# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_lf104
_database_code_depnum_ccdc_archive 'CCDC 2062243'
loop_
_audit_author_name
_audit_author_address
'Nathan T. Coles'
;FU Berlin
Germany
;
_audit_update_record             
;
2021-02-09 deposited with the CCDC.	2021-08-06 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_lf104               
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The flack parameter was found to be 0.059(4) with an R1 of 1.74% and wR2 of 4.2%. As the R values were already very low a BASF/Twin refinement has not been performed.
;
# Added during the CSD deposition process: Tuesday 09 February 2021 02:16 PM
# end Validation Reply Form

_audit_creation_date             2021-01-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
N.T.Coles@fu-berlin.de
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Al F20 O4 Te4, C18 H40 P Si4'
_chemical_formula_sum            'C18 H40 Al F20 O4 P Si4 Te4'
_chemical_formula_weight         1381.21
_chemical_absolute_configuration ?
_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'
Al Al 0.0645 0.0514 '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'
Te Te -0.5308 1.6751 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.0027(4)
_cell_length_b                   16.9978(5)
_cell_length_c                   21.5539(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.5900(10)
_cell_angle_gamma                90
_cell_volume                     4397.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.535
_shelx_estimated_absorpt_T_min   0.350
_exptl_absorpt_coefficient_mu    2.903
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3836
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1023 before and 0.0497 after correction.
The Ratio of minimum to maximum transmission is 0.3836.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             2608
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6.00 -8.00 7.00 0.1230
0.00 -8.00 1.00 0.1980
5.00 6.00 -6.00 0.0910
3.00 7.00 -4.00 0.0910
-2.00 1.00 2.00 0.1720
-2.00 -1.00 -8.00 0.1580
-5.00 6.00 -8.00 0.1170
1.00 0.00 7.00 0.1500
3.00 -6.00 -2.00 0.1980
-2.00 -4.00 7.00 0.1350
7.00 4.00 -3.00 0.0770

_exptl_crystal_size_max          0.458
_exptl_crystal_size_mid          0.328
_exptl_crystal_size_min          0.246
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            189889
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.540
_diffrn_reflns_theta_min         2.077
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                13205
_reflns_number_total             13410
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 6489 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.059(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         13410
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0174
_refine_ls_restrained_S_all      1.048
_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)+(0.0198P)²+6.6692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0421
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Te1 Te 0.49214(2) 0.88800(2) 0.67096(2) 0.02671(5) Uani 1 1 d . . . . .
Te2 Te 0.13391(2) 0.72340(2) 0.73786(2) 0.02961(5) Uani 1 1 d . . . . .
Te3 Te 0.12404(2) 0.88087(2) 0.52698(2) 0.02478(4) Uani 1 1 d . . . . .
Te4 Te 0.29368(2) 0.59068(2) 0.55734(2) 0.01823(4) Uani 1 1 d . . . . .
Al1 Al 0.29301(8) 0.77146(5) 0.61687(4) 0.02005(17) Uani 1 1 d . . . . .
F1 F 0.5598(3) 0.9636(2) 0.71823(17) 0.0639(9) Uani 1 1 d . . . . .
F2 F 0.6096(3) 0.8940(2) 0.6191(2) 0.0646(11) Uani 1 1 d . . . . .
F3 F 0.5656(3) 0.8170(2) 0.71892(18) 0.0736(11) Uani 1 1 d . . . . .
F4 F 0.3784(3) 0.8910(2) 0.72736(18) 0.0637(11) Uani 1 1 d . . . . .
F5 F 0.4237(3) 0.96811(19) 0.6296(2) 0.0789(12) Uani 1 1 d . . . . .
F6 F 0.0147(3) 0.7123(3) 0.78972(17) 0.0699(11) Uani 1 1 d . . . . .
F7 F 0.2190(3) 0.73724(18) 0.80793(11) 0.0497(7) Uani 1 1 d . . . . .
F8 F 0.1531(3) 0.61728(15) 0.74557(13) 0.0450(6) Uani 1 1 d . . . . .
F9 F 0.0357(2) 0.7091(2) 0.67341(14) 0.0497(7) Uani 1 1 d . . . . .
F10 F 0.1033(3) 0.82909(18) 0.73734(14) 0.0575(9) Uani 1 1 d . . . . .
F11 F 0.0457(3) 0.9179(2) 0.46005(14) 0.0618(9) Uani 1 1 d . . . . .
F12 F 0.2374(3) 0.8604(2) 0.47271(13) 0.0474(6) Uani 1 1 d . . . . .
F13 F 0.1783(3) 0.98045(15) 0.53657(16) 0.0586(8) Uani 1 1 d . . . . .
F14 F 0.0049(3) 0.9070(2) 0.57428(16) 0.0571(8) Uani 1 1 d . . . . .
F15 F 0.0640(3) 0.78466(17) 0.50988(16) 0.0553(8) Uani 1 1 d . . . . .
F16 F 0.2844(2) 0.48391(12) 0.54990(13) 0.0405(6) Uani 1 1 d . . . . .
