144 0.3531 0.6091 0.024 Uiso 1 1 calc R . .
C20A C 0.26579(18) 0.4450(8) 0.6087(5) 0.0329(18) Uani 1 1 d . A .
H20A H 0.2513 0.3691 0.5928 0.040 Uiso 1 1 calc R . .
H20B H 0.2685 0.4501 0.6609 0.040 Uiso 1 1 calc R . .
C21A C 0.2463(2) 0.5621(8) 0.5758(4) 0.038(2) Uani 1 1 d . . .
H21A H 0.2220 0.5649 0.5875 0.046 Uiso 1 1 calc R A .
H21B H 0.2594 0.6387 0.5957 0.046 Uiso 1 1 calc R . .
C22A C 0.24363(17) 0.5612(7) 0.4960(4) 0.0296(17) Uani 1 1 d . A .
H22A H 0.2322 0.6406 0.4761 0.036 Uiso 1 1 calc R . .
H22B H 0.2283 0.4899 0.4757 0.036 Uiso 1 1 calc R . .
C23A C 0.28057(17) 0.5485(6) 0.4751(4) 0.0226(14) Uani 1 1 d . . .
H23A H 0.2952 0.6238 0.4915 0.027 Uiso 1 1 calc R A .
H23B H 0.2778 0.5444 0.4229 0.027 Uiso 1 1 calc R . .
C24A C 0.43500(16) 0.5764(6) 0.3273(3) 0.0161(12) Uani 1 1 d . A .
H24A H 0.4414 0.5187 0.2902 0.019 Uiso 1 1 calc R . .
C25A C 0.41345(18) 0.6855(6) 0.2882(4) 0.0210(14) Uani 1 1 d . . .
H25A H 0.3916 0.6521 0.2577 0.025 Uiso 1 1 calc R A .
H25B H 0.4059 0.7443 0.3229 0.025 Uiso 1 1 calc R . .
C26A C 0.4361(2) 0.7558(7) 0.2432(4) 0.0301(17) Uani 1 1 d . A .
H26A H 0.4417 0.6985 0.2058 0.036 Uiso 1 1 calc R . .
H26B H 0.4223 0.8281 0.2197 0.036 Uiso 1 1 calc R . .
C27A C 0.4706(2) 0.8037(7) 0.2870(5) 0.0344(18) Uani 1 1 d . . .
H27A H 0.4651 0.8671 0.3214 0.041 Uiso 1 1 calc R A .
H27B H 0.4851 0.8458 0.2555 0.041 Uiso 1 1 calc R . .
C28A C 0.49234(18) 0.6961(7) 0.3267(4) 0.0274(16) Uani 1 1 d . A .
H28A H 0.5138 0.7313 0.3575 0.033 Uiso 1 1 calc R . .
H28B H 0.5005 0.6386 0.2921 0.033 Uiso 1 1 calc R . .
C29A C 0.47037(16) 0.6213(6) 0.3719(4) 0.0183(13) Uani 1 1 d . . .
H29A H 0.4653 0.6753 0.4111 0.022 Uiso 1 1 calc R A .
H29B H 0.4843 0.5473 0.3929 0.022 Uiso 1 1 calc R . .
C30A C 0.43575(15) 0.3286(5) 0.3986(3) 0.0123(11) Uani 1 1 d . A .
H30A H 0.4173 0.2612 0.3990 0.015 Uiso 1 1 calc R . .
C31A C 0.45556(17) 0.2906(6) 0.3382(4) 0.0199(13) Uani 1 1 d . . .
H31A H 0.4391 0.2968 0.2921 0.024 Uiso 1 1 calc R A .
H31B H 0.4759 0.3487 0.3373 0.024 Uiso 1 1 calc R . .
C32A C 0.4694(2) 0.1537(6) 0.3499(4) 0.0299(17) Uani 1 1 d . A .
H32A H 0.4490 0.0954 0.3489 0.036 Uiso 1 1 calc R . .
H32B H 0.4822 0.1293 0.3113 0.036 Uiso 1 1 calc R . .
C33A C 0.49458(19) 0.1423(7) 0.4204(4) 0.0280(16) Uani 1 1 d . . .
H33A H 0.5160 0.1955 0.4200 0.034 Uiso 1 1 calc R A .
H33B H 0.5026 0.0535 0.4280 0.034 Uiso 1 1 calc R . .
C34A C 0.47613(18) 0.1838(6) 0.4807(4) 0.0213(14) Uani 1 1 d . A .
H34A H 0.4936 0.1808 0.5257 0.026 Uiso 1 1 calc R . .
H34B H 0.4566 0.1236 0.4847 0.026 Uiso 1 1 calc R . .
C35A C 0.46042(16) 0.3177(5) 0.4705(3) 0.0176(12) Uani 1 1 d . . .
H35A H 0.4468 0.3367 0.5087 0.021 Uiso 1 1 calc R A .
H35B H 0.4801 0.3800 0.4735 0.021 Uiso 1 1 calc R . .
C36A C 0.34710(16) 0.6747(6) 0.4064(4) 0.0197(13) Uani 1 1 d . . .
O36A O 0.32659(15) 0.7251(5) 0.3651(3) 0.0384(15) Uani 1 1 d . A .
