# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_greg1105f
_database_code_depnum_ccdc_archive 'CCDC 1917784'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2019-05-22 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_date             2019-05-21
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H24 Cl O5 P Si2 W'
_chemical_formula_sum            'C15 H24 Cl O5 P Si2 W'
_chemical_formula_weight         590.79
_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'
Cl Cl 0.1484 0.1585 '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           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   18.1955(6)
_cell_length_b                   13.3383(5)
_cell_length_c                   18.5737(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4507.8(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.52
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   0.139
_shelx_estimated_absorpt_T_min   0.139
_exptl_absorpt_coefficient_mu    5.441
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.3157
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41787
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         3.246
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'ApexII detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  X8-KappaApexII
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5079
_reflns_number_total             5426
_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       ?
_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    ?
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0217
_refine_ls_restrained_S_all      1.171
_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)+(0.0061P)²+10.4934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0492
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
2.d X=CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.e 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
C1 C 0.08118(16) 0.6869(2) 0.18853(14) 0.0155(5) Uani 1 1 d . . . . .
H1A H 0.0319 0.6676 0.2064 0.019 Uiso 1 1 calc R . . . .
H1B H 0.0980 0.7455 0.2168 0.019 Uiso 1 1 calc R . . . .
C2 C 0.07532(18) 0.7162(2) 0.11052(15) 0.0186(6) Uani 1 1 d . . . . .
H2 H 0.1172 0.7450 0.0880 0.022 Uiso 1 1 calc R . . . .
C3 C 0.01566(19) 0.7043(3) 0.07195(17) 0.0256(7) Uani 1 1 d . . . . .
H3A H -0.0270 0.6758 0.0931 0.031 Uiso 1 1 calc R . . . .
H3B H 0.0151 0.7243 0.0228 0.031 Uiso 1 1 calc R . . . .
C4 C 0.14679(14) 0.5641(2) 0.29997(13) 0.0109(5) Uani 1 1 d . . . . .
H4 H 0.1701 0.4966 0.3054 0.013 Uiso 1 1 calc R . . . .
C5 C -0.01858(16) 0.4876(3) 0.27642(18) 0.0259(7) Uani 1 1 d . . . . .
H5A H -0.0025 0.4201 0.2627 0.039 Uiso 1 1 calc GR . . . .
H5B H -0.0223 0.5296 0.2333 0.039 Uiso 1 1 calc GR . . . .
H5C H -0.0667 0.4838 0.3000 0.039 Uiso 1 1 calc GR . . . .
C6 C 0.01002(19) 0.6662(3) 0.37068(17) 0.0258(7) Uani 1 1 d . . . . .
H6A H 0.0457 0.7017 0.4009 0.039 Uiso 1 1 calc GR . . . .
H6B H -0.0348 0.6536 0.3984 0.039 Uiso 1 1 calc GR . . . .
H6C H -0.0018 0.7074 0.3286 0.039 Uiso 1 1 calc GR . . . .
C7 C 0.0600(2) 0.4536(3) 0.41654(17) 0.0264(7) Uani 1 1 d . . . . .
H7A H 0.0892 0.4844 0.4550 0.040 Uiso 1 1 calc GR . . . .
H7B H 0.0847 0.3928 0.3995 0.040 Uiso 1 1 calc GR . . . .
H7C H 0.0112 0.4362 0.4351 0.040 Uiso 1 1 calc GR . . . .
C8 C 0.19996(19) 0.7851(2) 0.33548(17) 0.0239(7) Uani 1 1 d . . . . .
H8A H 0.1489 0.8063 0.3424 0.036 Uiso 1 1 calc GR . . . .
H8B H 0.2142 0.7961 0.2852 0.036 Uiso 1 1 calc GR . . . .
H8C H 0.2321 0.8243 0.3671 0.036 Uiso 1 1 calc GR . . . .
C9 C 0.18637(18) 0.6349(3) 0.45623(15) 0.0257(7) Uani 1 1 d . . . . .
H9A H 0.2168 0.6812 0.4844 0.039 Uiso 1 1 calc GR . . . .
H9B H 0.1963 0.5659 0.4715 0.039 Uiso 1 1 calc GR . . . .
H9C H 0.1343 0.6504 0.4641 0.039 Uiso 1 1 calc GR . . . .
