# 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_3815
_database_code_depnum_ccdc_archive 'CCDC 1440415'
_audit_update_record             
;
2015-12-03 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_audit_creation_date             2014-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        JMV416
_chemical_formula_moiety         'C31 H29 N2 O5 P S W'
_chemical_formula_sum            'C31 H29 N2 O5 P S W'
_chemical_formula_weight         756.44
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   9.6390(6)
_cell_length_b                   9.9715(5)
_cell_length_c                   16.9758(11)
_cell_angle_alpha                78.438(5)
_cell_angle_beta                 89.320(5)
_cell_angle_gamma                73.325(4)
_cell_volume                     1529.49(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6527
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      28.93
_cell_measurement_temperature    123
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_T_max  0.6566
_exptl_absorpt_correction_T_min  0.4692
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.1334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10474
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.61
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3957
_reflns_number_total             5403
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      0.899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0762
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
W W 0.56332(4) 0.84161(4) 0.17681(2) 0.01636(9) Uani 1 d . . .
S S 0.4565(2) 0.6621(2) 0.38352(12) 0.0207(5) Uani 1 d . . .
P P 0.3997(2) 0.7180(2) 0.25771(12) 0.0142(5) Uani 1 d . . .
O1 O 0.7728(6) 1.0054(6) 0.0844(4) 0.0357(16) Uani 1 d . . .
O2 O 0.6296(6) 0.6599(7) 0.0393(4) 0.0319(15) Uani 1 d . . .
O3 O 0.8288(6) 0.6243(7) 0.2885(4) 0.0382(18) Uani 1 d . . .
O4 O 0.5408(7) 1.0248(8) 0.3125(4) 0.047(2) Uani 1 d . . .
O5 O 0.3027(7) 1.0841(7) 0.0758(4) 0.0395(18) Uani 1 d . . .
N1 N 0.2473(6) 0.8209(7) 0.2924(4) 0.0183(14) Uani 1 d . . .
N2 N 0.1980(6) 0.8444(7) 0.4265(4) 0.0199(15) Uani 1 d . . .
C1 C 0.2750(8) 0.7920(8) 0.3751(5) 0.0195(17) Uani 1 d . . .
C2 C 0.2476(8) 0.7953(9) 0.5121(5) 0.026(2) Uani 1 d . . .
H2 H 0.3514 0.7361 0.5167 0.031 Uiso 1 calc . . R
C3 C 0.1549(10) 0.7065(11) 0.5539(5) 0.043(3) Uani 1 d . . .
H3A H 0.0535 0.7651 0.5498 0.064 Uiso 1 calc . . GR
H3B H 0.1874 0.6718 0.6108 0.064 Uiso 1 calc . . GR
H3C H 0.1637 0.6247 0.5284 0.064 Uiso 1 calc . . GR
C4 C 0.2330(9) 0.9278(10) 0.5477(5) 0.035(2) Uani 1 d . . .
H4A H 0.3025 0.9772 0.5236 0.052 Uiso 1 calc . . GR
H4B H 0.2529 0.8988 0.6061 0.052 Uiso 1 calc . . GR
H4C H 0.1343 0.9924 0.5362 0.052 Uiso 1 calc . . GR
C5 C 0.1309(7) 0.9470(8) 0.2480(5) 0.0177(17) Uani 1 d . . .
H5 H 0.1458 0.9522 0.1892 0.021 Uiso 1 calc . . R
C6 C -0.0177(8) 0.9255(9) 0.2638(5) 0.028(2) Uani 1 d . . .
H6A H -0.0212 0.8374 0.2478 0.042 Uiso 1 calc . . GR
H6B H -0.0923 1.0070 0.2325 0.042 Uiso 1 calc . . GR
H6C H -0.0352 0.9183 0.3213 0.042 Uiso 1 calc . . GR
C7 C 0.1403(9) 1.0858(9) 0.2666(5) 0.028(2) Uani 1 d . . .
H7A H 0.1056 1.0935 0.3205 0.042 Uiso 1 calc . . GR
H7B H 0.0801 1.1661 0.2268 0.042 Uiso 1 calc . . GR
H7C H 0.2412 1.0881 0.2647 0.042 Uiso 1 calc . . GR
C8 C 0.3502(7) 0.5538(8) 0.2336(4) 0.0159(16) Uani 1 d . . .
C9 C 0.3052(7) 0.4705(8) 0.3110(4) 0.0175(17) Uani 1 d . . .
C10 C 0.3908(7) 0.3362(8) 0.3517(5) 0.0223(19) Uani 1 d . . .
H10 H 0.4792 0.2911 0.3299 0.027 Uiso 1 calc . . R
C11 C 0.3491(9) 0.2695(10) 0.4219(5) 0.035(2) Uani 1 d . . .
H11 H 0.4102 0.1795 0.4491 0.042 Uiso 1 calc . . R
C12 C 0.2200(10) 0.3296(10) 0.4544(5) 0.037(2) Uani 1 d . . .
H12 H 0.1916 0.2819 0.5034 0.044 Uiso 1 calc . . R
C13 C 0.1324(8) 0.4616(9) 0.4139(5) 0.026(2) Uani 1 d . . .
H13 H 0.0426 0.5046 0.4350 0.032 Uiso 1 calc . . R
C14 C 0.1750(7) 0.5303(8) 0.3436(5) 0.0165(17) Uani 1 d . . .
H14 H 0.1140 0.6206 0.3167 0.020 Uiso 1 calc . . R
C15 C 0.4886(7) 0.4655(8) 0.2002(4) 0.0182(17) Uani 1 d . . .
C16 C 0.4856(8) 0.4166(8) 0.1298(5) 0.0206(18) Uani 1 d . . .
H16 H 0.3958 0.4371 0.1007 0.025 Uiso 1 calc . . R
C17 C 0.6120(8) 0.3380(9) 0.1009(5) 0.026(2) Uani 1 d . . .
H17 H 0.6082 0.3055 0.0522 0.031 Uiso 1 calc . . R
C18 C 0.7446(8) 0.3068(8) 0.1432(5) 0.026(2) Uani 1 d . . .
H18 H 0.8315 0.2529 0.1239 0.031 Uiso 1 calc . . R
C19 C 0.7470(8) 0.3559(8) 0.2138(5) 0.0237(19) Uani 1 d . . .
H19 H 0.8369 0.3360 0.2427 0.028 Uiso 1 calc . . R
C20 C 0.6210(8) 0.4334(8) 0.2433(5) 0.0208(18) Uani 1 d . . .
H20 H 0.6246 0.4646 0.2924 0.025 Uiso 1 calc . . R
C21 C 0.2248(7) 0.6050(8) 0.1691(4) 0.0154(16) Uani 1 d . . .