F17 F 0.4115(2) 0.58563(13) 0.50399(12) 0.0297(5) Uani 1 1 d . . . . .
F18 F 0.3879(2) 0.57579(17) 0.62344(12) 0.0400(6) Uani 1 1 d . . . . .
F19 F 0.1738(2) 0.58473(15) 0.60892(14) 0.0366(6) Uani 1 1 d . . . . .
F20 F 0.1989(2) 0.59672(16) 0.49027(11) 0.0359(5) Uani 1 1 d . . . . .
O1 O 0.4262(2) 0.81195(17) 0.62519(13) 0.0337(6) Uani 1 1 d . . . . .
O2 O 0.2534(2) 0.73296(15) 0.68804(12) 0.0242(5) Uani 1 1 d . . . . .
O3 O 0.2011(2) 0.84421(16) 0.59332(12) 0.0325(6) Uani 1 1 d . . . . .
O4 O 0.3035(3) 0.69701(14) 0.56183(12) 0.0283(5) Uani 1 1 d . . . . .
P1 P 0.74367(7) 0.52177(5) 0.35873(4) 0.02159(15) Uani 1 1 d . . . . .
Si3 Si 0.37898(7) 0.56395(6) 0.32331(4) 0.02209(16) Uani 1 1 d . . . . .
Si2 Si 0.65305(8) 0.72777(5) 0.47850(4) 0.02135(16) Uani 1 1 d . . . . .
Si1 Si 0.90691(7) 0.60161(5) 0.45059(4) 0.02249(16) Uani 1 1 d . . . . .
Si4 Si 0.59987(9) 0.42112(6) 0.27056(5) 0.0293(2) Uani 1 1 d . . . . .
C1 C 0.7606(3) 0.59343(17) 0.41258(14) 0.0196(5) Uani 1 1 d . . . . .
C2 C 0.6634(2) 0.63846(17) 0.42397(13) 0.0181(5) Uani 1 1 d . . . . .
C3 C 0.5583(2) 0.62340(17) 0.39335(12) 0.0172(5) Uani 1 1 d . . . . .
H3 H 0.499053 0.658276 0.402824 0.015(9) Uiso 1 1 calc R . . . .
C4 C 0.5330(2) 0.56070(17) 0.34954(14) 0.0189(5) Uani 1 1 d . . . . .
C5 C 0.6145(3) 0.50745(17) 0.32814(14) 0.0199(5) Uani 1 1 d . . . . .
C6 C 0.8635(3) 0.4740(2) 0.3254(2) 0.0337(8) Uani 1 1 d . . . . .
H6A H 0.850364 0.465638 0.280963 0.050 Uiso 1 1 calc R U . . .
H6B H 0.875603 0.423139 0.345853 0.050 Uiso 1 1 calc R U . . .
H6C H 0.929401 0.507231 0.331415 0.050 Uiso 1 1 calc R U . . .
C7 C 0.9687(3) 0.5007(2) 0.4582(2) 0.0347(8) Uani 1 1 d . . . . .
H7A H 1.019349 0.499231 0.494175 0.052 Uiso 1 1 calc R U . . .
H7B H 1.010173 0.487909 0.420591 0.052 Uiso 1 1 calc R U . . .
H7C H 0.909003 0.462098 0.463882 0.052 Uiso 1 1 calc R U . . .
C8 C 0.9041(3) 0.6364(2) 0.53242(17) 0.0320(7) Uani 1 1 d . . . . .
H8A H 0.861368 0.599197 0.557515 0.048 Uiso 1 1 calc R U . . .
H8B H 0.868969 0.688358 0.534091 0.048 Uiso 1 1 calc R U . . .
H8C H 0.980436 0.639841 0.548738 0.048 Uiso 1 1 calc R U . . .
C9 C 0.9901(3) 0.6654(2) 0.39806(18) 0.0297(7) Uani 1 1 d . . . . .
H9A H 0.956857 0.718023 0.396308 0.045 Uiso 1 1 calc R U . . .
H9B H 0.990533 0.642484 0.356347 0.045 Uiso 1 1 calc R U . . .
H9C H 1.066753 0.669253 0.413931 0.045 Uiso 1 1 calc R U . . .
C10 C 0.7688(3) 0.7989(2) 0.46416(18) 0.0303(7) Uani 1 1 d . . . . .
H10A H 0.762754 0.843268 0.492926 0.045 Uiso 1 1 calc R U . . .
H10B H 0.763752 0.818163 0.421374 0.045 Uiso 1 1 calc R U . . .
H10C H 0.840524 0.772429 0.470645 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6422(3) 0.6929(2) 0.56044(15) 0.0274(6) Uani 1 1 d . . . . .
H11A H 0.676243 0.640751 0.564275 0.041 Uiso 1 1 calc R U . . .
H11B H 0.563524 0.689917 0.571979 0.041 Uiso 1 1 calc R U . . .
H11C H 0.681039 0.729892 0.588046 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5215(3) 0.7829(2) 0.4595(2) 0.0338(8) Uani 1 1 d . . . . .
