# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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. 
# 
#######################################################################

data_dwb1638
_database_code_depnum_ccdc_archive 'CCDC 2177830'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H31 F15 N3 O, B F4'
_chemical_formula_sum            'C27 H31 B F19 N3 O'
_chemical_formula_weight         785.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H31 B1 F19 N3 O1'
_chemical_oxdiff_usercomment     'Alessio Riccobono NV 2457'
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'
B B 0.0090 0.0039 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   29.930(2)
_cell_length_b                   9.2437(5)
_cell_length_c                   11.7255(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.553(5)
_cell_angle_gamma                90
_cell_volume                     3222.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2936
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      69.0810
_cell_measurement_theta_min      4.9780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 0 0.0550
5 2 0 0.0290
-2 -2 5 0.0958
4 5 1 0.0429
5 -1 3 0.0997
-5 0 -3 0.0853
-2 5 1 0.0457
1 0 0 0.0307
-1 0 0 0.0488
-1 0 2 0.1147
1 -2 0 0.0583
3 -5 -2 0.0925

_exptl_crystal_size_max          0.249
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.079
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
-0.9829 2.0055 -0.0013 0.0415 0.0487 0.3319
5.0214 2.0039 -0.0058 -0.2565 0.1349 0.3084
-1.9677 -2.0053 5.0059 0.2224 0.5487 -0.4408
4.0578 5.0119 0.9923 -0.1960 0.3432 0.7801
5.0256 -1.0043 2.9987 -0.1753 0.4246 -0.2560
-5.0345 0.0017 -2.9977 0.1794 -0.4561 0.0920
-1.9465 5.0135 0.9968 0.1019 0.2570 0.8037
1.0007 -0.0003 -0.0007 -0.0497 0.0144 -0.0039
-1.0007 0.0003 0.0007 0.0497 -0.0144 0.0039
-0.9801 0.0000 2.0017 0.0956 0.2418 -0.0444
0.9829 -2.0055 0.0013 -0.0415 -0.0487 -0.3319
2.9370 -5.0136 -1.9980 -0.1746 -0.3708 -0.7834

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10892
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.094
_diffrn_reflns_theta_max         67.094
_diffrn_reflns_theta_min         4.461
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_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    -19.00  11.00   1.00   10.50    --    0.00  57.00  90.00   30
  2  ω     24.00  69.00   1.00   10.50    --    0.00  57.00  90.00   45
  3  ω     28.00 117.00   1.00   40.50    --   54.00  37.00   0.00   89
  4  ω    105.00 133.00   1.00   40.50    --  108.00 111.00 -30.00   28
  5  ω     85.00 178.00   1.00   40.50    --  108.00  25.00  60.00   93
  6  ω     66.00 109.00   1.00   40.50    --  108.00-111.00 150.00   43
  7  ω     39.00 102.00   1.00   40.50    --  108.00 -50.00  60.00   63
  8  ω     36.00  86.00   1.00   40.50    --  108.00 -37.00   0.00   50
  9  ω     41.00  92.00   1.00   40.50    --  108.00 -25.00 -90.00   51
 10  ω     46.00  75.00   1.00   40.50    --  108.00 -25.00-120.00   29
 11  ω     63.00  90.00   1.00   40.50    --  108.00 -37.00-180.00   27
 12  ω     40.00 115.00   1.00   40.50    --  108.00-111.00-150.00   75
 13  ω     36.00  91.00   1.00   40.50    --  108.00 -37.00-120.00   55
 14  ω     30.00  87.00   1.00   40.50    --   54.00-125.00-150.00   57
 15  ω    -17.00  80.00   1.00   40.50    --   54.00 -37.00-180.00   97
 16  ω    -28.00  44.00   1.00   10.50    --    0.00  77.00-180.00   72
 17  ω     32.00  65.00   1.00   40.50    --   54.00-126.00 125.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0496095000
_diffrn_orient_matrix_UB_12      -0.0036003000
_diffrn_orient_matrix_UB_13      0.0234853000
_diffrn_orient_matrix_UB_21      0.0144633000
_diffrn_orient_matrix_UB_22      0.0314551000
_diffrn_orient_matrix_UB_23      0.1278905000
_diffrn_orient_matrix_UB_31      -0.0038930000
_diffrn_orient_matrix_UB_32      0.1635738000
_diffrn_orient_matrix_UB_33      -0.0240669000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4202
_reflns_number_total             5692
_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 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         5692
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0769
_refine_ls_restrained_S_all      1.087
_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)+(0.0928P)²+7.1006P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2088
_refine_ls_wR_factor_ref         0.2261
_refine_special_details          
;
minor disordered component in perfluoronated chain- modelled after the major component- C-F bonds locked, FCF bond angles locked, CCC bond angles locked. EADP with major chain. Extends onto the ring but this was unable to be modelled, but please be aware.                    Full restraints/contraints:                                            DFIX 1.5 C31 C32
DFIX 1.34 F3A C29
DFIX 1.34 C29 F4A
DFIX 1.34 F11A C33
DFIX 1.34 F12A C33
DFIX 1.34 F9A C32
DFIX 1.34 F10A C32
DFIX 1.5 C29 C28
DFIX 1.5 C29 C30
DFIX 1.5 C30 C31
DFIX 1.34 F5A C30
DFIX 1.34 F6A C30
DFIX 1.5 C34 C33
DFIX 1.34 F13A C34
DFIX 1.34 C34 F14A
DFIX 1.34 C34 F15A
DFIX 1.5 C20A C28
DFIX 1.34 C28 F2A
DFIX 1.34 C28 F1A
DANG 2.17 F3A F4A
DANG 2.17 F5A F6A
DANG 2.17 F7A F8A
DANG 2.17 F9A F10A
DANG 2.17 F11A F12A
DANG 2.2 F1A F2A
DANG 2.6 C20A C29
DANG 2.6 C28 C30
DANG 2.6 C30 C32
DANG 2.6 C32 C34
DANG 2.6 C29 C31
DANG 2.6 C31 C33
DANG 2.17 F2A F1A
EADP C22 C29
EADP C32 C25
EADP C24 C31
EADP F8A F10
EADP F7A F9
EADP C33 C26
EADP F3A F6
EADP F4A F5
EADP F11A F9
EADP F12A F10
EADP F9A F11A
EADP F10A F12A
EADP C21 C28
EADP C30 C23
EADP F5A F7A
EADP F6A F8A
EADP C34 C33
EADP F15A F12A
EADP F13A F12A
EADP F14A F12A
EADP F1A F3A
EADP F2A F4A
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C31-C32
 1.5 with sigma of 0.02
 F3A-C29
 1.34 with sigma of 0.02
 C29-F4A
 1.34 with sigma of 0.02
 F11A-C33
 1.34 with sigma of 0.02
 F12A-C33
 1.34 with sigma of 0.02
 F9A-C32
 1.34 with sigma of 0.02
 F10A-C32
 1.34 with sigma of 0.02
 C29-C28
 1.5 with sigma of 0.02
 C29-C30
 1.5 with sigma of 0.02
 C30-C31
 1.5 with sigma of 0.02
 F5A-C30
 1.34 with sigma of 0.02
 F6A-C30
 1.34 with sigma of 0.02
 C34-C33
 1.5 with sigma of 0.02
 F13A-C34
 1.34 with sigma of 0.02
 C34-F14A
 1.34 with sigma of 0.02
 C34-F15A
 1.34 with sigma of 0.02
 C20A-C28
 1.5 with sigma of 0.02
 C28-F2A
 1.34 with sigma of 0.02
 C28-F1A
 1.34 with sigma of 0.02
 F3A-F4A
 2.17 with sigma of 0.04
 F5A-F6A
 2.17 with sigma of 0.04
 F7A-F8A
 2.17 with sigma of 0.04
 F9A-F10A
 2.17 with sigma of 0.04
 F11A-F12A
 2.17 with sigma of 0.04
 F1A-F2A
 2.2 with sigma of 0.04
 C20A-C29
 2.6 with sigma of 0.04
 C28-C30
 2.6 with sigma of 0.04
 C30-C32
 2.6 with sigma of 0.04
 C32-C34
 2.6 with sigma of 0.04
 C29-C31
 2.6 with sigma of 0.04
 C31-C33
 2.6 with sigma of 0.04
 F2A-F1A
 2.17 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C29)
Uanis(C32) = Uanis(C25)
Uanis(C24) = Uanis(C31)
Uanis(F8A) = Uanis(F10)
Uanis(F7A) = Uanis(F9)
Uanis(C33) = Uanis(C26)
Uanis(F3A) = Uanis(F6)
Uanis(F4A) = Uanis(F5)
Uanis(F11A) = Uanis(F9)
Uanis(F12A) = Uanis(F10)
Uanis(F9A) = Uanis(F11A)
Uanis(F10A) = Uanis(F12A)
Uanis(C21) = Uanis(C28)
Uanis(C30) = Uanis(C23)
Uanis(F5A) = Uanis(F7A)
Uanis(F6A) = Uanis(F8A)
Uanis(C34) = Uanis(C33)
Uanis(F15A) = Uanis(F12A)
Uanis(F13A) = Uanis(F12A)
Uanis(F14A) = Uanis(F12A)
Uanis(F1A) = Uanis(F3A)
Uanis(F2A) = Uanis(F4A)
4. Others
 Sof(C29)=Sof(C28)=Sof(C32)=Sof(C33)=Sof(C30)=Sof(C31)=Sof(F7A)=Sof(F8A)=
 Sof(F6A)=Sof(F5A)=Sof(F12A)=Sof(F11A)=Sof(F3A)=Sof(F4A)=Sof(F10A)=Sof(F9A)=
 Sof(C34)=Sof(F14A)=Sof(F13A)=Sof(F15A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F6)=Sof(F10)=Sof(F9)=Sof(F1)=Sof(F8)=Sof(F11)=Sof(F5)=Sof(F3)=Sof(F7)=
 Sof(F4)=Sof(F2)=Sof(F12)=Sof(F15)=Sof(F13)=Sof(F14)=Sof(C23)=Sof(C25)=Sof(C21)=
 Sof(C24)=Sof(C22)=Sof(C26)=Sof(C27)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C9(H9A,H9B), C7(H7A,H7B), C3(H3A,H3B), C6(H6A,
 H6B), C5(H5A,H5B), C4(H4A,H4B), C2(H2A,H2B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C12(H12), C16(H16)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
F6 F 0.46217(10) 0.7800(3) 0.4998(2) 0.0480(7) Uani 0.9733(17) 1 d . . P A 1
F10 F 0.54105(10) 0.9127(3) 0.4139(2) 0.0493(7) Uani 0.9733(17) 1 d . . P A 1
F9 F 0.54999(10) 0.7269(3) 0.5283(2) 0.0480(7) Uani 0.9733(17) 1 d . . P A 1
F1 F 0.37238(10) 0.8148(3) 0.4522(2) 0.0481(7) Uani 0.9733(17) 1 d . . P A 1
F8 F 0.50408(10) 0.5555(3) 0.3790(3) 0.0497(7) Uani 0.9733(17) 1 d . . P A 1
F11 F 0.59128(10) 0.5867(3) 0.3484(3) 0.0531(7) Uani 0.9733(17) 1 d . . P A 1
F5 F 0.45290(10) 0.8924(3) 0.3363(2) 0.0518(7) Uani 0.9733(17) 1 d . . P A 1
F3 F 0.41701(11) 0.5548(3) 0.4196(3) 0.0530(7) Uani 0.9733(17) 1 d . . P A 1
F7 F 0.50485(11) 0.7126(4) 0.2410(2) 0.0544(8) Uani 0.9733(17) 1 d . . P A 1
F17 F 0.24609(11) 0.8078(3) 0.2430(2) 0.0549(8) Uani 1 1 d . . . . .
F4 F 0.41901(10) 0.6201(3) 0.2415(2) 0.0552(8) Uani 0.9733(17) 1 d . . P A 1
F2 F 0.36649(10) 0.8441(3) 0.2672(2) 0.0549(8) Uani 0.9733(17) 1 d . . P A 1
F12 F 0.59140(11) 0.7994(4) 0.2686(2) 0.0602(8) Uani 0.9733(17) 1 d . . P A 1
F15 F 0.63891(10) 0.6862(4) 0.5392(3) 0.0598(8) Uani 0.9733(17) 1 d . . P A 1
F16 F 0.27638(12) 0.9050(4) 0.4109(2) 0.0684(9) Uani 1 1 d . . . . .
F19 F 0.26484(12) 1.0462(3) 0.2534(3) 0.0669(9) Uani 1 1 d . . . . .
F18 F 0.20569(11) 0.9647(4) 0.3379(3) 0.0714(10) Uani 1 1 d . . . . .
F13 F 0.63378(12) 0.9045(3) 0.4761(3) 0.0685(9) Uani 0.9733(17) 1 d . . P A 1
O1 O 0.13710(12) 0.2734(4) 0.5923(3) 0.0510(9) Uani 1 1 d . . . . .
F14 F 0.66849(11) 0.7436(4) 0.3875(3) 0.0711(10) Uani 0.9733(17) 1 d . . P A 1
N1 N 0.30548(13) 0.6026(4) 0.4178(3) 0.0413(9) Uani 1 1 d . . . . .
N2 N 0.27959(13) 0.5138(4) 0.2544(3) 0.0410(9) Uani 1 1 d . . . . .
N3 N 0.31688(13) 0.5899(4) 0.2351(3) 0.0435(9) Uani 1 1 d . . . B 1
C23 C 0.45868(17) 0.7627(5) 0.3855(4) 0.0386(10) Uani 0.9733(17) 1 d . . P A 1
C17 C 0.27148(16) 0.5229(5) 0.3639(4) 0.0418(11) Uani 1 1 d . . . . .
C14 C 0.23423(16) 0.4608(5) 0.4172(4) 0.0417(11) Uani 1 1 d . . . . .
C25 C 0.54602(17) 0.7685(5) 0.4189(4) 0.0398(11) Uani 0.9733(17) 1 d . . P A 1
C21 C 0.37112(17) 0.7459(5) 0.3514(4) 0.0409(11) Uani 0.9733(17) 1 d . . P A 1
C24 C 0.50364(17) 0.6975(5) 0.3541(4) 0.0404(11) Uani 0.9733(17) 1 d . . P A 1
C15 C 0.22276(17) 0.3141(5) 0.4024(4) 0.0430(11) Uani 1 1 d . . . . .
H15 H 0.237576 0.256140 0.353866 0.052 Uiso 1 1 calc R U . . .
C22 C 0.41673(17) 0.6677(5) 0.3485(4) 0.0404(11) Uani 0.9733(17) 1 d . . P A 1
C11 C 0.16747(16) 0.3432(5) 0.5344(4) 0.0446(11) Uani 1 1 d . . . . .
C13 C 0.21079(17) 0.5468(5) 0.4868(4) 0.0443(11) Uani 1 1 d . . . . .
H13 H 0.217732 0.644669 0.494474 0.053 Uiso 1 1 calc R U . . .
C26 C 0.59029(18) 0.7297(5) 0.3682(4) 0.0455(12) Uani 0.9733(17) 1 d . . P A 1
C12 C 0.17734(17) 0.4896(5) 0.5448(4) 0.0461(11) Uani 1 1 d . . . . .
H12 H 0.161538 0.548557 0.590436 0.055 Uiso 1 1 calc R U . . .
C16 C 0.18943(17) 0.2569(5) 0.4603(4) 0.0449(11) Uani 1 1 d . . . . .
H16 H 0.181443 0.160113 0.450135 0.054 Uiso 1 1 calc R U . . .
C18 C 0.31342(18) 0.6276(6) 0.5426(4) 0.0485(12) Uani 1 1 d . . . . .
H18A H 0.303964 0.723701 0.559624 0.073 Uiso 1 1 calc R U . . .
H18B H 0.344886 0.616861 0.568065 0.073 Uiso 1 1 calc R U . . .
H18C H 0.296579 0.558572 0.581517 0.073 Uiso 1 1 calc R U . . .
C19 C 0.25141(17) 0.4465(6) 0.1582(4) 0.0496(12) Uani 1 1 d . . . . .
H19A H 0.259308 0.484931 0.087175 0.074 Uiso 1 1 calc R U . . .
H19B H 0.220342 0.466723 0.164735 0.074 Uiso 1 1 calc R U . . .
H19C H 0.256150 0.343759 0.159911 0.074 Uiso 1 1 calc R U . . .
C10 C 0.11551(18) 0.3539(6) 0.6756(4) 0.0511(12) Uani 1 1 d . . . . .
H10A H 0.095764 0.426681 0.637586 0.061 Uiso 1 1 calc R U . . .
H10B H 0.137881 0.402151 0.728812 0.061 Uiso 1 1 calc R U . . .
C27 C 0.63349(19) 0.7685(6) 0.4469(5) 0.0512(13) Uani 0.9733(17) 1 d . . P A 1
C8 C 0.06095(18) 0.3261(6) 0.8222(4) 0.0535(13) Uani 1 1 d . . . . .
H8A H 0.080924 0.381568 0.876580 0.064 Uiso 1 1 calc R U . . .
H8B H 0.040582 0.393324 0.779277 0.064 Uiso 1 1 calc R U . . .
C9 C 0.08875(18) 0.2489(6) 0.7393(4) 0.0530(13) Uani 1 1 d . . . . .
H9A H 0.109158 0.181501 0.781961 0.064 Uiso 1 1 calc R U . . .
H9B H 0.068850 0.193795 0.684450 0.064 Uiso 1 1 calc R U . . .
C7 C 0.03390(18) 0.2226(6) 0.8875(4) 0.0539(13) Uani 1 1 d . . . . .
H7A H 0.054507 0.161743 0.935977 0.065 Uiso 1 1 calc R U . . .
H7B H 0.016312 0.160388 0.832890 0.065 Uiso 1 1 calc R U . . .
C3 C -0.08107(18) 0.1606(6) 1.1715(5) 0.0553(13) Uani 1 1 d . . . . .
H3A H -0.059818 0.100720 1.219062 0.066 Uiso 1 1 calc R U . . .
H3B H -0.098950 0.097499 1.118170 0.066 Uiso 1 1 calc R U . . .
C6 C 0.00247(18) 0.2971(6) 0.9616(4) 0.0545(13) Uani 1 1 d . . . . .
H6A H -0.018859 0.355334 0.912817 0.065 Uiso 1 1 calc R U . . .
H6B H 0.019875 0.361779 1.014540 0.065 Uiso 1 1 calc R U . . .
C5 C -0.02341(18) 0.1921(6) 1.0299(5) 0.0558(13) Uani 1 1 d . . . . .
H5A H -0.040599 0.127043 0.976878 0.067 Uiso 1 1 calc R U . . .
H5B H -0.002027 0.134269 1.078872 0.067 Uiso 1 1 calc R U . . .
C4 C -0.05530(19) 0.2654(6) 1.1042(5) 0.0589(14) Uani 1 1 d . . . . .
H4A H -0.038103 0.330124 1.157563 0.071 Uiso 1 1 calc R U . . .
H4B H -0.076615 0.323601 1.055351 0.071 Uiso 1 1 calc R U . . .
B1 B 0.2483(2) 0.9316(7) 0.3117(5) 0.0482(14) Uani 1 1 d . . . . .
C2 C -0.1120(2) 0.2359(7) 1.2478(5) 0.0644(15) Uani 1 1 d . . . . .
H2A H -0.094155 0.297964 1.301943 0.077 Uiso 1 1 calc R U . . .
H2B H -0.133134 0.296456 1.200512 0.077 Uiso 1 1 calc R U . . .
C1 C -0.1379(2) 0.1290(7) 1.3135(6) 0.0715(17) Uani 1 1 d . . . . .
H1A H -0.155040 0.065565 1.260330 0.107 Uiso 1 1 calc R U . . .
H1B H -0.157921 0.180746 1.357353 0.107 Uiso 1 1 calc R U . . .
H1C H -0.117215 0.073142 1.364297 0.107 Uiso 1 1 calc R U . . .
C29 C 0.4175(12) 0.753(6) 0.365(6) 0.0404(11) Uani 0.0267(17) 1 d D . P A 2
C28 C 0.3799(8) 0.653(6) 0.330(6) 0.0409(11) Uani 0.0267(17) 1 d D . P A 2
C32 C 0.5499(15) 0.694(8) 0.373(7) 0.0398(11) Uani 0.0267(17) 1 d D . P A 2
C33 C 0.5924(18) 0.768(9) 0.433(6) 0.0455(12) Uani 0.0267(17) 1 d D . P A 2
C30 C 0.4630(12) 0.698(7) 0.341(6) 0.0386(10) Uani 0.0267(17) 1 d D . P A 2
C31 C 0.5059(14) 0.754(14) 0.402(11) 0.0404(11) Uani 0.0267(17) 1 d D . P A 2
F7A F 0.513(4) 0.744(10) 0.513(7) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
F8A F 0.500(4) 0.907(9) 0.382(8) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F6A F 0.464(4) 0.707(9) 0.227(6) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F5A F 0.466(4) 0.556(8) 0.368(6) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
F12A F 0.580(4) 0.906(8) 0.438(8) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F11A F 0.596(4) 0.709(9) 0.538(7) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
F3A F 0.421(4) 0.792(10) 0.476(5) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
F4A F 0.416(4) 0.877(9) 0.305(7) 0.0518(7) Uani 0.0267(17) 1 d D . P A 2
F10A F 0.552(4) 0.698(9) 0.259(7) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F9A F 0.540(4) 0.556(9) 0.398(7) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
C34 C 0.6374(17) 0.732(9) 0.397(7) 0.0455(12) Uani 0.0267(17) 1 d D . P A 2
F14A F 0.641(4) 0.793(10) 0.295(8) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F13A F 0.631(4) 0.595(8) 0.360(9) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F15A F 0.674(3) 0.790(11) 0.455(9) 0.0493(7) Uani 0.0267(17) 1 d D . P A 2
F1A F 0.387(4) 0.544(10) 0.404(6) 0.0480(7) Uani 0.0267(17) 1 d D . P A 2
F2A F 0.375(4) 0.610(9) 0.222(6) 0.0518(7) Uani 0.0267(17) 1 d D . P A 2
C20A C 0.33159(16) 0.6434(5) 0.3353(3) 0.0399(10) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F6 C23 1.342(5) . ?
F10 C25 1.342(5) . ?
F9 C25 1.331(5) . ?
F1 C21 1.339(5) . ?
F8 C24 1.344(5) . ?
F11 C26 1.343(6) . ?
F5 C23 1.333(5) . ?
F3 C22 1.335(5) . ?
F7 C24 1.338(5) . ?
F17 B1 1.397(6) . ?
F4 C22 1.339(5) . ?
F2 C21 1.337(5) . ?
F12 C26 1.339(6) . ?
F15 C27 1.318(6) . ?
F16 B1 1.377(6) . ?
F19 B1 1.383(7) . ?
F18 B1 1.379(7) . ?
F13 C27 1.302(6) . ?
O1 C11 1.358(6) . ?
O1 C10 1.439(6) . ?
F14 C27 1.343(6) . ?
N1 C17 1.353(6) . ?
N1 C18 1.475(5) . ?
N1 C20A 1.364(6) . ?
N2 N3 1.360(6) . ?
N2 C17 1.336(6) . ?
N2 C19 1.468(6) . ?
N3 C20A 1.304(5) . ?
C23 C24 1.557(7) . ?
C23 C22 1.553(7) . ?
C17 C14 1.456(7) . ?
C14 C15 1.405(7) . ?
C14 C13 1.386(7) . ?
C25 C24 1.548(7) . ?
C25 C26 1.555(7) . ?
C21 C22 1.548(7) . ?
C21 C20A 1.511(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.375(7) . ?
C11 C12 1.388(7) . ?
C11 C16 1.397(7) . ?
C13 H13 0.9300 . ?
C13 C12 1.378(7) . ?
C26 C27 1.543(8) . ?
C12 H12 0.9300 . ?
C16 H16 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.509(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.526(7) . ?
C8 C7 1.516(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.517(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.515(8) . ?
C3 C2 1.527(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.525(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.522(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.519(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C29 C28 1.48(2) . ?
C29 C30 1.51(2) . ?
C29 F3A 1.34(2) . ?
C29 F4A 1.34(2) . ?
C28 F1A 1.33(2) . ?
C28 F2A 1.33(2) . ?
C28 C20A 1.46(2) . ?
C32 C33 1.54(8) . ?
C32 C31 1.51(2) . ?
C32 F10A 1.35(2) . ?
C32 F9A 1.35(2) . ?
C33 F12A 1.34(2) . ?
C33 F11A 1.34(2) . ?
C33 C34 1.49(2) . ?
C30 C31 1.49(2) . ?
C30 F6A 1.34(2) . ?
C30 F5A 1.34(2) . ?
C31 F7A 1.30(16) . ?
C31 F8A 1.44(16) . ?
C34 F14A 1.34(2) . ?
C34 F13A 1.34(2) . ?
C34 F15A 1.34(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 O1 C10 118.2(4) . . ?
C17 N1 C18 125.2(4) . . ?
C17 N1 C20A 106.3(4) . . ?
C20A N1 C18 128.3(4) . . ?
N3 N2 C19 120.1(4) . . ?
C17 N2 N3 111.7(4) . . ?
C17 N2 C19 127.8(4) . . ?
C20A N3 N2 104.1(4) . . ?
F6 C23 C24 108.1(4) . . ?
F6 C23 C22 108.3(4) . . ?
F5 C23 F6 108.5(3) . . ?
F5 C23 C24 108.6(4) . . ?
F5 C23 C22 109.1(4) . . ?
C22 C23 C24 114.1(4) . . ?
N1 C17 C14 125.9(4) . . ?
N2 C17 N1 105.9(4) . . ?
N2 C17 C14 128.3(4) . . ?
C15 C14 C17 121.0(4) . . ?
C13 C14 C17 119.4(4) . . ?
C13 C14 C15 119.5(5) . . ?
F10 C25 C24 108.6(4) . . ?
F10 C25 C26 107.9(4) . . ?
F9 C25 F10 109.1(4) . . ?
F9 C25 C24 109.2(4) . . ?
F9 C25 C26 108.4(4) . . ?
C24 C25 C26 113.6(4) . . ?
F1 C21 C22 107.8(4) . . ?
F1 C21 C20A 110.6(4) . . ?
F2 C21 F1 108.6(4) . . ?
F2 C21 C22 108.5(4) . . ?
F2 C21 C20A 108.7(4) . . ?
C20A C21 C22 112.6(4) . . ?
F8 C24 C23 108.3(4) . . ?
F8 C24 C25 108.7(4) . . ?
F7 C24 F8 108.4(4) . . ?
F7 C24 C23 108.4(4) . . ?
F7 C24 C25 109.2(4) . . ?
C25 C24 C23 113.7(4) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 H15 120.3 . . ?
F3 C22 F4 109.3(4) . . ?
F3 C22 C23 108.7(4) . . ?
F3 C22 C21 107.1(4) . . ?
F4 C22 C23 108.8(4) . . ?
F4 C22 C21 108.3(4) . . ?
C21 C22 C23 114.6(4) . . ?
O1 C11 C12 124.5(5) . . ?
O1 C11 C16 115.4(4) . . ?
C12 C11 C16 120.1(5) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 C14 121.0(5) . . ?
C12 C13 H13 119.5 . . ?
F11 C26 C25 109.3(4) . . ?
F11 C26 C27 107.4(4) . . ?
F12 C26 F11 108.7(4) . . ?
F12 C26 C25 109.3(4) . . ?
F12 C26 C27 107.9(4) . . ?
C27 C26 C25 114.2(4) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.4(5) . . ?
C13 C12 H12 120.3 . . ?
C15 C16 C11 120.4(5) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C10 H10A 110.1 . . ?
O1 C10 H10B 110.1 . . ?
O1 C10 C9 108.0(4) . . ?
H10A C10 H10B 108.4 . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
F15 C27 F14 107.3(4) . . ?
F15 C27 C26 111.9(4) . . ?
F13 C27 F15 110.2(5) . . ?
F13 C27 F14 108.7(5) . . ?
F13 C27 C26 111.2(4) . . ?
F14 C27 C26 107.5(4) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C7 C8 C9 112.8(5) . . ?
C10 C9 C8 111.9(5) . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C8 C7 C6 113.9(5) . . ?
H7A C7 H7B 107.7 . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C4 C3 C2 113.1(5) . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C7 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C7 C6 C5 113.5(5) . . ?
H6A C6 H6B 107.7 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.6 . . ?
C4 C5 C6 114.0(5) . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C3 C4 C5 113.8(5) . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
F16 B1 F17 108.9(4) . . ?
F16 B1 F19 109.6(5) . . ?
F16 B1 F18 110.1(4) . . ?
F19 B1 F17 109.8(4) . . ?
F18 B1 F17 109.1(5) . . ?
F18 B1 F19 109.4(5) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C1 C2 C3 112.3(5) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C28 C29 C30 114(3) . . ?
F3A C29 C28 114(6) . . ?
F3A C29 C30 107(6) . . ?
F3A C29 F4A 106(3) . . ?
F4A C29 C28 115(7) . . ?
F4A C29 C30 99(7) . . ?
F1A C28 C29 104(7) . . ?
F1A C28 F2A 113(3) . . ?
F1A C28 C20A 90(6) . . ?
F2A C28 C29 117(6) . . ?
F2A C28 C20A 91(6) . . ?
C20A C28 C29 139(4) . . ?
C31 C32 C33 116(4) . . ?
F10A C32 C33 108(6) . . ?
F10A C32 C31 111(8) . . ?
F10A C32 F9A 106(3) . . ?
F9A C32 C33 121(7) . . ?
F9A C32 C31 95(8) . . ?
F12A C33 C32 103(6) . . ?
F12A C33 F11A 110(3) . . ?
F12A C33 C34 119(8) . . ?
F11A C33 C32 103(7) . . ?
F11A C33 C34 101(7) . . ?
C34 C33 C32 120(5) . . ?
C31 C30 C29 123(3) . . ?
F6A C30 C29 106(7) . . ?
F6A C30 C31 110(8) . . ?
F5A C30 C29 109(6) . . ?
F5A C30 C31 101(8) . . ?
F5A C30 F6A 107(3) . . ?
C30 C31 C32 119(3) . . ?
F7A C31 C32 99(8) . . ?
F7A C31 C30 119(10) . . ?
F7A C31 F8A 104(6) . . ?
F8A C31 C32 115(10) . . ?
F8A C31 C30 101(8) . . ?
F14A C34 C33 110(8) . . ?
F14A C34 F13A 97(8) . . ?
F14A C34 F15A 98(8) . . ?
F13A C34 C33 102(7) . . ?
F13A C34 F15A 129(9) . . ?
F15A C34 C33 118(8) . . ?
N1 C20A C21 126.1(4) . . ?
N1 C20A C28 134(3) . . ?
N3 C20A N1 111.9(4) . . ?
N3 C20A C21 121.9(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F6 C23 C24 F8 77.4(4) . . . . ?
F6 C23 C24 F7 -165.1(4) . . . . ?
F6 C23 C24 C25 -43.5(5) . . . . ?
F6 C23 C22 F3 -45.9(5) . . . . ?
F6 C23 C22 F4 -164.8(4) . . . . ?
F6 C23 C22 C21 73.8(5) . . . . ?
F10 C25 C24 F8 -167.2(3) . . . . ?
F10 C25 C24 F7 74.6(5) . . . . ?
F10 C25 C24 C23 -46.6(5) . . . . ?
F10 C25 C26 F11 -166.4(4) . . . . ?
F10 C25 C26 F12 -47.7(5) . . . . ?
F10 C25 C26 C27 73.3(5) . . . . ?
F9 C25 C24 F8 -48.4(5) . . . . ?
F9 C25 C24 F7 -166.5(4) . . . . ?
F9 C25 C24 C23 72.3(5) . . . . ?
F9 C25 C26 F11 75.6(5) . . . . ?
F9 C25 C26 F12 -165.7(4) . . . . ?
F9 C25 C26 C27 -44.7(5) . . . . ?
F1 C21 C22 F3 73.0(5) . . . . ?
F1 C21 C22 F4 -169.3(4) . . . . ?
F1 C21 C22 C23 -47.7(5) . . . . ?
F1 C21 C20A N1 -12.0(6) . . . . ?
F1 C21 C20A N3 163.6(4) . . . . ?
F11 C26 C27 F15 -52.4(6) . . . . ?
F11 C26 C27 F13 -176.0(4) . . . . ?
F11 C26 C27 F14 65.1(5) . . . . ?
F5 C23 C24 F8 -165.1(3) . . . . ?
F5 C23 C24 F7 -47.6(5) . . . . ?
F5 C23 C24 C25 74.1(5) . . . . ?
F5 C23 C22 F3 -163.8(4) . . . . ?
F5 C23 C22 F4 77.3(5) . . . . ?
F5 C23 C22 C21 -44.0(5) . . . . ?
F2 C21 C22 F3 -169.6(3) . . . . ?
F2 C21 C22 F4 -51.8(5) . . . . ?
F2 C21 C22 C23 69.8(5) . . . . ?
F2 C21 C20A N1 -131.1(5) . . . . ?
F2 C21 C20A N3 44.5(6) . . . . ?
F12 C26 C27 F15 -169.3(4) . . . . ?
F12 C26 C27 F13 67.0(6) . . . . ?
F12 C26 C27 F14 -51.8(5) . . . . ?
O1 C11 C12 C13 176.1(4) . . . . ?
O1 C11 C16 C15 -176.1(4) . . . . ?
O1 C10 C9 C8 -174.6(4) . . . . ?
N1 C17 C14 C15 -129.5(5) . . . . ?
N1 C17 C14 C13 48.2(7) . . . . ?
N2 N3 C20A N1 0.8(5) . . . . ?
N2 N3 C20A C21 -175.3(4) . . . . ?
N2 C17 C14 C15 50.3(7) . . . . ?
N2 C17 C14 C13 -132.0(5) . . . . ?
N3 N2 C17 N1 -2.3(5) . . . . ?
N3 N2 C17 C14 177.8(4) . . . . ?
C17 N1 C20A N3 -2.3(5) . . . . ?
C17 N1 C20A C21 173.7(4) . . . . ?
C17 N1 C20A C28 -139(3) . . . . ?
C17 N2 N3 C20A 1.0(5) . . . . ?
C17 C14 C15 C16 175.5(4) . . . . ?
C17 C14 C13 C12 -175.6(4) . . . . ?
C14 C15 C16 C11 -0.8(7) . . . . ?
C14 C13 C12 C11 0.9(7) . . . . ?
C25 C26 C27 F15 69.0(6) . . . . ?
C25 C26 C27 F13 -54.7(6) . . . . ?
C25 C26 C27 F14 -173.5(4) . . . . ?
C24 C23 C22 F3 74.6(5) . . . . ?
C24 C23 C22 F4 -44.3(5) . . . . ?
C24 C23 C22 C21 -165.7(4) . . . . ?
C24 C25 C26 F11 -46.0(5) . . . . ?
C24 C25 C26 F12 72.8(5) . . . . ?
C24 C25 C26 C27 -166.3(4) . . . . ?
C15 C14 C13 C12 2.1(7) . . . . ?
C22 C23 C24 F8 -43.2(5) . . . . ?
C22 C23 C24 F7 74.3(5) . . . . ?
C22 C23 C24 C25 -164.0(4) . . . . ?
C22 C21 C20A N1 108.6(5) . . . . ?
C22 C21 C20A N3 -75.8(5) . . . . ?
C11 O1 C10 C9 -172.1(4) . . . . ?
C13 C14 C15 C16 -2.2(6) . . . . ?
C26 C25 C24 F8 72.7(5) . . . . ?
C26 C25 C24 F7 -45.4(5) . . . . ?
C26 C25 C24 C23 -166.6(4) . . . . ?
C12 C11 C16 C15 3.8(7) . . . . ?
C16 C11 C12 C13 -3.9(7) . . . . ?
C18 N1 C17 N2 -172.9(4) . . . . ?
C18 N1 C17 C14 6.9(7) . . . . ?
C18 N1 C20A N3 173.1(4) . . . . ?
C18 N1 C20A C21 -10.9(7) . . . . ?
C18 N1 C20A C28 37(3) . . . . ?
C19 N2 N3 C20A 175.2(4) . . . . ?
C19 N2 C17 N1 -176.0(4) . . . . ?
C19 N2 C17 C14 4.2(8) . . . . ?
C10 O1 C11 C12 -4.0(7) . . . . ?
C10 O1 C11 C16 175.9(4) . . . . ?
C8 C7 C6 C5 -178.1(4) . . . . ?
C9 C8 C7 C6 -174.3(4) . . . . ?
C7 C8 C9 C10 -179.8(4) . . . . ?
C7 C6 C5 C4 -179.7(4) . . . . ?
C6 C5 C4 C3 179.7(4) . . . . ?
C4 C3 C2 C1 179.3(5) . . . . ?
C2 C3 C4 C5 178.5(5) . . . . ?
C29 C28 C20A N1 -82(10) . . . . ?
C29 C30 C31 C32 -180(9) . . . . ?
C29 C30 C31 F7A 59(14) . . . . ?
C29 C30 C31 F8A -53(12) . . . . ?
C28 C29 C30 C31 -159(10) . . . . ?
C28 C29 C30 F6A 73(8) . . . . ?
C28 C29 C30 F5A -41(8) . . . . ?
C32 C33 C34 F14A 73(10) . . . . ?
C32 C33 C34 F13A -29(10) . . . . ?
C32 C33 C34 F15A -176(8) . . . . ?
C33 C32 C31 C30 176(10) . . . . ?
C33 C32 C31 F7A -54(12) . . . . ?
C33 C32 C31 F8A 56(12) . . . . ?
C30 C29 C28 F1A 69(8) . . . . ?
C30 C29 C28 F2A -56(9) . . . . ?
C30 C29 C28 C20A 177(8) . . . . ?
C31 C32 C33 F12A -36(11) . . . . ?
C31 C32 C33 F11A 79(10) . . . . ?
C31 C32 C33 C34 -170(10) . . . . ?
F6A C30 C31 C32 -54(15) . . . . ?
F6A C30 C31 F7A -175(9) . . . . ?
F6A C30 C31 F8A 73(8) . . . . ?
F5A C30 C31 C32 59(14) . . . . ?
F5A C30 C31 F7A -62(9) . . . . ?
F5A C30 C31 F8A -175(8) . . . . ?
F12A C33 C34 F14A -55(9) . . . . ?
F12A C33 C34 F13A -157(8) . . . . ?
F12A C33 C34 F15A 56(11) . . . . ?
F11A C33 C34 F14A -175(7) . . . . ?
F11A C33 C34 F13A 83(8) . . . . ?
F11A C33 C34 F15A -64(10) . . . . ?
F3A C29 C28 F1A -55(7) . . . . ?
F3A C29 C28 F2A -179(7) . . . . ?
F3A C29 C28 C20A 53(12) . . . . ?
F3A C29 C30 C31 -32(12) . . . . ?
F3A C29 C30 F6A -159(6) . . . . ?
F3A C29 C30 F5A 86(6) . . . . ?
F4A C29 C28 F1A -177(7) . . . . ?
F4A C29 C28 F2A 58(8) . . . . ?
F4A C29 C28 C20A -70(12) . . . . ?
F4A C29 C30 C31 78(11) . . . . ?
F4A C29 C30 F6A -49(6) . . . . ?
F4A C29 C30 F5A -164(6) . . . . ?
F10A C32 C33 F12A 90(7) . . . . ?
F10A C32 C33 F11A -156(7) . . . . ?
F10A C32 C33 C34 -45(10) . . . . ?
F10A C32 C31 C30 52(15) . . . . ?
F10A C32 C31 F7A -178(8) . . . . ?
F10A C32 C31 F8A -68(8) . . . . ?
F9A C32 C33 F12A -148(7) . . . . ?
F9A C32 C33 F11A -34(7) . . . . ?
F9A C32 C33 C34 77(9) . . . . ?
F9A C32 C31 C30 -57(14) . . . . ?
F9A C32 C31 F7A 73(8) . . . . ?
F9A C32 C31 F8A -177(8) . . . . ?
F1A C28 C20A N1 31(5) . . . . ?
F2A C28 C20A N1 143(4) . . . . ?
C20A N1 C17 N2 2.7(5) . . . . ?
C20A N1 C17 C14 -177.5(4) . . . . ?
C20A C21 C22 F3 -49.2(5) . . . . ?
C20A C21 C22 F4 68.5(5) . . . . ?
C20A C21 C22 C23 -169.9(3) . . . . ?