C37A C 0.41279(17) 0.7583(5) 0.4728(4) 0.0182(12) Uani 1 1 d U . .
O37A O 0.42526(14) 0.8546(4) 0.4672(3) 0.0320(13) Uani 1 1 d U A .
C38A C 0.36353(15) 0.6780(6) 0.5579(3) 0.0150(11) Uani 1 1 d . . .
O38A O 0.35187(16) 0.7235(4) 0.6013(3) 0.0324(13) Uani 1 1 d . A .
C39A C 0.42700(16) 0.5498(6) 0.5596(4) 0.0182(13) Uani 1 1 d . . .
O39A O 0.44965(13) 0.5383(5) 0.6080(3) 0.0312(13) Uani 1 1 d . A .
W1B W 0.113865(9) 0.59634(3) 0.019432(19) 0.02583(7) Uani 1 1 d . B .
N1B N 0.14823(18) 0.3223(6) 0.1611(3) 0.0292(14) Uani 1 1 d D . .
C2B C 0.17390(19) 0.3638(7) 0.1188(4) 0.0289(16) Uani 1 1 d . B .
H2BA H 0.1918 0.2958 0.1185 0.035 Uiso 1 1 calc R . .
H2BB H 0.1867 0.4383 0.1420 0.035 Uiso 1 1 calc R . .
P3B P 0.15486(5) 0.40664(18) 0.02444(11) 0.0239(4) Uani 1 1 d . . .
C4B C 0.1277(2) 0.4226(7) 0.1862(4) 0.0328(18) Uani 1 1 d . B .
H4BA H 0.1438 0.4945 0.2020 0.039 Uiso 1 1 calc R . .
H4BB H 0.1181 0.3917 0.2278 0.039 Uiso 1 1 calc R . .
P5B P 0.08951(5) 0.47998(19) 0.11763(11) 0.0292(4) Uani 1 1 d . . .
C6B C 0.1525(3) 0.2050(7) 0.1899(6) 0.031(3) Uani 0.63(3) 1 d PGDU B 1
N7B N 0.1243(3) 0.1770(9) 0.2244(7) 0.040(3) Uani 0.63(3) 1 d PGU B 1
C8B C 0.1212(3) 0.0567(11) 0.2518(7) 0.032(3) Uani 0.63(3) 1 d PGU B 1
H8BA H 0.1019 0.0375 0.2754 0.039 Uiso 0.63(3) 1 calc PR B 1
C9B C 0.1464(4) -0.0356(7) 0.2447(6) 0.038(3) Uani 0.63(3) 1 d PGU B 1
H9BA H 0.1443 -0.1178 0.2635 0.046 Uiso 0.63(3) 1 calc PR B 1
C10B C 0.1747(3) -0.0075(8) 0.2103(8) 0.034(3) Uani 0.63(3) 1 d PGU B 1
H10B H 0.1919 -0.0706 0.2054 0.041 Uiso 0.63(3) 1 calc PR B 1
C11B C 0.1777(3) 0.1127(10) 0.1829(7) 0.026(2) Uani 0.63(3) 1 d PGU B 1
H11B H 0.1971 0.1319 0.1593 0.031 Uiso 0.63(3) 1 calc PR B 1
C6" C 0.1463(6) 0.2029(12) 0.1872(11) 0.017(3) Uiso 0.37(3) 1 d PGDU B 2
N7" N 0.1714(5) 0.1233(17) 0.1653(10) 0.029(4) Uiso 0.37(3) 1 d PGU B 2
C8" C 0.1763(5) 0.0017(16) 0.1926(12) 0.039(4) Uiso 0.37(3) 1 d PGU B 2
H8"A H 0.1934 -0.0527 0.1776 0.046 Uiso 0.37(3) 1 calc PR B 2
C9" C 0.1562(6) -0.0404(12) 0.2418(11) 0.040(4) Uiso 0.37(3) 1 d PGU B 2
H9"A H 0.1595 -0.1236 0.2605 0.048 Uiso 0.37(3) 1 calc PR B 2
C10" C 0.1311(6) 0.0392(17) 0.2637(10) 0.026(4) Uiso 0.37(3) 1 d PGU B 2
H10D H 0.1174 0.0104 0.2973 0.031 Uiso 0.37(3) 1 calc PR B 2
C11" C 0.1262(5) 0.1609(16) 0.2364(11) 0.032(4) Uiso 0.37(3) 1 d PGU B 2
H11D H 0.1091 0.2153 0.2513 0.038 Uiso 0.37(3) 1 calc PR B 2
C12B C 0.1380(2) 0.2553(7) -0.0125(4) 0.0282(16) Uani 1 1 d . B .
H12B H 0.1219 0.2264 0.0203 0.034 Uiso 1 1 calc R . .
C13B C 0.1132(2) 0.2602(7) -0.0849(4) 0.0332(19) Uani 1 1 d . . .
H13C H 0.0945 0.3250 -0.0837 0.040 Uiso 1 1 calc R B .
H13D H 0.1273 0.2862 -0.1212 0.040 Uiso 1 1 calc R . .
C14B C 0.0954(2) 0.1347(8) -0.1062(5) 0.043(2) Uani 1 1 d . B .