H12A H 0.457004 0.750384 0.470086 0.051 Uiso 1 1 calc R U . . .
H12B H 0.519334 0.795097 0.415083 0.051 Uiso 1 1 calc R U . . .
H12C H 0.519636 0.831850 0.483442 0.051 Uiso 1 1 calc R U . . .
C13 C 0.3167(3) 0.6593(2) 0.3492(2) 0.0336(8) Uani 1 1 d . . . . .
H13A H 0.361918 0.703111 0.333867 0.050 Uiso 1 1 calc R U . . .
H13B H 0.314969 0.660886 0.394593 0.050 Uiso 1 1 calc R U . . .
H13C H 0.240682 0.663926 0.332556 0.050 Uiso 1 1 calc R U . . .
C14 C 0.3663(3) 0.5641(3) 0.23692(17) 0.0317(7) Uani 1 1 d . . . . .
H14A H 0.291946 0.545601 0.224655 0.048 Uiso 1 1 calc R U . . .
H14B H 0.422768 0.529039 0.219445 0.048 Uiso 1 1 calc R U . . .
H14C H 0.377612 0.617584 0.221305 0.048 Uiso 1 1 calc R U . . .
C15 C 0.3003(3) 0.4837(2) 0.36345(18) 0.0344(8) Uani 1 1 d . . . . .
H15A H 0.246804 0.459965 0.334324 0.052 Uiso 1 1 calc R U . . .
H15B H 0.260285 0.505767 0.398836 0.052 Uiso 1 1 calc R U . . .
H15C H 0.352627 0.443393 0.378171 0.052 Uiso 1 1 calc R U . . .
C16 C 0.6398(4) 0.4601(3) 0.19370(19) 0.0425(10) Uani 1 1 d . . . . .
H16A H 0.594998 0.506825 0.184061 0.064 Uiso 1 1 calc R U . . .
H16B H 0.626470 0.419816 0.161938 0.064 Uiso 1 1 calc R U . . .
H16C H 0.718902 0.474257 0.194411 0.064 Uiso 1 1 calc R U . . .
C17 C 0.6928(5) 0.3382(3) 0.2967(3) 0.0593(16) Uani 1 1 d . . . . .
H17A H 0.767080 0.345046 0.278964 0.089 Uiso 1 1 calc R U . . .
H17B H 0.661264 0.288016 0.282614 0.089 Uiso 1 1 calc R U . . .
H17C H 0.698624 0.338278 0.342064 0.089 Uiso 1 1 calc R U . . .
C18 C 0.4599(4) 0.3738(2) 0.2694(2) 0.0419(10) Uani 1 1 d . . . . .
H18A H 0.444714 0.351218 0.310327 0.063 Uiso 1 1 calc R U . . .
H18B H 0.458278 0.332007 0.238112 0.063 Uiso 1 1 calc R U . . .
H18C H 0.403022 0.413244 0.259282 0.063 Uiso 1 1 calc R 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
Te1 F1 1.825(3) . ?
Te1 F2 1.810(3) . ?
Te1 F3 1.812(3) . ?
Te1 F4 1.838(3) . ?
Te1 F5 1.819(3) . ?
Te1 O1 1.804(3) . ?
Te2 F6 1.834(3) . ?
Te2 F7 1.830(3) . ?
Te2 F8 1.826(3) . ?
Te2 F9 1.829(3) . ?
Te2 F10 1.834(3) . ?
Te2 O2 1.808(3) . ?
Te3 F11 1.826(3) . ?
Te3 F12 1.837(3) . ?
Te3 F13 1.825(3) . ?
Te3 F14 1.819(3) . ?
Te3 F15 1.823(3) . ?
Te3 O3 1.806(2) . ?
Te4 F16 1.825(2) . ?
Te4 F17 1.834(2) . ?
Te4 F18 1.827(2) . ?
Te4 F19 1.830(3) . ?
Te4 F20 1.833(2) . ?
Te4 O4 1.814(2) . ?
Al1 O1 1.748(3) . ?
Al1 O2 1.739(3) . ?
Al1 O3 1.730(3) . ?
Al1 O4 1.740(3) . ?
P1 C1 1.693(3) . ?
P1 C5 1.696(3) . ?
P1 C6 1.807(4) . ?
Si3 C4 1.928(3) . ?
Si3 C13 1.872(4) . ?
Si3 C14 1.867(4) . ?
Si3 C15 1.876(4) . ?
Si2 C2 1.925(3) . ?
Si2 C10 1.869(4) . ?
Si2 C11 1.869(3) . ?
Si2 C12 1.877(4) . ?
Si1 C1 1.935(3) . ?
Si1 C7 1.876(4) . ?
Si1 C8 1.861(4) . ?
Si1 C9 1.865(4) . ?
Si4 C5 1.929(3) . ?
Si4 C16 1.852(5) . ?
Si4 C17 1.881(5) . ?
Si4 C18 1.863(4) . ?
C1 C2 1.419(4) . ?
C2 C3 1.440(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.454(4) . ?
C4 C5 1.414(4) . ?
