# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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. 
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data_1a-Hexane
_database_code_depnum_ccdc_archive 'CCDC 2175101'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWB
_nottingham_internal_coll_number 18923
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   04/03/2021
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 12/05/2021
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 12/05/2021
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 13/05/2021
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 13/05/2021
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 13/05/2021
_refine_special_details          
;The crystals of the macrocycle diffracted weakly with resolution
 limit of 1.0 %A despite the use of synchrotron radiation. The
 data used in the refinement was truncated to a resolution of
 1.0 %A resulting in a low data to parameter ratio. Restraints
 were applied to the geometries and anisotropic displacement
 parameters of all atoms in the structure to aid the refinement.

 All C-S bonds C-F bonds in the structure were respectively
 restrained to have similar distances (SADI). The geometries
 of all phenyl and tetrafluorophenly rings were respectively
 restrained to have similar geometries reflecting their
 symmetry (SAME). All tetrafluorophenly moieties were restrained
 to have planar geometries (FLAT). Rigid bond and similarity
 restraints were applied to the anisotropic displacement
 parameters of all atoms in the structure (RIGU, SIMU).

 Electron density peaks indicative of hexane residues were
 observed in 1D channels running through the stacked
 macrocycles in the direction of the c-axis. The electron
 density peaks could not be developed into a sensible model
 for discreet ordered hexane residues and hence were accounted
 for with a solvent mask.

 A solvent mask was calculated and 600 electrons were found in
 a volume of 1140Å³ in 1 void per unit cell. This is
 consistent with the presence of 3[C6H14] per Asymmetric Unit 
 which account for 600 electrons per unit cell.,SQUEEZE
;
_vrf_PLAT089_1a-Hexane           
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       4.90 Note  
RESPONSE:
 The data used in the refinement was truncated to a resolution of
 1.0 %A resulting in a low data to parameter ratio. Restraints
 were applied to the geometries and anisotropic displacement
 parameters of all atoms in the structure to aid the refinement.
;
_vrf_PLAT340_1a-Hexane           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01748 Ang.  
RESPONSE:
 The crystals of the macrocycle diffracted weakly with resolution
 limit of 1.0 %A despite the use of synchrotron radiation. The
 data used in the refinement was truncated to a resolution of
 1.0 %A resulting in a low data to parameter ratio. Restraints
 were applied to the geometries and anisotropic displacement
 parameters of all atoms in the structure to aid the refinement.
;
_vrf_THETM01_1a-Hexane           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:
 The crystals of the macrocycle diffracted weakly with resolution
 limit of 1.0 %A despite the use of synchrotron radiation.
;
_audit_creation_date             2022-05-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H16 F16 S8, 3[C6H14]'
_chemical_formula_sum            'C66 H58 F16 S8'
_chemical_formula_weight         1411.60
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0019 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0124 0.0097 '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'
S S 0.1048 0.1164 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   34.3683(7)
_cell_length_b                   28.4432(5)
_cell_length_c                   5.44470(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5322.44(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.038426364171805
_cell_measurement_theta_min      0.8971284506740053
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            42986
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        20.147
_diffrn_reflns_theta_max         20.147
_diffrn_reflns_theta_min         0.901
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4168
_reflns_number_total             5593
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.3.3-g5efb02d60-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 3.3.3 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Flack x determined using 1475 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     1893
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1390P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.1926
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S8-C14 \\sim S8-C21 \\sim S7-C24 \\sim S7-C31 \\sim S6-C34 \\sim S6-C41 \\sim
S5-C44 \\sim S5-C51 \\sim S4-
 C54 \\sim S4-C61 \\sim S3-C64 \\sim S3-C71 \\sim S2-C74 \\sim S2-C81 \\sim
S1-C84 \\sim S1-C11
 with sigma of 0.02
 F30-C26 \\sim F29-C25 \\sim F27-C22 \\sim F28-C23 \\sim F47-C42 \\sim F48-C43
\\sim F50-C46 \\sim F49-C45
 \\sim F67-C62 \\sim F68-C63 \\sim F69-C65 \\sim F70-C66 \\sim F87-C82 \\sim
F88-C83 \\sim F89-C85 \\sim F90-C86
 with sigma of 0.02
3. Restrained planarity
 C21, C22, C23, C24, C25, C26, F27, F28, F29, F30
 with sigma of 0.1
 C81, C82, C83, C84, C85, C86, F87, F88, F89, F90
 with sigma of 0.1
 C61, C62, C63, C64, C65, C66, F67, F68, F69, F70
 with sigma of 0.1
 C41, C42, C43, C44, C45, C46, F47, F48, F49, F50
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C11, C16, C15, C14, C13, C12} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C15, C16, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C13, C12, C11, C16, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C11, C12, C13, C14, C15, C16}
{C21, C26, C25, C24, C23, C22} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C25, C26, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C23, C22, C21, C26, C25} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C21, C22, C23, C24, C25, C26}
{C11, C12, C13, C14, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04
{C11, C16, C15, C14, C13, C12} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C15, C16, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C13, C12, C11, C16, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C31, C32, C33, C34, C35, C36}
{C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{C21, C26, C25, C24, C23, C22} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C25, C26, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C23, C22, C21, C26, C25} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C41, C42, C43, C44, C45, C46}
{C11, C12, C13, C14, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04
{C11, C16, C15, C14, C13, C12} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C15, C16, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C13, C12, C11, C16, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C51, C52, C53, C54, C55, C56}
{C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{C21, C26, C25, C24, C23, C22} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C25, C26, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C23, C22, C21, C26, C25} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C61, C62, C63, C64, C65, C66}
{C11, C12, C13, C14, C15, C16} sigma for 1-2: 0.02, 1-3: 0.04
{C11, C16, C15, C14, C13, C12} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C15, C16, C11, C12, C13} sigma for 1-2: 0.02, 1-3: 0.04
{C14, C13, C12, C11, C16, C15} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C71, C72, C73, C74, C75, C76}
{C21, C22, C23, C24, C25, C26} sigma for 1-2: 0.02, 1-3: 0.04
{C21, C26, C25, C24, C23, C22} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C25, C26, C21, C22, C23} sigma for 1-2: 0.02, 1-3: 0.04
{C24, C23, C22, C21, C26, C25} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C81, C82, C83, C84, C85, C86}
7.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C32(H32), C33(H33), C35(H35),
 C36(H36), C52(H52), C53(H53), C55(H55), C56(H56), C72(H72), C73(H73), C75(H75),
  C76(H76)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.09264(13) 0.22280(13) 0.6058(9) 0.1476(16) Uani 1 1 d D U . . .
S2 S 0.24531(15) 0.22157(16) -0.0421(8) 0.1529(16) Uani 1 1 d D U . . .
S3 S 0.40192(14) 0.18091(12) 0.5451(9) 0.1556(18) Uani 1 1 d D U . . .
S4 S 0.51411(9) 0.35755(14) 0.3637(8) 0.1277(13) Uani 1 1 d D U . . .
S5 S 0.41955(8) 0.53858(12) 0.6712(7) 0.1063(10) Uani 1 1 d D U . . .
S6 S 0.27578(10) 0.54896(17) -0.0556(7) 0.1339(14) Uani 1 1 d D U . . .
S7 S 0.12358(9) 0.57776(11) 0.5749(8) 0.1152(11) Uani 1 1 d D U . . .
S8 S 0.00978(9) 0.40957(13) 0.2877(9) 0.1307(14) Uani 1 1 d D U . . .
C11 C 0.0715(4) 0.2746(4) 0.497(2) 0.114(4) Uani 1 1 d D U . . .
C12 C 0.0841(3) 0.2993(4) 0.287(2) 0.110(4) Uani 1 1 d D U . . .
H12 H 0.104585 0.287458 0.187090 0.132 Uiso 1 1 calc R U . . .
C13 C 0.0656(3) 0.3418(4) 0.229(2) 0.100(3) Uani 1 1 d D U . . .
H13 H 0.074033 0.359670 0.091461 0.120 Uiso 1 1 calc R U . . .
C14 C 0.0349(3) 0.3578(3) 0.371(2) 0.107(3) Uani 1 1 d D U . . .
C15 C 0.0223(4) 0.3357(5) 0.579(3) 0.133(4) Uani 1 1 d D U . . .
H15 H 0.001991 0.348502 0.676837 0.159 Uiso 1 1 calc R U . . .
C16 C 0.0405(4) 0.2932(5) 0.641(3) 0.135(4) Uani 1 1 d D U . . .
H16 H 0.032042 0.276475 0.782364 0.162 Uiso 1 1 calc R U . . .
C21 C 0.0447(3) 0.4522(4) 0.368(2) 0.109(3) Uani 1 1 d D U . . .
C22 C 0.0686(3) 0.4529(4) 0.570(2) 0.118(4) Uani 1 1 d D U . . .
C23 C 0.0924(3) 0.4902(4) 0.628(2) 0.105(3) Uani 1 1 d D U . . .
C24 C 0.0943(3) 0.5302(4) 0.482(2) 0.105(3) Uani 1 1 d D U . . .
C25 C 0.0694(3) 0.5302(4) 0.283(2) 0.111(3) Uani 1 1 d D U . . .
C26 C 0.0467(3) 0.4919(4) 0.222(2) 0.109(3) Uani 1 1 d D U . . .
F27 F 0.0682(3) 0.4165(2) 0.7295(16) 0.147(3) Uani 1 1 d D U . . .
F28 F 0.1144(2) 0.4857(2) 0.8352(16) 0.138(3) Uani 1 1 d D U . . .
F29 F 0.0704(2) 0.5677(3) 0.1316(17) 0.142(3) Uani 1 1 d D U . . .
F30 F 0.0251(2) 0.4949(3) 0.0154(18) 0.147(3) Uani 1 1 d D U . . .
C31 C 0.1662(3) 0.5647(4) 0.406(2) 0.099(3) Uani 1 1 d D U . . .
C32 C 0.1687(3) 0.5347(6) 0.203(3) 0.140(5) Uani 1 1 d D U . . .
H32 H 0.146608 0.516811 0.155137 0.167 Uiso 1 1 calc R U . . .
C33 C 0.2025(3) 0.5306(5) 0.071(3) 0.121(4) Uani 1 1 d D U . . .
H33 H 0.203235 0.510651 -0.069271 0.145 Uiso 1 1 calc R U . . .
C34 C 0.2350(3) 0.5547(5) 0.137(2) 0.117(4) Uani 1 1 d D U . . .
C35 C 0.2335(3) 0.5846(5) 0.338(3) 0.118(4) Uani 1 1 d D U . . .
H35 H 0.255717 0.602399 0.382856 0.142 Uiso 1 1 calc R U . . .
C36 C 0.1994(3) 0.5883(4) 0.473(3) 0.123(4) Uani 1 1 d D U . . .
H36 H 0.198999 0.607706 0.614710 0.148 Uiso 1 1 calc R U . . .
C41 C 0.3145(3) 0.5442(4) 0.152(2) 0.105(3) Uani 1 1 d D U . . .
C42 C 0.3154(3) 0.5128(4) 0.345(2) 0.096(3) Uani 1 1 d D U . . .
C43 C 0.3470(3) 0.5106(3) 0.5017(19) 0.093(3) Uani 1 1 d D U . . .
C44 C 0.3790(2) 0.5401(3) 0.4771(18) 0.082(3) Uani 1 1 d D U . . .
C45 C 0.3777(3) 0.5704(3) 0.281(2) 0.092(3) Uani 1 1 d D U . . .
C46 C 0.3467(3) 0.5735(4) 0.127(2) 0.097(3) Uani 1 1 d D U . . .
F47 F 0.28585(16) 0.4853(2) 0.3917(14) 0.118(2) Uani 1 1 d D U . . .
F48 F 0.34669(16) 0.4806(2) 0.6926(12) 0.1052(19) Uani 1 1 d D U . . .
F49 F 0.40830(17) 0.5998(2) 0.2357(15) 0.122(2) Uani 1 1 d D U . . .
F50 F 0.3474(2) 0.6041(2) -0.0653(14) 0.128(2) Uani 1 1 d D U . . .
C51 C 0.4431(3) 0.4864(4) 0.5691(19) 0.094(3) Uani 1 1 d D U . . .
C52 C 0.4335(3) 0.4617(3) 0.360(2) 0.087(3) Uani 1 1 d D U . . .
H52 H 0.412616 0.471587 0.257991 0.104 Uiso 1 1 calc R U . . .
C53 C 0.4555(3) 0.4214(4) 0.300(2) 0.090(3) Uani 1 1 d D U . . .
H53 H 0.449227 0.403516 0.157868 0.108 Uiso 1 1 calc R U . . .
C54 C 0.4861(3) 0.4082(4) 0.449(2) 0.101(3) Uani 1 1 d D U . . .
C55 C 0.4949(3) 0.4325(4) 0.658(2) 0.103(3) Uani 1 1 d D U . . .
H55 H 0.515959 0.422707 0.758959 0.123 Uiso 1 1 calc R U . . .
C56 C 0.4730(3) 0.4716(4) 0.723(2) 0.098(3) Uani 1 1 d D U . . .
H56 H 0.478363 0.488113 0.871458 0.118 Uiso 1 1 calc R U . . .
C61 C 0.4812(3) 0.3114(4) 0.407(2) 0.115(4) Uani 1 1 d D U . . .
C62 C 0.4546(3) 0.3067(4) 0.601(2) 0.112(3) Uani 1 1 d D U . . .
C63 C 0.4311(3) 0.2688(4) 0.634(2) 0.114(3) Uani 1 1 d D U . . .
C64 C 0.4305(3) 0.2315(4) 0.476(2) 0.122(4) Uani 1 1 d D U . . .
C65 C 0.4574(4) 0.2358(4) 0.284(2) 0.127(4) Uani 1 1 d D U . . .
C66 C 0.4809(4) 0.2739(5) 0.254(2) 0.125(4) Uani 1 1 d D U . . .
F67 F 0.45328(19) 0.3410(2) 0.7767(13) 0.1128(19) Uani 1 1 d D U . . .
F68 F 0.4071(2) 0.2700(2) 0.8313(15) 0.129(2) Uani 1 1 d D U . . .
F69 F 0.4596(3) 0.1987(3) 0.1265(16) 0.173(4) Uani 1 1 d D U . . .
F70 F 0.5057(2) 0.2742(3) 0.0556(17) 0.166(4) Uani 1 1 d D U . . .
C71 C 0.3579(4) 0.1965(4) 0.393(3) 0.132(4) Uani 1 1 d D U . . .
C72 C 0.3553(4) 0.2229(6) 0.186(3) 0.162(6) Uani 1 1 d D U . . .
H72 H 0.378560 0.234958 0.116432 0.195 Uiso 1 1 calc R U . . .
C73 C 0.3202(4) 0.2330(6) 0.072(3) 0.154(5) Uani 1 1 d D U . . .
H73 H 0.319651 0.254551 -0.061416 0.184 Uiso 1 1 calc R U . . .
C74 C 0.2860(4) 0.2121(4) 0.151(3) 0.132(4) Uani 1 1 d D U . . .
C75 C 0.2870(5) 0.1847(5) 0.363(3) 0.151(5) Uani 1 1 d D U . . .
H75 H 0.263880 0.171000 0.426146 0.182 Uiso 1 1 calc R U . . .
C76 C 0.3228(5) 0.1777(5) 0.480(3) 0.144(5) Uani 1 1 d D U . . .
H76 H 0.323290 0.159301 0.625356 0.172 Uiso 1 1 calc R U . . .
C81 C 0.2046(4) 0.2200(4) 0.157(2) 0.130(4) Uani 1 1 d D U . . .
C82 C 0.2015(4) 0.2495(4) 0.358(2) 0.123(4) Uani 1 1 d D U . . .
C83 C 0.1680(4) 0.2501(4) 0.491(3) 0.135(4) Uani 1 1 d D U . . .
C84 C 0.1357(4) 0.2212(4) 0.433(3) 0.128(4) Uani 1 1 d D U . . .
C85 C 0.1394(4) 0.1958(4) 0.229(3) 0.134(4) Uani 1 1 d D U . . .
C86 C 0.1726(5) 0.1934(4) 0.093(2) 0.132(4) Uani 1 1 d D U . . .
F87 F 0.2321(2) 0.2772(2) 0.4198(16) 0.141(3) Uani 1 1 d D U . . .
F88 F 0.1666(2) 0.2780(2) 0.6859(16) 0.134(2) Uani 1 1 d D U . . .
F89 F 0.1103(2) 0.1665(2) 0.1510(17) 0.148(3) Uani 1 1 d D U . . .
F90 F 0.1759(3) 0.1641(3) -0.1019(17) 0.172(4) Uani 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C11 1.745(10) . ?
S1 C84 1.753(13) . ?
S2 C74 1.769(12) . ?
S2 C81 1.769(12) . ?
S3 C64 1.781(12) . ?
S3 C71 1.781(12) . ?
S4 C54 1.793(10) . ?
S4 C61 1.747(12) . ?
S5 C44 1.748(9) . ?
S5 C51 1.779(10) . ?
S6 C34 1.756(11) . ?
S6 C41 1.752(10) . ?
S7 C24 1.761(10) . ?
S7 C31 1.769(10) . ?
S8 C14 1.766(11) . ?
S8 C21 1.762(10) . ?
C11 C12 1.411(13) . ?
C11 C16 1.425(14) . ?
C12 H12 0.9500 . ?
C12 C13 1.403(13) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(13) . ?
C14 C15 1.365(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.404(15) . ?
C16 H16 0.9500 . ?
C21 C22 1.375(13) . ?
C21 C26 1.382(13) . ?
C22 C23 1.375(13) . ?
C22 F27 1.351(12) . ?
C23 C24 1.392(13) . ?
C23 F28 1.362(12) . ?
C24 C25 1.380(13) . ?
C25 C26 1.378(13) . ?
C25 F29 1.348(12) . ?
C26 F30 1.351(12) . ?
C31 C32 1.401(14) . ?
C31 C36 1.373(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.371(14) . ?
C33 H33 0.9500 . ?
C33 C34 1.358(13) . ?
C34 C35 1.387(14) . ?
C35 H35 0.9500 . ?
C35 C36 1.387(14) . ?
C36 H36 0.9500 . ?
C41 C42 1.381(12) . ?
C41 C46 1.390(12) . ?
C42 C43 1.382(12) . ?
C42 F47 1.305(10) . ?
C43 C44 1.393(11) . ?
C43 F48 1.344(10) . ?
C44 C45 1.372(12) . ?
C45 C46 1.360(12) . ?
C45 F49 1.366(10) . ?
C46 F50 1.360(10) . ?
C51 C52 1.379(12) . ?
C51 C56 1.393(12) . ?
C52 H52 0.9500 . ?
C52 C53 1.409(12) . ?
C53 H53 0.9500 . ?
C53 C54 1.380(12) . ?
C54 C55 1.369(13) . ?
C55 H55 0.9500 . ?
C55 C56 1.389(14) . ?
C56 H56 0.9500 . ?
C61 C62 1.405(13) . ?
C61 C66 1.353(14) . ?
C62 C63 1.360(14) . ?
C62 F67 1.367(11) . ?
C63 C64 1.367(13) . ?
C63 F68 1.353(12) . ?
C64 C65 1.401(14) . ?
C65 C66 1.361(15) . ?
C65 F69 1.364(12) . ?
C66 F70 1.377(13) . ?
C71 C72 1.358(14) . ?
C71 C76 1.400(15) . ?
C72 H72 0.9500 . ?
C72 C73 1.386(15) . ?
C73 H73 0.9500 . ?
C73 C74 1.386(15) . ?
C74 C75 1.393(14) . ?
C75 H75 0.9500 . ?
C75 C76 1.400(15) . ?
C76 H76 0.9500 . ?
C81 C82 1.387(14) . ?
C81 C86 1.380(14) . ?
C82 C83 1.362(15) . ?
C82 F87 1.356(12) . ?
C83 C84 1.418(14) . ?
C83 F88 1.324(13) . ?
C84 C85 1.332(14) . ?
C85 C86 1.361(15) . ?
C85 F89 1.370(12) . ?
C86 F90 1.352(13) . ?

