# Electronic Supplementary Material (ESI) for ChemComm.
# 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_3853f
_database_code_depnum_ccdc_archive 'CCDC 1470387'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H23 O6 P Si2 W'
_chemical_formula_weight         558.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   9.7786(5)
_cell_length_b                   9.9521(4)
_cell_length_c                   21.9977(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2140.76(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5772
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.28
_exptl_crystal_description       block
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.606
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0971 before and 0.0572 after correction.
The Ratio of minimum to maximum transmission is 0.7102.
The λ/2 correction factor is 0.00150.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0

_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            15593
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.064
_diffrn_reflns_theta_max         27.986
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5137
_reflns_number_gt                4890
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.999

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] 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 
;
 Refined as an inversion twin.
;
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5137
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0221
_refine_ls_wR_factor_ref         0.0376
_refine_ls_wR_factor_gt          0.0369
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_refine_ls_shift/su_max          0.004
_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
W W -0.09950(2) -0.01884(2) -0.81460(2) 0.01335(5) Uani 1 1 d . . . . .
P P -0.34356(12) 0.03184(12) -0.83072(4) 0.0114(2) Uani 1 1 d . . . . .
Si1 Si -0.50095(17) 0.23633(13) -0.91224(6) 0.0206(3) Uani 1 1 d . . . . .
Si2 Si -0.47290(16) -0.07814(13) -0.95074(6) 0.0191(3) Uani 1 1 d . . . . .
O1 O -0.4056(4) 0.1493(3) -0.78384(12) 0.0165(7) Uani 1 1 d . . . . .
O2 O 0.2044(4) -0.0966(4) -0.78039(16) 0.0315(9) Uani 1 1 d . . . . .
O3 O -0.0586(4) -0.0997(3) -0.95299(14) 0.0322(11) Uani 1 1 d . . . . .
O4 O -0.1825(4) -0.3222(4) -0.78811(16) 0.0320(10) Uani 1 1 d . . . . .
O5 O -0.1536(4) 0.0714(4) -0.67728(13) 0.0322(9) Uani 1 1 d . . . . .
O6 O -0.0261(4) 0.2865(3) -0.84552(15) 0.0284(9) Uani 1 1 d . . . . .
C1 C -0.4849(5) 0.0527(5) -0.74828(19) 0.0218(12) Uani 1 1 d . . . . .
H1A H -0.5810 0.0816 -0.7429 0.026 Uiso 1 1 calc R U . . .
H1B H -0.4431 0.0349 -0.7081 0.026 Uiso 1 1 calc R U . . .
C2 C -0.4727(5) -0.0683(5) -0.79104(19) 0.0168(11) Uani 1 1 d . . . . .
H2A H -0.5559 -0.0870 -0.8152 0.020 Uiso 1 1 calc R U . . .
H2B H -0.4369 -0.1508 -0.7716 0.020 Uiso 1 1 calc R U . . .
C3 C -0.4012(6) 0.0726(4) -0.90669(16) 0.0136(9) Uani 1 1 d . . . . .
H3 H -0.3143 0.0934 -0.9287 0.016 Uiso 1 1 calc R U . . .
C4 C -0.6638(5) 0.2350(5) -0.8689(2) 0.0294(13) Uani 1 1 d . . . . .
H4A H -0.7218 0.1613 -0.8834 0.044 Uiso 1 1 calc R U . . .
H4B H -0.6443 0.2223 -0.8255 0.044 Uiso 1 1 calc R U . . .
H4C H -0.7114 0.3207 -0.8747 0.044 Uiso 1 1 calc R U . . .
C5 C -0.3863(7) 0.3749(4) -0.8864(2) 0.0305(14) Uani 1 1 d . . . . .
H5A H -0.3014 0.3731 -0.9101 0.046 Uiso 1 1 calc R U . . .
H5B H -0.4323 0.4614 -0.8924 0.046 Uiso 1 1 calc R U . . .
H5C H -0.3651 0.3630 -0.8432 0.046 Uiso 1 1 calc R U . . .
C6 C -0.5429(7) 0.2677(5) -0.9942(2) 0.0384(17) Uani 1 1 d . . . . .
H6A H -0.4584 0.2689 -1.0181 0.058 Uiso 1 1 calc R U . . .
H6B H -0.6030 0.1961 -1.0092 0.058 Uiso 1 1 calc R U . . .