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 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

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
F1 Te1 F4 86.59(14) . . ?
F2 Te1 F1 87.70(16) . . ?
F2 Te1 F3 90.7(2) . . ?
F2 Te1 F4 174.18(14) . . ?
F2 Te1 F5 90.3(2) . . ?
F3 Te1 F1 86.54(18) . . ?
F3 Te1 F4 90.1(2) . . ?
F3 Te1 F5 173.12(19) . . ?
F5 Te1 F1 86.70(18) . . ?
F5 Te1 F4 88.2(2) . . ?
O1 Te1 F1 178.98(17) . . ?
O1 Te1 F2 92.48(14) . . ?
O1 Te1 F3 92.45(15) . . ?
O1 Te1 F4 93.24(13) . . ?
O1 Te1 F5 94.30(17) . . ?
F7 Te2 F6 86.70(17) . . ?
F7 Te2 F10 89.39(15) . . ?
F8 Te2 F6 86.64(16) . . ?
F8 Te2 F7 89.03(14) . . ?
F8 Te2 F9 91.03(15) . . ?
F8 Te2 F10 173.47(14) . . ?
F9 Te2 F6 87.04(17) . . ?
F9 Te2 F7 173.73(14) . . ?
F9 Te2 F10 89.85(15) . . ?
F10 Te2 F6 86.95(17) . . ?
O2 Te2 F6 178.63(17) . . ?
O2 Te2 F7 92.25(13) . . ?
O2 Te2 F8 92.46(12) . . ?
O2 Te2 F9 94.01(12) . . ?
O2 Te2 F10 93.93(13) . . ?
F11 Te3 F12 86.63(15) . . ?
F13 Te3 F11 87.13(17) . . ?
F13 Te3 F12 88.97(16) . . ?
F14 Te3 F11 87.55(15) . . ?
F14 Te3 F12 174.06(15) . . ?
F14 Te3 F13 89.51(18) . . ?
F14 Te3 F15 91.20(17) . . ?
F15 Te3 F11 87.14(16) . . ?
F15 Te3 F12 89.74(16) . . ?
F15 Te3 F13 174.19(15) . . ?
O3 Te3 F11 179.80(17) . . ?
O3 Te3 F12 93.55(13) . . ?
O3 Te3 F13 92.93(14) . . ?
O3 Te3 F14 92.26(14) . . ?
O3 Te3 F15 92.80(14) . . ?
F16 Te4 F17 86.86(11) . . ?
F16 Te4 F18 88.15(13) . . ?
F16 Te4 F19 87.17(12) . . ?
F16 Te4 F20 87.10(13) . . ?
F18 Te4 F17 90.42(13) . . ?
F18 Te4 F19 90.15(14) . . ?
F18 Te4 F20 175.24(13) . . ?
F19 Te4 F17 173.98(10) . . ?
F19 Te4 F20 89.83(13) . . ?
F20 Te4 F17 89.11(12) . . ?
O4 Te4 F16 178.01(13) . . ?
O4 Te4 F17 91.72(12) . . ?
O4 Te4 F18 93.27(13) . . ?
O4 Te4 F19 94.23(12) . . ?
O4 Te4 F20 91.48(12) . . ?
O2 Al1 O1 108.41(14) . . ?
O2 Al1 O4 110.50(13) . . ?
O3 Al1 O1 109.18(16) . . ?
O3 Al1 O2 110.40(14) . . ?
O3 Al1 O4 111.73(14) . . ?
O4 Al1 O1 106.48(14) . . ?
Al1 O1 Te1 137.21(16) . . ?
Al1 O2 Te2 141.62(16) . . ?
Al1 O3 Te3 143.03(17) . . ?
Al1 O4 Te4 139.11(16) . . ?
C1 P1 C5 118.20(16) . . ?
C1 P1 C6 120.36(17) . . ?
C5 P1 C6 120.60(17) . . ?
C13 Si3 C4 108.78(16) . . ?
C13 Si3 C15 106.74(19) . . ?
C14 Si3 C4 111.12(15) . . ?
C14 Si3 C13 105.51(19) . . ?
C14 Si3 C15 115.12(18) . . ?
C15 Si3 C4 109.25(17) . . ?
C10 Si2 C2 110.86(15) . . ?
C10 Si2 C12 105.43(19) . . ?
C11 Si2 C2 109.45(15) . . ?
C11 Si2 C10 114.86(17) . . ?
C11 Si2 C12 107.30(18) . . ?
C12 Si2 C2 108.64(16) . . ?
C7 Si1 C1 109.14(15) . . ?
C8 Si1 C1 113.50(16) . . ?
C8 Si1 C7 102.61(19) . . ?
C8 Si1 C9 113.94(18) . . ?
C9 Si1 C1 105.91(15) . . ?
C9 Si1 C7 111.79(19) . . ?
C16 Si4 C5 106.31(18) . . ?
C16 Si4 C17 112.2(3) . . ?
C16 Si4 C18 112.6(2) . . ?
C17 Si4 C5 109.14(19) . . ?