_olex2_date_sample_data_collection 2016-06-17
_olex2_date_sample_submission    2016-06-08
_olex2_exptl_crystal_mounting_method 'oil on micromount 150 micrometres'
_olex2_submission_original_sample_id 'NV 2457'
_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 1.991
_oxdiff_exptl_absorpt_empirical_full_min 0.633
####################################################################### 
# 
# 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_dwb1673
_database_code_depnum_ccdc_archive 'CCDC 2177834'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H31 F19 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C31 H31 F25 N4 O5 S2'
_chemical_formula_weight         1078.72
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H31 F25 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio Riccobono ALR14'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   6.7112(2)
_cell_length_b                   8.5380(3)
_cell_length_c                   71.575(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.664(3)
_cell_angle_gamma                90
_cell_volume                     4099.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3984
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.8200
_cell_measurement_theta_min      5.2120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.674
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0225
-4 0 -1 0.1020
4 1 1 0.0978
0 1 0 0.0710
0 -1 0 0.0710
0 0 -1 0.0155

_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.038
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
-0.0000 -0.0000 1.0000 0.0123 0.0177 0.0008
-3.9989 0.0001 -0.9851 -0.7810 0.4804 0.0611
3.9988 1.0003 0.9885 0.7746 -0.4677 -0.2411
-0.0001 1.0005 0.0035 -0.0064 0.0126 -0.1799
0.0001 -1.0005 -0.0035 0.0064 -0.0126 0.1799
0.0000 0.0000 -1.0000 -0.0123 -0.0177 -0.0008

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            14305
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.707
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  11.50   0.75    0.75    --    0.00  57.00 -60.00   42
  2  ω     21.00  69.00   0.75    0.75    --    0.00  57.00 -60.00   64
  3  ω     33.00 121.50   0.75    1.00    --   54.00  57.00  30.00  118
  4  ω     85.00 174.25   0.75    2.00    --  108.00  37.00   0.00  119
  5  ω     80.00 144.50   0.75    2.00    --  108.00 -91.00-150.00   86
  6  ω     84.00 115.50   0.75    2.00    --  108.00-111.00-180.00   42
  7  ω     56.00  82.25   0.75    2.00    --  108.00-111.00-180.00   35
  8  ω     36.00  68.25   0.75    2.00    --  108.00 -91.00-150.00   43
  9  ω     36.00 152.25   0.75    2.00    --  108.00  12.00 -30.00  155
 10  ω     75.00 121.50   0.75    1.00    --   54.00  57.00 150.00   62
 11  ω     50.00 129.50   0.75    2.00    --  108.00 -63.00   0.00  106
 12  ω     59.00 103.25   0.75    1.00    --   54.00-125.00  60.00   59
 13  ω    -18.00  74.25   0.75    1.00    --   54.00 -37.00-120.00  123
 14  ω     -9.00  39.00   0.75    0.75    --    0.00  57.00  30.00   64
 15  ω     76.00 111.25   0.75    2.00    --  108.00 178.00  90.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1922803000
_diffrn_orient_matrix_UB_12      -0.0063989000
_diffrn_orient_matrix_UB_13      0.0122805000
_diffrn_orient_matrix_UB_21      -0.1244764000
_diffrn_orient_matrix_UB_22      0.0125453000
_diffrn_orient_matrix_UB_23      0.0176798000
_diffrn_orient_matrix_UB_31      -0.0154952000
_diffrn_orient_matrix_UB_32      -0.1798669000
_diffrn_orient_matrix_UB_33      0.0008167000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6207
_reflns_number_total             7264
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         7264
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0616
_refine_ls_restrained_S_all      1.159
_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)+(0.0397P)²+6.7533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1509
_refine_special_details          
;
Both the cation and anion exhibited disorder.
For the cation, the end of the perfluorononyl was disordered.
C16-C19 and their associated fluorines were and modelled in
two positions with refined occupancies of 0.766:0.234(3).  
The C-F bond lengths for the minor component were restrained
to be 1.35 angstroms.  Pairs of C-C bonds were restrained to
be equal e.g. C16-C17 & C16A-C17A.
The ADP of proximal atoms in the disordered part were constrained
to be equal e.g. C16 & C16A, F19 & F19A.