C22 C 0.2074(7) 0.7249(8) 0.1079(4) 0.0172(17) Uani 1 d . . .
H22 H 0.2730 0.7806 0.1059 0.021 Uiso 1 calc . . R
C23 C 0.0959(8) 0.7643(9) 0.0497(5) 0.023(2) Uani 1 d . . .
H23 H 0.0844 0.8484 0.0093 0.028 Uiso 1 calc . . R
C24 C 0.0024(8) 0.6854(9) 0.0490(5) 0.024(2) Uani 1 d . . .
H24 H -0.0738 0.7138 0.0087 0.029 Uiso 1 calc . . R
C25 C 0.0197(8) 0.5627(9) 0.1079(5) 0.027(2) Uani 1 d . . .
H25 H -0.0434 0.5052 0.1073 0.032 Uiso 1 calc . . R
C26 C 0.1286(8) 0.5237(9) 0.1676(5) 0.0233(18) Uani 1 d . . .
H26 H 0.1382 0.4404 0.2083 0.028 Uiso 1 calc . . R
C27 C 0.6967(9) 0.9449(11) 0.1184(5) 0.032(2) Uani 1 d . . .
C28 C 0.6006(9) 0.7213(10) 0.0900(6) 0.024(2) Uani 1 d . . .
C29 C 0.7344(9) 0.6966(10) 0.2476(5) 0.025(2) Uani 1 d . . .
C30 C 0.5457(9) 0.9603(9) 0.2633(6) 0.027(2) Uani 1 d . . .
C31 C 0.3930(9) 0.9945(9) 0.1122(5) 0.025(2) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.506(2) . ?
W C27 2.005(9) . ?
W C28 2.046(10) . ?
W C29 2.058(9) . ?
W C30 2.040(10) . ?
W C31 2.039(9) . ?
S P 2.132(3) . ?
S C1 1.841(7) . ?
P N1 1.707(6) . ?
P C8 1.949(8) . ?
O1 C27 1.157(10) . ?
O2 C28 1.141(10) . ?
O3 C29 1.126(9) . ?
O4 C30 1.145(11) . ?
O5 C31 1.133(9) . ?
N1 C1 1.388(9) . ?
N1 C5 1.497(8) . ?
N2 C1 1.237(10) . ?
N2 C2 1.476(9) . ?
C2 H2 1.0000 . ?
C2 C3 1.508(12) . ?
C2 C4 1.530(12) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 1.0000 . ?
C5 C6 1.521(10) . ?
C5 C7 1.507(11) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.536(10) . ?
C8 C15 1.544(9) . ?
C8 C21 1.542(9) . ?
C9 C10 1.400(10) . ?
C9 C14 1.387(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.360(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.379(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.390(11) . ?
C13 H13 0.9500 . ?
C13 C14 1.372(11) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(10) . ?
C15 C20 1.401(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.390(10) . ?
C17 H17 0.9500 . ?
C17 C18 1.396(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.387(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(10) . ?
C21 C26 1.399(10) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(10) . ?
C23 H23 0.9500 . ?
C23 C24 1.358(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(11) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(10) . ?
C26 H26 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 W P 176.3(3) . . ?
C27 W C28 86.4(4) . . ?
C27 W C29 91.0(3) . . ?
C27 W C30 89.7(4) . . ?
C27 W C31 88.6(3) . . ?
C28 W P 97.0(2) . . ?
C28 W C29 90.6(3) . . ?
C29 W P 87.7(2) . . ?
C30 W P 86.8(3) . . ?
C30 W C28 174.8(4) . . ?
C30 W C29 86.1(3) . . ?
C31 W P 92.5(2) . . ?
C31 W C28 93.3(3) . . ?
C31 W C29 176.0(4) . . ?
C31 W C30 90.0(4) . . ?
C1 S P 75.6(3) . . ?
S P W 113.18(10) . . ?
N1 P W 118.2(2) . . ?
N1 P S 80.2(2) . . ?
N1 P C8 106.5(3) . . ?
C8 P W 124.6(2) . . ?
C8 P S 105.0(2) . . ?
C1 N1 P 103.9(4) . . ?
C1 N1 C5 123.8(6) . . ?
C5 N1 P 129.7(5) . . ?
C1 N2 C2 119.2(6) . . ?
N1 C1 S 100.3(5) . . ?
N2 C1 S 131.4(6) . . ?
N2 C1 N1 128.3(7) . . ?
N2 C2 H2 109.7 . . ?
N2 C2 C3 108.4(7) . . ?
N2 C2 C4 107.8(7) . . ?
C3 C2 H2 109.7 . . ?
C3 C2 C4 111.5(7) . . ?
C4 C2 H2 109.7 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5 107.3 . . ?
N1 C5 C6 110.4(6) . . ?
N1 C5 C7 112.2(6) . . ?
C6 C5 H5 107.3 . . ?
C7 C5 H5 107.3 . . ?
C7 C5 C6 112.0(6) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 P 109.1(5) . . ?
C9 C8 C15 112.7(6) . . ?
C9 C8 C21 110.0(6) . . ?
C15 C8 P 105.2(5) . . ?
C21 C8 P 109.8(5) . . ?
C21 C8 C15 110.0(6) . . ?
C10 C9 C8 123.0(6) . . ?
C14 C9 C8 119.3(6) . . ?
C14 C9 C10 117.6(7) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(7) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(8) . . ?
C12 C11 H11 119.3 . . ?
C11 C12 H12 120.8 . . ?
C11 C12 C13 118.4(8) . . ?
C13 C12 H12 120.8 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(7) . . ?
C14 C13 H13 119.8 . . ?
C9 C14 H14 119.3 . . ?
C13 C14 C9 121.3(7) . . ?
C13 C14 H14 119.3 . . ?
C16 C15 C8 122.2(6) . . ?
C16 C15 C20 119.3(6) . . ?
C20 C15 C8 118.5(7) . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 121.0(7) . . ?
C17 C16 H16 119.5 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.1(8) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.6 . . ?
C19 C18 C17 118.7(7) . . ?
C19 C18 H18 120.6 . . ?
C18 C19 H19 119.3 . . ?
C18 C19 C20 121.5(7) . . ?
C20 C19 H19 119.3 . . ?
C15 C20 H20 120.3 . . ?
C19 C20 C15 119.5(8) . . ?
C19 C20 H20 120.3 . . ?
C22 C21 C8 122.8(7) . . ?
C22 C21 C26 117.4(7) . . ?
C26 C21 C8 119.6(6) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(7) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(7) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.0(7) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 H25 119.9 . . ?
C26 C25 C24 120.3(8) . . ?
C26 C25 H25 119.9 . . ?
C21 C26 H26 119.5 . . ?