C18 Si4 C5 114.41(18) . . ?
C18 Si4 C17 102.3(2) . . ?
P1 C1 Si1 116.34(17) . . ?
C2 C1 P1 114.4(2) . . ?
C2 C1 Si1 129.2(2) . . ?
C1 C2 Si2 126.1(2) . . ?
C1 C2 C3 122.9(3) . . ?
C3 C2 Si2 111.0(2) . . ?
C2 C3 H3 116.4 . . ?
C2 C3 C4 127.2(3) . . ?
C4 C3 H3 116.4 . . ?
C3 C4 Si3 111.3(2) . . ?
C5 C4 Si3 126.0(2) . . ?
C5 C4 C3 122.7(3) . . ?
P1 C5 Si4 115.87(18) . . ?
C4 C5 P1 114.5(2) . . ?
C4 C5 Si4 129.7(2) . . ?
P1 C6 H6A 109.5 . . ?
P1 C6 H6B 109.5 . . ?
P1 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 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 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 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si4 C18 H18A 109.5 . . ?
Si4 C18 H18B 109.5 . . ?
Si4 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

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
F2 Te1 O1 Al1 -161.7(3) . . . . ?
F3 Te1 O1 Al1 107.5(3) . . . . ?
F4 Te1 O1 Al1 17.3(3) . . . . ?
F5 Te1 O1 Al1 -71.2(3) . . . . ?
F7 Te2 O2 Al1 -142.7(3) . . . . ?
F8 Te2 O2 Al1 128.2(3) . . . . ?
F9 Te2 O2 Al1 36.9(3) . . . . ?
F10 Te2 O2 Al1 -53.2(3) . . . . ?
F12 Te3 O3 Al1 -38.1(3) . . . . ?
F13 Te3 O3 Al1 -127.2(3) . . . . ?
F14 Te3 O3 Al1 143.2(3) . . . . ?
F15 Te3 O3 Al1 51.9(3) . . . . ?
F17 Te4 O4 Al1 -139.9(3) . . . . ?
F18 Te4 O4 Al1 -49.4(3) . . . . ?
F19 Te4 O4 Al1 41.0(3) . . . . ?
F20 Te4 O4 Al1 130.9(3) . . . . ?
O1 Al1 O2 Te2 140.9(2) . . . . ?
O1 Al1 O3 Te3 104.6(3) . . . . ?
O1 Al1 O4 Te4 112.7(3) . . . . ?
O2 Al1 O1 Te1 -60.0(3) . . . . ?
O2 Al1 O3 Te3 -136.3(3) . . . . ?
O2 Al1 O4 Te4 -4.8(3) . . . . ?
O3 Al1 O1 Te1 60.3(3) . . . . ?
O3 Al1 O2 Te2 21.3(3) . . . . ?
O3 Al1 O4 Te4 -128.2(3) . . . . ?
O4 Al1 O1 Te1 -178.9(2) . . . . ?
O4 Al1 O2 Te2 -102.8(3) . . . . ?
O4 Al1 O3 Te3 -12.9(4) . . . . ?
P1 C1 C2 Si2 -176.55(16) . . . . ?
P1 C1 C2 C3 1.4(4) . . . . ?
Si3 C4 C5 P1 178.20(16) . . . . ?
Si3 C4 C5 Si4 -2.6(4) . . . . ?
Si2 C2 C3 C4 -179.2(2) . . . . ?
Si1 C1 C2 Si2 4.5(4) . . . . ?
Si1 C1 C2 C3 -177.6(2) . . . . ?
C1 P1 C5 Si4 -176.69(15) . . . . ?
C1 P1 C5 C4 2.6(3) . . . . ?
C1 C2 C3 C4 2.6(4) . . . . ?
C2 C3 C4 Si3 178.4(2) . . . . ?
C2 C3 C4 C5 -4.0(5) . . . . ?
C3 C4 C5 P1 1.0(4) . . . . ?
C3 C4 C5 Si4 -179.8(2) . . . . ?
C5 P1 C1 Si1 175.29(15) . . . . ?
C5 P1 C1 C2 -3.8(3) . . . . ?
C6 P1 C1 Si1 -15.2(3) . . . . ?
C6 P1 C1 C2 165.8(2) . . . . ?
C6 P1 C5 Si4 13.8(3) . . . . ?
C6 P1 C5 C4 -166.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_ntc_tms4_2
_database_code_depnum_ccdc_archive 'CCDC 2062244'
loop_
_audit_author_name
_audit_author_address
'Nathan T. Coles'
;FU Berlin
Germany
;
_audit_update_record             
;
2021-02-09 deposited with the CCDC.	2021-08-06 downloaded from the CCDC.
;
_audit_creation_date             2020-09-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
N.T.Coles@fu-berlin.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H37 P Si4'
_chemical_formula_sum            'C17 H37 P Si4'
_chemical_formula_weight         384.79
_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'
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'

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

_cell_length_a                   11.0213(5)
_cell_length_b                   11.8221(5)
_cell_length_c                   18.3959(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2396.89(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.76
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0954 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.9380.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.211
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            187764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.612
_diffrn_reflns_theta_min         2.759
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3075
_reflns_number_total             3375
_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 V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3375
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.330
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+0.9309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0849
_refine_special_details          
;The structure was found to be disordered across a special position. 