For the cation, one of the trifluoromethyl groups was modelled
in two positions with refined occupancies of 0.855:0.145(9).
The C-F bond lengths were restrained to be 1.35 angstroms.
The ADP of proximal atoms in the disordered part were constrained
to be equal, i.e. C30 & C30A, F20 & F20A, F21 & F21A, F22 & F22A.
The disordered C-S bond lengths were restrained to be equal, i.e.
C30-S1 & C30A-S1
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F12A-C16A = F11A-C16A = F16A-C18A = F15A-C18A = F19A-C19A = F18A-C19A = F17A-
 C19A
 1.35 with sigma of 0.01
 C17A-F13A = C17A-F14A = C15-F9A = C15-F10A
 1.35 with sigma of 0.01
 F20-C30 = F22-C30 = F21-C30 = F20A-C30A = F21A-C30A = F22A-C30A
 1.35 with sigma of 0.01
 C17-C16 \\sim C17A-C16A
 with sigma of 0.02
 C16-C15 \\sim C16A-C15
 with sigma of 0.02
 C18A-C17A \\sim C18-C17
 with sigma of 0.02
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
 S1-C30 \\sim S1-C30A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C18A) = Uanis(C18)
Uanis(F16) = Uanis(F16A)
Uanis(C16) = Uanis(C16A)
Uanis(C17A) = Uanis(C17)
Uanis(F19A) = Uanis(F19)
Uanis(C19) = Uanis(C19A)
Uanis(F9A) = Uanis(F9)
Uanis(F10) = Uanis(F10A)
Uanis(F11) = Uanis(F11A)
Uanis(F12A) = Uanis(F12)
Uanis(F21) = Uanis(F21A)
Uanis(F22) = Uanis(F22A)
Uanis(F20) = Uanis(F20A)
Uanis(C30A) = Uanis(C30)
4. Others
 Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=Sof(F18A)=
 Sof(F19A)=1-FVAR(1)
 Sof(C16)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=Sof(F19)=FVAR(1)
 Sof(C30A)=Sof(F20A)=Sof(F21A)=Sof(F22A)=1-FVAR(2)
 Sof(C30)=Sof(F20)=Sof(F21)=Sof(F22)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C)
;
_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
C1 C 0.2048(5) 0.1049(4) 0.67526(5) 0.0190(7) Uani 1 1 d . . . . .
C2 C 0.1682(5) 0.2533(4) 0.66765(5) 0.0185(7) Uani 1 1 d . . . . .
H2 H 0.2277 0.3436 0.6732 0.022 Uiso 1 1 calc R . . . .
C3 C 0.0434(5) 0.2669(4) 0.65185(5) 0.0174(7) Uani 1 1 d . . . . .
H3 H 0.0179 0.3671 0.6465 0.021 Uiso 1 1 calc R . . . .
C4 C -0.0440(5) 0.1342(4) 0.64384(5) 0.0168(7) Uani 1 1 d . . . . .
C5 C -0.0097(5) -0.0130(4) 0.65182(5) 0.0209(7) Uani 1 1 d . . . . .
H5 H -0.0715 -0.1033 0.6465 0.025 Uiso 1 1 calc R . . . .
C6 C 0.1143(5) -0.0271(4) 0.66748(5) 0.0229(7) Uani 1 1 d . . . . .
H6 H 0.1378 -0.1271 0.6729 0.027 Uiso 1 1 calc R . . . .
C7 C -0.1664(5) 0.1460(4) 0.62656(5) 0.0167(7) Uani 1 1 d . . . . .
C8 C -0.2633(5) 0.1762(4) 0.59767(5) 0.0180(7) Uani 1 1 d . . . . .
C9 C -0.4974(5) 0.0652(4) 0.63841(5) 0.0190(7) Uani 1 1 d . . . . .
H9A H -0.5699 -0.0284 0.6341 0.028 Uiso 1 1 calc GR . . . .
H9B H -0.5923 0.1502 0.6405 0.028 Uiso 1 1 calc GR . . . .
H9C H -0.4242 0.0417 0.6501 0.028 Uiso 1 1 calc GR . . . .
C10 C 0.1026(5) 0.2291(5) 0.60497(5) 0.0299(9) Uani 1 1 d . . . . .
H10A H 0.1593 0.1465 0.5973 0.045 Uiso 1 1 calc GR . . . .
H10B H 0.1836 0.2409 0.6165 0.045 Uiso 1 1 calc GR . . . .
H10C H 0.1014 0.3282 0.5980 0.045 Uiso 1 1 calc GR . . . .
C11 C -0.2492(5) 0.2026(4) 0.57705(5) 0.0216(7) Uani 1 1 d . . . . .
C12 C -0.4512(5) 0.1960(4) 0.56598(5) 0.0202(7) Uani 1 1 d . . . . .
C13 C -0.4404(5) 0.2509(4) 0.54537(5) 0.0215(7) Uani 1 1 d . . . . .
C14 C -0.6191(5) 0.1968(4) 0.53280(5) 0.0217(7) Uani 1 1 d . . . . .
C15 C -0.6385(5) 0.2810(4) 0.51367(5) 0.0194(7) Uani 1 1 d D . . . .
C20 C 0.4852(5) 0.1894(4) 0.69443(5) 0.0206(7) Uani 1 1 d . . . . .
H20A H 0.4290 0.2846 0.7002 0.025 Uiso 1 1 calc R . . . .
H20B H 0.5542 0.2200 0.6829 0.025 Uiso 1 1 calc R . . . .
C21 C 0.6276(5) 0.1086(4) 0.70797(5) 0.0227(7) Uani 1 1 d . . . . .
H21A H 0.6786 0.0127 0.7020 0.027 Uiso 1 1 calc R . . . .
H21B H 0.5535 0.0759 0.7191 0.027 Uiso 1 1 calc R . . . .
C22 C 0.8047(5) 0.2092(4) 0.71443(5) 0.0211(7) Uani 1 1 d . . . . .
H22A H 0.8841 0.2380 0.7035 0.025 Uiso 1 1 calc R . . . .
H22B H 0.7554 0.3070 0.7201 0.025 Uiso 1 1 calc R . . . .
C23 C 0.9364(5) 0.1218(4) 0.72862(5) 0.0220(7) Uani 1 1 d . . . . .
H23A H 0.9865 0.0253 0.7227 0.026 Uiso 1 1 calc R . . . .
H23B H 0.8542 0.0900 0.7392 0.026 Uiso 1 1 calc R . . . .
C24 C 1.1139(5) 0.2162(4) 0.73617(5) 0.0207(7) Uani 1 1 d . . . . .
H24A H 1.0649 0.3149 0.7416 0.025 Uiso 1 1 calc R . . . .
H24B H 1.2001 0.2439 0.7257 0.025 Uiso 1 1 calc R . . . .
C25 C 1.2381(5) 0.1283(4) 0.75097(5) 0.0220(7) Uani 1 1 d . . . . .
H25A H 1.1524 0.1029 0.7616 0.026 Uiso 1 1 calc R . . . .
H25B H 1.2838 0.0283 0.7456 0.026 Uiso 1 1 calc R . . . .
C26 C 1.4190(5) 0.2195(4) 0.75832(5) 0.0210(7) Uani 1 1 d . . . . .
H26A H 1.3731 0.3197 0.7637 0.025 Uiso 1 1 calc R . . . .
H26B H 1.5048 0.2447 0.7477 0.025 Uiso 1 1 calc R . . . .
C27 C 1.5437(5) 0.1320(4) 0.77320(5) 0.0233(7) Uani 1 1 d . . . . .
H27A H 1.4595 0.1097 0.7840 0.028 Uiso 1 1 calc R . . . .
H27B H 1.5866 0.0305 0.7680 0.028 Uiso 1 1 calc R . . . .
C28 C 1.7270(5) 0.2226(4) 0.77996(5) 0.0235(7) Uani 1 1 d . . . . .
H28A H 1.6840 0.3233 0.7854 0.028 Uiso 1 1 calc R . . . .
H28B H 1.8100 0.2468 0.7691 0.028 Uiso 1 1 calc R . . . .
C29 C 1.8533(6) 0.1336(5) 0.79454(6) 0.0310(9) Uani 1 1 d . . . . .
H29A H 1.7751 0.1160 0.8057 0.046 Uiso 1 1 calc GR . . . .
H29B H 1.9723 0.1951 0.7979 0.046 Uiso 1 1 calc GR . . . .
H29C H 1.8934 0.0325 0.7894 0.046 Uiso 1 1 calc GR . . . .
F1 F -0.1680(3) 0.3444(3) 0.57386(3) 0.0313(5) Uani 1 1 d . . . . .
F2 F -0.1268(3) 0.0933(3) 0.57014(3) 0.0354(6) Uani 1 1 d . . . . .
F3 F -0.5812(3) 0.2897(3) 0.57460(3) 0.0289(5) Uani 1 1 d . . . . .
F4 F -0.5188(3) 0.0484(3) 0.56658(3) 0.0314(5) Uani 1 1 d . . . . .
F5 F -0.4349(3) 0.4089(2) 0.54534(3) 0.0304(5) Uani 1 1 d . . . . .
F6 F -0.2717(3) 0.1984(3) 0.53805(3) 0.0312(5) Uani 1 1 d . . . . .
F7 F -0.7870(3) 0.2208(3) 0.54209(3) 0.0372(6) Uani 1 1 d . . . . .
F8 F -0.5990(4) 0.0428(2) 0.52987(3) 0.0370(6) Uani 1 1 d . . . . .
N1 N -0.3577(4) 0.1127(3) 0.62429(4) 0.0154(6) Uani 1 1 d . . . . .
N2 N -0.4218(4) 0.1312(3) 0.60626(4) 0.0179(6) Uani 1 1 d . . . . .
N3 N -0.1019(4) 0.1870(3) 0.60964(4) 0.0185(6) Uani 1 1 d . . . . .
O1 O 0.3301(4) 0.0773(3) 0.69016(3) 0.0242(5) Uani 1 1 d . . . . .
C16 C -0.7978(8) 0.2100(7) 0.49999(8) 0.0216(10) Uani 0.766(3) 1 d D . P A 1
C17 C -0.8249(8) 0.2946(7) 0.48089(9) 0.0195(9) Uani 0.766(3) 1 d D . P A 1
C18 C -0.9959(8) 0.2297(6) 0.46806(7) 0.0259(12) Uani 0.766(3) 1 d D . P A 1
C19 C -1.0247(10) 0.3043(8) 0.44867(8) 0.0315(12) Uani 0.766(3) 1 d D . P A 1
F9 F -0.6791(6) 0.4335(4) 0.51628(9) 0.0315(11) Uani 0.766(3) 1 d . . P A 1
F10 F -0.4586(10) 0.2720(7) 0.50589(16) 0.0319(15) Uani 0.766(3) 1 d . . P A 1
F11 F -0.9727(4) 0.2120(4) 0.50861(4) 0.0338(8) Uani 0.766(3) 1 d . . P A 1
F12 F -0.7479(6) 0.0609(3) 0.49647(5) 0.0360(8) Uani 0.766(3) 1 d . . P A 1
F13 F -0.8614(6) 0.4474(3) 0.48366(4) 0.0330(7) Uani 0.766(3) 1 d . . P A 1
F14 F -0.6538(4) 0.2819(4) 0.47173(4) 0.0345(8) Uani 0.766(3) 1 d . . P A 1
F15 F -1.1688(4) 0.2486(4) 0.47685(4) 0.0329(7) Uani 0.766(3) 1 d . . P A 1
F16 F -0.975(3) 0.0793(7) 0.4665(3) 0.0390(14) Uani 0.766(3) 1 d . . P A 1
F17 F -1.1727(7) 0.2344(6) 0.43973(7) 0.0501(12) Uani 0.766(3) 1 d . . P A 1
F18 F -0.8633(6) 0.2868(6) 0.43897(5) 0.0583(12) Uani 0.766(3) 1 d . . P A 1
F19 F -1.0595(8) 0.4564(5) 0.45037(7) 0.0458(12) Uani 0.766(3) 1 d . . P A 1
C16A C -0.766(2) 0.1953(19) 0.4986(2) 0.0216(10) Uani 0.234(3) 1 d D . P A 2
C17A C -0.853(2) 0.2978(19) 0.4827(3) 0.0195(9) Uani 0.234(3) 1 d D . P A 2
C18A C -0.909(2) 0.204(2) 0.4649(2) 0.0259(12) Uani 0.234(3) 1 d D . P A 2
C19A C -1.054(2) 0.289(2) 0.4519(2) 0.0315(12) Uani 0.234(3) 1 d D . P A 2
F9A F -0.738(3) 0.4129(16) 0.5176(4) 0.0315(11) Uani 0.234(3) 1 d D . P A 2
F10A F -0.462(3) 0.311(4) 0.5059(6) 0.0319(15) Uani 0.234(3) 1 d D . P A 2
F11A F -0.9122(14) 0.1158(15) 0.50678(14) 0.0338(8) Uani 0.234(3) 1 d D . P A 2
F12A F -0.6474(19) 0.0860(12) 0.49102(16) 0.0360(8) Uani 0.234(3) 1 d D . P A 2
F13A F -1.0165(18) 0.3688(16) 0.48918(15) 0.054(4) Uani 0.234(3) 1 d D . P A 2
F14A F -0.714(2) 0.4051(14) 0.47875(16) 0.047(4) Uani 0.234(3) 1 d D . P A 2
F15A F -0.7434(13) 0.1796(13) 0.45530(12) 0.036(3) Uani 0.234(3) 1 d D . P A 2
F16A F -0.968(10) 0.053(3) 0.4662(11) 0.0390(14) Uani 0.234(3) 1 d D . P A 2
F17A F -1.2395(14) 0.2980(14) 0.45829(15) 0.041(3) Uani 0.234(3) 1 d D . P A 2
F18A F -1.071(2) 0.2229(18) 0.43481(17) 0.044(4) Uani 0.234(3) 1 d D . P A 2
F19A F -0.988(3) 0.433(2) 0.4472(3) 0.0458(12) Uani 0.234(3) 1 d D . P A 2
C31 C 0.3058(6) 0.3785(4) 0.33173(6) 0.0295(9) Uani 1 1 d . . . . .
F23 F 0.3392(5) 0.4795(3) 0.31804(4) 0.0509(7) Uani 1 1 d . . . . .
F24 F 0.3413(4) 0.2346(3) 0.32538(3) 0.0398(6) Uani 1 1 d . . . . .
F25 F 0.1145(3) 0.3872(3) 0.33589(3) 0.0346(5) Uani 1 1 d . . . . .
N4 N 0.3914(5) 0.2980(4) 0.36628(5) 0.0294(7) Uani 1 1 d . . . . .
O2 O 0.1909(5) 0.4800(3) 0.38689(4) 0.0412(7) Uani 1 1 d . . . . .
O3 O 0.1801(4) 0.1921(3) 0.39017(4) 0.0362(7) Uani 1 1 d . . . . .
O4 O 0.4240(4) 0.5855(3) 0.35623(4) 0.0329(6) Uani 1 1 d . . . . .
O5 O 0.6613(4) 0.3863(4) 0.34603(5) 0.0459(8) Uani 1 1 d . . . . .
S1 S 0.28651(16) 0.33099(11) 0.38515(2) 0.0298(2) Uani 1 1 d D . . . .
S2 S 0.46728(14) 0.42467(10) 0.35205(2) 0.0277(2) Uani 1 1 d . . . . .
C30 C 0.5069(8) 0.3383(6) 0.40098(7) 0.0362(12) Uani 0.855(9) 1 d D . P B 1
F20 F 0.4532(8) 0.3628(5) 0.41852(5) 0.0556(13) Uani 0.855(9) 1 d D . P B 1
F21 F 0.6306(7) 0.4537(4) 0.39635(6) 0.0493(11) Uani 0.855(9) 1 d D . P B 1
F22 F 0.6122(7) 0.2054(5) 0.40063(7) 0.0483(12) Uani 0.855(9) 1 d D . P B 1
C30A C 0.449(3) 0.338(3) 0.4062(2) 0.0362(12) Uani 0.145(9) 1 d D . P B 2
F20A F 0.337(5) 0.354(3) 0.4213(3) 0.0556(13) Uani 0.145(9) 1 d D . P B 2
F21A F 0.559(4) 0.464(3) 0.4019(4) 0.0493(11) Uani 0.145(9) 1 d D . P B 2
F22A F 0.553(5) 0.204(3) 0.4055(5) 0.0483(12) Uani 0.145(9) 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.398(5) . ?
C1 C6 1.389(5) . ?
C1 O1 1.359(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(5) . ?
C4 C5 1.396(5) . ?
C4 C7 1.468(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.382(5) . ?
C6 H6 0.9500 . ?
C7 N1 1.321(4) . ?
C7 N3 1.345(4) . ?
C8 C11 1.499(5) . ?
C8 N2 1.302(4) . ?
C8 N3 1.365(4) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 N1 1.456(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N3 1.466(4) . ?
C11 C12 1.551(5) . ?
C11 F1 1.350(4) . ?
C11 F2 1.347(4) . ?
C12 C13 1.551(5) . ?
C12 F3 1.347(4) . ?
C12 F4 1.341(4) . ?
C13 C14 1.549(5) . ?
C13 F5 1.350(4) . ?
C13 F6 1.338(4) . ?
C14 C15 1.548(5) . ?
C14 F7 1.341(4) . ?
C14 F8 1.339(4) . ?
C15 C16 1.552(6) . ?
C15 F9 1.345(6) . ?
C15 F10 1.347(6) . ?
C15 C16A 1.541(16) . ?
C15 F9A 1.345(10) . ?
C15 F10A 1.344(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.508(5) . ?
C20 O1 1.441(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.527(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.522(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.524(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.525(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.523(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.530(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.520(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.528(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N1 N2 1.358(4) . ?
C16 C17 1.552(7) . ?
C16 F11 1.342(6) . ?
C16 F12 1.342(7) . ?
C17 C18 1.551(7) . ?
C17 F13 1.344(7) . ?
C17 F14 1.343(6) . ?
C18 C19 1.535(7) . ?
C18 F15 1.346(6) . ?
C18 F16 1.297(9) . ?
C19 F17 1.309(7) . ?
C19 F18 1.311(7) . ?
C19 F19 1.326(7) . ?
C16A C17A 1.538(16) . ?
C16A F11A 1.345(10) . ?
C16A F12A 1.348(10) . ?
C17A C18A 1.542(16) . ?
C17A F13A 1.346(10) . ?
C17A F14A 1.347(10) . ?
C18A C19A 1.515(16) . ?
C18A F15A 1.342(10) . ?
C18A F16A 1.352(11) . ?
C19A F17A 1.344(10) . ?
C19A F18A 1.347(10) . ?
C19A F19A 1.348(10) . ?
C31 F23 1.328(5) . ?
C31 F24 1.334(4) . ?
C31 F25 1.329(5) . ?
C31 S2 1.831(4) . ?
N4 S1 1.567(3) . ?
N4 S2 1.580(3) . ?
O2 S1 1.432(3) . ?
O3 S1 1.435(3) . ?
O4 S2 1.437(3) . ?
O5 S2 1.421(3) . ?
S1 C30 1.838(5) . ?
S1 C30A 1.837(7) . ?
C30 F20 1.332(5) . ?
C30 F21 1.337(5) . ?
C30 F22 1.338(5) . ?
C30A F20A 1.339(10) . ?
C30A F21A 1.342(10) . ?
C30A F22A 1.343(10) . ?

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
C6 C1 C2 120.6(3) . . ?
O1 C1 C2 124.1(3) . . ?
O1 C1 C6 115.3(3) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 C7 120.6(3) . . ?
C5 C4 C7 119.2(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 H6 120.0 . . ?
N1 C7 C4 127.4(3) . . ?
N1 C7 N3 106.4(3) . . ?
N3 C7 C4 126.1(3) . . ?
N2 C8 C11 125.8(3) . . ?
N2 C8 N3 111.6(3) . . ?
N3 C8 C11 122.4(3) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
C8 C11 C12 114.7(3) . . ?
F1 C11 C8 109.8(3) . . ?
F1 C11 C12 107.3(3) . . ?
F2 C11 C8 108.3(3) . . ?
F2 C11 C12 108.7(3) . . ?
F2 C11 F1 107.8(3) . . ?
C11 C12 C13 114.2(3) . . ?
F3 C12 C11 108.2(3) . . ?
F3 C12 C13 107.8(3) . . ?
F4 C12 C11 108.0(3) . . ?
F4 C12 C13 109.9(3) . . ?
F4 C12 F3 108.6(3) . . ?
C14 C13 C12 113.9(3) . . ?
F5 C13 C12 107.8(3) . . ?
F5 C13 C14 108.5(3) . . ?
F6 C13 C12 109.5(3) . . ?
F6 C13 C14 108.8(3) . . ?
F6 C13 F5 108.1(3) . . ?
C13 C14 C15 114.8(3) . . ?
F7 C14 C13 108.3(3) . . ?
F7 C14 C15 108.5(3) . . ?
F8 C14 C13 107.7(3) . . ?
F8 C14 C15 108.9(3) . . ?
F8 C14 F7 108.5(3) . . ?
C14 C15 C16 114.6(4) . . ?
F9 C15 C14 109.8(4) . . ?
F9 C15 C16 109.1(4) . . ?
F9 C15 F10 107.5(4) . . ?
F10 C15 C14 106.6(5) . . ?
F10 C15 C16 109.0(6) . . ?
C16A C15 C14 115.5(7) . . ?
F9A C15 C14 103.5(11) . . ?
F9A C15 C16A 106.0(12) . . ?
F10A C15 C14 113.5(18) . . ?
F10A C15 C16A 106(2) . . ?
F10A C15 F9A 112.2(16) . . ?
H20A C20 H20B 108.7 . . ?
C21 C20 H20A 110.6 . . ?
C21 C20 H20B 110.6 . . ?
O1 C20 H20A 110.6 . . ?
O1 C20 H20B 110.6 . . ?
O1 C20 C21 105.8(3) . . ?
C20 C21 H21A 108.7 . . ?
C20 C21 H21B 108.7 . . ?
C20 C21 C22 114.2(3) . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 111.0(3) . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C22 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
C22 C23 C24 114.2(3) . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C23 C24 C25 113.1(3) . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C24 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 C24 113.7(3) . . ?
C26 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
C25 C26 C27 113.9(3) . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C26 113.2(3) . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 109.0 . . ?
C27 C28 H28B 109.0 . . ?
C27 C28 C29 113.1(3) . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C7 N1 C9 128.2(3) . . ?
C7 N1 N2 111.8(3) . . ?
N2 N1 C9 120.0(3) . . ?
C8 N2 N1 104.1(3) . . ?
C7 N3 C8 106.1(3) . . ?
C7 N3 C10 126.7(3) . . ?
C8 N3 C10 127.2(3) . . ?
C1 O1 C20 118.5(3) . . ?
C15 C16 C17 115.8(5) . . ?
F11 C16 C15 107.5(4) . . ?
F11 C16 C17 108.5(4) . . ?
F12 C16 C15 108.5(4) . . ?
F12 C16 C17 107.4(5) . . ?
F12 C16 F11 108.9(5) . . ?
C18 C17 C16 114.9(5) . . ?
F13 C17 C16 109.8(5) . . ?
F13 C17 C18 107.4(5) . . ?
F14 C17 C16 108.2(5) . . ?
F14 C17 C18 108.1(5) . . ?
F14 C17 F13 108.2(5) . . ?
C19 C18 C17 117.3(5) . . ?
F15 C18 C17 108.3(4) . . ?
F15 C18 C19 106.6(4) . . ?
F16 C18 C17 108.9(10) . . ?
F16 C18 C19 110.0(11) . . ?
F16 C18 F15 105.0(9) . . ?
F17 C19 C18 109.1(5) . . ?
F17 C19 F18 108.4(6) . . ?
F17 C19 F19 111.0(6) . . ?
F18 C19 C18 110.3(5) . . ?
F18 C19 F19 108.1(5) . . ?
F19 C19 C18 110.0(5) . . ?
C17A C16A C15 116.1(12) . . ?
F11A C16A C15 109.3(12) . . ?
F11A C16A C17A 109.9(13) . . ?
F11A C16A F12A 105.8(13) . . ?
F12A C16A C15 106.8(12) . . ?
F12A C16A C17A 108.3(12) . . ?
C16A C17A C18A 113.1(13) . . ?
F13A C17A C16A 107.4(14) . . ?
F13A C17A C18A 109.8(13) . . ?
F13A C17A F14A 110.1(16) . . ?
F14A C17A C16A 106.7(14) . . ?
F14A C17A C18A 109.6(15) . . ?
C19A C18A C17A 113.2(15) . . ?
F15A C18A C17A 108.5(12) . . ?
F15A C18A C19A 106.4(12) . . ?
F15A C18A F16A 98(4) . . ?
F16A C18A C17A 120(3) . . ?
F16A C18A C19A 108(3) . . ?
F17A C19A C18A 113.4(12) . . ?
F17A C19A F18A 106.1(14) . . ?
F17A C19A F19A 110.4(16) . . ?
F18A C19A C18A 113.1(15) . . ?
F18A C19A F19A 100.2(16) . . ?
F19A C19A C18A 112.6(16) . . ?
F23 C31 F24 108.1(3) . . ?
F23 C31 F25 108.3(3) . . ?
F23 C31 S2 109.7(3) . . ?
F24 C31 S2 111.2(3) . . ?
F25 C31 F24 108.1(3) . . ?
F25 C31 S2 111.3(3) . . ?
S1 N4 S2 126.5(2) . . ?
N4 S1 C30 99.5(2) . . ?
N4 S1 C30A 116.3(9) . . ?
O2 S1 N4 116.61(18) . . ?
O2 S1 O3 119.02(19) . . ?
O2 S1 C30 105.7(2) . . ?
O2 S1 C30A 98.9(8) . . ?
O3 S1 N4 107.85(18) . . ?
O3 S1 C30 105.7(2) . . ?
O3 S1 C30A 96.4(8) . . ?
N4 S2 C31 99.81(18) . . ?
O4 S2 C31 104.63(18) . . ?
O4 S2 N4 116.65(18) . . ?
O5 S2 C31 103.7(2) . . ?
O5 S2 N4 110.66(19) . . ?
O5 S2 O4 118.42(18) . . ?
F20 C30 S1 110.6(3) . . ?
F20 C30 F21 107.7(4) . . ?
F20 C30 F22 108.0(4) . . ?
F21 C30 S1 111.5(4) . . ?
F21 C30 F22 106.8(4) . . ?
F22 C30 S1 112.1(4) . . ?
F20A C30A S1 109.2(13) . . ?
F20A C30A F21A 115(2) . . ?
F20A C30A F22A 115(2) . . ?
F21A C30A S1 98.9(15) . . ?
F21A C30A F22A 113(2) . . ?
F22A C30A S1 103.7(19) . . ?