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
C84 S1 C11 101.0(6) . . ?
C81 S2 C74 104.9(7) . . ?
C64 S3 C71 99.8(6) . . ?
C61 S4 C54 102.8(5) . . ?
C44 S5 C51 101.2(5) . . ?
C41 S6 C34 103.3(6) . . ?
C24 S7 C31 99.3(5) . . ?
C21 S8 C14 100.2(5) . . ?
C12 C11 S1 124.6(10) . . ?
C12 C11 C16 119.4(10) . . ?
C16 C11 S1 115.9(9) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 C11 118.2(11) . . ?
C13 C12 H12 120.9 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.2(10) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 S8 120.1(9) . . ?
C15 C14 S8 116.2(10) . . ?
C15 C14 C13 123.6(11) . . ?
C14 C15 H15 121.5 . . ?
C14 C15 C16 117.1(12) . . ?
C16 C15 H15 121.5 . . ?
C11 C16 H16 119.3 . . ?
C15 C16 C11 121.4(12) . . ?
C15 C16 H16 119.3 . . ?
C22 C21 S8 128.0(10) . . ?
C22 C21 C26 114.7(9) . . ?
C26 C21 S8 117.0(9) . . ?
C23 C22 C21 123.4(10) . . ?
F27 C22 C21 119.8(10) . . ?
F27 C22 C23 116.8(10) . . ?
C22 C23 C24 121.8(10) . . ?
F28 C23 C22 116.5(10) . . ?
F28 C23 C24 121.7(10) . . ?
C23 C24 S7 119.3(9) . . ?
C25 C24 S7 125.6(9) . . ?
C25 C24 C23 114.8(9) . . ?
C26 C25 C24 122.7(10) . . ?
F29 C25 C24 117.5(10) . . ?
F29 C25 C26 119.5(11) . . ?
C25 C26 C21 122.4(10) . . ?
F30 C26 C21 120.1(11) . . ?
F30 C26 C25 117.5(11) . . ?
C32 C31 S7 126.2(8) . . ?
C36 C31 S7 116.6(9) . . ?
C36 C31 C32 117.1(10) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 C31 121.2(11) . . ?
C33 C32 H32 119.4 . . ?
C32 C33 H33 119.5 . . ?
C34 C33 C32 121.0(11) . . ?
C34 C33 H33 119.5 . . ?
C33 C34 S6 116.8(10) . . ?
C33 C34 C35 119.1(10) . . ?
C35 C34 S6 123.9(9) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 C34 119.8(11) . . ?
C36 C35 H35 120.1 . . ?
C31 C36 C35 121.6(12) . . ?
C31 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C42 C41 S6 123.8(8) . . ?
C42 C41 C46 116.5(9) . . ?
C46 C41 S6 119.6(8) . . ?
C43 C42 C41 121.0(8) . . ?
F47 C42 C41 121.3(9) . . ?
F47 C42 C43 117.7(9) . . ?
C42 C43 C44 122.4(9) . . ?
F48 C43 C42 119.9(8) . . ?
F48 C43 C44 117.6(9) . . ?
C43 C44 S5 123.8(8) . . ?
C45 C44 S5 120.9(7) . . ?
C45 C44 C43 115.3(8) . . ?
C46 C45 C44 123.2(8) . . ?
C46 C45 F49 116.9(9) . . ?
F49 C45 C44 119.9(9) . . ?
C45 C46 C41 121.6(9) . . ?
C45 C46 F50 120.2(9) . . ?
F50 C46 C41 118.2(9) . . ?
C52 C51 S5 125.1(8) . . ?
C52 C51 C56 121.4(10) . . ?
C56 C51 S5 113.5(8) . . ?
C51 C52 H52 120.7 . . ?
C51 C52 C53 118.6(9) . . ?
C53 C52 H52 120.7 . . ?
C52 C53 H53 120.2 . . ?
C54 C53 C52 119.6(10) . . ?
C54 C53 H53 120.2 . . ?
C53 C54 S4 118.5(9) . . ?
C55 C54 S4 120.1(8) . . ?
C55 C54 C53 121.4(10) . . ?
C54 C55 H55 120.1 . . ?
C54 C55 C56 119.9(10) . . ?
C56 C55 H55 120.1 . . ?
C51 C56 H56 120.4 . . ?
C55 C56 C51 119.1(10) . . ?
C55 C56 H56 120.4 . . ?
C62 C61 S4 126.5(9) . . ?
C66 C61 S4 121.0(10) . . ?
C66 C61 C62 112.4(11) . . ?
C63 C62 C61 124.3(10) . . ?
C63 C62 F67 116.9(10) . . ?
F67 C62 C61 118.7(10) . . ?
C62 C63 C64 122.7(11) . . ?
F68 C63 C62 116.7(10) . . ?
F68 C63 C64 120.6(12) . . ?
C63 C64 S3 120.2(10) . . ?
C63 C64 C65 113.0(11) . . ?
C65 C64 S3 126.3(10) . . ?
C66 C65 C64 123.5(11) . . ?
F69 C65 C64 116.0(13) . . ?
F69 C65 C66 120.5(13) . . ?
C61 C66 C65 124.0(11) . . ?
C61 C66 F70 118.1(13) . . ?
C65 C66 F70 117.9(12) . . ?
C72 C71 S3 125.3(12) . . ?
C72 C71 C76 115.7(12) . . ?
C76 C71 S3 118.8(10) . . ?
C71 C72 H72 118.5 . . ?
C71 C72 C73 123.0(14) . . ?
C73 C72 H72 118.5 . . ?
C72 C73 H73 119.7 . . ?
C74 C73 C72 120.6(13) . . ?
C74 C73 H73 119.7 . . ?
C73 C74 S2 115.0(10) . . ?
C73 C74 C75 118.4(12) . . ?
C75 C74 S2 126.6(12) . . ?
C74 C75 H75 120.7 . . ?
C74 C75 C76 118.6(14) . . ?
C76 C75 H75 120.7 . . ?
C71 C76 H76 118.4 . . ?
C75 C76 C71 123.3(13) . . ?
C75 C76 H76 118.4 . . ?
C82 C81 S2 122.0(11) . . ?
C86 C81 S2 119.4(11) . . ?
C86 C81 C82 118.1(11) . . ?
C83 C82 C81 119.6(11) . . ?
F87 C82 C81 119.2(13) . . ?
F87 C82 C83 121.2(12) . . ?
C82 C83 C84 122.5(12) . . ?
F88 C83 C82 117.6(12) . . ?
F88 C83 C84 119.9(13) . . ?
C83 C84 S1 121.7(11) . . ?
C85 C84 S1 122.9(12) . . ?
C85 C84 C83 115.2(12) . . ?
C84 C85 C86 124.2(12) . . ?
C84 C85 F89 121.1(14) . . ?
C86 C85 F89 114.4(13) . . ?
C85 C86 C81 120.2(11) . . ?
F90 C86 C81 117.9(14) . . ?
F90 C86 C85 121.8(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C13 H13 F27 0.95 2.56 3.452(14) 157.0 1_554 yes
C15 H15 F69 0.95 3.15 3.806(16) 127.8 3_456 yes
C16 H16 F69 0.95 3.20 3.844(17) 127.1 3_456 yes
C16 H16 F70 0.95 2.26 3.194(16) 167.1 3_456 yes
C32 H32 F28 0.95 2.25 3.071(15) 144.7 1_554 yes
C32 H32 F29 0.95 2.99 3.528(15) 117.0 . yes
C33 H33 F28 0.95 3.18 3.529(14) 103.9 1_554 yes
C35 H35 S6 0.95 3.48 3.748(15) 98.8 1_556 yes
C35 H35 F90 0.95 2.94 3.864(16) 166.3 4 yes
C52 H52 F48 0.95 3.29 3.533(12) 97.2 . yes
C53 H53 F67 0.95 2.74 3.654(13) 162.5 1_554 yes
C55 H55 F49 0.95 2.68 3.477(13) 141.4 2_665 yes
C72 H72 F68 0.95 2.09 2.949(17) 149.9 1_554 yes
C72 H72 F69 0.95 2.97 3.664(18) 131.0 . yes
C73 H73 F68 0.95 3.09 3.426(18) 102.5 1_554 yes
C75 H75 S2 0.95 3.30 3.696(17) 107.7 1_556 yes

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
S1 C11 C12 C13 -176.7(9) . . . . ?
S1 C11 C16 C15 177.3(10) . . . . ?
S1 C84 C85 C86 -179.0(11) . . . . ?
S1 C84 C85 F89 -4.9(17) . . . . ?
S2 C74 C75 C76 174.2(12) . . . . ?
S2 C81 C82 C83 173.5(10) . . . . ?
S2 C81 C82 F87 -6.6(12) . . . . ?
S2 C81 C86 C85 -172.5(10) . . . . ?
S2 C81 C86 F90 9.6(17) . . . . ?
S3 C64 C65 C66 -173.8(11) . . . . ?
S3 C64 C65 F69 4.9(17) . . . . ?
S3 C71 C72 C73 178.4(14) . . . . ?
S3 C71 C76 C75 -174.8(11) . . . . ?
S4 C54 C55 C56 -179.8(9) . . . . ?
S4 C61 C62 C63 -176.1(9) . . . . ?
S4 C61 C62 F67 0.3(12) . . . . ?
S4 C61 C66 C65 176.8(11) . . . . ?
S4 C61 C66 F70 -3.6(15) . . . . ?
S5 C44 C45 C46 -179.0(9) . . . . ?
S5 C44 C45 F49 -0.1(14) . . . . ?
S5 C51 C52 C53 178.6(8) . . . . ?
S5 C51 C56 C55 -177.0(8) . . . . ?
S6 C34 C35 C36 177.1(11) . . . . ?
S6 C41 C42 C43 179.5(9) . . . . ?
S6 C41 C42 F47 -2.7(12) . . . . ?
S6 C41 C46 C45 -178.8(9) . . . . ?
S6 C41 C46 F50 -2.0(14) . . . . ?
S7 C24 C25 C26 -178.8(10) . . . . ?
S7 C24 C25 F29 7.4(18) . . . . ?
S7 C31 C32 C33 173.5(12) . . . . ?
S7 C31 C36 C35 -173.2(11) . . . . ?
S8 C14 C15 C16 176.7(10) . . . . ?
S8 C21 C22 C23 -173.5(10) . . . . ?
S8 C21 C22 F27 3.5(13) . . . . ?
S8 C21 C26 C25 171.9(10) . . . . ?
S8 C21 C26 F30 -6.2(15) . . . . ?
C11 S1 C84 C83 77.0(11) . . . . ?
C11 S1 C84 C85 -97.7(11) . . . . ?
C11 C12 C13 C14 -2.1(17) . . . . ?
C12 C11 C16 C15 -0.2(19) . . . . ?
C12 C13 C14 S8 -176.3(9) . . . . ?
C12 C13 C14 C15 3.6(18) . . . . ?
C13 C14 C15 C16 -3.2(18) . . . . ?
C14 S8 C21 C22 -39.9(10) . . . . ?
C14 S8 C21 C26 145.8(10) . . . . ?
C14 C15 C16 C11 1.4(19) . . . . ?
C16 C11 C12 C13 0.5(17) . . . . ?
C21 S8 C14 C13 -73.5(10) . . . . ?
C21 S8 C14 C15 106.6(10) . . . . ?
C21 C22 C23 C24 -0.8(13) . . . . ?
C21 C22 C23 F28 179.9(9) . . . . ?
C22 C21 C26 C25 -3.2(16) . . . . ?
C22 C21 C26 F30 178.7(9) . . . . ?
C22 C23 C24 S7 177.0(8) . . . . ?
C22 C23 C24 C25 2.7(16) . . . . ?
C23 C24 C25 C26 -5.0(19) . . . . ?
C23 C24 C25 F29 -178.8(11) . . . . ?
C24 S7 C31 C32 18.3(13) . . . . ?
C24 S7 C31 C36 -165.7(10) . . . . ?
C24 C25 C26 C21 6(2) . . . . ?
C24 C25 C26 F30 -176.2(11) . . . . ?
C26 C21 C22 C23 0.9(12) . . . . ?
C26 C21 C22 F27 178.0(11) . . . . ?
F27 C22 C23 C24 -178.0(11) . . . . ?
F27 C22 C23 F28 2.7(13) . . . . ?
F28 C23 C24 S7 -3.8(15) . . . . ?
F28 C23 C24 C25 -178.0(10) . . . . ?
F29 C25 C26 C21 179.2(11) . . . . ?
F29 C25 C26 F30 -2.6(18) . . . . ?
C31 S7 C24 C23 95.7(10) . . . . ?
C31 S7 C24 C25 -90.8(12) . . . . ?
C31 C32 C33 C34 2(2) . . . . ?
C32 C31 C36 C35 3(2) . . . . ?
C32 C33 C34 S6 -176.9(12) . . . . ?
C32 C33 C34 C35 -1(2) . . . . ?
C33 C34 C35 C36 2(2) . . . . ?
C34 S6 C41 C42 51.3(10) . . . . ?
C34 S6 C41 C46 -128.3(10) . . . . ?
C34 C35 C36 C31 -3(2) . . . . ?
C36 C31 C32 C33 -2(2) . . . . ?
C41 S6 C34 C33 -138.8(11) . . . . ?
C41 S6 C34 C35 46.0(14) . . . . ?
C41 C42 C43 C44 1.5(12) . . . . ?
C41 C42 C43 F48 178.2(9) . . . . ?
C42 C41 C46 C45 1.6(15) . . . . ?
C42 C41 C46 F50 178.4(8) . . . . ?
C42 C43 C44 S5 179.8(7) . . . . ?
C42 C43 C44 C45 -2.5(14) . . . . ?
C43 C44 C45 C46 3.2(15) . . . . ?
C43 C44 C45 F49 -177.9(9) . . . . ?
C44 S5 C51 C52 10.9(10) . . . . ?
C44 S5 C51 C56 -168.9(8) . . . . ?
C44 C45 C46 C41 -2.9(17) . . . . ?
C44 C45 C46 F50 -179.7(9) . . . . ?
C46 C41 C42 C43 -0.9(11) . . . . ?
C46 C41 C42 F47 176.8(11) . . . . ?
F47 C42 C43 C44 -176.4(10) . . . . ?
F47 C42 C43 F48 0.4(13) . . . . ?
F48 C43 C44 S5 3.0(14) . . . . ?
F48 C43 C44 C45 -179.3(9) . . . . ?
F49 C45 C46 C41 178.1(10) . . . . ?
F49 C45 C46 F50 1.4(15) . . . . ?
C51 S5 C44 C43 74.1(10) . . . . ?
C51 S5 C44 C45 -103.4(9) . . . . ?
C51 C52 C53 C54 -1.0(15) . . . . ?
C52 C51 C56 C55 3.2(16) . . . . ?
C52 C53 C54 S4 -178.6(8) . . . . ?
C52 C53 C54 C55 2.1(16) . . . . ?
C53 C54 C55 C56 -0.5(16) . . . . ?
C54 S4 C61 C62 -40.3(9) . . . . ?
C54 S4 C61 C66 143.7(10) . . . . ?
C54 C55 C56 C51 -2.1(16) . . . . ?
C56 C51 C52 C53 -1.7(15) . . . . ?
C61 S4 C54 C53 -68.5(10) . . . . ?
C61 S4 C54 C55 110.8(9) . . . . ?
C61 C62 C63 C64 -1.5(14) . . . . ?
C61 C62 C63 F68 180.0(9) . . . . ?
C62 C61 C66 C65 0.3(17) . . . . ?
C62 C61 C66 F70 179.9(9) . . . . ?
C62 C63 C64 S3 174.7(8) . . . . ?
C62 C63 C64 C65 2.1(16) . . . . ?
C63 C64 C65 C66 -1.7(18) . . . . ?
C63 C64 C65 F69 176.9(10) . . . . ?
C64 S3 C71 C72 31.6(15) . . . . ?
C64 S3 C71 C76 -153.2(12) . . . . ?
C64 C65 C66 C61 1(2) . . . . ?
C64 C65 C66 F70 -179.0(10) . . . . ?
C66 C61 C62 C63 0.2(12) . . . . ?
C66 C61 C62 F67 176.6(10) . . . . ?
F67 C62 C63 C64 -178.0(11) . . . . ?
F67 C62 C63 F68 3.5(12) . . . . ?
F68 C63 C64 S3 -6.8(15) . . . . ?
F68 C63 C64 C65 -179.4(10) . . . . ?
F69 C65 C66 C61 -178.0(10) . . . . ?
F69 C65 C66 F70 2.4(18) . . . . ?
C71 S3 C64 C63 91.8(11) . . . . ?
C71 S3 C64 C65 -96.7(12) . . . . ?
C71 C72 C73 C74 -7(3) . . . . ?
C72 C71 C76 C75 1(2) . . . . ?
C72 C73 C74 S2 -170.7(15) . . . . ?
C72 C73 C74 C75 7(3) . . . . ?
C73 C74 C75 C76 -3(2) . . . . ?
C74 S2 C81 C82 56.4(10) . . . . ?
C74 S2 C81 C86 -132.6(11) . . . . ?
C74 C75 C76 C71 -1(2) . . . . ?
C76 C71 C72 C73 3(3) . . . . ?
C81 S2 C74 C73 -150.5(13) . . . . ?
C81 S2 C74 C75 32.3(15) . . . . ?
C81 C82 C83 C84 0.5(14) . . . . ?
C81 C82 C83 F88 178.3(10) . . . . ?
C82 C81 C86 C85 -1.2(19) . . . . ?
C82 C81 C86 F90 -179.2(9) . . . . ?
C82 C83 C84 S1 -179.7(9) . . . . ?
C82 C83 C84 C85 -4.6(17) . . . . ?
C83 C84 C85 C86 6(2) . . . . ?
C83 C84 C85 F89 -179.9(11) . . . . ?
C84 S1 C11 C12 12.4(12) . . . . ?
C84 S1 C11 C16 -164.9(10) . . . . ?
C84 C85 C86 C81 -3(2) . . . . ?
C84 C85 C86 F90 174.5(11) . . . . ?
C86 C81 C82 C83 2.4(13) . . . . ?
C86 C81 C82 F87 -177.7(12) . . . . ?
F87 C82 C83 C84 -179.4(11) . . . . ?
F87 C82 C83 F88 -1.6(15) . . . . ?
F88 C83 C84 S1 2.6(16) . . . . ?
F88 C83 C84 C85 177.6(11) . . . . ?
F89 C85 C86 C81 -177.8(11) . . . . ?
F89 C85 C86 F90 0.1(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.237 0.880 -0.070 285.2 150.6 '3 C6H14'
2 0.263 0.380 -0.240 285.2 150.6 '3 C6H14'
3 0.737 0.620 -0.647 285.2 150.5 '3 C6H14'
4 0.763 0.120 -0.549 285.2 150.6 '3 C6H14'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane, hexane'
####################################################################### 
# 
# 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_1a-THF
_database_code_depnum_ccdc_archive 'CCDC 2175103'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWJ
_nottingham_internal_coll_number 19141
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '1.00, 10.00, 4.00'
_nottingham_internal_coll_frame_width 0.50
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   13/05/2022
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 24/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 25/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 25/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 25/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 25/05/2022
_refine_special_details          
;The crystal was integrated as a two component twin and
 the final structure refined against an HKLF5 reflection
 file resulting in a batch scale factor of 0.408(1).

 A large residual electron density peak of 2.69 eA-3
 is observed 0.23 %A from sulphur atom S2B. This peak
 is likely caused by a combination of deficiencies in the
 handling of the twinning and a minor unmodelled disorder
 component in the ring conformation.

 A solvent mask was calculated and 196 electrons were 
 found in a volume of 742Å³ in 1 void per unit cell. 
 This is consistent with the presence of 2[C4H8O] per
 Asymmetric Unit which account for 160 electrons per
 unit cell.,Twin,SQUEEZE
;
_vrf_PLAT084_1a-THF              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.37 Report
RESPONSE:
 The crystal was integrated as a two component twin and
 the final structure refined against an HKLF5 reflection
 file resulting in a batch scale factor of 0.408(1).
 Pores running through the crystal structure leave the
 opportunity for solvent guests to disorder which in
 turn raises the possibility of minor unmodelled
 disorder components in the macrocycle conformations.
;
_vrf_PLAT097_1a-THF              
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.69 eA-3  
RESPONSE:
 A large residual electron density peak of 2.69 eA-3
 is observed 0.23 %A from sulphur atom S2B. This peak
 is likely caused by a combination of deficiencies in the
 handling of the twinning and a minor unmodelled disorder
 component in the ring conformation.
;
_audit_creation_date             2022-05-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H8 F8 S4)'
_chemical_formula_sum            'C56 H32 F16 O2 S8'
_chemical_formula_weight         1297.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         C52H30F16S8N
_chemical_oxdiff_usercomment     
'OATSWJ #19141 MM-810 AT/SW fomblin oil on micromount'
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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.6071(3)
_cell_length_b                   14.6029(3)
_cell_length_c                   15.3344(3)
_cell_angle_alpha                97.914(2)
_cell_angle_beta                 98.988(2)
_cell_angle_gamma                110.147(2)
_cell_volume                     2764.52(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14778
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5300
_cell_measurement_theta_min      4.0690
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.395
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1312
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0289
0 1 0 0.0289
0 0 1 0.0039
0 0 -1 0.0219
5 -2 -1 0.1462
-5 2 1 0.1462

_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.026
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0009 -1.0006 -0.0045 0.1097 -0.0331 0.0093
-0.0009 1.0006 0.0045 -0.1097 0.0331 -0.0093
0.0000 -0.0035 1.0012 0.0096 0.1029 -0.0117
-0.0000 0.0035 -1.0012 -0.0096 -0.1029 0.0117
5.0040 -2.0055 -1.0005 0.0441 -0.0838 -0.5591
-5.0040 2.0055 1.0005 -0.0441 0.0838 0.5591