RIGU restraints were required for the phosphinine core (P1, C1-C5) 
to produce a stable model. SADI restraints were also used for all Si. 
This was chosen as this resulted in the shortening of Si2-C2 and 
lengthening of Si4-C5. Without these restraints C2-Si2 was found to be 
2.00 A (1.98 A with restraint) and C5-Si4 was found to be approximately 
1.7 A (1.82 A with restraint). These are closer to the bond lengths 
observed for the remaining Si-Cring bonds (1.90-1.91 A).,The structure was found to be disordered across a special position. RIGU restraints were required for the phosphinine core (P1, C1-C5) to produce a stable model. SADI restraints were also used for all Si-C distances. This was chosen as this resulted in the shortening of Si2-C2 and lengthening of Si4-C5. Without these restraints C2-Si2 was found to be 2.00 Å (1.98 Å with restraint) and C5-Si4 was found to be ~1.7 Å (1.82 Å with restraint). These are closer to the bond lengths observed for the remaining Si-Cring bonds (1.90-1.91 Å), which are typical of Si-Cring for this type of species .
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C1 \\sim Si1-C6 \\sim Si1-C8 \\sim Si1-C7
 with sigma of 0.02
 Si2-C2 \\sim Si2-C9 \\sim Si2-C10 \\sim Si2-C11
 with sigma of 0.02
 C2-C9 \\sim C2-C10 \\sim C2-C11 \\sim C9-C10 \\sim C9-C11 \\sim C10-C11
 with sigma of 0.04
 C1-C6 \\sim C1-C8 \\sim C1-C7 \\sim C6-C8 \\sim C6-C7 \\sim C8-C7
 with sigma of 0.04
 Si3-C4 \\sim Si3-C13 \\sim Si3-C14 \\sim Si3-C12
 with sigma of 0.02
 C4-C13 \\sim C4-C14 \\sim C4-C12 \\sim C13-C14 \\sim C13-C12 \\sim C14-C12
 with sigma of 0.04
 Si4-C5 \\sim Si4-C15 \\sim Si4-C16 \\sim Si4-C17
 with sigma of 0.02
 C5-C15 \\sim C5-C16 \\sim C5-C17 \\sim C16-C17 \\sim C16-C15 \\sim C17-C15
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 P1, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: P1(0.5) Si1(0.5) Si2(0.5) Si3(0.5) Si4(0.5) C1(0.5) C2(0.5)
 C3(0.5) H3(0.5) C4(0.5) C5(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C9(0.5) H9A(0.5)
 H9B(0.5) H9C(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) H11C(0.5) C12(0.5) H12A(0.5) H12B(0.5) H12C(0.5) C13(0.5) H13A(0.5)
 H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) H17A(0.5)
 H17B(0.5) H17C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
P1 P 0.54124(5) 0.44362(5) 0.59230(4) 0.02007(12) Uani 0.5 1 d . . P A -1
Si1 Si 0.3588(2) 0.5961(3) 0.66246(16) 0.0256(4) Uani 0.5 1 d D . P A -1
Si2 Si 0.2833(4) 0.7021(6) 0.4774(4) 0.0293(7) Uani 0.5 1 d D . P A -1
Si3 Si 0.6156(2) 0.4156(2) 0.34626(15) 0.0231(3) Uani 0.5 1 d D . P A -1
Si4 Si 0.7204(5) 0.3043(6) 0.5268(4) 0.0319(9) Uani 0.5 1 d D . P A -1
C1 C 0.4310(11) 0.5458(10) 0.5744(4) 0.0189(12) Uani 0.5 1 d D . P A -1
C2 C 0.4039(10) 0.5846(9) 0.5040(5) 0.0159(12) Uani 0.5 1 d D . P A -1
C3 C 0.46931(19) 0.53441(19) 0.44375(14) 0.0187(4) Uani 0.5 1 d . . P A -1
H3 H 0.447439 0.563245 0.397366 0.022 Uiso 0.5 1 calc R U P A -1
C4 C 0.5605(11) 0.4495(10) 0.4421(4) 0.0171(11) Uani 0.5 1 d D . P A -1
C5 C 0.5976(11) 0.4039(10) 0.5098(5) 0.0197(14) Uani 0.5 1 d D . P A -1
C6 C 0.4309(7) 0.7321(7) 0.6899(6) 0.0419(17) Uani 0.5 1 d D . P A -1
H6A H 0.513049 0.717409 0.707968 0.063 Uiso 0.5 1 calc R U P A -1