C25 C26 C21 121.0(7) . . ?
C25 C26 H26 119.5 . . ?
O1 C27 W 179.5(9) . . ?
O2 C28 W 174.3(8) . . ?
O3 C29 W 175.5(8) . . ?
O4 C30 W 177.6(7) . . ?
O5 C31 W 176.4(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P N1 C1 -110.7(4) . . . . ?
W P N1 C5 51.2(7) . . . . ?
W P C8 C9 156.3(3) . . . . ?
W P C8 C15 35.2(5) . . . . ?
W P C8 C21 -83.1(5) . . . . ?
S P N1 C1 0.4(4) . . . . ?
S P N1 C5 162.4(7) . . . . ?
S P C8 C9 23.5(5) . . . . ?
S P C8 C15 -97.6(4) . . . . ?
S P C8 C21 144.2(4) . . . . ?
P W C27 O1 -104(100) . . . . ?
P W C28 O2 -172(7) . . . . ?
P W C29 O3 -109(9) . . . . ?
P W C30 O4 115(22) . . . . ?
P W C31 O5 152(13) . . . . ?
P S C1 N1 0.4(4) . . . . ?
P S C1 N2 -177.8(9) . . . . ?
P N1 C1 S -0.5(5) . . . . ?
P N1 C1 N2 177.8(8) . . . . ?
P N1 C5 C6 127.8(7) . . . . ?
P N1 C5 C7 -106.4(7) . . . . ?
P C8 C9 C10 -109.0(8) . . . . ?
P C8 C9 C14 70.2(7) . . . . ?
P C8 C15 C16 -131.1(7) . . . . ?
P C8 C15 C20 49.4(8) . . . . ?
P C8 C21 C22 33.5(8) . . . . ?
P C8 C21 C26 -150.9(6) . . . . ?
N1 P C8 C9 -60.5(5) . . . . ?
N1 P C8 C15 178.4(4) . . . . ?
N1 P C8 C21 60.2(5) . . . . ?
C1 S P W 116.2(3) . . . . ?
C1 S P N1 -0.3(3) . . . . ?
C1 S P C8 -104.9(3) . . . . ?
C1 N1 C5 C6 -73.4(9) . . . . ?
C1 N1 C5 C7 52.4(9) . . . . ?
C1 N2 C2 C3 -108.5(9) . . . . ?
C1 N2 C2 C4 130.6(8) . . . . ?
C2 N2 C1 S -3.7(12) . . . . ?
C2 N2 C1 N1 178.6(7) . . . . ?
C5 N1 C1 S -163.8(6) . . . . ?
C5 N1 C1 N2 14.4(12) . . . . ?
C8 P N1 C1 103.3(5) . . . . ?
C8 P N1 C5 -94.8(7) . . . . ?
C8 C9 C10 C11 177.2(8) . . . . ?
C8 C9 C14 C13 -178.1(8) . . . . ?
C8 C15 C16 C17 179.7(7) . . . . ?
C8 C15 C20 C19 -179.1(7) . . . . ?
C8 C21 C22 C23 177.9(6) . . . . ?
C8 C21 C26 C25 -176.5(7) . . . . ?
C9 C8 C15 C16 110.2(8) . . . . ?
C9 C8 C15 C20 -69.3(9) . . . . ?
C9 C8 C21 C22 153.5(7) . . . . ?
C9 C8 C21 C26 -30.9(9) . . . . ?
C9 C10 C11 C12 1.6(15) . . . . ?
C10 C9 C14 C13 1.1(12) . . . . ?
C10 C11 C12 C13 -0.3(15) . . . . ?
C11 C12 C13 C14 -0.6(14) . . . . ?
C12 C13 C14 C9 0.2(13) . . . . ?
C14 C9 C10 C11 -2.0(12) . . . . ?
C15 C8 C9 C10 7.4(11) . . . . ?
C15 C8 C9 C14 -173.4(7) . . . . ?
C15 C8 C21 C22 -81.7(8) . . . . ?
C15 C8 C21 C26 93.8(8) . . . . ?
C15 C16 C17 C18 0.3(13) . . . . ?
C16 C15 C20 C19 1.3(12) . . . . ?
C16 C17 C18 C19 -0.2(12) . . . . ?
C17 C18 C19 C20 0.7(12) . . . . ?
C18 C19 C20 C15 -1.3(12) . . . . ?
C20 C15 C16 C17 -0.8(12) . . . . ?
C21 C8 C9 C10 130.6(8) . . . . ?
C21 C8 C9 C14 -50.3(9) . . . . ?
C21 C8 C15 C16 -13.0(10) . . . . ?
C21 C8 C15 C20 167.5(7) . . . . ?
C21 C22 C23 C24 -1.9(11) . . . . ?
C22 C21 C26 C25 -0.7(11) . . . . ?
C22 C23 C24 C25 -0.1(12) . . . . ?
C23 C24 C25 C26 1.6(13) . . . . ?
C24 C25 C26 C21 -1.2(12) . . . . ?
C26 C21 C22 C23 2.2(11) . . . . ?
C27 W P S -27(4) . . . . ?
C27 W P N1 64(4) . . . . ?
C27 W P C8 -156(4) . . . . ?
C27 W C28 O2 6(7) . . . . ?
C27 W C29 O3 67(9) . . . . ?
C27 W C30 O4 -64(22) . . . . ?
C27 W C31 O5 -25(13) . . . . ?
C28 W P S 132.1(2) . . . . ?
C28 W P N1 -136.8(3) . . . . ?
C28 W P C8 2.6(3) . . . . ?
C28 W C27 O1 97(100) . . . . ?
C28 W C29 O3 154(9) . . . . ?
C28 W C30 O4 -24(26) . . . . ?
C28 W C31 O5 -111(13) . . . . ?
C29 W P S 41.7(3) . . . . ?
C29 W P N1 132.8(4) . . . . ?
C29 W P C8 -87.8(4) . . . . ?
C29 W C27 O1 -173(100) . . . . ?
C29 W C28 O2 -85(7) . . . . ?
C29 W C30 O4 27(22) . . . . ?
C29 W C31 O5 60(16) . . . . ?
C30 W P S -44.5(2) . . . . ?
C30 W P N1 46.7(3) . . . . ?
C30 W P C8 -173.9(3) . . . . ?
C30 W C27 O1 -87(100) . . . . ?
C30 W C28 O2 -35(11) . . . . ?
C30 W C29 O3 -22(9) . . . . ?
C30 W C31 O5 65(13) . . . . ?
C31 W P S -134.3(3) . . . . ?
C31 W P N1 -43.2(4) . . . . ?
C31 W P C8 96.3(4) . . . . ?
C31 W C27 O1 3(100) . . . . ?