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
C1 C2 C3 C4 0.3(5) . . . . ?
C2 C1 C6 C5 1.4(6) . . . . ?
C2 C1 O1 C20 -22.9(5) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C2 C3 C4 C7 -176.4(3) . . . . ?
C3 C4 C5 C6 -1.2(5) . . . . ?
C3 C4 C7 N1 -117.3(4) . . . . ?
C3 C4 C7 N3 65.8(5) . . . . ?
C4 C5 C6 C1 0.0(6) . . . . ?
C4 C7 N1 C9 4.0(6) . . . . ?
C4 C7 N1 N2 -177.6(3) . . . . ?
C4 C7 N3 C8 177.5(3) . . . . ?
C4 C7 N3 C10 -0.5(6) . . . . ?
C5 C4 C7 N1 65.1(5) . . . . ?
C5 C4 C7 N3 -111.7(4) . . . . ?
C6 C1 C2 C3 -1.5(5) . . . . ?
C6 C1 O1 C20 155.9(3) . . . . ?
C7 C4 C5 C6 176.3(3) . . . . ?
C7 N1 N2 C8 0.3(4) . . . . ?
C8 C11 C12 C13 170.2(3) . . . . ?
C8 C11 C12 F3 50.1(4) . . . . ?
C8 C11 C12 F4 -67.3(4) . . . . ?
C9 N1 N2 C8 178.8(3) . . . . ?
C11 C8 N2 N1 175.6(3) . . . . ?
C11 C8 N3 C7 -175.9(3) . . . . ?
C11 C8 N3 C10 2.1(6) . . . . ?
C11 C12 C13 C14 161.7(3) . . . . ?
C11 C12 C13 F5 -77.8(4) . . . . ?
C11 C12 C13 F6 39.6(4) . . . . ?
C12 C13 C14 C15 166.2(3) . . . . ?
C12 C13 C14 F7 44.8(4) . . . . ?
C12 C13 C14 F8 -72.4(4) . . . . ?
C13 C14 C15 C16 171.4(3) . . . . ?
C13 C14 C15 F9 -65.4(4) . . . . ?
C13 C14 C15 F10 50.7(6) . . . . ?
C13 C14 C15 C16A 160.3(7) . . . . ?
C13 C14 C15 F9A -84.3(9) . . . . ?
C13 C14 C15 F10A 37.6(18) . . . . ?
C14 C15 C16 C17 178.4(4) . . . . ?
C14 C15 C16 F11 56.9(5) . . . . ?
C14 C15 C16 F12 -60.7(5) . . . . ?
C14 C15 C16A C17A 157.5(8) . . . . ?
C14 C15 C16A F11A 32.5(14) . . . . ?
C14 C15 C16A F12A -81.6(11) . . . . ?
C15 C16 C17 C18 -175.4(4) . . . . ?
C15 C16 C17 F13 -54.3(6) . . . . ?
C15 C16 C17 F14 63.6(6) . . . . ?
C15 C16A C17A C18A 158.7(10) . . . . ?
C15 C16A C17A F13A -80.0(14) . . . . ?
C15 C16A C17A F14A 38.1(16) . . . . ?
C20 C21 C22 C23 177.7(3) . . . . ?
C21 C20 O1 C1 -165.7(3) . . . . ?
C21 C22 C23 C24 -178.4(3) . . . . ?
C22 C23 C24 C25 177.5(3) . . . . ?
C23 C24 C25 C26 178.6(3) . . . . ?
C24 C25 C26 C27 179.9(3) . . . . ?
C25 C26 C27 C28 178.3(3) . . . . ?
C26 C27 C28 C29 -178.9(3) . . . . ?
F1 C11 C12 C13 47.9(4) . . . . ?
F1 C11 C12 F3 -72.1(3) . . . . ?
F1 C11 C12 F4 170.4(3) . . . . ?
F2 C11 C12 C13 -68.5(4) . . . . ?
F2 C11 C12 F3 171.5(3) . . . . ?
F2 C11 C12 F4 54.1(4) . . . . ?
F3 C12 C13 C14 -78.0(4) . . . . ?
F3 C12 C13 F5 42.5(4) . . . . ?
F3 C12 C13 F6 159.9(3) . . . . ?
F4 C12 C13 C14 40.2(4) . . . . ?
F4 C12 C13 F5 160.7(3) . . . . ?
F4 C12 C13 F6 -81.9(4) . . . . ?
F5 C13 C14 C15 46.1(4) . . . . ?
F5 C13 C14 F7 -75.3(4) . . . . ?
F5 C13 C14 F8 167.5(3) . . . . ?
F6 C13 C14 C15 -71.3(4) . . . . ?
F6 C13 C14 F7 167.3(3) . . . . ?
F6 C13 C14 F8 50.1(4) . . . . ?
F7 C14 C15 C16 -67.3(4) . . . . ?
F7 C14 C15 F9 55.8(4) . . . . ?
F7 C14 C15 F10 172.0(5) . . . . ?
F7 C14 C15 C16A -78.4(7) . . . . ?
F7 C14 C15 F9A 37.0(9) . . . . ?
F7 C14 C15 F10A 158.8(17) . . . . ?
F8 C14 C15 C16 50.6(4) . . . . ?
F8 C14 C15 F9 173.7(3) . . . . ?
F8 C14 C15 F10 -70.1(5) . . . . ?
F8 C14 C15 C16A 39.5(7) . . . . ?
F8 C14 C15 F9A 154.9(9) . . . . ?
F8 C14 C15 F10A -83.3(17) . . . . ?
N1 C7 N3 C8 0.2(4) . . . . ?
N1 C7 N3 C10 -177.9(3) . . . . ?
N2 C8 C11 C12 8.6(5) . . . . ?
N2 C8 C11 F1 129.5(3) . . . . ?
N2 C8 C11 F2 -113.0(4) . . . . ?
N2 C8 N3 C7 0.0(4) . . . . ?
N2 C8 N3 C10 178.0(3) . . . . ?
N3 C7 N1 C9 -178.6(3) . . . . ?
N3 C7 N1 N2 -0.3(4) . . . . ?
N3 C8 C11 C12 -176.1(3) . . . . ?
N3 C8 C11 F1 -55.2(4) . . . . ?
N3 C8 C11 F2 62.3(4) . . . . ?
N3 C8 N2 N1 -0.2(4) . . . . ?
O1 C1 C2 C3 177.2(3) . . . . ?
O1 C1 C6 C5 -177.4(3) . . . . ?
O1 C20 C21 C22 -179.6(3) . . . . ?
C16 C17 C18 C19 -177.6(5) . . . . ?
C16 C17 C18 F15 61.8(6) . . . . ?
C16 C17 C18 F16 -51.9(11) . . . . ?
C17 C18 C19 F17 179.2(5) . . . . ?
C17 C18 C19 F18 60.2(7) . . . . ?
C17 C18 C19 F19 -58.9(8) . . . . ?
F9 C15 C16 C17 54.9(6) . . . . ?
F9 C15 C16 F11 -66.6(6) . . . . ?
F9 C15 C16 F12 175.7(4) . . . . ?
F10 C15 C16 C17 -62.2(6) . . . . ?
F10 C15 C16 F11 176.3(5) . . . . ?
F10 C15 C16 F12 58.6(6) . . . . ?
F11 C16 C17 C18 -54.5(6) . . . . ?
F11 C16 C17 F13 66.6(6) . . . . ?
F11 C16 C17 F14 -175.5(4) . . . . ?
F12 C16 C17 C18 63.1(6) . . . . ?
F12 C16 C17 F13 -175.7(4) . . . . ?
F12 C16 C17 F14 -57.8(6) . . . . ?
F13 C17 C18 C19 59.9(7) . . . . ?
F13 C17 C18 F15 -60.7(6) . . . . ?
F13 C17 C18 F16 -174.4(11) . . . . ?
F14 C17 C18 C19 -56.7(7) . . . . ?
F14 C17 C18 F15 -177.3(4) . . . . ?
F14 C17 C18 F16 69.0(11) . . . . ?
F15 C18 C19 F17 -59.3(7) . . . . ?
F15 C18 C19 F18 -178.3(5) . . . . ?
F15 C18 C19 F19 62.6(6) . . . . ?
F16 C18 C19 F17 54.1(11) . . . . ?
F16 C18 C19 F18 -64.9(11) . . . . ?
F16 C18 C19 F19 175.9(10) . . . . ?
C16A C17A C18A C19A 161.2(12) . . . . ?
C16A C17A C18A F15A -80.9(16) . . . . ?
C16A C17A C18A F16A 30(4) . . . . ?
C17A C18A C19A F17A -71.9(19) . . . . ?
C17A C18A C19A F18A 167.2(14) . . . . ?
C17A C18A C19A F19A 54.5(16) . . . . ?
F9A C15 C16A C17A 43.6(15) . . . . ?
F9A C15 C16A F11A -81.5(16) . . . . ?
F9A C15 C16A F12A 164.5(14) . . . . ?
F10A C15 C16A C17A -75.9(18) . . . . ?
F10A C15 C16A F11A 159.1(17) . . . . ?
F10A C15 C16A F12A 45.1(19) . . . . ?
F11A C16A C17A C18A -76.6(15) . . . . ?
F11A C16A C17A F13A 44.7(17) . . . . ?
F11A C16A C17A F14A 162.8(13) . . . . ?
F12A C16A C17A C18A 38.5(15) . . . . ?
F12A C16A C17A F13A 159.8(13) . . . . ?
F12A C16A C17A F14A -82.1(16) . . . . ?
F13A C17A C18A C19A 41.3(19) . . . . ?
F13A C17A C18A F15A 159.2(14) . . . . ?
F13A C17A C18A F16A -89(4) . . . . ?
F14A C17A C18A C19A -79.8(16) . . . . ?
F14A C17A C18A F15A 38(2) . . . . ?
F14A C17A C18A F16A 149(4) . . . . ?
F15A C18A C19A F17A 169.0(14) . . . . ?
F15A C18A C19A F18A 48(2) . . . . ?
F15A C18A C19A F19A -64.6(18) . . . . ?
F16A C18A C19A F17A 65(4) . . . . ?
F16A C18A C19A F18A -56(4) . . . . ?
F16A C18A C19A F19A -169(4) . . . . ?
F23 C31 S2 N4 176.8(3) . . . . ?
F23 C31 S2 O4 55.8(3) . . . . ?
F23 C31 S2 O5 -68.9(3) . . . . ?
F24 C31 S2 N4 -63.6(3) . . . . ?
F24 C31 S2 O4 175.4(3) . . . . ?
F24 C31 S2 O5 50.6(3) . . . . ?
F25 C31 S2 N4 57.0(3) . . . . ?
F25 C31 S2 O4 -64.1(3) . . . . ?
F25 C31 S2 O5 171.2(3) . . . . ?
N4 S1 C30 F20 -178.8(3) . . . . ?
N4 S1 C30 F21 61.4(4) . . . . ?
N4 S1 C30 F22 -58.2(4) . . . . ?
N4 S1 C30A F20A -175.0(16) . . . . ?
N4 S1 C30A F21A 64.1(17) . . . . ?
N4 S1 C30A F22A -51.9(19) . . . . ?
O2 S1 C30 F20 60.0(4) . . . . ?
O2 S1 C30 F21 -59.9(4) . . . . ?
O2 S1 C30 F22 -179.5(3) . . . . ?
O2 S1 C30A F20A 59.4(18) . . . . ?
O2 S1 C30A F21A -61.6(16) . . . . ?
O2 S1 C30A F22A -177.5(17) . . . . ?
O3 S1 C30 F20 -67.1(4) . . . . ?
O3 S1 C30 F21 173.1(3) . . . . ?
O3 S1 C30 F22 53.5(4) . . . . ?
O3 S1 C30A F20A -61.4(18) . . . . ?
O3 S1 C30A F21A 177.7(15) . . . . ?
O3 S1 C30A F22A 61.7(18) . . . . ?
S1 N4 S2 C31 -116.4(3) . . . . ?
S1 N4 S2 O4 -4.4(4) . . . . ?
S1 N4 S2 O5 134.9(3) . . . . ?
S2 N4 S1 O2 22.4(4) . . . . ?
S2 N4 S1 O3 159.4(2) . . . . ?
S2 N4 S1 C30 -90.6(3) . . . . ?
S2 N4 S1 C30A -93.8(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-14
_olex2_date_sample_submission    2016-11-09
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id ALR14
_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 1.251
_oxdiff_exptl_absorpt_empirical_full_min 0.837
####################################################################### 
# 
# 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_dwb1677b
_database_code_depnum_ccdc_archive 'CCDC 2177836'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H39 F19 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C35 H39 F25 N4 O5 S2'
_chemical_formula_weight         1134.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C35 H39 F24 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio ALR16 rpt at 220C'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.75057(18)
_cell_length_b                   8.6616(2)
_cell_length_c                   78.211(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.192(2)
_cell_angle_gamma                90
_cell_volume                     4572.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7515
_cell_measurement_temperature    220.00(14)
_cell_measurement_theta_max      70.3810
_cell_measurement_theta_min      5.1950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0121
0 0 1 0.0091
1 0 -1 0.1740
-4 0 3 0.1847
0 -1 1 0.0268
0 1 -1 0.0432

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Evaporation of acetone/hexane'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.021
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
-0.0000 -0.0001 -0.9999 0.0101 0.0167 -0.0029
0.0000 0.0001 0.9999 -0.0101 -0.0167 0.0029
0.9999 -0.0002 -0.9997 -0.1851 0.1191 -0.0619
-3.9995 0.0005 2.9989 0.7504 -0.4597 0.2448
-0.0002 -1.0000 0.9998 -0.0370 0.0296 0.1726
0.0002 1.0000 -0.9998 0.0370 -0.0296 -0.1726