H6B H 0.382562 0.767528 0.728436 0.063 Uiso 0.5 1 calc R U P A -1
H6C H 0.434913 0.782820 0.647889 0.063 Uiso 0.5 1 calc R U P A -1
C7 C 0.3875(3) 0.4903(3) 0.73628(16) 0.0364(7) Uani 0.5 1 d D . P A -1
H7A H 0.354467 0.416660 0.721834 0.055 Uiso 0.5 1 calc R U P A -1
H7B H 0.348094 0.515427 0.781203 0.055 Uiso 0.5 1 calc R U P A -1
H7C H 0.475093 0.483318 0.744421 0.055 Uiso 0.5 1 calc R U P A -1
C8 C 0.1904(8) 0.6067(9) 0.6578(6) 0.047(2) Uani 0.5 1 d D . P A -1
H8A H 0.167676 0.668937 0.625330 0.071 Uiso 0.5 1 calc R U P A -1
H8B H 0.157966 0.621253 0.706540 0.071 Uiso 0.5 1 calc R U P A -1
H8C H 0.156904 0.535664 0.639144 0.071 Uiso 0.5 1 calc R U P A -1
C9 C 0.2847(13) 0.8303(11) 0.5399(9) 0.0362(17) Uani 0.5 1 d D . P A -1
H9A H 0.266396 0.806365 0.589681 0.054 Uiso 0.5 1 calc R U P A -1
H9B H 0.223404 0.884699 0.523573 0.054 Uiso 0.5 1 calc R U P A -1
H9C H 0.365008 0.865794 0.538505 0.054 Uiso 0.5 1 calc R U P A -1
C10 C 0.1242(9) 0.6337(11) 0.4758(8) 0.0369(14) Uani 0.5 1 d D . P A -1
H10A H 0.116175 0.586520 0.432231 0.055 Uiso 0.5 1 calc R U P A -1
H10B H 0.062232 0.693168 0.474964 0.055 Uiso 0.5 1 calc R U P A -1
H10C H 0.113448 0.586845 0.519210 0.055 Uiso 0.5 1 calc R U P A -1
C11 C 0.3256(4) 0.7451(4) 0.3797(3) 0.0414(9) Uani 0.5 1 d D . P A -1
H11A H 0.409598 0.772278 0.378699 0.062 Uiso 0.5 1 calc R U P A -1
H11B H 0.271208 0.805478 0.363259 0.062 Uiso 0.5 1 calc R U P A -1
H11C H 0.317512 0.679537 0.347521 0.062 Uiso 0.5 1 calc R U P A -1
C12 C 0.5719(4) 0.5332(3) 0.28284(16) 0.0373(7) Uani 0.5 1 d D . P A -1
H12A H 0.483287 0.536333 0.278535 0.056 Uiso 0.5 1 calc R U P A -1
H12B H 0.607555 0.519485 0.234857 0.056 Uiso 0.5 1 calc R U P A -1
H12C H 0.601899 0.605320 0.302041 0.056 Uiso 0.5 1 calc R U P A -1
C13 C 0.5380(6) 0.2843(7) 0.3117(5) 0.0329(12) Uani 0.5 1 d D . P A -1
H13A H 0.565129 0.218758 0.339989 0.049 Uiso 0.5 1 calc R U P A -1
H13B H 0.558654 0.272895 0.260349 0.049 Uiso 0.5 1 calc R U P A -1
H13C H 0.449983 0.292775 0.316615 0.049 Uiso 0.5 1 calc R U P A -1
C14 C 0.7852(7) 0.4060(7) 0.3362(6) 0.0343(13) Uani 0.5 1 d D . P A -1
H14A H 0.821567 0.479812 0.346871 0.052 Uiso 0.5 1 calc R U P A -1
H14B H 0.805343 0.383809 0.286314 0.052 Uiso 0.5 1 calc R U P A -1
H14C H 0.816972 0.349461 0.370172 0.052 Uiso 0.5 1 calc R U P A -1
C15 C 0.7285(15) 0.1841(11) 0.4651(9) 0.043(2) Uani 0.5 1 d D . P A -1
H15A H 0.652265 0.141575 0.467259 0.065 Uiso 0.5 1 calc R U P A -1
H15B H 0.795832 0.134791 0.479532 0.065 Uiso 0.5 1 calc R U P A -1
H15C H 0.741827 0.211192 0.415421 0.065 Uiso 0.5 1 calc R U P A -1
C16 C 0.8634(10) 0.3791(12) 0.5347(8) 0.051(3) Uani 0.5 1 d D . P A -1
H16A H 0.884365 0.413049 0.487788 0.076 Uiso 0.5 1 calc R U P A -1
H16B H 0.927209 0.325954 0.549240 0.076 Uiso 0.5 1 calc R U P A -1
H16C H 0.855955 0.438706 0.571493 0.076 Uiso 0.5 1 calc R U P A -1
C17 C 0.7033(4) 0.2217(4) 0.6130(3) 0.0447(10) Uani 0.5 1 d D . P A -1
H17A H 0.714318 0.272112 0.654729 0.067 Uiso 0.5 1 calc R U P A -1
H17B H 0.764461 0.161560 0.614505 0.067 Uiso 0.5 1 calc R U P A -1
H17C H 0.622056 0.188008 0.614839 0.067 Uiso 0.5 1 calc R U P A -1


_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
P1 C1 1.745(11) . ?