C31 W C28 O2 95(7) . . . . ?
C31 W C29 O3 -17(13) . . . . ?
C31 W C30 O4 -153(22) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4051h
_database_code_depnum_ccdc_archive 'CCDC 1440416'
_audit_update_record             
;
2015-12-03 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JMV-460
_chemical_formula_moiety         'C32 H29 N2 O6 P W'
_chemical_formula_sum            'C32 H29 N2 O6 P W'
_chemical_formula_weight         752.39
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5330(5)
_cell_length_b                   10.1180(5)
_cell_length_c                   17.1899(8)
_cell_angle_alpha                96.245(3)
_cell_angle_beta                 104.796(3)
_cell_angle_gamma                103.755(3)
_cell_volume                     1531.52(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4748
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.970
_cell_measurement_theta_min      2.857
_shelx_estimated_absorpt_T_max   0.861
_shelx_estimated_absorpt_T_min   0.654
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8377.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_unetI/netI     0.2368
_diffrn_reflns_Laue_measured_fraction_full 0.868
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10946
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.634
_diffrn_ambient_temperature      100
_diffrn_detector                 'ApexII detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2918
_reflns_number_total             4823
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.986
_refine_diff_density_min         -3.468
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4823
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0399P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1130
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
W W 0.74942(5) 0.55606(4) 0.33673(3) 0.02273(17) Uani 1 1 d . . . . .
P P 0.6489(3) 0.3147(3) 0.25497(15) 0.0200(7) Uani 1 1 d . . . . .
O1 O 0.3273(7) 0.2692(7) 0.2024(4) 0.0272(17) Uani 1 1 d . . . . .
O2 O 0.8665(9) 0.8599(7) 0.4404(4) 0.046(2) Uani 1 1 d . . . . .
O3 O 0.4175(9) 0.5326(8) 0.3499(5) 0.055(2) Uani 1 1 d . . . . .
O4 O 0.6670(9) 0.6628(7) 0.1677(5) 0.043(2) Uani 1 1 d . . . . .
O5 O 1.0818(9) 0.5975(8) 0.3172(4) 0.036(2) Uani 1 1 d . . . . .
O6 O 0.8401(8) 0.4781(7) 0.5145(4) 0.036(2) Uani 1 1 d . . . . .
N1 N 0.4840(9) 0.2912(8) 0.1181(5) 0.022(2) Uani 1 1 d . U . . .
N2 N 0.7299(9) 0.3174(8) 0.0986(5) 0.023(2) Uani 1 1 d . U . . .
C1 C 0.4459(11) 0.2840(10) 0.1869(6) 0.023(3) Uani 1 1 d . U . . .
C2 C 0.6452(11) 0.3057(9) 0.1441(6) 0.020(2) Uani 1 1 d . . . . .
C3 C 0.3952(11) 0.2959(10) 0.0363(5) 0.023(3) Uani 1 1 d . . . . .
H3 H 0.4651 0.3140 0.0017 0.027 Uiso 1 1 calc R . . . .
C4 C 0.3233(12) 0.4146(10) 0.0399(6) 0.031(3) Uani 1 1 d . . . . .
H4A H 0.2372 0.3888 0.0617 0.046 Uiso 1 1 calc GR . . . .
H4B H 0.2887 0.4343 -0.0152 0.046 Uiso 1 1 calc GR . . . .
H4C H 0.3979 0.4970 0.0755 0.046 Uiso 1 1 calc GR . . . .
C5 C 0.2795(11) 0.1579(10) -0.0014(6) 0.030(3) Uani 1 1 d . . . . .
H5A H 0.3306 0.0845 -0.0013 0.045 Uiso 1 1 calc GR . . . .
H5B H 0.2257 0.1602 -0.0578 0.045 Uiso 1 1 calc GR . . . .
H5C H 0.2074 0.1396 0.0304 0.045 Uiso 1 1 calc GR . . . .
C6 C 0.8926(11) 0.3341(10) 0.1382(6) 0.023(3) Uani 1 1 d . . . . .
H6 H 0.9113 0.3400 0.1986 0.027 Uiso 1 1 calc R . . . .
C7 C 0.9804(11) 0.4696(10) 0.1206(6) 0.028(3) Uani 1 1 d . U . . .
H7A H 0.9603 0.4642 0.0613 0.042 Uiso 1 1 calc GR . . . .
H7B H 1.0887 0.4847 0.1459 0.042 Uiso 1 1 calc GR . . . .
H7C H 0.9482 0.5467 0.1431 0.042 Uiso 1 1 calc GR . . . .
C8 C 0.9393(12) 0.2112(10) 0.1036(6) 0.031(3) Uani 1 1 d . . . . .
H8A H 0.8825 0.1261 0.1162 0.046 Uiso 1 1 calc GR . . . .
H8B H 1.0476 0.2250 0.1282 0.046 Uiso 1 1 calc GR . . . .
H8C H 0.9176 0.2037 0.0442 0.046 Uiso 1 1 calc GR . . . .
C9 C 0.6639(11) 0.1434(10) 0.2938(5) 0.024(3) Uani 1 1 d . . . . .
C10 C 0.5348(10) 0.0240(10) 0.2367(6) 0.018(2) Uani 1 1 d . . . . .
C11 C 0.5209(11) -0.0098(10) 0.1523(6) 0.024(3) Uani 1 1 d . U . . .
H11 H 0.5899 0.0455 0.1294 0.029 Uiso 1 1 calc R . . . .
C12 C 0.4070(11) -0.1233(10) 0.1023(6) 0.026(3) Uani 1 1 d . . . . .
H12 H 0.3983 -0.1428 0.0457 0.031 Uiso 1 1 calc R . . . .
C13 C 0.3080(12) -0.2070(11) 0.1334(6) 0.034(3) Uani 1 1 d . . . . .
H13 H 0.2316 -0.2843 0.0989 0.041 Uiso 1 1 calc R . . . .
C14 C 0.3206(12) -0.1770(11) 0.2167(6) 0.033(3) Uani 1 1 d . U . . .
H14 H 0.2525 -0.2346 0.2390 0.040 Uiso 1 1 calc R . . . .
C15 C 0.4306(11) -0.0652(11) 0.2663(6) 0.028(3) Uani 1 1 d . . . . .
H15 H 0.4370 -0.0470 0.3227 0.033 Uiso 1 1 calc R . . . .
C16 C 0.8196(11) 0.1222(10) 0.2955(6) 0.018(2) Uani 1 1 d . . . . .
C17 C 0.8347(12) -0.0018(11) 0.2624(6) 0.028(3) Uani 1 1 d . U . . .
H17 H 0.7473 -0.0764 0.2362 0.033 Uiso 1 1 calc R . . . .