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       93
_diffrn_reflns_limit_l_min       -92
_diffrn_reflns_number            32878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         4.524
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  72.00   0.75    1.50    --    0.00  57.00-150.00  136
  2  ω    -86.00 -35.00   0.75    1.50    --    0.00-178.00 150.00   68
  3  ω   -136.00 -80.50   0.75    6.00    --  -56.36 -94.00 150.00   74
  4  ω    -95.00  -2.00   0.75    6.00    --  -56.36 125.00-180.00  124
  5  ω   -133.00 -73.00   0.75    6.00    --  -56.36-125.00  60.00   80
  6  ω    -15.00  85.50   0.75    6.00    --   56.36 -61.00-120.00  134
  7  ω     70.00 136.00   0.75    6.00    --   56.36 162.00-107.00   88
  8  ω     21.00 132.00   0.75    6.00    --   56.36  45.00  30.00  148
  9  ω     82.00 178.00   0.75    6.00    --  112.72  63.00 -60.00  128
 10  ω     41.00 143.00   0.75    6.00    --  112.72 -63.00-150.00  136
 11  ω     34.00 115.00   0.75    6.00    --  112.72-111.00   0.00  108
 12  ω    100.00 178.00   0.75    6.00    --  112.72 111.00-120.00  104
 13  ω     34.00 115.00   0.75    6.00    --  112.72-111.00-180.00  108
 14  ω    100.00 178.00   0.75    6.00    --  112.72 111.00  60.00  104
 15  ω     34.00 115.00   0.75    6.00    --  112.72-111.00  60.00  108
 16  ω     50.00 177.50   0.75    6.00    --  112.72  25.00  60.00  170
 17  ω     38.00 143.00   0.75    6.00    --  112.72 -50.00 -30.00  140
 18  ω    -86.00 -35.00   0.75    1.50    --    0.00-178.00 -60.00   68
 19  ω    -75.00  36.00   0.75    1.50    --    0.00 -77.00  90.00  148
 20  ω   -135.00  -6.00   0.75    6.00    --  -56.36 -30.00-150.00  172
 21  ω   -133.00 -73.00   0.75    6.00    --  -56.36-125.00 -60.00   80
 22  ω    -95.00  -2.00   0.75    6.00    --  -56.36 125.00 -30.00  124
 23  ω   -136.00 -80.50   0.75    6.00    --  -56.36 -94.00   0.00   74
 24  ω     20.00 131.00   0.75    6.00    --   56.36  77.00  60.00  148
 25  ω     26.00 128.00   0.75    6.00    --   56.36  61.00 150.00  136
 26  ω     82.00 119.50   0.75    6.00    --  112.72  50.00 120.00   50
 27  ω    100.00 178.00   0.75    6.00    --  112.72 111.00 -30.00  104
 28  ω     50.00 177.50   0.75    6.00    --  112.72  25.00-150.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1951997000
_diffrn_orient_matrix_UB_12      0.0269372000
_diffrn_orient_matrix_UB_13      -0.0101143000
_diffrn_orient_matrix_UB_21      0.1024362000
_diffrn_orient_matrix_UB_22      -0.0462885000
_diffrn_orient_matrix_UB_23      -0.0166544000
_diffrn_orient_matrix_UB_31      -0.0590350000
_diffrn_orient_matrix_UB_32      -0.1696095000
_diffrn_orient_matrix_UB_33      0.0029413000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6582
_reflns_number_total             8131
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         8131
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0718
_refine_ls_restrained_S_all      1.068
_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)+(0.0302P)²+10.1459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1479
_refine_special_details          
;
The perfluoroalkyl chain was disordered.  The end of this chain was modelled
in two positions with refined occupancies of 0.745:0.255(3).  A two site 
model was used for the two terminal carbons and the fluorines of the 
trifluoromethyl and 3 difluoromethylenes were also modelled in two positions.
The ADP of closely-proximate atomes were constrained to be equal, ie. C19 & C19A,
C18 & C18A, F13 & F14A, F16 & F15A, F17 & F19A and F19 & F18A. The terminal 
C18-C19 bond lengths were restrained to be equal.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F13) = Uanis(F14A)
Uanis(F17) = Uanis(F19A)
Uanis(F19) = Uanis(F18A)
Uanis(C19) = Uanis(C19A)
Uanis(C18) = Uanis(C18A)
Uanis(F16) = Uanis(F15A)
4. Others
 Sof(C18A)=Sof(C19A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=
 Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=1-FVAR(1)
 Sof(C18)=Sof(C19)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=
 Sof(F17)=Sof(F18)=Sof(F19)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3232(5) 0.3938(4) 0.33955(4) 0.0329(8) Uani 1 1 d . . . . .
C2 C 0.3581(5) 0.2479(4) 0.34610(4) 0.0331(8) Uani 1 1 d . . . . .
H2 H 0.301375 0.161629 0.340883 0.040 Uiso 1 1 calc R U . . .
C3 C 0.4792(5) 0.2316(4) 0.36062(4) 0.0316(8) Uani 1 1 d . . . . .
H3 H 0.502378 0.134268 0.365270 0.038 Uiso 1 1 calc R U . . .
C4 C 0.5653(4) 0.3613(4) 0.36812(4) 0.0276(7) Uani 1 1 d . . . . .
C5 C 0.5323(5) 0.5070(4) 0.36118(5) 0.0383(9) Uani 1 1 d . . . . .
H5 H 0.591430 0.593246 0.366186 0.046 Uiso 1 1 calc R U . . .
C6 C 0.4112(5) 0.5232(4) 0.34683(5) 0.0402(9) Uani 1 1 d . . . . .
H6 H 0.389016 0.620339 0.342097 0.048 Uiso 1 1 calc R U . . .
C7 C 0.6858(5) 0.3474(4) 0.38399(4) 0.0273(7) Uani 1 1 d . . . . .
C8 C 0.7800(5) 0.3156(4) 0.41030(4) 0.0297(7) Uani 1 1 d . . . . .
C9 C 0.4171(5) 0.2597(6) 0.40342(5) 0.0569(13) Uani 1 1 d . . . . .
H9A H 0.420887 0.168704 0.410425 0.085 Uiso 1 1 calc R U . . .
H9B H 0.344190 0.238493 0.393018 0.085 Uiso 1 1 calc R U . . .
H9C H 0.353611 0.341775 0.409475 0.085 Uiso 1 1 calc R U . . .
C10 C 1.0149(5) 0.4302(4) 0.37314(4) 0.0316(8) Uani 1 1 d . . . . .
H10A H 1.076636 0.525002 0.376722 0.047 Uiso 1 1 calc R U . . .
H10B H 0.945747 0.445989 0.362429 0.047 Uiso 1 1 calc R U . . .
H10C H 1.114418 0.352219 0.371791 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7649(5) 0.2874(5) 0.42916(4) 0.0358(8) Uani 1 1 d . . . . .
C12 C 0.9619(5) 0.2986(4) 0.43943(4) 0.0330(8) Uani 1 1 d . . . . .
C13 C 0.9500(5) 0.2444(5) 0.45828(4) 0.0371(9) Uani 1 1 d . . . . .
C14 C 1.1247(5) 0.2986(5) 0.46985(4) 0.0354(8) Uani 1 1 d . . . . .
C15 C 1.1400(5) 0.2191(5) 0.48752(4) 0.0370(8) Uani 1 1 d . . . . .
C16 C 1.2897(6) 0.2918(5) 0.50020(5) 0.0423(9) Uani 1 1 d . . . . .
C17 C 1.3266(6) 0.2081(5) 0.51724(5) 0.0413(9) Uani 1 1 d . . . . .
C18A C 1.397(3) 0.292(3) 0.5324(3) 0.0472(17) Uani 0.255(3) 1 d D . P A 2
C19A C 1.556(5) 0.206(6) 0.5430(4) 0.055(2) Uani 0.255(3) 1 d D . P A 2
C20 C 0.0492(5) 0.3109(4) 0.32141(4) 0.0365(8) Uani 1 1 d . . . . .
H20A H -0.019567 0.277042 0.331508 0.044 Uiso 1 1 calc R U . . .
H20B H 0.108041 0.221717 0.315996 0.044 Uiso 1 1 calc R U . . .
C21 C -0.0916(6) 0.3922(5) 0.30915(5) 0.0411(9) Uani 1 1 d . . . . .
H21A H -0.018227 0.427354 0.299355 0.049 Uiso 1 1 calc R U . . .
H21B H -0.144773 0.482556 0.314765 0.049 Uiso 1 1 calc R U . . .
C22 C -0.2627(5) 0.2914(4) 0.30290(5) 0.0367(8) Uani 1 1 d . . . . .
H22A H -0.340901 0.259991 0.312564 0.044 Uiso 1 1 calc R U . . .
H22B H -0.210798 0.199039 0.297593 0.044 Uiso 1 1 calc R U . . .
C23 C -0.3945(5) 0.3775(4) 0.29003(5) 0.0391(9) Uani 1 1 d . . . . .
H23A H -0.447594 0.468391 0.295553 0.047 Uiso 1 1 calc R U . . .
H23B H -0.313390 0.412498 0.280694 0.047 Uiso 1 1 calc R U . . .
C24 C -0.5660(5) 0.2835(4) 0.28264(5) 0.0362(8) Uani 1 1 d . . . . .
H24A H -0.650132 0.251086 0.291882 0.043 Uiso 1 1 calc R U . . .
H24B H -0.513960 0.191297 0.277306 0.043 Uiso 1 1 calc R U . . .
C25 C -0.6902(5) 0.3722(4) 0.26952(5) 0.0362(8) Uani 1 1 d . . . . .
H25A H -0.739863 0.465256 0.274849 0.043 Uiso 1 1 calc R U . . .
H25B H -0.605832 0.403433 0.260251 0.043 Uiso 1 1 calc R U . . .
C26 C -0.8646(5) 0.2817(4) 0.26211(5) 0.0365(8) Uani 1 1 d . . . . .
H26A H -0.948417 0.249307 0.271373 0.044 Uiso 1 1 calc R U . . .
H26B H -0.815151 0.189431 0.256610 0.044 Uiso 1 1 calc R U . . .
C27 C -0.9892(5) 0.3733(4) 0.24916(5) 0.0362(8) Uani 1 1 d . . . . .
H27A H -1.037926 0.465837 0.254651 0.043 Uiso 1 1 calc R U . . .
H27B H -0.905353 0.405298 0.239879 0.043 Uiso 1 1 calc R U . . .
C28 C -1.1646(5) 0.2835(4) 0.24175(5) 0.0359(8) Uani 1 1 d . . . . .
H28A H -1.249469 0.252911 0.251016 0.043 Uiso 1 1 calc R U . . .
H28B H -1.115970 0.190144 0.236421 0.043 Uiso 1 1 calc R U . . .
C29 C -1.2873(5) 0.3740(4) 0.22861(5) 0.0374(8) Uani 1 1 d . . . . .
H29A H -1.335704 0.467539 0.233909 0.045 Uiso 1 1 calc R U . . .
H29B H -1.202873 0.404011 0.219295 0.045 Uiso 1 1 calc R U . . .
C30 C -1.4625(5) 0.2831(4) 0.22140(5) 0.0387(9) Uani 1 1 d . . . . .
H30A H -1.546327 0.253032 0.230757 0.046 Uiso 1 1 calc R U . . .
H30B H -1.413525 0.189354 0.216172 0.046 Uiso 1 1 calc R U . . .
C31 C -1.5874(6) 0.3707(5) 0.20823(5) 0.0406(9) Uani 1 1 d . . . . .
H31A H -1.634189 0.465579 0.213340 0.049 Uiso 1 1 calc R U . . .
H31B H -1.504820 0.398312 0.198698 0.049 Uiso 1 1 calc R U . . .
C32 C -1.7642(6) 0.2793(5) 0.20153(5) 0.0458(10) Uani 1 1 d . . . . .
H32A H -1.845364 0.250170 0.211094 0.055 Uiso 1 1 calc R U . . .
H32B H -1.717030 0.185135 0.196272 0.055 Uiso 1 1 calc R U . . .
C33 C -1.8924(7) 0.3672(6) 0.18850(6) 0.0575(12) Uani 1 1 d . . . . .
H33A H -1.937587 0.461685 0.193505 0.086 Uiso 1 1 calc R U . . .
H33B H -2.004537 0.304974 0.185188 0.086 Uiso 1 1 calc R U . . .
H33C H -1.815851 0.390054 0.178608 0.086 Uiso 1 1 calc R U . . .
F1 F 0.6873(3) 0.1469(3) 0.43190(3) 0.0571(7) Uani 1 1 d . . . . .
F2 F 0.6383(3) 0.3923(4) 0.43548(3) 0.0643(8) Uani 1 1 d . . . . .
F3 F 1.0944(3) 0.2078(3) 0.43168(3) 0.0486(6) Uani 1 1 d . . . . .
F4 F 1.0257(4) 0.4437(3) 0.43879(3) 0.0542(6) Uani 1 1 d . . . . .
F5 F 0.9468(4) 0.0901(3) 0.45832(3) 0.0588(7) Uani 1 1 d . . . . .
F6 F 0.7818(3) 0.2932(4) 0.46486(3) 0.0633(8) Uani 1 1 d . . . . .
F7 F 1.2921(3) 0.2775(4) 0.46159(3) 0.0627(8) Uani 1 1 d . . . . .
F8 F 1.1024(4) 0.4507(3) 0.47236(3) 0.0661(8) Uani 1 1 d . . . . .
F9 F 1.1913(5) 0.0726(3) 0.48516(3) 0.0731(9) Uani 1 1 d . . . . .
F10 F 0.9625(3) 0.2212(4) 0.49449(3) 0.0682(9) Uani 1 1 d . . . . .
F11A F 1.415(3) 0.370(2) 0.4937(2) 0.081(7) Uani 0.255(3) 1 d . . P A 2
F12A F 1.147(3) 0.408(2) 0.5078(2) 0.078(6) Uani 0.255(3) 1 d . . P A 2
F13A F 1.506(2) 0.1312(19) 0.51037(15) 0.095(6) Uani 0.255(3) 1 d . . P A 2
F14A F 1.210(2) 0.1014(12) 0.51981(14) 0.0622(11) Uani 0.255(3) 1 d . . P A 2
F15A F 1.488(8) 0.403(4) 0.5280(5) 0.074(2) Uani 0.255(3) 1 d . . P A 2
F16A F 1.2444(16) 0.3273(16) 0.54082(12) 0.077(4) Uani 0.255(3) 1 d . . P A 2
F17A F 1.7251(16) 0.1938(18) 0.53886(14) 0.086(4) Uani 0.255(3) 1 d . . P A 2
F18A F 1.561(4) 0.267(4) 0.5591(3) 0.105(2) Uani 0.255(3) 1 d . . P A 2
F19A F 1.462(4) 0.089(3) 0.5492(3) 0.095(2) Uani 0.255(3) 1 d . . P A 2
N1 N 0.6200(4) 0.3059(4) 0.39936(3) 0.0315(7) Uani 1 1 d . . . . .
N2 N 0.8750(4) 0.3807(3) 0.38599(3) 0.0260(6) Uani 1 1 d . . . . .
N3 N 0.9380(4) 0.3610(3) 0.40255(3) 0.0286(6) Uani 1 1 d . . . . .
O1 O 0.1990(4) 0.4234(3) 0.32587(3) 0.0461(7) Uani 1 1 d . . . . .
C18 C 1.4846(10) 0.2767(9) 0.52942(9) 0.0472(17) Uani 0.745(3) 1 d D . P A 1
C19 C 1.5130(15) 0.2046(16) 0.54720(10) 0.055(2) Uani 0.745(3) 1 d D . P A 1
C34 C 0.0227(9) -0.1700(7) 0.40981(7) 0.0748(16) Uani 1 1 d . . . . .
C35 C -0.1618(8) -0.1229(5) 0.34587(6) 0.0549(12) Uani 1 1 d . . . . .
F20 F 0.1422(6) -0.0538(4) 0.40635(5) 0.1079(13) Uani 1 1 d . . . . .
F21 F -0.0402(6) -0.1516(5) 0.42530(4) 0.1185(14) Uani 1 1 d . . . . .
F22 F 0.1261(5) -0.2992(4) 0.40919(5) 0.0989(11) Uani 1 1 d . . . . .
F23 F -0.1290(6) -0.0237(4) 0.33339(4) 0.0954(11) Uani 1 1 d . . . . .
F24 F -0.1277(5) -0.2628(3) 0.34006(4) 0.0745(8) Uani 1 1 d . . . . .
F25 F -0.3509(4) -0.1152(3) 0.34978(4) 0.0698(8) Uani 1 1 d . . . . .
N4 N -0.0761(6) -0.2014(4) 0.37728(4) 0.0525(9) Uani 1 1 d . . . . .
O2 O -0.2801(6) -0.0274(4) 0.39610(5) 0.0730(10) Uani 1 1 d . . . . .
O3 O -0.2901(5) -0.3109(4) 0.39844(4) 0.0651(9) Uani 1 1 d . . . . .
O4 O -0.0477(5) 0.0804(3) 0.36818(4) 0.0638(9) Uani 1 1 d . . . . .
O5 O 0.1903(5) -0.1122(4) 0.35861(5) 0.0828(12) Uani 1 1 d . . . . .
S1 S -0.18509(18) -0.17340(13) 0.39436(2) 0.0530(3) Uani 1 1 d . . . . .
S2 S -0.00267(16) -0.07641(12) 0.36430(2) 0.0509(3) Uani 1 1 d . . . . .
F11 F 1.4713(8) 0.2838(7) 0.49223(7) 0.0610(16) Uani 0.745(3) 1 d . . P A 1
F12 F 1.2503(9) 0.4365(6) 0.50281(7) 0.0637(16) Uani 0.745(3) 1 d . . P A 1
F13 F 1.3579(8) 0.0585(4) 0.51529(5) 0.0622(11) Uani 0.745(3) 1 d . . P A 1
F14 F 1.1473(5) 0.2197(5) 0.52558(4) 0.0620(12) Uani 0.745(3) 1 d . . P A 1
F15 F 1.6595(5) 0.2557(6) 0.52156(4) 0.0768(13) Uani 0.745(3) 1 d . . P A 1
F16 F 1.459(2) 0.4323(11) 0.53117(15) 0.074(2) Uani 0.745(3) 1 d . . P A 1
F17 F 1.5479(11) 0.0521(7) 0.54578(8) 0.095(2) Uani 0.745(3) 1 d . . P A 1
F18 F 1.3518(8) 0.2192(8) 0.55565(5) 0.120(2) Uani 0.745(3) 1 d . . P A 1
F19 F 1.6495(9) 0.2796(10) 0.55576(9) 0.105(2) Uani 0.745(3) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.383(5) . ?
C1 C6 1.386(5) . ?
C1 O1 1.369(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.392(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.389(5) . ?
C4 C5 1.390(5) . ?
C4 C7 1.474(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.382(5) . ?
C6 H6 0.9300 . ?
C7 N1 1.340(4) . ?
C7 N2 1.316(4) . ?
C8 C11 1.501(5) . ?
C8 N1 1.366(4) . ?
C8 N3 1.298(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 N1 1.468(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N2 1.458(4) . ?
C11 C12 1.542(5) . ?
C11 F1 1.344(4) . ?
C11 F2 1.348(4) . ?
C12 C13 1.551(5) . ?
C12 F3 1.345(4) . ?
C12 F4 1.330(4) . ?
C13 C14 1.545(5) . ?
C13 F5 1.337(4) . ?
C13 F6 1.325(4) . ?
C14 C15 1.545(5) . ?
C14 F7 1.326(4) . ?
C14 F8 1.341(4) . ?
C15 C16 1.537(5) . ?
C15 F9 1.329(5) . ?
C15 F10 1.327(4) . ?
C16 C17 1.533(5) . ?
C16 F11A 1.204(17) . ?
C16 F12A 1.523(17) . ?
C16 F11 1.389(7) . ?
C16 F12 1.298(7) . ?
C17 C18A 1.46(3) . ?
C17 F13A 1.491(13) . ?
C17 F14A 1.234(12) . ?
C17 C18 1.535(8) . ?
C17 F13 1.322(5) . ?
C17 F14 1.391(5) . ?
C18A C19A 1.538(18) . ?
C18A F15A 1.20(6) . ?
C18A F16A 1.27(2) . ?
C19A F17A 1.20(4) . ?
C19A F18A 1.37(5) . ?
C19A F19A 1.29(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.510(5) . ?
C20 O1 1.442(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.521(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.525(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.520(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.520(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.519(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.526(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.521(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.524(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.519(5) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.521(5) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.516(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.527(5) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
N2 N3 1.365(4) . ?
C18 C19 1.533(7) . ?
C18 F15 1.355(7) . ?
C18 F16 1.366(13) . ?
C19 F17 1.346(15) . ?
C19 F18 1.291(9) . ?
C19 F19 1.302(14) . ?
C34 F20 1.321(6) . ?
C34 F21 1.302(6) . ?
C34 F22 1.320(7) . ?
C34 S1 1.833(6) . ?
C35 F23 1.323(5) . ?
C35 F24 1.316(5) . ?
C35 F25 1.320(5) . ?
C35 S2 1.825(5) . ?
N4 S1 1.558(4) . ?
N4 S2 1.571(4) . ?
O2 S1 1.425(3) . ?
O3 S1 1.426(3) . ?
O4 S2 1.425(3) . ?
O5 S2 1.420(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 121.2(3) . . ?
O1 C1 C2 123.9(3) . . ?
O1 C1 C6 114.9(3) . . ?
C1 C2 H2 120.4 . . ?
C1 C2 C3 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C7 120.6(3) . . ?
C5 C4 C7 118.9(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 120.2 . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 H6 120.2 . . ?
N1 C7 C4 126.2(3) . . ?
N2 C7 C4 126.8(3) . . ?
N2 C7 N1 106.9(3) . . ?
N1 C8 C11 122.4(3) . . ?
N3 C8 C11 125.6(3) . . ?
N3 C8 N1 111.9(3) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
C8 C11 C12 115.2(3) . . ?
F1 C11 C8 109.8(3) . . ?
F1 C11 C12 108.0(3) . . ?
F1 C11 F2 107.4(3) . . ?
F2 C11 C8 107.9(3) . . ?
F2 C11 C12 108.3(3) . . ?
C11 C12 C13 114.5(3) . . ?
F3 C12 C11 107.6(3) . . ?
F3 C12 C13 107.4(3) . . ?
F4 C12 C11 108.4(3) . . ?
F4 C12 C13 110.2(3) . . ?
F4 C12 F3 108.4(3) . . ?
C14 C13 C12 114.3(3) . . ?
F5 C13 C12 107.8(3) . . ?
F5 C13 C14 108.3(3) . . ?
F6 C13 C12 109.5(3) . . ?
F6 C13 C14 109.0(3) . . ?
F6 C13 F5 107.7(3) . . ?
C13 C14 C15 115.1(3) . . ?
F7 C14 C13 108.7(3) . . ?
F7 C14 C15 109.4(3) . . ?
F7 C14 F8 107.8(3) . . ?
F8 C14 C13 107.3(3) . . ?
F8 C14 C15 108.2(3) . . ?
C16 C15 C14 115.2(3) . . ?
F9 C15 C14 108.3(3) . . ?
F9 C15 C16 108.1(3) . . ?
F10 C15 C14 108.5(3) . . ?
F10 C15 C16 108.5(3) . . ?
F10 C15 F9 108.1(3) . . ?
C17 C16 C15 117.4(3) . . ?
F11A C16 C15 114.7(8) . . ?
F11A C16 C17 122.0(8) . . ?
F11A C16 F12A 104.3(13) . . ?
F12A C16 C15 96.1(7) . . ?
F12A C16 C17 93.9(7) . . ?
F11 C16 C15 105.4(4) . . ?
F11 C16 C17 103.8(4) . . ?
F12 C16 C15 111.3(4) . . ?
F12 C16 C17 110.5(4) . . ?
F12 C16 F11 107.7(5) . . ?
C16 C17 C18 117.0(4) . . ?
C18A C17 C16 120.9(10) . . ?
C18A C17 F13A 105.3(10) . . ?
F13A C17 C16 90.9(6) . . ?
F14A C17 C16 113.8(6) . . ?
F14A C17 C18A 116.0(11) . . ?
F14A C17 F13A 104.5(10) . . ?
F13 C17 C16 112.7(4) . . ?
F13 C17 C18 109.9(4) . . ?
F13 C17 F14 105.6(4) . . ?
F14 C17 C16 104.3(3) . . ?
F14 C17 C18 106.3(4) . . ?
C17 C18A C19A 114(2) . . ?
F15A C18A C17 109(2) . . ?
F15A C18A C19A 101(3) . . ?
F15A C18A F16A 113(3) . . ?
F16A C18A C17 106.7(16) . . ?
F16A C18A C19A 114(2) . . ?
F17A C19A C18A 124(3) . . ?
F17A C19A F18A 106(3) . . ?
F17A C19A F19A 121(3) . . ?
F18A C19A C18A 108(3) . . ?
F19A C19A C18A 104(3) . . ?
F19A C19A F18A 88(2) . . ?
H20A C20 H20B 108.8 . . ?
C21 C20 H20A 110.6 . . ?
C21 C20 H20B 110.6 . . ?
O1 C20 H20A 110.6 . . ?
O1 C20 H20B 110.6 . . ?
O1 C20 C21 105.5(3) . . ?
C20 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C20 C21 C22 113.6(3) . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
C21 C22 C23 111.1(3) . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C22 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.7(3) . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
C23 C24 C25 113.0(3) . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 H24A 109.0 . . ?
C25 C24 H24B 109.0 . . ?
C24 C25 H25A 108.7 . . ?
C24 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 C24 114.1(3) . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C25 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
C25 C26 C27 113.4(3) . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 H26A 108.9 . . ?
C27 C26 H26B 108.9 . . ?
C26 C27 H27A 108.8 . . ?
C26 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C26 113.6(3) . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C27 C28 C29 113.7(3) . . ?
H28A C28 H28B 107.7 . . ?
C29 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C28 C29 H29A 109.0 . . ?
C28 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C30 C29 C28 113.1(3) . . ?
C30 C29 H29A 109.0 . . ?
C30 C29 H29B 109.0 . . ?
C29 C30 H30A 108.7 . . ?
C29 C30 H30B 108.7 . . ?
C29 C30 C31 114.2(3) . . ?
H30A C30 H30B 107.6 . . ?
C31 C30 H30A 108.7 . . ?
C31 C30 H30B 108.7 . . ?
C30 C31 H31A 108.9 . . ?
C30 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 C30 113.3(3) . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C31 C32 H32A 108.8 . . ?
C31 C32 H32B 108.8 . . ?
C31 C32 C33 113.7(4) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.8 . . ?
C33 C32 H32B 108.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C7 N1 C8 105.9(3) . . ?
C7 N1 C9 126.5(3) . . ?
C8 N1 C9 127.6(3) . . ?
C7 N2 C10 128.5(3) . . ?
C7 N2 N3 111.6(3) . . ?
N3 N2 C10 119.8(3) . . ?
C8 N3 N2 103.8(3) . . ?
C1 O1 C20 118.6(3) . . ?
C19 C18 C17 118.5(7) . . ?
F15 C18 C17 105.5(5) . . ?
F15 C18 C19 105.3(6) . . ?
F15 C18 F16 107.0(9) . . ?
F16 C18 C17 110.8(7) . . ?
F16 C18 C19 109.0(9) . . ?
F17 C19 C18 110.1(8) . . ?
F18 C19 C18 109.5(7) . . ?
F18 C19 F17 106.8(9) . . ?
F18 C19 F19 106.4(9) . . ?
F19 C19 C18 109.7(9) . . ?
F19 C19 F17 114.2(9) . . ?
F20 C34 S1 109.8(4) . . ?
F21 C34 F20 108.0(5) . . ?
F21 C34 F22 108.7(5) . . ?
F21 C34 S1 110.8(5) . . ?
F22 C34 F20 108.3(5) . . ?
F22 C34 S1 111.1(3) . . ?
F23 C35 S2 109.5(3) . . ?
F24 C35 F23 108.1(4) . . ?
F24 C35 F25 107.7(4) . . ?
F24 C35 S2 111.8(4) . . ?
F25 C35 F23 108.4(4) . . ?
F25 C35 S2 111.2(3) . . ?
S1 N4 S2 127.4(2) . . ?
N4 S1 C34 101.5(3) . . ?
O2 S1 C34 105.2(3) . . ?
O2 S1 N4 116.2(2) . . ?
O2 S1 O3 119.5(2) . . ?
O3 S1 C34 104.1(2) . . ?
O3 S1 N4 107.9(2) . . ?
N4 S2 C35 99.8(2) . . ?
O4 S2 C35 104.7(2) . . ?
O4 S2 N4 116.6(2) . . ?
O5 S2 C35 103.5(2) . . ?
O5 S2 N4 110.8(2) . . ?
O5 S2 O4 118.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -1.0(5) . . . . ?
C2 C1 C6 C5 -1.7(6) . . . . ?
C2 C1 O1 C20 21.0(5) . . . . ?
C2 C3 C4 C5 -0.4(5) . . . . ?
C2 C3 C4 C7 176.9(3) . . . . ?
C3 C4 C5 C6 0.7(6) . . . . ?
C3 C4 C7 N1 -66.1(5) . . . . ?
C3 C4 C7 N2 117.6(4) . . . . ?
C4 C5 C6 C1 0.3(6) . . . . ?
C4 C7 N1 C8 -177.3(3) . . . . ?
C4 C7 N1 C9 2.7(6) . . . . ?
C4 C7 N2 C10 -3.9(6) . . . . ?
C4 C7 N2 N3 177.3(3) . . . . ?
C5 C4 C7 N1 111.2(4) . . . . ?
C5 C4 C7 N2 -65.1(5) . . . . ?
C6 C1 C2 C3 2.0(5) . . . . ?
C6 C1 O1 C20 -157.8(3) . . . . ?
C7 C4 C5 C6 -176.6(3) . . . . ?
C7 N2 N3 C8 -0.3(4) . . . . ?
C8 C11 C12 C13 -170.9(3) . . . . ?
C8 C11 C12 F3 -51.5(4) . . . . ?
C8 C11 C12 F4 65.6(4) . . . . ?
C10 N2 N3 C8 -179.2(3) . . . . ?
C11 C8 N1 C7 176.1(3) . . . . ?
C11 C8 N1 C9 -3.8(6) . . . . ?
C11 C8 N3 N2 -175.7(3) . . . . ?
C11 C12 C13 C14 -163.0(3) . . . . ?
C11 C12 C13 F5 76.5(4) . . . . ?
C11 C12 C13 F6 -40.4(4) . . . . ?
C12 C13 C14 C15 -167.7(3) . . . . ?
C12 C13 C14 F7 -44.6(4) . . . . ?
C12 C13 C14 F8 71.8(4) . . . . ?
C13 C14 C15 C16 -169.7(3) . . . . ?
C13 C14 C15 F9 69.1(4) . . . . ?
C13 C14 C15 F10 -48.0(4) . . . . ?
C14 C15 C16 C17 -173.9(3) . . . . ?
C14 C15 C16 F11A -20.3(13) . . . . ?
C14 C15 C16 F12A 88.5(8) . . . . ?
C14 C15 C16 F11 -59.0(5) . . . . ?
C14 C15 C16 F12 57.4(5) . . . . ?
C15 C16 C17 C18A -154.8(10) . . . . ?
C15 C16 C17 F13A 96.8(8) . . . . ?
C15 C16 C17 F14A -9.5(9) . . . . ?
C15 C16 C17 C18 176.8(4) . . . . ?
C15 C16 C17 F13 47.9(6) . . . . ?
C15 C16 C17 F14 -66.1(5) . . . . ?
C16 C17 C18A C19A -139(2) . . . . ?
C16 C17 C18A F15A -27(3) . . . . ?
C16 C17 C18A F16A 94.9(16) . . . . ?
C16 C17 C18 C19 174.8(6) . . . . ?
C16 C17 C18 F15 -67.7(6) . . . . ?
C16 C17 C18 F16 47.8(9) . . . . ?
C17 C18A C19A F17A 75(5) . . . . ?
C17 C18A C19A F18A -160(2) . . . . ?
C17 C18A C19A F19A -68(3) . . . . ?
C17 C18 C19 F17 54.9(10) . . . . ?
C17 C18 C19 F18 -62.3(12) . . . . ?
C17 C18 C19 F19 -178.7(7) . . . . ?
C20 C21 C22 C23 -177.6(3) . . . . ?
C21 C20 O1 C1 166.3(3) . . . . ?
C21 C22 C23 C24 178.1(3) . . . . ?
C22 C23 C24 C25 -178.5(3) . . . . ?
C23 C24 C25 C26 -179.2(3) . . . . ?
C24 C25 C26 C27 179.2(3) . . . . ?
C25 C26 C27 C28 -179.7(3) . . . . ?
C26 C27 C28 C29 -179.1(3) . . . . ?
C27 C28 C29 C30 -179.7(3) . . . . ?
C28 C29 C30 C31 -179.9(3) . . . . ?
C29 C30 C31 C32 -178.6(3) . . . . ?
C30 C31 C32 C33 179.1(4) . . . . ?
F1 C11 C12 C13 -47.8(4) . . . . ?
F1 C11 C12 F3 71.6(3) . . . . ?
F1 C11 C12 F4 -171.3(3) . . . . ?
F2 C11 C12 C13 68.2(4) . . . . ?
F2 C11 C12 F3 -172.4(3) . . . . ?
F2 C11 C12 F4 -55.2(4) . . . . ?
F3 C12 C13 C14 77.5(4) . . . . ?
F3 C12 C13 F5 -43.0(4) . . . . ?
F3 C12 C13 F6 -159.9(3) . . . . ?
F4 C12 C13 C14 -40.5(4) . . . . ?
F4 C12 C13 F5 -161.0(3) . . . . ?
F4 C12 C13 F6 82.1(4) . . . . ?
F5 C13 C14 C15 -47.5(4) . . . . ?
F5 C13 C14 F7 75.6(4) . . . . ?
F5 C13 C14 F8 -168.0(3) . . . . ?
F6 C13 C14 C15 69.4(4) . . . . ?
F6 C13 C14 F7 -167.5(3) . . . . ?
F6 C13 C14 F8 -51.1(4) . . . . ?
F7 C14 C15 C16 67.5(4) . . . . ?
F7 C14 C15 F9 -53.6(4) . . . . ?
F7 C14 C15 F10 -170.7(3) . . . . ?
F8 C14 C15 C16 -49.7(4) . . . . ?
F8 C14 C15 F9 -170.9(3) . . . . ?
F8 C14 C15 F10 72.0(4) . . . . ?
F9 C15 C16 C17 -52.7(5) . . . . ?
F9 C15 C16 F11A 100.9(12) . . . . ?
F9 C15 C16 F12A -150.2(8) . . . . ?
F9 C15 C16 F11 62.2(4) . . . . ?
F9 C15 C16 F12 178.7(4) . . . . ?
F10 C15 C16 C17 64.3(5) . . . . ?
F10 C15 C16 F11A -142.1(12) . . . . ?
F10 C15 C16 F12A -33.3(8) . . . . ?
F10 C15 C16 F11 179.2(4) . . . . ?
F10 C15 C16 F12 -64.4(5) . . . . ?
F11A C16 C17 C18A 53.7(17) . . . . ?
F11A C16 C17 F13A -54.7(15) . . . . ?
F11A C16 C17 F14A -161.0(15) . . . . ?
F12A C16 C17 C18A -55.8(13) . . . . ?
F12A C16 C17 F13A -164.3(10) . . . . ?
F12A C16 C17 F14A 89.5(11) . . . . ?
F13A C17 C18A C19A -38(2) . . . . ?
F13A C17 C18A F15A 74(3) . . . . ?
F13A C17 C18A F16A -164.5(16) . . . . ?
F14A C17 C18A C19A 77(2) . . . . ?
F14A C17 C18A F15A -172(3) . . . . ?
F14A C17 C18A F16A -50(2) . . . . ?
F15A C18A C19A F17A -41(5) . . . . ?
F15A C18A C19A F18A 83(3) . . . . ?
F15A C18A C19A F19A 176(3) . . . . ?
F16A C18A C19A F17A -162(4) . . . . ?
F16A C18A C19A F18A -38(4) . . . . ?
F16A C18A C19A F19A 55(4) . . . . ?
N1 C7 N2 C10 179.2(3) . . . . ?
N1 C7 N2 N3 0.4(4) . . . . ?
N1 C8 C11 C12 178.2(3) . . . . ?
N1 C8 C11 F1 56.1(5) . . . . ?
N1 C8 C11 F2 -60.7(5) . . . . ?
N1 C8 N3 N2 0.0(4) . . . . ?
N2 C7 N1 C8 -0.4(4) . . . . ?
N2 C7 N1 C9 179.6(4) . . . . ?
N3 C8 C11 C12 -6.5(6) . . . . ?
N3 C8 C11 F1 -128.7(4) . . . . ?
N3 C8 C11 F2 114.5(4) . . . . ?
N3 C8 N1 C7 0.3(4) . . . . ?
N3 C8 N1 C9 -179.7(4) . . . . ?
O1 C1 C2 C3 -176.7(3) . . . . ?
O1 C1 C6 C5 177.1(3) . . . . ?
O1 C20 C21 C22 -179.9(3) . . . . ?
F20 C34 S1 N4 62.5(5) . . . . ?
F20 C34 S1 O2 -59.0(5) . . . . ?
F20 C34 S1 O3 174.5(4) . . . . ?
F21 C34 S1 N4 -178.2(4) . . . . ?
F21 C34 S1 O2 60.3(5) . . . . ?
F21 C34 S1 O3 -66.2(5) . . . . ?
F22 C34 S1 N4 -57.3(5) . . . . ?
F22 C34 S1 O2 -178.7(4) . . . . ?
F22 C34 S1 O3 54.8(5) . . . . ?
F23 C35 S2 N4 177.2(3) . . . . ?
F23 C35 S2 O4 56.2(4) . . . . ?
F23 C35 S2 O5 -68.5(4) . . . . ?
F24 C35 S2 N4 -63.1(3) . . . . ?
F24 C35 S2 O4 176.0(3) . . . . ?
F24 C35 S2 O5 51.3(4) . . . . ?
F25 C35 S2 N4 57.4(4) . . . . ?
F25 C35 S2 O4 -63.6(4) . . . . ?
F25 C35 S2 O5 171.7(3) . . . . ?
S1 N4 S2 C35 -114.8(3) . . . . ?
S1 N4 S2 O4 -2.8(4) . . . . ?
S1 N4 S2 O5 136.7(3) . . . . ?
S2 N4 S1 C34 -93.4(4) . . . . ?
S2 N4 S1 O2 20.1(4) . . . . ?
S2 N4 S1 O3 157.5(3) . . . . ?
F11 C16 C17 C18 61.0(6) . . . . ?
F11 C16 C17 F13 -67.9(5) . . . . ?
F11 C16 C17 F14 178.1(4) . . . . ?
F12 C16 C17 C18 -54.2(6) . . . . ?
F12 C16 C17 F13 176.9(5) . . . . ?
F12 C16 C17 F14 62.9(5) . . . . ?
F13 C17 C18 C19 -55.0(8) . . . . ?
F13 C17 C18 F15 62.5(6) . . . . ?
F13 C17 C18 F16 178.0(8) . . . . ?
F14 C17 C18 C19 58.8(8) . . . . ?
F14 C17 C18 F15 176.3(4) . . . . ?
F14 C17 C18 F16 -68.2(9) . . . . ?
F15 C18 C19 F17 -62.7(10) . . . . ?
F15 C18 C19 F18 -179.9(9) . . . . ?
F15 C18 C19 F19 63.7(10) . . . . ?
F16 C18 C19 F17 -177.2(10) . . . . ?
F16 C18 C19 F18 65.6(13) . . . . ?
F16 C18 C19 F19 -50.8(12) . . . . ?