H14C H 0.0783 0.1154 -0.0743 0.052 Uiso 1 1 calc R . .
H14D H 0.0815 0.1416 -0.1550 0.052 Uiso 1 1 calc R . .
C15B C 0.1217(2) 0.0273(8) -0.1033(5) 0.045(2) Uani 1 1 d . . .
H15C H 0.1364 0.0391 -0.1406 0.054 Uiso 1 1 calc R B .
H15D H 0.1085 -0.0535 -0.1126 0.054 Uiso 1 1 calc R . .
C16B C 0.1460(2) 0.0213(7) -0.0315(5) 0.040(2) Uani 1 1 d . B .
H16C H 0.1317 -0.0016 0.0049 0.049 Uiso 1 1 calc R . .
H16D H 0.1643 -0.0454 -0.0322 0.049 Uiso 1 1 calc R . .
C17B C 0.16432(19) 0.1445(7) -0.0125(5) 0.0328(18) Uani 1 1 d . . .
H17C H 0.1803 0.1630 -0.0466 0.039 Uiso 1 1 calc R B .
H17D H 0.1794 0.1373 0.0351 0.039 Uiso 1 1 calc R . .
C18B C 0.19835(19) 0.4300(7) -0.0058(4) 0.0266(15) Uani 1 1 d . B .
H18B H 0.2137 0.3558 0.0119 0.032 Uiso 1 1 calc R . .
C19B C 0.1953(2) 0.4314(8) -0.0868(4) 0.0320(17) Uani 1 1 d . . .
H19C H 0.1839 0.3520 -0.1068 0.038 Uiso 1 1 calc R B .
H19D H 0.1798 0.5028 -0.1069 0.038 Uiso 1 1 calc R . .
C20B C 0.2321(2) 0.4448(8) -0.1078(5) 0.0376(19) Uani 1 1 d . B .
H20C H 0.2291 0.4515 -0.1600 0.045 Uiso 1 1 calc R . .
H20D H 0.2465 0.3681 -0.0929 0.045 Uiso 1 1 calc R . .
C21B C 0.2522(2) 0.5611(8) -0.0740(5) 0.040(2) Uani 1 1 d . . .
H21C H 0.2767 0.5621 -0.0854 0.048 Uiso 1 1 calc R B .
H21D H 0.2397 0.6385 -0.0941 0.048 Uiso 1 1 calc R . .
C22B C 0.2547(2) 0.5613(8) 0.0056(5) 0.0350(19) Uani 1 1 d . B .
H22C H 0.2660 0.6412 0.0251 0.042 Uiso 1 1 calc R . .
H22D H 0.2703 0.4907 0.0262 0.042 Uiso 1 1 calc R . .
C23B C 0.21827(18) 0.5481(7) 0.0271(4) 0.0273(15) Uani 1 1 d . . .
H23C H 0.2037 0.6241 0.0118 0.033 Uiso 1 1 calc R B .
H23D H 0.2214 0.5426 0.0794 0.033 Uiso 1 1 calc R . .
C24B C 0.0649(2) 0.5732(7) 0.1732(5) 0.0338(18) Uani 1 1 d . B .
H24B H 0.0586 0.5157 0.2106 0.041 Uiso 1 1 calc R . .
C25B C 0.0866(2) 0.6841(8) 0.2111(5) 0.042(2) Uani 1 1 d . . .
H25C H 0.0939 0.7417 0.1756 0.050 Uiso 1 1 calc R B .
H25D H 0.1086 0.6516 0.2416 0.050 Uiso 1 1 calc R . .
C26B C 0.0638(3) 0.7574(9) 0.2568(5) 0.049(2) Uani 1 1 d . B .
H26C H 0.0583 0.7015 0.2949 0.059 Uiso 1 1 calc R . .
H26D H 0.0776 0.8305 0.2794 0.059 Uiso 1 1 calc R . .
C27B C 0.0286(3) 0.8044(9) 0.2117(6) 0.051(3) Uani 1 1 d . . .
H27C H 0.0141 0.8477 0.2425 0.062 Uiso 1 1 calc R B .
H27D H 0.0340 0.8663 0.1764 0.062 Uiso 1 1 calc R . .
C28B C 0.0072(2) 0.6958(8) 0.1736(5) 0.044(2) Uani 1 1 d . B .
H28C H -0.0146 0.7294 0.1429 0.053 Uiso 1 1 calc R . .
H28D H -0.0005 0.6386 0.2089 0.053 Uiso 1 1 calc R . .
C29B C 0.0293(2) 0.6220(8) 0.1287(5) 0.039(2) Uani 1 1 d . . .
H29C H 0.0347 0.6770 0.0903 0.047 Uiso 1 1 calc R B .
H29D H 0.0151 0.5492 0.1066 0.047 Uiso 1 1 calc R . .
C30B C 0.0643(2) 0.3283(7) 0.1021(4) 0.0334(18) Uani 1 1 d . B .
H30B H 0.0828 0.2615 0.1006 0.040 Uiso 1 1 calc R . .
C31B C 0.0446(3) 0.2891(8) 0.1613(5) 0.045(2) Uani 1 1 d . . .
H31C H 0.0611 0.2948 0.2074 0.054 Uiso 1 1 calc R B .