C10 C 0.30576(16) 0.6036(3) 0.34833(17) 0.0225(6) Uani 1 1 d . . . . .
H10A H 0.3223 0.6136 0.2986 0.034 Uiso 1 1 calc GR . . . .
H10B H 0.3081 0.5321 0.3603 0.034 Uiso 1 1 calc GR . . . .
H10C H 0.3376 0.6414 0.3811 0.034 Uiso 1 1 calc GR . . . .
C11 C 0.14457(15) 0.3112(2) 0.05735(15) 0.0159(6) Uani 1 1 d . . . . .
C12 C 0.16595(16) 0.5263(2) 0.03865(14) 0.0159(5) Uani 1 1 d . . . . .
C13 C 0.03117(17) 0.4463(2) 0.10014(15) 0.0187(6) Uani 1 1 d . . . . .
C14 C 0.12046(16) 0.3420(2) 0.20871(15) 0.0162(6) Uani 1 1 d . . . . .
C15 C 0.25144(16) 0.4167(2) 0.14110(15) 0.0147(5) Uani 1 1 d . . . . .
O1 O 0.14751(12) 0.24231(17) 0.02092(12) 0.0239(5) Uani 1 1 d . . . . .
O2 O 0.18231(13) 0.57827(17) -0.00724(11) 0.0250(5) Uani 1 1 d . . . . .
O3 O -0.02930(12) 0.45134(19) 0.08629(13) 0.0295(5) Uani 1 1 d . . . . .
O4 O 0.10963(13) 0.29202(17) 0.25780(11) 0.0262(5) Uani 1 1 d . . . . .
O5 O 0.31280(12) 0.40823(17) 0.15021(13) 0.0254(5) Uani 1 1 d . . . . .
Si1 Si 0.05019(4) 0.54415(6) 0.34034(4) 0.01672(16) Uani 1 1 d . . . . .
Si2 Si 0.20885(5) 0.64871(6) 0.35777(4) 0.01591(16) Uani 1 1 d . . . . .
P1 P 0.14539(4) 0.58179(5) 0.20299(4) 0.01046(13) Uani 1 1 d . . . . .
Cl1 Cl 0.24244(4) 0.65799(5) 0.17681(3) 0.01632(13) Uani 1 1 d . . . . .
W1 W 0.14112(2) 0.43177(2) 0.12277(2) 0.00973(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(4) . ?
C1 P1 1.844(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.310(4) . ?
C3 H3A 0.9500 . ?
C3 H3B 0.9500 . ?
C4 H4 1.0000 . ?
C4 Si1 1.929(3) . ?
C4 Si2 1.924(3) . ?
C4 P1 1.817(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 Si1 1.882(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 Si1 1.872(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 Si1 1.869(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 Si2 1.873(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 Si2 1.883(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 Si2 1.872(3) . ?
C11 O1 1.142(4) . ?
C11 W1 2.017(3) . ?
C12 O2 1.138(4) . ?
C12 W1 2.058(3) . ?
C13 O3 1.132(4) . ?
C13 W1 2.053(3) . ?
C14 O4 1.146(4) . ?
C14 W1 2.031(3) . ?
C15 O5 1.135(4) . ?
C15 W1 2.046(3) . ?
P1 Cl1 2.0947(10) . ?
P1 W1 2.4961(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C2 C1 P1 112.52(19) . . ?
P1 C1 H1A 109.1 . . ?
P1 C1 H1B 109.1 . . ?
C1 C2 H2 118.2 . . ?
C3 C2 C1 123.6(3) . . ?
C3 C2 H2 118.2 . . ?
C2 C3 H3A 120.0 . . ?
C2 C3 H3B 120.0 . . ?
H3A C3 H3B 120.0 . . ?
Si1 C4 H4 102.9 . . ?
Si2 C4 H4 102.9 . . ?
Si2 C4 Si1 113.50(13) . . ?
P1 C4 H4 102.9 . . ?
P1 C4 Si1 112.98(13) . . ?
P1 C4 Si2 119.04(14) . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
O1 C11 W1 178.8(3) . . ?
O2 C12 W1 177.5(3) . . ?
O3 C13 W1 177.6(3) . . ?
O4 C14 W1 179.0(3) . . ?
O5 C15 W1 179.0(3) . . ?
C5 Si1 C4 114.56(13) . . ?
C6 Si1 C4 110.65(14) . . ?