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11514
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.476
_diffrn_reflns_theta_min         2.982
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  10.00   0.50    1.00    --    0.00  57.00-150.00   70
  2  ω    -33.00  -1.00   0.50    1.00    --    0.00 -82.00   0.00   64
  3  ω     12.00  38.00   0.50    1.00    --    0.00 -82.00   0.00   52
  4  ω    -32.00   3.00   0.50    1.00    --    0.00  57.00 150.00   70
  5  ω     60.00  89.00   0.50    1.00    --    0.00  57.00-150.00   58
  6  ω      6.00  86.00   0.50    1.00    --    0.00  57.00 150.00  160
  7  ω    -26.00  50.00   0.50    1.00    --    0.00 -82.00  60.00  152
  8  ω     20.00  57.00   0.50    1.00    --    0.00  57.00-150.00   74
  9  ω    -30.00 108.00   0.50    4.00    --   57.50 -82.00 -60.00  276
 10  ω     14.00  40.00   0.50    4.00    --   57.50  71.00  -8.49   52
 11  ω     12.00  45.00   0.50    4.00    --   57.50  72.00-127.80   66
 12  ω     11.00 141.00   0.50    4.00    --   57.50  72.00 156.09  260
 13  ω    -16.00 102.00   0.50    4.00    --   57.50 -61.00 150.00  236
 14  ω    -24.00  98.00   0.50    4.00    --   57.50 -82.00 150.00  244
 15  ω     73.00 130.00   0.50    4.00    --   57.50  72.00  89.44  114
 16  ω     12.00 105.00   0.50    4.00    --   57.50  70.00 -58.96  186
 17  ω     11.00  47.00   0.50    4.00    --   57.50  72.00  38.57   72
 18  ω     11.00  67.00   0.50    4.00    --   57.50  72.00-114.45  112
 19  ω     60.00 144.00   0.50    4.00    --   57.50  72.00-154.81  168
 20  ω     72.00 123.00   0.50    4.00    --   57.50  72.00  38.57  102
 21  ω     13.00 119.00   0.50    4.00    --   57.50  71.00  57.70  212
 22  ω     11.00  55.00   0.50    4.00    --   57.50  72.00  89.44   88
 23  ω     11.00 142.00   0.50    4.00    --   57.50  70.00 139.20  262
 24  ω     56.00 137.00   0.50    4.00    --   57.50  72.00-127.80  162
 25  ω     12.00  46.00   0.50    4.00    --   57.50  72.00-154.81   68
 26  ω     11.00 146.00   0.50    4.00    --   57.50  70.00 -27.94  270
 27  ω     97.00 144.00   0.50    4.00    --   57.50  72.00-114.45   94
 28  ω     46.00 146.00   0.50    4.00    --   57.50  71.00  -8.49  200
 29  ω     -2.00 104.00   0.50    4.00    --   57.50 -61.00 -60.00  212
 30  ω     67.00 104.00   0.50    4.00    --   57.50 -82.00   0.00   74
 31  ω     68.00 190.00   0.50   10.00    --  115.00  63.00-105.98  244
 32  ω    110.00 204.00   0.50   10.00    --  115.00  47.00 -11.60  188
 33  ω    137.00 201.00   0.50   10.00    --  115.00  47.00  34.98  128
 34  ω     35.00  97.00   0.50   10.00    --  115.00  47.00 -11.60  124
 35  ω     62.00 132.00   0.50   10.00    --  115.00 -82.00 120.00  140
 36  ω    167.00 203.00   0.50   10.00    --  115.00  73.00 -18.06   72
 37  ω     34.00  68.00   0.50   10.00    --  115.00  47.00  34.98   68
 38  ω     67.00 131.00   0.50   10.00    --  115.00  73.00 -18.06  128
 39  ω     68.00 100.00   0.50   10.00    --  115.00  65.00-180.00   64
 40  ω    147.00 204.00   0.50   10.00    --  115.00  50.00 155.68  114
 41  ω     68.00 156.00   0.50   10.00    --  115.00  65.00-120.00  176
 42  ω     53.00 101.00   0.50   10.00    --  115.00  50.00 155.68   96
 43  ω     68.00 133.00   0.50   10.00    --  115.00  65.00  30.00  130
 44  ω     73.00 203.00   0.50   10.00    --  115.00  47.00 131.92  260
 45  ω    161.00 189.00   0.50   10.00    --  115.00  65.00-150.00   56
 46  ω     68.00 153.00   0.50   10.00    --  115.00  65.00-150.00  170
 47  ω     34.00  60.00   0.50   10.00    --  115.00  47.00 131.92   52
 48  ω     34.00 167.00   0.50   10.00    --  115.00  47.00  86.01  266
 49  ω    127.00 203.00   0.50   10.00    --  115.00  54.00  60.00  152
 50  ω     70.00  99.00   0.50   10.00    --  115.00  54.00  60.00   58
 51  ω    100.00 170.00   0.50   10.00    --  115.00  47.00 151.18  140
 52  ω    158.00 200.00   0.50   10.00    --  115.00  65.00-180.00   84
 53  ω     33.00  62.00   0.50   10.00    --  115.00  47.00 151.18   58
 54  ω     79.00 144.00   0.50   10.00    --  115.00 -82.00   0.00  130
 55  ω    133.00 166.00   0.50   10.00    --  115.00 -82.00 -60.00   66
 56  ω     63.00  90.00   0.50   10.00    --  115.00  54.00  30.00   54
 57  ω    103.00 165.00   0.50   10.00    --  115.00  54.00  30.00  124
 58  ω     69.00 102.00   0.50   10.00    --  115.00  65.00  90.00   66
 59  ω    145.00 203.00   0.50   10.00    --  115.00  65.00  90.00  116
 60  ω     89.00 176.00   0.50   10.00    --  115.00  47.00-154.66  174
 61  ω     38.00  77.00   0.50   10.00    --  115.00 -82.00 -60.00   78
 62  ω     27.00  52.00   0.50   10.00    --  115.00  43.00 -60.00   50
 63  ω    178.00 203.00   0.50   10.00    --  115.00  54.00-150.00   50
 64  ω     63.00 112.00   0.50   10.00    --  115.00  54.00-150.00   98
 65  ω     34.00  70.00   0.50   10.00    --  115.00  47.00-154.66   72
 66  ω     65.00 142.00   0.50   10.00    --  115.00 -82.00  60.00  154
 67  ω     62.00 141.00   0.50   10.00    --  115.00 -82.00-150.00  158
 68  ω     30.00 152.00   0.50   10.00    --  115.00 -82.00 -90.00  244
 69  ω     75.00 201.00   0.50   10.00    --  115.00  47.00 -38.92  252
 70  ω    175.00 204.00   0.50   10.00    --  115.00  65.00 -60.00   58
 71  ω    118.00 144.00   0.50   10.00    --  115.00  65.00 -60.00   52
 72  ω    116.00 192.00   0.50   10.00    --  115.00  74.00 -96.72  152
 73  ω     68.00  94.00   0.50   10.00    --  115.00  65.00 -60.00   52
 74  ω     86.00 126.00   0.50   10.00    --  115.00 -82.00 -60.00   80
 75  ω    150.00 198.00   0.50   10.00    --  115.00  43.00 -60.00   96
 76  ω     40.00  67.00   0.50   10.00    --  115.00 -82.00   0.00   54
 77  ω     67.00  93.00   0.50   10.00    --  115.00  74.00 -96.72   52
 78  ω     33.00  59.00   0.50   10.00    --  115.00  47.00 -38.92   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0333226000
_diffrn_orient_matrix_UB_12      -0.1097039000
_diffrn_orient_matrix_UB_13      0.0091696000
_diffrn_orient_matrix_UB_21      0.0169285000
_diffrn_orient_matrix_UB_22      0.0326784000
_diffrn_orient_matrix_UB_23      0.1028865000
_diffrn_orient_matrix_UB_31      -0.1178097000
_diffrn_orient_matrix_UB_32      -0.0093432000
_diffrn_orient_matrix_UB_33      -0.0116945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9518
_reflns_number_total             11514
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         2.689
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.633
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     534
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.1245
_refine_ls_restrained_S_all      1.598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3507
_refine_ls_wR_factor_ref         0.3658
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.592(10)
 0.408(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B), C42B(H42B), C43B(H43B),
 C45B(H45B), C46B(H46B), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A),
 C42A(H42A), C43A(H43A), C45A(H45A), C46A(H46A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1B S 0.85494(10) 0.80557(8) 1.03327(7) 0.0394(3) Uani 1 1 d . . . . .
S2B S 0.95732(9) 1.06796(8) 0.73586(7) 0.0343(3) Uani 1 1 d . . . . .
S3B S 0.87186(9) 0.74703(9) 0.38079(7) 0.0403(3) Uani 1 1 d . . . . .
S4B S 0.39076(9) 0.64105(7) 0.17695(8) 0.0363(3) Uani 1 1 d . . . . .
C11B C 0.8812(3) 0.8744(3) 0.9476(3) 0.0305(8) Uani 1 1 d . . . . .
C12B C 0.9722(4) 0.8885(3) 0.9129(3) 0.0351(9) Uani 1 1 d . . . . .
C13B C 0.9950(3) 0.9466(3) 0.8489(3) 0.0343(9) Uani 1 1 d . . . . .
C14B C 0.9277(3) 0.9918(3) 0.8152(3) 0.0281(8) Uani 1 1 d . . . . .
C15B C 0.8368(4) 0.9793(3) 0.8509(3) 0.0367(9) Uani 1 1 d . . . . .
C16B C 0.8132(4) 0.9206(3) 0.9145(3) 0.0358(9) Uani 1 1 d . . . . .
F17B F 1.0430(3) 0.8475(3) 0.9413(2) 0.0607(8) Uani 1 1 d . . . . .
F18B F 1.0840(2) 0.9553(3) 0.8172(2) 0.0587(8) Uani 1 1 d . . . . .
F19B F 0.7693(2) 1.0230(3) 0.8253(2) 0.0574(8) Uani 1 1 d . . . . .
F20B F 0.7257(3) 0.9123(3) 0.9475(2) 0.0632(9) Uani 1 1 d . . . . .
C21B C 0.9307(3) 0.9754(3) 0.6374(3) 0.0309(8) Uani 1 1 d . . . . .
C22B C 1.0126(3) 0.9492(3) 0.6107(3) 0.0339(9) Uani 1 1 d . . . . .
H22B H 1.083538 0.979705 0.646513 0.041 Uiso 1 1 calc R U . . .
C23B C 0.9913(3) 0.8789(3) 0.5321(3) 0.0341(9) Uani 1 1 d . . . . .
H23B H 1.047017 0.860534 0.514715 0.041 Uiso 1 1 calc R U . . .
C24B C 0.8869(3) 0.8354(3) 0.4790(3) 0.0293(8) Uani 1 1 d . . . . .
C25B C 0.8057(4) 0.8611(4) 0.5045(3) 0.0371(9) Uani 1 1 d . . . . .
H25B H 0.734653 0.830633 0.468971 0.045 Uiso 1 1 calc R U . . .
C26B C 0.8289(3) 0.9325(3) 0.5832(3) 0.0347(9) Uani 1 1 d . . . . .
H26B H 0.773358 0.951870 0.599775 0.042 Uiso 1 1 calc R U . . .
C31B C 0.7370(3) 0.7158(3) 0.3251(3) 0.0309(8) Uani 1 1 d . . . . .
C32B C 0.7122(3) 0.7580(3) 0.2523(3) 0.0322(8) Uani 1 1 d . . . . .
C33B C 0.6085(4) 0.7302(3) 0.2047(3) 0.0317(8) Uani 1 1 d . . . . .
C34B C 0.5235(3) 0.6602(3) 0.2283(3) 0.0313(8) Uani 1 1 d . . . . .
C35B C 0.5466(4) 0.6170(3) 0.2993(3) 0.0382(10) Uani 1 1 d . . . . .
C36B C 0.6528(4) 0.6435(4) 0.3466(3) 0.0403(10) Uani 1 1 d . . . . .
F37B F 0.7904(2) 0.8287(2) 0.2298(2) 0.0567(8) Uani 1 1 d . . . . .
F38B F 0.5913(2) 0.7712(2) 0.13559(18) 0.0468(7) Uani 1 1 d . . . . .
F39B F 0.4693(3) 0.5511(2) 0.3271(2) 0.0638(9) Uani 1 1 d . . . . .
F40B F 0.6715(3) 0.6003(3) 0.4158(2) 0.0681(10) Uani 1 1 d . . . . .
C41B C 0.3311(3) 0.5124(3) 0.1263(3) 0.0294(8) Uani 1 1 d . . . . .
C42B C 0.3863(3) 0.4571(3) 0.0905(3) 0.0353(9) Uani 1 1 d . . . . .
H42B H 0.461915 0.486024 0.097512 0.042 Uiso 1 1 calc R U . . .
C43B C 0.3292(4) 0.3589(3) 0.0443(3) 0.0333(9) Uani 1 1 d . . . . .
H43B H 0.365903 0.320246 0.019957 0.040 Uiso 1 1 calc R U . . .
C44B C 0.2176(3) 0.3172(3) 0.0338(3) 0.0307(8) Uani 1 1 d . . . . .
C45B C 0.1639(3) 0.3730(3) 0.0697(3) 0.0394(10) Uani 1 1 d . . . . .
H45B H 0.088084 0.344677 0.061559 0.047 Uiso 1 1 calc R U . . .
C46B C 0.2201(4) 0.4700(3) 0.1175(3) 0.0369(9) Uani 1 1 d . . . . .
H46B H 0.183475 0.507434 0.144068 0.044 Uiso 1 1 calc R U . . .
S1A S 0.47335(9) 1.07393(7) 0.74121(7) 0.0323(3) Uani 1 1 d . . . . .
S2A S 0.36894(9) 0.74834(9) 0.38237(7) 0.0416(3) Uani 1 1 d . . . . .
S3A S -0.10518(9) 0.64406(8) 0.17262(8) 0.0417(3) Uani 1 1 d . . . . .
S4A S -0.34843(9) 0.19172(7) -0.03213(6) 0.0326(3) Uani 1 1 d . . . . .
C11A C 0.4409(3) 0.9842(3) 0.6396(3) 0.0276(8) Uani 1 1 d . . . . .
C12A C 0.5160(3) 0.9512(3) 0.6115(3) 0.0300(8) Uani 1 1 d . . . . .
C13A C 0.4892(3) 0.8807(3) 0.5323(3) 0.0285(8) Uani 1 1 d . . . . .
C14A C 0.3857(3) 0.8388(3) 0.4784(3) 0.0299(8) Uani 1 1 d . . . . .
C15A C 0.3116(3) 0.8741(4) 0.5063(3) 0.0379(10) Uani 1 1 d . . . . .
C16A C 0.3385(4) 0.9457(3) 0.5854(3) 0.0358(9) Uani 1 1 d . . . . .
F17A F 0.6178(2) 0.9874(2) 0.6579(2) 0.0555(8) Uani 1 1 d . . . . .
F18A F 0.5663(2) 0.8510(2) 0.50681(19) 0.0486(7) Uani 1 1 d . . . . .
F19A F 0.2118(3) 0.8436(3) 0.4588(2) 0.0779(12) Uani 1 1 d . . . . .
F20A F 0.2634(2) 0.9758(3) 0.6095(2) 0.0621(9) Uani 1 1 d . . . . .
C21A C 0.2345(3) 0.7158(3) 0.3233(3) 0.0332(9) Uani 1 1 d . . . . .
C22A C 0.2156(4) 0.7608(3) 0.2513(3) 0.0358(9) Uani 1 1 d . . . . .
H22A H 0.273242 0.809045 0.235075 0.043 Uiso 1 1 calc R U . . .
C23A C 0.1104(4) 0.7334(3) 0.2038(3) 0.0351(9) Uani 1 1 d . . . . .
H23A H 0.095970 0.763918 0.155040 0.042 Uiso 1 1 calc R U . . .
C24A C 0.0270(3) 0.6622(3) 0.2267(3) 0.0324(9) Uani 1 1 d . . . . .
C25A C 0.0461(4) 0.6162(4) 0.2975(4) 0.0448(11) Uani 1 1 d . . . . .
H25A H -0.011721 0.568876 0.314315 0.054 Uiso 1 1 calc R U . . .
C26A C 0.1511(4) 0.6405(4) 0.3433(3) 0.0444(11) Uani 1 1 d . . . . .
H26A H 0.165879 0.605632 0.388335 0.053 Uiso 1 1 calc R U . . .
C31A C -0.1644(3) 0.5166(3) 0.1227(3) 0.0325(9) Uani 1 1 d . . . . .
C32A C -0.1113(3) 0.4590(3) 0.0871(3) 0.0339(9) Uani 1 1 d . . . . .
C33A C -0.1673(3) 0.3593(3) 0.0438(3) 0.0278(8) Uani 1 1 d . . . . .
C34A C -0.2783(3) 0.3151(3) 0.0310(3) 0.0278(8) Uani 1 1 d . . . . .
C35A C -0.3308(3) 0.3734(3) 0.0642(3) 0.0333(9) Uani 1 1 d . . . . .
C36A C -0.2756(4) 0.4707(3) 0.1100(3) 0.0319(8) Uani 1 1 d . . . . .
F37A F -0.0054(2) 0.4972(2) 0.0912(2) 0.0540(8) Uani 1 1 d . . . . .
F38A F -0.1114(2) 0.3087(2) 0.0114(2) 0.0530(7) Uani 1 1 d . . . . .
F39A F -0.4365(2) 0.3367(2) 0.0553(2) 0.0614(9) Uani 1 1 d . . . . .
F40A F -0.3298(2) 0.5252(2) 0.1414(2) 0.0569(8) Uani 1 1 d . . . . .
C41A C -0.3784(3) 0.1253(3) 0.0557(3) 0.0286(8) Uani 1 1 d . . . . .
C42A C -0.4748(3) 0.1103(3) 0.0832(3) 0.0329(9) Uani 1 1 d . . . . .
H42A H -0.521646 0.140270 0.058670 0.040 Uiso 1 1 calc R U . . .
C43A C -0.5029(3) 0.0510(3) 0.1472(3) 0.0321(8) Uani 1 1 d . . . . .
H43A H -0.568402 0.041254 0.166046 0.038 Uiso 1 1 calc R U . . .
C44A C -0.4342(3) 0.0068(3) 0.1827(3) 0.0281(8) Uani 1 1 d . . . . .
C45A C -0.3383(4) 0.0214(3) 0.1548(3) 0.0372(9) Uani 1 1 d . . . . .
H45A H -0.292257 -0.009798 0.178277 0.045 Uiso 1 1 calc R U . . .
C46A C -0.3096(3) 0.0812(3) 0.0929(3) 0.0335(9) Uani 1 1 d . . . . .
H46A H -0.242982 0.092332 0.075700 0.040 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
S1B C11B 1.768(4) . ?
S1B C44B 1.790(4) 2_666 ?
S2B C14B 1.760(4) . ?
S2B C21B 1.780(4) . ?
S3B C24B 1.778(4) . ?
S3B C31B 1.770(4) . ?
S4B C34B 1.763(4) . ?
S4B C41B 1.773(4) . ?
C11B C12B 1.384(6) . ?
C11B C16B 1.395(7) . ?
C12B C13B 1.387(7) . ?
C12B F17B 1.348(5) . ?
C13B C14B 1.379(6) . ?
C13B F18B 1.347(5) . ?
C14B C15B 1.395(6) . ?
C15B C16B 1.390(7) . ?
C15B F19B 1.328(5) . ?
C16B F20B 1.338(5) . ?
C21B C22B 1.395(6) . ?
C21B C26B 1.379(6) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.391(6) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.400(6) . ?
C24B C25B 1.376(6) . ?
C25B H25B 0.9500 . ?
C25B C26B 1.396(6) . ?
C26B H26B 0.9500 . ?
C31B C32B 1.397(6) . ?
C31B C36B 1.385(6) . ?
C32B C33B 1.375(6) . ?
C32B F37B 1.332(5) . ?
C33B C34B 1.389(6) . ?
C33B F38B 1.316(5) . ?
C34B C35B 1.379(6) . ?
C35B C36B 1.405(7) . ?
C35B F39B 1.330(5) . ?
C36B F40B 1.340(6) . ?
C41B C42B 1.392(6) . ?
C41B C46B 1.397(6) . ?
C42B H42B 0.9500 . ?
C42B C43B 1.394(6) . ?
C43B H43B 0.9500 . ?
C43B C44B 1.401(6) . ?
C44B C45B 1.382(6) . ?
C45B H45B 0.9500 . ?
C45B C46B 1.387(6) . ?
C46B H46B 0.9500 . ?
S1A C11A 1.778(4) . ?
S1A C44A 1.782(4) 2_566 ?
S2A C14A 1.766(4) . ?
S2A C21A 1.776(4) . ?
S3A C24A 1.772(4) . ?
S3A C31A 1.756(4) . ?
S4A C34A 1.772(4) . ?
S4A C41A 1.783(4) . ?
C11A C12A 1.373(6) . ?
C11A C16A 1.385(6) . ?
C12A C13A 1.388(6) . ?
C12A F17A 1.338(5) . ?
C13A C14A 1.394(6) . ?
C13A F18A 1.355(5) . ?
C14A C15A 1.378(6) . ?
C15A C16A 1.395(6) . ?
C15A F19A 1.326(5) . ?
C16A F20A 1.326(5) . ?
C21A C22A 1.393(7) . ?
C21A C26A 1.391(7) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.393(6) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.380(6) . ?
C24A C25A 1.389(7) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.388(7) . ?
C26A H26A 0.9500 . ?
C31A C32A 1.393(6) . ?
C31A C36A 1.396(6) . ?
C32A C33A 1.398(6) . ?
C32A F37A 1.341(5) . ?
C33A C34A 1.392(6) . ?
C33A F38A 1.332(5) . ?
C34A C35A 1.382(6) . ?
C35A C36A 1.379(6) . ?
C35A F39A 1.327(5) . ?
C36A F40A 1.348(5) . ?
C41A C42A 1.395(6) . ?
C41A C46A 1.403(6) . ?
C42A H42A 0.9500 . ?
C42A C43A 1.407(6) . ?
C43A H43A 0.9500 . ?
C43A C44A 1.394(6) . ?
C44A C45A 1.392(6) . ?
C45A H45A 0.9500 . ?
C45A C46A 1.387(6) . ?
C46A H46A 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
C11B S1B C44B 100.35(18) . 2_666 ?
C14B S2B C21B 100.02(19) . . ?
C31B S3B C24B 102.81(19) . . ?
C34B S4B C41B 104.9(2) . . ?
C12B C11B S1B 121.8(3) . . ?
C12B C11B C16B 116.9(4) . . ?
C16B C11B S1B 121.2(3) . . ?
C11B C12B C13B 121.5(4) . . ?
F17B C12B C11B 121.1(4) . . ?
F17B C12B C13B 117.4(4) . . ?
C14B C13B C12B 122.0(4) . . ?
F18B C13B C12B 118.0(4) . . ?
F18B C13B C14B 120.0(4) . . ?
C13B C14B S2B 122.4(3) . . ?
C13B C14B C15B 116.9(4) . . ?
C15B C14B S2B 120.6(3) . . ?
C16B C15B C14B 121.3(4) . . ?
F19B C15B C14B 121.4(4) . . ?
F19B C15B C16B 117.3(4) . . ?
C15B C16B C11B 121.3(4) . . ?
F20B C16B C11B 119.7(4) . . ?
F20B C16B C15B 118.8(4) . . ?
C22B C21B S2B 121.2(3) . . ?
C26B C21B S2B 119.8(3) . . ?
C26B C21B C22B 118.9(4) . . ?
C21B C22B H22B 119.7 . . ?
C23B C22B C21B 120.6(4) . . ?
C23B C22B H22B 119.7 . . ?
C22B C23B H23B 120.3 . . ?
C22B C23B C24B 119.4(4) . . ?
C24B C23B H23B 120.3 . . ?
C23B C24B S3B 114.3(3) . . ?
C25B C24B S3B 125.3(3) . . ?
C25B C24B C23B 120.4(4) . . ?
C24B C25B H25B 120.3 . . ?
C24B C25B C26B 119.3(4) . . ?
C26B C25B H25B 120.3 . . ?
C21B C26B C25B 121.3(4) . . ?
C21B C26B H26B 119.3 . . ?
C25B C26B H26B 119.3 . . ?
C32B C31B S3B 120.8(3) . . ?
C36B C31B S3B 121.8(3) . . ?
C36B C31B C32B 117.2(4) . . ?
C33B C32B C31B 121.6(4) . . ?
F37B C32B C31B 119.4(4) . . ?
F37B C32B C33B 119.0(4) . . ?
C32B C33B C34B 121.2(4) . . ?
F38B C33B C32B 118.4(4) . . ?
F38B C33B C34B 120.4(4) . . ?
C33B C34B S4B 119.5(3) . . ?
C35B C34B S4B 122.1(4) . . ?
C35B C34B C33B 118.0(4) . . ?
C34B C35B C36B 120.9(4) . . ?
F39B C35B C34B 121.4(4) . . ?
F39B C35B C36B 117.6(4) . . ?
C31B C36B C35B 121.0(4) . . ?
F40B C36B C31B 120.0(4) . . ?
F40B C36B C35B 118.9(4) . . ?
C42B C41B S4B 124.2(3) . . ?
C42B C41B C46B 120.8(4) . . ?
C46B C41B S4B 114.8(3) . . ?
C41B C42B H42B 120.4 . . ?
C41B C42B C43B 119.2(4) . . ?
C43B C42B H42B 120.4 . . ?
C42B C43B H43B 120.0 . . ?
C42B C43B C44B 120.0(4) . . ?
C44B C43B H43B 120.0 . . ?
C43B C44B S1B 119.0(3) . 2_666 ?
C45B C44B S1B 120.7(3) . 2_666 ?
C45B C44B C43B 120.2(4) . . ?
C44B C45B H45B 119.8 . . ?
C44B C45B C46B 120.4(4) . . ?
C46B C45B H45B 119.8 . . ?
C41B C46B H46B 120.3 . . ?
C45B C46B C41B 119.4(4) . . ?
C45B C46B H46B 120.3 . . ?
C11A S1A C44A 100.01(18) . 2_566 ?
C14A S2A C21A 104.7(2) . . ?
C31A S3A C24A 104.7(2) . . ?
C34A S4A C41A 101.02(17) . . ?
C12A C11A S1A 121.6(3) . . ?
C12A C11A C16A 117.4(4) . . ?
C16A C11A S1A 121.0(3) . . ?
C11A C12A C13A 120.9(4) . . ?
F17A C12A C11A 121.4(4) . . ?
F17A C12A C13A 117.7(4) . . ?
C12A C13A C14A 122.4(4) . . ?
F18A C13A C12A 118.8(4) . . ?
F18A C13A C14A 118.9(4) . . ?
C13A C14A S2A 114.7(3) . . ?
C15A C14A S2A 129.1(3) . . ?
C15A C14A C13A 116.2(4) . . ?
C14A C15A C16A 121.5(4) . . ?
F19A C15A C14A 122.0(4) . . ?
F19A C15A C16A 116.4(4) . . ?
C11A C16A C15A 121.5(4) . . ?
F20A C16A C11A 119.7(4) . . ?
F20A C16A C15A 118.8(4) . . ?
C22A C21A S2A 118.7(3) . . ?
C26A C21A S2A 120.5(4) . . ?
C26A C21A C22A 120.6(4) . . ?
C21A C22A H22A 120.7 . . ?
C23A C22A C21A 118.6(4) . . ?
C23A C22A H22A 120.7 . . ?
C22A C23A H23A 119.7 . . ?
C24A C23A C22A 120.6(4) . . ?
C24A C23A H23A 119.7 . . ?
C23A C24A S3A 117.4(3) . . ?
C23A C24A C25A 120.8(4) . . ?
C25A C24A S3A 121.4(4) . . ?
C24A C25A H25A 120.5 . . ?
C26A C25A C24A 119.0(5) . . ?
C26A C25A H25A 120.5 . . ?
C21A C26A H26A 119.9 . . ?
C25A C26A C21A 120.2(4) . . ?
C25A C26A H26A 119.9 . . ?
C32A C31A S3A 125.5(3) . . ?
C32A C31A C36A 116.8(4) . . ?
C36A C31A S3A 117.5(3) . . ?
C31A C32A C33A 121.0(4) . . ?
F37A C32A C31A 121.7(4) . . ?
F37A C32A C33A 117.3(4) . . ?
C34A C33A C32A 121.5(4) . . ?
F38A C33A C32A 117.7(4) . . ?
F38A C33A C34A 120.8(4) . . ?
C33A C34A S4A 120.5(3) . . ?
C35A C34A S4A 122.1(3) . . ?
C35A C34A C33A 117.2(4) . . ?
C36A C35A C34A 121.6(4) . . ?
F39A C35A C34A 121.0(4) . . ?
F39A C35A C36A 117.4(4) . . ?
C35A C36A C31A 121.9(4) . . ?
F40A C36A C31A 118.3(4) . . ?
F40A C36A C35A 119.8(4) . . ?
C42A C41A S4A 120.1(3) . . ?
C42A C41A C46A 119.3(4) . . ?
C46A C41A S4A 120.5(3) . . ?
C41A C42A H42A 119.8 . . ?
C41A C42A C43A 120.3(4) . . ?
C43A C42A H42A 119.8 . . ?
C42A C43A H43A 120.2 . . ?
C44A C43A C42A 119.6(4) . . ?
C44A C43A H43A 120.2 . . ?
C43A C44A S1A 119.6(3) . 2_566 ?
C45A C44A S1A 120.4(3) . 2_566 ?
C45A C44A C43A 119.9(4) . . ?
C44A C45A H45A 119.7 . . ?
C46A C45A C44A 120.5(4) . . ?
C46A C45A H45A 119.7 . . ?
C41A C46A H46A 119.9 . . ?
C45A C46A C41A 120.3(4) . . ?
C45A C46A H46A 119.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22B H22B F18B 0.95 2.69 3.143(6) 110.0 . yes
C22B H22B F37B 0.95 2.93 3.669(5) 135.6 2_776 yes
C22B H22B F20A 0.95 2.61 3.302(5) 129.6 1_655 yes
C23B H23B F19A 0.95 2.60 3.536(5) 169.0 1_655 yes
C23B H23B F20A 0.95 2.86 3.417(5) 118.4 1_655 yes
C25B H25B F40B 0.95 3.12 3.563(6) 110.2 . yes
C25B H25B F18A 0.95 2.55 3.216(5) 127.2 . yes
C25B H25B F20A 0.95 3.21 3.433(6) 95.2 2_676 yes
C26B H26B F17A 0.95 2.60 3.545(5) 172.5 . yes
C26B H26B F18A 0.95 2.73 3.306(5) 119.9 . yes
C26B H26B F19A 0.95 3.19 3.624(7) 110.1 2_676 yes
C42B H42B F39A 0.95 3.01 3.502(6) 113.9 1_655 yes
C42B H42B F40A 0.95 2.65 3.567(5) 163.8 1_655 yes
C43B H43B F38B 0.95 2.81 3.646(5) 147.2 2_665 yes
C43B H43B F39A 0.95 2.58 3.296(6) 132.6 1_655 yes
C45B H45B F17B 0.95 2.75 3.432(5) 129.6 2_666 yes
C45B H45B F37A 0.95 2.94 3.414(6) 112.3 . yes
C45B H45B F38A 0.95 2.55 3.466(5) 162.7 . yes
C46B H46B F37A 0.95 2.52 3.199(6) 128.8 . yes
C22A H22A F19B 0.95 2.94 3.471(6) 116.6 2_676 yes
C22A H22A F17A 0.95 2.93 3.530(5) 122.3 2_676 yes
C23A H23A S2B 0.95 3.13 3.390(5) 97.4 2_676 yes
C23A H23A F19B 0.95 2.96 3.492(6) 116.5 2_676 yes
C23A H23A F38A 0.95 2.69 3.275(5) 120.1 2_565 yes
C42A H42A F20B 0.95 2.60 3.266(5) 127.9 2_566 yes
C42A H42A F39A 0.95 2.71 3.265(6) 117.9 . yes
C43A H43A F19B 0.95 2.60 3.520(5) 163.6 2_566 yes
C43A H43A F20B 0.95 2.87 3.397(6) 116.2 2_566 yes
C43A H43A F17A 0.95 2.93 3.607(5) 129.1 2_566 yes
C45A H45A F18B 0.95 2.65 3.311(6) 126.8 2_666 yes
C45A H45A F38B 0.95 2.96 3.400(5) 109.5 1_445 yes
C45A H45A F20A 0.95 3.16 3.590(6) 109.2 2_566 yes
C46A H46A F17B 0.95 2.62 3.558(5) 168.0 2_666 yes
C46A H46A F18B 0.95 2.85 3.408(6) 118.8 2_666 yes
C46A H46A F20B 0.95 2.92 3.305(6) 105.9 1_444 yes