C18 C 0.9778(12) -0.0185(11) 0.2671(6) 0.029(3) Uani 1 1 d . . . . .
H18 H 0.9871 -0.1049 0.2445 0.035 Uiso 1 1 calc R . . . .
C19 C 1.1035(12) 0.0873(11) 0.3038(6) 0.031(3) Uani 1 1 d . . . . .
H19 H 1.2003 0.0752 0.3061 0.037 Uiso 1 1 calc R . . . .
C20 C 1.0914(13) 0.2128(11) 0.3376(6) 0.031(3) Uani 1 1 d . . . . .
H20 H 1.1794 0.2875 0.3626 0.038 Uiso 1 1 calc R . . . .
C21 C 0.9505(11) 0.2291(10) 0.3350(5) 0.022(3) Uani 1 1 d . . . . .
H21 H 0.9425 0.3141 0.3604 0.026 Uiso 1 1 calc R . . . .
C22 C 0.6437(11) 0.1674(9) 0.3792(6) 0.020(2) Uani 1 1 d . . . . .
C23 C 0.7366(11) 0.1304(9) 0.4459(6) 0.019(2) Uani 1 1 d . U . . .
H23 H 0.8177 0.0959 0.4388 0.023 Uiso 1 1 calc R . . . .
C24 C 0.7117(12) 0.1434(10) 0.5223(6) 0.026(3) Uani 1 1 d . . . . .
H24 H 0.7743 0.1170 0.5670 0.031 Uiso 1 1 calc R . . . .
C25 C 0.5934(12) 0.1959(11) 0.5323(6) 0.030(3) Uani 1 1 d . . . . .
H25 H 0.5769 0.2057 0.5846 0.036 Uiso 1 1 calc R . . . .
C26 C 0.4995(12) 0.2340(10) 0.4684(6) 0.026(3) Uani 1 1 d . . . . .
H26 H 0.4205 0.2707 0.4767 0.031 Uiso 1 1 calc R . . . .
C27 C 0.5234(11) 0.2174(9) 0.3916(6) 0.022(3) Uani 1 1 d . . . . .
H27 H 0.4574 0.2402 0.3468 0.026 Uiso 1 1 calc R . . . .
C28 C 0.8236(13) 0.7481(12) 0.4017(6) 0.034(3) Uani 1 1 d . U . . .
C29 C 0.5370(14) 0.5383(11) 0.3446(6) 0.036(3) Uani 1 1 d . . . . .
C30 C 0.6962(12) 0.6246(10) 0.2300(7) 0.030(3) Uani 1 1 d . . . . .
C31 C 0.9620(13) 0.5773(11) 0.3249(6) 0.026(3) Uani 1 1 d . . . . .
C32 C 0.8050(12) 0.4998(10) 0.4472(7) 0.027(3) 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
W P 2.512(3) . ?
W C28 1.999(12) . ?
W C29 2.031(13) . ?
W C30 2.018(12) . ?
W C31 2.051(12) . ?
W C32 2.019(12) . ?
P C1 1.921(10) . ?
P C2 1.889(9) . ?
P C9 1.948(10) . ?
O1 C1 1.206(10) . ?
O2 C28 1.169(11) . ?
O3 C29 1.155(12) . ?
O4 C30 1.167(11) . ?
O5 C31 1.155(12) . ?
O6 C32 1.180(11) . ?
N1 C1 1.328(11) . ?
N1 C2 1.453(12) . ?
N1 C3 1.456(11) . ?
N2 C2 1.255(11) . ?
N2 C6 1.486(12) . ?
C3 H3 1.0000 . ?
C3 C4 1.520(13) . ?
C3 C5 1.514(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6 1.0000 . ?
C6 C7 1.532(12) . ?
C6 C8 1.528(13) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.535(13) . ?
C9 C16 1.543(13) . ?
C9 C22 1.531(12) . ?
C10 C11 1.418(12) . ?
C10 C15 1.412(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.367(12) . ?
C13 H13 0.9500 . ?
C13 C14 1.399(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.370(13) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(13) . ?
C16 C21 1.398(12) . ?
C17 H17 0.9500 . ?
C17 C18 1.398(13) . ?
C18 H18 0.9500 . ?
C18 C19 1.356(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.381(14) . ?
C20 H20 0.9500 . ?
C20 C21 1.382(14) . ?
C21 H21 0.9500 . ?
C22 C23 1.405(12) . ?
C22 C27 1.412(13) . ?
C23 H23 0.9500 . ?
C23 C24 1.390(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.396(14) . ?
C25 H25 0.9500 . ?
C25 C26 1.381(14) . ?
C26 H26 0.9500 . ?
C26 C27 1.395(12) . ?
C27 H27 0.9500 . ?

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
C28 W P 178.4(3) . . ?
C28 W C29 91.6(4) . . ?
C28 W C30 92.3(4) . . ?
C28 W C31 88.3(4) . . ?
C28 W C32 84.1(4) . . ?
C29 W P 86.8(3) . . ?
C29 W C31 177.8(4) . . ?
C30 W P 87.5(3) . . ?
C30 W C29 90.2(4) . . ?
C30 W C31 87.7(4) . . ?
C30 W C32 176.4(4) . . ?
C31 W P 93.3(3) . . ?
C32 W P 96.1(3) . . ?
C32 W C29 89.4(4) . . ?
C32 W C31 92.8(4) . . ?
C1 P W 110.9(3) . . ?
C1 P C9 107.6(4) . . ?
C2 P W 113.6(3) . . ?
C2 P C1 69.8(4) . . ?
C2 P C9 112.5(4) . . ?
C9 P W 127.5(3) . . ?
C1 N1 C2 103.1(8) . . ?
C1 N1 C3 130.7(9) . . ?
C2 N1 C3 126.0(7) . . ?
C2 N2 C6 116.7(8) . . ?
O1 C1 P 132.1(8) . . ?
O1 C1 N1 133.0(10) . . ?
N1 C1 P 94.8(6) . . ?
N1 C2 P 92.1(6) . . ?
N2 C2 P 142.2(8) . . ?
N2 C2 N1 125.5(9) . . ?
N1 C3 H3 108.1 . . ?
N1 C3 C4 109.8(7) . . ?
N1 C3 C5 110.3(8) . . ?
C4 C3 H3 108.1 . . ?
C5 C3 H3 108.1 . . ?
C5 C3 C4 112.4(8) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6 109.6 . . ?
N2 C6 C7 106.9(8) . . ?
N2 C6 C8 110.0(8) . . ?
C7 C6 H6 109.6 . . ?
C8 C6 H6 109.6 . . ?
C8 C6 C7 111.0(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P 108.5(6) . . ?
C10 C9 C16 111.6(8) . . ?
