# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_s21sel6
_database_code_depnum_ccdc_archive 'CCDC 2129310'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28'
_chemical_formula_sum            'C32 H28'
_chemical_formula_weight         412.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   11.9223(4)
_cell_length_b                   4.9868(2)
_cell_length_c                   18.1330(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.446(3)
_cell_angle_gamma                90
_cell_volume                     1066.39(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2562
_cell_measurement_theta_min      4.7700
_cell_measurement_theta_max      72.6540

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.543
_shelx_estimated_absorpt_T_min   0.895
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_T_min  0.85750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.783
_oxdiff_exptl_absorpt_empirical_full_max 1.239
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            6420
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.748
_diffrn_reflns_theta_max         72.881
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.724
_diffrn_reflns_point_group_measured_fraction_full 0.750
_reflns_number_total             3075
_reflns_number_gt                2758
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.321
_reflns_Friedel_fraction_max     0.400
_reflns_Friedel_fraction_full    0.429

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

_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0510P)²+0.0537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.4(10)
_chemical_absolute_configuration unk
_refine_ls_number_reflns         3075
_refine_ls_number_parameters     293
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5548(2) 0.0692(5) 0.18614(14) 0.0226(5) Uani 1 1 d . . . . .
H1A H 0.524102 -0.085695 0.155496 0.027 Uiso 1 1 calc R U . . .
H1B H 0.605569 -0.000982 0.230026 0.027 Uiso 1 1 calc R U . . .
C2 C 0.6230(2) 0.2453(5) 0.14055(14) 0.0212(5) Uani 1 1 d . . . . .
C3 C 0.6063(2) 0.2255(6) 0.06308(15) 0.0243(6) Uani 1 1 d . . . . .
H3 H 0.552181 0.100776 0.039652 0.029 Uiso 1 1 calc R U . . .
C4 C 0.6660(2) 0.3817(6) 0.01928(14) 0.0257(6) Uani 1 1 d . . . . .
H4 H 0.652038 0.362702 -0.033398 0.031 Uiso 1 1 calc R U . . .
C5 C 0.7465(2) 0.5674(5) 0.05137(14) 0.0225(5) Uani 1 1 d . . . . .
C6 C 0.8118(2) 0.7295(6) 0.00756(15) 0.0269(6) Uani 1 1 d . . . . .
H6 H 0.800877 0.709326 -0.045102 0.032 Uiso 1 1 calc R U . . .
C7 C 0.8879(2) 0.9086(6) 0.03958(15) 0.0279(6) Uani 1 1 d . . . . .
H7 H 0.929140 1.014209 0.009201 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9078(2) 0.9427(6) 0.11899(15) 0.0245(6) Uani 1 1 d . . . . .
C9 C 0.9857(2) 1.1318(6) 0.15330(17) 0.0289(6) Uani 1 1 d . . . . .
H9 H 1.025537 1.243439 0.123517 0.035 Uiso 1 1 calc R U . . .
C10 C 1.0051(2) 1.1572(6) 0.23029(17) 0.0322(7) Uani 1 1 d . . . . .
H10 H 1.058834 1.284521 0.252766 0.039 Uiso 1 1 calc R U . . .
C11 C 0.9469(2) 0.9983(6) 0.27478(15) 0.0289(6) Uani 1 1 d . . . . .
H11 H 0.961595 1.017395 0.327441 0.035 Uiso 1 1 calc R U . . .
C12 C 0.8665(2) 0.8096(6) 0.24298(15) 0.0243(6) Uani 1 1 d . . . . .
C13 C 0.8033(2) 0.6454(6) 0.28655(14) 0.0245(6) Uani 1 1 d . . . . .
H13 H 0.816122 0.662460 0.339297 0.029 Uiso 1 1 calc R U . . .
C14 C 0.7256(2) 0.4661(5) 0.25477(14) 0.0224(5) Uani 1 1 d . . . . .
H14 H 0.685198 0.360612 0.285671 0.027 Uiso 1 1 calc R U . . .
C15 C 0.70300(19) 0.4318(5) 0.17509(14) 0.0202(5) Uani 1 1 d . . . . .
C16 C 0.7651(2) 0.5925(5) 0.13043(14) 0.0206(5) Uani 1 1 d . . . . .
C17 C 0.8467(2) 0.7813(5) 0.16399(15) 0.0222(5) Uani 1 1 d . . . . .
C18 C 0.4576(2) 0.2213(5) 0.21239(14) 0.0197(5) Uani 1 1 d . . . . .
C19 C 0.41798(19) 0.2298(5) 0.28164(14) 0.0187(5) Uani 1 1 d . . . . .
C20 C 0.4516(2) 0.0769(5) 0.34684(14) 0.0197(5) Uani 1 1 d . . . . .
C21 C 0.5332(2) -0.1530(5) 0.34457(15) 0.0244(5) Uani 1 1 d . . . . .
H21A H 0.529123 -0.272143 0.387072 0.037 Uiso 1 1 calc R U . . .
H21B H 0.610438 -0.082962 0.347118 0.037 Uiso 1 1 calc R U . . .
H21C H 0.512918 -0.253253 0.298037 0.037 Uiso 1 1 calc R U . . .
C22 C 0.4148(2) 0.1164(6) 0.41569(14) 0.0244(5) Uani 1 1 d . . . . .
H22 H 0.447635 -0.004942 0.453149 0.029 Uiso 1 1 calc R U . . .
C23 C 0.3393(2) 0.2987(6) 0.44069(14) 0.0235(6) Uani 1 1 d . . . . .
H23 H 0.335507 0.289426 0.492586 0.028 Uiso 1 1 calc R U . . .
C24 C 0.2693(2) 0.4903(5) 0.40246(14) 0.0216(5) Uani 1 1 d . . . . .
C25 C 0.1878(2) 0.6513(6) 0.44261(14) 0.0252(6) Uani 1 1 d . . . . .
H25 H 0.180409 0.833294 0.419221 0.030 Uiso 1 1 calc R U . . .
C26 C 0.2256(3) 0.6908(7) 0.52601(15) 0.0349(7) Uani 1 1 d . . . . .
H26A H 0.220939 0.519517 0.551902 0.052 Uiso 1 1 calc R U . . .
H26B H 0.176006 0.822209 0.545230 0.052 Uiso 1 1 calc R U . . .
H26C H 0.303941 0.755946 0.534476 0.052 Uiso 1 1 calc R U . . .
C27 C 0.0707(2) 0.5195(7) 0.42876(16) 0.0356(7) Uani 1 1 d . . . . .
H27A H 0.017302 0.625030 0.453117 0.053 Uiso 1 1 calc R U . . .
H27B H 0.075681 0.337391 0.449268 0.053 Uiso 1 1 calc R U . . .
H27C H 0.044240 0.511778 0.375021 0.053 Uiso 1 1 calc R U . . .
C28 C 0.2627(2) 0.5376(5) 0.32566(14) 0.0205(5) Uani 1 1 d . . . . .
H28 H 0.206776 0.665058 0.306373 0.025 Uiso 1 1 calc R U . . .
C29 C 0.3230(2) 0.4316(5) 0.27325(14) 0.0185(5) Uani 1 1 d . . . . .
C30 C 0.3071(2) 0.5188(5) 0.19787(13) 0.0202(5) Uani 1 1 d . . . . .
C31 C 0.2196(2) 0.7169(6) 0.16409(14) 0.0232(5) Uani 1 1 d . . . . .
H31A H 0.242632 0.897989 0.181030 0.035 Uiso 1 1 calc R U . . .
H31B H 0.146370 0.673586 0.179550 0.035 Uiso 1 1 calc R U . . .
H31C H 0.212816 0.708489 0.109616 0.035 Uiso 1 1 calc R U . . .
C32 C 0.3885(2) 0.3961(5) 0.16315(14) 0.0214(5) Uani 1 1 d . . . . .
H32 H 0.397422 0.424734 0.112542 0.026 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
C1 C18 1.519(3) . ?
C1 C2 1.521(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.393(3) . ?
C2 C15 1.411(4) . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C5 C16 1.424(3) . ?
C5 C6 1.440(4) . ?
C6 C7 1.342(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.435(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.403(4) . ?
C8 C17 1.421(4) . ?
C9 C10 1.387(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.405(4) . ?
C11 H11 0.9500 . ?
C12 C17 1.424(4) . ?
C12 C13 1.427(4) . ?
C13 C14 1.354(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.440(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.422(3) . ?
C16 C17 1.425(3) . ?
C18 C19 1.406(3) . ?
C18 C32 1.421(3) . ?
C19 C20 1.415(3) . ?
C19 C29 1.505(3) . ?
C20 C22 1.397(4) . ?
C20 C21 1.507(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.401(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.386(4) . ?
C23 H23 0.9500 . ?
C24 C28 1.403(3) . ?
C24 C25 1.525(3) . ?
C25 C26 1.526(4) . ?
C25 C27 1.530(4) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.379(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.420(3) . ?
C30 C32 1.376(3) . ?
C30 C31 1.500(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 C1 C2 112.1(2) . . ?
C18 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
C18 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C15 118.8(2) . . ?
C3 C2 C1 119.9(2) . . ?
C15 C2 C1 121.3(2) . . ?
C4 C3 C2 122.0(2) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 121.0(2) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C16 118.3(2) . . ?
C4 C5 C6 122.4(2) . . ?
C16 C5 C6 119.3(2) . . ?
C7 C6 C5 121.4(2) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C6 C7 C8 121.0(3) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C17 119.2(2) . . ?
C9 C8 C7 121.7(3) . . ?
C17 C8 C7 119.1(2) . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C10 C11 C12 120.9(3) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C17 118.8(2) . . ?
C11 C12 C13 122.7(2) . . ?
C17 C12 C13 118.5(2) . . ?
C14 C13 C12 121.8(2) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 121.4(2) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C2 C15 C16 119.5(2) . . ?
C2 C15 C14 122.6(2) . . ?
C16 C15 C14 117.9(2) . . ?
C15 C16 C5 120.5(2) . . ?
C15 C16 C17 120.6(2) . . ?
C5 C16 C17 118.9(2) . . ?
C8 C17 C12 119.9(2) . . ?
C8 C17 C16 120.3(2) . . ?
C12 C17 C16 119.8(2) . . ?
C19 C18 C32 107.6(2) . . ?
C19 C18 C1 131.8(2) . . ?
C32 C18 C1 120.5(2) . . ?
C18 C19 C20 129.7(2) . . ?
C18 C19 C29 106.0(2) . . ?
C20 C19 C29 124.2(2) . . ?
C22 C20 C19 125.7(2) . . ?
C22 C20 C21 114.9(2) . . ?
C19 C20 C21 119.5(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 C23 133.0(2) . . ?
C20 C22 H22 113.5 . . ?
C23 C22 H22 113.5 . . ?
C24 C23 C22 130.9(2) . . ?
C24 C23 H23 114.6 . . ?
C22 C23 H23 114.6 . . ?
C23 C24 C28 123.6(2) . . ?
C23 C24 C25 120.2(2) . . ?
C28 C24 C25 116.0(2) . . ?
C24 C25 C26 115.2(2) . . ?
C24 C25 C27 109.0(2) . . ?
C26 C25 C27 110.3(2) . . ?
C24 C25 H25 107.4 . . ?
C26 C25 H25 107.4 . . ?
C27 C25 H25 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C24 131.4(2) . . ?
C29 C28 H28 114.3 . . ?
C24 C28 H28 114.3 . . ?
C28 C29 C30 122.4(2) . . ?
C28 C29 C19 130.3(2) . . ?
C30 C29 C19 107.1(2) . . ?
C32 C30 C29 107.5(2) . . ?
C32 C30 C31 126.9(2) . . ?
C29 C30 C31 125.6(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C18 111.6(2) . . ?
C30 C32 H32 124.2 . . ?
C18 C32 H32 124.2 . . ?

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
C18 C1 C2 C3 -101.6(3) . . . . ?
C18 C1 C2 C15 77.9(3) . . . . ?
C15 C2 C3 C4 0.3(4) . . . . ?
C1 C2 C3 C4 179.8(2) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C3 C4 C5 C16 -0.3(4) . . . . ?
C3 C4 C5 C6 178.7(3) . . . . ?
C4 C5 C6 C7 179.3(3) . . . . ?
C16 C5 C6 C7 -1.7(4) . . . . ?
C5 C6 C7 C8 0.7(4) . . . . ?
C6 C7 C8 C9 -179.0(3) . . . . ?
C6 C7 C8 C17 0.8(4) . . . . ?
C17 C8 C9 C10 1.5(4) . . . . ?
C7 C8 C9 C10 -178.7(3) . . . . ?
C8 C9 C10 C11 -0.8(4) . . . . ?
C9 C10 C11 C12 -0.4(4) . . . . ?
C10 C11 C12 C17 0.8(4) . . . . ?
C10 C11 C12 C13 -178.9(3) . . . . ?
C11 C12 C13 C14 179.5(2) . . . . ?
C17 C12 C13 C14 -0.2(4) . . . . ?
C12 C13 C14 C15 0.1(4) . . . . ?
C3 C2 C15 C16 -0.6(3) . . . . ?
C1 C2 C15 C16 179.9(2) . . . . ?
C3 C2 C15 C14 179.9(2) . . . . ?
C1 C2 C15 C14 0.4(4) . . . . ?
C13 C14 C15 C2 179.6(2) . . . . ?
C13 C14 C15 C16 0.1(4) . . . . ?
C2 C15 C16 C5 0.4(3) . . . . ?
C14 C15 C16 C5 179.9(2) . . . . ?
C2 C15 C16 C17 -179.7(2) . . . . ?
C14 C15 C16 C17 -0.2(3) . . . . ?
C4 C5 C16 C15 0.1(3) . . . . ?
C6 C5 C16 C15 -179.0(2) . . . . ?
C4 C5 C16 C17 -179.8(2) . . . . ?
C6 C5 C16 C17 1.1(4) . . . . ?
C9 C8 C17 C12 -1.1(4) . . . . ?
C7 C8 C17 C12 179.1(2) . . . . ?
C9 C8 C17 C16 178.5(2) . . . . ?
C7 C8 C17 C16 -1.3(4) . . . . ?
C11 C12 C17 C8 0.0(4) . . . . ?
C13 C12 C17 C8 179.7(2) . . . . ?
C11 C12 C17 C16 -179.6(2) . . . . ?
C13 C12 C17 C16 0.1(3) . . . . ?
C15 C16 C17 C8 -179.5(2) . . . . ?
C5 C16 C17 C8 0.4(3) . . . . ?
C15 C16 C17 C12 0.1(4) . . . . ?
C5 C16 C17 C12 180.0(2) . . . . ?
C2 C1 C18 C19 -135.7(3) . . . . ?
C2 C1 C18 C32 43.5(3) . . . . ?
C32 C18 C19 C20 174.2(2) . . . . ?
C1 C18 C19 C20 -6.5(5) . . . . ?
C32 C18 C19 C29 -2.6(3) . . . . ?
C1 C18 C19 C29 176.6(3) . . . . ?
C18 C19 C20 C22 173.6(3) . . . . ?
C29 C19 C20 C22 -10.1(4) . . . . ?
C18 C19 C20 C21 -7.1(4) . . . . ?
C29 C19 C20 C21 169.2(2) . . . . ?
C19 C20 C22 C23 0.8(5) . . . . ?
C21 C20 C22 C23 -178.5(3) . . . . ?
C20 C22 C23 C24 5.4(5) . . . . ?
C22 C23 C24 C28 -0.4(5) . . . . ?
C22 C23 C24 C25 175.5(3) . . . . ?
C23 C24 C25 C26 28.2(4) . . . . ?
C28 C24 C25 C26 -155.6(3) . . . . ?
C23 C24 C25 C27 -96.4(3) . . . . ?
C28 C24 C25 C27 79.8(3) . . . . ?
C23 C24 C28 C29 -4.7(4) . . . . ?
C25 C24 C28 C29 179.3(3) . . . . ?
C24 C28 C29 C30 -176.4(3) . . . . ?
C24 C28 C29 C19 -0.8(5) . . . . ?
C18 C19 C29 C28 -172.5(3) . . . . ?
C20 C19 C29 C28 10.4(4) . . . . ?
C18 C19 C29 C30 3.6(3) . . . . ?
C20 C19 C29 C30 -173.4(2) . . . . ?
C28 C29 C30 C32 173.3(2) . . . . ?
C19 C29 C30 C32 -3.2(3) . . . . ?
C28 C29 C30 C31 -4.6(4) . . . . ?
C19 C29 C30 C31 178.9(2) . . . . ?
C29 C30 C32 C18 1.7(3) . . . . ?
C31 C30 C32 C18 179.5(2) . . . . ?
C19 C18 C32 C30 0.7(3) . . . . ?
C1 C18 C32 C30 -178.7(2) . . . . ?

_refine_diff_density_max         0.175
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.039

####################################################################### 
# 
# 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_e21sel2
_database_code_depnum_ccdc_archive 'CCDC 2129311'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H26 N S, F6 P'
_chemical_formula_sum            'C22 H26 F6 N P S'
_chemical_formula_weight         481.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   8.3278(3)
_cell_length_b                   12.1332(3)
_cell_length_c                   21.8785(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.317(3)
_cell_angle_gamma                90
_cell_volume                     2187.42(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13989
_cell_measurement_theta_min      3.7170
_cell_measurement_theta_max      27.5200

_exptl_crystal_description       prism
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.706
_exptl_crystal_size_min          0.482
_exptl_absorpt_coefficient_mu    0.282
_shelx_estimated_absorpt_T_min   0.817
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_T_min  0.91084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.879
_oxdiff_exptl_absorpt_empirical_full_max 1.190
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0734
_diffrn_reflns_number            35610
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.988
_diffrn_reflns_theta_max         27.440
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4984
_reflns_number_gt                4422
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;