C6 Si1 C5 106.18(15) . . ?
C7 Si1 C4 107.26(14) . . ?
C7 Si1 C5 106.40(16) . . ?
C7 Si1 C6 111.79(15) . . ?
C8 Si2 C4 113.31(13) . . ?
C8 Si2 C9 106.92(15) . . ?
C9 Si2 C4 110.92(13) . . ?
C10 Si2 C4 108.19(13) . . ?
C10 Si2 C8 111.90(16) . . ?
C10 Si2 C9 105.32(15) . . ?
C1 P1 Cl1 97.55(10) . . ?
C1 P1 W1 120.18(9) . . ?
C4 P1 C1 104.59(12) . . ?
C4 P1 Cl1 106.34(9) . . ?
C4 P1 W1 119.23(9) . . ?
Cl1 P1 W1 106.06(3) . . ?
C11 W1 C12 91.40(11) . . ?
C11 W1 C13 88.98(11) . . ?
C11 W1 C14 90.52(11) . . ?
C11 W1 C15 89.50(11) . . ?
C11 W1 P1 176.41(8) . . ?
C12 W1 P1 87.42(8) . . ?
C13 W1 C12 90.04(12) . . ?
C13 W1 P1 94.40(8) . . ?
C14 W1 C12 177.17(11) . . ?
C14 W1 C13 92.07(12) . . ?
C14 W1 C15 89.59(11) . . ?
C14 W1 P1 90.53(8) . . ?
C15 W1 C12 88.35(11) . . ?
C15 W1 C13 177.76(11) . . ?
C15 W1 P1 87.08(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
C2 C1 P1 C4 177.3(2) . . . . ?
C2 C1 P1 Cl1 68.2(2) . . . . ?
C2 C1 P1 W1 -45.4(2) . . . . ?
Si1 C4 P1 C1 54.77(17) . . . . ?
Si1 C4 P1 Cl1 157.35(11) . . . . ?
Si1 C4 P1 W1 -83.02(14) . . . . ?
Si2 C4 P1 C1 -82.19(17) . . . . ?
Si2 C4 P1 Cl1 20.39(16) . . . . ?
Si2 C4 P1 W1 140.01(11) . . . . ?
P1 C1 C2 C3 113.0(3) . . . . ?

_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_greg1388
_database_code_depnum_ccdc_archive 'CCDC 1917786'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2019-05-22 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_audit_creation_date             2019-05-22
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H24 Br O5 P Si2 W'
_chemical_formula_sum            'C15 H24 Br O5 P Si2 W'
_chemical_formula_weight         635.25
_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'
Br Br -0.2901 2.4595 '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'

_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           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   18.0162(4)
_cell_length_b                   13.6552(3)
_cell_length_c                   18.5562(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4565.1(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6633
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   0.767
_shelx_estimated_absorpt_T_min   0.102
_exptl_absorpt_coefficient_mu    7.006
_exptl_absorpt_correction_T_max  0.11035
_exptl_absorpt_correction_T_min  0.0496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            41145
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.994
_diffrn_reflns_theta_min         2.469
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3857
_reflns_number_total             5494
_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       ?
_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    ?
_refine_diff_density_max         2.023
_refine_diff_density_min         -2.310
_refine_diff_density_rms         0.257
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0393
_refine_ls_restrained_S_all      0.956
_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)+(0.0558P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0973
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
2.d X=CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.e 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
C1 C -0.0809(3) 0.3156(4) 0.8110(3) 0.0294(12) Uani 1 1 d . . . . .
H1A H -0.0980 0.2589 0.7823 0.035 Uiso 1 1 calc R . . . .
H1B H -0.0307 0.3336 0.7939 0.035 Uiso 1 1 calc R . . . .
C2 C -0.0766(3) 0.2865(4) 0.8880(3) 0.0351(14) Uani 1 1 d . . . . .
H2 H -0.1193 0.2587 0.9099 0.042 Uiso 1 1 calc R . . . .
C3 C -0.0162(3) 0.2974(4) 0.9274(4) 0.0430(15) Uani 1 1 d . . . . .
H3A H 0.0272 0.3251 0.9068 0.052 Uiso 1 1 calc R . . . .
H3B H -0.0162 0.2777 0.9765 0.052 Uiso 1 1 calc R . . . .