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
S1B C11B C12B C13B -176.8(3) . . . . ?
S1B C11B C12B F17B 2.1(6) . . . . ?
S1B C11B C16B C15B 176.3(3) . . . . ?
S1B C11B C16B F20B -0.5(6) . . . . ?
S1B C44B C45B C46B -176.5(4) 2_666 . . . ?
S2B C14B C15B C16B -179.1(3) . . . . ?
S2B C14B C15B F19B 1.1(6) . . . . ?
S2B C21B C22B C23B -178.1(3) . . . . ?
S2B C21B C26B C25B 178.7(4) . . . . ?
S3B C24B C25B C26B -179.5(3) . . . . ?
S3B C31B C32B C33B 176.1(3) . . . . ?
S3B C31B C32B F37B -5.7(6) . . . . ?
S3B C31B C36B C35B -177.6(4) . . . . ?
S3B C31B C36B F40B 5.1(7) . . . . ?
S4B C34B C35B C36B -171.7(4) . . . . ?
S4B C34B C35B F39B 6.5(7) . . . . ?
S4B C41B C42B C43B -173.6(3) . . . . ?
S4B C41B C46B C45B 172.7(4) . . . . ?
C11B C12B C13B C14B -1.2(7) . . . . ?
C11B C12B C13B F18B -178.8(4) . . . . ?
C12B C11B C16B C15B -1.0(6) . . . . ?
C12B C11B C16B F20B -177.9(4) . . . . ?
C12B C13B C14B S2B 178.5(3) . . . . ?
C12B C13B C14B C15B 2.2(6) . . . . ?
C13B C14B C15B C16B -2.7(6) . . . . ?
C13B C14B C15B F19B 177.4(4) . . . . ?
C14B S2B C21B C22B -94.5(4) . . . . ?
C14B S2B C21B C26B 89.3(4) . . . . ?
C14B C15B C16B C11B 2.2(7) . . . . ?
C14B C15B C16B F20B 179.1(4) . . . . ?
C16B C11B C12B C13B 0.6(6) . . . . ?
C16B C11B C12B F17B 179.5(4) . . . . ?
F17B C12B C13B C14B 179.8(4) . . . . ?
F17B C12B C13B F18B 2.2(6) . . . . ?
F18B C13B C14B S2B -3.9(6) . . . . ?
F18B C13B C14B C15B 179.8(4) . . . . ?
F19B C15B C16B C11B -177.9(4) . . . . ?
F19B C15B C16B F20B -1.0(6) . . . . ?
C21B S2B C14B C13B 74.1(4) . . . . ?
C21B S2B C14B C15B -109.7(4) . . . . ?
C21B C22B C23B C24B 1.0(7) . . . . ?
C22B C21B C26B C25B 2.4(7) . . . . ?
C22B C23B C24B S3B 180.0(3) . . . . ?
C22B C23B C24B C25B -0.6(7) . . . . ?
C23B C24B C25B C26B 1.1(7) . . . . ?
C24B S3B C31B C32B 100.5(4) . . . . ?
C24B S3B C31B C36B -84.6(4) . . . . ?
C24B C25B C26B C21B -2.1(7) . . . . ?
C26B C21B C22B C23B -1.8(7) . . . . ?
C31B S3B C24B C23B -174.9(3) . . . . ?
C31B S3B C24B C25B 5.7(5) . . . . ?
C31B C32B C33B C34B 1.3(7) . . . . ?
C31B C32B C33B F38B -178.3(4) . . . . ?
C32B C31B C36B C35B -2.5(7) . . . . ?
C32B C31B C36B F40B -179.9(4) . . . . ?
C32B C33B C34B S4B 170.3(3) . . . . ?
C32B C33B C34B C35B -1.9(6) . . . . ?
C33B C34B C35B C36B 0.3(7) . . . . ?
C33B C34B C35B F39B 178.4(4) . . . . ?
C34B S4B C41B C42B -32.7(4) . . . . ?
C34B S4B C41B C46B 152.5(3) . . . . ?
C34B C35B C36B C31B 2.0(8) . . . . ?
C34B C35B C36B F40B 179.3(5) . . . . ?
C36B C31B C32B C33B 0.9(7) . . . . ?
C36B C31B C32B F37B 179.1(4) . . . . ?
F37B C32B C33B C34B -176.9(4) . . . . ?
F37B C32B C33B F38B 3.5(6) . . . . ?
F38B C33B C34B S4B -10.2(6) . . . . ?
F38B C33B C34B C35B 177.7(4) . . . . ?
F39B C35B C36B C31B -176.3(5) . . . . ?
F39B C35B C36B F40B 1.1(7) . . . . ?
C41B S4B C34B C33B 122.8(3) . . . . ?
C41B S4B C34B C35B -65.3(4) . . . . ?
C41B C42B C43B C44B 0.5(7) . . . . ?
C42B C41B C46B C45B -2.3(7) . . . . ?
C42B C43B C44B S1B 175.2(3) . . . 2_666 ?
C42B C43B C44B C45B -0.5(7) . . . . ?
C43B C44B C45B C46B -1.0(7) . . . . ?
C44B S1B C11B C12B -88.9(4) 2_666 . . . ?
C44B S1B C11B C16B 93.9(4) 2_666 . . . ?
C44B C45B C46B C41B 2.4(7) . . . . ?
C46B C41B C42B C43B 0.9(7) . . . . ?
S1A C11A C12A C13A 179.7(3) . . . . ?
S1A C11A C12A F17A -2.1(6) . . . . ?
S1A C11A C16A C15A -179.0(4) . . . . ?
S1A C11A C16A F20A -0.1(6) . . . . ?
S1A C44A C45A C46A 177.6(3) 2_566 . . . ?
S2A C14A C15A C16A 179.2(4) . . . . ?
S2A C14A C15A F19A -2.0(8) . . . . ?
S2A C21A C22A C23A 178.5(3) . . . . ?
S2A C21A C26A C25A 179.3(4) . . . . ?
S3A C24A C25A C26A -173.8(4) . . . . ?
S3A C31A C32A C33A -176.1(3) . . . . ?
S3A C31A C32A F37A 2.5(7) . . . . ?
S3A C31A C36A C35A 174.1(4) . . . . ?
S3A C31A C36A F40A -3.8(6) . . . . ?
S4A C34A C35A C36A -177.2(3) . . . . ?
S4A C34A C35A F39A 4.7(6) . . . . ?
S4A C41A C42A C43A 174.7(3) . . . . ?
S4A C41A C46A C45A -173.6(3) . . . . ?
C11A C12A C13A C14A -1.2(6) . . . . ?
C11A C12A C13A F18A 179.4(4) . . . . ?
C12A C11A C16A C15A 1.5(7) . . . . ?
C12A C11A C16A F20A -179.6(4) . . . . ?
C12A C13A C14A S2A -178.4(3) . . . . ?
C12A C13A C14A C15A 2.6(6) . . . . ?
C13A C14A C15A C16A -1.9(7) . . . . ?
C13A C14A C15A F19A 176.9(5) . . . . ?
C14A S2A C21A C22A 97.9(4) . . . . ?
C14A S2A C21A C26A -87.9(4) . . . . ?
C14A C15A C16A C11A -0.1(8) . . . . ?
C14A C15A C16A F20A -179.0(5) . . . . ?
C16A C11A C12A C13A -0.8(6) . . . . ?
C16A C11A C12A F17A 177.4(4) . . . . ?
F17A C12A C13A C14A -179.5(4) . . . . ?
F17A C12A C13A F18A 1.2(6) . . . . ?
F18A C13A C14A S2A 1.0(5) . . . . ?
F18A C13A C14A C15A -178.1(4) . . . . ?
F19A C15A C16A C11A -178.9(5) . . . . ?
F19A C15A C16A F20A 2.1(7) . . . . ?
C21A S2A C14A C13A -175.7(3) . . . . ?
C21A S2A C14A C15A 3.2(5) . . . . ?
C21A C22A C23A C24A -0.9(7) . . . . ?
C22A C21A C26A C25A -6.5(8) . . . . ?
C22A C23A C24A S3A 171.9(3) . . . . ?
C22A C23A C24A C25A -0.2(7) . . . . ?
C23A C24A C25A C26A -2.0(8) . . . . ?
C24A S3A C31A C32A -33.6(4) . . . . ?
C24A S3A C31A C36A 152.5(4) . . . . ?
C24A C25A C26A C21A 5.3(8) . . . . ?
C26A C21A C22A C23A 4.2(7) . . . . ?
C31A S3A C24A C23A 124.1(4) . . . . ?
C31A S3A C24A C25A -63.8(5) . . . . ?
C31A C32A C33A C34A 2.9(7) . . . . ?
C31A C32A C33A F38A 180.0(4) . . . . ?
C32A C31A C36A C35A -0.3(7) . . . . ?
C32A C31A C36A F40A -178.2(4) . . . . ?
C32A C33A C34A S4A 174.8(3) . . . . ?
C32A C33A C34A C35A -1.1(6) . . . . ?
C33A C34A C35A C36A -1.4(6) . . . . ?
C33A C34A C35A F39A -179.5(4) . . . . ?
C34A S4A C41A C42A 91.5(3) . . . . ?
C34A S4A C41A C46A -93.4(3) . . . . ?
C34A C35A C36A C31A 2.1(7) . . . . ?
C34A C35A C36A F40A -180.0(4) . . . . ?
C36A C31A C32A C33A -2.2(7) . . . . ?
C36A C31A C32A F37A 176.4(4) . . . . ?
F37A C32A C33A C34A -175.7(4) . . . . ?
F37A C32A C33A F38A 1.4(6) . . . . ?
F38A C33A C34A S4A -2.2(5) . . . . ?
F38A C33A C34A C35A -178.0(4) . . . . ?
F39A C35A C36A C31A -179.7(4) . . . . ?
F39A C35A C36A F40A -1.8(7) . . . . ?
C41A S4A C34A C33A 104.9(3) . . . . ?
C41A S4A C34A C35A -79.4(4) . . . . ?
C41A C42A C43A C44A -0.4(6) . . . . ?
C42A C41A C46A C45A 1.5(6) . . . . ?
C42A C43A C44A S1A -176.5(3) . . . 2_566 ?
C42A C43A C44A C45A 0.0(6) . . . . ?
C43A C44A C45A C46A 1.1(6) . . . . ?
C44A S1A C11A C12A -94.1(4) 2_566 . . . ?
C44A S1A C11A C16A 86.5(4) 2_566 . . . ?
C44A C45A C46A C41A -1.9(7) . . . . ?
C46A C41A C42A C43A -0.4(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.275 0.500 0.500 742.0 195.7 '4 C4H8O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.714
_oxdiff_twin_integration_method  simultaneous
_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 0.592(10) 422 43765 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.408(10) 254 43765 nmt 0.9999 0.0034 -0.0012 0.0048 1.0001 0.0182 -0.0083
-0.0237 0.9969