H6C H -0.5894 0.3545 -0.9982 0.058 Uiso 1 1 calc R U . . .
C7 C -0.6627(6) -0.0870(6) -0.9482(2) 0.0310(14) Uani 1 1 d . . . . .
H7A H -0.7013 -0.0031 -0.9640 0.046 Uiso 1 1 calc R U . . .
H7B H -0.6942 -0.1625 -0.9732 0.046 Uiso 1 1 calc R U . . .
H7C H -0.6927 -0.1001 -0.9061 0.046 Uiso 1 1 calc R U . . .
C8 C -0.4121(7) -0.0608(5) -1.03081(17) 0.0316(14) Uani 1 1 d . . . . .
H8A H -0.3120 -0.0563 -1.0313 0.047 Uiso 1 1 calc R U . . .
H8B H -0.4425 -0.1386 -1.0546 0.047 Uiso 1 1 calc R U . . .
H8C H -0.4499 0.0215 -1.0486 0.047 Uiso 1 1 calc R U . . .
C9 C -0.4056(7) -0.2401(4) -0.92019(18) 0.0248(12) Uani 1 1 d . . . . .
H9A H -0.3054 -0.2385 -0.9209 0.037 Uiso 1 1 calc R U . . .
H9B H -0.4373 -0.2522 -0.8783 0.037 Uiso 1 1 calc R U . . .
H9C H -0.4387 -0.3146 -0.9453 0.037 Uiso 1 1 calc R U . . .
C10 C 0.0961(6) -0.0661(5) -0.7940(2) 0.0215(10) Uani 1 1 d . . . . .
C11 C -0.0725(5) -0.0700(4) -0.9029(2) 0.0198(12) Uani 1 1 d . . . . .
C12 C -0.1518(5) -0.2121(5) -0.7970(2) 0.0208(11) Uani 1 1 d . . . . .
C13 C -0.1334(5) 0.0379(5) -0.7260(2) 0.0209(11) Uani 1 1 d . . . . .
C14 C -0.0522(5) 0.1775(5) -0.83468(19) 0.0192(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
W C10 2.022(6) . ?
W C11 2.025(5) . ?
W C12 2.028(5) . ?
W C14 2.056(5) . ?
W C13 2.056(5) . ?
W P 2.4649(12) . ?
P O1 1.672(3) . ?
P C3 1.810(4) . ?
P C2 1.830(5) . ?
Si1 C4 1.857(5) . ?
Si1 C5 1.866(5) . ?
Si1 C6 1.876(5) . ?
Si1 C3 1.903(5) . ?
Si2 C7 1.859(6) . ?
Si2 C9 1.866(5) . ?
Si2 C8 1.867(4) . ?
Si2 C3 1.918(4) . ?
O1 C1 1.462(5) . ?
O2 C10 1.141(6) . ?
O3 C11 1.149(5) . ?
O4 C12 1.153(6) . ?
O5 C13 1.140(5) . ?
O6 C14 1.140(5) . ?
C1 C2 1.532(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 1.0000 . ?
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 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?

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
C10 W C11 91.91(19) . . ?
C10 W C12 88.6(2) . . ?
C11 W C12 88.69(18) . . ?
C10 W C14 93.2(2) . . ?
C11 W C14 90.19(17) . . ?
C12 W C14 177.9(2) . . ?
C10 W C13 90.21(18) . . ?
C11 W C13 177.7(2) . . ?
C12 W C13 92.26(19) . . ?
C14 W C13 88.80(18) . . ?
C10 W P 174.95(13) . . ?
C11 W P 92.28(15) . . ?
C12 W P 88.71(15) . . ?
C14 W P 89.58(15) . . ?
C13 W P 85.66(13) . . ?
O1 P C3 107.44(18) . . ?
O1 P C2 80.57(19) . . ?
C3 P C2 110.3(2) . . ?
O1 P W 113.91(14) . . ?
C3 P W 118.72(18) . . ?
C2 P W 119.22(17) . . ?
C4 Si1 C5 111.3(3) . . ?
C4 Si1 C6 107.9(3) . . ?
C5 Si1 C6 107.5(3) . . ?
C4 Si1 C3 113.6(2) . . ?
C5 Si1 C3 107.8(2) . . ?
C6 Si1 C3 108.5(2) . . ?
C7 Si2 C9 107.5(3) . . ?
C7 Si2 C8 110.5(3) . . ?
C9 Si2 C8 107.9(2) . . ?