C4 C -0.1451(3) 0.4374(3) 0.6984(3) 0.0240(11) Uani 1 1 d . . . . .
H4 H -0.1686 0.5033 0.6925 0.029 Uiso 1 1 calc R . . . .
C5 C -0.0063(4) 0.3384(5) 0.6275(4) 0.0454(16) Uani 1 1 d . . . . .
H5A H -0.0429 0.3039 0.5977 0.068 Uiso 1 1 calc GR . . . .
H5B H 0.0068 0.2976 0.6690 0.068 Uiso 1 1 calc GR . . . .
H5C H 0.0382 0.3516 0.5989 0.068 Uiso 1 1 calc GR . . . .
C6 C -0.0555(4) 0.5471(4) 0.5856(4) 0.0518(18) Uani 1 1 d . . . . .
H6A H -0.0792 0.6068 0.6038 0.078 Uiso 1 1 calc GR . . . .
H6B H -0.0859 0.5193 0.5468 0.078 Uiso 1 1 calc GR . . . .
H6C H -0.0061 0.5630 0.5668 0.078 Uiso 1 1 calc GR . . . .
C7 C 0.0223(3) 0.5090(4) 0.7265(3) 0.0331(13) Uani 1 1 d . . . . .
H7A H 0.0274 0.4643 0.7675 0.050 Uiso 1 1 calc GR . . . .
H7B H 0.0047 0.5728 0.7436 0.050 Uiso 1 1 calc GR . . . .
H7C H 0.0706 0.5170 0.7029 0.050 Uiso 1 1 calc GR . . . .
C8 C -0.3052(3) 0.3956(5) 0.6469(4) 0.0413(15) Uani 1 1 d . . . . .
H8A H -0.3082 0.4659 0.6366 0.062 Uiso 1 1 calc GR . . . .
H8B H -0.3233 0.3830 0.6958 0.062 Uiso 1 1 calc GR . . . .
H8C H -0.3358 0.3596 0.6122 0.062 Uiso 1 1 calc GR . . . .
C9 C -0.1971(4) 0.2211(4) 0.6605(4) 0.0449(16) Uani 1 1 d . . . . .
H9A H -0.2100 0.2098 0.7111 0.067 Uiso 1 1 calc GR . . . .
H9B H -0.1457 0.2004 0.6520 0.067 Uiso 1 1 calc GR . . . .
H9C H -0.2305 0.1833 0.6295 0.067 Uiso 1 1 calc GR . . . .
C10 C -0.1826(3) 0.3705(5) 0.5417(3) 0.0432(15) Uani 1 1 d . . . . .
H10A H -0.1921 0.4384 0.5274 0.065 Uiso 1 1 calc GR . . . .
H10B H -0.2132 0.3264 0.5124 0.065 Uiso 1 1 calc GR . . . .
H10C H -0.1301 0.3551 0.5342 0.065 Uiso 1 1 calc GR . . . .
C11 C -0.1425(3) 0.6835(4) 0.9417(3) 0.0273(12) Uani 1 1 d . . . . .
C12 C -0.0290(3) 0.5508(4) 0.9009(3) 0.0314(13) Uani 1 1 d . . . . .
C13 C -0.1664(3) 0.4756(4) 0.9592(3) 0.0267(12) Uani 1 1 d . . . . .
C14 C -0.2503(3) 0.5862(4) 0.8568(3) 0.0310(12) Uani 1 1 d . . . . .
C15 C -0.1168(3) 0.6541(4) 0.7912(3) 0.0296(12) Uani 1 1 d . . . . .
Br Br -0.25189(3) 0.34287(4) 0.82515(3) 0.03178(14) Uani 1 1 d . . . . .
O1 O -0.1448(2) 0.7503(3) 0.9795(2) 0.0359(10) Uani 1 1 d . . . . .
O2 O 0.0321(2) 0.5454(3) 0.9149(3) 0.0461(11) Uani 1 1 d . . . . .
O3 O -0.1838(2) 0.4259(3) 1.0055(2) 0.0426(10) Uani 1 1 d . . . . .
O4 O -0.3123(2) 0.5965(3) 0.8468(3) 0.0425(10) Uani 1 1 d . . . . .
O5 O -0.1049(2) 0.7019(3) 0.7416(2) 0.0412(10) Uani 1 1 d . . . . .
P P -0.14482(7) 0.42025(9) 0.79582(8) 0.0239(3) Uani 1 1 d . . . . .