_twin_special_details            
;
Component 2 rotated by 1.2052° 
 around [-0.94 0.30 0.16] (reciprocal) or [-1.00 -0.05 -0.01] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: tetrahydrofuran'
####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 2175106'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWI
_nottingham_internal_coll_number 19140
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   09/05/2022
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 09/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 09/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 25/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 25/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 25/05/2022
_refine_special_details          SQUEEZE
_audit_creation_date             2022-05-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H32 F16 S8'
_chemical_formula_sum            'C56 H32 F16 S8'
_chemical_formula_weight         1265.29
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0019 0.0015 '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 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1048 0.1164 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5286(2)
_cell_length_b                   10.3554(2)
_cell_length_c                   14.2500(4)
_cell_angle_alpha                75.540(2)
_cell_angle_beta                 89.177(2)
_cell_angle_gamma                73.340(2)
_cell_volume                     1301.90(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.678120671249744
_cell_measurement_theta_min      1.4290450194019093
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9922883275879729
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.1.018: AIMLESS, version 0.7.7 : 23/04/21
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26997
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         35.968
_diffrn_reflns_theta_min         2.059
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7278
_reflns_number_total             11650
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         11650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1370
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C43(H43), C46(H46)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1 S 1.33873(4) 0.21612(4) 0.57054(3) 0.02772(9) Uani 1 1 d . . . . .
S2 S 1.23070(4) 0.52318(4) 0.12113(3) 0.02718(9) Uani 1 1 d . . . . .
S3 S 0.54715(4) 0.61849(5) 0.06552(3) 0.02869(9) Uani 1 1 d . . . . .
S4 S 0.23924(5) 0.97271(4) 0.35949(3) 0.02875(9) Uani 1 1 d . . . . .
C11 C 1.31970(16) 0.30645(16) 0.44687(11) 0.0240(3) Uani 1 1 d . . . . .
C12 C 1.22446(17) 0.44064(16) 0.41428(11) 0.0254(3) Uani 1 1 d . . . . .
C13 C 1.19869(16) 0.50649(15) 0.31681(11) 0.0239(3) Uani 1 1 d . . . . .
C14 C 1.26746(16) 0.44238(16) 0.24632(11) 0.0233(3) Uani 1 1 d . . . . .
C15 C 1.36774(16) 0.31078(16) 0.27888(12) 0.0248(3) Uani 1 1 d . . . . .
C16 C 1.39415(16) 0.24475(16) 0.37739(12) 0.0245(3) Uani 1 1 d . . . . .
F17 F 1.15207(11) 0.50661(10) 0.47846(7) 0.0328(2) Uani 1 1 d . . . . .
F18 F 1.10456(11) 0.63578(10) 0.28941(7) 0.0314(2) Uani 1 1 d . . . . .
F19 F 1.43901(11) 0.24397(11) 0.21506(7) 0.0328(2) Uani 1 1 d . . . . .
F20 F 1.48876(11) 0.11682(10) 0.40329(7) 0.0321(2) Uani 1 1 d . . . . .
C21 C 1.03638(15) 0.55255(16) 0.11248(11) 0.0236(3) Uani 1 1 d . . . . .
C22 C 0.94347(17) 0.68823(16) 0.07862(11) 0.0244(3) Uani 1 1 d . . . . .
C23 C 0.79396(16) 0.70438(16) 0.06687(10) 0.0235(3) Uani 1 1 d . . . . .
H23 H 0.728284 0.795136 0.042219 0.028 Uiso 1 1 calc R U . . .
C24 C 0.73873(16) 0.58991(16) 0.09057(11) 0.0236(3) Uani 1 1 d . . . . .
C25 C 0.83140(17) 0.45398(16) 0.12625(11) 0.0249(3) Uani 1 1 d . . . . .
C26 C 0.98169(16) 0.43811(16) 0.13558(11) 0.0247(3) Uani 1 1 d . . . . .
H26 H 1.047975 0.347198 0.158195 0.030 Uiso 1 1 calc R U . . .
C27 C 0.9999(2) 0.81496(18) 0.05408(13) 0.0328(4) Uani 1 1 d . . . . .
H27A H 1.063836 0.810144 -0.000202 0.049 Uiso 1 1 calc R U . . .
H27B H 1.055545 0.816738 0.110819 0.049 Uiso 1 1 calc R U . . .
H27C H 0.916750 0.899839 0.035799 0.049 Uiso 1 1 calc R U . . .
C28 C 0.7748(2) 0.32830(18) 0.15156(13) 0.0326(4) Uani 1 1 d . . . . .
H28A H 0.705515 0.337238 0.202689 0.049 Uiso 1 1 calc R U . . .
H28B H 0.857223 0.243758 0.174623 0.049 Uiso 1 1 calc R U . . .
H28C H 0.725008 0.322267 0.093811 0.049 Uiso 1 1 calc R U . . .
C31 C 0.46994(16) 0.71937(17) 0.14744(11) 0.0255(3) Uani 1 1 d . . . . .
C32 C 0.38992(17) 0.85884(18) 0.11524(11) 0.0278(3) Uani 1 1 d . . . . .
C33 C 0.31986(18) 0.93541(17) 0.17827(12) 0.0276(3) Uani 1 1 d . . . . .
C34 C 0.32482(16) 0.87406(17) 0.27773(11) 0.0251(3) Uani 1 1 d . . . . .
C35 C 0.40349(17) 0.73390(17) 0.31029(11) 0.0259(3) Uani 1 1 d . . . . .
C36 C 0.47665(16) 0.65899(16) 0.24742(11) 0.0249(3) Uani 1 1 d . . . . .
F37 F 0.37661(12) 0.92318(12) 0.01966(7) 0.0392(3) Uani 1 1 d . . . . .
F38 F 0.24455(12) 1.06949(11) 0.14198(7) 0.0389(2) Uani 1 1 d . . . . .
F39 F 0.40909(11) 0.66762(10) 0.40482(7) 0.0307(2) Uani 1 1 d . . . . .
F40 F 0.55353(11) 0.52462(10) 0.28406(7) 0.0319(2) Uani 1 1 d . . . . .
C41 C 0.08154(16) 0.91236(16) 0.38269(11) 0.0228(3) Uani 1 1 d . . . . .
C42 C 0.06180(16) 0.83861(15) 0.47647(11) 0.0221(3) Uani 1 1 d . . . . .
C43 C -0.06879(16) 0.80217(15) 0.49039(10) 0.0223(3) Uani 1 1 d . . . . .
H43 H -0.086595 0.755211 0.553683 0.027 Uiso 1 1 calc R U . . .
C44 C -0.17294(16) 0.83194(15) 0.41548(11) 0.0219(3) Uani 1 1 d . . . . .
C45 C -0.15252(16) 0.90388(15) 0.32083(11) 0.0231(3) Uani 1 1 d . . . . .
C46 C -0.02460(17) 0.94400(16) 0.30712(11) 0.0238(3) Uani 1 1 d . . . . .
H46 H -0.008940 0.994499 0.244376 0.029 Uiso 1 1 calc R U . . .
C47 C 0.17448(17) 0.79657(17) 0.56024(11) 0.0270(3) Uani 1 1 d . . . . .
H47A H 0.134007 0.755436 0.620069 0.040 Uiso 1 1 calc R U . . .
H47B H 0.199929 0.878958 0.567456 0.040 Uiso 1 1 calc R U . . .
H47C H 0.262706 0.728007 0.547609 0.040 Uiso 1 1 calc R U . . .
C48 C -0.26546(18) 0.93784(19) 0.23837(11) 0.0295(3) Uani 1 1 d . . . . .
H48A H -0.271140 0.851241 0.224706 0.044 Uiso 1 1 calc R U . . .
H48B H -0.237185 0.996359 0.180343 0.044 Uiso 1 1 calc R U . . .
H48C H -0.361433 0.987997 0.256475 0.044 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
S1 C11 1.7613(16) . ?
S1 C44 1.7819(14) 2_666 ?
S2 C14 1.7634(15) . ?
S2 C21 1.7891(14) . ?
S3 C24 1.7898(14) . ?
S3 C31 1.7717(16) . ?
S4 C34 1.7764(16) . ?
S4 C41 1.7829(14) . ?
C11 C12 1.392(2) . ?
C11 C16 1.388(2) . ?
C12 C13 1.377(2) . ?
C12 F17 1.3426(18) . ?
C13 C14 1.394(2) . ?
C13 F18 1.3453(17) . ?
C14 C15 1.391(2) . ?
C15 C16 1.391(2) . ?
C15 F19 1.3393(18) . ?
C16 F20 1.3359(18) . ?
C21 C22 1.397(2) . ?
C21 C26 1.392(2) . ?
C22 C23 1.394(2) . ?
C22 C27 1.518(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.396(2) . ?
C24 C25 1.401(2) . ?
C25 C26 1.398(2) . ?
C25 C28 1.509(2) . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C31 C32 1.388(2) . ?
C31 C36 1.400(2) . ?
C32 C33 1.384(2) . ?
C32 F37 1.3485(19) . ?
C33 C34 1.396(2) . ?
C33 F38 1.3383(19) . ?
C34 C35 1.390(2) . ?
C35 C36 1.382(2) . ?
C35 F39 1.3446(18) . ?
C36 F40 1.3450(18) . ?
C41 C42 1.404(2) . ?
C41 C46 1.398(2) . ?
C42 C43 1.398(2) . ?
C42 C47 1.509(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.382(2) . ?
C44 C45 1.409(2) . ?
C45 C46 1.393(2) . ?
C45 C48 1.509(2) . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 S1 C44 101.45(7) . 2_666 ?
C14 S2 C21 99.77(7) . . ?
C31 S3 C24 100.77(7) . . ?
C34 S4 C41 100.03(7) . . ?
C12 C11 S1 121.24(12) . . ?
C16 C11 S1 121.47(12) . . ?
C16 C11 C12 117.24(14) . . ?
C13 C12 C11 121.42(14) . . ?
F17 C12 C11 119.81(14) . . ?
F17 C12 C13 118.74(14) . . ?
C12 C13 C14 121.61(14) . . ?
F18 C13 C12 118.87(13) . . ?
F18 C13 C14 119.51(14) . . ?
C13 C14 S2 122.05(12) . . ?
C15 C14 S2 120.88(12) . . ?
C15 C14 C13 117.06(14) . . ?
C16 C15 C14 121.19(14) . . ?
F19 C15 C14 120.16(14) . . ?
F19 C15 C16 118.64(14) . . ?
C11 C16 C15 121.33(14) . . ?
F20 C16 C11 120.65(14) . . ?
F20 C16 C15 117.95(14) . . ?
C22 C21 S2 119.68(11) . . ?
C26 C21 S2 118.83(12) . . ?
C26 C21 C22 121.42(13) . . ?
C21 C22 C27 122.53(14) . . ?
C23 C22 C21 117.33(13) . . ?
C23 C22 C27 120.13(14) . . ?
C22 C23 H23 119.3 . . ?
C22 C23 C24 121.34(14) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 S3 118.43(12) . . ?
C23 C24 C25 121.41(13) . . ?
C25 C24 S3 119.99(11) . . ?
C24 C25 C28 122.51(13) . . ?
C26 C25 C24 116.97(13) . . ?
C26 C25 C28 120.50(15) . . ?
C21 C26 C25 121.49(14) . . ?
C21 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C31 S3 121.77(12) . . ?
C32 C31 C36 116.71(14) . . ?
C36 C31 S3 121.32(12) . . ?
C33 C32 C31 122.07(15) . . ?
F37 C32 C31 119.95(14) . . ?
F37 C32 C33 117.98(15) . . ?
C32 C33 C34 120.99(15) . . ?
F38 C33 C32 118.76(14) . . ?
F38 C33 C34 120.24(14) . . ?
C33 C34 S4 121.26(13) . . ?
C35 C34 S4 121.52(12) . . ?
C35 C34 C33 117.19(14) . . ?
C36 C35 C34 121.57(14) . . ?
F39 C35 C34 120.13(14) . . ?
F39 C35 C36 118.30(14) . . ?
C35 C36 C31 121.43(15) . . ?
F40 C36 C31 120.05(14) . . ?
F40 C36 C35 118.51(14) . . ?
C42 C41 S4 120.31(11) . . ?
C46 C41 S4 119.10(11) . . ?
C46 C41 C42 120.54(13) . . ?
C41 C42 C47 123.17(13) . . ?
C43 C42 C41 117.03(13) . . ?
C43 C42 C47 119.79(13) . . ?
C42 C43 H43 118.8 . . ?
C44 C43 C42 122.43(14) . . ?
C44 C43 H43 118.8 . . ?
C43 C44 S1 123.88(11) . 2_666 ?
C43 C44 C45 120.74(13) . . ?
C45 C44 S1 115.38(11) . 2_666 ?
C44 C45 C48 121.41(13) . . ?
C46 C45 C44 117.08(13) . . ?
C46 C45 C48 121.51(14) . . ?
C41 C46 H46 118.9 . . ?
C45 C46 C41 122.14(14) . . ?
C45 C46 H46 118.9 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C23 H23 F37 0.95 2.71 3.6229(19) 160.9 2_675 yes
C23 H23 F38 0.95 2.70 3.2455(18) 117.4 2_675 yes
C27 H27B F18 0.98 2.71 3.407(2) 128.3 . yes
C27 H27C F38 0.98 2.88 3.403(2) 114.1 2_675 yes
C28 H28A F19 0.98 2.95 3.5979(19) 124.3 1_455 yes
C28 H28A F40 0.98 2.58 3.390(2) 139.6 . yes
C43 H43 S4 0.95 3.31 3.5872(15) 99.5 2_576 yes
C43 H43 F17 0.95 3.09 3.4331(17) 103.2 2_666 yes
C47 H47B S4 0.98 2.93 3.1432(16) 93.1 . yes
C47 H47B F20 0.98 3.02 3.6472(17) 123.3 2_766 yes
C47 H47C F17 0.98 3.14 3.5415(18) 106.0 1_455 yes
C47 H47C F39 0.98 2.56 3.3628(19) 139.7 . yes
C48 H48B F37 0.98 2.98 3.6479(19) 126.6 2_575 yes
C48 H48C S1 0.98 2.78 2.9766(17) 91.7 2_666 yes
C48 H48C F19 0.98 2.71 3.532(2) 141.5 1_365 yes

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
S1 C11 C12 C13 -173.73(11) . . . . ?
S1 C11 C12 F17 4.16(19) . . . . ?
S1 C11 C16 C15 173.40(11) . . . . ?
S1 C11 C16 F20 -3.49(19) . . . . ?
S1 C44 C45 C46 179.61(11) 2_666 . . . ?
S1 C44 C45 C48 0.53(19) 2_666 . . . ?
S2 C14 C15 C16 -178.14(11) . . . . ?
S2 C14 C15 F19 0.60(19) . . . . ?
S2 C21 C22 C23 175.62(11) . . . . ?
S2 C21 C22 C27 -3.8(2) . . . . ?
S2 C21 C26 C25 -177.22(11) . . . . ?
S3 C24 C25 C26 174.15(11) . . . . ?
S3 C24 C25 C28 -4.3(2) . . . . ?
S3 C31 C32 C33 174.95(12) . . . . ?
S3 C31 C32 F37 -3.9(2) . . . . ?
S3 C31 C36 C35 -173.12(11) . . . . ?
S3 C31 C36 F40 5.77(18) . . . . ?
S4 C34 C35 C36 -176.49(11) . . . . ?
S4 C34 C35 F39 3.92(19) . . . . ?
S4 C41 C42 C43 176.15(11) . . . . ?
S4 C41 C42 C47 -4.7(2) . . . . ?
S4 C41 C46 C45 -178.00(12) . . . . ?
C11 C12 C13 C14 -0.5(2) . . . . ?
C11 C12 C13 F18 179.43(13) . . . . ?
C12 C11 C16 C15 -3.9(2) . . . . ?
C12 C11 C16 F20 179.18(12) . . . . ?
C12 C13 C14 S2 177.80(11) . . . . ?
C12 C13 C14 C15 -2.4(2) . . . . ?
C13 C14 C15 C16 2.0(2) . . . . ?
C13 C14 C15 F19 -179.22(12) . . . . ?
C14 S2 C21 C22 120.95(13) . . . . ?
C14 S2 C21 C26 -62.01(13) . . . . ?
C14 C15 C16 C11 1.1(2) . . . . ?
C14 C15 C16 F20 178.11(12) . . . . ?
C16 C11 C12 C13 3.6(2) . . . . ?
C16 C11 C12 F17 -178.50(12) . . . . ?
F17 C12 C13 C14 -178.38(12) . . . . ?
F17 C12 C13 F18 1.5(2) . . . . ?
F18 C13 C14 S2 -2.10(18) . . . . ?
F18 C13 C14 C15 177.71(12) . . . . ?
F19 C15 C16 C11 -177.61(12) . . . . ?
F19 C15 C16 F20 -0.64(19) . . . . ?
C21 S2 C14 C13 -56.94(13) . . . . ?
C21 S2 C14 C15 123.25(12) . . . . ?
C21 C22 C23 C24 1.8(2) . . . . ?
C22 C21 C26 C25 -0.2(2) . . . . ?
C22 C23 C24 S3 -175.81(11) . . . . ?
C22 C23 C24 C25 -0.6(2) . . . . ?
C23 C24 C25 C26 -1.0(2) . . . . ?
C23 C24 C25 C28 -179.42(14) . . . . ?
C24 S3 C31 C32 111.84(13) . . . . ?
C24 S3 C31 C36 -73.49(13) . . . . ?
C24 C25 C26 C21 1.4(2) . . . . ?
C26 C21 C22 C23 -1.3(2) . . . . ?
C26 C21 C22 C27 179.22(15) . . . . ?
C27 C22 C23 C24 -178.79(14) . . . . ?
C28 C25 C26 C21 179.87(14) . . . . ?
C31 S3 C24 C23 -66.43(13) . . . . ?
C31 S3 C24 C25 118.32(13) . . . . ?
C31 C32 C33 C34 -1.1(2) . . . . ?
C31 C32 C33 F38 -179.96(14) . . . . ?
C32 C31 C36 C35 1.8(2) . . . . ?
C32 C31 C36 F40 -179.29(13) . . . . ?
C32 C33 C34 S4 178.34(12) . . . . ?
C32 C33 C34 C35 0.4(2) . . . . ?
C33 C34 C35 C36 1.5(2) . . . . ?
C33 C34 C35 F39 -178.12(13) . . . . ?
C34 S4 C41 C42 116.16(13) . . . . ?
C34 S4 C41 C46 -66.21(14) . . . . ?
C34 C35 C36 C31 -2.6(2) . . . . ?
C34 C35 C36 F40 178.46(12) . . . . ?
C36 C31 C32 C33 0.0(2) . . . . ?
C36 C31 C32 F37 -178.85(13) . . . . ?
F37 C32 C33 C34 177.78(14) . . . . ?
F37 C32 C33 F38 -1.0(2) . . . . ?
F38 C33 C34 S4 -2.8(2) . . . . ?
F38 C33 C34 C35 179.19(13) . . . . ?
F39 C35 C36 C31 176.96(12) . . . . ?
F39 C35 C36 F40 -1.95(19) . . . . ?
C41 S4 C34 C33 104.67(13) . . . . ?
C41 S4 C34 C35 -77.45(13) . . . . ?
C41 C42 C43 C44 2.3(2) . . . . ?
C42 C41 C46 C45 -0.4(2) . . . . ?
C42 C43 C44 S1 178.50(12) . . . 2_666 ?
C42 C43 C44 C45 -1.3(2) . . . . ?
C43 C44 C45 C46 -0.6(2) . . . . ?
C43 C44 C45 C48 -179.68(15) . . . . ?
C44 S1 C11 C12 74.95(13) 2_666 . . . ?
C44 S1 C11 C16 -102.28(12) 2_666 . . . ?
C44 C45 C46 C41 1.4(2) . . . . ?
C46 C41 C42 C43 -1.5(2) . . . . ?
C46 C41 C42 C47 177.66(14) . . . . ?
C47 C42 C43 C44 -176.87(14) . . . . ?
C48 C45 C46 C41 -179.52(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform'
####################################################################### 
# 
# 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_1a-DMF
_database_code_depnum_ccdc_archive 'CCDC 2175105'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWM
_nottingham_internal_coll_number 19184
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   09/05/2022
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 09/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 09/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 24/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 24/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 24/05/2022
_refine_special_details          
;A solvent mask was calculated and 240 electrons were 
found in a volume of 1102Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
2[C3H7NO] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.,SQUEEZE
;
_audit_creation_date             2022-05-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H16 F16 S8'
_chemical_formula_sum            'C54 H30 F16 N2 O2 S8'
_chemical_formula_weight         1299.28
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0160 0.0100 '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 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0071 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1190 0.1170 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_H-M_alt        'P 42/n'
_space_group_name_Hall           '-P 4bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -z-1/2'

_cell_length_a                   19.8473(2)
_cell_length_b                   19.8473(2)
_cell_length_c                   13.19340(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5197.08(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.88788643132704
_cell_measurement_theta_min      1.3988005227080926
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.961
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9854052353473588
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.1.018: AIMLESS, version 0.7.7 : 23/04/21
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            73694
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.339
_diffrn_reflns_theta_min         1.406
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5194
_reflns_number_total             6454
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.dev (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 3.10.dev0 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0529
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0858P)²+2.4346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1490
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C22B(H22B), C23B(H23B),
 C25B(H25B), C26B(H26B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1A S 0.40799(3) 0.72168(3) 0.08862(4) 0.02256(14) Uani 1 1 d . . . . .
S2A S 0.62973(3) 0.49913(3) 0.00553(4) 0.02665(16) Uani 1 1 d . . . . .
C11A C 0.43814(12) 0.76350(11) 0.19765(16) 0.0204(4) Uani 1 1 d . . . . .
C12A C 0.50544(12) 0.77823(12) 0.21792(16) 0.0219(4) Uani 1 1 d . . . . .
C13A C 0.52469(12) 0.81093(12) 0.30605(17) 0.0224(5) Uani 1 1 d . . . . .
C14A C 0.47797(12) 0.83429(11) 0.37683(16) 0.0220(4) Uani 1 1 d . . . . .
C15A C 0.41049(12) 0.82125(11) 0.35470(17) 0.0228(5) Uani 1 1 d . . . . .
C16A C 0.39174(12) 0.78598(11) 0.26914(17) 0.0218(4) Uani 1 1 d . . . . .
F17A F 0.55387(7) 0.75874(7) 0.15411(10) 0.0271(3) Uani 1 1 d . . . . .
F18A F 0.59070(7) 0.81828(7) 0.32352(10) 0.0282(3) Uani 1 1 d . . . . .
F19A F 0.36227(7) 0.84076(7) 0.41913(11) 0.0300(3) Uani 1 1 d . . . . .
F20A F 0.32571(7) 0.77312(7) 0.25521(11) 0.0285(3) Uani 1 1 d . . . . .
C21A C 0.56671(12) 0.55942(12) 0.03588(16) 0.0218(4) Uani 1 1 d . . . . .
C22A C 0.53651(12) 0.56503(12) 0.13097(16) 0.0230(5) Uani 1 1 d . . . . .
H22A H 0.549192 0.535394 0.184189 0.028 Uiso 1 1 calc R U . . .
C23A C 0.48776(12) 0.61415(12) 0.14764(16) 0.0231(5) Uani 1 1 d . . . . .
H23A H 0.466919 0.617876 0.212219 0.028 Uiso 1 1 calc R U . . .
C24A C 0.46955(12) 0.65767(12) 0.07021(16) 0.0211(4) Uani 1 1 d . . . . .
C25A C 0.49762(13) 0.65032(12) -0.02600(17) 0.0248(5) Uani 1 1 d . . . . .
H25A H 0.483734 0.679008 -0.079718 0.030 Uiso 1 1 calc R U . . .
C26A C 0.54592(13) 0.60100(13) -0.04323(17) 0.0272(5) Uani 1 1 d . . . . .
H26A H 0.564767 0.595616 -0.108926 0.033 Uiso 1 1 calc R U . . .
S1B S 0.41538(3) 0.71170(3) 0.57800(4) 0.02603(15) Uani 1 1 d . . . . .
S2B S 0.47945(3) 0.86759(3) 0.98427(4) 0.02567(15) Uani 1 1 d . . . . .
C11B C 0.47772(12) 0.64929(12) 0.56810(16) 0.0226(5) Uani 1 1 d . . . . .
C12B C 0.51147(13) 0.63941(12) 0.47698(17) 0.0261(5) Uani 1 1 d . . . . .
C13B C 0.55776(13) 0.58840(13) 0.46431(16) 0.0252(5) Uani 1 1 d . . . . .
C14B C 0.57359(11) 0.54362(12) 0.54146(16) 0.0210(4) Uani 1 1 d . . . . .
C15B C 0.53845(12) 0.55232(12) 0.63202(16) 0.0233(5) Uani 1 1 d . . . . .
C16B C 0.49225(12) 0.60340(12) 0.64467(16) 0.0227(5) Uani 1 1 d . . . . .
F17B F 0.49851(9) 0.67982(8) 0.39792(11) 0.0401(4) Uani 1 1 d . . . . .
F18B F 0.58869(9) 0.58235(8) 0.37382(10) 0.0384(4) Uani 1 1 d . . . . .
F19B F 0.54751(8) 0.50870(8) 0.70862(11) 0.0326(3) Uani 1 1 d . . . . .
F20B F 0.45908(8) 0.60704(8) 0.73319(10) 0.0307(3) Uani 1 1 d . . . . .
C21B C 0.46629(12) 0.82708(11) 0.86584(16) 0.0222(4) Uani 1 1 d . . . . .
C22B C 0.51906(12) 0.79815(13) 0.81128(18) 0.0269(5) Uani 1 1 d . . . . .
H22B H 0.564132 0.802706 0.834518 0.032 Uiso 1 1 calc R U . . .
C23B C 0.50547(12) 0.76252(13) 0.72252(17) 0.0262(5) Uani 1 1 d . . . . .
H23B H 0.541270 0.743721 0.683998 0.031 Uiso 1 1 calc R U . . .
C24B C 0.43885(12) 0.75468(11) 0.69069(16) 0.0216(4) Uani 1 1 d . . . . .
C25B C 0.38641(12) 0.78421(12) 0.74513(18) 0.0255(5) Uani 1 1 d . . . . .
H25B H 0.341232 0.779331 0.722512 0.031 Uiso 1 1 calc R U . . .
C26B C 0.40023(13) 0.82079(13) 0.83250(18) 0.0265(5) Uani 1 1 d . . . . .
H26B H 0.364614 0.841409 0.869273 0.032 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
S1A C11A 1.765(2) . ?
S1A C24A 1.779(2) . ?
S2A C14A 1.759(2) 8_756 ?
S2A C21A 1.777(2) . ?
C11A C12A 1.393(3) . ?
C11A C16A 1.392(3) . ?
C12A C13A 1.385(3) . ?
C12A F17A 1.335(3) . ?
C13A C14A 1.395(3) . ?
C13A F18A 1.338(3) . ?
C14A C15A 1.395(3) . ?
C15A C16A 1.379(3) . ?
C15A F19A 1.337(3) . ?
C16A F20A 1.348(3) . ?
C21A C22A 1.395(3) . ?
C21A C26A 1.393(3) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.391(3) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.386(3) . ?
C24A C25A 1.394(3) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.389(3) . ?
C26A H26A 0.9500 . ?
S1B C11B 1.756(2) . ?
S1B C24B 1.776(2) . ?
S2B C14B 1.761(2) 6_577 ?
S2B C21B 1.776(2) . ?
C11B C12B 1.390(3) . ?
C11B C16B 1.390(3) . ?
C12B C13B 1.377(3) . ?
C12B F17B 1.341(3) . ?
C13B C14B 1.387(3) . ?
C13B F18B 1.348(3) . ?
C14B C15B 1.394(3) . ?
C15B C16B 1.377(3) . ?
C15B F19B 1.343(2) . ?
C16B F20B 1.343(2) . ?
C21B C22B 1.394(3) . ?
C21B C26B 1.389(3) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.394(3) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.396(3) . ?
C24B C25B 1.394(3) . ?
C25B H25B 0.9500 . ?
C25B C26B 1.390(3) . ?
C26B H26B 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
C11A S1A C24A 102.37(10) . . ?
C14A S2A C21A 104.34(10) 8_756 . ?
C12A C11A S1A 125.46(17) . . ?
C16A C11A S1A 118.60(17) . . ?
C16A C11A C12A 115.9(2) . . ?
C13A C12A C11A 121.6(2) . . ?
F17A C12A C11A 120.6(2) . . ?
F17A C12A C13A 117.8(2) . . ?
C12A C13A C14A 122.3(2) . . ?
F18A C13A C12A 117.7(2) . . ?
F18A C13A C14A 119.9(2) . . ?
C13A C14A S2A 124.52(18) . 6_576 ?
C15A C14A S2A 119.28(17) . 6_576 ?
C15A C14A C13A 115.9(2) . . ?
C16A C15A C14A 121.6(2) . . ?
F19A C15A C14A 120.0(2) . . ?
F19A C15A C16A 118.3(2) . . ?
C15A C16A C11A 122.6(2) . . ?
F20A C16A C11A 119.4(2) . . ?
F20A C16A C15A 118.0(2) . . ?
C22A C21A S2A 123.99(18) . . ?
C26A C21A S2A 116.02(17) . . ?
C26A C21A C22A 119.9(2) . . ?
C21A C22A H22A 120.1 . . ?
C23A C22A C21A 119.8(2) . . ?
C23A C22A H22A 120.1 . . ?
C22A C23A H23A 119.9 . . ?
C24A C23A C22A 120.1(2) . . ?
C24A C23A H23A 119.9 . . ?
C23A C24A S1A 121.57(17) . . ?
C23A C24A C25A 120.1(2) . . ?
C25A C24A S1A 118.26(17) . . ?
C24A C25A H25A 120.0 . . ?
C26A C25A C24A 119.9(2) . . ?
C26A C25A H25A 120.0 . . ?
C21A C26A H26A 120.0 . . ?
C25A C26A C21A 120.0(2) . . ?
C25A C26A H26A 120.0 . . ?
C11B S1B C24B 102.50(11) . . ?
C14B S2B C21B 103.70(11) 6_577 . ?
C12B C11B S1B 120.23(18) . . ?
C12B C11B C16B 115.9(2) . . ?
C16B C11B S1B 123.65(18) . . ?
C13B C12B C11B 122.0(2) . . ?
F17B C12B C11B 119.7(2) . . ?
F17B C12B C13B 118.2(2) . . ?
C12B C13B C14B 122.2(2) . . ?
F18B C13B C12B 118.5(2) . . ?
F18B C13B C14B 119.3(2) . . ?
C13B C14B S2B 118.17(17) . 8_757 ?
C13B C14B C15B 115.9(2) . . ?
C15B C14B S2B 125.90(18) . 8_757 ?
C16B C15B C14B 121.9(2) . . ?
F19B C15B C14B 119.9(2) . . ?
F19B C15B C16B 118.2(2) . . ?
C15B C16B C11B 122.2(2) . . ?
F20B C16B C11B 119.7(2) . . ?
F20B C16B C15B 118.1(2) . . ?
C22B C21B S2B 122.00(18) . . ?
C26B C21B S2B 117.27(18) . . ?
C26B C21B C22B 120.6(2) . . ?
C21B C22B H22B 120.1 . . ?
C23B C22B C21B 119.8(2) . . ?
C23B C22B H22B 120.1 . . ?
C22B C23B H23B 120.3 . . ?
C22B C23B C24B 119.5(2) . . ?
C24B C23B H23B 120.3 . . ?
C23B C24B S1B 123.62(18) . . ?
C25B C24B S1B 115.94(18) . . ?
C25B C24B C23B 120.4(2) . . ?
C24B C25B H25B 120.0 . . ?
C26B C25B C24B 120.0(2) . . ?
C26B C25B H25B 120.0 . . ?
C21B C26B C25B 119.7(2) . . ?
C21B C26B H26B 120.1 . . ?
C25B C26B H26B 120.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22A H22A F18B 0.95 2.78 3.385(3) 122.1 . yes
C22A H22A F19B 0.95 2.54 3.066(3) 115.1 5_666 yes
C22A H22A F20B 0.95 3.03 3.858(3) 145.9 5_666 yes
C23A H23A F17B 0.95 2.81 3.556(3) 135.9 . yes
C23A H23A F18B 0.95 3.30 3.649(3) 104.1 . yes
C23A H23A F19B 0.95 2.74 3.167(3) 108.5 5_666 yes
C25A H25A F20B 0.95 2.89 3.379(3) 112.9 1_554 yes
C26A H26A F19B 0.95 2.98 3.752(3) 139.2 1_554 yes
C26A H26A F20B 0.95 2.96 3.418(3) 110.7 1_554 yes
C25B H25B S1A 0.95 3.35 3.860(3) 116.1 2_655 yes
C25B H25B F20A 0.95 2.52 3.136(3) 122.4 4_465 yes
C25B H25B F20A 0.95 2.49 3.274(3) 140.3 2_655 yes
C26B H26B F20A 0.95 3.14 3.590(3) 111.1 2_655 yes
C26B H26B F17B 0.95 3.26 3.964(3) 132.2 2_655 yes