_refine_special_details          
;
the PF6 anion shows rotational disorder in the ratio 75:25.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0821P)²+2.7651P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4984
_refine_ls_number_parameters     341
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S 0.91002(7) 0.36576(5) 0.54332(3) 0.02427(18) Uani 1 1 d . . . . .
N N 1.1031(3) 0.2169(2) 0.60694(12) 0.0344(5) Uani 1 1 d . . . . .
C1 C 1.0381(3) 0.3161(2) 0.60715(12) 0.0276(5) Uani 1 1 d . . . . .
C2 C 1.0800(4) 0.1467(3) 0.55198(16) 0.0418(7) Uani 1 1 d . . . . .
H2A H 0.984053 0.171318 0.524035 0.063 Uiso 1 1 calc R U . . .
H2B H 1.064727 0.070142 0.564239 0.063 Uiso 1 1 calc R U . . .
H2C H 1.175815 0.151565 0.530847 0.063 Uiso 1 1 calc R U . . .
C3 C 1.2075(4) 0.1738(3) 0.66205(17) 0.0443(8) Uani 1 1 d . . . . .
H3A H 1.255749 0.103711 0.651837 0.066 Uiso 1 1 calc R U . . .
H3B H 1.142250 0.162108 0.695329 0.066 Uiso 1 1 calc R U . . .
H3C H 1.293941 0.227015 0.675563 0.066 Uiso 1 1 calc R U . . .
C4 C 1.0581(3) 0.3942(2) 0.65625(12) 0.0316(6) Uani 1 1 d . . . . .
H4 H 1.121740 0.381525 0.695261 0.038 Uiso 1 1 calc R U . . .
C5 C 0.9753(3) 0.4892(2) 0.64074(12) 0.0293(5) Uani 1 1 d . . . . .
H5 H 0.979499 0.550460 0.667985 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8821(3) 0.4905(2) 0.58093(11) 0.0236(5) Uani 1 1 d . . . . .
C7 C 0.7836(3) 0.5770(2) 0.55874(11) 0.0237(5) Uani 1 1 d . . . . .
H7 H 0.782962 0.637446 0.586286 0.028 Uiso 1 1 calc R U . . .
C8 C 0.6835(3) 0.58967(19) 0.50137(11) 0.0214(5) Uani 1 1 d . . . . .
C9 C 0.6807(3) 0.5165(2) 0.44982(11) 0.0228(5) Uani 1 1 d . . . . .
H9 H 0.739583 0.449372 0.450758 0.027 Uiso 1 1 calc R U . . .
C10 C 0.5819(3) 0.5560(2) 0.39897(11) 0.0238(5) Uani 1 1 d . . . . .
C11 C 0.5485(4) 0.5013(2) 0.33727(13) 0.0340(6) Uani 1 1 d . . . . .
H11A H 0.576648 0.551656 0.305426 0.051 Uiso 1 1 calc R U . . .
H11B H 0.433091 0.482374 0.328356 0.051 Uiso 1 1 calc R U . . .
H11C H 0.613823 0.434114 0.337560 0.051 Uiso 1 1 calc R U . . .
C12 C 0.5155(3) 0.65859(19) 0.41525(11) 0.0212(5) Uani 1 1 d . . . . .
C13 C 0.4170(3) 0.7209(2) 0.37133(12) 0.0252(5) Uani 1 1 d . . . . .
H13 H 0.395514 0.688079 0.331568 0.030 Uiso 1 1 calc R U . . .
C14 C 0.3452(3) 0.8229(2) 0.37613(12) 0.0266(5) Uani 1 1 d . . . . .
C15 C 0.2520(3) 0.8775(2) 0.31860(13) 0.0326(6) Uani 1 1 d . . . . .
H15 H 0.153650 0.913121 0.331232 0.039 Uiso 1 1 calc R U . . .
C16 C 0.1939(4) 0.7978(3) 0.26631(15) 0.0443(8) Uani 1 1 d . . . . .
H16A H 0.117632 0.835625 0.234881 0.066 Uiso 1 1 calc R U . . .
H16B H 0.139489 0.734995 0.282649 0.066 Uiso 1 1 calc R U . . .
H16C H 0.287078 0.771493 0.247754 0.066 Uiso 1 1 calc R U . . .
C17 C 0.3565(4) 0.9695(3) 0.29614(15) 0.0457(8) Uani 1 1 d . . . . .
H17A H 0.454872 0.937369 0.283782 0.068 Uiso 1 1 calc R U . . .
H17B H 0.386651 1.022530 0.329622 0.068 Uiso 1 1 calc R U . . .
H17C H 0.294483 1.007182 0.260728 0.068 Uiso 1 1 calc R U . . .
C18 C 0.3527(3) 0.8817(2) 0.43178(14) 0.0314(6) Uani 1 1 d . . . . .
H18 H 0.299903 0.951298 0.428131 0.038 Uiso 1 1 calc R U . . .
C19 C 0.4240(3) 0.8551(2) 0.49094(13) 0.0294(6) Uani 1 1 d . . . . .
H19 H 0.401653 0.906814 0.521217 0.035 Uiso 1 1 calc R U . . .
C20 C 0.5236(3) 0.7666(2) 0.51560(11) 0.0248(5) Uani 1 1 d . . . . .
C21 C 0.5709(4) 0.7720(3) 0.58496(13) 0.0354(6) Uani 1 1 d . . . . .
H21A H 0.682698 0.798730 0.594679 0.053 Uiso 1 1 calc R U . . .
H21B H 0.562843 0.698313 0.602621 0.053 Uiso 1 1 calc R U . . .
H21C H 0.497724 0.822418 0.602501 0.053 Uiso 1 1 calc R U . . .
C22 C 0.5753(3) 0.67995(19) 0.48101(11) 0.0204(5) Uani 1 1 d . . . . .
P P 0.62103(11) 0.67048(7) 0.14943(4) 0.0405(2) Uani 1 1 d . . . . .
F1 F 0.5942(9) 0.5770(3) 0.1963(2) 0.098(2) Uani 0.725(9) 1 d . U P A 1
F2 F 0.7342(6) 0.5895(4) 0.1159(3) 0.0606(14) Uani 0.725(9) 1 d . U P A 1
F3 F 0.4712(5) 0.6152(5) 0.1056(3) 0.0949(19) Uani 0.725(9) 1 d . U P A 1
F4 F 0.4979(8) 0.7468(4) 0.1779(3) 0.0839(18) Uani 0.725(9) 1 d . U P A 1
F5 F 0.7739(6) 0.7133(6) 0.1912(2) 0.115(2) Uani 0.725(9) 1 d . U P A 1
F6 F 0.6415(10) 0.7584(6) 0.0992(3) 0.087(2) Uani 0.725(9) 1 d . U P A 1
F1A F 0.489(2) 0.5915(16) 0.1511(12) 0.125(6) Uani 0.275(9) 1 d . U P A 2
F2A F 0.672(3) 0.6051(19) 0.0993(10) 0.111(7) Uani 0.275(9) 1 d . U P A 2
F3A F 0.476(2) 0.701(2) 0.1076(10) 0.149(7) Uani 0.275(9) 1 d . U P A 2
F4A F 0.571(2) 0.7498(15) 0.2047(7) 0.084(4) Uani 0.275(9) 1 d . U P A 2
F5A F 0.7406(18) 0.6223(12) 0.1949(6) 0.101(5) Uani 0.275(9) 1 d . U P A 2
F6A F 0.697(3) 0.7759(15) 0.1243(10) 0.093(6) Uani 0.275(9) 1 d . U P A 2


_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
S C1 1.738(3) . ?
S C6 1.754(3) . ?
N C1 1.321(4) . ?
N C2 1.463(4) . ?
N C3 1.476(4) . ?
C1 C4 1.424(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.360(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.422(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(3) . ?
C7 C8 1.411(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.433(3) . ?
C8 C22 1.447(3) . ?
C9 C10 1.371(3) . ?
C9 H9 0.9500 . ?
C10 C12 1.428(3) . ?
C10 C11 1.494(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.393(3) . ?
C12 C22 1.476(3) . ?
C13 C14 1.384(4) . ?
C13 H13 0.9500 . ?
C14 C18 1.405(4) . ?
C14 C15 1.531(3) . ?
C15 C16 1.522(5) . ?
C15 C17 1.539(4) . ?
C15 H15 1.0000 . ?
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 C19 1.382(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.415(4) . ?
C19 H19 0.9500 . ?
C20 C22 1.399(3) . ?
C20 C21 1.513(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
P F5A 1.427(11) . ?
P F3A 1.453(17) . ?
P F1A 1.461(15) . ?
P F2A 1.47(2) . ?
P F5 1.545(4) . ?
P F6 1.559(6) . ?
P F6A 1.560(18) . ?
P F1 1.566(3) . ?
P F4 1.576(5) . ?
P F3 1.606(4) . ?
P F2 1.610(5) . ?
P F4A 1.645(14) . ?
F1A F3A 1.63(3) . ?

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
C1 S C6 91.70(13) . . ?
C1 N C2 121.9(2) . . ?
C1 N C3 120.9(3) . . ?
C2 N C3 117.2(3) . . ?
N C1 C4 127.3(2) . . ?
N C1 S 121.2(2) . . ?
C4 C1 S 111.5(2) . . ?
N C2 H2A 109.5 . . ?
N C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N C3 H3A 109.5 . . ?
N C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C1 112.1(2) . . ?
C5 C4 H4 124.0 . . ?
C1 C4 H4 124.0 . . ?
C4 C5 C6 115.4(3) . . ?
C4 C5 H5 122.3 . . ?
C6 C5 H5 122.3 . . ?
C7 C6 C5 123.4(2) . . ?
C7 C6 S 127.23(19) . . ?
C5 C6 S 109.31(19) . . ?
C6 C7 C8 130.0(2) . . ?
C6 C7 H7 115.0 . . ?
C8 C7 H7 115.0 . . ?
C7 C8 C9 124.9(2) . . ?
C7 C8 C22 128.2(2) . . ?
C9 C8 C22 106.7(2) . . ?
C10 C9 C8 111.2(2) . . ?
C10 C9 H9 124.4 . . ?
C8 C9 H9 124.4 . . ?
C9 C10 C12 108.1(2) . . ?
C9 C10 C11 126.1(2) . . ?
C12 C10 C11 125.8(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C10 120.8(2) . . ?
C13 C12 C22 131.2(2) . . ?
C10 C12 C22 108.0(2) . . ?
C14 C13 C12 130.6(2) . . ?
C14 C13 H13 114.7 . . ?
C12 C13 H13 114.7 . . ?
C13 C14 C18 123.7(2) . . ?
C13 C14 C15 119.8(2) . . ?
C18 C14 C15 116.5(2) . . ?
C16 C15 C14 114.3(2) . . ?
C16 C15 C17 110.7(3) . . ?
C14 C15 C17 109.5(2) . . ?
C16 C15 H15 107.3 . . ?
C14 C15 H15 107.3 . . ?
C17 C15 H15 107.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 130.7(2) . . ?
C19 C18 H18 114.6 . . ?
C14 C18 H18 114.6 . . ?
C18 C19 C20 133.1(2) . . ?
C18 C19 H19 113.5 . . ?
C20 C19 H19 113.5 . . ?
C22 C20 C19 125.0(2) . . ?
C22 C20 C21 121.3(2) . . ?
C19 C20 C21 113.8(2) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 C8 129.0(2) . . ?
C20 C22 C12 124.9(2) . . ?
C8 C22 C12 105.9(2) . . ?
F5A P F3A 167.5(12) . . ?
F5A P F1A 99.4(11) . . ?
F3A P F1A 68.1(13) . . ?
F5A P F2A 93.0(10) . . ?
F3A P F2A 88.4(12) . . ?
F1A P F2A 87.9(12) . . ?
F5 P F6 91.2(4) . . ?
F5A P F6A 107.8(11) . . ?
F3A P F6A 84.6(12) . . ?
F1A P F6A 152.8(13) . . ?
F2A P F6A 90.3(11) . . ?
F5 P F1 92.3(4) . . ?
F6 P F1 176.1(4) . . ?
F5 P F4 95.5(3) . . ?
F6 P F4 91.2(4) . . ?
F1 P F4 90.2(3) . . ?
F5 P F3 174.6(3) . . ?
F6 P F3 91.1(4) . . ?
F1 P F3 85.2(3) . . ?
F4 P F3 89.3(3) . . ?
F5 P F2 89.3(3) . . ?
F6 P F2 88.0(3) . . ?
F1 P F2 90.2(2) . . ?
F4 P F2 175.1(3) . . ?
F3 P F2 85.9(3) . . ?
F5A P F4A 87.3(8) . . ?
F3A P F4A 92.1(10) . . ?
F1A P F4A 95.4(10) . . ?
F2A P F4A 176.6(11) . . ?
F6A P F4A 86.4(9) . . ?
P F1A F3A 55.7(9) . . ?
P F3A F1A 56.2(9) . . ?

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 N C1 C4 -176.5(3) . . . . ?
C3 N C1 C4 1.3(4) . . . . ?
C2 N C1 S 4.2(4) . . . . ?
C3 N C1 S -178.0(2) . . . . ?
C6 S C1 N 179.5(2) . . . . ?
C6 S C1 C4 0.1(2) . . . . ?
N C1 C4 C5 179.2(3) . . . . ?
S C1 C4 C5 -1.4(3) . . . . ?
C1 C4 C5 C6 2.3(3) . . . . ?
C4 C5 C6 C7 176.2(2) . . . . ?
C4 C5 C6 S -2.2(3) . . . . ?
C1 S C6 C7 -177.2(2) . . . . ?
C1 S C6 C5 1.08(19) . . . . ?
C5 C6 C7 C8 -179.2(2) . . . . ?
S C6 C7 C8 -1.1(4) . . . . ?
C6 C7 C8 C9 -8.5(4) . . . . ?
C6 C7 C8 C22 176.6(2) . . . . ?
C7 C8 C9 C10 -174.5(2) . . . . ?
C22 C8 C9 C10 1.3(3) . . . . ?
C8 C9 C10 C12 0.3(3) . . . . ?
C8 C9 C10 C11 -179.4(2) . . . . ?
C9 C10 C12 C13 176.5(2) . . . . ?
C11 C10 C12 C13 -3.8(4) . . . . ?
C9 C10 C12 C22 -1.8(3) . . . . ?
C11 C10 C12 C22 177.9(2) . . . . ?
C10 C12 C13 C14 -177.5(2) . . . . ?
C22 C12 C13 C14 0.3(4) . . . . ?
C12 C13 C14 C18 -4.5(4) . . . . ?
C12 C13 C14 C15 175.3(2) . . . . ?
C13 C14 C15 C16 21.6(4) . . . . ?
C18 C14 C15 C16 -158.7(3) . . . . ?
C13 C14 C15 C17 -103.3(3) . . . . ?
C18 C14 C15 C17 76.5(3) . . . . ?
C13 C14 C18 C19 -1.3(5) . . . . ?
C15 C14 C18 C19 179.0(3) . . . . ?
C14 C18 C19 C20 6.0(5) . . . . ?
C18 C19 C20 C22 0.4(5) . . . . ?
C18 C19 C20 C21 -179.0(3) . . . . ?
C19 C20 C22 C8 176.3(2) . . . . ?
C21 C20 C22 C8 -4.3(4) . . . . ?
C19 C20 C22 C12 -9.3(4) . . . . ?
C21 C20 C22 C12 170.1(2) . . . . ?
C7 C8 C22 C20 -11.4(4) . . . . ?
C9 C8 C22 C20 172.9(2) . . . . ?
C7 C8 C22 C12 173.3(2) . . . . ?
C9 C8 C22 C12 -2.3(2) . . . . ?
C13 C12 C22 C20 9.1(4) . . . . ?
C10 C12 C22 C20 -173.0(2) . . . . ?
C13 C12 C22 C8 -175.4(2) . . . . ?
C10 C12 C22 C8 2.5(2) . . . . ?
F5A P F1A F3A 178.3(12) . . . . ?
F2A P F1A F3A -89.1(14) . . . . ?
F6A P F1A F3A -3(3) . . . . ?
F4A P F1A F3A 90.1(12) . . . . ?
F5A P F3A F1A -8(5) . . . . ?
F2A P F3A F1A 88.4(13) . . . . ?
F6A P F3A F1A 178.8(12) . . . . ?
F4A P F3A F1A -95.0(12) . . . . ?

_refine_diff_density_max         0.429
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_s21sel5
_database_code_depnum_ccdc_archive 'CCDC 2129313'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H29, F6 P'
_chemical_formula_sum            'C30 H29 F6 P'
_chemical_formula_weight         534.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+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                   10.5171(3)
_cell_length_b                   19.2813(6)
_cell_length_c                   25.1199(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5093.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4733
_cell_measurement_theta_min      4.8740
_cell_measurement_theta_max      68.1950