H31D H 0.0244 0.3477 0.1625 0.054 Uiso 1 1 calc R . .
C32B C 0.0305(3) 0.1556(8) 0.1505(5) 0.049(2) Uani 1 1 d . B .
H32C H 0.0180 0.1324 0.1897 0.059 Uiso 1 1 calc R . .
H32D H 0.0508 0.0965 0.1512 0.059 Uiso 1 1 calc R . .
C33B C 0.0048(3) 0.1433(9) 0.0806(5) 0.050(3) Uani 1 1 d . . .
H33C H -0.0165 0.1973 0.0812 0.060 Uiso 1 1 calc R B .
H33D H -0.0034 0.0546 0.0737 0.060 Uiso 1 1 calc R . .
C34B C 0.0231(2) 0.1831(8) 0.0199(5) 0.042(2) Uani 1 1 d . B .
H34C H 0.0057 0.1792 -0.0251 0.050 Uiso 1 1 calc R . .
H34D H 0.0429 0.1238 0.0165 0.050 Uiso 1 1 calc R . .
C35B C 0.0380(2) 0.3174(8) 0.0312(5) 0.038(2) Uani 1 1 d . . .
H35C H 0.0179 0.3775 0.0309 0.046 Uiso 1 1 calc R B .
H35D H 0.0504 0.3402 -0.0081 0.046 Uiso 1 1 calc R . .
C36B C 0.1518(2) 0.6721(7) 0.0946(5) 0.0346(19) Uani 1 1 d . . .
O36B O 0.17338(17) 0.7233(6) 0.1355(4) 0.0528(19) Uani 1 1 d . B .
C37B C 0.0885(2) 0.7546(8) 0.0272(5) 0.041(2) Uani 1 1 d . . .
O37B O 0.07429(17) 0.8527(6) 0.0327(4) 0.0509(17) Uani 1 1 d . B .
C38B C 0.1354(2) 0.6759(7) -0.0538(5) 0.0335(18) Uani 1 1 d . . .
O38B O 0.14866(16) 0.7244(5) -0.0997(3) 0.0408(15) Uani 1 1 d . B .
C39B C 0.0739(2) 0.5493(7) -0.0621(4) 0.0322(17) Uani 1 1 d . . .
O39B O 0.05019(16) 0.5374(6) -0.1083(3) 0.0453(17) Uani 1 1 d . B .
C40 C 0.2896(6) 0.607(2) 0.1942(12) 0.035(6) Uiso 0.272(4) 1 d PDU C 1
H40A H 0.2989 0.5624 0.1566 0.053 Uiso 0.272(4) 1 calc PR C 1
H40B H 0.3096 0.6360 0.2303 0.053 Uiso 0.272(4) 1 calc PR C 1
H40C H 0.2755 0.6803 0.1739 0.053 Uiso 0.272(4) 1 calc PR C 1
C41 C 0.2684(4) 0.5277(14) 0.2244(9) 0.044(6) Uiso 0.272(4) 1 d PGDU C 1
C42 C 0.2712(6) 0.3973(15) 0.2183(13) 0.046(7) Uiso 0.272(4) 1 d PGDU C 1
H42A H 0.2880 0.3623 0.1926 0.055 Uiso 0.272(4) 1 calc PR C 1
C43 C 0.2494(7) 0.3182(13) 0.2500(15) 0.036(5) Uiso 0.272(4) 1 d PGDU C 1
H43A H 0.2514 0.2291 0.2459 0.043 Uiso 0.272(4) 1 calc PR C 1
C44 C 0.2248(6) 0.3695(18) 0.2877(12) 0.038(6) Uiso 0.272(4) 1 d PGDU C 1
H44A H 0.2099 0.3155 0.3093 0.045 Uiso 0.272(4) 1 calc PR C 1
C45 C 0.2220(5) 0.500(2) 0.2937(11) 0.042(6) Uiso 0.272(4) 1 d PGDU C 1
H45A H 0.2052 0.5349 0.3194 0.050 Uiso 0.272(4) 1 calc PR C 1
C46 C 0.2438(5) 0.5790(14) 0.2621(10) 0.030(5) Uiso 0.272(4) 1 d PGDU C 1
H46A H 0.2418 0.6681 0.2662 0.037 Uiso 0.272(4) 1 calc PR C 1
C40' C 0.2821(7) 0.399(2) 0.1985(15) 0.051(8) Uiso 0.259(10) 1 d PDU D 2
H40D H 0.3014 0.3579 0.2312 0.076 Uiso 0.259(10) 1 calc PR D 2
H40E H 0.2921 0.4666 0.1728 0.076 Uiso 0.259(10) 1 calc PR D 2
H40F H 0.2700 0.3371 0.1646 0.076 Uiso 0.259(10) 1 calc PR D 2
C41' C 0.2582(4) 0.4497(15) 0.2355(9) 0.028(5) Uiso 0.259(10) 1 d PGDU D 2
C42' C 0.2374(6) 0.3714(13) 0.2700(12) 0.048(7) Uiso 0.259(10) 1 d PGDU D 2
H42B H 0.2399 0.2822 0.2677 0.058 Uiso 0.259(10) 1 calc PR D 2
C43' C 0.2129(5) 0.4235(19) 0.3077(12) 0.040(6) Uiso 0.259(10) 1 d PGDU D 2