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
S1A C11A C12A C13A -179.55(18) . . . . ?
S1A C11A C12A F17A -2.2(3) . . . . ?
S1A C11A C16A C15A -177.59(18) . . . . ?
S1A C11A C16A F20A 2.4(3) . . . . ?
S1A C24A C25A C26A 179.87(19) . . . . ?
S2A C14A C15A C16A -172.22(18) 6_576 . . . ?
S2A C14A C15A F19A 5.1(3) 6_576 . . . ?
S2A C21A C22A C23A 179.68(18) . . . . ?
S2A C21A C26A C25A -178.97(19) . . . . ?
C11A S1A C24A C23A 52.4(2) . . . . ?
C11A S1A C24A C25A -130.11(19) . . . . ?
C11A C12A C13A C14A -3.6(4) . . . . ?
C11A C12A C13A F18A 174.7(2) . . . . ?
C12A C11A C16A C15A 0.5(3) . . . . ?
C12A C11A C16A F20A -179.43(19) . . . . ?
C12A C13A C14A S2A 174.86(18) . . . 6_576 ?
C12A C13A C14A C15A 1.5(3) . . . . ?
C13A C14A C15A C16A 1.5(3) . . . . ?
C13A C14A C15A F19A 178.8(2) . . . . ?
C14A S2A C21A C22A -23.2(2) 8_756 . . . ?
C14A S2A C21A C26A 159.21(19) 8_756 . . . ?
C14A C15A C16A C11A -2.6(3) . . . . ?
C14A C15A C16A F20A 177.4(2) . . . . ?
C16A C11A C12A C13A 2.5(3) . . . . ?
C16A C11A C12A F17A 179.9(2) . . . . ?
F17A C12A C13A C14A 178.9(2) . . . . ?
F17A C12A C13A F18A -2.8(3) . . . . ?
F18A C13A C14A S2A -3.4(3) . . . 6_576 ?
F18A C13A C14A C15A -176.7(2) . . . . ?
F19A C15A C16A C11A -180.0(2) . . . . ?
F19A C15A C16A F20A 0.0(3) . . . . ?
C21A C22A C23A C24A -0.4(4) . . . . ?
C22A C21A C26A C25A 3.3(4) . . . . ?
C22A C23A C24A S1A -179.43(18) . . . . ?
C22A C23A C24A C25A 3.1(4) . . . . ?
C23A C24A C25A C26A -2.6(4) . . . . ?
C24A S1A C11A C12A 40.3(2) . . . . ?
C24A S1A C11A C16A -141.73(18) . . . . ?
C24A C25A C26A C21A -0.6(4) . . . . ?
C26A C21A C22A C23A -2.8(4) . . . . ?
S1B C11B C12B C13B -176.0(2) . . . . ?
S1B C11B C12B F17B 3.1(3) . . . . ?
S1B C11B C16B C15B 175.70(19) . . . . ?
S1B C11B C16B F20B -2.2(3) . . . . ?
S1B C24B C25B C26B -177.89(19) . . . . ?
S2B C14B C15B C16B -178.70(19) 8_757 . . . ?
S2B C14B C15B F19B -1.1(3) 8_757 . . . ?
S2B C21B C22B C23B 175.16(19) . . . . ?
S2B C21B C26B C25B -174.15(19) . . . . ?
C11B S1B C24B C23B 32.4(2) . . . . ?
C11B S1B C24B C25B -150.84(18) . . . . ?
C11B C12B C13B C14B 0.1(4) . . . . ?
C11B C12B C13B F18B -179.6(2) . . . . ?
C12B C11B C16B C15B 1.6(4) . . . . ?
C12B C11B C16B F20B -176.3(2) . . . . ?
C12B C13B C14B S2B 178.8(2) . . . 8_757 ?
C12B C13B C14B C15B 1.6(4) . . . . ?
C13B C14B C15B C16B -1.7(3) . . . . ?
C13B C14B C15B F19B 175.9(2) . . . . ?
C14B S2B C21B C22B 53.0(2) 6_577 . . . ?
C14B S2B C21B C26B -131.57(19) 6_577 . . . ?
C14B C15B C16B C11B 0.1(4) . . . . ?
C14B C15B C16B F20B 178.0(2) . . . . ?
C16B C11B C12B C13B -1.7(4) . . . . ?
C16B C11B C12B F17B 177.5(2) . . . . ?
F17B C12B C13B C14B -179.1(2) . . . . ?
F17B C12B C13B F18B 1.2(4) . . . . ?
F18B C13B C14B S2B -1.4(3) . . . 8_757 ?
F18B C13B C14B C15B -178.7(2) . . . . ?
F19B C15B C16B C11B -177.5(2) . . . . ?
F19B C15B C16B F20B 0.4(3) . . . . ?
C21B C22B C23B C24B -1.7(4) . . . . ?
C22B C21B C26B C25B 1.3(4) . . . . ?
C22B C23B C24B S1B 178.86(19) . . . . ?
C22B C23B C24B C25B 2.3(4) . . . . ?
C23B C24B C25B C26B -1.0(4) . . . . ?
C24B S1B C11B C12B -131.3(2) . . . . ?
C24B S1B C11B C16B 54.9(2) . . . . ?
C24B C25B C26B C21B -0.8(4) . . . . ?
C26B C21B C22B C23B -0.1(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.250 -0.750 480.7 120.4 '4 C3H7NO'
2 0.250 0.750 0.993 34.6 0.0 ?
3 0.250 0.750 0.493 34.6 0.0 ?
4 0.750 0.750 -0.652 480.7 118.4 '4 C3H7NO'
5 0.750 0.250 0.007 34.6 0.0 ?
6 0.750 0.250 0.507 34.6 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethylformamide'
####################################################################### 
# 
# 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_1a-CHCl3
_database_code_depnum_ccdc_archive 'CCDC 2175102'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWC
_nottingham_internal_coll_number 18979
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time 30.00
_nottingham_internal_coll_frame_width 0.50
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   16/03/2021
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 12/05/2021
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 12/05/2021
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 13/05/2021
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 13/05/2021
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date ?
_refine_special_details          
;Crystals of the macrocycle diffracted weakly with a resolution limit
 of 1.35 A, despite the use of an intense rotating anode copper source.
 The data used in the refinement was truncated to a resolution of 1.35 A
 consequently resulting in a very low data-parameter ratio of 2.65. To
 aid refinement of the structure with such a low data to parameter ratio
 restraints were applied to the geometries and anisotropic displacement
 parameters of all atoms in the structure.

 Additional weak diffraction peaks were observed inbetween the main peaks
 along both the a and b axes. The peaks were too weak to extract any
 information or use for indexing a large unit cell of a superstructure.
 The origin of the potential superstructure is likely to be either
 disorder in the chloroform solvent residues or the the disorder of the
 phenyl and tetrafluorophenyl rings. 

 Occupational disorder is observed for the phenyl and tetrafluorophenyl
 rings of the macrocycle: each ring is modelled with as having half
 occupancy of each such moiety. The chloroform residue is modelled with
 its occupancy fixed at a value of 0.5.

 Geometric similarity restraints were applied the geometries of all
 chemically similar 1,2 and 1,3 distances in the structure (SADI, SAME).
 The phenyl and tetrafluorophenyl moieties were restrained to have
 planar geometries (FLAT). The three C-Cl bond lengths of the
 chloroform residue were restrained to have target distances taken from
 the Olex2 FragmentDB (DFIX).

 Rigid bond and similarity restraints were applied to the anisotropic
 displacement parameters of all atoms in the structure (RIGU, SIMU).,Evidence of a weak super lattice in the diffraction pattern.
;
_vrf_PLAT082_1a-CHCl3            
;
PROBLEM: High R1 Value ..................................       0.18 Report
RESPONSE:
 The crystal diffracted weakly (I/sig 13.1) and had a diffraction resolution
 limit of 1.35 A, likely as a result of major disorder in the structure.
;
_vrf_PLAT084_1a-CHCl3            
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.48 Report
RESPONSE:
 The crystal diffracted weakly (I/sig 13.1) and had a diffraction resolution
 limit of 1.35 A, likely as a result of major disorder in the structure.
;
_vrf_PLAT088_1a-CHCl3            
;
PROBLEM: Poor Data / Parameter Ratio ....................       2.65 Note  
RESPONSE:
 The crystal of the disordered macrocycle had a diffraction resolution
 limit of 1.35 A depsite use of a high-intensity rotating anode source.
 Restraints were applied to the geometries and anisotropic displacement
 parameters of all atoms in the structure to aid refinement with a low
 data to parameter ratio.
;
_vrf_PLAT340_1a-CHCl3            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0375 Ang.  
RESPONSE:
 The crystal diffracted weakly (I/sig 13.1) and had a diffraction resolution
 limit of 1.35 A, likely as a result of major disorder in the structure.
 Similarity restraints were applied to all chemically similar 1,2 and 1,3
 distances in the structure to aid refinement of a chemically sensible model.
;
_vrf_THETM01_1a-CHCl3            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:
 The crystal of the disordered macrocycle had a diffraction resolution
 limit of 1.35 A depsite use of a high-intensity rotating anode source.
;
_audit_creation_date             2021-05-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H16 F16 S8, C H Cl3'
_chemical_formula_sum            'C49 H17 Cl3 F16 S8'
_chemical_formula_weight         1272.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         C48H16F16S8
_chemical_oxdiff_usercomment     'OATSWC #18979 MM-755 AT/SW Fomblin micromount'
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'
Cl Cl 0.3639 0.7018 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.7916(16)
_cell_length_b                   13.818(4)
_cell_length_c                   15.064(4)
_cell_angle_alpha                78.57(2)
_cell_angle_beta                 81.39(2)
_cell_angle_gamma                82.79(2)
_cell_volume                     1363.3(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1379
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      44.2960
_cell_measurement_theta_min      3.9770
_shelx_estimated_absorpt_T_max   0.864
_shelx_estimated_absorpt_T_min   0.257
_exptl_absorpt_coefficient_mu    5.198
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             634
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0145
0 1 0 0.0145
0 3 5 0.0145
0 -3 -5 0.0145
-4 -2 -3 0.1546
4 1 3 0.1917
0 -1 5 0.0144
0 1 -5 0.0144

_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.029
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0004 -1.0003 0.0122 0.0125 0.1136 -0.0088
-0.0004 1.0003 -0.0122 -0.0125 -0.1136 0.0088
0.0014 3.0667 4.9824 -0.5405 -0.1877 0.0551
-0.0014 -3.0667 -4.9824 0.5405 0.1877 -0.0551
-4.0078 -2.0246 -2.9890 0.2511 0.1216 0.8859
4.0082 1.0243 3.0012 -0.2386 -0.0080 -0.8947
0.0032 -0.9346 5.0311 -0.4906 0.2666 0.0199
-0.0032 0.9346 -5.0311 0.4906 -0.2666 -0.0199