C16 C9 P 109.2(6) . . ?
C22 C9 P 103.2(6) . . ?
C22 C9 C10 111.2(7) . . ?
C22 C9 C16 112.7(8) . . ?
C11 C10 C9 121.7(8) . . ?
C15 C10 C9 121.9(8) . . ?
C15 C10 C11 116.2(8) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.7(9) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.3(9) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 120.4 . . ?
C12 C13 C14 119.1(9) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.3(9) . . ?
C15 C14 H14 119.8 . . ?
C10 C15 H15 118.8 . . ?
C14 C15 C10 122.4(9) . . ?
C14 C15 H15 118.8 . . ?
C17 C16 C9 121.9(9) . . ?
C17 C16 C21 118.4(9) . . ?
C21 C16 C9 119.7(8) . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.4(9) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.5(9) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(10) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.6(10) . . ?
C21 C20 H20 120.2 . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.9(9) . . ?
C20 C21 H21 119.6 . . ?
C23 C22 C9 121.0(9) . . ?
C23 C22 C27 118.2(9) . . ?
C27 C22 C9 120.6(9) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 121.0(9) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.9(9) . . ?
C25 C24 H24 120.6 . . ?
C24 C25 H25 119.0 . . ?
C26 C25 C24 122.0(9) . . ?
C26 C25 H25 119.0 . . ?
C25 C26 H26 120.7 . . ?
C25 C26 C27 118.6(10) . . ?
C27 C26 H26 120.7 . . ?
C22 C27 H27 119.4 . . ?
C26 C27 C22 121.3(9) . . ?
C26 C27 H27 119.4 . . ?
O2 C28 W 179.3(9) . . ?
O3 C29 W 177.9(10) . . ?
O4 C30 W 178.7(10) . . ?
O5 C31 W 175.7(10) . . ?
O6 C32 W 174.5(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P C2 N1 -101.7(5) . . . . ?
W P C2 N2 71.8(13) . . . . ?
P C9 C10 C11 61.3(10) . . . . ?
P C9 C10 C15 -123.9(9) . . . . ?
P C9 C16 C17 -131.9(8) . . . . ?
P C9 C16 C21 51.2(10) . . . . ?
P C9 C22 C23 -136.2(8) . . . . ?
P C9 C22 C27 48.8(10) . . . . ?
C1 P C2 N1 3.1(5) . . . . ?
C1 P C2 N2 176.6(14) . . . . ?
C1 N1 C2 P -4.3(7) . . . . ?
C1 N1 C2 N2 -179.4(9) . . . . ?
C1 N1 C3 C4 54.8(13) . . . . ?
C1 N1 C3 C5 -69.6(12) . . . . ?
C2 N1 C1 P 4.2(7) . . . . ?
C2 N1 C1 O1 -178.5(11) . . . . ?
C2 N1 C3 C4 -119.5(10) . . . . ?
C2 N1 C3 C5 116.1(10) . . . . ?
C2 N2 C6 C7 -122.7(9) . . . . ?
C2 N2 C6 C8 116.7(9) . . . . ?
C3 N1 C1 P -171.0(8) . . . . ?
C3 N1 C1 O1 6.2(18) . . . . ?
C3 N1 C2 P 171.3(8) . . . . ?
C3 N1 C2 N2 -3.8(15) . . . . ?
C6 N2 C2 P 6.7(17) . . . . ?
C6 N2 C2 N1 178.7(8) . . . . ?
C9 P C2 N1 104.4(6) . . . . ?
C9 P C2 N2 -82.1(13) . . . . ?
C9 C10 C11 C12 176.7(9) . . . . ?
C9 C10 C15 C14 -176.0(9) . . . . ?
C9 C16 C17 C18 -178.1(8) . . . . ?
C9 C16 C21 C20 179.9(9) . . . . ?
C9 C22 C23 C24 -175.6(8) . . . . ?
C9 C22 C27 C26 177.1(8) . . . . ?
C10 C9 C16 C17 -12.0(12) . . . . ?
C10 C9 C16 C21 171.1(8) . . . . ?
C10 C9 C22 C23 107.7(10) . . . . ?
C10 C9 C22 C27 -67.3(11) . . . . ?
C10 C11 C12 C13 -1.5(15) . . . . ?
C11 C10 C15 C14 -0.9(14) . . . . ?
C11 C12 C13 C14 0.6(16) . . . . ?
C12 C13 C14 C15 0.2(15) . . . . ?
C13 C14 C15 C10 0.0(16) . . . . ?
C15 C10 C11 C12 1.6(14) . . . . ?
C16 C9 C10 C11 -59.1(11) . . . . ?
C16 C9 C10 C15 115.7(10) . . . . ?
C16 C9 C22 C23 -18.5(12) . . . . ?
C16 C9 C22 C27 166.5(8) . . . . ?
C16 C17 C18 C19 -0.5(15) . . . . ?
C17 C16 C21 C20 2.9(14) . . . . ?
C17 C18 C19 C20 0.7(15) . . . . ?
C18 C19 C20 C21 1.0(15) . . . . ?
C19 C20 C21 C16 -2.7(15) . . . . ?
C21 C16 C17 C18 -1.2(14) . . . . ?
C22 C9 C10 C11 174.1(9) . . . . ?
C22 C9 C10 C15 -11.1(13) . . . . ?
C22 C9 C16 C17 114.0(10) . . . . ?
C22 C9 C16 C21 -62.9(11) . . . . ?
C22 C23 C24 C25 -0.9(14) . . . . ?
C23 C22 C27 C26 2.0(13) . . . . ?
C23 C24 C25 C26 0.6(15) . . . . ?
C24 C25 C26 C27 0.9(15) . . . . ?
C25 C26 C27 C22 -2.2(14) . . . . ?
C27 C22 C23 C24 -0.4(13) . . . . ?

_olex2_submission_original_sample_id JMV-460
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4100f
_database_code_depnum_ccdc_archive 'CCDC 1440417'
_audit_update_record             
;
2015-12-03 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_audit_creation_date             2015-12-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JMV474
_chemical_formula_moiety         'C29 H24 N O5 P W'
_chemical_formula_sum            'C29 H24 N O5 P W'
_chemical_formula_weight         681.31
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   13.1709(10)
_cell_length_b                   13.0975(9)
_cell_length_c                   15.6670(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.408(2)
_cell_angle_gamma                90
_cell_volume                     2701.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.958
_cell_measurement_theta_min      2.193
_shelx_estimated_absorpt_T_max   0.475
_shelx_estimated_absorpt_T_min   0.420
_exptl_absorpt_coefficient_mu    4.373
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.6326.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26296
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         3.727
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker KappaApex-II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5797
_reflns_number_total             6501
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6501
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0128P)²+1.4734P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0473
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
W W 0.92517(2) 0.79174(2) 0.51987(2) 0.01477(4) Uani 1 1 d . . . . .