Si1 Si -0.04679(9) 0.45676(12) 0.65980(10) 0.0324(4) Uani 1 1 d . . . . .
Si2 Si -0.20652(9) 0.35431(12) 0.63933(9) 0.0319(4) Uani 1 1 d . . . . .
W W -0.13962(2) 0.56696(2) 0.87612(2) 0.02285(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.485(8) . ?
C1 P 1.857(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.319(8) . ?
C3 H3A 0.9500 . ?
C3 H3B 0.9500 . ?
C4 H4 1.0000 . ?
C4 P 1.824(6) . ?
C4 Si1 1.929(5) . ?
C4 Si2 1.927(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 Si1 1.872(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 Si1 1.856(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 Si1 1.895(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 Si2 1.871(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 Si2 1.869(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 Si2 1.876(7) . ?
C11 O1 1.151(6) . ?
C11 W 2.003(5) . ?
C12 O2 1.133(7) . ?
C12 W 2.057(6) . ?
C13 O3 1.139(6) . ?
C13 W 2.041(6) . ?
C14 O4 1.141(7) . ?
C14 W 2.042(6) . ?
C15 O5 1.148(7) . ?
C15 W 2.017(6) . ?
Br P 2.2659(14) . ?
P W 2.4986(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1A C1 H1B 107.8 . . ?
C2 C1 H1A 109.1 . . ?
C2 C1 H1B 109.1 . . ?
C2 C1 P 112.6(4) . . ?
P C1 H1A 109.1 . . ?
P C1 H1B 109.1 . . ?
C1 C2 H2 118.4 . . ?
C3 C2 C1 123.2(6) . . ?
C3 C2 H2 118.4 . . ?
C2 C3 H3A 120.0 . . ?
C2 C3 H3B 120.0 . . ?
H3A C3 H3B 120.0 . . ?
P C4 H4 103.0 . . ?
P C4 Si1 112.5(3) . . ?
P C4 Si2 119.3(3) . . ?
Si1 C4 H4 103.0 . . ?
Si2 C4 H4 103.0 . . ?
Si2 C4 Si1 113.4(3) . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
O1 C11 W 179.4(5) . . ?
O2 C12 W 177.6(5) . . ?
O3 C13 W 177.6(5) . . ?
O4 C14 W 179.2(6) . . ?
O5 C15 W 178.1(5) . . ?
C1 P Br 97.60(18) . . ?
C1 P W 120.21(18) . . ?
C4 P C1 104.6(2) . . ?
C4 P Br 107.20(17) . . ?
C4 P W 119.23(16) . . ?
Br P W 105.22(6) . . ?
C5 Si1 C4 111.0(3) . . ?
C5 Si1 C7 106.2(3) . . ?
C6 Si1 C4 106.8(3) . . ?
C6 Si1 C5 111.7(3) . . ?
C6 Si1 C7 106.8(3) . . ?
C7 Si1 C4 114.4(2) . . ?
C8 Si2 C4 109.0(3) . . ?
C8 Si2 C10 104.8(3) . . ?
C9 Si2 C4 113.7(3) . . ?
C9 Si2 C8 111.4(3) . . ?
C9 Si2 C10 107.3(3) . . ?
C10 Si2 C4 110.4(3) . . ?
C11 W C12 88.5(2) . . ?
C11 W C13 91.2(2) . . ?
C11 W C14 88.8(2) . . ?
C11 W C15 90.6(2) . . ?
C11 W P 176.31(15) . . ?
C12 W P 94.79(16) . . ?
C13 W C12 89.7(2) . . ?
C13 W C14 88.9(2) . . ?
C13 W P 87.21(15) . . ?
C14 W C12 177.0(2) . . ?
C14 W P 87.82(15) . . ?
C15 W C12 92.3(2) . . ?
C15 W C13 177.3(2) . . ?
C15 W C14 89.2(2) . . ?
C15 W P 90.85(16) . . ?

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
C2 C1 P C4 -176.8(4) . . . . ?
C2 C1 P Br -66.7(4) . . . . ?
C2 C1 P W 45.9(4) . . . . ?
P C1 C2 C3 -112.7(6) . . . . ?
Si1 C4 P C1 -55.7(3) . . . . ?
Si1 C4 P Br -158.60(18) . . . . ?