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             2224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.374
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    1.505
_shelx_estimated_absorpt_T_min   0.603
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_T_min  0.67944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.673
_oxdiff_exptl_absorpt_empirical_full_max 1.431
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            32580
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.519
_diffrn_reflns_theta_max         68.440
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4677
_reflns_number_gt                3523
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+1.0820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4677
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.75498(18) 0.17487(11) 0.74788(8) 0.0239(4) Uani 1 1 d . . . . .
C2 C 0.79149(18) 0.16007(11) 0.80357(9) 0.0237(4) Uani 1 1 d . . . . .
C3 C 0.7518(2) 0.20206(11) 0.84603(9) 0.0265(5) Uani 1 1 d . . . . .
H3 H 0.701156 0.241857 0.839110 0.032 Uiso 1 1 calc R U . . .
C4 C 0.7854(2) 0.18622(12) 0.89786(9) 0.0284(5) Uani 1 1 d . . . . .
H4 H 0.756765 0.214860 0.926199 0.034 Uiso 1 1 calc R U . . .
C5 C 0.8606(2) 0.12895(12) 0.90881(9) 0.0293(5) Uani 1 1 d . . . . .
H5 H 0.884163 0.118568 0.944444 0.035 Uiso 1 1 calc R U . . .
C6 C 0.9013(2) 0.08691(12) 0.86737(9) 0.0316(5) Uani 1 1 d . . . . .
H6 H 0.952971 0.047618 0.874583 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8665(2) 0.10215(12) 0.81547(9) 0.0273(5) Uani 1 1 d . . . . .
H7 H 0.894160 0.072733 0.787421 0.033 Uiso 1 1 calc R U . . .
C8 C 0.8050(2) 0.12609(11) 0.70667(8) 0.0245(4) Uani 1 1 d . . . . .
C9 C 0.7334(2) 0.06877(12) 0.69188(10) 0.0335(5) Uani 1 1 d . . . . .
H9 H 0.649144 0.063767 0.704997 0.040 Uiso 1 1 calc R U . . .
C10 C 0.7831(3) 0.01887(13) 0.65830(10) 0.0404(6) Uani 1 1 d . . . . .
H10 H 0.733429 -0.020245 0.648458 0.049 Uiso 1 1 calc R U . . .
C11 C 0.9055(3) 0.02632(14) 0.63915(10) 0.0414(6) Uani 1 1 d . . . . .
H11 H 0.940795 -0.008409 0.616745 0.050 Uiso 1 1 calc R U . . .
C12 C 0.9768(2) 0.08375(15) 0.65233(11) 0.0432(6) Uani 1 1 d . . . . .
H12 H 1.060113 0.089236 0.638334 0.052 Uiso 1 1 calc R U . . .
C13 C 0.9262(2) 0.13369(14) 0.68625(10) 0.0352(5) Uani 1 1 d . . . . .
H13 H 0.975252 0.173287 0.695423 0.042 Uiso 1 1 calc R U . . .
C14 C 0.67501(19) 0.22763(11) 0.73483(9) 0.0269(5) Uani 1 1 d . . . . .
H14 H 0.642973 0.255679 0.762880 0.032 Uiso 1 1 calc R U . . .
C15 C 0.63589(19) 0.24374(11) 0.68171(9) 0.0249(4) Uani 1 1 d . . . . .
H15 H 0.676219 0.220338 0.653027 0.030 Uiso 1 1 calc R U . . .
C16 C 0.5429(2) 0.29135(11) 0.67019(8) 0.0245(4) Uani 1 1 d . . . . .
C17 C 0.4716(2) 0.32831(12) 0.71062(8) 0.0273(5) Uani 1 1 d . . . . .
H17 H 0.482739 0.322105 0.747849 0.033 Uiso 1 1 calc R U . . .
C18 C 0.3877(2) 0.37255(12) 0.68862(9) 0.0266(5) Uani 1 1 d . . . . .
C19 C 0.2967(2) 0.41865(14) 0.71740(9) 0.0382(6) Uani 1 1 d . . . . .
H19A H 0.320227 0.467212 0.711427 0.057 Uiso 1 1 calc R U . . .
H19B H 0.299858 0.408441 0.755597 0.057 Uiso 1 1 calc R U . . .
H19C H 0.210433 0.410550 0.704077 0.057 Uiso 1 1 calc R U . . .
C20 C 0.39984(19) 0.36801(11) 0.63115(8) 0.0224(4) Uani 1 1 d . . . . .
C21 C 0.32669(19) 0.41045(11) 0.59834(9) 0.0232(4) Uani 1 1 d . . . . .
H21 H 0.271341 0.441214 0.616671 0.028 Uiso 1 1 calc R U . . .
C22 C 0.32148(19) 0.41513(11) 0.54327(9) 0.0228(4) Uani 1 1 d . . . . .
C23 C 0.23858(19) 0.47209(11) 0.51980(9) 0.0251(4) Uani 1 1 d . . . . .
H23 H 0.183357 0.490198 0.549079 0.030 Uiso 1 1 calc R U . . .
C24 C 0.3238(2) 0.53183(12) 0.50135(10) 0.0303(5) Uani 1 1 d . . . . .
H24A H 0.385512 0.514513 0.475300 0.045 Uiso 1 1 calc R U . . .
H24B H 0.369147 0.551201 0.532034 0.045 Uiso 1 1 calc R U . . .
H24C H 0.271448 0.567998 0.484925 0.045 Uiso 1 1 calc R U . . .
C25 C 0.1512(2) 0.44732(12) 0.47516(9) 0.0306(5) Uani 1 1 d . . . . .
H25A H 0.098607 0.486078 0.462837 0.046 Uiso 1 1 calc R U . . .
H25B H 0.096293 0.410101 0.488465 0.046 Uiso 1 1 calc R U . . .
H25C H 0.202663 0.429882 0.445513 0.046 Uiso 1 1 calc R U . . .
C26 C 0.3902(2) 0.37222(11) 0.50900(9) 0.0266(5) Uani 1 1 d . . . . .
H26 H 0.374375 0.379809 0.472225 0.032 Uiso 1 1 calc R U . . .
C27 C 0.47732(19) 0.32061(11) 0.51975(9) 0.0252(4) Uani 1 1 d . . . . .
H27 H 0.508399 0.298073 0.488741 0.030 Uiso 1 1 calc R U . . .
C28 C 0.52963(18) 0.29450(10) 0.56735(9) 0.0224(4) Uani 1 1 d . . . . .
C29 C 0.6265(2) 0.23808(12) 0.55957(9) 0.0288(5) Uani 1 1 d . . . . .
H29A H 0.632289 0.226496 0.521662 0.043 Uiso 1 1 calc R U . . .
H29B H 0.600835 0.196846 0.579691 0.043 Uiso 1 1 calc R U . . .
H29C H 0.709546 0.254115 0.572289 0.043 Uiso 1 1 calc R U . . .
C30 C 0.49513(18) 0.31654(10) 0.61856(8) 0.0204(4) Uani 1 1 d . . . . .
P P 0.03623(5) 0.66226(3) 0.39722(2) 0.02636(14) Uani 1 1 d . . . . .
F1 F -0.09625(12) 0.68044(8) 0.42486(6) 0.0404(4) Uani 1 1 d . . . . .
F2 F 0.16829(14) 0.64510(9) 0.36992(7) 0.0531(4) Uani 1 1 d . . . . .
F3 F -0.02992(16) 0.66979(9) 0.34016(6) 0.0497(4) Uani 1 1 d . . . . .
F4 F 0.07036(14) 0.74305(7) 0.39646(6) 0.0432(4) Uani 1 1 d . . . . .
F5 F 0.09999(15) 0.65580(9) 0.45460(6) 0.0526(4) Uani 1 1 d . . . . .
F6 F 0.00084(14) 0.58195(8) 0.39822(7) 0.0486(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 C14 1.360(3) . ?
C1 C2 1.478(3) . ?
C1 C8 1.494(3) . ?
C2 C7 1.400(3) . ?
C2 C3 1.403(3) . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.382(3) . ?
C8 C9 1.388(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.430(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.372(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.450(3) . ?
C16 C30 1.473(3) . ?
C17 C18 1.346(3) . ?
C17 H17 0.9500 . ?
C18 C20 1.452(3) . ?
C18 C19 1.492(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.393(3) . ?
C20 C30 1.445(3) . ?
C21 C22 1.387(3) . ?
C21 H21 0.9500 . ?
C22 C26 1.396(3) . ?
C22 C23 1.521(3) . ?
C23 C25 1.526(3) . ?
C23 C24 1.532(3) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.379(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.409(3) . ?
C27 H27 0.9500 . ?
C28 C30 1.402(3) . ?
C28 C29 1.503(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
P F2 1.5839(15) . ?
P F6 1.5927(15) . ?
P F5 1.5945(15) . ?
P F1 1.5957(14) . ?
P F4 1.5986(14) . ?
P F3 1.5999(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 C1 C2 122.2(2) . . ?
C14 C1 C8 121.4(2) . . ?
C2 C1 C8 116.27(18) . . ?
C7 C2 C3 117.8(2) . . ?
C7 C2 C1 120.2(2) . . ?
C3 C2 C1 122.06(19) . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.6(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.5(2) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 121.3(2) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C13 C8 C9 119.0(2) . . ?
C13 C8 C1 121.0(2) . . ?
C9 C8 C1 119.73(19) . . ?
C10 C9 C8 120.8(2) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.5(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 120.4(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.7(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C8 C13 C12 120.5(2) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C1 C14 C15 124.4(2) . . ?
C1 C14 H14 117.8 . . ?
C15 C14 H14 117.8 . . ?
C16 C15 C14 123.2(2) . . ?
C16 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C15 C16 C17 123.3(2) . . ?
C15 C16 C30 130.5(2) . . ?
C17 C16 C30 106.15(18) . . ?
C18 C17 C16 111.29(19) . . ?
C18 C17 H17 124.4 . . ?
C16 C17 H17 124.4 . . ?
C17 C18 C20 108.19(19) . . ?
C17 C18 C19 126.8(2) . . ?
C20 C18 C19 125.0(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C30 131.1(2) . . ?
C21 C20 C18 120.27(19) . . ?
C30 C20 C18 108.66(18) . . ?
C22 C21 C20 130.5(2) . . ?
C22 C21 H21 114.7 . . ?
C20 C21 H21 114.7 . . ?
C21 C22 C26 123.79(19) . . ?
C21 C22 C23 117.12(19) . . ?
C26 C22 C23 119.06(19) . . ?
C22 C23 C25 113.82(18) . . ?
C22 C23 C24 108.94(17) . . ?
C25 C23 C24 111.43(18) . . ?
C22 C23 H23 107.5 . . ?
C25 C23 H23 107.5 . . ?
C24 C23 H23 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 130.6(2) . . ?
C27 C26 H26 114.7 . . ?
C22 C26 H26 114.7 . . ?
C26 C27 C28 133.1(2) . . ?
C26 C27 H27 113.5 . . ?
C28 C27 H27 113.5 . . ?
C30 C28 C27 124.68(19) . . ?
C30 C28 C29 120.92(19) . . ?
C27 C28 C29 114.38(19) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 C20 126.02(19) . . ?
C28 C30 C16 128.26(19) . . ?
C20 C30 C16 105.69(18) . . ?
F2 P F6 90.49(9) . . ?
F2 P F5 90.36(10) . . ?
F6 P F5 90.47(9) . . ?
F2 P F1 179.34(10) . . ?
F6 P F1 90.16(8) . . ?
F5 P F1 89.49(9) . . ?
F2 P F4 90.08(9) . . ?
F6 P F4 179.42(9) . . ?
F5 P F4 89.57(9) . . ?
F1 P F4 89.27(8) . . ?
F2 P F3 90.70(10) . . ?
F6 P F3 90.04(9) . . ?
F5 P F3 178.82(10) . . ?
F1 P F3 89.44(8) . . ?
F4 P F3 89.91(9) . . ?

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
C14 C1 C2 C7 175.3(2) . . . . ?
C8 C1 C2 C7 -1.4(3) . . . . ?
C14 C1 C2 C3 -3.8(3) . . . . ?
C8 C1 C2 C3 179.54(19) . . . . ?
C7 C2 C3 C4 -0.3(3) . . . . ?
C1 C2 C3 C4 178.78(19) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
C3 C4 C5 C6 -0.6(3) . . . . ?
C4 C5 C6 C7 -0.1(3) . . . . ?
C5 C6 C7 C2 0.6(3) . . . . ?
C3 C2 C7 C6 -0.4(3) . . . . ?
C1 C2 C7 C6 -179.5(2) . . . . ?
C14 C1 C8 C13 100.5(3) . . . . ?
C2 C1 C8 C13 -82.8(3) . . . . ?
C14 C1 C8 C9 -85.1(3) . . . . ?
C2 C1 C8 C9 91.5(2) . . . . ?
C13 C8 C9 C10 1.6(4) . . . . ?
C1 C8 C9 C10 -172.9(2) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
C9 C10 C11 C12 -1.5(4) . . . . ?
C10 C11 C12 C13 1.6(4) . . . . ?
C9 C8 C13 C12 -1.5(4) . . . . ?
C1 C8 C13 C12 172.9(2) . . . . ?
C11 C12 C13 C8 -0.1(4) . . . . ?
C2 C1 C14 C15 -179.44(19) . . . . ?
C8 C1 C14 C15 -3.0(3) . . . . ?
C1 C14 C15 C16 171.4(2) . . . . ?
C14 C15 C16 C17 -2.3(3) . . . . ?
C14 C15 C16 C30 176.8(2) . . . . ?
C15 C16 C17 C18 179.1(2) . . . . ?
C30 C16 C17 C18 -0.2(3) . . . . ?
C16 C17 C18 C20 -0.7(3) . . . . ?
C16 C17 C18 C19 179.1(2) . . . . ?
C17 C18 C20 C21 -177.7(2) . . . . ?
C19 C18 C20 C21 2.5(3) . . . . ?
C17 C18 C20 C30 1.4(2) . . . . ?
C19 C18 C20 C30 -178.4(2) . . . . ?
C30 C20 C21 C22 1.5(4) . . . . ?
C18 C20 C21 C22 -179.7(2) . . . . ?
C20 C21 C22 C26 3.4(4) . . . . ?
C20 C21 C22 C23 -174.7(2) . . . . ?
C21 C22 C23 C25 -132.7(2) . . . . ?
C26 C22 C23 C25 49.1(3) . . . . ?
C21 C22 C23 C24 102.3(2) . . . . ?
C26 C22 C23 C24 -75.9(2) . . . . ?
C21 C22 C26 C27 -2.8(4) . . . . ?
C23 C22 C26 C27 175.2(2) . . . . ?
C22 C26 C27 C28 -2.0(4) . . . . ?
C26 C27 C28 C30 3.2(4) . . . . ?
C26 C27 C28 C29 -178.2(2) . . . . ?
C27 C28 C30 C20 1.3(3) . . . . ?
C29 C28 C30 C20 -177.26(19) . . . . ?
C27 C28 C30 C16 178.8(2) . . . . ?
C29 C28 C30 C16 0.3(3) . . . . ?
C21 C20 C30 C28 -4.5(4) . . . . ?
C18 C20 C30 C28 176.49(19) . . . . ?
C21 C20 C30 C16 177.5(2) . . . . ?
C18 C20 C30 C16 -1.5(2) . . . . ?
C15 C16 C30 C28 3.8(4) . . . . ?
C17 C16 C30 C28 -176.9(2) . . . . ?
C15 C16 C30 C20 -178.2(2) . . . . ?
C17 C16 C30 C20 1.1(2) . . . . ?

_refine_diff_density_max         0.258
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_s21sel7
_database_code_depnum_ccdc_archive 'CCDC 2129312'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C22 H22 Br, F6 P'
_chemical_formula_sum            'C22 H22 Br F6 P'
_chemical_formula_weight         511.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   7.5877(2)
_cell_length_b                   26.8100(12)
_cell_length_c                   31.9061(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6490.5(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8052
_cell_measurement_theta_min      4.4670
_cell_measurement_theta_max      72.2970

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             3096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    3.820
_shelx_estimated_absorpt_T_min   0.468
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_T_min  0.63398
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.654
_oxdiff_exptl_absorpt_empirical_full_max 1.359
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            44869
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         4.308
_diffrn_reflns_theta_max         68.808
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11920
_reflns_number_gt                8673
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.988
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 two of the three PF6 groups show rotational disorder 
 in the ratio 40:60
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0639P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11920
_refine_ls_number_parameters     897
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1370
_refine_ls_wR_factor_gt          0.1239
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.00627(12) 0.04410(4) 0.57861(3) 0.0509(2) Uani 1 1 d . . . . .
C1 C 0.9331(11) 0.2614(3) 0.5228(2) 0.040(2) Uani 1 1 d . . . . .
H1 H 0.923866 0.285262 0.544741 0.048 Uiso 1 1 calc R U . . .
C2 C 0.9391(10) 0.2096(3) 0.5356(2) 0.0361(18) Uani 1 1 d . . . . .
C3 C 1.0139(10) 0.1977(3) 0.5750(2) 0.0368(18) Uani 1 1 d . . . . .
H3 H 1.053461 0.223905 0.592742 0.044 Uiso 1 1 calc R U . . .
C4 C 1.0305(10) 0.1492(4) 0.5880(2) 0.042(2) Uani 1 1 d . . . . .
H4 H 1.081532 0.141736 0.614503 0.050 Uiso 1 1 calc R U . . .
C5 C 0.9724(10) 0.1115(3) 0.5624(2) 0.0373(19) Uani 1 1 d . . . . .
C6 C 0.8923(10) 0.1213(3) 0.5242(2) 0.0385(19) Uani 1 1 d . . . . .
H6 H 0.850799 0.094958 0.506889 0.046 Uiso 1 1 calc R U . . .
C7 C 0.8749(10) 0.1699(3) 0.5121(2) 0.0359(19) Uani 1 1 d . . . . .
H7 H 0.816403 0.176909 0.486403 0.043 Uiso 1 1 calc R U . . .
C8 C 0.9391(10) 0.2802(3) 0.4826(3) 0.0384(19) Uani 1 1 d . . . . .
C9 C 0.9749(11) 0.2511(3) 0.4450(3) 0.041(2) Uani 1 1 d . . . . .
H9 H 0.976160 0.215662 0.443731 0.049 Uiso 1 1 calc R U . . .
C10 C 1.0055(12) 0.2811(3) 0.4128(2) 0.0396(18) Uani 1 1 d . . . . .
C11 C 1.0527(15) 0.2657(4) 0.3690(3) 0.054(3) Uani 1 1 d . . . . .
H11A H 0.973312 0.282129 0.349068 0.081 Uiso 1 1 calc R U . . .
H11B H 1.041029 0.229423 0.366243 0.081 Uiso 1 1 calc R U . . .
H11C H 1.174590 0.275456 0.362965 0.081 Uiso 1 1 calc R U . . .
C12 C 0.9911(11) 0.3324(3) 0.4262(2) 0.0376(17) Uani 1 1 d . . . . .
C13 C 1.0242(10) 0.3722(3) 0.3986(2) 0.0368(18) Uani 1 1 d . . . . .
H13 H 1.048545 0.362423 0.370544 0.044 Uiso 1 1 calc R U . . .
C14 C 1.0274(10) 0.4223(3) 0.4053(2) 0.0356(18) Uani 1 1 d . . . . .
C15 C 1.0709(11) 0.4577(3) 0.3697(3) 0.0423(19) Uani 1 1 d . . . . .
H15 H 1.141661 0.485759 0.381574 0.051 Uiso 1 1 calc R U . . .
C16 C 1.1775(13) 0.4346(4) 0.3346(3) 0.055(3) Uani 1 1 d . . . . .
H16A H 1.103253 0.411303 0.318763 0.082 Uiso 1 1 calc R U . . .
H16B H 1.278249 0.416540 0.346413 0.082 Uiso 1 1 calc R U . . .
H16C H 1.220125 0.460866 0.315796 0.082 Uiso 1 1 calc R U . . .
C17 C 0.8994(13) 0.4798(3) 0.3523(3) 0.050(2) Uani 1 1 d . . . . .
H17A H 0.926976 0.503967 0.330269 0.076 Uiso 1 1 calc R U . . .
H17B H 0.835148 0.496500 0.374985 0.076 Uiso 1 1 calc R U . . .
H17C H 0.826352 0.452998 0.340704 0.076 Uiso 1 1 calc R U . . .
C18 C 0.9854(11) 0.4446(3) 0.4439(3) 0.045(2) Uani 1 1 d . . . . .
H18 H 1.001286 0.479728 0.444809 0.054 Uiso 1 1 calc R U . . .
C19 C 0.9250(11) 0.4238(3) 0.4808(3) 0.042(2) Uani 1 1 d . . . . .
H19 H 0.896955 0.447640 0.501783 0.050 Uiso 1 1 calc R U . . .
C20 C 0.8969(10) 0.3741(3) 0.4934(2) 0.0355(18) Uani 1 1 d . . . . .
C21 C 0.8072(12) 0.3689(4) 0.5361(3) 0.044(2) Uani 1 1 d . . . . .
H21A H 0.731253 0.339354 0.536092 0.066 Uiso 1 1 calc R U . . .
H21B H 0.735759 0.398659 0.541693 0.066 Uiso 1 1 calc R U . . .
H21C H 0.897017 0.365453 0.558020 0.066 Uiso 1 1 calc R U . . .
C22 C 0.9417(10) 0.3332(3) 0.4700(2) 0.0354(18) Uani 1 1 d . . . . .
Br2 Br 0.61287(13) 0.95123(5) 0.74915(3) 0.0584(3) Uani 1 1 d . . . . .
C31 C 0.4774(12) 0.7379(4) 0.6893(3) 0.051(2) Uani 1 1 d . . . . .
H31 H 0.459401 0.714754 0.711467 0.061 Uiso 1 1 calc R U . . .
C32 C 0.5066(12) 0.7894(4) 0.7016(3) 0.046(2) Uani 1 1 d . . . . .
C33 C 0.5781(13) 0.7983(4) 0.7412(3) 0.051(2) Uani 1 1 d . . . . .
H33 H 0.604757 0.770858 0.758857 0.061 Uiso 1 1 calc R U . . .
C34 C 0.6114(12) 0.8463(4) 0.7553(3) 0.051(2) Uani 1 1 d . . . . .
H34 H 0.664216 0.851873 0.781877 0.061 Uiso 1 1 calc R U . . .
C35 C 0.5664(11) 0.8854(4) 0.7300(2) 0.042(2) Uani 1 1 d . . . . .
C36 C 0.4888(12) 0.8785(4) 0.6910(3) 0.046(2) Uani 1 1 d . . . . .
H36 H 0.456719 0.906334 0.674256 0.056 Uiso 1 1 calc R U . . .
C37 C 0.4593(10) 0.8311(4) 0.6773(2) 0.044(2) Uani 1 1 d . . . . .
H37 H 0.405792 0.826084 0.650692 0.052 Uiso 1 1 calc R U . . .
C38 C 0.4729(11) 0.7184(4) 0.6491(3) 0.045(2) Uani 1 1 d . . . . .
C39 C 0.4405(11) 0.6662(4) 0.6370(3) 0.047(2) Uani 1 1 d . . . . .
C40 C 0.3896(12) 0.6262(4) 0.6623(3) 0.055(3) Uani 1 1 d . . . . .
C41 C 0.3448(17) 0.6333(5) 0.7084(3) 0.081(4) Uani 1 1 d . . . . .
H41A H 0.281304 0.603980 0.718675 0.121 Uiso 1 1 calc R U . . .
H41B H 0.270479 0.662997 0.711606 0.121 Uiso 1 1 calc R U . . .
H41C H 0.453668 0.637683 0.724469 0.121 Uiso 1 1 calc R U . . .
C42 C 0.3759(14) 0.5771(4) 0.6485(3) 0.058(3) Uani 1 1 d . . . . .
H42 H 0.348832 0.554344 0.670426 0.069 Uiso 1 1 calc R U . . .
C43 C 0.3929(14) 0.5542(5) 0.6102(4) 0.066(3) Uani 1 1 d . . . . .
H43 H 0.377817 0.519054 0.610418 0.079 Uiso 1 1 calc R U . . .
C44 C 0.4291(14) 0.5748(4) 0.5709(3) 0.059(3) Uani 1 1 d . . . . .
C45 C 0.439(2) 0.5396(5) 0.5331(4) 0.085(4) Uani 1 1 d . . . . .
H45 H 0.496815 0.560046 0.510786 0.102 Uiso 1 1 calc R U . . .
C46 C 0.275(2) 0.5274(9) 0.5161(5) 0.191(13) Uani 1 1 d . . . . .
H46A H 0.287931 0.498906 0.497114 0.287 Uiso 1 1 calc R U . . .
H46B H 0.228566 0.556035 0.500592 0.287 Uiso 1 1 calc R U . . .
H46C H 0.193431 0.518633 0.538779 0.287 Uiso 1 1 calc R U . . .
C47 C 0.5659(15) 0.4980(4) 0.5406(4) 0.072(3) Uani 1 1 d . . . . .
H47A H 0.684322 0.511683 0.544879 0.107 Uiso 1 1 calc R U . . .
H47B H 0.566610 0.475609 0.516360 0.107 Uiso 1 1 calc R U . . .
H47C H 0.530059 0.479350 0.565659 0.107 Uiso 1 1 calc R U . . .
C48 C 0.4658(12) 0.6240(4) 0.5643(3) 0.053(2) Uani 1 1 d . . . . .
H48 H 0.491315 0.632203 0.535982 0.064 Uiso 1 1 calc R U . . .
C49 C 0.4724(12) 0.6645(4) 0.5921(3) 0.050(2) Uani 1 1 d . . . . .
C50 C 0.5180(13) 0.7135(4) 0.5780(3) 0.052(2) Uani 1 1 d . . . . .
C51 C 0.5589(17) 0.7272(4) 0.5338(3) 0.070(3) Uani 1 1 d . . . . .
H51A H 0.584549 0.762935 0.532107 0.105 Uiso 1 1 calc R U . . .
H51B H 0.457424 0.719346 0.515973 0.105 Uiso 1 1 calc R U . . .
H51C H 0.661687 0.708177 0.524222 0.105 Uiso 1 1 calc R U . . .
C52 C 0.5178(13) 0.7446(4) 0.6113(3) 0.055(2) Uani 1 1 d . . . . .
H52 H 0.543898 0.779250 0.609899 0.066 Uiso 1 1 calc R U . . .
Br3 Br 0.42367(15) 0.91482(4) 0.42011(3) 0.0588(3) Uani 1 1 d . . . . .
C61 C 0.4963(12) 0.7022(4) 0.3530(3) 0.045(2) Uani 1 1 d . . . . .
H61 H 0.493967 0.677619 0.374417 0.054 Uiso 1 1 calc R U . . .
C62 C 0.4831(11) 0.7537(3) 0.3666(2) 0.041(2) Uani 1 1 d . . . . .
C63 C 0.5323(11) 0.7653(4) 0.4086(3) 0.048(2) Uani 1 1 d . . . . .
H63 H 0.578669 0.739750 0.425971 0.058 Uiso 1 1 calc R U . . .
C64 C 0.5142(12) 0.8125(4) 0.4245(3) 0.045(2) Uani 1 1 d . . . . .
H64 H 0.544708 0.819714 0.452726 0.055 Uiso 1 1 calc R U . . .
C65 C 0.4505(11) 0.8493(4) 0.3983(2) 0.046(2) Uani 1 1 d . . . . .
C66 C 0.3996(12) 0.8399(4) 0.3573(2) 0.045(2) Uani 1 1 d . . . . .
H66 H 0.356142 0.865946 0.340036 0.054 Uiso 1 1 calc R U . . .
C67 C 0.4134(11) 0.7921(4) 0.3423(3) 0.045(2) Uani 1 1 d . . . . .
H67 H 0.374533 0.784989 0.314615 0.054 Uiso 1 1 calc R U . . .
C68 C 0.5116(11) 0.6850(3) 0.3132(2) 0.0396(19) Uani 1 1 d . . . . .
C69 C 0.5277(10) 0.6327(3) 0.3001(2) 0.040(2) Uani 1 1 d . . . . .
C70 C 0.4854(11) 0.5899(4) 0.3233(2) 0.044(2) Uani 1 1 d . . . . .
C71 C 0.3885(14) 0.5928(4) 0.3649(3) 0.058(3) Uani 1 1 d . . . . .
H71A H 0.308431 0.621515 0.364614 0.087 Uiso 1 1 calc R U . . .
H71B H 0.474070 0.596758 0.387665 0.087 Uiso 1 1 calc R U . . .
H71C H 0.320647 0.562176 0.369222 0.087 Uiso 1 1 calc R U . . .
C72 C 0.5306(12) 0.5408(4) 0.3117(3) 0.050(2) Uani 1 1 d . . . . .
H72 H 0.512280 0.516816 0.333215 0.060 Uiso 1 1 calc R U . . .
C73 C 0.5961(13) 0.5214(4) 0.2753(3) 0.052(2) Uani 1 1 d . . . . .
H73 H 0.623796 0.486867 0.276603 0.063 Uiso 1 1 calc R U . . .
C74 C 0.6301(10) 0.5441(4) 0.2357(3) 0.042(2) Uani 1 1 d . . . . .
C75 C 0.6695(13) 0.5082(4) 0.2000(3) 0.052(2) Uani 1 1 d . . . . .
H75 H 0.749815 0.481706 0.211019 0.063 Uiso 1 1 calc R U . . .
C76 C 0.7570(14) 0.5316(4) 0.1623(3) 0.060(3) Uani 1 1 d . . . . .
H76A H 0.797792 0.505292 0.143320 0.089 Uiso 1 1 calc R U . . .
H76B H 0.857799 0.551653 0.171507 0.089 Uiso 1 1 calc R U . . .
H76C H 0.672215 0.552965 0.147701 0.089 Uiso 1 1 calc R U . . .
C77 C 0.4937(14) 0.4834(4) 0.1883(3) 0.063(3) Uani 1 1 d . . . . .
H77A H 0.409808 0.508935 0.179103 0.095 Uiso 1 1 calc R U . . .
H77B H 0.446043 0.465897 0.212774 0.095 Uiso 1 1 calc R U . . .
H77C H 0.513064 0.459458 0.165525 0.095 Uiso 1 1 calc R U . . .
C78 C 0.6178(10) 0.5940(3) 0.2290(2) 0.0373(19) Uani 1 1 d . . . . .
H78 H 0.637730 0.603875 0.200841 0.045 Uiso 1 1 calc R U . . .
C79 C 0.5810(10) 0.6337(3) 0.2565(2) 0.0361(18) Uani 1 1 d . . . . .
C80 C 0.5858(11) 0.6845(3) 0.2431(2) 0.0374(18) Uani 1 1 d . . . . .
C81 C 0.6342(14) 0.7009(4) 0.1997(2) 0.049(2) Uani 1 1 d . . . . .
H81A H 0.751903 0.688429 0.192727 0.073 Uiso 1 1 calc R U . . .
H81B H 0.634081 0.737470 0.198434 0.073 Uiso 1 1 calc R U . . .
H81C H 0.548259 0.687717 0.179687 0.073 Uiso 1 1 calc R U . . .
C82 C 0.5463(11) 0.7140(3) 0.2757(2) 0.039(2) Uani 1 1 d . . . . .
H82 H 0.541633 0.749416 0.274430 0.047 Uiso 1 1 calc R U . . .
P1 P 0.2581(3) 0.38057(11) 0.61033(8) 0.0522(7) Uani 1 1 d . . . . .
F1 F 0.1860(8) 0.3310(2) 0.58749(18) 0.0686(17) Uani 1 1 d . . . . .
F2 F 0.3302(10) 0.4300(3) 0.6321(2) 0.088(2) Uani 1 1 d . . . . .
F3 F 0.3329(16) 0.3480(4) 0.6460(2) 0.136(4) Uani 1 1 d . . . . .
F4 F 0.0764(12) 0.3853(3) 0.6329(3) 0.119(3) Uani 1 1 d . . . . .
F5 F 0.1871(11) 0.4125(3) 0.5730(3) 0.110(3) Uani 1 1 d . . . . .
F6 F 0.4384(9) 0.3734(3) 0.5863(2) 0.111(3) Uani 1 1 d . . . . .
P2 P 0.8513(4) 0.61223(12) 0.44370(8) 0.0597(7) Uani 1 1 d . . . . .
F7 F 0.7855(12) 0.6610(4) 0.4213(3) 0.127(3) Uani 1 1 d . . . . .
F8 F 0.9048(17) 0.5651(3) 0.4677(3) 0.134(4) Uani 1 1 d . . . . .
F9 F 0.707(3) 0.5696(8) 0.4279(10) 0.119(12) Uani 0.41(2) 1 d . . P A 1
F10 F 0.737(6) 0.6258(12) 0.4834(8) 0.157(19) Uani 0.41(2) 1 d . . P A 1
F11 F 1.010(4) 0.6401(12) 0.4624(16) 0.186(18) Uani 0.41(2) 1 d . . P A 1
F12 F 0.995(3) 0.5865(10) 0.4146(7) 0.134(12) Uani 0.41(2) 1 d . . P A 1
F9A F 0.7990(19) 0.5933(6) 0.3988(4) 0.088(5) Uani 0.59(2) 1 d . . P A 2
F10A F 0.653(2) 0.6119(9) 0.4574(5) 0.127(9) Uani 0.59(2) 1 d . . P A 2
F11A F 0.906(3) 0.6418(6) 0.4826(4) 0.094(6) Uani 0.59(2) 1 d . . P A 2
F12A F 1.0368(17) 0.6269(9) 0.4259(6) 0.128(8) Uani 0.59(2) 1 d . . P A 2
P3 P 0.6612(4) 0.35410(11) 0.28050(8) 0.0532(7) Uani 1 1 d . . . . .
F13 F 0.5757(10) 0.3974(3) 0.3066(2) 0.089(2) Uani 1 1 d . . . . .
F14 F 0.7472(11) 0.3104(3) 0.2544(2) 0.102(3) Uani 1 1 d . . . . .
F15 F 0.555(4) 0.3785(17) 0.2400(9) 0.129(13) Uani 0.37(2) 1 d . . P B 1
F16 F 0.513(4) 0.3231(9) 0.2897(13) 0.112(13) Uani 0.37(2) 1 d . . P B 1
F17 F 0.762(4) 0.3499(12) 0.3202(5) 0.099(10) Uani 0.37(2) 1 d . . P B 1
F18 F 0.805(2) 0.4015(7) 0.2657(7) 0.065(7) Uani 0.37(2) 1 d . . P B 1
F15A F 0.476(2) 0.3386(9) 0.2618(8) 0.137(11) Uani 0.63(2) 1 d . . P B 2
F16A F 0.624(3) 0.3128(5) 0.3179(4) 0.093(6) Uani 0.63(2) 1 d . . P B 2
F17A F 0.8473(18) 0.3597(6) 0.2992(6) 0.098(6) Uani 0.63(2) 1 d . . P B 2
F18A F 0.694(3) 0.3852(6) 0.2432(4) 0.110(7) Uani 0.63(2) 1 d . . P B 2