C7 Si2 C3 112.7(2) . . ?
C9 Si2 C3 111.4(2) . . ?
C8 Si2 C3 106.7(2) . . ?
C1 O1 P 93.6(2) . . ?
O1 C1 C2 98.4(3) . . ?
O1 C1 H1A 112.1 . . ?
C2 C1 H1A 112.1 . . ?
O1 C1 H1B 112.1 . . ?
C2 C1 H1B 112.1 . . ?
H1A C1 H1B 109.7 . . ?
C1 C2 P 85.4(3) . . ?
C1 C2 H2A 114.4 . . ?
P C2 H2A 114.4 . . ?
C1 C2 H2B 114.4 . . ?
P C2 H2B 114.4 . . ?
H2A C2 H2B 111.5 . . ?
P C3 Si1 114.3(2) . . ?
P C3 Si2 113.9(2) . . ?
Si1 C3 Si2 116.7(3) . . ?
P C3 H3 103.2 . . ?
Si1 C3 H3 103.2 . . ?
Si2 C3 H3 103.2 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 W 177.0(4) . . ?
O3 C11 W 179.2(5) . . ?
O4 C12 W 178.7(4) . . ?
O5 C13 W 178.7(4) . . ?
O6 C14 W 179.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 P O1 C1 118.7(3) . . . . ?
C2 P O1 C1 10.2(3) . . . . ?
W P O1 C1 -107.7(3) . . . . ?
P O1 C1 C2 -12.2(3) . . . . ?
O1 C1 C2 P 11.1(3) . . . . ?
O1 P C2 C1 -9.8(3) . . . . ?
C3 P C2 C1 -115.0(3) . . . . ?
W P C2 C1 102.4(3) . . . . ?
O1 P C3 Si1 3.9(3) . . . . ?
C2 P C3 Si1 90.0(3) . . . . ?
W P C3 Si1 -127.2(2) . . . . ?
O1 P C3 Si2 -133.8(3) . . . . ?
C2 P C3 Si2 -47.7(3) . . . . ?
W P C3 Si2 95.1(3) . . . . ?

_refine_diff_density_max         0.450
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.093

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_3760f
_database_code_depnum_ccdc_archive 'CCDC 1470388'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_date             2014-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        AKY-424
_chemical_formula_moiety         'C14 H24 I O6 P Si2 W'
_chemical_formula_sum            'C14 H24 I O6 P Si2 W'
_chemical_formula_weight         686.23
_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'
I I -0.4742 1.8119 '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'
Si Si 0.0817 0.0704 '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                   9.179(3)
_cell_length_b                   10.433(4)
_cell_length_c                   14.066(5)
_cell_angle_alpha                86.293(10)
_cell_angle_beta                 81.810(10)
_cell_angle_gamma                65.584(9)
_cell_volume                     1214.0(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5405
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.59
_exptl_absorpt_coefficient_mu    6.216
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.3610
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1401 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.4840.
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    1.877
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8231
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.46
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                2777
_reflns_number_total             3734
_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    'XS (Sheldrick, 2008)'
_refine_diff_density_max         5.694
_refine_diff_density_min         -4.762
_refine_diff_density_rms         0.431
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3734
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1918
_refine_ls_R_factor_gt           0.1405
_refine_ls_restrained_S_all      1.224
_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)+(0.0001P)²+196.1710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3049
_refine_ls_wR_factor_ref         0.3359
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H
 2.4 with sigma of 0.01
 P-H
 1.43 with sigma of 0.01
3. Rigid bond restraints
 Si1, C4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq:
with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(O6) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
5.a Ternary CH refined with riding coordinates:
 C3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C5(H5A,
 H5B,H5C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
W W -0.02028(19) 0.26122(14) 0.16267(11) 0.0341(5) Uani 1 d . . . .
I I 0.4548(5) 0.2589(4) 0.4502(3) 0.0774(12) Uani 1 d . . . .
P P 0.0957(12) 0.0489(8) 0.2649(8) 0.040(2) Uani 1 d . . D .
H H -0.022(12) 0.05(4) 0.345(3) 0.048 Uiso 1 d . . DR .
Si2 Si 0.3715(12) -0.2219(9) 0.1670(8) 0.038(3) Uani 1 d . . . .
Si1 Si 0.0668(15) -0.2278(11) 0.3108(8) 0.049(3) Uani 1 d . . . U
O4 O 0.318(3) 0.292(2) 0.137(2) 0.053(8) Uani 1 d . . . .