Si1 C4 P W 82.2(3) . . . . ?
Si2 C4 P C1 80.8(3) . . . . ?
Si2 C4 P Br -22.1(3) . . . . ?
Si2 C4 P W -141.3(2) . . . . ?

_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_greg1387
_database_code_depnum_ccdc_archive 'CCDC 1917785'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2019-05-22 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_greg1387            
;
PROBLEM: Check Calcd Resid. Dens.  0.77A   From W              -3.67 eA-3
RESPONSE: Since all significant peaks/holes are equally distributed around the heavy atom, it is probably an artefact of absorption effects. Trials for finding twinning were not successful. Nevertheless, the influence of the residual peaks and holes on structural  parameters should be negligible.
;
_vrf_PLAT971_greg1387            
;
PROBLEM: Check Calcd Resid. Dens.  0.95A   From W               2.73 eA-3
RESPONSE: Since all significant peaks/holes are equally distributed around the heavy atom, it is probably an artefact of absorption effects. Trials for finding twinning were not successful. Nevertheless, the influence of the residual peaks and holes on structural  parameters should be negligible.
;
_vrf_PLAT971_greg1387_2          
;
PROBLEM: Check Calcd Resid. Dens.  0.86A   From W               2.60 eA-3
RESPONSE: Since all significant peaks/holes are equally distributed around the heavy atom, it is probably an artefact of absorption effects. Trials for finding twinning were not successful. Nevertheless, the influence of the residual peaks and holes on structural  parameters should be negligible.
;
_vrf_PLAT971_greg1387_3          
;
PROBLEM: Check Calcd Resid. Dens.  0.96A   From W               2.56 eA-3
RESPONSE: Since all significant peaks/holes are equally distributed around the heavy atom, it is probably an artefact of absorption effects. Trials for finding twinning were not successful. Nevertheless, the influence of the residual peaks and holes on structural  parameters should be negligible.
;
# Added during the CSD deposition process: Wednesday 22 May 2019 12:25 PM
# end Validation Reply Form

_audit_creation_date             2019-05-21
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H24 F O5 P Si2 W'
_chemical_formula_sum            'C15 H24 F O5 P Si2 W'
_chemical_formula_weight         574.34
_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'
F F 0.0171 0.0103 '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'

_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                   9.4372(3)
_cell_length_b                   18.8621(6)
_cell_length_c                   12.3957(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.0074(18)
_cell_angle_gamma                90
_cell_volume                     2201.11(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5325
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   0.219
_shelx_estimated_absorpt_T_min   0.138
_exptl_absorpt_coefficient_mu    5.458
_exptl_absorpt_correction_T_max  0.1527
_exptl_absorpt_correction_T_min  0.0533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1526
_diffrn_reflns_av_unetI/netI     0.0899
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18174
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_min         2.626
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3509
_reflns_number_total             3962
_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       ?
_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    ?
_refine_diff_density_max         2.864
_refine_diff_density_min         -3.100
_refine_diff_density_rms         0.277
_refine_ls_extinction_coef       0.0055(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3962
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0567
_refine_ls_restrained_S_all      1.029
_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)+(0.1006P)²+1.4652P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1529
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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
2. Rigid bond restraints
 O1, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5, C15
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 W, C11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Ternary CH refined with riding coordinates:
 C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2)
3.d X=CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.e 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
C1 C 0.3348(7) 0.7618(4) 0.6194(6) 0.0280(16) Uani 1 1 d . . . . .
H1A H 0.3324 0.7179 0.5755 0.034 Uiso 1 1 calc R . . . .
H1B H 0.2476 0.7630 0.6594 0.034 Uiso 1 1 calc R . . . .
C2 C 0.3364(8) 0.8252(4) 0.5455(6) 0.0350(18) Uani 1 1 d . . . . .
H2 H 0.4087 0.8264 0.4960 0.042 Uiso 1 1 calc R . . . .
C3 C 0.2499(10) 0.8774(5) 0.5429(7) 0.043(2) Uani 1 1 d . . . . .
H3A H 0.1756 0.8785 0.5909 0.052 Uiso 1 1 calc R . . . .
H3B H 0.2598 0.9150 0.4931 0.052 Uiso 1 1 calc R . . . .
C4 C 0.4923(6) 0.6725(3) 0.7750(5) 0.0200(13) Uani 1 1 d . . . . .