_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
Br1 C5 1.897(9) . ?
C1 C8 1.381(11) . ?
C1 C2 1.449(12) . ?
C1 H1 0.9500 . ?
C2 C7 1.391(11) . ?
C2 C3 1.415(11) . ?
C3 C4 1.373(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(11) . ?
C6 C7 1.365(12) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.457(11) . ?
C8 C22 1.475(12) . ?
C9 C10 1.324(11) . ?
C9 H9 0.9500 . ?
C10 C12 1.446(12) . ?
C10 C11 1.502(11) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.406(11) . ?
C12 C22 1.445(11) . ?
C13 C14 1.362(11) . ?
C13 H13 0.9500 . ?
C14 C18 1.407(11) . ?
C14 C15 1.516(11) . ?
C15 C16 1.514(12) . ?
C15 C17 1.533(12) . ?
C15 H15 1.0000 . ?
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 C19 1.381(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.408(12) . ?
C19 H19 0.9500 . ?
C20 C22 1.371(11) . ?
C20 C21 1.530(11) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Br2 C35 1.899(10) . ?
C31 C38 1.386(12) . ?
C31 C32 1.454(14) . ?
C31 H31 0.9500 . ?
C32 C33 1.395(12) . ?
C32 C37 1.407(13) . ?
C33 C34 1.387(14) . ?
C33 H33 0.9500 . ?
C34 C35 1.366(13) . ?
C34 H34 0.9500 . ?
C35 C36 1.389(11) . ?
C36 C37 1.364(13) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C52 1.436(13) . ?
C38 C39 1.472(14) . ?
C39 C40 1.398(13) . ?
C39 C49 1.454(12) . ?
C40 C42 1.393(15) . ?
C40 C41 1.520(14) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.374(14) . ?
C42 H42 0.9500 . ?
C43 C44 1.398(15) . ?
C43 H43 0.9500 . ?
C44 C48 1.362(14) . ?
C44 C45 1.533(14) . ?
C45 C46 1.40(2) . ?
C45 C47 1.492(16) . ?
C45 H45 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.403(13) . ?
C48 H48 0.9500 . ?
C49 C50 1.431(14) . ?
C50 C52 1.350(13) . ?
C50 C51 1.490(13) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52 0.9500 . ?
Br3 C65 1.900(10) . ?
C61 C68 1.356(11) . ?
C61 C62 1.453(12) . ?
C61 H61 0.9500 . ?
C62 C67 1.393(12) . ?
C62 C63 1.424(11) . ?
C63 C64 1.370(13) . ?
C63 H63 0.9500 . ?
C64 C65 1.379(13) . ?
C64 H64 0.9500 . ?
C65 C66 1.388(11) . ?
C66 C67 1.372(13) . ?
C66 H66 0.9500 . ?
C67 H67 0.9500 . ?
C68 C82 1.450(11) . ?
C68 C69 1.467(13) . ?
C69 C70 1.403(12) . ?
C69 C79 1.451(11) . ?
C70 C72 1.408(14) . ?
C70 C71 1.520(12) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.367(13) . ?
C72 H72 0.9500 . ?
C73 C74 1.427(12) . ?
C73 H73 0.9500 . ?
C74 C78 1.358(13) . ?
C74 C75 1.521(12) . ?
C75 C76 1.509(13) . ?
C75 C77 1.537(13) . ?
C75 H75 1.0000 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 C79 1.406(11) . ?
C78 H78 0.9500 . ?
C79 C80 1.427(12) . ?
C80 C82 1.342(11) . ?
C80 C81 1.498(10) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82 0.9500 . ?
P1 F3 1.545(8) . ?
P1 F4 1.561(8) . ?
P1 F5 1.562(7) . ?
P1 F6 1.580(7) . ?
P1 F2 1.595(7) . ?
P1 F1 1.611(7) . ?
P2 F11A 1.529(13) . ?
P2 F8 1.532(9) . ?
P2 F11 1.54(3) . ?
P2 F10A 1.567(15) . ?
P2 F12A 1.568(17) . ?
P2 F7 1.570(9) . ?
P2 F9A 1.572(11) . ?
P2 F10 1.58(2) . ?
P2 F12 1.588(17) . ?
P2 F9 1.663(19) . ?
P3 F16 1.43(2) . ?
P3 F18A 1.475(13) . ?
P3 F17 1.483(19) . ?
P3 F17A 1.540(11) . ?
P3 F13 1.568(7) . ?
P3 F14 1.579(7) . ?
P3 F15A 1.583(15) . ?
P3 F16A 1.652(12) . ?
P3 F15 1.66(3) . ?
P3 F18 1.740(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
C8 C1 C2 127.7(8) . . ?
C8 C1 H1 116.2 . . ?
C2 C1 H1 116.2 . . ?
C7 C2 C3 116.7(8) . . ?
C7 C2 C1 124.8(7) . . ?
C3 C2 C1 118.5(8) . . ?
C4 C3 C2 121.3(8) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.2(7) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 121.6(8) . . ?
C4 C5 Br1 119.6(6) . . ?
C6 C5 Br1 118.7(7) . . ?
C7 C6 C5 118.2(8) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C6 C7 C2 122.9(7) . . ?
C6 C7 H7 118.5 . . ?
C2 C7 H7 118.5 . . ?
C1 C8 C9 125.1(8) . . ?
C1 C8 C22 127.3(8) . . ?
C9 C8 C22 106.8(7) . . ?
C10 C9 C8 110.1(8) . . ?
C10 C9 H9 124.9 . . ?
C8 C9 H9 124.9 . . ?
C9 C10 C12 109.7(8) . . ?
C9 C10 C11 126.6(8) . . ?
C12 C10 C11 123.7(8) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C22 129.9(8) . . ?
C13 C12 C10 121.5(7) . . ?
C22 C12 C10 108.5(8) . . ?
C14 C13 C12 130.8(8) . . ?
C14 C13 H13 114.6 . . ?
C12 C13 H13 114.6 . . ?
C13 C14 C18 123.6(8) . . ?
C13 C14 C15 120.2(7) . . ?
C18 C14 C15 116.2(8) . . ?
C16 C15 C14 114.5(8) . . ?
C16 C15 C17 110.2(7) . . ?
C14 C15 C17 109.1(7) . . ?
C16 C15 H15 107.6 . . ?
C14 C15 H15 107.6 . . ?
C17 C15 H15 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 130.6(8) . . ?
C19 C18 H18 114.7 . . ?
C14 C18 H18 114.7 . . ?
C18 C19 C20 132.6(8) . . ?
C18 C19 H19 113.7 . . ?
C20 C19 H19 113.7 . . ?
C22 C20 C19 124.3(8) . . ?
C22 C20 C21 121.6(8) . . ?
C19 C20 C21 114.1(7) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 C12 127.1(8) . . ?
C20 C22 C8 128.1(8) . . ?
C12 C22 C8 104.7(7) . . ?
C38 C31 C32 127.7(9) . . ?
C38 C31 H31 116.2 . . ?
C32 C31 H31 116.2 . . ?
C33 C32 C37 117.5(9) . . ?
C33 C32 C31 117.8(9) . . ?
C37 C32 C31 124.6(8) . . ?
C34 C33 C32 121.6(9) . . ?
C34 C33 H33 119.2 . . ?
C32 C33 H33 119.2 . . ?
C35 C34 C33 118.4(8) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C35 C36 122.1(9) . . ?
C34 C35 Br2 118.5(7) . . ?
C36 C35 Br2 119.4(7) . . ?
C37 C36 C35 118.9(9) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C36 C37 C32 121.4(8) . . ?
C36 C37 H37 119.3 . . ?
C32 C37 H37 119.3 . . ?
C31 C38 C52 126.0(10) . . ?
C31 C38 C39 127.2(9) . . ?
C52 C38 C39 106.5(8) . . ?
C40 C39 C49 126.3(10) . . ?
C40 C39 C38 128.6(9) . . ?
C49 C39 C38 105.1(8) . . ?
C42 C40 C39 124.3(10) . . ?
C42 C40 C41 114.1(10) . . ?
C39 C40 C41 121.6(10) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C40 134.1(11) . . ?
C43 C42 H42 112.9 . . ?
C40 C42 H42 112.9 . . ?
C42 C43 C44 129.9(11) . . ?
C42 C43 H43 115.1 . . ?
C44 C43 H43 115.1 . . ?
C48 C44 C43 124.1(10) . . ?
C48 C44 C45 117.7(10) . . ?
C43 C44 C45 118.1(10) . . ?
C46 C45 C47 117.5(14) . . ?
C46 C45 C44 113.9(12) . . ?
C47 C45 C44 111.5(10) . . ?
C46 C45 H45 104.0 . . ?
C47 C45 H45 104.0 . . ?
C44 C45 H45 104.0 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 C49 131.2(10) . . ?
C44 C48 H48 114.4 . . ?
C49 C48 H48 114.4 . . ?
C48 C49 C50 121.5(9) . . ?
C48 C49 C39 129.8(10) . . ?
C50 C49 C39 108.7(9) . . ?
C52 C50 C49 108.7(9) . . ?
C52 C50 C51 126.4(10) . . ?
C49 C50 C51 124.9(10) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 C38 111.0(10) . . ?
C50 C52 H52 124.5 . . ?
C38 C52 H52 124.5 . . ?
C68 C61 C62 127.6(8) . . ?
C68 C61 H61 116.2 . . ?
C62 C61 H61 116.2 . . ?
C67 C62 C63 117.6(9) . . ?
C67 C62 C61 124.1(8) . . ?
C63 C62 C61 118.2(8) . . ?
C64 C63 C62 121.6(9) . . ?
C64 C63 H63 119.2 . . ?
C62 C63 H63 119.2 . . ?
C63 C64 C65 118.1(8) . . ?
C63 C64 H64 120.9 . . ?
C65 C64 H64 120.9 . . ?
C64 C65 C66 122.5(9) . . ?
C64 C65 Br3 118.5(6) . . ?
C66 C65 Br3 118.9(8) . . ?
C67 C66 C65 118.6(9) . . ?
C67 C66 H66 120.7 . . ?
C65 C66 H66 120.7 . . ?
C66 C67 C62 121.5(8) . . ?
C66 C67 H67 119.2 . . ?
C62 C67 H67 119.2 . . ?
C61 C68 C82 127.2(9) . . ?
C61 C68 C69 126.6(8) . . ?
C82 C68 C69 105.4(7) . . ?
C70 C69 C79 125.7(9) . . ?
C70 C69 C68 127.9(8) . . ?
C79 C69 C68 106.1(7) . . ?
C69 C70 C72 124.9(8) . . ?
C69 C70 C71 121.8(9) . . ?
C72 C70 C71 113.3(8) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 C70 131.8(9) . . ?
C73 C72 H72 114.1 . . ?
C70 C72 H72 114.1 . . ?
C72 C73 C74 131.0(10) . . ?
C72 C73 H73 114.5 . . ?
C74 C73 H73 114.5 . . ?
C78 C74 C73 123.1(9) . . ?
C78 C74 C75 121.4(8) . . ?
C73 C74 C75 115.4(9) . . ?
C76 C75 C74 114.8(8) . . ?
C76 C75 C77 111.6(9) . . ?
C74 C75 C77 106.6(8) . . ?
C76 C75 H75 107.9 . . ?
C74 C75 H75 107.9 . . ?
C77 C75 H75 107.9 . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C74 C78 C79 131.5(8) . . ?
C74 C78 H78 114.3 . . ?
C79 C78 H78 114.3 . . ?
C78 C79 C80 122.1(7) . . ?
C78 C79 C69 129.7(8) . . ?
C80 C79 C69 108.2(7) . . ?
C82 C80 C79 109.0(7) . . ?
C82 C80 C81 126.7(8) . . ?
C79 C80 C81 124.3(8) . . ?
C80 C81 H81A 109.5 . . ?
C80 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C80 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C80 C82 C68 111.3(8) . . ?
C80 C82 H82 124.4 . . ?
C68 C82 H82 124.4 . . ?
F3 P1 F4 91.7(6) . . ?
F3 P1 F5 177.8(6) . . ?
F4 P1 F5 90.1(5) . . ?
F3 P1 F6 88.3(6) . . ?
F4 P1 F6 177.1(5) . . ?
F5 P1 F6 89.8(5) . . ?
F3 P1 F2 91.3(5) . . ?
F4 P1 F2 92.0(4) . . ?
F5 P1 F2 89.8(5) . . ?
F6 P1 F2 90.9(4) . . ?
F3 P1 F1 89.5(5) . . ?
F4 P1 F1 88.6(4) . . ?
F5 P1 F1 89.4(4) . . ?
F6 P1 F1 88.5(4) . . ?
F2 P1 F1 179.0(4) . . ?
F11A P2 F8 87.1(7) . . ?
F8 P2 F11 89.9(17) . . ?
F11A P2 F10A 92.1(10) . . ?
F8 P2 F10A 96.3(10) . . ?
F11A P2 F12A 85.4(11) . . ?
F8 P2 F12A 98.7(9) . . ?
F10A P2 F12A 164.7(12) . . ?
F11A P2 F7 91.4(8) . . ?
F8 P2 F7 176.0(6) . . ?
F11 P2 F7 91.2(16) . . ?
F10A P2 F7 80.0(9) . . ?
F12A P2 F7 84.9(8) . . ?
F11A P2 F9A 167.4(9) . . ?
F8 P2 F9A 104.9(7) . . ?
F10A P2 F9A 90.6(9) . . ?
F12A P2 F9A 88.7(8) . . ?
F7 P2 F9A 76.9(7) . . ?
F8 P2 F10 86.2(10) . . ?
F11 P2 F10 90(2) . . ?
F7 P2 F10 89.9(10) . . ?
F8 P2 F12 75.7(11) . . ?
F11 P2 F12 84.3(16) . . ?
F7 P2 F12 108.2(11) . . ?
F10 P2 F12 161.2(15) . . ?
F8 P2 F9 76.1(10) . . ?
F11 P2 F9 165.6(17) . . ?
F7 P2 F9 103.0(9) . . ?
F10 P2 F9 92(2) . . ?
F12 P2 F9 88.7(13) . . ?
F16 P3 F17 100.7(18) . . ?
F18A P3 F17A 95.9(11) . . ?
F16 P3 F13 89.8(12) . . ?
F18A P3 F13 94.5(7) . . ?
F17 P3 F13 79.5(11) . . ?
F17A P3 F13 95.8(7) . . ?
F16 P3 F14 90.1(12) . . ?
F18A P3 F14 85.7(7) . . ?
F17 P3 F14 100.4(11) . . ?
F17A P3 F14 84.1(7) . . ?
F13 P3 F14 179.8(5) . . ?
F18A P3 F15A 89.6(12) . . ?
F17A P3 F15A 170.4(10) . . ?
F13 P3 F15A 91.5(8) . . ?
F14 P3 F15A 88.5(8) . . ?
F18A P3 F16A 172.3(8) . . ?
F17A P3 F16A 86.7(9) . . ?
F13 P3 F16A 92.5(5) . . ?
F14 P3 F16A 87.3(6) . . ?
F15A P3 F16A 86.9(11) . . ?
F16 P3 F15 90.4(17) . . ?
F17 P3 F15 161(2) . . ?
F13 P3 F15 85.4(14) . . ?
F14 P3 F15 94.7(14) . . ?
F16 P3 F18 166.8(15) . . ?
F17 P3 F18 88.1(13) . . ?
F13 P3 F18 82.1(6) . . ?
F14 P3 F18 98.1(6) . . ?
F15 P3 F18 78.7(14) . . ?