O2 O -0.186(3) 0.545(2) 0.050(2) 0.050(8) Uani 1 d . . . .
O1 O 0.254(3) 0.022(2) 0.3165(19) 0.042(7) Uani 1 d . . D .
O5 O 0.106(3) 0.092(3) -0.036(2) 0.050(7) Uani 1 d . . . .
O3 O -0.160(4) 0.438(3) 0.3587(19) 0.065(10) Uani 1 d . . . .
O6 O -0.321(4) 0.197(3) 0.181(2) 0.069(9) Uani 1 d . . . U
C1 C 0.259(4) 0.133(3) 0.373(3) 0.034(9) Uani 1 d . . . .
H1A H 0.1973 0.2273 0.3465 0.041 Uiso 1 calc . . R .
H1B H 0.2134 0.1287 0.4408 0.041 Uiso 1 calc . . R .
C14 C -0.212(7) 0.218(5) 0.169(4) 0.065(13) Uani 1 d . . . U
C9 C 0.457(6) -0.098(4) 0.108(3) 0.055(11) Uani 1 d . . . U
H9A H 0.4589 -0.0353 0.1561 0.083 Uiso 1 calc . . GR .
H9B H 0.3904 -0.0423 0.0590 0.083 Uiso 1 calc . . GR .
H9C H 0.5674 -0.1520 0.0773 0.083 Uiso 1 calc . . GR .
C2 C 0.428(6) 0.105(5) 0.367(4) 0.070(15) Uani 1 d . . . .
H2A H 0.4717 0.1106 0.2987 0.084 Uiso 1 calc . . R .
H2B H 0.4887 0.0095 0.3912 0.084 Uiso 1 calc . . R .
C4 C -0.156(6) -0.145(5) 0.321(3) 0.063(12) Uani 1 d . . . U
H4A H -0.1897 -0.1351 0.2572 0.094 Uiso 1 calc . . GR .
H4B H -0.1954 -0.0512 0.3499 0.094 Uiso 1 calc . . GR .
H4C H -0.2000 -0.2031 0.3618 0.094 Uiso 1 calc . . GR .
C6 C 0.137(7) -0.415(5) 0.273(4) 0.074(14) Uani 1 d . . . U
H6A H 0.0511 -0.4478 0.2935 0.111 Uiso 1 calc . . GR .
H6B H 0.2329 -0.4745 0.3036 0.111 Uiso 1 calc . . GR .
H6C H 0.1637 -0.4220 0.2033 0.111 Uiso 1 calc . . GR .
C8 C 0.499(4) -0.310(4) 0.259(3) 0.047(11) Uani 1 d . . . .
H8A H 0.6044 -0.3756 0.2285 0.070 Uiso 1 calc . . GR .
H8B H 0.4486 -0.3625 0.3016 0.070 Uiso 1 calc . . GR .
H8C H 0.5122 -0.2403 0.2958 0.070 Uiso 1 calc . . GR .
C5 C 0.143(6) -0.247(5) 0.434(3) 0.060(13) Uani 1 d . . . .
H5A H 0.1113 -0.1530 0.4609 0.091 Uiso 1 calc . . GR .
H5B H 0.2614 -0.2958 0.4262 0.091 Uiso 1 calc . . GR .
H5C H 0.0967 -0.3007 0.4779 0.091 Uiso 1 calc . . GR .
C11 C -0.110(5) 0.370(4) 0.286(3) 0.042(9) Uani 1 d . . . U
C3 C 0.151(5) -0.125(3) 0.223(3) 0.035(9) Uani 1 d . . . .
H3 H 0.0880 -0.1097 0.1677 0.042 Uiso 1 calc . . R .
C10 C -0.124(4) 0.445(3) 0.085(2) 0.025(7) Uani 1 d . . . U
C7 C 0.372(5) -0.339(4) 0.071(3) 0.058(12) Uani 1 d . . . .
H7A H 0.2801 -0.2880 0.0352 0.088 Uiso 1 calc . . GR .
H7B H 0.3635 -0.4233 0.1004 0.088 Uiso 1 calc . . GR .
H7C H 0.4726 -0.3655 0.0269 0.088 Uiso 1 calc . . GR .
C13 C 0.064(5) 0.157(4) 0.038(3) 0.046(9) Uani 1 d . . . U
C12 C 0.189(5) 0.285(4) 0.154(3) 0.041(9) Uani 1 d . . . U


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.486(8) . ?