_olex2_date_sample_data_collection 2017-07-12
_olex2_date_sample_submission    2016-11-24
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id ALR16
_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.737
####################################################################### 
# 
# 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_dwb1669
_database_code_depnum_ccdc_archive 'CCDC 2177831'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H31 F15 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C29 H31 F21 N4 O5 S2'
_chemical_formula_weight         978.70
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H31 F21 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio NV 2521'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.6955(2)
_cell_length_b                   8.5499(2)
_cell_length_c                   68.538(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3923.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7688
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.7350
_cell_measurement_theta_min      5.1690
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1976
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0189
0 -1 0 0.1000
0 1 0 0.0660
-1 0 0 0.1281
0 0 1 0.0129
1 0 0 0.1251

_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.032
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
-0.0000 -0.0001 -0.9999 -0.0192 0.0116 0.0011
0.0004 -1.0000 0.0023 -0.0365 -0.0444 -0.1707
-0.0004 1.0000 -0.0023 0.0365 0.0444 0.1707
-1.0002 -0.0006 -0.0006 -0.1095 -0.1889 0.0726
0.0000 0.0001 0.9999 0.0192 -0.0116 -0.0011
1.0002 0.0006 0.0006 0.1095 0.1889 -0.0726

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            18397
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         3.870
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  69.00   0.75    0.75    --    0.00  77.00 150.00  132
  2  ω     10.00 127.00   0.75    1.00    --   54.00  19.00  60.00  156
  3  ω     33.00 123.00   0.75    1.00    --   54.00  57.00 -60.00  120
  4  ω     23.00 110.00   0.75    1.00    --   54.00-125.00  60.00  116
  5  ω     23.00 110.00   0.75    1.00    --   54.00-125.00 -30.00  116
  6  ω     74.00 177.50   0.75    3.00    --  108.00  25.00 -90.00  138
  7  ω     74.00 177.50   0.75    3.00    --  108.00  25.00   0.00  138
  8  ω     40.00 130.00   0.75    3.00    --  108.00 -63.00  60.00  120
  9  ω     36.00 115.50   0.75    3.00    --  108.00-111.00  90.00  106
 10  ω     36.00 115.50   0.75    3.00    --  108.00-111.00-150.00  106
 11  ω     40.00 130.00   0.75    3.00    --  108.00 -63.00-180.00  120
 12  ω    -72.00  25.50   0.75    0.75    --    0.00 -37.00  30.00  130
 13  ω     33.00  78.00   0.75    1.00    --   54.00  57.00-180.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1094917000
_diffrn_orient_matrix_UB_12      0.0365846000
_diffrn_orient_matrix_UB_13      0.0192391000
_diffrn_orient_matrix_UB_21      0.1888521000
_diffrn_orient_matrix_UB_22      0.0445009000
_diffrn_orient_matrix_UB_23      -0.0115833000
_diffrn_orient_matrix_UB_31      -0.0727299000
_diffrn_orient_matrix_UB_32      0.1707048000
_diffrn_orient_matrix_UB_33      -0.0010917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6503
_reflns_number_total             6928
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 2370 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(10)
_refine_ls_extinction_coef       0.000188(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         6928
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.194
_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)+5.6663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0886
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C)
;
_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
C1 C 0.2709(7) 0.3672(5) 0.67161(6) 0.0161(9) Uani 1 1 d . . . . .
C2 C 0.3572(7) 0.5001(6) 0.66347(7) 0.0202(10) Uani 1 1 d . . . . .
H2 H 0.3374 0.5974 0.6692 0.024 Uiso 1 1 calc R . . . .
C3 C 0.4721(7) 0.4873(6) 0.64682(7) 0.0186(10) Uani 1 1 d . . . . .
H3 H 0.5287 0.5762 0.6413 0.022 Uiso 1 1 calc R . . . .
C4 C 0.5036(7) 0.3415(6) 0.63829(6) 0.0164(10) Uani 1 1 d . . . . .
C5 C 0.4213(7) 0.2087(5) 0.64660(6) 0.0170(9) Uani 1 1 d . . . . .
H5 H 0.4439 0.1114 0.6409 0.020 Uiso 1 1 calc R . . . .
C6 C 0.3045(6) 0.2202(5) 0.66344(6) 0.0148(9) Uani 1 1 d . . . . .
H6 H 0.2500 0.1311 0.6691 0.018 Uiso 1 1 calc R . . . .
C7 C 0.6288(7) 0.3302(5) 0.62083(6) 0.0150(9) Uani 1 1 d . . . . .
C8 C 0.7443(7) 0.2900(5) 0.59184(6) 0.0167(9) Uani 1 1 d . . . . .
C9 C 0.9552(7) 0.4112(5) 0.63559(6) 0.0167(9) Uani 1 1 d . . . . .
H9A H 1.0601 0.3356 0.6371 0.025 Uiso 1 1 calc GR . . . .
H9B H 0.8818 0.4194 0.6476 0.025 Uiso 1 1 calc GR . . . .
H9C H 1.0120 0.5111 0.6324 0.025 Uiso 1 1 calc GR . . . .
C10 C 0.3701(7) 0.2417(7) 0.59671(7) 0.0269(12) Uani 1 1 d . . . . .
H10A H 0.3377 0.2939 0.5847 0.040 Uiso 1 1 calc GR . . . .
H10B H 0.2773 0.2727 0.6067 0.040 Uiso 1 1 calc GR . . . .
H10C H 0.3624 0.1306 0.5948 0.040 Uiso 1 1 calc GR . . . .
C11 C 0.7640(7) 0.2491(6) 0.57052(7) 0.0214(10) Uani 1 1 d . . . . .
C12 C 0.7449(8) 0.3931(6) 0.55705(7) 0.0237(10) Uani 1 1 d . . . . .
C13 C 0.7326(8) 0.3538(6) 0.53496(7) 0.0251(11) Uani 1 1 d . . . . .
C14 C 0.7883(8) 0.4925(6) 0.52154(7) 0.0271(12) Uani 1 1 d . . . . .
C15 C 0.7233(9) 0.4690(6) 0.49983(7) 0.0256(11) Uani 1 1 d . . . . .
C16 C 0.8279(11) 0.5816(7) 0.48541(8) 0.0367(15) Uani 1 1 d . . . . .
C17 C 0.7356(12) 0.5863(7) 0.46468(8) 0.0438(16) Uani 1 1 d . . . . .
C18 C 0.0008(7) 0.2807(6) 0.69201(6) 0.0169(10) Uani 1 1 d . . . . .
H18A H 0.0580 0.1878 0.6979 0.020 Uiso 1 1 calc R . . . .
H18B H -0.0705 0.2505 0.6803 0.020 Uiso 1 1 calc R . . . .
C19 C -0.1379(7) 0.3620(5) 0.70617(6) 0.0191(10) Uani 1 1 d . . . . .
H19A H -0.1896 0.4558 0.7000 0.023 Uiso 1 1 calc R . . . .
H19B H -0.0615 0.3941 0.7175 0.023 Uiso 1 1 calc R . . . .
C20 C -0.3134(6) 0.2622(5) 0.71295(6) 0.0165(9) Uani 1 1 d . . . . .
H20A H -0.3945 0.2338 0.7018 0.020 Uiso 1 1 calc R . . . .
H20B H -0.2632 0.1665 0.7188 0.020 Uiso 1 1 calc R . . . .
C21 C -0.4421(7) 0.3488(5) 0.72777(7) 0.0198(10) Uani 1 1 d . . . . .
H21A H -0.3580 0.3810 0.7386 0.024 Uiso 1 1 calc R . . . .
H21B H -0.4940 0.4428 0.7217 0.024 Uiso 1 1 calc R . . . .
C22 C -0.6155(7) 0.2553(5) 0.73577(6) 0.0166(10) Uani 1 1 d . . . . .
H22A H -0.5648 0.1595 0.7415 0.020 Uiso 1 1 calc R . . . .
H22B H -0.7033 0.2268 0.7251 0.020 Uiso 1 1 calc R . . . .
C23 C -0.7361(7) 0.3437(5) 0.75112(6) 0.0181(9) Uani 1 1 d . . . . .
H23A H -0.7837 0.4409 0.7455 0.022 Uiso 1 1 calc R . . . .
H23B H -0.6490 0.3698 0.7620 0.022 Uiso 1 1 calc R . . . .
C24 C -0.9149(7) 0.2512(5) 0.75887(6) 0.0198(10) Uani 1 1 d . . . . .
H24A H -1.0021 0.2252 0.7480 0.024 Uiso 1 1 calc R . . . .
H24B H -0.8673 0.1540 0.7645 0.024 Uiso 1 1 calc R . . . .
C25 C -1.0350(7) 0.3393(5) 0.77422(6) 0.0185(10) Uani 1 1 d . . . . .
H25A H -0.9489 0.3623 0.7852 0.022 Uiso 1 1 calc R . . . .
H25B H -1.0789 0.4381 0.7687 0.022 Uiso 1 1 calc R . . . .
C26 C -1.2164(8) 0.2495(5) 0.78143(7) 0.0213(10) Uani 1 1 d . . . . .
H26A H -1.1722 0.1514 0.7871 0.026 Uiso 1 1 calc R . . . .
H26B H -1.3012 0.2250 0.7704 0.026 Uiso 1 1 calc R . . . .
C27 C -1.3394(8) 0.3378(6) 0.79656(7) 0.0290(12) Uani 1 1 d . . . . .
H27A H -1.2590 0.3570 0.8079 0.043 Uiso 1 1 calc GR . . . .
H27B H -1.4537 0.2765 0.8001 0.043 Uiso 1 1 calc GR . . . .
H27C H -1.3828 0.4357 0.7912 0.043 Uiso 1 1 calc GR . . . .
F1 F 0.9472(5) 0.1855(4) 0.56789(4) 0.0339(7) Uani 1 1 d . . . . .
F2 F 0.6276(5) 0.1427(3) 0.56513(4) 0.0290(7) Uani 1 1 d . . . . .
F3 F 0.9032(5) 0.4857(4) 0.56034(4) 0.0360(8) Uani 1 1 d . . . . .
F4 F 0.5794(5) 0.4702(4) 0.56238(4) 0.0339(8) Uani 1 1 d . . . . .
F5 F 0.8550(5) 0.2345(3) 0.53101(4) 0.0347(8) Uani 1 1 d . . . . .
F6 F 0.5449(5) 0.3097(4) 0.53106(4) 0.0342(7) Uani 1 1 d . . . . .
F7 F 0.9872(5) 0.5121(4) 0.52197(4) 0.0379(8) Uani 1 1 d . . . . .
F8 F 0.7003(5) 0.6224(3) 0.52834(4) 0.0363(8) Uani 1 1 d . . . . .
F9 F 0.7640(5) 0.3212(3) 0.49451(4) 0.0298(7) Uani 1 1 d . . . . .
F10 F 0.5255(5) 0.4912(4) 0.49865(4) 0.0343(8) Uani 1 1 d . . . . .
F11 F 1.0200(6) 0.5383(4) 0.48351(4) 0.0447(9) Uani 1 1 d . . . . .
F12 F 0.8211(7) 0.7270(4) 0.49266(4) 0.0549(12) Uani 1 1 d . . . . .
F13 F 0.7342(6) 0.4448(4) 0.45702(4) 0.0431(9) Uani 1 1 d . . . . .
F14 F 0.5530(7) 0.6422(5) 0.46499(5) 0.0680(13) Uani 1 1 d . . . . .
F15 F 0.8491(8) 0.6764(5) 0.45346(5) 0.0735(15) Uani 1 1 d . . . . .
N1 N 0.8210(6) 0.3618(4) 0.61997(5) 0.0149(8) Uani 1 1 d . . . . .
N2 N 0.8974(6) 0.3371(5) 0.60180(5) 0.0169(8) Uani 1 1 d . . . . .
N3 N 0.5742(6) 0.2845(5) 0.60272(5) 0.0158(8) Uani 1 1 d . . . . .
O1 O 0.1545(5) 0.3928(4) 0.68752(4) 0.0227(8) Uani 1 1 d . . . . .
C28 C 0.2709(9) 0.6451(5) 0.33542(7) 0.0256(11) Uani 1 1 d . . . . .
C29 C 0.4538(12) 0.6865(7) 0.40811(8) 0.0489(18) Uani 1 1 d . . . . .
F16 F 0.3039(6) 0.5446(4) 0.32094(4) 0.0429(9) Uani 1 1 d . . . . .
F17 F 0.3073(5) 0.7892(3) 0.32862(4) 0.0340(8) Uani 1 1 d . . . . .
F18 F 0.0789(5) 0.6383(3) 0.34012(4) 0.0319(7) Uani 1 1 d . . . . .
F19 F 0.5703(8) 0.5655(4) 0.40379(6) 0.0677(14) Uani 1 1 d . . . . .
F20 F 0.5625(7) 0.8163(4) 0.40734(6) 0.0598(11) Uani 1 1 d . . . . .
F21 F 0.3852(9) 0.6695(5) 0.42610(5) 0.0775(16) Uani 1 1 d . . . . .
N4 N 0.3570(7) 0.7266(4) 0.37113(6) 0.0250(10) Uani 1 1 d . . . . .
O2 O 0.3850(5) 0.4396(4) 0.36074(5) 0.0250(8) Uani 1 1 d . . . . .
O3 O 0.6251(6) 0.6357(4) 0.34945(6) 0.0368(10) Uani 1 1 d . . . . .
O4 O 0.1453(7) 0.5498(4) 0.39290(6) 0.0421(11) Uani 1 1 d . . . . .
O5 O 0.1423(6) 0.8369(4) 0.39612(5) 0.0337(9) Uani 1 1 d . . . . .
S1 S 0.43068(19) 0.59919(13) 0.35618(2) 0.0220(3) Uani 1 1 d . . . . .
S2 S 0.2451(2) 0.69716(14) 0.39094(2) 0.0275(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.392(6) . ?
C1 C6 1.394(6) . ?
C1 O1 1.359(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.392(6) . ?
C4 C5 1.385(6) . ?
C4 C7 1.465(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.398(6) . ?
C6 H6 0.9300 . ?
C7 N1 1.316(6) . ?
C7 N3 1.351(6) . ?
C8 C11 1.508(6) . ?
C8 N2 1.296(6) . ?
C8 N3 1.362(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 N1 1.460(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N3 1.473(6) . ?
C11 C12 1.544(6) . ?
C11 F1 1.354(6) . ?
C11 F2 1.341(6) . ?
C12 C13 1.553(6) . ?
C12 F3 1.342(6) . ?
C12 F4 1.340(6) . ?
C13 C14 1.546(7) . ?
C13 F5 1.337(6) . ?
C13 F6 1.339(6) . ?
C14 C15 1.563(6) . ?
C14 F7 1.342(6) . ?
C14 F8 1.341(6) . ?
C15 C16 1.547(8) . ?
C15 F9 1.344(6) . ?
C15 F10 1.340(6) . ?
C16 C17 1.550(7) . ?
C16 F11 1.345(8) . ?
C16 F12 1.340(6) . ?
C17 F13 1.319(7) . ?
C17 F14 1.313(9) . ?
C17 F15 1.328(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.512(6) . ?
C18 O1 1.440(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.525(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.524(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.512(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.526(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.529(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.523(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.520(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.524(6) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N1 N2 1.363(5) . ?
C28 F16 1.331(5) . ?
C28 F17 1.340(6) . ?
C28 F18 1.327(6) . ?
C28 S1 1.823(5) . ?
C29 F19 1.330(7) . ?
C29 F20 1.328(8) . ?
C29 F21 1.324(7) . ?
C29 S2 1.829(7) . ?
N4 S1 1.574(4) . ?
N4 S2 1.571(4) . ?
O2 S1 1.433(3) . ?
O3 S1 1.416(4) . ?
O4 S2 1.432(4) . ?
O5 S2 1.424(4) . ?

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
C2 C1 C6 120.5(4) . . ?
O1 C1 C2 115.4(4) . . ?
O1 C1 C6 124.1(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C7 119.3(4) . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 C7 120.6(4) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.3(4) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.0(4) . . ?
C1 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
N1 C7 C4 125.6(4) . . ?
N1 C7 N3 106.4(4) . . ?
N3 C7 C4 127.9(4) . . ?
N2 C8 C11 120.9(4) . . ?
N2 C8 N3 112.5(4) . . ?
N3 C8 C11 126.6(4) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
C8 C11 C12 112.8(4) . . ?
F1 C11 C8 107.5(4) . . ?
F1 C11 C12 108.4(4) . . ?
F2 C11 C8 111.4(4) . . ?
F2 C11 C12 108.7(4) . . ?
F2 C11 F1 107.9(4) . . ?
C11 C12 C13 114.5(4) . . ?
F3 C12 C11 107.7(4) . . ?
F3 C12 C13 109.5(4) . . ?
F4 C12 C11 107.3(4) . . ?
F4 C12 C13 109.2(4) . . ?
F4 C12 F3 108.5(4) . . ?
C14 C13 C12 113.7(4) . . ?
F5 C13 C12 109.3(4) . . ?
F5 C13 C14 108.5(4) . . ?
F5 C13 F6 108.7(4) . . ?
F6 C13 C12 107.8(4) . . ?
F6 C13 C14 108.9(4) . . ?
C13 C14 C15 113.6(4) . . ?
F7 C14 C13 108.8(4) . . ?
F7 C14 C15 108.2(4) . . ?
F8 C14 C13 108.8(4) . . ?
F8 C14 C15 108.3(4) . . ?
F8 C14 F7 109.0(4) . . ?
C16 C15 C14 113.7(4) . . ?
F9 C15 C14 108.8(4) . . ?
F9 C15 C16 108.7(4) . . ?
F10 C15 C14 108.3(4) . . ?
F10 C15 C16 108.7(4) . . ?
F10 C15 F9 108.5(4) . . ?
C15 C16 C17 114.9(5) . . ?
F11 C16 C15 108.9(5) . . ?
F11 C16 C17 107.4(5) . . ?
F12 C16 C15 108.9(4) . . ?
F12 C16 C17 107.6(5) . . ?
F12 C16 F11 108.9(5) . . ?
F13 C17 C16 110.1(5) . . ?
F13 C17 F15 107.8(5) . . ?
F14 C17 C16 111.5(5) . . ?
F14 C17 F13 109.5(6) . . ?
F14 C17 F15 109.3(6) . . ?
F15 C17 C16 108.5(6) . . ?
H18A C18 H18B 108.7 . . ?
C19 C18 H18A 110.6 . . ?
C19 C18 H18B 110.6 . . ?
O1 C18 H18A 110.6 . . ?
O1 C18 H18B 110.6 . . ?
O1 C18 C19 105.7(4) . . ?
C18 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
C18 C19 C20 114.3(4) . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C19 C20 H20A 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 C19 111.5(4) . . ?
C21 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
C20 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 C20 114.8(4) . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C21 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
C21 C22 C23 113.2(4) . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C22 C23 C24 113.4(4) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 C23 113.4(4) . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 C24 113.4(4) . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
C25 C26 C27 113.8(4) . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C7 N1 C9 128.9(4) . . ?
C7 N1 N2 112.1(4) . . ?
N2 N1 C9 118.9(4) . . ?
C8 N2 N1 103.4(4) . . ?
C7 N3 C8 105.5(4) . . ?
C7 N3 C10 125.4(4) . . ?
C8 N3 C10 129.1(4) . . ?
C1 O1 C18 118.3(4) . . ?
F16 C28 F17 107.7(4) . . ?
F16 C28 S1 110.2(4) . . ?
F17 C28 S1 111.2(4) . . ?
F18 C28 F16 108.3(4) . . ?
F18 C28 F17 107.5(4) . . ?
F18 C28 S1 111.7(3) . . ?
F19 C29 S2 110.1(4) . . ?
F20 C29 F19 108.6(6) . . ?
F20 C29 S2 110.6(4) . . ?
F21 C29 F19 109.0(5) . . ?
F21 C29 F20 108.6(5) . . ?
F21 C29 S2 109.9(6) . . ?
S2 N4 S1 127.0(3) . . ?
N4 S1 C28 100.1(2) . . ?
O2 S1 C28 104.5(2) . . ?
O2 S1 N4 116.7(2) . . ?
O3 S1 C28 103.8(3) . . ?
O3 S1 N4 110.3(2) . . ?
O3 S1 O2 118.5(2) . . ?
N4 S2 C29 101.5(3) . . ?
O4 S2 C29 104.6(3) . . ?
O4 S2 N4 116.4(2) . . ?
O5 S2 C29 104.5(3) . . ?
O5 S2 N4 108.2(2) . . ?
O5 S2 O4 119.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.7(7) . . . . ?
C2 C1 C6 C5 -1.9(7) . . . . ?
C2 C1 O1 C18 155.4(4) . . . . ?
C2 C3 C4 C5 -0.7(7) . . . . ?
C2 C3 C4 C7 -178.9(4) . . . . ?
C3 C4 C5 C6 0.7(7) . . . . ?
C3 C4 C7 N1 64.8(7) . . . . ?
C3 C4 C7 N3 -116.1(5) . . . . ?
C4 C5 C6 C1 0.6(7) . . . . ?
C4 C7 N1 C9 1.4(8) . . . . ?
C4 C7 N1 N2 178.7(4) . . . . ?
C4 C7 N3 C8 -178.5(4) . . . . ?
C4 C7 N3 C10 2.5(8) . . . . ?
C5 C4 C7 N1 -113.5(6) . . . . ?
C5 C4 C7 N3 65.7(7) . . . . ?
C6 C1 C2 C3 2.0(7) . . . . ?
C6 C1 O1 C18 -24.2(7) . . . . ?
C7 C4 C5 C6 179.0(4) . . . . ?
C7 N1 N2 C8 0.1(5) . . . . ?
C8 C11 C12 C13 -171.4(4) . . . . ?
C8 C11 C12 F3 66.6(5) . . . . ?
C8 C11 C12 F4 -50.0(6) . . . . ?
C9 N1 N2 C8 177.7(4) . . . . ?
C11 C8 N2 N1 179.9(4) . . . . ?
C11 C8 N3 C7 179.7(4) . . . . ?
C11 C8 N3 C10 -1.3(8) . . . . ?
C11 C12 C13 C14 -159.5(5) . . . . ?
C11 C12 C13 F5 -38.1(6) . . . . ?
C11 C12 C13 F6 79.8(5) . . . . ?
C12 C13 C14 C15 -164.7(4) . . . . ?
C12 C13 C14 F7 74.6(6) . . . . ?
C12 C13 C14 F8 -44.0(6) . . . . ?
C13 C14 C15 C16 -163.7(5) . . . . ?
C13 C14 C15 F9 -42.4(6) . . . . ?
C13 C14 C15 F10 75.3(5) . . . . ?
C14 C15 C16 C17 -167.5(5) . . . . ?
C14 C15 C16 F11 71.9(5) . . . . ?
C14 C15 C16 F12 -46.8(7) . . . . ?
C15 C16 C17 F13 -57.0(8) . . . . ?
C15 C16 C17 F14 64.8(7) . . . . ?
C15 C16 C17 F15 -174.8(5) . . . . ?
C18 C19 C20 C21 177.7(4) . . . . ?
C19 C18 O1 C1 -163.7(4) . . . . ?
C19 C20 C21 C22 -177.9(4) . . . . ?
C20 C21 C22 C23 177.8(4) . . . . ?
C21 C22 C23 C24 178.5(4) . . . . ?
C22 C23 C24 C25 179.9(4) . . . . ?
C23 C24 C25 C26 178.1(4) . . . . ?
C24 C25 C26 C27 -179.1(4) . . . . ?
F1 C11 C12 C13 69.7(6) . . . . ?
F1 C11 C12 F3 -52.3(5) . . . . ?
F1 C11 C12 F4 -168.9(4) . . . . ?
F2 C11 C12 C13 -47.4(6) . . . . ?
F2 C11 C12 F3 -169.4(4) . . . . ?
F2 C11 C12 F4 74.0(4) . . . . ?
F3 C12 C13 C14 -38.4(6) . . . . ?
F3 C12 C13 F5 82.9(5) . . . . ?
F3 C12 C13 F6 -159.2(4) . . . . ?
F4 C12 C13 C14 80.2(6) . . . . ?
F4 C12 C13 F5 -158.5(4) . . . . ?
F4 C12 C13 F6 -40.6(5) . . . . ?
F5 C13 C14 C15 73.5(6) . . . . ?
F5 C13 C14 F7 -47.1(5) . . . . ?
F5 C13 C14 F8 -165.7(4) . . . . ?
F6 C13 C14 C15 -44.6(6) . . . . ?
F6 C13 C14 F7 -165.2(4) . . . . ?
F6 C13 C14 F8 76.2(5) . . . . ?
F7 C14 C15 C16 -42.7(6) . . . . ?
F7 C14 C15 F9 78.5(5) . . . . ?
F7 C14 C15 F10 -163.7(4) . . . . ?
F8 C14 C15 C16 75.3(6) . . . . ?
F8 C14 C15 F9 -163.5(4) . . . . ?
F8 C14 C15 F10 -45.7(6) . . . . ?
F9 C15 C16 C17 71.1(7) . . . . ?
F9 C15 C16 F11 -49.5(6) . . . . ?
F9 C15 C16 F12 -168.1(5) . . . . ?
F10 C15 C16 C17 -46.8(6) . . . . ?
F10 C15 C16 F11 -167.3(4) . . . . ?
F10 C15 C16 F12 74.0(6) . . . . ?
F11 C16 C17 F13 64.4(7) . . . . ?
F11 C16 C17 F14 -173.9(5) . . . . ?
F11 C16 C17 F15 -53.4(7) . . . . ?
F12 C16 C17 F13 -178.5(6) . . . . ?
F12 C16 C17 F14 -56.7(7) . . . . ?
F12 C16 C17 F15 63.7(7) . . . . ?
N1 C7 N3 C8 0.8(5) . . . . ?
N1 C7 N3 C10 -178.2(4) . . . . ?
N2 C8 C11 C12 -85.2(6) . . . . ?
N2 C8 C11 F1 34.2(6) . . . . ?
N2 C8 C11 F2 152.3(4) . . . . ?
N2 C8 N3 C7 -0.8(5) . . . . ?
N2 C8 N3 C10 178.2(5) . . . . ?
N3 C7 N1 C9 -177.9(4) . . . . ?
N3 C7 N1 N2 -0.6(5) . . . . ?
N3 C8 C11 C12 94.2(6) . . . . ?
N3 C8 C11 F1 -146.3(4) . . . . ?
N3 C8 C11 F2 -28.3(6) . . . . ?
N3 C8 N2 N1 0.4(5) . . . . ?
O1 C1 C2 C3 -177.6(4) . . . . ?
O1 C1 C6 C5 177.7(4) . . . . ?
O1 C18 C19 C20 -179.8(4) . . . . ?
F16 C28 S1 N4 -177.6(4) . . . . ?
F16 C28 S1 O2 -56.4(4) . . . . ?
F16 C28 S1 O3 68.4(4) . . . . ?
F17 C28 S1 N4 63.0(4) . . . . ?
F17 C28 S1 O2 -175.8(3) . . . . ?
F17 C28 S1 O3 -51.0(4) . . . . ?
F18 C28 S1 N4 -57.1(4) . . . . ?
F18 C28 S1 O2 64.0(4) . . . . ?
F18 C28 S1 O3 -171.2(3) . . . . ?
F19 C29 S2 N4 -63.1(5) . . . . ?
F19 C29 S2 O4 58.3(6) . . . . ?
F19 C29 S2 O5 -175.5(5) . . . . ?
F20 C29 S2 N4 57.0(5) . . . . ?
F20 C29 S2 O4 178.4(4) . . . . ?
F20 C29 S2 O5 -55.4(5) . . . . ?
F21 C29 S2 N4 176.9(4) . . . . ?
F21 C29 S2 O4 -61.7(5) . . . . ?
F21 C29 S2 O5 64.4(5) . . . . ?
S1 N4 S2 C29 91.8(4) . . . . ?
S1 N4 S2 O4 -21.0(5) . . . . ?
S1 N4 S2 O5 -158.5(3) . . . . ?
S2 N4 S1 C28 114.3(4) . . . . ?
S2 N4 S1 O2 2.3(5) . . . . ?
S2 N4 S1 O3 -136.8(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-08
_olex2_date_sample_submission    2016-11-04
_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 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.851
####################################################################### 
# 
# 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_dwb1675
_database_code_depnum_ccdc_archive 'CCDC 2177835'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2016-11-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H31 F19 N3 O, C F3 O3 S'
_chemical_formula_sum            'C30 H31 F22 N3 O4 S'
_chemical_formula_weight         947.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H31 F22 N3 O4 S1'
_chemical_oxdiff_usercomment     'Alessio Riccobono ALR11'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.9391(3)
_cell_length_b                   11.5678(10)
_cell_length_c                   20.8049(17)
_cell_angle_alpha                82.290(7)
_cell_angle_beta                 89.720(5)
_cell_angle_gamma                82.993(5)
_cell_volume                     1879.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3295
_cell_measurement_temperature    109.95(10)
_cell_measurement_theta_max      70.6170
_cell_measurement_theta_min      6.3980
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.169
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             956.000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0094
0 0 -1 0.0074
1 0 0 0.0674
-1 0 0 0.0848
0 -1 0 0.0538
0 1 0 0.0488