H4 H 0.5546 0.6786 0.8430 0.024 Uiso 1 1 calc R . . . .
C5 C 0.7845(8) 0.6259(4) 0.7128(7) 0.0326(18) Uani 1 1 d . . . . .
H5A H 0.8158 0.6274 0.7898 0.049 Uiso 1 1 calc GR . . . .
H5B H 0.7997 0.6724 0.6803 0.049 Uiso 1 1 calc GR . . . .
H5C H 0.8391 0.5900 0.6765 0.049 Uiso 1 1 calc GR . . . .
C6 C 0.5746(8) 0.5126(4) 0.7567(6) 0.0336(17) Uani 1 1 d . . . . .
H6A H 0.4738 0.5006 0.7592 0.050 Uiso 1 1 calc GR . . . .
H6B H 0.6204 0.5120 0.8301 0.050 Uiso 1 1 calc GR . . . .
H6C H 0.6207 0.4779 0.7119 0.050 Uiso 1 1 calc GR . . . .
C7 C 0.5249(7) 0.5988(4) 0.5523(6) 0.0313(16) Uani 1 1 d . . . . .
H7A H 0.5425 0.6443 0.5174 0.047 Uiso 1 1 calc GR . . . .
H7B H 0.4227 0.5890 0.5473 0.047 Uiso 1 1 calc GR . . . .
H7C H 0.5746 0.5610 0.5162 0.047 Uiso 1 1 calc GR . . . .
C8 C 0.3591(8) 0.5863(5) 0.9499(7) 0.0409(19) Uani 1 1 d . . . . .
H8A H 0.4194 0.6134 1.0027 0.061 Uiso 1 1 calc GR . . . .
H8B H 0.4099 0.5437 0.9289 0.061 Uiso 1 1 calc GR . . . .
H8C H 0.2714 0.5725 0.9823 0.061 Uiso 1 1 calc GR . . . .
C9 C 0.2034(7) 0.5923(4) 0.7228(7) 0.0362(18) Uani 1 1 d . . . . .
H9A H 0.2577 0.5521 0.6975 0.054 Uiso 1 1 calc GR . . . .
H9B H 0.1765 0.6237 0.6618 0.054 Uiso 1 1 calc GR . . . .
H9C H 0.1175 0.5749 0.7543 0.054 Uiso 1 1 calc GR . . . .
C10 C 0.2030(7) 0.7166(4) 0.8746(6) 0.0336(17) Uani 1 1 d . . . . .
H10A H 0.1160 0.6973 0.9019 0.050 Uiso 1 1 calc GR . . . .
H10B H 0.1783 0.7488 0.8141 0.050 Uiso 1 1 calc GR . . . .
H10C H 0.2564 0.7427 0.9325 0.050 Uiso 1 1 calc GR . . . .
C11 C 0.6193(7) 0.9451(4) 0.9264(6) 0.0257(14) Uani 1 1 d . U . . .
C12 C 0.7577(7) 0.8284(4) 0.8266(6) 0.0308(16) Uani 1 1 d . . . . .
C13 C 0.5240(6) 0.8025(4) 0.9671(6) 0.0260(15) Uani 1 1 d . . . . .
C14 C 0.3422(8) 0.8924(4) 0.8316(6) 0.0292(16) Uani 1 1 d . . . . .
C15 C 0.5710(7) 0.9249(4) 0.6989(6) 0.0267(14) Uani 1 1 d . U . . .
F F 0.6091(4) 0.7541(2) 0.6287(3) 0.0268(9) Uani 1 1 d . . . . .
O1 O 0.6597(5) 0.9918(3) 0.9780(4) 0.0335(12) Uani 1 1 d . U . . .
O2 O 0.8708(5) 0.8087(3) 0.8211(5) 0.0484(15) Uani 1 1 d . . . . .
O3 O 0.5053(5) 0.7700(3) 1.0423(4) 0.0353(13) Uani 1 1 d . . . . .
O4 O 0.2259(5) 0.9067(3) 0.8293(4) 0.0352(12) Uani 1 1 d . . . . .
O5 O 0.5788(6) 0.9614(3) 0.6277(4) 0.0422(14) Uani 1 1 d . U . . .
P P 0.49094(17) 0.75990(9) 0.71633(14) 0.0216(4) Uani 1 1 d . . . . .