W C14 1.98(6) . ?
W C11 2.01(4) . ?
W C10 2.07(3) . ?
W C13 2.00(4) . ?
W C12 2.02(5) . ?
I C2 2.16(5) . ?
P H 1.430(10) . ?
P O1 1.63(2) . ?
P C3 1.79(3) . ?
Si2 C9 1.87(4) . ?
Si2 C8 1.81(4) . ?
Si2 C3 1.93(4) . ?
Si2 C7 1.88(5) . ?
Si1 C4 1.85(5) . ?
Si1 C6 1.88(5) . ?
Si1 C5 1.93(4) . ?
Si1 C3 1.87(4) . ?
O4 C12 1.20(5) . ?
O2 C10 1.09(3) . ?
O1 C1 1.46(4) . ?
O5 C13 1.21(5) . ?
O3 C11 1.21(4) . ?
O6 C14 1.10(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.44(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C3 H3 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 W P 87.0(14) . . ?
C14 W C11 90.8(19) . . ?
C14 W C10 92.8(16) . . ?
C14 W C13 88.3(19) . . ?
C14 W C12 174.5(17) . . ?
C11 W P 86.6(10) . . ?
C11 W C10 90.0(13) . . ?
C11 W C12 92.6(16) . . ?
C10 W P 176.5(9) . . ?
C13 W P 94.8(11) . . ?
C13 W C11 178.3(16) . . ?
C13 W C10 88.6(13) . . ?
C13 W C12 88.3(17) . . ?
C12 W P 88.9(10) . . ?
C12 W C10 91.5(14) . . ?
W P H 109(10) . . ?
O1 P W 120.0(10) . . ?
O1 P H 102.9(14) . . ?
O1 P C3 99.5(14) . . ?
C3 P W 122.5(12) . . ?
C3 P H 100(10) . . ?
C9 Si2 C3 112.3(17) . . ?
C9 Si2 C7 107(2) . . ?
C8 Si2 C9 105(2) . . ?
C8 Si2 C3 110.6(16) . . ?
C8 Si2 C7 115.4(18) . . ?
C7 Si2 C3 106.8(17) . . ?
C4 Si1 C6 108(3) . . ?
C4 Si1 C5 112(2) . . ?
C4 Si1 C3 109.1(19) . . ?
C6 Si1 C5 103(2) . . ?
C3 Si1 C6 112(2) . . ?
C3 Si1 C5 112.0(19) . . ?
C1 O1 P 120.8(18) . . ?
O1 C1 H1A 110.8 . . ?
O1 C1 H1B 110.8 . . ?
H1A C1 H1B 108.8 . . ?
C2 C1 O1 105(3) . . ?
C2 C1 H1A 110.8 . . ?
C2 C1 H1B 110.8 . . ?
O6 C14 W 174(5) . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
I C2 H2A 109.8 . . ?
I C2 H2B 109.8 . . ?
C1 C2 I 109(3) . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C11 W 177(4) . . ?
P C3 Si2 116(2) . . ?
P C3 Si1 111.8(19) . . ?
P C3 H3 103.6 . . ?
Si2 C3 H3 103.6 . . ?
Si1 C3 Si2 116.6(15) . . ?
Si1 C3 H3 103.6 . . ?
O2 C10 W 175(3) . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O5 C13 W 176(4) . . ?
O4 C12 W 171(3) . . ?

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 O1 C1 51(3) . . . . ?
W P C3 Si2 92.5(18) . . . . ?
W P C3 Si1 -130.9(13) . . . . ?
P W C14 O6 64(42) . . . . ?
P W C11 O3 108(67) . . . . ?
P W C10 O2 -25(47) . . . . ?
P W C13 O5 90(46) . . . . ?
P W C12 O4 105(19) . . . . ?
P O1 C1 C2 -152(3) . . . . ?
O1 P C3 Si2 -43(2) . . . . ?
O1 P C3 Si1 94(2) . . . . ?
O1 C1 C2 I -179(2) . . . . ?
C14 W P O1 -166.4(19) . . . . ?
C14 W P C3 67(2) . . . . ?
C14 W C11 O3 -165(67) . . . . ?
C14 W C10 O2 62(33) . . . . ?
C14 W C13 O5 3(46) . . . . ?
C14 W C12 O4 63(30) . . . . ?
C9 Si2 C3 P -30(3) . . . . ?