P P 0.76694(5) 0.73148(5) 0.60101(4) 0.01523(13) Uani 1 1 d . . . . .
O1 O 1.13226(15) 0.86584(14) 0.44727(13) 0.0312(5) Uani 1 1 d . . . . .
O2 O 0.95165(15) 0.96009(14) 0.66571(12) 0.0291(4) Uani 1 1 d . . . . .
O3 O 0.80809(16) 0.95774(15) 0.40582(13) 0.0347(5) Uani 1 1 d . . . . .
O4 O 0.89519(14) 0.62900(14) 0.37010(11) 0.0243(4) Uani 1 1 d . . . . .
O5 O 1.05290(16) 0.63092(16) 0.63017(13) 0.0354(5) Uani 1 1 d . . . . .
N N 0.65728(17) 0.92267(16) 0.61250(15) 0.0251(5) Uani 1 1 d . . . . .
C1 C 0.69671(19) 0.84446(19) 0.60485(16) 0.0188(5) Uani 1 1 d . . . . .
C2 C 0.60885(19) 1.01474(18) 0.64511(16) 0.0194(5) Uani 1 1 d . . . . .
C3 C 0.6825(2) 1.0605(2) 0.71026(18) 0.0324(7) Uani 1 1 d . . . . .
H3A H 0.6961 1.0110 0.7560 0.049 Uiso 1 1 calc GR . . . .
H3B H 0.6529 1.1225 0.7344 0.049 Uiso 1 1 calc GR . . . .
H3C H 0.7462 1.0777 0.6826 0.049 Uiso 1 1 calc GR . . . .
C4 C 0.5932(3) 1.0888(2) 0.57159(19) 0.0357(7) Uani 1 1 d . . . . .
H4A H 0.6588 1.1043 0.5464 0.054 Uiso 1 1 calc GR . . . .
H4B H 0.5627 1.1519 0.5927 0.054 Uiso 1 1 calc GR . . . .
H4C H 0.5479 1.0581 0.5282 0.054 Uiso 1 1 calc GR . . . .
C5 C 0.5101(2) 0.9804(2) 0.6842(2) 0.0338(7) Uani 1 1 d . . . . .
H5A H 0.4666 0.9485 0.6401 0.051 Uiso 1 1 calc GR . . . .
H5B H 0.4751 1.0397 0.7079 0.051 Uiso 1 1 calc GR . . . .
H5C H 0.5248 0.9310 0.7298 0.051 Uiso 1 1 calc GR . . . .
C6 C 0.66177(17) 0.64228(17) 0.55245(14) 0.0138(5) Uani 1 1 d . . . . .
C7 C 0.56228(18) 0.67277(17) 0.59405(15) 0.0146(5) Uani 1 1 d . . . . .
C8 C 0.5575(2) 0.67675(18) 0.68341(16) 0.0182(5) Uani 1 1 d . . . . .
H8 H 0.6168 0.6631 0.7172 0.022 Uiso 1 1 calc R . . . .
C9 C 0.4677(2) 0.70022(19) 0.72303(17) 0.0235(6) Uani 1 1 d . . . . .
H9 H 0.4659 0.7021 0.7836 0.028 Uiso 1 1 calc R . . . .
C10 C 0.3805(2) 0.72095(19) 0.67512(19) 0.0273(6) Uani 1 1 d . . . . .
H10 H 0.3191 0.7375 0.7026 0.033 Uiso 1 1 calc R . . . .
C11 C 0.3833(2) 0.71744(19) 0.58740(18) 0.0236(6) Uani 1 1 d . . . . .
H11 H 0.3238 0.7319 0.5542 0.028 Uiso 1 1 calc R . . . .
C12 C 0.47375(19) 0.69262(17) 0.54704(16) 0.0179(5) Uani 1 1 d . . . . .
H12 H 0.4745 0.6893 0.4865 0.021 Uiso 1 1 calc R . . . .
C13 C 0.65543(17) 0.64912(18) 0.45449(14) 0.0147(5) Uani 1 1 d . . . . .
C14 C 0.65091(18) 0.74381(19) 0.41307(16) 0.0175(5) Uani 1 1 d . . . . .
H14 H 0.6526 0.8047 0.4460 0.021 Uiso 1 1 calc R . . . .
C15 C 0.64403(19) 0.7501(2) 0.32542(16) 0.0204(5) Uani 1 1 d . . . . .
H15 H 0.6414 0.8152 0.2986 0.024 Uiso 1 1 calc R . . . .
C16 C 0.64094(19) 0.6620(2) 0.27576(16) 0.0220(6) Uani 1 1 d . . . . .
H16 H 0.6368 0.6665 0.2153 0.026 Uiso 1 1 calc R . . . .
C17 C 0.64402(19) 0.5681(2) 0.31560(16) 0.0206(5) Uani 1 1 d . . . . .
H17 H 0.6414 0.5075 0.2823 0.025 Uiso 1 1 calc R . . . .
C18 C 0.65089(18) 0.56170(19) 0.40418(15) 0.0176(5) Uani 1 1 d . . . . .
H18 H 0.6525 0.4965 0.4307 0.021 Uiso 1 1 calc R . . . .
C19 C 0.69587(18) 0.53522(18) 0.58155(14) 0.0144(5) Uani 1 1 d . . . . .
C20 C 0.63241(19) 0.46967(18) 0.62586(15) 0.0171(5) Uani 1 1 d . . . . .
H20 H 0.5653 0.4907 0.6380 0.020 Uiso 1 1 calc R . . . .
C21 C 0.6660(2) 0.37424(19) 0.65246(16) 0.0217(5) Uani 1 1 d . . . . .
H21 H 0.6218 0.3311 0.6831 0.026 Uiso 1 1 calc R . . . .
C22 C 0.7633(2) 0.34092(19) 0.63497(16) 0.0223(6) Uani 1 1 d . . . . .
H22 H 0.7864 0.2760 0.6543 0.027 Uiso 1 1 calc R . . . .
C23 C 0.8264(2) 0.40417(19) 0.58874(16) 0.0213(5) Uani 1 1 d . . . . .
H23 H 0.8926 0.3818 0.5750 0.026 Uiso 1 1 calc R . . . .
C24 C 0.79294(19) 0.49973(18) 0.56268(15) 0.0180(5) Uani 1 1 d . . . . .
H24 H 0.8370 0.5422 0.5312 0.022 Uiso 1 1 calc R . . . .
C25 C 1.0560(2) 0.83864(19) 0.47266(16) 0.0209(5) Uani 1 1 d . . . . .