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
C8 C1 C2 C7 -30.4(14) . . . . ?
C8 C1 C2 C3 150.1(8) . . . . ?
C7 C2 C3 C4 3.4(12) . . . . ?
C1 C2 C3 C4 -177.1(8) . . . . ?
C2 C3 C4 C5 -0.3(12) . . . . ?
C3 C4 C5 C6 -2.0(12) . . . . ?
C3 C4 C5 Br1 176.5(6) . . . . ?
C4 C5 C6 C7 1.1(12) . . . . ?
Br1 C5 C6 C7 -177.5(6) . . . . ?
C5 C6 C7 C2 2.3(12) . . . . ?
C3 C2 C7 C6 -4.4(12) . . . . ?
C1 C2 C7 C6 176.1(8) . . . . ?
C2 C1 C8 C9 -8.1(14) . . . . ?
C2 C1 C8 C22 -176.7(8) . . . . ?
C1 C8 C9 C10 -167.8(8) . . . . ?
C22 C8 C9 C10 2.8(10) . . . . ?
C8 C9 C10 C12 -0.5(10) . . . . ?
C8 C9 C10 C11 178.1(9) . . . . ?
C9 C10 C12 C13 177.4(7) . . . . ?
C11 C10 C12 C13 -1.2(14) . . . . ?
C9 C10 C12 C22 -2.0(10) . . . . ?
C11 C10 C12 C22 179.3(8) . . . . ?
C22 C12 C13 C14 3.3(15) . . . . ?
C10 C12 C13 C14 -176.0(8) . . . . ?
C12 C13 C14 C18 -3.6(14) . . . . ?
C12 C13 C14 C15 178.8(8) . . . . ?
C13 C14 C15 C16 -23.7(11) . . . . ?
C18 C14 C15 C16 158.5(8) . . . . ?
C13 C14 C15 C17 100.3(9) . . . . ?
C18 C14 C15 C17 -77.4(9) . . . . ?
C13 C14 C18 C19 -4.4(14) . . . . ?
C15 C14 C18 C19 173.3(8) . . . . ?
C14 C18 C19 C20 5.2(17) . . . . ?
C18 C19 C20 C22 5.7(15) . . . . ?
C18 C19 C20 C21 -173.2(9) . . . . ?
C19 C20 C22 C12 -13.2(13) . . . . ?
C21 C20 C22 C12 165.7(8) . . . . ?
C19 C20 C22 C8 171.3(8) . . . . ?
C21 C20 C22 C8 -9.8(13) . . . . ?
C13 C12 C22 C20 7.8(14) . . . . ?
C10 C12 C22 C20 -172.8(8) . . . . ?
C13 C12 C22 C8 -175.8(8) . . . . ?
C10 C12 C22 C8 3.6(9) . . . . ?
C1 C8 C22 C20 -17.2(13) . . . . ?
C9 C8 C22 C20 172.5(8) . . . . ?
C1 C8 C22 C12 166.5(8) . . . . ?
C9 C8 C22 C12 -3.9(8) . . . . ?
C38 C31 C32 C33 -153.6(9) . . . . ?
C38 C31 C32 C37 29.8(15) . . . . ?
C37 C32 C33 C34 -3.6(14) . . . . ?
C31 C32 C33 C34 179.5(9) . . . . ?
C32 C33 C34 C35 2.3(14) . . . . ?
C33 C34 C35 C36 0.1(13) . . . . ?
C33 C34 C35 Br2 -179.7(7) . . . . ?
C34 C35 C36 C37 -1.1(13) . . . . ?
Br2 C35 C36 C37 178.7(6) . . . . ?
C35 C36 C37 C32 -0.3(13) . . . . ?
C33 C32 C37 C36 2.6(13) . . . . ?
C31 C32 C37 C36 179.2(9) . . . . ?
C32 C31 C38 C52 8.2(16) . . . . ?
C32 C31 C38 C39 -179.0(9) . . . . ?
C31 C38 C39 C40 7.4(16) . . . . ?
C52 C38 C39 C40 -178.7(9) . . . . ?
C31 C38 C39 C49 -172.8(9) . . . . ?
C52 C38 C39 C49 1.1(10) . . . . ?
C49 C39 C40 C42 5.7(15) . . . . ?
C38 C39 C40 C42 -174.6(9) . . . . ?
C49 C39 C40 C41 -174.6(9) . . . . ?
C38 C39 C40 C41 5.1(15) . . . . ?
C39 C40 C42 C43 -4.8(19) . . . . ?
C41 C40 C42 C43 175.5(12) . . . . ?
C40 C42 C43 C44 -1(2) . . . . ?
C42 C43 C44 C48 4.2(19) . . . . ?
C42 C43 C44 C45 -179.6(11) . . . . ?
C48 C44 C45 C46 -101.4(18) . . . . ?
C43 C44 C45 C46 82.1(18) . . . . ?
C48 C44 C45 C47 122.7(12) . . . . ?
C43 C44 C45 C47 -53.7(16) . . . . ?
C43 C44 C48 C49 -1.9(18) . . . . ?
C45 C44 C48 C49 -178.1(10) . . . . ?
C44 C48 C49 C50 178.7(10) . . . . ?
C44 C48 C49 C39 -0.3(18) . . . . ?
C40 C39 C49 C48 -2.1(16) . . . . ?
C38 C39 C49 C48 178.1(9) . . . . ?
C40 C39 C49 C50 178.7(9) . . . . ?
C38 C39 C49 C50 -1.1(10) . . . . ?
C48 C49 C50 C52 -178.6(9) . . . . ?
C39 C49 C50 C52 0.6(11) . . . . ?
C48 C49 C50 C51 1.3(15) . . . . ?
C39 C49 C50 C51 -179.5(9) . . . . ?
C49 C50 C52 C38 0.2(12) . . . . ?
C51 C50 C52 C38 -179.8(10) . . . . ?
C31 C38 C52 C50 173.2(9) . . . . ?
C39 C38 C52 C50 -0.8(11) . . . . ?
C68 C61 C62 C67 27.5(15) . . . . ?
C68 C61 C62 C63 -157.3(9) . . . . ?
C67 C62 C63 C64 -0.8(13) . . . . ?
C61 C62 C63 C64 -176.3(8) . . . . ?
C62 C63 C64 C65 -1.5(13) . . . . ?
C63 C64 C65 C66 2.0(13) . . . . ?
C63 C64 C65 Br3 179.7(7) . . . . ?
C64 C65 C66 C67 0.0(13) . . . . ?
Br3 C65 C66 C67 -177.7(7) . . . . ?
C65 C66 C67 C62 -2.5(13) . . . . ?
C63 C62 C67 C66 2.9(13) . . . . ?
C61 C62 C67 C66 178.1(9) . . . . ?
C62 C61 C68 C82 10.6(15) . . . . ?
C62 C61 C68 C69 178.9(8) . . . . ?
C61 C68 C69 C70 18.4(14) . . . . ?
C82 C68 C69 C70 -171.3(8) . . . . ?
C61 C68 C69 C79 -167.1(8) . . . . ?
C82 C68 C69 C79 3.2(9) . . . . ?
C79 C69 C70 C72 17.5(13) . . . . ?
C68 C69 C70 C72 -169.0(8) . . . . ?
C79 C69 C70 C71 -164.5(8) . . . . ?
C68 C69 C70 C71 9.0(13) . . . . ?
C69 C70 C72 C73 -11.5(15) . . . . ?
C71 C70 C72 C73 170.4(10) . . . . ?
C70 C72 C73 C74 -4.6(18) . . . . ?
C72 C73 C74 C78 7.6(16) . . . . ?
C72 C73 C74 C75 -168.4(10) . . . . ?
C78 C74 C75 C76 21.3(12) . . . . ?
C73 C74 C75 C76 -162.6(8) . . . . ?
C78 C74 C75 C77 -102.8(10) . . . . ?
C73 C74 C75 C77 73.3(10) . . . . ?
C73 C74 C78 C79 3.2(14) . . . . ?
C75 C74 C78 C79 179.0(8) . . . . ?
C74 C78 C79 C80 175.9(8) . . . . ?
C74 C78 C79 C69 -6.6(14) . . . . ?
C70 C69 C79 C78 -6.5(13) . . . . ?
C68 C69 C79 C78 178.8(8) . . . . ?
C70 C69 C79 C80 171.3(8) . . . . ?
C68 C69 C79 C80 -3.4(8) . . . . ?
C78 C79 C80 C82 -179.7(7) . . . . ?
C69 C79 C80 C82 2.3(9) . . . . ?
C78 C79 C80 C81 -1.7(13) . . . . ?
C69 C79 C80 C81 -179.7(8) . . . . ?
C79 C80 C82 C68 -0.2(10) . . . . ?
C81 C80 C82 C68 -178.2(8) . . . . ?
C61 C68 C82 C80 168.3(9) . . . . ?
C69 C68 C82 C80 -1.9(10) . . . . ?

_refine_diff_density_max         0.906
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.070

####################################################################### 
# 
# 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_s21sel8
_database_code_depnum_ccdc_archive 'CCDC 2129314'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C32 H40 N O), 4(F6 P), 2(H2.50 O1.25), 3(H2 O)'
_chemical_formula_sum            'C128 H171 F24 N4 O9.50 P4'
_chemical_formula_weight         2497.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

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

_cell_length_a                   12.3599(10)
_cell_length_b                   12.9645(7)
_cell_length_c                   20.9049(12)
_cell_angle_alpha                75.138(5)
_cell_angle_beta                 74.245(6)
_cell_angle_gamma                83.084(6)
_cell_volume                     3111.5(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5289
_cell_measurement_theta_min      8.8520
_cell_measurement_theta_max      68.0310