C9 Si2 C3 Si1 -165(2) . . . . ?
C4 Si1 C3 P 64(3) . . . . ?
C4 Si1 C3 Si2 -159(2) . . . . ?
C6 Si1 C3 P -175(2) . . . . ?
C6 Si1 C3 Si2 -39(3) . . . . ?
C8 Si2 C3 P 86(2) . . . . ?
C8 Si2 C3 Si1 -48(3) . . . . ?
C5 Si1 C3 P -60(3) . . . . ?
C5 Si1 C3 Si2 76(2) . . . . ?
C11 W P O1 -75.4(17) . . . . ?
C11 W P C3 158(2) . . . . ?
C11 W C14 O6 -23(42) . . . . ?
C11 W C10 O2 -29(33) . . . . ?
C11 W C13 O5 -56(87) . . . . ?
C11 W C12 O4 -169(19) . . . . ?
C3 P O1 C1 -172(3) . . . . ?
C10 W P O1 -80(17) . . . . ?
C10 W P C3 154(16) . . . . ?
C10 W C14 O6 -113(42) . . . . ?
C10 W C11 O3 -72(67) . . . . ?
C10 W C13 O5 -90(46) . . . . ?
C10 W C12 O4 -79(19) . . . . ?
C7 Si2 C3 P -147(2) . . . . ?
C7 Si2 C3 Si1 78(2) . . . . ?
C13 W P O1 105.5(18) . . . . ?
C13 W P C3 -21(2) . . . . ?
C13 W C14 O6 159(42) . . . . ?
C13 W C11 O3 -106(87) . . . . ?
C13 W C10 O2 150(33) . . . . ?
C13 W C12 O4 10(19) . . . . ?
C12 W P O1 17.3(16) . . . . ?
C12 W P C3 -109(2) . . . . ?
C12 W C14 O6 106(43) . . . . ?
C12 W C11 O3 19(67) . . . . ?
C12 W C10 O2 -122(33) . . . . ?
C12 W C13 O5 179(100) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

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

####################################################################### 
# 
# 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_mo_4626f
_database_code_depnum_ccdc_archive 'CCDC 1483069'
_audit_update_record             
;
2016-06-01 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;
_audit_creation_date             2016-05-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        AKY-554
_chemical_formula_moiety         'C15 H25 O6 P Si2 W'
_chemical_formula_sum            'C15 H25 O6 P Si2 W'
_chemical_formula_weight         572.35
_chemical_absolute_configuration ad
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   9.2343(4)
_cell_length_b                   10.3502(4)
_cell_length_c                   23.1652(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2214.06(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6576
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.64
_shelx_estimated_absorpt_T_max   0.773
_shelx_estimated_absorpt_T_min   0.333
_exptl_absorpt_coefficient_mu    5.422
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0962 before and 0.0663 after correction.
The Ratio of minimum to maximum transmission is 0.6352.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17907
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.639
_diffrn_ambient_temperature      123
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4514
_reflns_number_total             5344
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.887
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
##_refine_ls_abs_structure_Flack    0.503(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         5344
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0129P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0584
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.497(10) 0.503(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C)
;
_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 0.05640(3) 0.92090(3) 0.67529(2) 0.02010(8) Uani 1 1 d . . . . .
P P 0.28972(18) 0.91327(19) 0.62120(7) 0.0151(4) Uani 1 1 d . . . . .
Si1 Si 0.4555(3) 1.17638(18) 0.62815(9) 0.0217(5) Uani 1 1 d . . . . .
Si2 Si 0.4024(2) 1.0378(2) 0.50484(9) 0.0247(5) Uani 1 1 d . . . . .
O1 O 0.2861(5) 0.7990(4) 0.5722(2) 0.0216(12) Uani 1 1 d . . . . .
O2 O -0.2445(6) 0.9307(7) 0.7406(2) 0.0452(15) Uani 1 1 d . . . . .
O3 O 0.0496(7) 1.2276(5) 0.6753(2) 0.0406(13) Uani 1 1 d . . . . .
O4 O -0.0857(6) 0.9273(7) 0.5508(2) 0.0485(16) Uani 1 1 d . . . . .
O5 O 0.0440(8) 0.6137(5) 0.6709(3) 0.0527(16) Uani 1 1 d . . . . .
O6 O 0.2310(6) 0.9179(7) 0.7942(2) 0.0449(15) Uani 1 1 d . . . . .