H43B H 0.1987 0.3700 0.3313 0.048 Uiso 0.259(10) 1 calc PR D 2
C44' C 0.2093(5) 0.554(2) 0.3111(11) 0.061(9) Uiso 0.259(10) 1 d PGDU D 2
H44B H 0.1926 0.5896 0.3369 0.073 Uiso 0.259(10) 1 calc PR D 2
C45' C 0.2301(6) 0.6323(14) 0.2767(13) 0.048(7) Uiso 0.259(10) 1 d PGDU D 2
H45B H 0.2275 0.7215 0.2790 0.058 Uiso 0.259(10) 1 calc PR D 2
C46' C 0.2545(5) 0.5802(14) 0.2389(11) 0.037(7) Uiso 0.259(10) 1 d PGDU D 2
H46B H 0.2687 0.6338 0.2154 0.045 Uiso 0.259(10) 1 calc PR D 2
C40" C 0.2561(7) 0.7157(19) 0.2396(15) 0.041(8) Uiso 0.254(11) 1 d PD E 3
H40G H 0.2806 0.7479 0.2439 0.061 Uiso 0.254(11) 1 calc PR E 3
H40H H 0.2457 0.7450 0.2799 0.061 Uiso 0.254(11) 1 calc PR E 3
H40I H 0.2416 0.7467 0.1955 0.061 Uiso 0.254(11) 1 calc PR E 3
C41" C 0.2566(5) 0.5878(14) 0.2389(11) 0.049(8) Uiso 0.254(11) 1 d PGDU E 3
C42" C 0.2800(6) 0.525(2) 0.2028(14) 0.049(7) Uiso 0.254(11) 1 d PGDU E 3
H42C H 0.2956 0.5715 0.1789 0.058 Uiso 0.254(11) 1 calc PR E 3
C43" C 0.2806(7) 0.393(2) 0.2018(16) 0.048(8) Uiso 0.254(11) 1 d PGDU E 3
H43C H 0.2966 0.3503 0.1772 0.058 Uiso 0.254(11) 1 calc PR E 3
C44" C 0.2578(7) 0.3251(15) 0.2369(14) 0.043(7) Uiso 0.254(11) 1 d PGDU E 3
H44C H 0.2582 0.2354 0.2362 0.051 Uiso 0.254(11) 1 calc PR E 3
C45" C 0.2344(6) 0.3882(19) 0.2729(13) 0.041(6) Uiso 0.254(11) 1 d PGDU E 3
H45C H 0.2188 0.3415 0.2968 0.049 Uiso 0.254(11) 1 calc PR E 3
C46" C 0.2338(5) 0.5196(19) 0.2739(11) 0.029(5) Uiso 0.254(11) 1 d PGDU E 3
H46C H 0.2178 0.5626 0.2986 0.035 Uiso 0.254(11) 1 calc PR E 3
C40* C 0.2165(9) 0.652(3) 0.2984(19) 0.052(10) Uiso 0.215(12) 1 d PDU F 4
H40J H 0.2243 0.6562 0.3499 0.078 Uiso 0.215(12) 1 calc PR F 4
H40K H 0.1908 0.6343 0.2875 0.078 Uiso 0.215(12) 1 calc PR F 4
H40L H 0.2214 0.7327 0.2772 0.078 Uiso 0.215(12) 1 calc PR F 4
C41* C 0.2346(6) 0.5581(19) 0.2717(13) 0.042(7) Uiso 0.215(12) 1 d PGDU F 4
C42* C 0.2604(8) 0.5866(19) 0.2310(16) 0.055(8) Uiso 0.215(12) 1 d PGDU F 4
H42D H 0.2655 0.6723 0.2218 0.067 Uiso 0.215(12) 1 calc PR F 4
C43* C 0.2787(8) 0.490(3) 0.2038(16) 0.039(7) Uiso 0.215(12) 1 d PGDU F 4
H43D H 0.2963 0.5094 0.1760 0.047 Uiso 0.215(12) 1 calc PR F 4
C44* C 0.2712(8) 0.365(2) 0.2172(16) 0.043(7) Uiso 0.215(12) 1 d PGDU F 4
H44D H 0.2836 0.2984 0.1986 0.051 Uiso 0.215(12) 1 calc PR F 4
C45* C 0.2454(8) 0.3360(17) 0.2579(16) 0.043(7) Uiso 0.215(12) 1 d PGDU F 4
H45D H 0.2402 0.2503 0.2671 0.051 Uiso 0.215(12) 1 calc PR F 4
C46* C 0.2271(6) 0.433(2) 0.2852(13) 0.038(6) Uiso 0.215(12) 1 d PGDU F 4
H46D H 0.2095 0.4132 0.3130 0.045 Uiso 0.215(12) 1 calc PR F 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
W1A C38A 2.010(7) . ?
W1A C37A 2.027(6) . ?
W1A C36A 2.028(6) . ?
W1A C39A 2.036(6) . ?
W1A P3A 2.5420(15) . ?
W1A P5A 2.5596(16) . ?
N1A C6A 1.377(7) . ?
N1A C6' 1.420(12) . ?
N1A C2A 1.451(8) . ?
N1A C4A 1.469(8) . ?