_exptl_crystal_description       block
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             1319
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.371
_shelx_estimated_absorpt_T_min   0.726
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_T_min  0.90720
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.792
_oxdiff_exptl_absorpt_empirical_full_max 1.374
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            20034
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.521
_diffrn_reflns_theta_max         68.847
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             20034
_reflns_number_gt                12243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;Refined as a 2-component twin.
 the two PF6 groups show rotational disorder 
 in the ratio 70:30. All OH-hydrogen atoms have been located in 
 the difference Fourier map and were refined with bond lenghts restraints,Twin
;
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6852 14079 6155 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3148 14112 6155 nmt 0.0270 -0.9511 -0.0157 -1.0488 -0.0264 0.0135 -0.0029
0.0072 -1.0006
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by 179.8855° 
around [0.70 -0.71 -0.00] (reciprocal) or [0.73 -0.68 -0.01] (direct)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1451P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20034
_refine_ls_number_parameters     890
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0807
_refine_ls_wR_factor_ref         0.2420
_refine_ls_wR_factor_gt          0.2207
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.2714(3) 0.6359(3) 0.87709(16) 0.0451(9) Uani 1 1 d . . . . .
O1 O 0.0879(3) 0.5854(3) 0.71690(14) 0.0449(7) Uani 1 1 d D . . . .
H1A H 0.068902 0.629936 0.684311 0.067 Uiso 1 1 calc DR U . . .
C1 C 0.2813(3) 0.6312(3) 0.61138(18) 0.0341(8) Uani 1 1 d . . . . .
H1 H 0.229921 0.583305 0.610038 0.015(8) Uiso 1 1 calc R . . . .
C2 C 0.2753(3) 0.6490(3) 0.67512(17) 0.0326(8) Uani 1 1 d . . . . .
C3 C 0.1753(3) 0.6200(3) 0.73006(18) 0.0334(8) Uani 1 1 d . . . . .
C4 C 0.1701(3) 0.6225(3) 0.79661(17) 0.0321(8) Uani 1 1 d . . . . .
C5 C 0.0602(4) 0.5976(3) 0.85274(18) 0.0379(9) Uani 1 1 d . . . . .
C6 C 0.0459(4) 0.4768(4) 0.8742(2) 0.0468(10) Uani 1 1 d . . . . .
H6A H 0.044888 0.450765 0.834291 0.070 Uiso 1 1 calc R U . . .
H6B H -0.025035 0.461660 0.909075 0.070 Uiso 1 1 calc R U . . .
H6C H 0.108828 0.440616 0.892899 0.070 Uiso 1 1 calc R U . . .
C7 C -0.0428(4) 0.6558(5) 0.8302(2) 0.0619(14) Uani 1 1 d . . . . .
H7A H -0.067564 0.615496 0.803473 0.093 Uiso 1 1 calc R U . . .
H7B H -0.023439 0.727328 0.802109 0.093 Uiso 1 1 calc R U . . .
H7C H -0.103673 0.661967 0.870615 0.093 Uiso 1 1 calc R U . . .
C8 C 0.0685(4) 0.6383(4) 0.9135(2) 0.0470(11) Uani 1 1 d . . . . .
H8A H 0.061986 0.717372 0.901630 0.056 Uiso 1 1 calc R U . . .
H8B H 0.004390 0.613044 0.952826 0.056 Uiso 1 1 calc R U . . .
C9 C 0.1743(4) 0.6028(4) 0.9343(2) 0.0496(11) Uani 1 1 d . . . . .
H9A H 0.175867 0.633925 0.972570 0.060 Uiso 1 1 calc R U . . .
H9B H 0.178200 0.524037 0.950359 0.060 Uiso 1 1 calc R U . . .
C10 C 0.3741(5) 0.6444(6) 0.8985(2) 0.080(2) Uani 1 1 d . . . . .
H10A H 0.375840 0.589104 0.940915 0.096 Uiso 1 1 calc R U . . .
H10B H 0.372224 0.715262 0.908555 0.096 Uiso 1 1 calc R U . . .
C11 C 0.4818(5) 0.6298(5) 0.8422(3) 0.0678(14) Uani 1 1 d . . . . .
H11A H 0.548970 0.644504 0.854950 0.081 Uiso 1 1 calc R U . . .
H11B H 0.490532 0.555529 0.836522 0.081 Uiso 1 1 calc R U . . .
C12 C 0.4703(4) 0.7076(3) 0.77602(19) 0.0399(9) Uani 1 1 d . . . . .
C13 C 0.4504(6) 0.8217(5) 0.7845(3) 0.0698(15) Uani 1 1 d . . . . .
H13A H 0.462706 0.871281 0.739436 0.105 Uiso 1 1 calc R U . . .
H13B H 0.502820 0.835003 0.808914 0.105 Uiso 1 1 calc R U . . .
H13C H 0.372866 0.832401 0.810775 0.105 Uiso 1 1 calc R U . . .
C14 C 0.5789(5) 0.7022(8) 0.7213(3) 0.097(3) Uani 1 1 d . . . . .
H14A H 0.588219 0.632693 0.709517 0.145 Uiso 1 1 calc R U . . .
H14B H 0.642636 0.711324 0.738479 0.145 Uiso 1 1 calc R U . . .
H14C H 0.576158 0.759232 0.680512 0.145 Uiso 1 1 calc R U . . .
C15 C 0.3688(3) 0.6792(3) 0.75760(19) 0.0348(8) Uani 1 1 d . . . . .
C16 C 0.3670(3) 0.6824(3) 0.69248(18) 0.0343(8) Uani 1 1 d . . . . .
H16 H 0.430326 0.708264 0.656600 0.041 Uiso 1 1 calc R U . . .
C17 C 0.2684(3) 0.6458(3) 0.81227(17) 0.0337(8) Uani 1 1 d . . . . .
C18 C 0.3558(3) 0.6769(3) 0.54805(17) 0.0332(8) Uani 1 1 d . . . . .
C19 C 0.3995(3) 0.7792(3) 0.53192(19) 0.0379(8) Uani 1 1 d . . . . .
H19 H 0.391917 0.821258 0.564151 0.045 Uiso 1 1 calc R U . . .
C20 C 0.4543(4) 0.8100(3) 0.46387(19) 0.0387(9) Uani 1 1 d . . . . .
C21 C 0.5074(4) 0.9142(4) 0.4285(2) 0.0496(11) Uani 1 1 d . . . . .
H21A H 0.589466 0.902226 0.416301 0.074 Uiso 1 1 calc R U . . .
H21B H 0.486072 0.963293 0.459159 0.074 Uiso 1 1 calc R U . . .
H21C H 0.481391 0.945450 0.387014 0.074 Uiso 1 1 calc R U . . .
C22 C 0.4515(3) 0.7247(3) 0.43349(18) 0.0327(8) Uani 1 1 d . . . . .
C23 C 0.4987(3) 0.7326(3) 0.36413(19) 0.0395(9) Uani 1 1 d . . . . .
H23 H 0.530713 0.798835 0.339734 0.047 Uiso 1 1 calc R U . . .
C24 C 0.5066(4) 0.6595(3) 0.32492(18) 0.0389(9) Uani 1 1 d . . . . .
C25 C 0.5565(4) 0.6969(4) 0.2478(2) 0.0484(10) Uani 1 1 d . . . . .
H25 H 0.573752 0.773491 0.238649 0.058 Uiso 1 1 calc R U . . .
C26 C 0.4705(4) 0.6935(4) 0.2088(2) 0.0556(12) Uani 1 1 d . . . . .
H26A H 0.503258 0.718997 0.159704 0.083 Uiso 1 1 calc R U . . .
H26B H 0.403988 0.739342 0.223355 0.083 Uiso 1 1 calc R U . . .
H26C H 0.448465 0.619857 0.218249 0.083 Uiso 1 1 calc R U . . .
C27 C 0.6664(5) 0.6364(5) 0.2239(2) 0.0618(14) Uani 1 1 d . . . . .
H27A H 0.652448 0.561412 0.229510 0.093 Uiso 1 1 calc R U . . .
H27B H 0.718281 0.640663 0.251125 0.093 Uiso 1 1 calc R U . . .
H27C H 0.699810 0.668017 0.175578 0.093 Uiso 1 1 calc R U . . .
C28 C 0.4748(4) 0.5551(4) 0.3516(2) 0.0439(10) Uani 1 1 d . . . . .
H28 H 0.492686 0.512294 0.319029 0.053 Uiso 1 1 calc R U . . .
C29 C 0.4213(3) 0.5017(3) 0.4173(2) 0.0388(9) Uani 1 1 d . . . . .
H29 H 0.411886 0.428346 0.421643 0.047 Uiso 1 1 calc R U . . .
C30 C 0.3784(3) 0.5359(3) 0.47866(18) 0.0340(8) Uani 1 1 d . . . . .
C31 C 0.3184(4) 0.4525(3) 0.53776(19) 0.0392(9) Uani 1 1 d . . . . .
H31A H 0.237621 0.472466 0.548909 0.059 Uiso 1 1 calc R U . . .
H31B H 0.347973 0.447232 0.577541 0.059 Uiso 1 1 calc R U . . .
H31C H 0.330398 0.383252 0.525365 0.059 Uiso 1 1 calc R U . . .
C32 C 0.3894(3) 0.6378(3) 0.48649(17) 0.0326(8) Uani 1 1 d . . . . .
N2 N 0.8655(3) 0.1854(3) 0.63534(17) 0.0453(8) Uani 1 1 d . . . . .
O2 O 0.8790(3) 0.3897(2) 0.79133(14) 0.0449(7) Uani 1 1 d D . . . .
H2 H 0.824(6) 0.401(7) 0.826(3) 0.13(3) Uiso 1 1 d D . . . .
C41 C 0.8496(3) 0.2078(3) 0.89667(18) 0.0344(8) Uani 1 1 d . . . . .
H41 H 0.896414 0.260941 0.896414 0.041 Uiso 1 1 calc R U . . .
C42 C 0.8296(3) 0.2076(3) 0.83464(18) 0.0343(8) Uani 1 1 d . . . . .
C43 C 0.8561(3) 0.2995(3) 0.77822(18) 0.0339(8) Uani 1 1 d . . . . .
C44 C 0.8611(3) 0.2971(3) 0.71224(18) 0.0323(8) Uani 1 1 d . . . . .
C45 C 0.8873(3) 0.3974(3) 0.65327(19) 0.0382(9) Uani 1 1 d . . . . .
C46 C 0.8187(4) 0.4970(4) 0.6709(2) 0.0508(11) Uani 1 1 d . . . . .
H46A H 0.818722 0.551819 0.628766 0.076 Uiso 1 1 calc R U . . .
H46B H 0.852192 0.524347 0.700294 0.076 Uiso 1 1 calc R U . . .
H46C H 0.741136 0.478594 0.694978 0.076 Uiso 1 1 calc R U . . .
C47 C 1.0137(4) 0.4157(4) 0.6342(2) 0.0487(11) Uani 1 1 d . . . . .
H47A H 1.056717 0.354019 0.618974 0.073 Uiso 1 1 calc R U . . .
H47B H 1.035072 0.424602 0.674272 0.073 Uiso 1 1 calc R U . . .
H47C H 1.030010 0.480195 0.597307 0.073 Uiso 1 1 calc R U . . .
C48 C 0.8535(4) 0.3766(4) 0.5926(2) 0.0506(11) Uani 1 1 d . . . . .
H48A H 0.770382 0.377795 0.603072 0.061 Uiso 1 1 calc R U . . .
H48B H 0.879181 0.435191 0.552003 0.061 Uiso 1 1 calc R U . . .
C49 C 0.9003(4) 0.2739(4) 0.5759(2) 0.0529(12) Uani 1 1 d . . . . .
H49A H 0.873603 0.264466 0.537279 0.064 Uiso 1 1 calc R U . . .
H49B H 0.983550 0.273995 0.561653 0.064 Uiso 1 1 calc R U . . .
C50 C 0.8652(5) 0.0815(4) 0.6184(2) 0.0568(13) Uani 1 1 d . . . . .
H50A H 0.934457 0.072006 0.582725 0.068 Uiso 1 1 calc R U . . .
H50B H 0.799978 0.082362 0.599270 0.068 Uiso 1 1 calc R U . . .
C51 C 0.8590(5) -0.0120(4) 0.6792(2) 0.0533(11) Uani 1 1 d . . . . .
H51A H 0.932791 -0.025676 0.690749 0.064 Uiso 1 1 calc R U . . .
H51B H 0.841990 -0.076674 0.667607 0.064 Uiso 1 1 calc R U . . .
C52 C 0.7686(4) 0.0101(3) 0.7404(2) 0.0386(9) Uani 1 1 d . . . . .
C53 C 0.6546(4) 0.0370(4) 0.7226(2) 0.0474(10) Uani 1 1 d . . . . .
H53A H 0.659651 0.101105 0.685145 0.071 Uiso 1 1 calc R U . . .
H53B H 0.597043 0.050112 0.762788 0.071 Uiso 1 1 calc R U . . .
H53C H 0.634283 -0.023006 0.708509 0.071 Uiso 1 1 calc R U . . .
C54 C 0.7597(5) -0.0877(3) 0.8000(2) 0.0514(11) Uani 1 1 d . . . . .
H54A H 0.738287 -0.148428 0.787056 0.077 Uiso 1 1 calc R U . . .
H54B H 0.702433 -0.072559 0.839712 0.077 Uiso 1 1 calc R U . . .
H54C H 0.832541 -0.105041 0.811448 0.077 Uiso 1 1 calc R U . . .
C55 C 0.8026(3) 0.1089(3) 0.75630(19) 0.0351(8) Uani 1 1 d . . . . .
C56 C 0.7958(3) 0.1166(3) 0.82019(18) 0.0328(8) Uani 1 1 d . . . . .
H56 H 0.767161 0.058894 0.857275 0.039 Uiso 1 1 calc R U . . .
C57 C 0.8439(3) 0.1986(3) 0.69913(18) 0.0323(8) Uani 1 1 d . . . . .
C58 C 0.8070(4) 0.1363(3) 0.96090(18) 0.0352(8) Uani 1 1 d . . . . .
C59 C 0.6985(4) 0.0953(3) 0.9795(2) 0.0412(9) Uani 1 1 d . . . . .
H59 H 0.651267 0.103686 0.949226 0.049 Uiso 1 1 calc R U . . .
C60 C 0.6707(4) 0.0418(3) 1.0474(2) 0.0431(10) Uani 1 1 d . . . . .
C61 C 0.5590(5) -0.0043(4) 1.0846(2) 0.0586(13) Uani 1 1 d . . . . .
H61A H 0.504615 0.023011 1.056946 0.088 Uiso 1 1 calc R U . . .
H61B H 0.532174 0.016295 1.128457 0.088 Uiso 1 1 calc R U . . .
H61C H 0.567140 -0.082397 1.092790 0.088 Uiso 1 1 calc R U . . .
C62 C 0.7615(4) 0.0449(3) 1.07477(19) 0.0394(9) Uani 1 1 d . . . . .
C63 C 0.7581(4) 0.0008(3) 1.1436(2) 0.0466(11) Uani 1 1 d . . . . .
H63 H 0.690146 -0.032156 1.169535 0.056 Uiso 1 1 calc R U . . .
C64 C 0.8353(5) -0.0032(3) 1.1803(2) 0.0467(11) Uani 1 1 d . . . . .
C65 C 0.7934(12) -0.0486(5) 1.2585(3) 0.046(3) Uani 0.83(3) 1 d . . P A 1
H65 H 0.711898 -0.062358 1.268628 0.056 Uiso 0.83(3) 1 calc R U P A 1
C65A C 0.858(5) -0.046(2) 1.2532(13) 0.045(10) Uani 0.17(3) 1 d . . P A 2
H65A H 0.939461 -0.033485 1.243919 0.054 Uiso 0.17(3) 1 calc R U P A 2
C66 C 0.8027(5) 0.0347(5) 1.2961(2) 0.0647(14) Uani 1 1 d . . . . .
H66A H 0.881496 0.052422 1.285248 0.097 Uiso 1 1 calc R U . A 1
H66B H 0.775716 0.006131 1.345440 0.097 Uiso 1 1 calc R U . A 1
H66C H 0.756835 0.099226 1.281736 0.097 Uiso 1 1 calc R U . A 1
C67 C 0.8550(7) -0.1530(5) 1.2797(3) 0.090(2) Uani 1 1 d . . . . .
H67A H 0.934301 -0.141159 1.273583 0.135 Uiso 1 1 calc R U . A 1
H67B H 0.849469 -0.201020 1.251407 0.135 Uiso 1 1 calc R U . A 1
H67C H 0.821434 -0.185421 1.327822 0.135 Uiso 1 1 calc R U . A 1
C68 C 0.9428(5) 0.0304(4) 1.1518(2) 0.0540(12) Uani 1 1 d . . . . .
H68 H 0.988117 0.017693 1.183521 0.065 Uiso 1 1 calc R U . . .
C69 C 0.9986(4) 0.0799(3) 1.0846(2) 0.0457(10) Uani 1 1 d . . . . .
H69 H 1.075818 0.090373 1.078598 0.055 Uiso 1 1 calc R U . . .
C70 C 0.9599(4) 0.1170(3) 1.02429(19) 0.0367(8) Uani 1 1 d . . . . .
C71 C 1.0459(4) 0.1728(3) 0.9629(2) 0.0412(9) Uani 1 1 d . . . . .
H71A H 1.045905 0.146145 0.923108 0.062 Uiso 1 1 calc R U . . .
H71B H 1.120709 0.158664 0.972015 0.062 Uiso 1 1 calc R U . . .
H71C H 1.027172 0.249935 0.953748 0.062 Uiso 1 1 calc R U . . .
C72 C 0.8512(4) 0.1048(3) 1.02000(18) 0.0347(8) Uani 1 1 d . . . . .
P1 P 0.22526(12) 0.15712(13) 0.47292(7) 0.0595(4) Uani 1 1 d . . . . .
F1 F 0.3412(3) 0.2116(4) 0.4563(2) 0.0870(11) Uani 1 1 d . . . . .
F2 F 0.1084(3) 0.1034(3) 0.4866(2) 0.0882(12) Uani 1 1 d . . . . .
F3 F 0.1776(8) 0.1849(8) 0.5442(4) 0.119(3) Uani 0.694(11) 1 d . U P B 1
F4 F 0.2747(5) 0.1049(6) 0.4089(3) 0.084(2) Uani 0.694(11) 1 d . U P B 1
F5 F 0.1791(7) 0.2556(5) 0.4326(6) 0.115(4) Uani 0.694(11) 1 d . U P B 1
F6 F 0.2728(5) 0.0427(5) 0.5178(4) 0.0817(19) Uani 0.694(11) 1 d . U P B 1
F3A F 0.1569(12) 0.2871(11) 0.4809(9) 0.090(5) Uani 0.306(11) 1 d . U P B 2
F4A F 0.2834(11) 0.0672(10) 0.4617(12) 0.109(7) Uani 0.306(11) 1 d . U P B 2
F5A F 0.2112(12) 0.2062(14) 0.3921(6) 0.080(5) Uani 0.306(11) 1 d . U P B 2
F6A F 0.2295(17) 0.146(2) 0.5450(7) 0.124(8) Uani 0.306(11) 1 d . U P B 2
P2 P 0.37355(15) 0.30473(11) 0.00313(6) 0.0646(4) Uani 1 1 d . . . . .
F7 F 0.3467(5) 0.3755(4) -0.0629(2) 0.132(2) Uani 1 1 d . . . . .
F8 F 0.4180(5) 0.2412(3) 0.0679(2) 0.1072(15) Uani 1 1 d . . . . .
F9 F 0.3112(8) 0.3821(7) 0.0466(4) 0.123(3) Uani 0.719(10) 1 d . U P C 1
F10 F 0.4242(10) 0.2114(5) -0.0332(3) 0.116(3) Uani 0.719(10) 1 d . U P C 1
F11 F 0.4862(7) 0.3629(8) -0.0250(4) 0.135(4) Uani 0.719(10) 1 d . U P C 1
F12 F 0.2673(6) 0.2304(7) 0.0374(4) 0.123(3) Uani 0.719(10) 1 d . U P C 1
F9A F 0.396(3) 0.4124(12) 0.0228(12) 0.133(9) Uani 0.281(10) 1 d . U P C 2
F10A F 0.334(2) 0.242(2) -0.0418(14) 0.141(9) Uani 0.281(10) 1 d . U P C 2
F11A F 0.4900(18) 0.2699(16) -0.0324(12) 0.122(7) Uani 0.281(10) 1 d . U P C 2
F12A F 0.2281(17) 0.3442(17) 0.0160(9) 0.131(9) Uani 0.281(10) 1 d . U P C 2
O3 O 0.2761(5) 0.5719(3) 0.0943(2) 0.0778(13) Uani 1 1 d D . . . .
H3A H 0.344(3) 0.598(3) 0.088(2) 0.031(12) Uiso 1 1 d D . . . .
H3B H 0.295(4) 0.510(3) 0.086(3) 0.076(19) Uiso 1 1 d D . . . .
O4 O 0.0353(4) 0.7017(4) 0.6043(2) 0.0798(13) Uani 1 1 d D . . . .
H4A H 0.058126 0.769504 0.588694 0.096 Uiso 1 1 d DR U . . .
H4B H -0.035283 0.712084 0.606465 0.096 Uiso 1 1 d DR U . . .
O5 O 0.1298(10) 0.8859(8) 0.5573(6) 0.081(4) Uani 0.5 1 d D . P D 1
H5A H 0.171493 0.938651 0.543757 0.097 Uiso 0.5 1 d DR U P D 1
H5B H 0.091342 0.887985 0.597972 0.097 Uiso 0.5 1 d DR U P D 1
O6 O 0.0886(19) 0.849(2) 0.5812(12) 0.103(10) Uani 0.25 1 d D . P E 2
H6D H 0.066483 0.902381 0.558510 0.123 Uiso 0.25 1 d DR U P E 2
H6E H 0.153683 0.839782 0.568510 0.123 Uiso 0.25 1 d DR U P E 2


_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
N1 C17 1.338(5) . ?
N1 C9 1.461(5) . ?
N1 C10 1.481(7) . ?
O1 C3 1.337(5) . ?
O1 H1A 0.8400 . ?
C1 C2 1.391(5) . ?
C1 C18 1.421(5) . ?
C1 H1 0.9500 . ?
C2 C16 1.424(6) . ?
C2 C3 1.452(5) . ?
C3 C4 1.383(5) . ?
C4 C17 1.425(6) . ?
C4 C5 1.540(5) . ?
C5 C7 1.524(7) . ?
C5 C8 1.527(6) . ?
C5 C6 1.533(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.473(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.548(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.520(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C14 1.517(7) . ?
C12 C13 1.517(7) . ?
C12 C15 1.518(6) . ?
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 C16 1.358(5) . ?
C15 C17 1.463(5) . ?
C16 H16 0.9500 . ?
C18 C19 1.417(6) . ?
C18 C32 1.442(5) . ?
C19 C20 1.376(5) . ?
C19 H19 0.9500 . ?
C20 C22 1.418(6) . ?
C20 C21 1.497(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.390(5) . ?
C22 C32 1.480(5) . ?
C23 C24 1.382(6) . ?
C23 H23 0.9500 . ?
C24 C28 1.386(6) . ?
C24 C25 1.532(5) . ?
C25 C27 1.511(7) . ?
C25 C26 1.515(7) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.390(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.411(5) . ?
C29 H29 0.9500 . ?
C30 C32 1.399(6) . ?
C30 C31 1.502(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N2 C57 1.339(5) . ?
N2 C49 1.465(6) . ?
N2 C50 1.478(6) . ?
O2 C43 1.345(5) . ?
O2 H2 0.87(3) . ?
C41 C42 1.385(5) . ?
C41 C58 1.426(5) . ?
C41 H41 0.9500 . ?
C42 C56 1.424(6) . ?
C42 C43 1.442(5) . ?
C43 C44 1.372(5) . ?
C44 C57 1.424(6) . ?
C44 C45 1.542(5) . ?
C45 C46 1.527(6) . ?
C45 C48 1.531(6) . ?
C45 C47 1.536(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.474(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.506(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.518(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C54 1.522(6) . ?
C52 C53 1.531(6) . ?
C52 C55 1.534(5) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.344(5) . ?
C55 C57 1.463(5) . ?
C56 H56 0.9500 . ?
C58 C59 1.420(6) . ?
C58 C72 1.430(5) . ?
C59 C60 1.379(6) . ?
C59 H59 0.9500 . ?
C60 C62 1.400(7) . ?
C60 C61 1.499(6) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.397(5) . ?
C62 C72 1.485(5) . ?
C63 C64 1.365(7) . ?
C63 H63 0.9500 . ?
C64 C68 1.374(8) . ?
C64 C65 1.552(7) . ?
C64 C65A 1.57(3) . ?
C65 C67 1.495(10) . ?
C65 C66 1.519(9) . ?
C65 H65 1.0000 . ?
C65A C67 1.36(3) . ?
C65A C66 1.52(4) . ?
C65A H65A 1.0000 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C69 1.407(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.418(6) . ?
C69 H69 0.9500 . ?
C70 C72 1.401(6) . ?
C70 C71 1.506(6) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
P1 F4A 1.334(11) . ?
P1 F5 1.483(5) . ?
P1 F6A 1.492(16) . ?
P1 F3 1.563(7) . ?
P1 F1 1.587(4) . ?
P1 F4 1.596(5) . ?
P1 F2 1.603(4) . ?
P1 F6 1.674(6) . ?
P1 F5A 1.694(12) . ?
P1 F3A 1.818(13) . ?
P2 F11A 1.50(2) . ?
P2 F9 1.524(6) . ?
P2 F7 1.543(4) . ?
P2 F11 1.560(6) . ?
P2 F10 1.569(6) . ?
P2 F10A 1.58(2) . ?
P2 F8 1.594(4) . ?
P2 F12 1.615(7) . ?
P2 F9A 1.627(17) . ?
P2 F12A 1.77(2) . ?
F7 F10A 1.68(2) . ?
O3 H3A 0.90(2) . ?
O3 H3B 0.86(3) . ?
O4 H4A 0.9057 . ?
O4 H4B 0.8575 . ?
O5 H5A 0.8483 . ?
O5 H5B 0.8599 . ?
O6 H4A 1.1016 . ?
O6 H6D 0.7950 . ?
O6 H6E 0.7806 . ?