C1 C 0.3761(9) 0.6883(7) 0.5855(3) 0.032(2) Uani 1 1 d . U . . .
H1A H 0.4551 0.6810 0.5568 0.038 Uiso 1 1 calc R . . . .
H1B H 0.3174 0.6083 0.5838 0.038 Uiso 1 1 calc R . . . .
C2 C 0.4387(12) 0.7044(7) 0.6448(4) 0.045(2) Uani 1 1 d . U . . .
H2A H 0.5349 0.6625 0.6470 0.054 Uiso 1 1 calc R . . . .
H2B H 0.3744 0.6640 0.6739 0.054 Uiso 1 1 calc R . . . .
C3 C 0.4524(9) 0.8485(6) 0.6562(3) 0.0247(16) Uani 1 1 d . . . . .
H3A H 0.5416 0.8841 0.6387 0.030 Uiso 1 1 calc R . . . .
H3B H 0.4526 0.8672 0.6981 0.030 Uiso 1 1 calc R . . . .
C4 C 0.3418(7) 1.0595(6) 0.5832(3) 0.0141(15) Uani 1 1 d . . . . .
H4 H 0.2477 1.1065 0.5791 0.017 Uiso 1 1 calc R . . . .
C5 C 0.4314(11) 1.1586(7) 0.7075(3) 0.033(2) Uani 1 1 d . . . . .
H5A H 0.3279 1.1527 0.7166 0.050 Uiso 1 1 calc GR . . . .
H5B H 0.4731 1.2337 0.7272 0.050 Uiso 1 1 calc GR . . . .
H5C H 0.4805 1.0800 0.7207 0.050 Uiso 1 1 calc GR . . . .
C6 C 0.3967(10) 1.3445(7) 0.6096(4) 0.039(2) Uani 1 1 d . . . . .
H6A H 0.4004 1.3563 0.5677 0.058 Uiso 1 1 calc GR . . . .
H6B H 0.4615 1.4068 0.6283 0.058 Uiso 1 1 calc GR . . . .
H6C H 0.2974 1.3583 0.6232 0.058 Uiso 1 1 calc GR . . . .
C7 C 0.6525(9) 1.1553(8) 0.6138(4) 0.034(2) Uani 1 1 d . . . . .
H7A H 0.6851 1.0728 0.6300 0.051 Uiso 1 1 calc GR . . . .
H7B H 0.7065 1.2262 0.6317 0.051 Uiso 1 1 calc GR . . . .
H7C H 0.6696 1.1557 0.5720 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.4575(11) 1.1991(8) 0.4741(4) 0.045(2) Uani 1 1 d . . . . .
H8A H 0.3846 1.2641 0.4841 0.067 Uiso 1 1 calc GR . . . .
H8B H 0.4653 1.1924 0.4320 0.067 Uiso 1 1 calc GR . . . .
H8C H 0.5514 1.2246 0.4902 0.067 Uiso 1 1 calc GR . . . .
C9 C 0.5587(9) 0.9261(9) 0.4960(3) 0.0420(19) Uani 1 1 d . . . . .
H9A H 0.6446 0.9637 0.5143 0.063 Uiso 1 1 calc GR . . . .
H9B H 0.5775 0.9126 0.4548 0.063 Uiso 1 1 calc GR . . . .
H9C H 0.5362 0.8431 0.5143 0.063 Uiso 1 1 calc GR . . . .
C10 C 0.2466(9) 0.9776(8) 0.4607(3) 0.035(2) Uani 1 1 d . U . . .
H10A H 0.2224 0.8893 0.4725 0.052 Uiso 1 1 calc GR . . . .
H10B H 0.2732 0.9783 0.4198 0.052 Uiso 1 1 calc GR . . . .
H10C H 0.1625 1.0338 0.4668 0.052 Uiso 1 1 calc GR . . . .
C11 C -0.1354(8) 0.9256(9) 0.7170(3) 0.0320(18) Uani 1 1 d . . . . .
C12 C 0.0545(8) 1.1163(6) 0.6756(3) 0.0224(14) Uani 1 1 d . . . . .
C13 C -0.0360(8) 0.9247(8) 0.5957(3) 0.0296(17) Uani 1 1 d . . . . .
C14 C 0.0489(10) 0.7234(7) 0.6731(4) 0.0352(18) Uani 1 1 d . . . . .