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5179
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        34.815
_diffrn_reflns_theta_max         34.815
_diffrn_reflns_theta_min         4.031
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS3 R 200K Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     12.00 122.00   0.50   30.00    --   34.70  52.00  26.76  220
  2  ω     13.00 108.00   0.50   30.00    --   34.70  69.00 -56.93  190
  3  ω      8.00  53.00   0.50   30.00    --   34.70  71.00 124.05   90
  4  ω     -2.00  56.00   0.50   30.00    --   34.70 -82.00 -60.00  116
  5  ω    -16.00  56.00   0.50   30.00    --   34.70 -82.00-150.00  144
  6  ω     -1.00  68.00   0.50   30.00    --   34.70 -82.00  30.00  138
  7  ω    -25.00  67.00   0.50   30.00    --   34.70 -82.00 150.00  184
  8  ω      4.00  68.00   0.50   30.00    --   34.70 -82.00  60.00  128
  9  ω    -17.00  63.00   0.50   30.00    --   34.70 -77.00   0.00  160
 10  ω     15.00 110.00   0.50   30.00    --   34.70  38.00-120.00  190
 11  ω    -42.00  49.00   0.50   30.00    --   34.70 -77.00 120.00  182
 12  ω    -22.00  68.00   0.50   30.00    --   34.70 -82.00-120.00  180
 13  ω     12.00  99.00   0.50   30.00    --   34.70  38.00 150.00  174
 14  ω    -46.00  47.00   0.50   30.00    --   34.70 -57.00 -60.00  186
 15  ω      9.00  66.00   0.50   30.00    --   34.70  68.00  47.54  114
 16  ω      9.00  98.00   0.50   30.00    --   34.70  69.00 142.03  178
 17  ω      8.00  46.00   0.50   30.00    --   34.70  72.00 -17.44   76
 18  ω     90.00 121.00   0.50   30.00    --   34.70  72.00 -17.44   62
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'XtalLAB PRO MM007, PILATUS3 R 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0188819000
_diffrn_orient_matrix_UB_12      -0.0136573000
_diffrn_orient_matrix_UB_13      -0.1000707000
_diffrn_orient_matrix_UB_21      0.0029754000
_diffrn_orient_matrix_UB_22      -0.1131501000
_diffrn_orient_matrix_UB_23      0.0319655000
_diffrn_orient_matrix_UB_31      -0.2297537000
_diffrn_orient_matrix_UB_32      0.0087609000
_diffrn_orient_matrix_UB_33      0.0057373000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'rotating anode'
_diffrn_source_type              'MicroMax 007 HF'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                812
_reflns_number_total             1148
_reflns_odcompleteness_completeness 96.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     44.45
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.287
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         1148
_refine_ls_number_restraints     1164
_refine_ls_R_factor_all          0.2063
_refine_ls_R_factor_gt           0.1755
_refine_ls_restrained_S_all      1.608
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4535
_refine_ls_wR_factor_ref         0.4768
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1S-Cl4S = C1S-Cl2S = C1S-Cl3S
 1.78 with sigma of 0.02
 Cl2S-Cl3S \\sim Cl3S-Cl4S \\sim Cl4S-Cl2S
 with sigma of 0.02
 S1-C11 \\sim S1_$1-C44 \\sim S2-C14 \\sim S2-C21 \\sim S3-C24 \\sim S3-C31
\\sim S4-C34 \\sim S4-C41 \\sim S1-
 C44_$1 \\sim S1-C11 \\sim S2-C14 \\sim S2-C21 \\sim S3-C24 \\sim S3-C31 \\sim
S4-C34 \\sim S4-C41
 with sigma of 0.02
 S1-C12 \\sim S1-C16 \\sim S2-C22 \\sim S2-C26 \\sim S2-C13 \\sim S2-C15 \\sim
S3-C23 \\sim S3-C25 \\sim S3-
 C32 \\sim S3-C36 \\sim S4-C33 \\sim S4-C35 \\sim S4-C42 \\sim S4-C46 \\sim
S1-C45_$1 \\sim S1-C43_$1
 with sigma of 0.02
3. Restrained planarity
 C41, C42, C43, C44, C45, C46, F47, F48, F49, F50
 with sigma of 0.1
 C21, C22, C23, C24, C25, C26, F27, F28, F29, F30
 with sigma of 0.1
 C11, C12, C13, C14, C15, C16, F17, F18, F19, F20
 with sigma of 0.1
 C31, C32, C33, C34, C35, C36, F37, F38, F39, F40
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{C11, C16, C15, C14, C13, C12, F20, F19, F18, F17} sigma for 1-2: 0.02, 1-3:
0.04
as in
{C11, C12, C13, C14, C15, C16, F17, F18, F19, F20}
{C11, C16, C15, C14, C13, C12, F20, F19, F18, F17} sigma for 1-2: 0.02, 1-3:
0.04
{C11, C12, C13, C14, C15, C16, F17, F18, F19, F20} sigma for 1-2: 0.02, 1-3:
0.04
as in
{C21, C22, C23, C24, C25, C26, F27, F28, F29, F30}
{C11, C12, C13, C14, C15, C16, F17, F18, F19, F20} sigma for 1-2: 0.02, 1-3:
0.04
{C11, C16, C15, C14, C13, C12, F20, F19, F18, F17} sigma for 1-2: 0.02, 1-3:
0.04
as in
{C31, C32, C33, C34, C35, C36, F37, F38, F39, F40}
{C11, C12, C13, C14, C15, C16, F17, F18, F19, F20} sigma for 1-2: 0.02, 1-3:
0.04
{C11, C16, C15, C14, C13, C12, F20, F19, F18, F17} sigma for 1-2: 0.02, 1-3:
0.04
as in
{C41, C42, C43, C44, C45, C46, F47, F48, F49, F50}
7. Others
 Fixed Sof: H12(0.5) H13(0.5) H15(0.5) H16(0.5) F17(0.5) F18(0.5) F19(0.5)
 F20(0.5) H22(0.5) H23(0.5) H25(0.5) H26(0.5) F27(0.5) F28(0.5) F29(0.5)
 F30(0.5) H32(0.5) H33(0.5) H35(0.5) H36(0.5) F37(0.5) F38(0.5) F39(0.5)
 F40(0.5) H42(0.5) H43(0.5) H45(0.5) H46(0.5) F47(0.5) F48(0.5) F49(0.5)
 F50(0.5) C1S(0.5) H1S(0.5) Cl2S(0.5) Cl3S(0.5) Cl4S(0.5)
8.a Ternary CH refined with riding coordinates:
 C1S(H1S)
8.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45),
  C46(H46)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1 S -0.5017(17) 0.2680(11) -0.1116(8) 0.155(7) Uani 1 1 d D U . . .
S2 S -0.3514(16) -0.0707(9) 0.2304(7) 0.118(5) Uani 1 1 d D U . . .
S3 S -0.3707(17) 0.1919(8) 0.5338(7) 0.120(5) Uani 1 1 d D U . . .
S4 S -0.3423(16) 0.6354(9) 0.3258(8) 0.133(6) Uani 1 1 d D U . . .
C11 C -0.450(3) 0.172(2) -0.0191(18) 0.123(12) Uani 1 1 d D U . . .
C12 C -0.263(4) 0.1489(19) 0.0096(17) 0.131(14) Uani 1 1 d D U . . .
H12 H -0.152882 0.183552 -0.020972 0.157 Uiso 0.5 1 calc R U P A 2
C13 C -0.242(4) 0.0737(18) 0.0847(16) 0.123(13) Uani 1 1 d D U . . .
H13 H -0.112893 0.057468 0.103333 0.148 Uiso 0.5 1 calc R U P B 2
C14 C -0.391(3) 0.022(2) 0.1335(19) 0.112(11) Uani 1 1 d D U . . .
C15 C -0.572(4) 0.048(2) 0.1041(19) 0.117(12) Uani 1 1 d D U . . .
H15 H -0.680914 0.012755 0.136010 0.140 Uiso 0.5 1 calc R U P C 2
C16 C -0.608(4) 0.121(2) 0.031(2) 0.125(13) Uani 1 1 d D U . . .
H16 H -0.739493 0.137800 0.014194 0.150 Uiso 0.5 1 calc R U P D 2
F17 F -0.108(6) 0.200(4) -0.024(3) 0.21(3) Uani 0.5 1 d D U P E 1
F18 F -0.065(5) 0.050(3) 0.116(3) 0.16(2) Uani 0.5 1 d D U P F 1
F19 F -0.724(5) -0.005(3) 0.144(3) 0.17(2) Uani 0.5 1 d D U P G 1
F20 F -0.784(4) 0.140(3) -0.001(2) 0.138(17) Uani 0.5 1 d D U P H 1
C21 C -0.359(3) 0.0055(18) 0.3128(17) 0.098(10) Uani 1 1 d D U . . .
C22 C -0.183(4) 0.0183(17) 0.3438(15) 0.108(12) Uani 1 1 d D U . . .
H22 H -0.057467 -0.011534 0.319872 0.130 Uiso 0.5 1 calc R U P I 1
C23 C -0.195(4) 0.0753(17) 0.4102(16) 0.106(11) Uani 1 1 d D U . . .
H23 H -0.073906 0.084213 0.430553 0.127 Uiso 0.5 1 calc R U P J 1
C24 C -0.367(3) 0.120(2) 0.448(2) 0.108(10) Uani 1 1 d D U . . .
C25 C -0.533(4) 0.106(2) 0.415(2) 0.115(12) Uani 1 1 d D U . . .
H25 H -0.656623 0.138454 0.438208 0.138 Uiso 0.5 1 calc R U P K 1
C26 C -0.539(4) 0.048(2) 0.351(2) 0.114(12) Uani 1 1 d D U . . .
H26 H -0.662301 0.037022 0.333564 0.137 Uiso 0.5 1 calc R U P L 1
F27 F -0.007(4) -0.023(3) 0.310(3) 0.129(15) Uani 0.5 1 d D U P M 2
F28 F -0.024(5) 0.088(3) 0.439(2) 0.111(13) Uani 0.5 1 d D U P N 2
F29 F -0.708(5) 0.149(3) 0.449(3) 0.135(15) Uani 0.5 1 d D U P O 2
F30 F -0.711(4) 0.037(3) 0.323(3) 0.111(13) Uani 0.5 1 d D U P P 2
C31 C -0.357(3) 0.3144(18) 0.4712(19) 0.107(10) Uani 1 1 d D U . . .
C32 C -0.183(4) 0.3598(16) 0.4596(17) 0.111(12) Uani 1 1 d D U . . .
H32 H -0.067233 0.324699 0.483636 0.134 Uiso 0.5 1 calc R U P Q 2
C33 C -0.176(4) 0.4571(15) 0.4127(18) 0.109(12) Uani 1 1 d D U . . .
H33 H -0.056526 0.487923 0.407214 0.130 Uiso 0.5 1 calc R U P R 2
C34 C -0.333(3) 0.5085(19) 0.375(2) 0.111(11) Uani 1 1 d D U . . .
C35 C -0.501(4) 0.4603(17) 0.387(2) 0.117(12) Uani 1 1 d D U . . .
H35 H -0.614260 0.495800 0.361262 0.141 Uiso 0.5 1 calc R U P S 2
C36 C -0.522(4) 0.3657(17) 0.433(2) 0.116(12) Uani 1 1 d D U . . .
H36 H -0.643929 0.336493 0.438892 0.140 Uiso 0.5 1 calc R U P T 2
F37 F -0.017(5) 0.312(3) 0.491(3) 0.126(15) Uani 0.5 1 d D U P U 1
F38 F -0.004(5) 0.497(3) 0.406(3) 0.117(14) Uani 0.5 1 d D U P V 1
F39 F -0.661(5) 0.515(3) 0.356(3) 0.116(14) Uani 0.5 1 d D U P W 1
F40 F -0.700(5) 0.331(3) 0.447(3) 0.134(17) Uani 0.5 1 d D U P X 1
C41 C -0.099(3) 0.6550(19) 0.2711(17) 0.108(10) Uani 1 1 d D U . . .
C42 C -0.004(3) 0.7310(18) 0.2900(17) 0.112(12) Uani 1 1 d D U . . .
H42 H -0.062977 0.766877 0.336619 0.134 Uiso 0.5 1 calc R U P Y 1
C43 C 0.175(3) 0.753(2) 0.2400(16) 0.108(12) Uani 1 1 d D U . . .
H43 H 0.240823 0.803468 0.253929 0.130 Uiso 0.5 1 calc R U P Z 1
C44 C 0.264(4) 0.705(2) 0.171(2) 0.115(12) Uani 1 1 d D U . . .
C45 C 0.176(4) 0.626(2) 0.161(2) 0.123(12) Uani 1 1 d D U . . .
H45 H 0.248005 0.583927 0.122072 0.148 Uiso 0.5 1 calc R U P A 1
C46 C -0.012(4) 0.604(2) 0.202(2) 0.117(12) Uani 1 1 d D U . . .
H46 H -0.078762 0.555592 0.184813 0.140 Uiso 0.5 1 calc R U P B 1
F47 F -0.092(5) 0.777(3) 0.358(2) 0.125(15) Uani 0.5 1 d D U P C 2
F48 F 0.265(5) 0.824(3) 0.262(2) 0.131(15) Uani 0.5 1 d D U P D 2
F49 F 0.258(6) 0.580(3) 0.092(3) 0.170(19) Uani 0.5 1 d D U P E 2
F50 F -0.094(5) 0.533(3) 0.177(3) 0.134(15) Uani 0.5 1 d D U P F 2
C1S C 0.021(6) 0.281(4) 0.173(2) 0.19(3) Uani 0.5 1 d D U P G 1
H1S H 0.056860 0.211775 0.162055 0.229 Uiso 0.5 1 calc R U P G 1
Cl2S Cl -0.240(5) 0.299(3) 0.2079(19) 0.215(13) Uani 0.5 1 d D U P G 1
Cl3S Cl 0.158(5) 0.301(3) 0.258(2) 0.273(18) Uani 0.5 1 d D U P G 1
Cl4S Cl 0.086(5) 0.365(2) 0.0703(16) 0.200(13) Uani 0.5 1 d D U P G 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C11 1.77(2) . ?
S1 C44 1.77(2) 2_565 ?
S2 C14 1.77(2) . ?
S2 C21 1.77(2) . ?
S3 C24 1.77(2) . ?
S3 C31 1.77(2) . ?
S4 C34 1.76(2) . ?
S4 C41 1.76(2) . ?
C11 C12 1.380(19) . ?
C11 C16 1.39(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.39(3) . ?
C12 F17 1.32(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.35(2) . ?
C13 F18 1.34(2) . ?
C14 C15 1.35(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.38(3) . ?
C15 F19 1.34(2) . ?
C16 H16 0.9500 . ?
C16 F20 1.33(2) . ?
C21 C22 1.39(2) . ?
C21 C26 1.38(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.38(3) . ?
C22 F27 1.33(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.35(2) . ?
C23 F28 1.34(2) . ?
C24 C25 1.35(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.38(3) . ?
C25 F29 1.34(2) . ?
C26 H26 0.9500 . ?
C26 F30 1.34(2) . ?
C31 C32 1.38(2) . ?
C31 C36 1.39(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.39(3) . ?
C32 F37 1.33(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.34(2) . ?
C33 F38 1.34(2) . ?
C34 C35 1.37(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.37(3) . ?
C35 F39 1.33(2) . ?
C36 H36 0.9500 . ?
C36 F40 1.32(2) . ?
C41 C42 1.39(2) . ?
C41 C46 1.39(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.37(3) . ?
C42 F47 1.34(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.36(2) . ?
C43 F48 1.34(2) . ?
C44 C45 1.36(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.38(3) . ?
C45 F49 1.34(2) . ?
C46 H46 0.9500 . ?
C46 F50 1.33(2) . ?
C1S H1S 1.0000 . ?
C1S Cl2S 1.77(2) . ?
C1S Cl3S 1.76(2) . ?
C1S Cl4S 1.77(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 S1 C44 104.8(15) . 2_565 ?
C14 S2 C21 99.7(15) . . ?
C31 S3 C24 103.8(15) . . ?
C34 S4 C41 105.7(13) . . ?
C12 C11 S1 122.9(16) . . ?
C12 C11 C16 119(3) . . ?
C16 C11 S1 118.3(16) . . ?
C11 C12 H12 121.2 . . ?
C11 C12 C13 118(2) . . ?
C13 C12 H12 121.2 . . ?
F17 C12 C11 125(2) . . ?
F17 C12 C13 117(2) . . ?
C12 C13 H13 117.2 . . ?
C14 C13 C12 126(2) . . ?
C14 C13 H13 117.2 . . ?
F18 C13 C12 120(2) . . ?
F18 C13 C14 115(2) . . ?
C13 C14 S2 122.3(16) . . ?
C13 C14 C15 115(3) . . ?
C15 C14 S2 122.8(16) . . ?
C14 C15 H15 118.0 . . ?
C14 C15 C16 124(2) . . ?
C16 C15 H15 118.0 . . ?
F19 C15 C14 119(2) . . ?
F19 C15 C16 117(2) . . ?
C11 C16 H16 120.4 . . ?
C15 C16 C11 119(2) . . ?
C15 C16 H16 120.4 . . ?
F20 C16 C11 118(2) . . ?
F20 C16 C15 123(2) . . ?
C22 C21 S2 119.8(16) . . ?
C26 C21 S2 120.7(16) . . ?
C26 C21 C22 119(3) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118(2) . . ?
C23 C22 H22 120.9 . . ?
F27 C22 C21 121(2) . . ?
F27 C22 C23 121(2) . . ?
C22 C23 H23 117.6 . . ?
C24 C23 C22 125(2) . . ?
C24 C23 H23 117.6 . . ?
F28 C23 C22 118(2) . . ?
F28 C23 C24 118(2) . . ?
C23 C24 S3 122.0(16) . . ?
C25 C24 S3 123.2(16) . . ?
C25 C24 C23 115(3) . . ?
C24 C25 H25 117.4 . . ?
C24 C25 C26 125(3) . . ?
C26 C25 H25 117.4 . . ?
F29 C25 C24 118(2) . . ?
F29 C25 C26 117(2) . . ?
C21 C26 C25 118(2) . . ?
C21 C26 H26 121.2 . . ?
C25 C26 H26 121.2 . . ?
F30 C26 C21 121(2) . . ?
F30 C26 C25 121(2) . . ?
C32 C31 S3 120.8(16) . . ?
C32 C31 C36 119(3) . . ?
C36 C31 S3 120.0(16) . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120(2) . . ?
C33 C32 H32 120.0 . . ?
F37 C32 C31 121(2) . . ?
F37 C32 C33 119(2) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 C32 122(2) . . ?
C34 C33 H33 118.9 . . ?
F38 C33 C32 117(2) . . ?
F38 C33 C34 121(2) . . ?
C33 C34 S4 124.1(17) . . ?
C33 C34 C35 116(3) . . ?
C35 C34 S4 119.6(16) . . ?
C34 C35 H35 117.0 . . ?
C34 C35 C36 126(2) . . ?
C36 C35 H35 117.0 . . ?
F39 C35 C34 115(2) . . ?
F39 C35 C36 119(2) . . ?
C31 C36 H36 121.7 . . ?
C35 C36 C31 117(2) . . ?
C35 C36 H36 121.7 . . ?
F40 C36 C31 123(2) . . ?
F40 C36 C35 120(2) . . ?
C42 C41 S4 119.0(16) . . ?
C46 C41 S4 120.4(16) . . ?
C46 C41 C42 120(3) . . ?
C41 C42 H42 120.8 . . ?
C43 C42 C41 118(2) . . ?
C43 C42 H42 120.8 . . ?
F47 C42 C41 118(2) . . ?
F47 C42 C43 124(2) . . ?
C42 C43 H43 118.3 . . ?
C44 C43 C42 123(2) . . ?
C44 C43 H43 118.3 . . ?
F48 C43 C42 117(2) . . ?
F48 C43 C44 120(2) . . ?
C43 C44 S1 122.0(16) . 2_565 ?
C43 C44 C45 116(3) . . ?
C45 C44 S1 121.2(16) . 2_565 ?
C44 C45 H45 117.9 . . ?
C44 C45 C46 124(2) . . ?
C46 C45 H45 117.9 . . ?
F49 C45 C44 117(2) . . ?
F49 C45 C46 117(2) . . ?
C41 C46 H46 121.6 . . ?
C45 C46 C41 117(2) . . ?
C45 C46 H46 121.6 . . ?
F50 C46 C41 124(2) . . ?
F50 C46 C45 119(2) . . ?
Cl2S C1S H1S 109.0 . . ?
Cl2S C1S Cl4S 110(2) . . ?
Cl3S C1S H1S 109.0 . . ?
Cl3S C1S Cl2S 111(2) . . ?
Cl3S C1S Cl4S 109(2) . . ?
Cl4S C1S H1S 109.0 . . ?

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
S1 C11 C12 C13 178(3) . . . . ?
S1 C11 C12 F17 5(4) . . . . ?
S1 C11 C16 C15 -179(3) . . . . ?
S1 C11 C16 F20 8(5) . . . . ?
S1 C44 C45 C46 -177(3) 2_565 . . . ?
S1 C44 C45 F49 -12(6) 2_565 . . . ?
S2 C14 C15 C16 178(3) . . . . ?
S2 C14 C15 F19 -7(6) . . . . ?
S2 C21 C22 C23 -178(2) . . . . ?
S2 C21 C22 F27 2(3) . . . . ?
S2 C21 C26 C25 180(3) . . . . ?
S2 C21 C26 F30 -4(5) . . . . ?
S3 C24 C25 C26 -178(3) . . . . ?
S3 C24 C25 F29 0(5) . . . . ?
S3 C31 C32 C33 -178(2) . . . . ?
S3 C31 C32 F37 3(3) . . . . ?
S3 C31 C36 C35 179(3) . . . . ?
S3 C31 C36 F40 6(5) . . . . ?
S4 C34 C35 C36 -172(3) . . . . ?
S4 C34 C35 F39 3(5) . . . . ?
S4 C41 C42 C43 -173(2) . . . . ?
S4 C41 C42 F47 9(3) . . . . ?
S4 C41 C46 C45 178(3) . . . . ?
S4 C41 C46 F50 -5(5) . . . . ?
C11 C12 C13 C14 -1(2) . . . . ?
C11 C12 C13 F18 -179(3) . . . . ?
C12 C11 C16 C15 -3(4) . . . . ?
C12 C11 C16 F20 -177(3) . . . . ?
C12 C13 C14 S2 -178(2) . . . . ?
C12 C13 C14 C15 0(4) . . . . ?
C13 C14 C15 C16 0(6) . . . . ?
C13 C14 C15 F19 175(4) . . . . ?
C14 S2 C21 C22 -106.5(15) . . . . ?
C14 S2 C21 C26 78(3) . . . . ?
C14 C15 C16 C11 2(6) . . . . ?
C14 C15 C16 F20 175(4) . . . . ?
C16 C11 C12 C13 3(2) . . . . ?
C16 C11 C12 F17 -170(4) . . . . ?
F17 C12 C13 C14 172(4) . . . . ?
F17 C12 C13 F18 -5(4) . . . . ?
F18 C13 C14 S2 -1(4) . . . . ?
F18 C13 C14 C15 177(3) . . . . ?
F19 C15 C16 C11 -174(4) . . . . ?
F19 C15 C16 F20 -1(6) . . . . ?
C21 S2 C14 C13 80(3) . . . . ?
C21 S2 C14 C15 -98(3) . . . . ?
C21 C22 C23 C24 1(2) . . . . ?
C21 C22 C23 F28 -179(2) . . . . ?
C22 C21 C26 C25 4(4) . . . . ?
C22 C21 C26 F30 180(3) . . . . ?
C22 C23 C24 S3 179.9(19) . . . . ?
C22 C23 C24 C25 -1(4) . . . . ?
C23 C24 C25 C26 3(6) . . . . ?
C23 C24 C25 F29 -179(3) . . . . ?
C24 S3 C31 C32 -106.4(16) . . . . ?
C24 S3 C31 C36 74(3) . . . . ?
C24 C25 C26 C21 -4(6) . . . . ?
C24 C25 C26 F30 179(4) . . . . ?
C26 C21 C22 C23 -2(2) . . . . ?
C26 C21 C22 F27 178(3) . . . . ?
F27 C22 C23 C24 -180(3) . . . . ?
F27 C22 C23 F28 1(3) . . . . ?
F28 C23 C24 S3 0(4) . . . . ?
F28 C23 C24 C25 179(3) . . . . ?
F29 C25 C26 C21 177(3) . . . . ?
F29 C25 C26 F30 1(6) . . . . ?
C31 S3 C24 C23 93(3) . . . . ?
C31 S3 C24 C25 -86(3) . . . . ?
C31 C32 C33 C34 -2(2) . . . . ?
C31 C32 C33 F38 178(3) . . . . ?
C32 C31 C36 C35 -1(4) . . . . ?
C32 C31 C36 F40 -174(3) . . . . ?
C32 C33 C34 S4 173(2) . . . . ?
C32 C33 C34 C35 1(4) . . . . ?
C33 C34 C35 C36 0(6) . . . . ?
C33 C34 C35 F39 175(3) . . . . ?
C34 S4 C41 C42 -128.0(18) . . . . ?
C34 S4 C41 C46 60(3) . . . . ?
C34 C35 C36 C31 0(6) . . . . ?
C34 C35 C36 F40 174(4) . . . . ?
C36 C31 C32 C33 2(2) . . . . ?
C36 C31 C32 F37 -177(3) . . . . ?
F37 C32 C33 C34 177(3) . . . . ?
F37 C32 C33 F38 -3(3) . . . . ?
F38 C33 C34 S4 -8(4) . . . . ?
F38 C33 C34 C35 -179(3) . . . . ?
F39 C35 C36 C31 -174(3) . . . . ?
F39 C35 C36 F40 -1(6) . . . . ?
C41 S4 C34 C33 37(3) . . . . ?
C41 S4 C34 C35 -152(3) . . . . ?
C41 C42 C43 C44 1(2) . . . . ?
C41 C42 C43 F48 -178(3) . . . . ?
C42 C41 C46 C45 5(4) . . . . ?
C42 C41 C46 F50 -178(3) . . . . ?
C42 C43 C44 S1 -177(2) . . . 2_565 ?
C42 C43 C44 C45 -7(4) . . . . ?
C43 C44 C45 C46 13(6) . . . . ?
C43 C44 C45 F49 178(4) . . . . ?
C44 S1 C11 C12 17(2) 2_565 . . . ?
C44 S1 C11 C16 -168(2) 2_565 . . . ?
C44 C45 C46 C41 -12(6) . . . . ?
C44 C45 C46 F50 171(4) . . . . ?
C46 C41 C42 C43 -1(2) . . . . ?
C46 C41 C42 F47 -179(3) . . . . ?
F47 C42 C43 C44 179(3) . . . . ?
F47 C42 C43 F48 0(3) . . . . ?
F48 C43 C44 S1 2(4) . . . 2_565 ?
F48 C43 C44 C45 172(3) . . . . ?
F49 C45 C46 C41 -178(4) . . . . ?
F49 C45 C46 F50 5(6) . . . . ?