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
C17 N1 C9 121.7(4) . . ?
C17 N1 C10 124.3(4) . . ?
C9 N1 C10 113.6(4) . . ?
C3 O1 H1A 109.5 . . ?
C2 C1 C18 127.1(4) . . ?
C2 C1 H1 116.5 . . ?
C18 C1 H1 116.5 . . ?
C1 C2 C16 123.8(3) . . ?
C1 C2 C3 118.8(4) . . ?
C16 C2 C3 117.0(3) . . ?
O1 C3 C4 118.9(3) . . ?
O1 C3 C2 119.4(3) . . ?
C4 C3 C2 121.6(4) . . ?
C3 C4 C17 118.9(3) . . ?
C3 C4 C5 120.1(4) . . ?
C17 C4 C5 121.0(3) . . ?
C7 C5 C8 106.8(4) . . ?
C7 C5 C6 110.1(4) . . ?
C8 C5 C6 110.1(3) . . ?
C7 C5 C4 112.4(3) . . ?
C8 C5 C4 107.5(3) . . ?
C6 C5 C4 109.9(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C5 113.4(4) . . ?
C9 C8 H8A 108.9 . . ?
C5 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C5 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N1 C9 C8 110.7(3) . . ?
N1 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N1 C10 C11 111.3(4) . . ?
N1 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
N1 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 107.9(5) . . ?
C12 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C14 C12 C13 107.5(5) . . ?
C14 C12 C15 113.1(4) . . ?
C13 C12 C15 108.1(4) . . ?
C14 C12 C11 109.1(5) . . ?
C13 C12 C11 111.1(4) . . ?
C15 C12 C11 108.0(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 118.1(4) . . ?
C16 C15 C12 123.0(3) . . ?
C17 C15 C12 118.9(3) . . ?
C15 C16 C2 123.5(3) . . ?
C15 C16 H16 118.3 . . ?
C2 C16 H16 118.3 . . ?
N1 C17 C4 120.8(3) . . ?
N1 C17 C15 118.7(4) . . ?
C4 C17 C15 120.4(3) . . ?
C19 C18 C1 124.3(4) . . ?
C19 C18 C32 107.1(3) . . ?
C1 C18 C32 128.1(4) . . ?
C20 C19 C18 111.7(4) . . ?
C20 C19 H19 124.1 . . ?
C18 C19 H19 124.1 . . ?
C19 C20 C22 107.3(4) . . ?
C19 C20 C21 126.3(4) . . ?
C22 C20 C21 126.4(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C20 121.1(4) . . ?
C23 C22 C32 130.3(4) . . ?
C20 C22 C32 108.5(3) . . ?
C24 C23 C22 130.5(4) . . ?
C24 C23 H23 114.8 . . ?
C22 C23 H23 114.8 . . ?
C23 C24 C28 123.9(3) . . ?
C23 C24 C25 117.3(4) . . ?
C28 C24 C25 118.9(4) . . ?
C27 C25 C26 113.1(4) . . ?
C27 C25 C24 112.0(4) . . ?
C26 C25 C24 110.6(4) . . ?
C27 C25 H25 106.9 . . ?
C26 C25 H25 106.9 . . ?
C24 C25 H25 106.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 C29 131.7(4) . . ?
C24 C28 H28 114.2 . . ?
C29 C28 H28 114.2 . . ?
C28 C29 C30 132.1(4) . . ?
C28 C29 H29 113.9 . . ?
C30 C29 H29 113.9 . . ?
C32 C30 C29 124.7(4) . . ?
C32 C30 C31 120.8(3) . . ?
C29 C30 C31 114.4(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 C18 128.4(3) . . ?
C30 C32 C22 126.0(3) . . ?
C18 C32 C22 105.3(3) . . ?
C57 N2 C49 121.3(4) . . ?
C57 N2 C50 124.2(4) . . ?
C49 N2 C50 114.3(4) . . ?
C43 O2 H2 106(6) . . ?
C42 C41 C58 126.6(4) . . ?
C42 C41 H41 116.7 . . ?
C58 C41 H41 116.7 . . ?
C41 C42 C56 123.6(3) . . ?
C41 C42 C43 119.3(4) . . ?
C56 C42 C43 116.6(3) . . ?
O2 C43 C44 119.4(3) . . ?
O2 C43 C42 118.1(3) . . ?
C44 C43 C42 122.5(4) . . ?
C43 C44 C57 118.2(3) . . ?
C43 C44 C45 121.2(4) . . ?
C57 C44 C45 120.5(3) . . ?
C46 C45 C48 107.3(4) . . ?
C46 C45 C47 110.2(4) . . ?
C48 C45 C47 110.3(3) . . ?
C46 C45 C44 112.4(3) . . ?
C48 C45 C44 107.0(3) . . ?
C47 C45 C44 109.6(3) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C49 C48 C45 113.7(4) . . ?
C49 C48 H48A 108.8 . . ?
C45 C48 H48A 108.8 . . ?
C49 C48 H48B 108.8 . . ?
C45 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
N2 C49 C48 110.2(3) . . ?
N2 C49 H49A 109.6 . . ?
C48 C49 H49A 109.6 . . ?
N2 C49 H49B 109.6 . . ?
C48 C49 H49B 109.6 . . ?
H49A C49 H49B 108.1 . . ?
N2 C50 C51 113.1(4) . . ?
N2 C50 H50A 109.0 . . ?
C51 C50 H50A 109.0 . . ?
N2 C50 H50B 109.0 . . ?
C51 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
C50 C51 C52 110.7(4) . . ?
C50 C51 H51A 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C52 C51 H51B 109.5 . . ?
H51A C51 H51B 108.1 . . ?
C51 C52 C54 109.7(4) . . ?
C51 C52 C53 110.5(4) . . ?
C54 C52 C53 109.4(4) . . ?
C51 C52 C55 106.3(3) . . ?
C54 C52 C55 112.8(3) . . ?
C53 C52 C55 108.1(3) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 C57 118.8(4) . . ?
C56 C55 C52 122.9(3) . . ?
C57 C55 C52 118.3(3) . . ?
C55 C56 C42 122.7(3) . . ?
C55 C56 H56 118.6 . . ?
C42 C56 H56 118.6 . . ?
N2 C57 C44 121.6(3) . . ?
N2 C57 C55 118.7(4) . . ?
C44 C57 C55 119.8(3) . . ?
C59 C58 C41 122.3(4) . . ?
C59 C58 C72 107.3(3) . . ?
C41 C58 C72 129.7(4) . . ?
C60 C59 C58 110.9(4) . . ?
C60 C59 H59 124.5 . . ?
C58 C59 H59 124.5 . . ?
C59 C60 C62 108.0(4) . . ?
C59 C60 C61 124.6(5) . . ?
C62 C60 C61 127.3(4) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C60 122.1(4) . . ?
C63 C62 C72 129.4(4) . . ?
C60 C62 C72 108.4(3) . . ?
C64 C63 C62 131.4(5) . . ?
C64 C63 H63 114.3 . . ?
C62 C63 H63 114.3 . . ?
C63 C64 C68 123.9(4) . . ?
C63 C64 C65 115.3(7) . . ?
C68 C64 C65 120.8(7) . . ?
C63 C64 C65A 143(2) . . ?
C68 C64 C65A 92(2) . . ?
C67 C65 C66 113.9(7) . . ?
C67 C65 C64 110.1(7) . . ?
C66 C65 C64 109.5(6) . . ?
C67 C65 H65 107.7 . . ?
C66 C65 H65 107.7 . . ?
C64 C65 H65 107.7 . . ?
C67 C65A C66 122(2) . . ?
C67 C65A C64 117(2) . . ?
C66 C65A C64 108(3) . . ?
C67 C65A H65A 102.1 . . ?
C66 C65A H65A 102.1 . . ?
C64 C65A H65A 102.1 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 C68 C69 132.2(5) . . ?
C64 C68 H68 113.9 . . ?
C69 C68 H68 113.9 . . ?
C68 C69 C70 131.4(5) . . ?
C68 C69 H69 114.3 . . ?
C70 C69 H69 114.3 . . ?
C72 C70 C69 124.4(4) . . ?
C72 C70 C71 121.0(3) . . ?
C69 C70 C71 114.6(4) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C70 C72 C58 127.8(3) . . ?
C70 C72 C62 126.5(4) . . ?
C58 C72 C62 105.4(4) . . ?
F4A P1 F6A 99.4(15) . . ?
F5 P1 F3 96.5(6) . . ?
F4A P1 F1 88.6(7) . . ?
F5 P1 F1 89.8(3) . . ?
F6A P1 F1 82.7(8) . . ?
F3 P1 F1 95.2(4) . . ?
F5 P1 F4 94.1(6) . . ?
F3 P1 F4 168.6(5) . . ?
F1 P1 F4 89.1(2) . . ?
F4A P1 F2 91.2(7) . . ?
F5 P1 F2 88.8(3) . . ?
F6A P1 F2 99.5(8) . . ?
F3 P1 F2 86.8(4) . . ?
F1 P1 F2 177.7(2) . . ?
F4 P1 F2 89.2(3) . . ?
F5 P1 F6 177.3(4) . . ?
F3 P1 F6 84.4(4) . . ?
F1 P1 F6 92.7(3) . . ?
F4 P1 F6 84.8(4) . . ?
F2 P1 F6 88.7(3) . . ?
F4A P1 F5A 96.2(12) . . ?
F6A P1 F5A 163.6(13) . . ?
F1 P1 F5A 92.6(4) . . ?
F2 P1 F5A 85.2(4) . . ?
F4A P1 F3A 174.1(8) . . ?
F6A P1 F3A 83.6(12) . . ?
F1 P1 F3A 86.7(5) . . ?
F2 P1 F3A 93.3(5) . . ?
F5A P1 F3A 80.4(9) . . ?
F11A P2 F7 94.4(8) . . ?
F9 P2 F7 93.3(4) . . ?
F9 P2 F11 96.3(5) . . ?
F7 P2 F11 83.1(4) . . ?
F9 P2 F10 170.7(5) . . ?
F7 P2 F10 91.6(3) . . ?
F11 P2 F10 92.1(6) . . ?
F11A P2 F10A 84.1(12) . . ?
F7 P2 F10A 65.2(11) . . ?
F11A P2 F8 80.3(8) . . ?
F9 P2 F8 86.9(4) . . ?
F7 P2 F8 171.4(3) . . ?
F11 P2 F8 88.4(3) . . ?
F10 P2 F8 89.4(4) . . ?
F10A P2 F8 120.5(11) . . ?
F9 P2 F12 87.4(5) . . ?
F7 P2 F12 104.1(4) . . ?
F11 P2 F12 171.8(5) . . ?
F10 P2 F12 83.8(5) . . ?
F8 P2 F12 84.5(4) . . ?
F11A P2 F9A 102.3(16) . . ?
F7 P2 F9A 88.7(6) . . ?
F10A P2 F9A 153.7(13) . . ?
F8 P2 F9A 85.8(6) . . ?
F11A P2 F12A 159.0(11) . . ?
F7 P2 F12A 68.4(6) . . ?
F10A P2 F12A 77.8(14) . . ?
F8 P2 F12A 118.1(6) . . ?
F9A P2 F12A 89.8(13) . . ?
P2 F7 F10A 58.6(10) . . ?
P2 F10A F7 56.3(7) . . ?
H3A O3 H3B 102(3) . . ?
H4A O4 H4B 101.2 . . ?
H5A O5 H5B 106.1 . . ?
H4A O6 H6D 124.1 . . ?
H4A O6 H6E 102.5 . . ?
H6D O6 H6E 111.1 . . ?

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
C18 C1 C2 C16 -24.9(6) . . . . ?
C18 C1 C2 C3 162.9(4) . . . . ?
C1 C2 C3 O1 -5.4(5) . . . . ?
C16 C2 C3 O1 -178.2(3) . . . . ?
C1 C2 C3 C4 171.4(4) . . . . ?
C16 C2 C3 C4 -1.3(5) . . . . ?
O1 C3 C4 C17 171.8(3) . . . . ?
C2 C3 C4 C17 -5.1(5) . . . . ?
O1 C3 C4 C5 -6.7(5) . . . . ?
C2 C3 C4 C5 176.4(3) . . . . ?
C3 C4 C5 C7 -46.2(5) . . . . ?
C17 C4 C5 C7 135.4(4) . . . . ?
C3 C4 C5 C8 -163.4(4) . . . . ?
C17 C4 C5 C8 18.1(5) . . . . ?
C3 C4 C5 C6 76.7(5) . . . . ?
C17 C4 C5 C6 -101.7(4) . . . . ?
C7 C5 C8 C9 -170.5(4) . . . . ?
C6 C5 C8 C9 70.0(5) . . . . ?
C4 C5 C8 C9 -49.7(4) . . . . ?
C17 N1 C9 C8 -30.5(6) . . . . ?
C10 N1 C9 C8 156.1(5) . . . . ?
C5 C8 C9 N1 57.0(5) . . . . ?
C17 N1 C10 C11 -18.2(8) . . . . ?
C9 N1 C10 C11 155.0(5) . . . . ?
N1 C10 C11 C12 52.9(7) . . . . ?
C10 C11 C12 C14 175.0(5) . . . . ?
C10 C11 C12 C13 56.7(6) . . . . ?
C10 C11 C12 C15 -61.7(5) . . . . ?
C14 C12 C15 C16 -19.8(7) . . . . ?
C13 C12 C15 C16 99.0(5) . . . . ?
C11 C12 C15 C16 -140.6(4) . . . . ?
C14 C12 C15 C17 159.5(5) . . . . ?
C13 C12 C15 C17 -81.6(5) . . . . ?
C11 C12 C15 C17 38.7(5) . . . . ?
C17 C15 C16 C2 -3.8(6) . . . . ?
C12 C15 C16 C2 175.6(4) . . . . ?
C1 C2 C16 C15 -166.4(4) . . . . ?
C3 C2 C16 C15 6.0(6) . . . . ?
C9 N1 C17 C4 -1.1(6) . . . . ?
C10 N1 C17 C4 171.5(5) . . . . ?
C9 N1 C17 C15 180.0(4) . . . . ?
C10 N1 C17 C15 -7.4(7) . . . . ?
C3 C4 C17 N1 -171.5(4) . . . . ?
C5 C4 C17 N1 6.9(6) . . . . ?
C3 C4 C17 C15 7.4(5) . . . . ?
C5 C4 C17 C15 -174.2(3) . . . . ?
C16 C15 C17 N1 175.9(4) . . . . ?
C12 C15 C17 N1 -3.5(5) . . . . ?
C16 C15 C17 C4 -3.0(5) . . . . ?
C12 C15 C17 C4 177.6(3) . . . . ?
C2 C1 C18 C19 -30.0(7) . . . . ?
C2 C1 C18 C32 158.8(4) . . . . ?
C1 C18 C19 C20 -170.1(4) . . . . ?
C32 C18 C19 C20 2.6(5) . . . . ?
C18 C19 C20 C22 -2.3(5) . . . . ?
C18 C19 C20 C21 178.0(4) . . . . ?
C19 C20 C22 C23 178.9(4) . . . . ?
C21 C20 C22 C23 -1.4(7) . . . . ?
C19 C20 C22 C32 1.0(5) . . . . ?
C21 C20 C22 C32 -179.2(4) . . . . ?
C20 C22 C23 C24 178.9(4) . . . . ?
C32 C22 C23 C24 -3.7(8) . . . . ?
C22 C23 C24 C28 -6.2(8) . . . . ?
C22 C23 C24 C25 175.4(4) . . . . ?
C23 C24 C25 C27 115.2(5) . . . . ?
C28 C24 C25 C27 -63.4(6) . . . . ?
C23 C24 C25 C26 -117.7(5) . . . . ?
C28 C24 C25 C26 63.8(6) . . . . ?
C23 C24 C28 C29 6.5(8) . . . . ?
C25 C24 C28 C29 -175.1(5) . . . . ?
C24 C28 C29 C30 2.1(9) . . . . ?
C28 C29 C30 C32 -4.9(7) . . . . ?
C28 C29 C30 C31 175.5(4) . . . . ?
C29 C30 C32 C18 -175.0(4) . . . . ?
C31 C30 C32 C18 4.6(6) . . . . ?
C29 C30 C32 C22 -3.0(6) . . . . ?
C31 C30 C32 C22 176.6(4) . . . . ?
C19 C18 C32 C30 171.4(4) . . . . ?
C1 C18 C32 C30 -16.2(7) . . . . ?
C19 C18 C32 C22 -1.9(4) . . . . ?
C1 C18 C32 C22 170.6(4) . . . . ?
C23 C22 C32 C30 9.5(7) . . . . ?
C20 C22 C32 C30 -172.9(4) . . . . ?
C23 C22 C32 C18 -177.0(4) . . . . ?
C20 C22 C32 C18 0.6(4) . . . . ?
C58 C41 C42 C56 -22.1(7) . . . . ?
C58 C41 C42 C43 165.3(4) . . . . ?
C41 C42 C43 O2 -12.5(6) . . . . ?
C56 C42 C43 O2 174.4(4) . . . . ?
C41 C42 C43 C44 166.1(4) . . . . ?
C56 C42 C43 C44 -7.0(6) . . . . ?
O2 C43 C44 C57 175.9(4) . . . . ?
C42 C43 C44 C57 -2.7(6) . . . . ?
O2 C43 C44 C45 -2.7(6) . . . . ?
C42 C43 C44 C45 178.8(4) . . . . ?
C43 C44 C45 C46 -46.6(5) . . . . ?
C57 C44 C45 C46 134.8(4) . . . . ?
C43 C44 C45 C48 -164.2(4) . . . . ?
C57 C44 C45 C48 17.3(5) . . . . ?
C43 C44 C45 C47 76.2(5) . . . . ?
C57 C44 C45 C47 -102.4(4) . . . . ?
C46 C45 C48 C49 -171.5(4) . . . . ?
C47 C45 C48 C49 68.5(5) . . . . ?
C44 C45 C48 C49 -50.7(5) . . . . ?
C57 N2 C49 C48 -28.8(6) . . . . ?
C50 N2 C49 C48 155.6(4) . . . . ?
C45 C48 C49 N2 57.6(5) . . . . ?
C57 N2 C50 C51 -10.5(7) . . . . ?
C49 N2 C50 C51 164.9(4) . . . . ?
N2 C50 C51 C52 46.6(6) . . . . ?
C50 C51 C52 C54 177.0(4) . . . . ?
C50 C51 C52 C53 56.3(5) . . . . ?
C50 C51 C52 C55 -60.7(5) . . . . ?
C51 C52 C55 C56 -137.0(4) . . . . ?
C54 C52 C55 C56 -16.7(6) . . . . ?
C53 C52 C55 C56 104.4(4) . . . . ?
C51 C52 C55 C57 43.3(5) . . . . ?
C54 C52 C55 C57 163.6(4) . . . . ?
C53 C52 C55 C57 -75.3(4) . . . . ?
C57 C55 C56 C42 -1.6(6) . . . . ?
C52 C55 C56 C42 178.7(4) . . . . ?
C41 C42 C56 C55 -163.6(4) . . . . ?
C43 C42 C56 C55 9.2(6) . . . . ?
C49 N2 C57 C44 -4.3(6) . . . . ?
C50 N2 C57 C44 170.8(4) . . . . ?
C49 N2 C57 C55 176.3(4) . . . . ?
C50 N2 C57 C55 -8.6(6) . . . . ?
C43 C44 C57 N2 -168.9(4) . . . . ?
C45 C44 C57 N2 9.7(6) . . . . ?
C43 C44 C57 C55 10.5(6) . . . . ?
C45 C44 C57 C55 -170.9(3) . . . . ?
C56 C55 C57 N2 170.8(4) . . . . ?
C52 C55 C57 N2 -9.4(6) . . . . ?
C56 C55 C57 C44 -8.6(6) . . . . ?
C52 C55 C57 C44 171.1(4) . . . . ?
C42 C41 C58 C59 -34.8(6) . . . . ?
C42 C41 C58 C72 155.1(4) . . . . ?
C41 C58 C59 C60 -170.7(4) . . . . ?
C72 C58 C59 C60 1.3(5) . . . . ?
C58 C59 C60 C62 -1.0(5) . . . . ?
C58 C59 C60 C61 175.5(4) . . . . ?
C59 C60 C62 C63 177.6(4) . . . . ?
C61 C60 C62 C63 1.3(7) . . . . ?
C59 C60 C62 C72 0.2(5) . . . . ?
C61 C60 C62 C72 -176.1(4) . . . . ?
C60 C62 C63 C64 -178.8(4) . . . . ?
C72 C62 C63 C64 -2.0(7) . . . . ?
C62 C63 C64 C68 -6.5(8) . . . . ?
C62 C63 C64 C65 173.2(5) . . . . ?
C62 C63 C64 C65A -178(2) . . . . ?
C63 C64 C65 C67 112.9(9) . . . . ?
C68 C64 C65 C67 -67.4(9) . . . . ?
C63 C64 C65 C66 -121.0(8) . . . . ?
C68 C64 C65 C66 58.7(9) . . . . ?
C63 C64 C65A C67 59(5) . . . . ?
C68 C64 C65A C67 -114(4) . . . . ?
C63 C64 C65A C66 -84(3) . . . . ?
C68 C64 C65A C66 103(3) . . . . ?
C63 C64 C68 C69 4.3(8) . . . . ?
C65 C64 C68 C69 -175.4(5) . . . . ?
C65A C64 C68 C69 179.5(14) . . . . ?
C64 C68 C69 C70 3.9(9) . . . . ?
C68 C69 C70 C72 -3.7(7) . . . . ?
C68 C69 C70 C71 176.0(4) . . . . ?
C69 C70 C72 C58 -177.6(4) . . . . ?
C71 C70 C72 C58 2.7(6) . . . . ?
C69 C70 C72 C62 -5.1(6) . . . . ?
C71 C70 C72 C62 175.2(3) . . . . ?
C59 C58 C72 C70 172.6(4) . . . . ?
C41 C58 C72 C70 -16.1(7) . . . . ?
C59 C58 C72 C62 -1.1(4) . . . . ?
C41 C58 C72 C62 170.1(4) . . . . ?
C63 C62 C72 C70 9.6(6) . . . . ?
C60 C62 C72 C70 -173.3(4) . . . . ?
C63 C62 C72 C58 -176.6(4) . . . . ?
C60 C62 C72 C58 0.6(4) . . . . ?
F11A P2 F7 F10A 81.4(13) . . . . ?
F9A P2 F7 F10A -176.4(16) . . . . ?
F12A P2 F7 F10A -86.1(14) . . . . ?
F11A P2 F10A F7 -97.6(9) . . . . ?
F8 P2 F10A F7 -172.7(4) . . . . ?
F9A P2 F10A F7 8(4) . . . . ?
F12A P2 F10A F7 71.7(8) . . . . ?