_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.017
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
0.0000 0.0001 0.9999 -0.0060 0.0745 -0.0020
-0.0000 -0.0001 -0.9999 0.0060 -0.0745 0.0020
1.0001 -0.0000 0.0001 -0.0119 0.0065 0.1951
-1.0001 0.0000 -0.0001 0.0119 -0.0065 -0.1951
0.0000 -1.0000 0.0012 -0.1350 0.0077 0.0082
-0.0000 1.0000 -0.0012 0.1350 -0.0077 -0.0082

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10985
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.062
_diffrn_reflns_theta_max         67.062
_diffrn_reflns_theta_min         3.885
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      109.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9929
_diffrn_measured_fraction_theta_max 0.9930
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  20.00   1.00    6.00    --    0.00 -77.00 -90.00   51
  2  ω     32.00  69.00   1.00    6.00    --    0.00  57.00  30.00   37
  3  ω    -70.00 -37.00   1.00    6.00    --    0.00 -77.00 -90.00   33
  4  ω     -6.00  28.00   1.00    6.00    --    0.00  57.00  30.00   34
  5  ω      0.00  75.00   1.00   24.00    --   54.00 -57.00  60.00   75
  6  ω     -8.00 115.00   1.00   24.00    --   54.00   0.00  90.00  123
  7  ω     11.00  59.00   1.00   24.00    --   54.00 -99.00  30.00   48
  8  ω     25.00 118.00   1.00   24.00    --   54.00  77.00 -90.00   93
  9  ω     35.00 119.00   1.00   24.00    --   54.00-137.00-116.00   84
 10  ω     64.00 116.00   1.00   24.00    --  108.00-111.00-180.00   52
 11  ω     64.00 134.00   1.00   24.00    --  108.00 -37.00 150.00   70
 12  ω     74.00 151.00   1.00   24.00    --  108.00 178.00  60.00   77
 13  ω     48.00 129.00   1.00   24.00    --  108.00 -63.00   0.00   81
 14  ω     75.00 108.00   1.00   24.00    --  108.00-111.00  90.00   33
 15  ω     39.00 117.00   1.00   24.00    --  108.00 -50.00  90.00   78
 16  ω     38.00 109.00   1.00   24.00    --  108.00-132.00  59.00   71
 17  ω    130.00 161.00   1.00   24.00    --  108.00  63.00  90.00   31
 18  ω     40.00 129.00   1.00   24.00    --  108.00 -63.00-180.00   89
 19  ω     36.00 140.00   1.00   24.00    --  108.00 -25.00 -30.00  104
 20  ω     36.00 177.00   1.00   24.00    --  108.00   0.00  60.00  141
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0118584000
_diffrn_orient_matrix_UB_12      0.1349469000
_diffrn_orient_matrix_UB_13      -0.0060078000
_diffrn_orient_matrix_UB_21      0.0065091000
_diffrn_orient_matrix_UB_22      -0.0076124000
_diffrn_orient_matrix_UB_23      0.0744622000
_diffrn_orient_matrix_UB_31      0.1950573000
_diffrn_orient_matrix_UB_32      -0.0081618000
_diffrn_orient_matrix_UB_33      -0.0019775000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5218
_reflns_number_total             6665
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         6665
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0662
_refine_ls_restrained_S_all      1.077
_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)+(0.0644P)²+2.4557P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1667
_refine_special_details          
;
The structure exhibited disorder in both the cation and anion.

For the cation, the majority of the perfluoro nonyl chain was disordered,
with C14-C19 and F5-F19 being modelled in two positions with refined
occupancies of 0.949:0.041(2).  The equivalent pairs of C-C bonds were 
restrained to be equal e.g. C14-C15 and C14A-C15A.  For the minor 
conformer, the C-F bond lengths were restrained to be 1.35 angstroms,
the F-C-F distances to 2.18 angstroms and C16A-C-18 & C17A-C19A to 
2.6 angstroms.  The ADP were constrained to be equal for atoms for 
equivalent atoms pairs,  e.g. C14 & C14A, F7 & F7A.  In three cases,
pairs of atoms were constrained to occupy the same site, F13 & F13A,
F16 & F16A, F19 & F19A.

For the anion, the oxygens were modelled in two positions differing by
rotation about the C-S bond with occupancies of 0.688:0.312(8).  
S-O distances were restrained to be equal, adjacent oxygens were
constrained to have the same ADP e.g. O2 & O2A.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{F13A, F13}
{F19, F19A}
{F16, F16A}
3. Restrained distances
 F5A-C13 = F6A-C13 = F7A-C14A = F8A-C14A = F9A-C15A = F10A-C15A
 1.35 with sigma of 0.02
 F11A-C16A = F12A-C16A = F13A-C17A = F14A-C17A = F15A-C18A = F16A-C18A
 1.35 with sigma of 0.02
 F17A-C19A = F18A-C19A = F19A-C19A
 1.35 with sigma of 0.02
 F6A-F5A = F7A-F8A = F9A-F10A = F11A-F12A = F13A-F14A = F15A-F16A
 2.18 with sigma of 0.04
 F17A-F18A = F17A-F19A = F18A-F19A
 2.18 with sigma of 0.04
 C19A-C17A
 2.6 with sigma of 0.04
 C16A-C18A
 2.6 with sigma of 0.04
 S1-O2 \\sim S1-O2A \\sim S1-O4A \\sim S1-O4 \\sim S1-O3 \\sim S1-O3A
 with sigma of 0.02
 C13-C14A \\sim C14-C13
 with sigma of 0.02
 C16A-C15A \\sim C16-C15
 with sigma of 0.02
 C15-C14 \\sim C15A-C14A
 with sigma of 0.02
 C17-C16 \\sim C17A-C16A
 with sigma of 0.02
 C18A-C19A \\sim C19-C18
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O2A)
Uanis(O4A) = Uanis(O4)
Uanis(O3) = Uanis(O3A)
Uanis(C14) = Uanis(C14A)
Uanis(C16) = Uanis(C16A)
Uanis(F12A) = Uanis(F12)
Uanis(C17A) = Uanis(C17)
Uanis(C18) = Uanis(C18A)
Uanis(F8A) = Uanis(F8)
Uanis(F7A) = Uanis(F7)
Uanis(F9) = Uanis(F9A)
Uanis(F11) = Uanis(F11A)
Uanis(F14A) = Uanis(F14)
Uanis(F10) = Uanis(F10A)
Uanis(F13A) = Uanis(F13)
Uanis(F15) = Uanis(F15A)
Uanis(C19A) = Uanis(C19)
Uanis(F19A) = Uanis(F17)
Uanis(F16) = Uanis(F16A)
Uanis(F5A) = Uanis(F5)
Uanis(F6A) = Uanis(F6)
Uanis(F18A) = Uanis(F17)
5. Others
 Sof(O2A)=Sof(O3A)=Sof(O4A)=1-FVAR(1)
 Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
 Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(C19A)=Sof(F5A)=Sof(F6A)=
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=
 Sof(F15A)=Sof(F16A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=1-FVAR(2)
 Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=Sof(C18)=Sof(C19)=Sof(F5)=Sof(F6)=Sof(F7)=
 Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=
 Sof(F17)=Sof(F18)=Sof(F19)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C)
;
_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
C1 C 0.6818(4) 0.3982(3) 0.31159(16) 0.0253(8) Uani 1 1 d . . . . .
C2 C 0.5963(4) 0.3079(3) 0.34295(17) 0.0269(8) Uani 1 1 d . . . . .
H2 H 0.5271 0.2700 0.3189 0.032 Uiso 1 1 calc R . . . .
C3 C 0.6132(4) 0.2747(3) 0.40842(16) 0.0240(7) Uani 1 1 d . . . . .
H3 H 0.5538 0.2157 0.4286 0.029 Uiso 1 1 calc R . . . .
C4 C 0.7199(4) 0.3293(3) 0.44521(16) 0.0212(7) Uani 1 1 d . . . . .
C5 C 0.8048(4) 0.4200(3) 0.41401(17) 0.0239(7) Uani 1 1 d . . . . .
H5 H 0.8748 0.4573 0.4380 0.029 Uiso 1 1 calc R . . . .
C6 C 0.7859(4) 0.4546(3) 0.34792(17) 0.0263(8) Uani 1 1 d . . . . .
H6 H 0.8424 0.5152 0.3277 0.032 Uiso 1 1 calc R . . . .
C7 C 0.7380(4) 0.2924(3) 0.51482(16) 0.0201(7) Uani 1 1 d . . . . .
C8 C 0.7482(4) 0.2856(3) 0.61906(16) 0.0221(7) Uani 1 1 d . . . . .
C9 C 0.7029(5) 0.4893(3) 0.55502(18) 0.0292(8) Uani 1 1 d . . . . .
H9A H 0.6241 0.5142 0.5871 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.6573 0.5186 0.5125 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.8086 0.5194 0.5605 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.7737(5) 0.0724(3) 0.51626(19) 0.0359(9) Uani 1 1 d . . . . .
H10A H 0.8469 0.0133 0.5431 0.054 Uiso 1 1 calc GR . . . .
H10B H 0.8204 0.0846 0.4736 0.054 Uiso 1 1 calc GR . . . .
H10C H 0.6635 0.0471 0.5136 0.054 Uiso 1 1 calc GR . . . .
C11 C 0.7437(4) 0.3262(3) 0.68446(17) 0.0248(7) Uani 1 1 d . . . . .
C12 C 0.7695(4) 0.2254(3) 0.74121(16) 0.0241(7) Uani 1 1 d . . . . .
C13 C 0.7849(5) 0.2664(3) 0.80915(18) 0.0291(8) Uani 1 1 d D . . . .
C14 C 0.7346(5) 0.1756(3) 0.86497(18) 0.0248(8) Uani 0.9587(19) 1 d D . P A 1
C14A C 0.788(6) 0.179(4) 0.8724(18) 0.0248(8) Uani 0.0413(19) 1 d D . P A 2
C15 C 0.7877(5) 0.1976(3) 0.93387(18) 0.0253(8) Uani 0.9587(19) 1 d D . P A 1
C15A C 0.715(6) 0.196(6) 0.941(2) 0.02(2) Uiso 0.0413(19) 1 d D . P A 2
C16 C 0.6987(5) 0.1258(3) 0.98928(18) 0.0262(8) Uani 0.9587(19) 1 d D . P A 1
C16A C 0.784(6) 0.117(6) 1.003(2) 0.0262(8) Uani 0.0413(19) 1 d D . P A 2
C17 C 0.7607(5) 0.1337(3) 1.05830(18) 0.0259(8) Uani 0.9587(19) 1 d D . P A 1
C17A C 0.699(5) 0.136(2) 1.068(2) 0.0259(8) Uani 0.0413(19) 1 d D . P A 2
C18 C 0.6673(5) 0.0624(4) 1.1133(2) 0.0337(9) Uani 0.9587(19) 1 d D . P A 1
C18A C 0.742(6) 0.050(3) 1.124(2) 0.0337(9) Uani 0.0413(19) 1 d D . P A 2
C19 C 0.7171(6) 0.0750(4) 1.1827(2) 0.0360(10) Uani 0.9587(19) 1 d D . P A 1
C19A C 0.673(6) 0.0721(19) 1.191(2) 0.0360(10) Uani 0.0413(19) 1 d D . P A 2
C20 C 0.7425(5) 0.5095(3) 0.20893(17) 0.0281(8) Uani 1 1 d . . . . .
H20A H 0.8643 0.4908 0.2154 0.034 Uiso 1 1 calc R . . . .
H20B H 0.7081 0.5870 0.2210 0.034 Uiso 1 1 calc R . . . .
C21 C 0.6945(5) 0.5056(3) 0.13923(17) 0.0293(8) Uani 1 1 d . . . . .
H21A H 0.5727 0.5260 0.1342 0.035 Uiso 1 1 calc R . . . .
H21B H 0.7219 0.4256 0.1297 0.035 Uiso 1 1 calc R . . . .
C22 C 0.7814(5) 0.5869(3) 0.08999(17) 0.0283(8) Uani 1 1 d . . . . .
H22A H 0.9034 0.5677 0.0950 0.034 Uiso 1 1 calc R . . . .
H22B H 0.7520 0.6673 0.0983 0.034 Uiso 1 1 calc R . . . .
C23 C 0.7303(5) 0.5768(3) 0.02051(17) 0.0296(8) Uani 1 1 d . . . . .
H23A H 0.7556 0.4954 0.0133 0.036 Uiso 1 1 calc R . . . .
H23B H 0.6086 0.5980 0.0157 0.036 Uiso 1 1 calc R . . . .
C24 C 0.8174(5) 0.6529(3) -0.03132(17) 0.0296(8) Uani 1 1 d . . . . .
H24A H 0.9392 0.6311 -0.0270 0.036 Uiso 1 1 calc R . . . .
H24B H 0.7932 0.7343 -0.0240 0.036 Uiso 1 1 calc R . . . .
C25 C 0.7630(5) 0.6426(4) -0.10042(17) 0.0339(9) Uani 1 1 d . . . . .
H25A H 0.7854 0.5610 -0.1076 0.041 Uiso 1 1 calc R . . . .
H25B H 0.6416 0.6658 -0.1051 0.041 Uiso 1 1 calc R . . . .
C26 C 0.8534(5) 0.7176(4) -0.15193(17) 0.0327(9) Uani 1 1 d . . . . .
H26A H 0.8339 0.7987 -0.1436 0.039 Uiso 1 1 calc R . . . .
H26B H 0.9744 0.6927 -0.1478 0.039 Uiso 1 1 calc R . . . .
C27 C 0.7983(5) 0.7123(5) -0.22122(19) 0.0441(11) Uani 1 1 d . . . . .
H27A H 0.6783 0.7407 -0.2261 0.053 Uiso 1 1 calc R . . . .
H27B H 0.8135 0.6310 -0.2292 0.053 Uiso 1 1 calc R . . . .
C28 C 0.8966(6) 0.7845(5) -0.2718(2) 0.0507(12) Uani 1 1 d . . . . .
H28A H 0.8856 0.8647 -0.2620 0.061 Uiso 1 1 calc R . . . .
H28B H 1.0158 0.7537 -0.2674 0.061 Uiso 1 1 calc R . . . .
C29 C 0.8440(7) 0.7873(6) -0.3409(2) 0.0670(16) Uani 1 1 d . . . . .
H29A H 0.9224 0.8261 -0.3688 0.101 Uiso 1 1 calc GR . . . .
H29B H 0.7322 0.8293 -0.3478 0.101 Uiso 1 1 calc GR . . . .
H29C H 0.8436 0.7084 -0.3504 0.101 Uiso 1 1 calc GR . . . .
F1 F 0.5918(3) 0.3897(2) 0.69167(10) 0.0395(6) Uani 1 1 d . . . . .
F2 F 0.8644(3) 0.3980(2) 0.68981(10) 0.0399(6) Uani 1 1 d . . . . .
F3 F 0.6366(3) 0.1637(2) 0.74092(10) 0.0359(5) Uani 1 1 d . . . . .
F4 F 0.9110(3) 0.1550(2) 0.73227(10) 0.0395(6) Uani 1 1 d . . . . .
F5 F 0.6886(4) 0.3690(2) 0.81095(12) 0.0427(7) Uani 0.9587(19) 1 d . . P A 1
F5A F 0.633(4) 0.332(5) 0.817(3) 0.0427(7) Uani 0.0413(19) 1 d D . P A 2
F6 F 0.9479(3) 0.2838(3) 0.81831(13) 0.0442(7) Uani 0.9587(19) 1 d . . P A 1
F6A F 0.903(6) 0.339(5) 0.814(4) 0.0442(7) Uani 0.0413(19) 1 d D . P A 2
F7 F 0.5657(3) 0.1801(2) 0.86256(11) 0.0422(6) Uani 0.9587(19) 1 d . . P A 1
F7A F 0.960(6) 0.161(5) 0.878(3) 0.0422(6) Uani 0.0413(19) 1 d D . P A 2
F8 F 0.8057(3) 0.0687(2) 0.85530(14) 0.0388(7) Uani 0.9587(19) 1 d . . P A 1
F8A F 0.738(8) 0.079(6) 0.858(4) 0.0388(7) Uani 0.0413(19) 1 d D . P A 2
F9 F 0.7490(6) 0.3122(3) 0.93937(18) 0.0394(10) Uani 0.9587(19) 1 d . . P A 1
F9A F 0.755(14) 0.306(9) 0.927(7) 0.0394(10) Uani 0.0413(19) 1 d D . P A 2
F10 F 0.9561(3) 0.1697(2) 0.94067(10) 0.0382(6) Uani 0.9587(19) 1 d . . P A 1
F10A F 0.544(6) 0.200(5) 0.936(3) 0.0382(6) Uani 0.0413(19) 1 d D . P A 2
F11 F 0.5317(3) 0.1624(3) 0.98564(11) 0.0452(7) Uani 0.9587(19) 1 d . . P A 1
F11A F 0.953(6) 0.120(6) 1.006(3) 0.0452(7) Uani 0.0413(19) 1 d D . P A 2
F12 F 0.7219(5) 0.0119(4) 0.9798(4) 0.0411(8) Uani 0.9587(19) 1 d . . P A 1
F12A F 0.760(13) 0.015(11) 0.982(10) 0.0411(8) Uani 0.0413(19) 1 d D . P A 2
F13 F 0.7343(3) 0.24760(19) 1.06749(11) 0.0432(6) Uani 0.9587(19) 1 d . . P A 1
F13A F 0.7343(3) 0.24760(19) 1.06749(11) 0.0432(6) Uani 0.0413(19) 1 d D . P A
2
F14 F 0.9266(3) 0.0966(2) 1.06451(11) 0.0393(6) Uani 0.9587(19) 1 d . . P A 1
F14A F 0.535(5) 0.125(4) 1.055(3) 0.0393(6) Uani 0.0413(19) 1 d D . P A 2
F15 F 0.5008(3) 0.0897(3) 1.10668(12) 0.0496(7) Uani 0.9587(19) 1 d . . P A 1
F15A F 0.908(6) 0.062(5) 1.130(3) 0.0496(7) Uani 0.0413(19) 1 d D . P A 2
F16 F 0.7071(4) -0.0530(2) 1.10717(12) 0.0541(7) Uani 0.9587(19) 1 d . . P A 1
F16A F 0.7071(4) -0.0530(2) 1.10717(12) 0.0541(7) Uani 0.0413(19) 1 d D . P A 2
F17 F 0.6256(4) 0.0123(3) 1.22401(13) 0.0563(8) Uani 0.9587(19) 1 d . . P A 1
F17A F 0.510(6) 0.055(5) 1.186(3) 0.07(2) Uani 0.0413(19) 1 d D . P A 2
F18 F 0.8785(3) 0.0414(3) 1.19470(13) 0.0598(8) Uani 0.9587(19) 1 d . . P A 1
F18A F 0.755(7) 0.002(4) 1.240(3) 0.0563(8) Uani 0.0413(19) 1 d D . P A 2
F19 F 0.6832(4) 0.1860(2) 1.19363(12) 0.0538(7) Uani 0.9587(19) 1 d . . P A 1
F19A F 0.6832(4) 0.1860(2) 1.19363(12) 0.0563(8) Uani 0.0413(19) 1 d D . P . .
N1 N 0.7588(3) 0.1820(2) 0.54439(13) 0.0218(6) Uani 1 1 d . . . . .
N2 N 0.7648(3) 0.1766(2) 0.60980(13) 0.0225(6) Uani 1 1 d . . . . .
N3 N 0.7311(3) 0.3613(2) 0.56264(13) 0.0200(6) Uani 1 1 d . . . . .
O1 O 0.6545(3) 0.4230(2) 0.24704(11) 0.0301(6) Uani 1 1 d . . . . .
C30 C 0.2698(5) 0.1349(3) 0.62589(19) 0.0330(9) Uani 1 1 d . . . . .
F20 F 0.1457(3) 0.0665(2) 0.63030(14) 0.0513(7) Uani 1 1 d . . . . .
F21 F 0.2644(5) 0.1864(3) 0.67847(13) 0.0769(10) Uani 1 1 d . . . . .
F22 F 0.4124(3) 0.0632(3) 0.62726(17) 0.0714(10) Uani 1 1 d . . . . .
O2 O 0.2855(10) 0.1704(4) 0.5022(2) 0.0571(17) Uani 0.688(8) 1 d D . P B 1
O2A O 0.177(2) 0.1694(11) 0.5075(5) 0.0571(17) Uani 0.312(8) 1 d D . P B 2
O3 O 0.0980(10) 0.3171(13) 0.5642(10) 0.044(3) Uani 0.688(8) 1 d D . P B 1
O3A O 0.082(2) 0.302(3) 0.552(3) 0.044(3) Uani 0.312(8) 1 d D . P B 2
O4 O 0.3930(7) 0.3082(6) 0.5642(3) 0.0345(14) Uani 0.688(8) 1 d D . P B 1
O4A O 0.4002(17) 0.2875(15) 0.5412(7) 0.0345(14) Uani 0.312(8) 1 d D . P B 2
S1 S 0.24919(12) 0.24130(8) 0.55329(4) 0.0307(2) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.401(5) . ?
C1 C6 1.396(5) . ?
C1 O1 1.348(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.367(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.403(4) . ?
C4 C5 1.400(5) . ?
C4 C7 1.457(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(5) . ?
C6 H6 0.9300 . ?
C7 N1 1.332(4) . ?
C7 N3 1.353(4) . ?
C8 C11 1.496(5) . ?
C8 N2 1.292(4) . ?
C8 N3 1.364(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 N3 1.458(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.459(4) . ?
C11 C12 1.539(5) . ?
C11 F1 1.352(4) . ?
C11 F2 1.357(4) . ?
C12 C13 1.560(5) . ?
C12 F3 1.344(4) . ?
C12 F4 1.333(4) . ?
C13 C14 1.543(5) . ?
C13 C14A 1.54(2) . ?
C13 F5 1.336(4) . ?
C13 F5A 1.37(2) . ?
C13 F6 1.352(4) . ?
C13 F6A 1.34(2) . ?
C14 C15 1.558(5) . ?
C14 F7 1.336(4) . ?
C14 F8 1.336(4) . ?
C14A C15A 1.56(2) . ?
C14A F7A 1.36(2) . ?
C14A F8A 1.35(2) . ?
C15 C16 1.548(5) . ?
C15 F9 1.344(5) . ?
C15 F10 1.340(5) . ?
C15A C16A 1.54(2) . ?
C15A F9A 1.35(2) . ?
C15A F10A 1.35(2) . ?
C16 C17 1.538(5) . ?
C16 F11 1.342(4) . ?
C16 F12 1.348(5) . ?
C16A C17A 1.53(2) . ?
C16A F11A 1.35(2) . ?
C16A F12A 1.35(2) . ?
C17 C18 1.559(5) . ?
C17 F13 1.348(4) . ?
C17 F14 1.335(4) . ?
C17A C18A 1.45(5) . ?
C17A F13A 1.35(2) . ?
C17A F14A 1.35(2) . ?
C18 C19 1.528(6) . ?
C18 F15 1.325(5) . ?
C18 F16 1.357(5) . ?
C18A C19A 1.52(2) . ?
C18A F15A 1.35(2) . ?
C18A F16A 1.35(2) . ?
C19 F17 1.322(5) . ?
C19 F18 1.308(5) . ?
C19 F19 1.329(5) . ?
C19A F17A 1.34(2) . ?
C19A F18A 1.33(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.509(5) . ?
C20 O1 1.439(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.517(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.527(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.518(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.527(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.520(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.520(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.527(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.493(6) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
N1 N2 1.355(4) . ?
C30 F20 1.332(4) . ?
C30 F21 1.312(5) . ?
C30 F22 1.317(5) . ?
C30 S1 1.811(4) . ?
O2 S1 1.435(4) . ?
O2A S1 1.504(10) . ?
O3 S1 1.433(7) . ?
O3A S1 1.423(14) . ?
O4 S1 1.489(5) . ?
O4A S1 1.380(11) . ?