C2A P3A 1.865(6) . ?
P3A C18A 1.868(6) . ?
P3A C12A 1.894(6) . ?
C4A P5A 1.862(6) . ?
P5A C24A 1.871(6) . ?
P5A C30A 1.877(5) . ?
C6A N7A 1.3900 . ?
C6A C11A 1.3900 . ?
N7A C8A 1.3900 . ?
C8A C9A 1.3900 . ?
C9A C10A 1.3900 . ?
C10A C11A 1.3900 . ?
C6' N7' 1.3900 . ?
C6' C11' 1.3900 . ?
N7' C8' 1.3900 . ?
C8' C9' 1.3900 . ?
C9' C10' 1.3900 . ?
C10' C11' 1.3900 . ?
C12A C17A 1.528(8) . ?
C12A C13A 1.537(9) . ?
C13A C14A 1.541(9) . ?
C14A C15A 1.533(9) . ?
C15A C16A 1.533(9) . ?
C16A C17A 1.564(8) . ?
C18A C19A 1.526(9) . ?
C18A C23A 1.549(8) . ?
C19A C20A 1.533(9) . ?
C20A C21A 1.522(11) . ?
C21A C22A 1.515(11) . ?
C22A C23A 1.532(9) . ?
C24A C25A 1.532(8) . ?
C24A C29A 1.532(8) . ?
C25A C26A 1.517(9) . ?
C26A C27A 1.512(11) . ?
C27A C28A 1.526(10) . ?
C28A C29A 1.528(9) . ?
C30A C35A 1.527(8) . ?
C30A C31A 1.544(8) . ?
C31A C32A 1.544(8) . ?
C32A C33A 1.514(10) . ?
C33A C34A 1.521(10) . ?
C34A C35A 1.536(8) . ?
C36A O36A 1.139(7) . ?
C37A O37A 1.136(7) . ?
C38A O38A 1.120(8) . ?
C39A O39A 1.153(7) . ?
W1B C38B 1.941(9) . ?
W1B C37B 1.949(10) . ?
W1B C36B 2.012(8) . ?
W1B C39B 2.037(8) . ?
W1B P3B 2.5305(19) . ?
W1B P5B 2.559(2) . ?
N1B C6B 1.357(8) . ?
N1B C6" 1.365(12) . ?
N1B C2B 1.444(10) . ?
N1B C4B 1.450(9) . ?
C2B P3B 1.880(7) . ?
P3B C12B 1.820(7) . ?
P3B C18B 1.862(7) . ?
C4B P5B 1.875(7) . ?
P5B C24B 1.829(8) . ?
P5B C30B 1.865(8) . ?
C6B N7B 1.3900 . ?
C6B C11B 1.3900 . ?
N7B C8B 1.3900 . ?
C8B C9B 1.3900 . ?
C9B C10B 1.3900 . ?
C10B C11B 1.3900 . ?
C6" N7" 1.3900 . ?
C6" C11" 1.3900 . ?
N7" C8" 1.3900 . ?
C8" C9" 1.3900 . ?
C9" C10" 1.3900 . ?
C10" C11" 1.3900 . ?
C12B C13B 1.534(10) . ?
C12B C17B 1.542(10) . ?
C13B C14B 1.513(11) . ?
C14B C15B 1.508(11) . ?
C15B C16B 1.516(11) . ?
C16B C17B 1.491(10) . ?
C18B C23B 1.537(10) . ?
C18B C19B 1.538(11) . ?
C19B C20B 1.529(11) . ?
C20B C21B 1.530(11) . ?
C21B C22B 1.513(12) . ?
C22B C23B 1.521(10) . ?
C24B C25B 1.540(11) . ?
C24B C29B 1.552(10) . ?
C25B C26B 1.547(12) . ?
C26B C27B 1.539(13) . ?
C27B C28B 1.516(12) . ?
C28B C29B 1.521(12) . ?
C30B C31B 1.525(12) . ?
C30B C35B 1.541(11) . ?
C31B C32B 1.511(11) . ?
C32B C33B 1.516(12) . ?
C33B C34B 1.518(13) . ?
C34B C35B 1.530(11) . ?
C36B O36B 1.161(9) . ?
C37B O37B 1.184(10) . ?
C38B O38B 1.205(10) . ?
C39B O39B 1.151(9) . ?
C40 C41 1.363(17) . ?
C41 C42 1.3900 . ?
C41 C46 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?
C45 C46 1.3900 . ?
C40' C41' 1.359(18) . ?
C41' C42' 1.3900 . ?
C41' C46' 1.3900 . ?
C42' C43' 1.3900 . ?
C43' C44' 1.3900 . ?
C44' C45' 1.3900 . ?
C45' C46' 1.3900 . ?
C40" C41" 1.353(17) . ?
C41" C42" 1.3900 . ?
C41" C46" 1.3900 . ?
C42" C43" 1.3900 . ?
C43" C44" 1.3900 . ?
C44" C45" 1.3900 . ?
C45" C46" 1.3900 . ?
C40* C41* 1.358(17) . ?
C41* C42* 1.3900 . ?
C41* C46* 1.3900 . ?
C42* C43* 1.3900 . ?
C43* C44* 1.3900 . ?