_refine_diff_density_max         1.023
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.074

####################################################################### 
# 
# 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_s21sel2
_database_code_depnum_ccdc_archive 'CCDC 2129315'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok-Kohn'
;University of Bath
United Kingdom
;
_audit_update_record             
;
2021-12-16 deposited with the CCDC.	2022-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H23 S, F6 P, C2 H3 N'
_chemical_formula_sum            'C26 H26 F6 N P S'
_chemical_formula_weight         529.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   7.4072(2)
_cell_length_b                   15.5867(5)
_cell_length_c                   21.6148(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.378(2)
_cell_angle_gamma                90
_cell_volume                     2462.16(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3975
_cell_measurement_theta_min      5.0150
_cell_measurement_theta_max      72.8550

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.334
_shelx_estimated_absorpt_T_min   0.593
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_T_min  0.86900
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.676
_oxdiff_exptl_absorpt_empirical_full_max 1.477
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            16632
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.512
_diffrn_reflns_theta_max         72.905
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4834
_reflns_number_gt                3812
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 PF6 shows rotational disorder in the ratio 70:30
 bond lenghts have been equalised and all F atoms have
 been refined with ADP restraints.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0463P)²+1.2339P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4834
_refine_ls_number_parameters     376
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1048
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S S 0.12000(7) 0.38551(4) 0.43394(3) 0.02536(14) Uani 1 1 d . . . . .
C1 C 0.0168(3) 0.41186(16) 0.35829(10) 0.0252(5) Uani 1 1 d . . . . .
C2 C -0.0630(3) 0.35447(18) 0.31224(11) 0.0318(5) Uani 1 1 d . . . . .
H2 H -0.064550 0.294522 0.320050 0.038 Uiso 1 1 calc R U . . .
C3 C -0.1393(3) 0.38818(19) 0.25505(11) 0.0350(6) Uani 1 1 d . . . . .
H3 H -0.193995 0.350631 0.222720 0.042 Uiso 1 1 calc R U . . .
C4 C -0.1381(3) 0.47654(19) 0.24347(11) 0.0347(6) Uani 1 1 d . . . . .
H4 H -0.193478 0.497835 0.203692 0.042 Uiso 1 1 calc R U . . .
C5 C -0.0582(3) 0.53314(17) 0.28872(11) 0.0306(5) Uani 1 1 d . . . . .
H5 H -0.057538 0.592965 0.280363 0.037 Uiso 1 1 calc R U . . .
C6 C 0.0228(3) 0.50076(16) 0.34771(10) 0.0255(5) Uani 1 1 d . . . . .
C7 C 0.1146(3) 0.54536(15) 0.40131(11) 0.0259(5) Uani 1 1 d . . . . .
H7 H 0.132474 0.605731 0.402237 0.031 Uiso 1 1 calc R U . . .
C8 C 0.1745(3) 0.49304(14) 0.45141(11) 0.0239(4) Uani 1 1 d . . . . .
C9 C 0.2685(3) 0.52567(15) 0.50959(10) 0.0236(4) Uani 1 1 d . . . . .
H9 H 0.292956 0.585523 0.510135 0.028 Uiso 1 1 calc R U . . .
C10 C 0.3289(3) 0.48346(14) 0.56484(10) 0.0225(4) Uani 1 1 d . . . . .
C11 C 0.4322(3) 0.51870(15) 0.62355(10) 0.0218(4) Uani 1 1 d . . . . .
C12 C 0.4799(3) 0.60406(14) 0.63760(10) 0.0229(4) Uani 1 1 d . . . . .
C13 C 0.4154(3) 0.67622(15) 0.59265(11) 0.0297(5) Uani 1 1 d . . . . .
H13A H 0.473872 0.671083 0.555277 0.045 Uiso 1 1 calc R U . . .
H13B H 0.448355 0.731406 0.613141 0.045 Uiso 1 1 calc R U . . .
H13C H 0.282276 0.672930 0.580404 0.045 Uiso 1 1 calc R U . . .
C14 C 0.5905(3) 0.63155(15) 0.69383(11) 0.0266(5) Uani 1 1 d . . . . .
H14 H 0.616913 0.691224 0.694485 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6677(3) 0.58945(15) 0.74774(11) 0.0268(5) Uani 1 1 d . . . . .
H15 H 0.740455 0.624647 0.777928 0.032 Uiso 1 1 calc R U . . .
C16 C 0.6568(3) 0.50345(15) 0.76545(10) 0.0248(5) Uani 1 1 d . . . . .
C17 C 0.7466(3) 0.48076(17) 0.83167(10) 0.0284(5) Uani 1 1 d . . . . .
H17 H 0.867340 0.510859 0.839949 0.034 Uiso 1 1 calc R U . . .
C18 C 0.6291(4) 0.51601(19) 0.87815(12) 0.0372(6) Uani 1 1 d . . . . .
H18A H 0.615476 0.578218 0.872661 0.056 Uiso 1 1 calc R U . . .
H18B H 0.688596 0.503486 0.921088 0.056 Uiso 1 1 calc R U . . .
H18C H 0.508199 0.488859 0.870392 0.056 Uiso 1 1 calc R U . . .
C19 C 0.7826(4) 0.38552(18) 0.84257(12) 0.0383(6) Uani 1 1 d . . . . .
H19A H 0.665873 0.354805 0.838623 0.057 Uiso 1 1 calc R U . . .
H19B H 0.851909 0.376694 0.884733 0.057 Uiso 1 1 calc R U . . .
H19C H 0.853368 0.363640 0.811379 0.057 Uiso 1 1 calc R U . . .
C20 C 0.5652(3) 0.44118(15) 0.72673(11) 0.0260(5) Uani 1 1 d . . . . .
H20 H 0.566732 0.385627 0.744885 0.031 Uiso 1 1 calc R U . . .
C21 C 0.4710(3) 0.44657(15) 0.66535(10) 0.0236(5) Uani 1 1 d . . . . .
C22 C 0.3885(3) 0.37065(15) 0.63410(11) 0.0270(5) Uani 1 1 d . . . . .
C23 C 0.3916(4) 0.28337(16) 0.66259(12) 0.0384(6) Uani 1 1 d . . . . .
H23A H 0.321345 0.243664 0.632741 0.058 Uiso 1 1 calc R U . . .
H23B H 0.337063 0.285778 0.700933 0.058 Uiso 1 1 calc R U . . .
H23C H 0.518334 0.263331 0.672802 0.058 Uiso 1 1 calc R U . . .
C24 C 0.3067(3) 0.39307(15) 0.57569(11) 0.0264(5) Uani 1 1 d . . . . .
H24 H 0.243043 0.354408 0.545838 0.032 Uiso 1 1 calc R U . . .
N N 0.7486(4) 0.83283(17) 0.65374(14) 0.0530(7) Uani 1 1 d . . . . .
C31 C 0.7414(4) 0.85748(19) 0.60415(16) 0.0441(7) Uani 1 1 d . . . . .
C32 C 0.7294(5) 0.8913(3) 0.54082(17) 0.0673(10) Uani 1 1 d . . . . .
H32A H 0.823590 0.864444 0.520246 0.101 Uiso 1 1 calc R U . . .
H32B H 0.748485 0.953535 0.542688 0.101 Uiso 1 1 calc R U . . .
H32C H 0.608261 0.878708 0.516902 0.101 Uiso 1 1 calc R U . . .
P P 0.16508(9) 0.68522(5) 0.93591(3) 0.03450(17) Uani 1 1 d . . . . .
F1 F 0.2124(15) 0.6353(6) 0.9975(4) 0.094(3) Uani 0.720(15) 1 d . U P A 1
F3 F 0.0669(12) 0.7572(5) 0.9710(3) 0.0685(19) Uani 0.720(15) 1 d . U P A 1
F2 F 0.1224(10) 0.7414(3) 0.8714(2) 0.0728(16) Uani 0.720(15) 1 d . U P A 1
F4 F 0.3470(10) 0.7401(6) 0.9525(3) 0.111(3) Uani 0.720(15) 1 d . U P A 1
F5 F 0.2626(13) 0.6170(9) 0.8983(5) 0.085(3) Uani 0.720(15) 1 d . U P A 1
F6 F -0.0183(8) 0.6388(6) 0.9149(3) 0.100(2) Uani 0.720(15) 1 d . U P A 1
F1A F 0.283(3) 0.6488(18) 0.9980(11) 0.095(7) Uani 0.280(15) 1 d . U P A 2
F2A F 0.046(3) 0.7145(16) 0.8781(6) 0.107(7) Uani 0.280(15) 1 d . U P A 2
F3A F 0.036(3) 0.7335(14) 0.9758(11) 0.084(6) Uani 0.280(15) 1 d . U P A 2
F4A F 0.297(3) 0.7595(7) 0.9410(9) 0.089(5) Uani 0.280(15) 1 d . U P A 2
F5A F 0.293(2) 0.631(2) 0.9029(14) 0.056(4) Uani 0.280(15) 1 d . U P A 2
F6A F 0.035(2) 0.6036(11) 0.9427(12) 0.097(6) Uani 0.280(15) 1 d . U P A 2


_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
S C1 1.738(2) . ?
S C8 1.751(2) . ?
C1 C2 1.396(3) . ?
C1 C6 1.406(3) . ?
C2 C3 1.377(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.411(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.425(3) . ?
C7 C8 1.370(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.428(3) . ?
C9 C10 1.373(3) . ?
C9 H9 0.9500 . ?
C10 C24 1.442(3) . ?
C10 C11 1.477(3) . ?
C11 C12 1.397(3) . ?
C11 C21 1.442(3) . ?
C12 C14 1.417(3) . ?
C12 C13 1.512(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.378(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.400(3) . ?
C15 H15 0.9500 . ?
C16 C20 1.385(3) . ?
C16 C17 1.519(3) . ?
C17 C19 1.520(4) . ?
C17 C18 1.534(3) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.397(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.448(3) . ?
C22 C24 1.354(3) . ?
C22 C23 1.492(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24 0.9500 . ?
N C31 1.132(4) . ?
C31 C32 1.456(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
P F2A 1.477(11) . ?
P F4A 1.509(13) . ?
P F5A 1.53(2) . ?
P F1 1.532(7) . ?
P F6 1.541(5) . ?
P F3A 1.577(19) . ?
P F1A 1.58(2) . ?
P F5 1.583(11) . ?
P F4 1.587(6) . ?
P F3 1.595(7) . ?
P F6A 1.618(13) . ?
P F2 1.633(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S C8 91.56(11) . . ?
C2 C1 C6 122.4(2) . . ?
C2 C1 S 126.1(2) . . ?
C6 C1 S 111.42(17) . . ?
C3 C2 C1 117.4(3) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C2 C3 C4 121.5(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 121.2(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 118.9(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C1 C6 C5 118.6(2) . . ?
C1 C6 C7 111.8(2) . . ?
C5 C6 C7 129.5(2) . . ?
C8 C7 C6 113.7(2) . . ?
C8 C7 H7 123.1 . . ?
C6 C7 H7 123.1 . . ?
C7 C8 C9 122.2(2) . . ?
C7 C8 S 111.45(17) . . ?
C9 C8 S 126.38(18) . . ?
C10 C9 C8 129.7(2) . . ?
C10 C9 H9 115.2 . . ?
C8 C9 H9 115.2 . . ?
C9 C10 C24 125.4(2) . . ?
C9 C10 C11 128.2(2) . . ?
C24 C10 C11 106.30(19) . . ?
C12 C11 C21 126.1(2) . . ?
C12 C11 C10 128.2(2) . . ?
C21 C11 C10 105.72(19) . . ?
C11 C12 C14 124.4(2) . . ?
C11 C12 C13 121.8(2) . . ?
C14 C12 C13 113.8(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C12 133.1(2) . . ?
C15 C14 H14 113.4 . . ?
C12 C14 H14 113.4 . . ?
C14 C15 C16 130.8(2) . . ?
C14 C15 H15 114.6 . . ?
C16 C15 H15 114.6 . . ?
C20 C16 C15 123.4(2) . . ?
C20 C16 C17 120.2(2) . . ?
C15 C16 C17 116.4(2) . . ?
C16 C17 C19 114.4(2) . . ?
C16 C17 C18 109.01(19) . . ?
C19 C17 C18 110.6(2) . . ?
C16 C17 H17 107.5 . . ?
C19 C17 H17 107.5 . . ?
C18 C17 H17 107.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C16 C20 C21 130.6(2) . . ?
C16 C20 H20 114.7 . . ?
C21 C20 H20 114.7 . . ?
C20 C21 C11 131.3(2) . . ?
C20 C21 C22 120.1(2) . . ?
C11 C21 C22 108.60(19) . . ?
C24 C22 C21 108.3(2) . . ?
C24 C22 C23 126.5(2) . . ?
C21 C22 C23 125.2(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 C10 111.0(2) . . ?
C22 C24 H24 124.5 . . ?
C10 C24 H24 124.5 . . ?
N C31 C32 178.4(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
F2A P F4A 96.6(11) . . ?
F2A P F5A 96.0(13) . . ?
F4A P F5A 91.0(12) . . ?
F1 P F6 94.8(4) . . ?
F2A P F3A 89.1(10) . . ?
F4A P F3A 92.2(10) . . ?
F5A P F3A 173.6(15) . . ?
F2A P F1A 176.1(13) . . ?
F4A P F1A 87.3(11) . . ?
F5A P F1A 84.3(15) . . ?
F3A P F1A 90.3(13) . . ?
F1 P F5 92.7(6) . . ?
F6 P F5 89.3(4) . . ?
F1 P F4 90.6(4) . . ?
F6 P F4 174.3(3) . . ?
F5 P F4 92.1(5) . . ?
F1 P F3 90.1(4) . . ?
F6 P F3 91.2(4) . . ?
F5 P F3 177.1(5) . . ?
F4 P F3 87.1(4) . . ?
F2A P F6A 92.2(9) . . ?
F4A P F6A 170.6(10) . . ?
F5A P F6A 91.6(11) . . ?
F3A P F6A 84.4(9) . . ?
F1A P F6A 83.9(11) . . ?
F1 P F2 177.3(4) . . ?
F6 P F2 87.8(3) . . ?
F5 P F2 87.8(5) . . ?
F4 P F2 86.7(3) . . ?
F3 P F2 89.4(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 S C1 C2 179.0(2) . . . . ?
C8 S C1 C6 -0.77(17) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
S C1 C2 C3 179.51(18) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C2 C1 C6 C5 1.3(3) . . . . ?
S C1 C6 C5 -178.91(17) . . . . ?
C2 C1 C6 C7 -178.7(2) . . . . ?
S C1 C6 C7 1.0(2) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
C4 C5 C6 C7 179.3(2) . . . . ?
C1 C6 C7 C8 -0.8(3) . . . . ?
C5 C6 C7 C8 179.1(2) . . . . ?
C6 C7 C8 C9 -179.6(2) . . . . ?
C6 C7 C8 S 0.2(2) . . . . ?
C1 S C8 C7 0.32(17) . . . . ?
C1 S C8 C9 -179.9(2) . . . . ?
C7 C8 C9 C10 176.3(2) . . . . ?
S C8 C9 C10 -3.5(4) . . . . ?
C8 C9 C10 C24 -0.6(4) . . . . ?
C8 C9 C10 C11 177.5(2) . . . . ?
C9 C10 C11 C12 5.2(4) . . . . ?
C24 C10 C11 C12 -176.5(2) . . . . ?
C9 C10 C11 C21 -176.4(2) . . . . ?
C24 C10 C11 C21 1.9(2) . . . . ?
C21 C11 C12 C14 6.5(3) . . . . ?
C10 C11 C12 C14 -175.4(2) . . . . ?
C21 C11 C12 C13 -173.5(2) . . . . ?
C10 C11 C12 C13 4.6(3) . . . . ?
C11 C12 C14 C15 -4.3(4) . . . . ?
C13 C12 C14 C15 175.6(2) . . . . ?
C12 C14 C15 C16 -2.1(5) . . . . ?
C14 C15 C16 C20 3.4(4) . . . . ?
C14 C15 C16 C17 -174.6(2) . . . . ?
C20 C16 C17 C19 19.6(3) . . . . ?
C15 C16 C17 C19 -162.4(2) . . . . ?
C20 C16 C17 C18 -104.8(3) . . . . ?
C15 C16 C17 C18 73.2(3) . . . . ?
C15 C16 C20 C21 1.0(4) . . . . ?
C17 C16 C20 C21 178.9(2) . . . . ?
C16 C20 C21 C11 -2.9(4) . . . . ?
C16 C20 C21 C22 178.8(2) . . . . ?
C12 C11 C21 C20 -2.0(4) . . . . ?
C10 C11 C21 C20 179.5(2) . . . . ?
C12 C11 C21 C22 176.4(2) . . . . ?
C10 C11 C21 C22 -2.1(2) . . . . ?
C20 C21 C22 C24 -179.9(2) . . . . ?
C11 C21 C22 C24 1.4(3) . . . . ?
C20 C21 C22 C23 1.1(4) . . . . ?
C11 C21 C22 C23 -177.6(2) . . . . ?
C21 C22 C24 C10 -0.2(3) . . . . ?
C23 C22 C24 C10 178.8(2) . . . . ?
C9 C10 C24 C22 177.3(2) . . . . ?
C11 C10 C24 C22 -1.1(3) . . . . ?

_refine_diff_density_max         0.365
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.051