C26 C 0.94177(19) 0.89877(19) 0.61401(16) 0.0196(5) Uani 1 1 d . . . . .
C27 C 0.8479(2) 0.89767(19) 0.44742(16) 0.0214(5) Uani 1 1 d . . . . .
C28 C 0.90459(19) 0.68699(19) 0.42393(16) 0.0187(5) Uani 1 1 d . . . . .
C29 C 1.0056(2) 0.6878(2) 0.59127(17) 0.0215(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
W P 2.5908(6) . ?
W C25 1.989(3) . ?
W C26 2.043(3) . ?
W C27 2.047(3) . ?
W C28 2.048(3) . ?
W C29 2.041(3) . ?
P C1 1.747(3) . ?
P C6 1.952(2) . ?
O1 C25 1.147(3) . ?
O2 C26 1.146(3) . ?
O3 C27 1.141(3) . ?
O4 C28 1.139(3) . ?
O5 C29 1.139(3) . ?
N C1 1.156(3) . ?
N C2 1.462(3) . ?
C2 C3 1.515(4) . ?
C2 C4 1.516(4) . ?
C2 C5 1.520(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.531(3) . ?
C6 C13 1.538(3) . ?
C6 C19 1.538(3) . ?
C7 C8 1.404(3) . ?
C7 C12 1.388(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.376(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.400(3) . ?
C13 C18 1.391(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.376(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.392(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.379(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(3) . ?
C19 C24 1.399(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.386(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(3) . ?
C24 H24 0.9500 . ?

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
C25 W P 172.40(8) . . ?
C25 W C26 88.76(10) . . ?
C25 W C27 90.44(10) . . ?
C25 W C28 91.96(10) . . ?
C25 W C29 88.12(11) . . ?
C26 W P 85.86(7) . . ?
C26 W C27 88.75(10) . . ?
C26 W C28 178.16(10) . . ?
C27 W P 94.81(7) . . ?
C27 W C28 89.55(10) . . ?
C28 W P 93.58(7) . . ?
C29 W P 86.61(8) . . ?
C29 W C26 90.97(10) . . ?
C29 W C27 178.53(10) . . ?
C29 W C28 90.75(10) . . ?
C1 P W 101.06(8) . . ?
C1 P C6 98.58(11) . . ?
C6 P W 124.25(7) . . ?
C1 N C2 165.5(3) . . ?
N C1 P 173.6(2) . . ?
N C2 C3 106.5(2) . . ?
N C2 C4 108.4(2) . . ?
N C2 C5 106.4(2) . . ?
C3 C2 C4 109.4(2) . . ?
C3 C2 C5 112.7(2) . . ?
C4 C2 C5 113.2(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 P 106.54(15) . . ?
C7 C6 C13 112.56(19) . . ?
C7 C6 C19 111.00(19) . . ?
C13 C6 P 112.01(15) . . ?
C13 C6 C19 110.93(18) . . ?
C19 C6 P 103.35(15) . . ?
C8 C7 C6 119.6(2) . . ?
C12 C7 C6 122.7(2) . . ?
C12 C7 C8 117.7(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.5(3) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.2 . . ?
C11 C10 C9 119.5(2) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 121.1(2) . . ?
C7 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C6 121.0(2) . . ?
C18 C13 C6 121.2(2) . . ?
C18 C13 C14 117.8(2) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.1(2) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.5(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.1(2) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 121.1(2) . . ?
C13 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C20 C19 C6 122.3(2) . . ?
C20 C19 C24 117.5(2) . . ?
C24 C19 C6 120.1(2) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 120.9(2) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.9(2) . . ?
C22 C21 H21 119.6 . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.8(2) . . ?
C23 C22 H22 120.6 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C19 C24 H24 119.2 . . ?
C23 C24 C19 121.6(2) . . ?
C23 C24 H24 119.2 . . ?
O1 C25 W 178.5(2) . . ?
O2 C26 W 178.7(2) . . ?
O3 C27 W 177.6(2) . . ?
O4 C28 W 178.6(2) . . ?
O5 C29 W 178.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P C6 C7 C8 -52.9(2) . . . . ?
P C6 C7 C12 130.1(2) . . . . ?
P C6 C13 C14 -49.1(3) . . . . ?
P C6 C13 C18 132.9(2) . . . . ?
P C6 C19 C20 125.6(2) . . . . ?
P C6 C19 C24 -55.4(2) . . . . ?
C1 N C2 C3 55.5(11) . . . . ?
C1 N C2 C4 173.1(9) . . . . ?
C1 N C2 C5 -64.9(11) . . . . ?
C6 C7 C8 C9 -177.5(2) . . . . ?
C6 C7 C12 C11 178.1(2) . . . . ?
C6 C13 C14 C15 -179.2(2) . . . . ?
C6 C13 C18 C17 179.3(2) . . . . ?
C6 C19 C20 C21 -178.9(2) . . . . ?
C6 C19 C24 C23 179.3(2) . . . . ?
C7 C6 C13 C14 71.0(3) . . . . ?
C7 C6 C13 C18 -107.1(2) . . . . ?
C7 C6 C19 C20 11.8(3) . . . . ?
C7 C6 C19 C24 -169.2(2) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C8 C7 C12 C11 1.1(3) . . . . ?
C8 C9 C10 C11 0.4(4) . . . . ?
C9 C10 C11 C12 0.3(4) . . . . ?
C10 C11 C12 C7 -1.0(4) . . . . ?
C12 C7 C8 C9 -0.4(4) . . . . ?
C13 C6 C7 C8 -176.0(2) . . . . ?
C13 C6 C7 C12 6.9(3) . . . . ?
C13 C6 C19 C20 -114.2(2) . . . . ?
C13 C6 C19 C24 64.8(3) . . . . ?
C13 C14 C15 C16 0.3(4) . . . . ?
C14 C13 C18 C17 1.2(4) . . . . ?
C14 C15 C16 C17 0.5(4) . . . . ?
C15 C16 C17 C18 -0.5(4) . . . . ?
C16 C17 C18 C13 -0.4(4) . . . . ?
C18 C13 C14 C15 -1.1(4) . . . . ?
C19 C6 C7 C8 58.9(3) . . . . ?
C19 C6 C7 C12 -118.1(2) . . . . ?
C19 C6 C13 C14 -164.0(2) . . . . ?
C19 C6 C13 C18 18.0(3) . . . . ?
C19 C20 C21 C22 -0.7(4) . . . . ?
C20 C19 C24 C23 -1.7(4) . . . . ?
C20 C21 C22 C23 -1.2(4) . . . . ?
C21 C22 C23 C24 1.6(4) . . . . ?
C22 C23 C24 C19 -0.1(4) . . . . ?
C24 C19 C20 C21 2.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