C15 C 0.1670(8) 0.9183(9) 0.7518(3) 0.0281(17) 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 2.4937(17) . ?
W C11 2.018(8) . ?
W C12 2.023(7) . ?
W C13 2.031(8) . ?
W C14 2.046(7) . ?
W C15 2.046(8) . ?
P O1 1.640(5) . ?
P C3 1.835(7) . ?
P C4 1.816(6) . ?
Si1 C4 1.910(7) . ?
Si1 C5 1.862(7) . ?
Si1 C6 1.872(7) . ?
Si1 C7 1.863(8) . ?
Si2 C4 1.912(6) . ?
Si2 C8 1.885(8) . ?
Si2 C9 1.861(9) . ?
Si2 C10 1.872(8) . ?
O1 C1 1.449(8) . ?
O2 C11 1.148(9) . ?
O3 C12 1.152(7) . ?
O4 C13 1.139(8) . ?
O5 C14 1.138(8) . ?
O6 C15 1.146(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.499(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.520(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 W P 178.4(2) . . ?
C11 W C12 88.1(3) . . ?
C11 W C13 93.8(3) . . ?
C11 W C14 90.3(4) . . ?
C11 W C15 91.4(3) . . ?
C12 W P 92.4(2) . . ?
C12 W C13 88.9(3) . . ?
C12 W C14 177.3(3) . . ?
C12 W C15 90.8(3) . . ?
C13 W P 84.7(2) . . ?
C13 W C14 89.0(3) . . ?
C13 W C15 174.9(3) . . ?
C14 W P 89.2(3) . . ?
C14 W C15 91.4(4) . . ?
C15 W P 90.2(2) . . ?
O1 P W 110.7(2) . . ?
O1 P C3 93.4(3) . . ?
O1 P C4 105.7(3) . . ?
C3 P W 119.8(3) . . ?
C4 P W 116.5(2) . . ?
C4 P C3 107.6(3) . . ?
C5 Si1 C4 114.2(3) . . ?
C5 Si1 C6 106.5(4) . . ?
C5 Si1 C7 106.4(5) . . ?
C6 Si1 C4 107.7(3) . . ?
C7 Si1 C4 111.4(3) . . ?
C7 Si1 C6 110.6(4) . . ?
C8 Si2 C4 109.5(3) . . ?
C9 Si2 C4 113.8(3) . . ?
C9 Si2 C8 107.4(4) . . ?
C9 Si2 C10 109.2(4) . . ?
C10 Si2 C4 109.4(3) . . ?
C10 Si2 C8 107.2(4) . . ?
C1 O1 P 114.3(4) . . ?
O1 C1 H1A 109.8 . . ?
O1 C1 H1B 109.8 . . ?
O1 C1 C2 109.2(6) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
C1 C2 C3 107.5(6) . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
P C3 H3A 111.3 . . ?
P C3 H3B 111.3 . . ?
C2 C3 P 102.3(6) . . ?
C2 C3 H3A 111.3 . . ?
C2 C3 H3B 111.3 . . ?
H3A C3 H3B 109.2 . . ?
P C4 Si1 114.1(3) . . ?
P C4 Si2 116.1(3) . . ?
P C4 H4 102.8 . . ?
Si1 C4 Si2 115.5(3) . . ?
Si1 C4 H4 102.8 . . ?
Si2 C4 H4 102.8 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 W 178.7(9) . . ?
O3 C12 W 178.2(7) . . ?
O4 C13 W 178.9(7) . . ?
O5 C14 W 178.7(8) . . ?
O6 C15 W 178.8(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 O1 C1 -108.3(5) . . . . ?
W P C3 C2 86.0(5) . . . . ?
W P C4 Si1 89.9(3) . . . . ?
W P C4 Si2 -131.9(3) . . . . ?
P O1 C1 C2 5.3(9) . . . . ?
O1 P C3 C2 -30.2(6) . . . . ?
O1 P C4 Si1 -146.8(3) . . . . ?
O1 P C4 Si2 -8.6(4) . . . . ?
O1 C1 C2 C3 -28.7(10) . . . . ?
C1 C2 C3 P 37.0(9) . . . . ?
C3 P O1 C1 15.4(6) . . . . ?
C3 P C4 Si1 -47.9(4) . . . . ?
C3 P C4 Si2 90.3(4) . . . . ?
C4 P O1 C1 124.7(5) . . . . ?
C4 P C3 C2 -137.9(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.497(10)
2 0.503(10)