Si1 Si 0.59127(18) 0.60308(10) 0.69718(16) 0.0238(4) Uani 1 1 d . . . . .
Si2 Si 0.3146(2) 0.64241(10) 0.82745(18) 0.0260(5) Uani 1 1 d . . . . .
W W 0.55157(3) 0.86228(2) 0.83329(2) 0.0222(2) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.507(10) . ?
C1 P 1.836(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.278(12) . ?
C3 H3A 0.9500 . ?
C3 H3B 0.9500 . ?
C4 H4 1.0000 . ?
C4 P 1.801(6) . ?
C4 Si1 1.909(6) . ?
C4 Si2 1.927(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 Si1 1.870(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 Si1 1.870(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 Si1 1.861(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 Si2 1.875(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 Si2 1.867(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 Si2 1.870(8) . ?
C11 O1 1.138(8) . ?
C11 W 2.019(7) . ?
C12 O2 1.137(8) . ?
C12 W 2.054(7) . ?
C13 O3 1.139(8) . ?
C13 W 2.038(8) . ?
C14 O4 1.129(8) . ?
C14 W 2.054(7) . ?
C15 O5 1.125(9) . ?
C15 W 2.061(7) . ?
F P 1.615(4) . ?
P W 2.4582(17) . ?

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
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
C2 C1 P 111.8(5) . . ?
P C1 H1A 109.3 . . ?
P C1 H1B 109.3 . . ?
C1 C2 H2 116.8 . . ?
C3 C2 C1 126.4(8) . . ?
C3 C2 H2 116.8 . . ?
C2 C3 H3A 120.0 . . ?
C2 C3 H3B 120.0 . . ?
H3A C3 H3B 120.0 . . ?
P C4 H4 102.9 . . ?
P C4 Si1 114.4(3) . . ?
P C4 Si2 115.1(3) . . ?
Si1 C4 H4 102.9 . . ?
Si1 C4 Si2 115.9(3) . . ?
Si2 C4 H4 102.9 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
O1 C11 W 178.8(6) . . ?
O2 C12 W 178.5(6) . . ?
O3 C13 W 178.1(6) . . ?
O4 C14 W 177.7(6) . . ?
O5 C15 W 177.0(7) . . ?
C1 P W 120.9(2) . . ?
C4 P C1 105.4(3) . . ?
C4 P W 119.1(2) . . ?
F P C1 97.0(3) . . ?
F P C4 103.0(3) . . ?
F P W 107.87(17) . . ?
C5 Si1 C4 107.3(3) . . ?
C6 Si1 C4 111.7(3) . . ?
C6 Si1 C5 106.1(3) . . ?
C7 Si1 C4 111.9(3) . . ?
C7 Si1 C5 111.7(4) . . ?
C7 Si1 C6 108.0(3) . . ?
C8 Si2 C4 106.8(3) . . ?
C9 Si2 C4 112.0(3) . . ?
C9 Si2 C8 111.1(4) . . ?
C9 Si2 C10 107.1(4) . . ?
C10 Si2 C4 114.0(3) . . ?
C10 Si2 C8 105.6(4) . . ?
C11 W C12 90.0(3) . . ?
C11 W C13 90.9(3) . . ?
C11 W C14 93.3(3) . . ?
C11 W C15 88.7(3) . . ?
C11 W P 174.96(19) . . ?
C12 W C14 176.4(3) . . ?
C12 W C15 90.4(3) . . ?
C12 W P 85.06(19) . . ?
C13 W C12 92.1(3) . . ?
C13 W C14 89.1(3) . . ?
C13 W C15 177.5(2) . . ?
C13 W P 90.42(19) . . ?
C14 W C15 88.5(3) . . ?
C14 W P 91.5(2) . . ?
C15 W P 90.2(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
C2 C1 P C4 -167.2(5) . . . . ?
C2 C1 P F -61.6(6) . . . . ?
C2 C1 P W 54.1(6) . . . . ?
P C1 C2 C3 -113.1(8) . . . . ?
Si1 C4 P C1 88.2(4) . . . . ?
Si1 C4 P F -12.9(4) . . . . ?
Si1 C4 P W -132.2(2) . . . . ?
Si2 C4 P C1 -49.8(4) . . . . ?
Si2 C4 P F -150.9(3) . . . . ?
Si2 C4 P W 89.9(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