P1 C5 1.707(11) . ?
Si1 C1 1.900(7) . ?
Si1 C6 1.863(9) . ?
Si1 C7 1.874(4) . ?
Si1 C8 1.862(8) . ?
Si2 C2 1.983(8) . ?
Si2 C9 1.902(11) . ?
Si2 C10 1.931(10) . ?
Si2 C11 1.925(7) . ?
Si3 C4 1.907(7) . ?
Si3 C12 1.879(4) . ?
Si3 C13 1.883(8) . ?
Si3 C14 1.882(8) . ?
Si4 C5 1.820(10) . ?
Si4 C15 1.821(11) . ?
Si4 C16 1.813(11) . ?
Si4 C17 1.872(6) . ?
C1 C2 1.406(9) . ?
C2 C3 1.449(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.421(11) . ?
C4 C5 1.417(10) . ?
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 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

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
C5 P1 C1 106.0(4) . . ?
C6 Si1 C1 108.8(5) . . ?
C6 Si1 C7 107.9(4) . . ?
C7 Si1 C1 109.8(4) . . ?
C8 Si1 C1 113.6(5) . . ?
C8 Si1 C6 112.3(4) . . ?
C8 Si1 C7 104.3(4) . . ?
C9 Si2 C2 113.8(6) . . ?
C9 Si2 C10 110.5(6) . . ?
C9 Si2 C11 110.6(6) . . ?
C10 Si2 C2 108.6(6) . . ?
C11 Si2 C2 104.7(4) . . ?
C11 Si2 C10 108.4(6) . . ?
C12 Si3 C4 109.7(4) . . ?
C12 Si3 C13 106.5(3) . . ?
C12 Si3 C14 103.8(3) . . ?
C13 Si3 C4 110.0(5) . . ?
C14 Si3 C4 114.8(5) . . ?
C14 Si3 C13 111.6(3) . . ?
C5 Si4 C15 115.7(7) . . ?
C5 Si4 C17 114.1(4) . . ?
C15 Si4 C17 97.2(6) . . ?
C16 Si4 C5 110.2(7) . . ?
C16 Si4 C15 112.8(7) . . ?
C16 Si4 C17 105.9(6) . . ?
P1 C1 Si1 110.3(5) . . ?
C2 C1 P1 123.2(6) . . ?
C2 C1 Si1 126.4(8) . . ?
C1 C2 Si2 126.7(8) . . ?
C1 C2 C3 117.7(7) . . ?
C3 C2 Si2 115.6(5) . . ?
C2 C3 H3 114.4 . . ?
C4 C3 C2 131.1(5) . . ?
C4 C3 H3 114.4 . . ?
C3 C4 Si3 113.2(6) . . ?
C5 C4 Si3 129.8(9) . . ?
C5 C4 C3 117.0(6) . . ?
P1 C5 Si4 107.2(5) . . ?
C4 C5 P1 124.9(8) . . ?
C4 C5 Si4 127.7(8) . . ?
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 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
Si1 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 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C13 H13A 109.5 . . ?
Si3 C13 H13B 109.5 . . ?
Si3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si4 C15 H15A 109.5 . . ?
Si4 C15 H15B 109.5 . . ?
Si4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si4 C16 H16A 109.5 . . ?
Si4 C16 H16B 109.5 . . ?
Si4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si4 C17 H17A 109.5 . . ?
Si4 C17 H17B 109.5 . . ?
Si4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

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
P1 C1 C2 Si2 -178.7(8) . . . . ?
P1 C1 C2 C3 1.6(15) . . . . ?
Si1 C1 C2 Si2 0.0(16) . . . . ?
Si1 C1 C2 C3 -179.6(8) . . . . ?
Si2 C2 C3 C4 180.0(7) . . . . ?
Si3 C4 C5 P1 179.2(8) . . . . ?
Si3 C4 C5 Si4 5.3(18) . . . . ?
C1 P1 C5 Si4 176.1(6) . . . . ?
C1 P1 C5 C4 1.1(12) . . . . ?
C1 C2 C3 C4 -0.3(13) . . . . ?
C2 C3 C4 Si3 -180.0(7) . . . . ?
C2 C3 C4 C5 -0.5(12) . . . . ?
C3 C4 C5 P1 -0.1(16) . . . . ?
C3 C4 C5 Si4 -174.1(9) . . . . ?
C5 P1 C1 Si1 179.2(6) . . . . ?
C5 P1 C1 C2 -1.9(10) . . . . ?
C15 Si4 C5 P1 139.9(8) . . . . ?
C15 Si4 C5 C4 -45.3(14) . . . . ?
C16 Si4 C5 P1 -90.6(8) . . . . ?
C16 Si4 C5 C4 84.3(13) . . . . ?
C17 Si4 C5 P1 28.4(9) . . . . ?
C17 Si4 C5 C4 -156.8(11) . . . . ?

_olex2_submission_original_sample_id NTC-TMS4_2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_chemical_properties_physical    Air-sensitive