C44* C45* 1.3900 . ?
C45* C46* 1.3900 . ?

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
C38A W1A C37A 88.8(2) . . ?
C38A W1A C36A 90.3(3) . . ?
C37A W1A C36A 84.8(3) . . ?
C38A W1A C39A 86.0(2) . . ?
C37A W1A C39A 85.5(3) . . ?
C36A W1A C39A 169.7(3) . . ?
C38A W1A P3A 91.40(16) . . ?
C37A W1A P3A 171.27(19) . . ?
C36A W1A P3A 86.44(18) . . ?
C39A W1A P3A 103.20(18) . . ?
C38A W1A P5A 175.61(16) . . ?
C37A W1A P5A 95.40(19) . . ?
C36A W1A P5A 88.9(2) . . ?
C39A W1A P5A 95.57(18) . . ?
P3A W1A P5A 84.25(5) . . ?
C6A N1A C2A 119.6(6) . . ?
C6' N1A C2A 126.5(11) . . ?
C6A N1A C4A 121.2(7) . . ?
C6' N1A C4A 115.0(12) . . ?
C2A N1A C4A 117.0(5) . . ?
N1A C2A P3A 115.3(4) . . ?
C2A P3A C18A 96.6(3) . . ?
C2A P3A C12A 101.1(3) . . ?
C18A P3A C12A 106.8(3) . . ?
C2A P3A W1A 110.2(2) . . ?
C18A P3A W1A 118.68(19) . . ?
C12A P3A W1A 119.59(17) . . ?
N1A C4A P5A 112.8(4) . . ?
C4A P5A C24A 100.8(3) . . ?
C4A P5A C30A 99.0(3) . . ?
C24A P5A C30A 104.1(3) . . ?
C4A P5A W1A 110.5(2) . . ?
C24A P5A W1A 116.4(2) . . ?
C30A P5A W1A 122.7(2) . . ?
N1A C6A N7A 113.1(9) . . ?
N1A C6A C11A 126.7(8) . . ?
N7A C6A C11A 120.0 . . ?
C6A N7A C8A 120.0 . . ?
N7A C8A C9A 120.0 . . ?
C10A C9A C8A 120.0 . . ?
C9A C10A C11A 120.0 . . ?
C10A C11A C6A 120.0 . . ?
N7' C6' C11' 120.0 . . ?
N7' C6' N1A 108.6(18) . . ?
C11' C6' N1A 131.4(18) . . ?
C8' N7' C6' 120.0 . . ?
N7' C8' C9' 120.0 . . ?
C8' C9' C10' 120.0 . . ?
C11' C10' C9' 120.0 . . ?
C10' C11' C6' 120.0 . . ?
C17A C12A C13A 110.4(5) . . ?
C17A C12A P3A 113.7(4) . . ?
C13A C12A P3A 112.1(4) . . ?
C12A C13A C14A 109.9(5) . . ?
C15A C14A C13A 110.8(5) . . ?
C14A C15A C16A 111.4(6) . . ?
C15A C16A C17A 110.7(5) . . ?
C12A C17A C16A 107.9(5) . . ?
C19A C18A C23A 109.3(5) . . ?
C19A C18A P3A 114.6(4) . . ?
C23A C18A P3A 110.8(5) . . ?
C18A C19A C20A 111.2(5) . . ?
C21A C20A C19A 111.5(6) . . ?
C22A C21A C20A 110.8(7) . . ?
C21A C22A C23A 111.5(6) . . ?
C22A C23A C18A 111.0(6) . . ?
C25A C24A C29A 112.1(5) . . ?
C25A C24A P5A 114.0(4) . . ?
C29A C24A P5A 110.2(4) . . ?
C26A C25A C24A 110.0(6) . . ?
C27A C26A C25A 111.8(7) . . ?
C26A C27A C28A 111.3(6) . . ?
C27A C28A C29A 111.7(6) . . ?
C28A C29A C24A 110.9(5) . . ?
C35A C30A C31A 110.9(5) . . ?
C35A C30A P5A 115.6(4) . . ?
C31A C30A P5A 114.6(4) . . ?
C32A C31A C30A 109.6(5) . . ?
C33A C32A C31A 110.4(6) . . ?
C32A C33A C34A 110.8(6) . . ?
C33A C34A C35A 113.0(6) . . ?
C30A C35A C34A 110.2(5) . . ?
O36A C36A W1A 176.1(6) . . ?
O37A C37A W1A 173.8(6) . . ?
O38A C38A W1A 178.9(6) . . ?
O39A C39A W1A 171.0(5) . . ?
C38B W1B C37B 87.7(4) . . ?
C38B W1B C36B 90.3(3) . . ?
C37B W1B C36B 84.4(3) . . ?
C38B W1B C39B 84.4(3) . . ?
C37B W1B C39B 87.6(3) . . ?
C36B W1B C39B 170.6(3) . . ?
C38B W1B P3B 92.0(2) . . ?
C37B W1B P3B 170.5(2) . . ?
C36B W1B P3B 86.1(2) . . ?
C39B W1B P3B 101.8(2) . . ?
C38B W1B P5B 175.6(2) . . ?
C37B W1B P5B 96.3(3) . . ?
C36B W1B P5B 88.3(3) . . ?