_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.835
_oxdiff_exptl_absorpt_empirical_full_min 0.367
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform'
####################################################################### 
# 
# 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_1a-Pyridine
_database_code_depnum_ccdc_archive 'CCDC 2175104'
loop_
_audit_author_name
_audit_author_address
'Stephen Argent'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_nottingham_internal_coll_name   OATSWO
_nottingham_internal_coll_number 19186
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'fine \w scans'
_nottingham_internal_coll_frame_time 0.2
_nottingham_internal_coll_frame_width 0.01
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   09/05/2022
_nottingham_internal_coll_location DLS
_nottingham_internal_coll_instrument i19-EH1
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_date 09/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 09/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 19/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_self_archive_date ?
_nottingham_internal_self_validation_date ?
_nottingham_internal_self_validation_user ?
_nottingham_internal_validation_date 19/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 19/05/2022
_refine_special_details          ?
_audit_creation_date             2022-05-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H16 F16 S8, 4(C5 H5 N)'
_chemical_formula_sum            'C68 H36 F16 N4 S8'
_chemical_formula_weight         1469.49
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0019 0.0015 '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 0.0124 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0037 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1048 0.1164 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   5.89701(12)
_cell_length_b                   32.2682(3)
_cell_length_c                   16.4767(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 95.0947(16)
_cell_angle_gamma                90.0
_cell_volume                     3122.89(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.92536400161465
_cell_measurement_theta_min      1.2171085816981666
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.979
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9796951000161046
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.1.018: AIMLESS, version 0.7.7 : 23/04/21
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62385
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         35.972
_diffrn_reflns_theta_min         1.223
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      100(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   Synchrotron
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9446
_reflns_number_total             14951
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       'GDA - generic data acquisition software'
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 3.dev (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 3.10.dev0 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         14951
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0669P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1390
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26), C42(H42), C43(H43), C45(H45),
 C46(H46), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C2A(H2A), C3A(H3A),
  C4A(H4A), C5A(H5A), C6A(H6A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1 S 0.40226(7) 0.33660(2) 0.77749(2) 0.03095(8) Uani 1 1 d . . . . .
S2 S 1.04999(6) 0.48990(2) 0.72722(3) 0.03759(10) Uani 1 1 d . . . . .
S3 S 0.54562(7) 0.65337(2) 0.82530(2) 0.03344(9) Uani 1 1 d . . . . .
S4 S 0.66845(7) 0.77951(2) 0.53396(2) 0.02923(8) Uani 1 1 d . . . . .
C11 C 0.5869(2) 0.37777(3) 0.75779(7) 0.0226(2) Uani 1 1 d . . . . .
C12 C 0.5148(2) 0.41052(4) 0.70646(7) 0.0238(2) Uani 1 1 d . . . . .
C13 C 0.6520(2) 0.44449(4) 0.69679(8) 0.0251(2) Uani 1 1 d . . . . .
C14 C 0.8642(2) 0.44817(4) 0.74013(8) 0.0260(2) Uani 1 1 d . . . . .
C15 C 0.9353(2) 0.41555(4) 0.79136(8) 0.0254(2) Uani 1 1 d . . . . .
C16 C 0.8015(2) 0.38082(4) 0.79897(7) 0.0244(2) Uani 1 1 d . . . . .
F17 F 0.30931(14) 0.40899(3) 0.66475(5) 0.03169(17) Uani 1 1 d . . . . .
F18 F 0.57604(15) 0.47465(2) 0.64518(5) 0.03442(19) Uani 1 1 d . . . . .
F19 F 1.13916(14) 0.41774(3) 0.83485(5) 0.03488(19) Uani 1 1 d . . . . .
F20 F 0.88222(15) 0.35019(2) 0.84844(5) 0.03347(18) Uani 1 1 d . . . . .
C21 C 0.8915(2) 0.53374(4) 0.75422(8) 0.0259(2) Uani 1 1 d . . . . .
C22 C 0.9777(2) 0.57170(4) 0.73105(9) 0.0285(3) Uani 1 1 d . . . . .
H22 H 1.108074 0.572559 0.701112 0.034 Uiso 1 1 calc R U . . .
C23 C 0.8735(3) 0.60822(4) 0.75164(9) 0.0308(3) Uani 1 1 d . . . . .
H23 H 0.935764 0.634078 0.737300 0.037 Uiso 1 1 calc R U . . .
C24 C 0.6780(2) 0.60731(4) 0.79321(8) 0.0248(2) Uani 1 1 d . . . . .
C25 C 0.5906(2) 0.56930(4) 0.81615(8) 0.0257(2) Uani 1 1 d . . . . .
H25 H 0.456954 0.568448 0.844324 0.031 Uiso 1 1 calc R U . . .
C26 C 0.6994(2) 0.53258(4) 0.79771(9) 0.0286(3) Uani 1 1 d . . . . .
H26 H 0.642611 0.506761 0.814788 0.034 Uiso 1 1 calc R U . . .
C31 C 0.5880(2) 0.68711(4) 0.74364(7) 0.0249(2) Uani 1 1 d . . . . .
C32 C 0.4209(2) 0.69204(4) 0.67909(8) 0.0269(2) Uani 1 1 d . . . . .
C33 C 0.4449(2) 0.72018(4) 0.61731(8) 0.0259(2) Uani 1 1 d . . . . .
C34 C 0.6385(2) 0.74407(3) 0.61420(7) 0.0219(2) Uani 1 1 d . . . . .
C35 C 0.8061(2) 0.73941(3) 0.67861(7) 0.0215(2) Uani 1 1 d . . . . .
C36 C 0.7811(2) 0.71205(4) 0.74216(7) 0.0228(2) Uani 1 1 d . . . . .
F37 F 0.22925(15) 0.66954(3) 0.67600(6) 0.0416(2) Uani 1 1 d . . . . .
F38 F 0.27212(14) 0.72413(3) 0.55892(5) 0.0376(2) Uani 1 1 d . . . . .
F39 F 0.99701(14) 0.76209(2) 0.68038(5) 0.02917(17) Uani 1 1 d . . . . .
F40 F 0.94945(14) 0.70967(3) 0.80220(5) 0.03177(18) Uani 1 1 d . . . . .
C41 C 0.6371(2) 0.74411(3) 0.45001(7) 0.0235(2) Uani 1 1 d . . . . .
C42 C 0.8107(2) 0.71592(4) 0.43827(9) 0.0303(3) Uani 1 1 d . . . . .
H42 H 0.941012 0.714472 0.476459 0.036 Uiso 1 1 calc R U . . .
C43 C 0.7929(2) 0.69002(4) 0.37078(9) 0.0297(3) Uani 1 1 d . . . . .
H43 H 0.909835 0.670556 0.362996 0.036 Uiso 1 1 calc R U . . .
C44 C 0.6033(2) 0.69269(3) 0.31465(7) 0.0226(2) Uani 1 1 d . . . . .
C45 C 0.4276(2) 0.72019(4) 0.32699(7) 0.0231(2) Uani 1 1 d . . . . .
H45 H 0.296924 0.721411 0.288943 0.028 Uiso 1 1 calc R U . . .
C46 C 0.4436(2) 0.74589(4) 0.39513(7) 0.0234(2) Uani 1 1 d . . . . .
H46 H 0.323485 0.764499 0.404120 0.028 Uiso 1 1 calc R U . . .
N1B N 0.2696(3) 0.53422(4) 1.01592(10) 0.0471(3) Uani 1 1 d . . . . .
C2B C 0.0871(3) 0.55514(6) 0.98323(11) 0.0454(4) Uani 1 1 d . . . . .
H2B H -0.047688 0.539907 0.967786 0.054 Uiso 1 1 calc R U . . .
C3B C 0.0833(3) 0.59702(6) 0.97080(10) 0.0433(4) Uani 1 1 d . . . . .
H3B H -0.050204 0.610182 0.946675 0.052 Uiso 1 1 calc R U . . .
C4B C 0.2778(3) 0.62012(5) 0.99400(9) 0.0371(3) Uani 1 1 d . . . . .
H4B H 0.279330 0.649342 0.987010 0.045 Uiso 1 1 calc R U . . .
C5B C 0.4683(3) 0.59934(5) 1.02745(9) 0.0336(3) Uani 1 1 d . . . . .
H5B H 0.604405 0.613981 1.043925 0.040 Uiso 1 1 calc R U . . .
C6B C 0.4572(3) 0.55659(5) 1.03656(10) 0.0389(3) Uani 1 1 d . . . . .
H6B H 0.590013 0.542462 1.058638 0.047 Uiso 1 1 calc R U . . .
N1A N 0.1713(3) 0.61557(5) 0.45979(9) 0.0461(3) Uani 1 1 d . . . . .
C2A C 0.1211(3) 0.57773(6) 0.48696(11) 0.0460(4) Uani 1 1 d . . . . .
H2A H -0.023726 0.566295 0.469759 0.055 Uiso 1 1 calc R U . . .
C3A C 0.2685(4) 0.55451(5) 0.53861(11) 0.0479(4) Uani 1 1 d . . . . .
H3A H 0.226070 0.527745 0.555931 0.058 Uiso 1 1 calc R U . . .
C4A C 0.4785(3) 0.57092(5) 0.56453(11) 0.0494(4) Uani 1 1 d . . . . .
H4A H 0.582757 0.555874 0.600628 0.059 Uiso 1 1 calc R U . . .
C5A C 0.5338(3) 0.60960(5) 0.53696(11) 0.0437(4) Uani 1 1 d . . . . .
H5A H 0.677909 0.621594 0.553136 0.052 Uiso 1 1 calc R U . . .
C6A C 0.3760(3) 0.63068(5) 0.48534(10) 0.0400(3) Uani 1 1 d . . . . .
H6A H 0.415474 0.657426 0.467028 0.048 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
S1 C11 1.7660(12) . ?
S1 C44 1.7860(12) 3_666 ?
S2 C14 1.7606(13) . ?
S2 C21 1.7739(13) . ?
S3 C24 1.7810(12) . ?
S3 C31 1.7657(12) . ?
S4 C34 1.7688(12) . ?
S4 C41 1.7909(12) . ?
C11 C12 1.3959(17) . ?
C11 C16 1.3855(18) . ?
C12 C13 1.3798(18) . ?
C12 F17 1.3400(15) . ?
C13 C14 1.3899(19) . ?
C13 F18 1.3430(14) . ?
C14 C15 1.3904(18) . ?
C15 C16 1.3828(18) . ?
C15 F19 1.3454(15) . ?
C16 F20 1.3412(14) . ?
C21 C22 1.3925(17) . ?
C21 C26 1.3937(19) . ?
C22 H22 0.9500 . ?
C22 C23 1.3851(18) . ?
C23 H23 0.9500 . ?
C23 C24 1.3922(19) . ?
C24 C25 1.3956(17) . ?
C25 H25 0.9500 . ?
C25 C26 1.3935(18) . ?
C26 H26 0.9500 . ?
C31 C32 1.3936(19) . ?
C31 C36 1.3960(18) . ?
C32 C33 1.3806(19) . ?
C32 F37 1.3404(15) . ?
C33 C34 1.3821(18) . ?
C33 F38 1.3440(15) . ?
C34 C35 1.3928(17) . ?
C35 C36 1.3875(16) . ?
C35 F39 1.3409(14) . ?
C36 F40 1.3401(14) . ?
C41 C42 1.3959(19) . ?
C41 C46 1.3927(18) . ?
C42 H42 0.9500 . ?
C42 C43 1.3876(19) . ?
C43 H43 0.9500 . ?
C43 C44 1.3887(18) . ?
C44 C45 1.3930(17) . ?
C45 H45 0.9500 . ?
C45 C46 1.3923(17) . ?
C46 H46 0.9500 . ?
N1B C2B 1.342(2) . ?
N1B C6B 1.340(2) . ?
C2B H2B 0.9500 . ?
C2B C3B 1.366(3) . ?
C3B H3B 0.9500 . ?
C3B C4B 1.393(2) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.380(2) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.390(2) . ?
C6B H6B 0.9500 . ?
N1A C2A 1.342(2) . ?
N1A C6A 1.335(2) . ?
C2A H2A 0.9500 . ?
C2A C3A 1.382(3) . ?
C3A H3A 0.9500 . ?
C3A C4A 1.379(3) . ?
C4A H4A 0.9500 . ?
C4A C5A 1.377(2) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.382(2) . ?
C6A H6A 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
C11 S1 C44 101.95(5) . 3_666 ?
C14 S2 C21 103.43(6) . . ?
C31 S3 C24 101.12(6) . . ?
C34 S4 C41 98.88(5) . . ?
C12 C11 S1 121.42(10) . . ?
C16 C11 S1 120.98(9) . . ?
C16 C11 C12 117.31(11) . . ?
C13 C12 C11 121.42(12) . . ?
F17 C12 C11 119.72(11) . . ?
F17 C12 C13 118.86(11) . . ?
C12 C13 C14 121.26(11) . . ?
F18 C13 C12 118.88(12) . . ?
F18 C13 C14 119.85(11) . . ?
C13 C14 S2 123.02(10) . . ?
C13 C14 C15 117.16(11) . . ?
C15 C14 S2 119.66(10) . . ?
C16 C15 C14 121.66(12) . . ?
F19 C15 C14 119.38(12) . . ?
F19 C15 C16 118.96(11) . . ?
C15 C16 C11 121.12(11) . . ?
F20 C16 C11 120.31(11) . . ?
F20 C16 C15 118.55(12) . . ?
C22 C21 S2 114.81(10) . . ?
C22 C21 C26 119.84(11) . . ?
C26 C21 S2 125.31(9) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.03(12) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.49(11) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 S3 122.16(9) . . ?
C23 C24 C25 119.58(11) . . ?
C25 C24 S3 118.09(10) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 119.99(12) . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.02(11) . . ?
C21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C32 C31 S3 120.90(10) . . ?
C32 C31 C36 116.33(11) . . ?
C36 C31 S3 122.65(10) . . ?
C33 C32 C31 121.71(12) . . ?
F37 C32 C31 120.26(12) . . ?
F37 C32 C33 118.02(12) . . ?
C32 C33 C34 122.24(12) . . ?
F38 C33 C32 117.98(12) . . ?
F38 C33 C34 119.78(11) . . ?
C33 C34 S4 121.74(9) . . ?
C33 C34 C35 116.36(11) . . ?
C35 C34 S4 121.88(9) . . ?
C36 C35 C34 121.86(11) . . ?
F39 C35 C34 119.68(10) . . ?
F39 C35 C36 118.45(11) . . ?
C35 C36 C31 121.43(11) . . ?
F40 C36 C31 120.40(11) . . ?
F40 C36 C35 118.16(11) . . ?
C42 C41 S4 119.73(10) . . ?
C46 C41 S4 119.84(10) . . ?
C46 C41 C42 120.39(11) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 C41 119.94(12) . . ?
C43 C42 H42 120.0 . . ?
C42 C43 H43 120.1 . . ?
C42 C43 C44 119.72(12) . . ?
C44 C43 H43 120.1 . . ?
C43 C44 S1 119.10(10) . 3_666 ?
C43 C44 C45 120.49(11) . . ?
C45 C44 S1 120.23(9) . 3_666 ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 119.95(11) . . ?
C46 C45 H45 120.0 . . ?
C41 C46 H46 120.3 . . ?
C45 C46 C41 119.46(11) . . ?
C45 C46 H46 120.3 . . ?
C6B N1B C2B 116.47(15) . . ?
N1B C2B H2B 118.0 . . ?
N1B C2B C3B 124.03(16) . . ?
C3B C2B H2B 118.0 . . ?
C2B C3B H3B 120.5 . . ?
C2B C3B C4B 119.07(16) . . ?
C4B C3B H3B 120.5 . . ?
C3B C4B H4B 121.0 . . ?
C5B C4B C3B 118.08(16) . . ?
C5B C4B H4B 121.0 . . ?
C4B C5B H5B 120.6 . . ?
C4B C5B C6B 118.76(15) . . ?
C6B C5B H5B 120.6 . . ?
N1B C6B C5B 123.58(16) . . ?
N1B C6B H6B 118.2 . . ?
C5B C6B H6B 118.2 . . ?
C6A N1A C2A 116.55(15) . . ?
N1A C2A H2A 118.2 . . ?
N1A C2A C3A 123.58(18) . . ?
C3A C2A H2A 118.2 . . ?
C2A C3A H3A 120.6 . . ?
C4A C3A C2A 118.74(16) . . ?
C4A C3A H3A 120.6 . . ?
C3A C4A H4A 120.7 . . ?
C5A C4A C3A 118.58(16) . . ?
C5A C4A H4A 120.7 . . ?
C4A C5A H5A 120.6 . . ?
C4A C5A C6A 118.85(17) . . ?
C6A C5A H5A 120.6 . . ?
N1A C6A C5A 123.69(16) . . ?
N1A C6A H6A 118.2 . . ?
C5A C6A H6A 118.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22 H22 F37 0.95 3.24 3.6370(15) 107.0 1_655 yes
C23 H23 F37 0.95 2.37 3.2148(15) 147.3 1_655 yes
C23 H23 F40 0.95 2.66 3.3979(15) 134.7 . yes
C26 H26 F18 0.95 2.97 3.1647(17) 92.7 . yes
C26 H26 N1B 0.95 3.09 3.743(2) 127.4 3_667 yes
C42 H42 F38 0.95 2.30 3.2348(15) 168.3 1_655 yes
C43 H43 F17 0.95 2.89 3.2943(15) 106.8 3_666 yes
C43 H43 N1A 0.95 2.76 3.510(2) 136.2 1_655 yes
C45 H45 F39 0.95 2.46 3.3941(14) 167.9 4_475 yes
C45 H45 F40 0.95 3.04 3.6103(15) 119.6 4_475 yes
C46 H46 S3 0.95 3.28 3.5178(12) 96.9 4_575 yes
C46 H46 F40 0.95 2.78 3.4783(15) 131.1 4_475 yes
C2B H2B N1B 0.95 2.75 3.570(2) 144.9 3_567 yes
C4B H4B S3 0.95 3.21 3.4860(15) 98.7 . yes
C5B H5B F19 0.95 2.61 3.1428(17) 116.2 3_767 yes
C6B H6B F19 0.95 2.60 3.1533(18) 117.2 3_767 yes
C6B H6B N1B 0.95 2.92 3.489(2) 120.1 3_667 yes
C2A H2A F17 0.95 2.78 3.427(2) 126.3 3_566 yes
C3A H3A F18 0.95 2.97 3.528(2) 118.9 . yes
C4A H4A F18 0.95 2.72 3.4075(18) 129.5 . yes
C6A H6A F38 0.95 2.80 3.3272(18) 115.6 . yes

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
S1 C11 C12 C13 174.10(10) . . . . ?
S1 C11 C12 F17 -6.64(16) . . . . ?
S1 C11 C16 C15 -171.82(10) . . . . ?
S1 C11 C16 F20 6.97(16) . . . . ?
S1 C44 C45 C46 -173.67(9) 3_666 . . . ?
S2 C14 C15 C16 -175.41(10) . . . . ?
S2 C14 C15 F19 4.71(17) . . . . ?
S2 C21 C22 C23 -177.47(12) . . . . ?
S2 C21 C26 C25 179.23(11) . . . . ?
S3 C24 C25 C26 -175.12(11) . . . . ?
S3 C31 C32 C33 175.88(10) . . . . ?
S3 C31 C32 F37 -3.43(17) . . . . ?
S3 C31 C36 C35 -177.59(9) . . . . ?
S3 C31 C36 F40 3.31(16) . . . . ?
S4 C34 C35 C36 179.02(9) . . . . ?
S4 C34 C35 F39 -0.35(16) . . . . ?
S4 C41 C42 C43 -176.37(11) . . . . ?
S4 C41 C46 C45 175.63(9) . . . . ?
C11 C12 C13 C14 -2.42(19) . . . . ?
C11 C12 C13 F18 178.48(11) . . . . ?
C12 C11 C16 C15 2.05(17) . . . . ?
C12 C11 C16 F20 -179.16(11) . . . . ?
C12 C13 C14 S2 177.56(10) . . . . ?
C12 C13 C14 C15 2.17(19) . . . . ?
C13 C14 C15 C16 0.15(19) . . . . ?
C13 C14 C15 F19 -179.74(11) . . . . ?
C14 S2 C21 C22 -165.46(11) . . . . ?
C14 S2 C21 C26 16.82(15) . . . . ?
C14 C15 C16 C11 -2.30(19) . . . . ?
C14 C15 C16 F20 178.89(11) . . . . ?
C16 C11 C12 C13 0.26(18) . . . . ?
C16 C11 C12 F17 179.52(10) . . . . ?
F17 C12 C13 C14 178.32(11) . . . . ?
F17 C12 C13 F18 -0.78(17) . . . . ?
F18 C13 C14 S2 -3.35(18) . . . . ?
F18 C13 C14 C15 -178.74(11) . . . . ?
F19 C15 C16 C11 177.59(11) . . . . ?
F19 C15 C16 F20 -1.22(17) . . . . ?
C21 S2 C14 C13 60.63(13) . . . . ?
C21 S2 C14 C15 -124.09(11) . . . . ?
C21 C22 C23 C24 -2.1(2) . . . . ?
C22 C21 C26 C25 1.6(2) . . . . ?
C22 C23 C24 S3 176.94(11) . . . . ?
C22 C23 C24 C25 1.8(2) . . . . ?
C23 C24 C25 C26 0.3(2) . . . . ?
C24 S3 C31 C32 94.69(11) . . . . ?
C24 S3 C31 C36 -89.46(11) . . . . ?
C24 C25 C26 C21 -1.9(2) . . . . ?
C26 C21 C22 C23 0.4(2) . . . . ?
C31 S3 C24 C23 36.24(13) . . . . ?
C31 S3 C24 C25 -148.51(11) . . . . ?
C31 C32 C33 C34 2.2(2) . . . . ?
C31 C32 C33 F38 -177.55(11) . . . . ?
C32 C31 C36 C35 -1.56(17) . . . . ?
C32 C31 C36 F40 179.34(11) . . . . ?
C32 C33 C34 S4 179.17(10) . . . . ?
C32 C33 C34 C35 -2.28(18) . . . . ?
C33 C34 C35 C36 0.47(17) . . . . ?
C33 C34 C35 F39 -178.90(11) . . . . ?
C34 S4 C41 C42 -71.58(11) . . . . ?
C34 S4 C41 C46 110.83(11) . . . . ?
C34 C35 C36 C31 1.47(18) . . . . ?
C34 C35 C36 F40 -179.41(10) . . . . ?
C36 C31 C32 C33 -0.23(18) . . . . ?
C36 C31 C32 F37 -179.53(11) . . . . ?
F37 C32 C33 C34 -178.46(11) . . . . ?
F37 C32 C33 F38 1.77(18) . . . . ?
F38 C33 C34 S4 -1.06(17) . . . . ?
F38 C33 C34 C35 177.49(11) . . . . ?
F39 C35 C36 C31 -179.16(10) . . . . ?
F39 C35 C36 F40 -0.04(16) . . . . ?
C41 S4 C34 C33 -58.63(11) . . . . ?
C41 S4 C34 C35 122.90(10) . . . . ?
C41 C42 C43 C44 0.8(2) . . . . ?
C42 C41 C46 C45 -1.94(18) . . . . ?
C42 C43 C44 S1 172.98(11) . . . 3_666 ?
C42 C43 C44 C45 -2.12(19) . . . . ?
C43 C44 C45 C46 1.38(18) . . . . ?
C44 S1 C11 C12 75.85(11) 3_666 . . . ?
C44 S1 C11 C16 -110.53(10) 3_666 . . . ?
C44 C45 C46 C41 0.66(18) . . . . ?
C46 C41 C42 C43 1.2(2) . . . . ?
N1B C2B C3B C4B -0.9(3) . . . . ?
C2B N1B C6B C5B 1.5(3) . . . . ?
C2B C3B C4B C5B 1.1(2) . . . . ?
C3B C4B C5B C6B -0.1(2) . . . . ?
C4B C5B C6B N1B -1.2(2) . . . . ?
C6B N1B C2B C3B -0.4(3) . . . . ?
N1A C2A C3A C4A 0.5(3) . . . . ?
C2A N1A C6A C5A 0.1(2) . . . . ?
C2A C3A C4A C5A -0.9(3) . . . . ?
C3A C4A C5A C6A 0.8(3) . . . . ?
C4A C5A C6A N1A -0.5(3) . . . . ?
C6A N1A C2A C3A -0.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pyridine'