C39B W1B P5B 97.5(2) . . ?
P3B W1B P5B 83.75(7) . . ?
C6B N1B C2B 117.6(7) . . ?
C6" N1B C2B 124.9(10) . . ?
C6B N1B C4B 124.5(8) . . ?
C6" N1B C4B 119.2(10) . . ?
C2B N1B C4B 115.0(6) . . ?
N1B C2B P3B 115.6(5) . . ?
C12B P3B C18B 105.4(3) . . ?
C12B P3B C2B 102.1(3) . . ?
C18B P3B C2B 97.1(3) . . ?
C12B P3B W1B 120.8(2) . . ?
C18B P3B W1B 117.1(2) . . ?
C2B P3B W1B 110.8(2) . . ?
N1B C4B P5B 113.4(5) . . ?
C24B P5B C30B 104.8(4) . . ?
C24B P5B C4B 100.1(4) . . ?
C30B P5B C4B 98.2(4) . . ?
C24B P5B W1B 117.4(3) . . ?
C30B P5B W1B 122.6(3) . . ?
C4B P5B W1B 109.7(3) . . ?
N1B C6B N7B 110.0(9) . . ?
N1B C6B C11B 129.6(9) . . ?
N7B C6B C11B 120.0 . . ?
C6B N7B C8B 120.0 . . ?
N7B C8B C9B 120.0 . . ?
C10B C9B C8B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C10B C11B C6B 120.0 . . ?
N1B C6" N7" 111.5(14) . . ?
N1B C6" C11" 128.1(14) . . ?
N7" C6" C11" 120.0 . . ?
C6" N7" C8" 120.0 . . ?
N7" C8" C9" 120.0 . . ?
C10" C9" C8" 120.0 . . ?
C11" C10" C9" 120.0 . . ?
C10" C11" C6" 120.0 . . ?
C13B C12B C17B 108.5(6) . . ?
C13B C12B P3B 116.0(5) . . ?
C17B C12B P3B 119.1(5) . . ?
C14B C13B C12B 112.7(7) . . ?
C15B C14B C13B 112.9(7) . . ?
C14B C15B C16B 110.9(7) . . ?
C17B C16B C15B 111.5(7) . . ?
C16B C17B C12B 113.1(6) . . ?
C23B C18B C19B 110.5(6) . . ?
C23B C18B P3B 112.2(5) . . ?
C19B C18B P3B 114.0(5) . . ?
C20B C19B C18B 111.1(6) . . ?
C19B C20B C21B 111.9(7) . . ?
C22B C21B C20B 111.4(7) . . ?
C21B C22B C23B 112.3(6) . . ?
C22B C23B C18B 111.5(6) . . ?
C25B C24B C29B 110.2(6) . . ?
C25B C24B P5B 113.6(6) . . ?
C29B C24B P5B 110.1(6) . . ?
C24B C25B C26B 110.0(7) . . ?
C27B C26B C25B 111.1(8) . . ?
C28B C27B C26B 111.3(7) . . ?
C27B C28B C29B 111.1(8) . . ?
C28B C29B C24B 111.9(7) . . ?
C31B C30B C35B 108.1(7) . . ?
C31B C30B P5B 114.9(6) . . ?
C35B C30B P5B 116.0(6) . . ?
C32B C31B C30B 111.1(8) . . ?
C31B C32B C33B 111.0(8) . . ?
C32B C33B C34B 110.1(8) . . ?
C33B C34B C35B 110.9(8) . . ?
C34B C35B C30B 111.0(7) . . ?
O36B C36B W1B 175.4(7) . . ?
O37B C37B W1B 177.7(7) . . ?
O38B C38B W1B 179.3(8) . . ?
O39B C39B W1B 172.0(7) . . ?
C40 C41 C42 121.1(8) . . ?
C40 C41 C46 118.9(8) . . ?
C42 C41 C46 120.0 . . ?
C43 C42 C41 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C44 C45 C46 120.0 . . ?
C45 C46 C41 120.0 . . ?
C40' C41' C42' 120.3(8) . . ?
C40' C41' C46' 119.7(8) . . ?
C42' C41' C46' 120.0 . . ?
C41' C42' C43' 120.0 . . ?
C44' C43' C42' 120.0 . . ?
C43' C44' C45' 120.0 . . ?
C46' C45' C44' 120.0 . . ?
C45' C46' C41' 120.0 . . ?
C40" C41" C42" 119.8(8) . . ?
C40" C41" C46" 120.2(8) . . ?
C42" C41" C46" 120.0 . . ?
C43" C42" C41" 120.0 . . ?
C42" C43" C44" 120.0 . . ?
C45" C44" C43" 120.0 . . ?
C44" C45" C46" 120.0 . . ?
C45" C46" C41" 120.0 . . ?
C40* C41* C42* 120.5(8) . . ?
C40* C41* C46* 119.5(8) . . ?
C42* C41* C46* 120.0 . . ?
C43* C42* C41* 120.0 . . ?
C42* C43* C44* 120.0 . . ?
C45* C44* C43* 120.0 . . ?
C44* C45* C46* 120.0 . . ?
C45* C46* C41* 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.913
_diffrn_reflns_theta_full        31.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.696
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.134

#===END