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
C6 C1 C2 119.3(3) . . ?
O1 C1 C2 115.3(3) . . ?
O1 C1 C6 125.4(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C7 119.7(3) . . ?
C5 C4 C3 118.9(3) . . ?
C5 C4 C7 121.4(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.9(3) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 H6 120.1 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
N1 C7 C4 126.3(3) . . ?
N1 C7 N3 105.9(3) . . ?
N3 C7 C4 127.8(3) . . ?
N2 C8 C11 124.2(3) . . ?
N2 C8 N3 112.9(3) . . ?
N3 C8 C11 122.9(3) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C9 H9A 109.5 . . ?
N3 C9 H9B 109.5 . . ?
N3 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C8 C11 C12 113.9(3) . . ?
F1 C11 C8 108.9(3) . . ?
F1 C11 C12 108.2(3) . . ?
F1 C11 F2 107.0(3) . . ?
F2 C11 C8 110.9(3) . . ?
F2 C11 C12 107.7(3) . . ?
C11 C12 C13 114.4(3) . . ?
F3 C12 C11 107.5(3) . . ?
F3 C12 C13 109.2(3) . . ?
F4 C12 C11 109.5(3) . . ?
F4 C12 C13 107.3(3) . . ?
F4 C12 F3 108.8(3) . . ?
C14 C13 C12 112.7(3) . . ?
C14A C13 C12 122(2) . . ?
F5 C13 C12 110.1(3) . . ?
F5 C13 C14 109.3(3) . . ?
F5 C13 F6 107.5(3) . . ?
F5A C13 C12 105(3) . . ?
F5A C13 C14A 99(3) . . ?
F6 C13 C12 108.3(3) . . ?
F6 C13 C14 108.8(3) . . ?
F6A C13 C12 115(3) . . ?
F6A C13 C14A 109(4) . . ?
F6A C13 F5A 105(3) . . ?
C13 C14 C15 114.6(3) . . ?
F7 C14 C13 106.9(3) . . ?
F7 C14 C15 108.6(3) . . ?
F8 C14 C13 108.9(3) . . ?
F8 C14 C15 108.3(3) . . ?
F8 C14 F7 109.5(3) . . ?
C13 C14A C15A 131(4) . . ?
F7A C14A C13 95(3) . . ?
F7A C14A C15A 108(4) . . ?
F8A C14A C13 108(5) . . ?
F8A C14A C15A 106(5) . . ?
F8A C14A F7A 106(3) . . ?
C16 C15 C14 113.3(3) . . ?
F9 C15 C14 109.2(3) . . ?
F9 C15 C16 108.1(3) . . ?
F10 C15 C14 108.5(3) . . ?
F10 C15 C16 109.1(3) . . ?
F10 C15 F9 108.6(3) . . ?
C16A C15A C14A 122(4) . . ?
F9A C15A C14A 85(7) . . ?
F9A C15A C16A 120(8) . . ?
F9A C15A F10A 108(3) . . ?
F10A C15A C14A 108(4) . . ?
F10A C15A C16A 110(4) . . ?
C17 C16 C15 115.5(3) . . ?
F11 C16 C15 108.6(3) . . ?
F11 C16 C17 108.1(3) . . ?
F11 C16 F12 108.1(3) . . ?
F12 C16 C15 108.2(4) . . ?
F12 C16 C17 108.1(4) . . ?
C17A C16A C15A 119(4) . . ?
F11A C16A C15A 108(4) . . ?
F11A C16A C17A 112(4) . . ?
F12A C16A C15A 95(10) . . ?
F12A C16A C17A 114(9) . . ?
F12A C16A F11A 107(3) . . ?
C16 C17 C18 114.6(3) . . ?
F13 C17 C16 107.5(3) . . ?
F13 C17 C18 107.5(3) . . ?
F14 C17 C16 110.3(3) . . ?
F14 C17 C18 108.0(3) . . ?
F14 C17 F13 108.8(3) . . ?
C18A C17A C16A 119(3) . . ?
F13A C17A C16A 96(4) . . ?
F13A C17A C18A 119(3) . . ?
F14A C17A C16A 102(4) . . ?
F14A C17A C18A 104(3) . . ?
F14A C17A F13A 115(3) . . ?
C19 C18 C17 116.0(3) . . ?
F15 C18 C17 110.5(3) . . ?
F15 C18 C19 108.3(3) . . ?
F15 C18 F16 108.7(3) . . ?
F16 C18 C17 107.0(3) . . ?
F16 C18 C19 106.0(3) . . ?
C17A C18A C19A 120(3) . . ?
F15A C18A C17A 99(4) . . ?
F15A C18A C19A 103(4) . . ?
F15A C18A F16A 116(3) . . ?
F16A C18A C17A 105(3) . . ?
F16A C18A C19A 113(3) . . ?
F17 C19 C18 109.4(4) . . ?
F17 C19 F19 106.8(3) . . ?
F18 C19 C18 112.1(3) . . ?
F18 C19 F17 109.5(4) . . ?
F18 C19 F19 108.2(4) . . ?
F19 C19 C18 110.7(3) . . ?
F17A C19A C18A 103(4) . . ?
F18A C19A C18A 113(4) . . ?
F18A C19A F17A 112(3) . . ?
H20A C20 H20B 108.7 . . ?
C21 C20 H20A 110.6 . . ?
C21 C20 H20B 110.6 . . ?
O1 C20 H20A 110.6 . . ?
O1 C20 H20B 110.6 . . ?
O1 C20 C21 105.9(3) . . ?
C20 C21 H21A 108.6 . . ?
C20 C21 H21B 108.6 . . ?
C20 C21 C22 114.6(3) . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C21 C22 C23 112.0(3) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C22 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.6(3) . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C23 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
C23 C24 C25 113.8(3) . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 C24 113.3(3) . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C25 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 C25 114.6(3) . . ?
C27 C26 H26A 108.6 . . ?
C27 C26 H26B 108.6 . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
C26 C27 C28 113.3(4) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 108.2 . . ?
C27 C28 H28B 108.2 . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 C27 116.2(4) . . ?
C29 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C7 N1 C10 129.3(3) . . ?
C7 N1 N2 112.1(3) . . ?
N2 N1 C10 118.6(3) . . ?
C8 N2 N1 103.7(3) . . ?
C7 N3 C8 105.4(3) . . ?
C7 N3 C9 126.9(3) . . ?
C8 N3 C9 127.6(3) . . ?
C1 O1 C20 120.5(3) . . ?
F20 C30 S1 111.9(3) . . ?
F21 C30 F20 107.0(3) . . ?
F21 C30 F22 108.1(4) . . ?
F21 C30 S1 111.5(3) . . ?
F22 C30 F20 105.9(3) . . ?
F22 C30 S1 112.1(3) . . ?
O2 S1 C30 103.3(3) . . ?
O2 S1 O4 111.3(3) . . ?
O2A S1 C30 99.6(5) . . ?
O3 S1 C30 103.5(9) . . ?
O3 S1 O2 129.1(7) . . ?
O3 S1 O4 105.8(6) . . ?
O3A S1 C30 107(2) . . ?
O3A S1 O2A 84.5(14) . . ?
O4 S1 C30 99.6(3) . . ?
O4A S1 C30 110.0(8) . . ?
O4A S1 O2A 121.9(7) . . ?
O4A S1 O3A 128.2(19) . . ?

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
C1 C2 C3 C4 -1.3(5) . . . . ?
C2 C1 C6 C5 0.7(5) . . . . ?
C2 C1 O1 C20 -176.5(3) . . . . ?
C2 C3 C4 C5 1.6(5) . . . . ?
C2 C3 C4 C7 -179.4(3) . . . . ?
C3 C4 C5 C6 -0.7(5) . . . . ?
C3 C4 C7 N1 44.2(5) . . . . ?
C3 C4 C7 N3 -133.1(4) . . . . ?
C4 C5 C6 C1 -0.4(5) . . . . ?
C4 C7 N1 C10 2.0(6) . . . . ?
C4 C7 N1 N2 -177.5(3) . . . . ?
C4 C7 N3 C8 177.6(3) . . . . ?
C4 C7 N3 C9 0.3(5) . . . . ?
C5 C4 C7 N1 -136.8(3) . . . . ?
C5 C4 C7 N3 45.8(5) . . . . ?
C6 C1 C2 C3 0.2(5) . . . . ?
C6 C1 O1 C20 3.5(5) . . . . ?
C7 C4 C5 C6 -179.7(3) . . . . ?
C7 N1 N2 C8 -0.3(3) . . . . ?
C8 C11 C12 C13 173.6(3) . . . . ?
C8 C11 C12 F3 -64.8(4) . . . . ?
C8 C11 C12 F4 53.2(4) . . . . ?
C10 N1 N2 C8 -179.9(3) . . . . ?
C11 C8 N2 N1 178.8(3) . . . . ?
C11 C8 N3 C7 -178.7(3) . . . . ?
C11 C8 N3 C9 -1.4(5) . . . . ?
C11 C12 C13 C14 155.5(3) . . . . ?
C11 C12 C13 C14A 172(2) . . . . ?
C11 C12 C13 F5 33.1(4) . . . . ?
C11 C12 C13 F5A 62(3) . . . . ?
C11 C12 C13 F6 -84.1(4) . . . . ?
C11 C12 C13 F6A -53(3) . . . . ?
C12 C13 C14 C15 166.2(3) . . . . ?
C12 C13 C14 F7 -73.5(4) . . . . ?
C12 C13 C14 F8 44.8(4) . . . . ?
C12 C13 C14A C15A -145(4) . . . . ?
C12 C13 C14A F7A 96(4) . . . . ?
C12 C13 C14A F8A -14(4) . . . . ?
C13 C14 C15 C16 165.7(3) . . . . ?
C13 C14 C15 F9 45.1(5) . . . . ?
C13 C14 C15 F10 -73.0(4) . . . . ?
C13 C14A C15A C16A -157(5) . . . . ?
C13 C14A C15A F9A -34(7) . . . . ?
C13 C14A C15A F10A 73(7) . . . . ?
C14 C15 C16 C17 173.6(3) . . . . ?
C14 C15 C16 F11 -64.9(4) . . . . ?
C14 C15 C16 F12 52.3(5) . . . . ?
C14A C15A C16A C17A -177(5) . . . . ?
C14A C15A C16A F11A 54(7) . . . . ?
C14A C15A C16A F12A -56(8) . . . . ?
C15 C16 C17 C18 179.0(3) . . . . ?
C15 C16 C17 F13 59.6(4) . . . . ?
C15 C16 C17 F14 -58.9(4) . . . . ?
C15A C16A C17A C18A 169(4) . . . . ?
C15A C16A C17A F13A -62(5) . . . . ?
C15A C16A C17A F14A 55(6) . . . . ?
C16 C17 C18 C19 -175.9(3) . . . . ?
C16 C17 C18 F15 -52.2(5) . . . . ?
C16 C17 C18 F16 66.0(4) . . . . ?
C16A C17A C18A C19A 174(4) . . . . ?
C16A C17A C18A F15A 63(4) . . . . ?
C16A C17A C18A F16A -57(5) . . . . ?
C17 C18 C19 F17 178.6(3) . . . . ?
C17 C18 C19 F18 -59.7(5) . . . . ?
C17 C18 C19 F19 61.2(5) . . . . ?
C17A C18A C19A F17A 74(4) . . . . ?
C17A C18A C19A F18A -164(4) . . . . ?
C20 C21 C22 C23 178.8(3) . . . . ?
C21 C20 O1 C1 174.6(3) . . . . ?
C21 C22 C23 C24 -178.0(3) . . . . ?
C22 C23 C24 C25 -179.3(3) . . . . ?
C23 C24 C25 C26 -179.0(3) . . . . ?
C24 C25 C26 C27 -178.3(3) . . . . ?
C25 C26 C27 C28 -177.6(4) . . . . ?
C26 C27 C28 C29 -177.5(4) . . . . ?
F1 C11 C12 C13 -65.2(4) . . . . ?
F1 C11 C12 F3 56.4(3) . . . . ?
F1 C11 C12 F4 174.4(3) . . . . ?
F2 C11 C12 C13 50.2(4) . . . . ?
F2 C11 C12 F3 171.8(3) . . . . ?
F2 C11 C12 F4 -70.2(3) . . . . ?
F3 C12 C13 C14 34.9(4) . . . . ?
F3 C12 C13 C14A 51(2) . . . . ?
F3 C12 C13 F5 -87.4(4) . . . . ?
F3 C12 C13 F5A -59(3) . . . . ?
F3 C12 C13 F6 155.3(3) . . . . ?
F3 C12 C13 F6A -174(3) . . . . ?
F4 C12 C13 C14 -82.8(4) . . . . ?
F4 C12 C13 C14A -66(2) . . . . ?
F4 C12 C13 F5 154.8(3) . . . . ?
F4 C12 C13 F5A -177(3) . . . . ?
F4 C12 C13 F6 37.6(4) . . . . ?
F4 C12 C13 F6A 68(3) . . . . ?
F5 C13 C14 C15 -71.0(4) . . . . ?
F5 C13 C14 F7 49.4(4) . . . . ?
F5 C13 C14 F8 167.6(3) . . . . ?
F5A C13 C14A C15A -32(6) . . . . ?
F5A C13 C14A F7A -151(4) . . . . ?
F5A C13 C14A F8A 100(4) . . . . ?
F6 C13 C14 C15 46.1(4) . . . . ?
F6 C13 C14 F7 166.5(3) . . . . ?
F6 C13 C14 F8 -75.3(4) . . . . ?
F6A C13 C14A C15A 78(6) . . . . ?
F6A C13 C14A F7A -42(5) . . . . ?
F6A C13 C14A F8A -151(5) . . . . ?
F7 C14 C15 C16 46.2(4) . . . . ?
F7 C14 C15 F9 -74.3(4) . . . . ?
F7 C14 C15 F10 167.6(3) . . . . ?
F7A C14A C15A C16A -43(7) . . . . ?
F7A C14A C15A F9A 80(6) . . . . ?
F7A C14A C15A F10A -172(5) . . . . ?
F8 C14 C15 C16 -72.6(4) . . . . ?
F8 C14 C15 F9 166.9(3) . . . . ?
F8 C14 C15 F10 48.7(4) . . . . ?
F8A C14A C15A C16A 71(7) . . . . ?
F8A C14A C15A F9A -166(7) . . . . ?
F8A C14A C15A F10A -58(6) . . . . ?
F9 C15 C16 C17 -65.3(4) . . . . ?
F9 C15 C16 F11 56.3(4) . . . . ?
F9 C15 C16 F12 173.4(4) . . . . ?
F9A C15A C16A C17A 78(8) . . . . ?
F9A C15A C16A F11A -50(8) . . . . ?
F9A C15A C16A F12A -160(8) . . . . ?
F10 C15 C16 C17 52.6(4) . . . . ?
F10 C15 C16 F11 174.2(3) . . . . ?
F10 C15 C16 F12 -68.7(4) . . . . ?
F10A C15A C16A C17A -49(7) . . . . ?
F10A C15A C16A F11A -178(6) . . . . ?
F10A C15A C16A F12A 73(7) . . . . ?
F11 C16 C17 C18 57.2(4) . . . . ?
F11 C16 C17 F13 -62.2(4) . . . . ?
F11 C16 C17 F14 179.3(3) . . . . ?
F11A C16A C17A C18A -64(6) . . . . ?
F11A C16A C17A F13A 65(5) . . . . ?
F11A C16A C17A F14A -178(5) . . . . ?
F12 C16 C17 C18 -59.6(4) . . . . ?
F12 C16 C17 F13 -179.0(3) . . . . ?
F12 C16 C17 F14 62.5(4) . . . . ?
F12A C16A C17A C18A 58(8) . . . . ?
F12A C16A C17A F13A -173(7) . . . . ?
F12A C16A C17A F14A -56(7) . . . . ?
F13 C17 C18 C19 -56.5(5) . . . . ?
F13 C17 C18 F15 67.2(4) . . . . ?
F13 C17 C18 F16 -174.6(3) . . . . ?
F13A C17A C18A C19A 57(5) . . . . ?
F13A C17A C18A F15A -54(4) . . . . ?
F13A C17A C18A F16A -174(3) . . . . ?
F14 C17 C18 C19 60.7(4) . . . . ?
F14 C17 C18 F15 -175.5(3) . . . . ?
F14 C17 C18 F16 -57.4(4) . . . . ?
F14A C17A C18A C19A -73(4) . . . . ?
F14A C17A C18A F15A 176(4) . . . . ?
F14A C17A C18A F16A 56(4) . . . . ?
F15 C18 C19 F17 53.7(5) . . . . ?
F15 C18 C19 F18 175.4(4) . . . . ?
F15 C18 C19 F19 -63.7(4) . . . . ?
F15A C18A C19A F17A -177(4) . . . . ?
F15A C18A C19A F18A -55(4) . . . . ?
F16 C18 C19 F17 -62.8(4) . . . . ?
F16 C18 C19 F18 58.9(4) . . . . ?
F16 C18 C19 F19 179.8(3) . . . . ?
F16A C18A C19A F17A -51(4) . . . . ?
F16A C18A C19A F18A 70(5) . . . . ?
N1 C7 N3 C8 -0.2(3) . . . . ?
N1 C7 N3 C9 -177.5(3) . . . . ?
N2 C8 C11 C12 2.8(5) . . . . ?
N2 C8 C11 F1 -118.1(3) . . . . ?
N2 C8 C11 F2 124.4(3) . . . . ?
N2 C8 N3 C7 0.0(4) . . . . ?
N2 C8 N3 C9 177.2(3) . . . . ?
N3 C7 N1 C10 179.8(3) . . . . ?
N3 C7 N1 N2 0.3(4) . . . . ?
N3 C8 C11 C12 -178.7(3) . . . . ?
N3 C8 C11 F1 60.4(4) . . . . ?
N3 C8 C11 F2 -57.1(4) . . . . ?
N3 C8 N2 N1 0.2(4) . . . . ?
O1 C1 C2 C3 -179.8(3) . . . . ?
O1 C1 C6 C5 -179.3(3) . . . . ?
O1 C20 C21 C22 -177.1(3) . . . . ?
F20 C30 S1 O2 -69.3(4) . . . . ?
F20 C30 S1 O2A -34.5(7) . . . . ?
F20 C30 S1 O3 67.0(5) . . . . ?
F20 C30 S1 O3A 52.8(13) . . . . ?
F20 C30 S1 O4 176.0(4) . . . . ?
F20 C30 S1 O4A -163.6(7) . . . . ?
F21 C30 S1 O2 170.9(4) . . . . ?
F21 C30 S1 O2A -154.3(7) . . . . ?
F21 C30 S1 O3 -52.7(5) . . . . ?
F21 C30 S1 O3A -67.0(13) . . . . ?
F21 C30 S1 O4 56.2(4) . . . . ?
F21 C30 S1 O4A 76.6(7) . . . . ?
F22 C30 S1 O2 49.5(5) . . . . ?
F22 C30 S1 O2A 84.4(7) . . . . ?
F22 C30 S1 O3 -174.1(5) . . . . ?
F22 C30 S1 O3A 171.6(13) . . . . ?
F22 C30 S1 O4 -65.2(4) . . . . ?
F22 C30 S1 O4A -44.8(7) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-11-21
_olex2_date_sample_submission    2016-11-19
_olex2_exptl_crystal_mounting_method 'oil on 150 micrometre micromount'
_olex2_submission_original_sample_id ALR11
_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 1.678
_oxdiff_exptl_absorpt_empirical_full_min 0.740
####################################################################### 
# 
# 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_dwb1671
_database_code_depnum_ccdc_archive 'CCDC 2177833'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'B F4, C29 H31 F19 N3 O, C3 H6 O'
_chemical_formula_sum            'C32 H37 B F23 N3 O2'
_chemical_formula_weight         943.45
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H31 B1 F23 N3 O1'
_chemical_oxdiff_usercomment     'Alessio Riccobono ALR17'
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'
B B 0.0090 0.0039 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   37.0798(6)
_cell_length_b                   9.45070(11)
_cell_length_c                   11.29828(17)
_cell_angle_alpha                90
_cell_angle_beta                 98.5285(14)
_cell_angle_gamma                90
_cell_volume                     3915.48(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10558
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.9520
_cell_measurement_theta_min      4.6630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.1100
0 -2 -5 0.1064
0 2 5 0.0738
-2 0 5 0.3460
2 0 -5 0.3315
0 0 -1 0.0554
1 5 -1 0.1296
0 0 1 0.0469
-5 0 -4 0.3777
5 0 4 0.3605
0 1 0 0.0671

_exptl_crystal_size_max          0.796
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.102
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
0.0002 -1.0005 -0.0008 -0.0021 0.0223 -0.1615
0.0017 -2.0004 -5.0048 -0.2117 0.0116 -0.3249
-0.0017 2.0004 5.0048 0.2117 -0.0116 0.3249
-2.0010 0.0001 5.0010 0.2101 -0.2401 -0.0358
2.0010 -0.0001 -5.0010 -0.2101 0.2401 0.0358
0.0002 0.0001 -1.0006 -0.0415 -0.0066 -0.0004
0.9990 5.0024 -0.9957 -0.0324 0.0184 0.8260
-0.0002 -0.0001 1.0006 0.0415 0.0066 0.0004
-4.9986 0.0024 -4.0081 -0.1598 -0.7093 -0.0954
4.9986 -0.0024 4.0081 0.1598 0.7093 0.0954
-0.0002 1.0005 0.0008 0.0021 -0.0223 0.1615

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20003
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         3.616
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  70.00   1.00    7.50    --    0.00  77.00  60.00  100
  2  ω    -18.00  80.00   1.00   30.00    --   54.00 -37.00  60.00   98
  3  ω     23.00 111.00   1.00   30.00    --   54.00-125.00  60.00   88
  4  ω     28.00 126.00   1.00   30.00    --   54.00  37.00-120.00   98
  5  ω     86.00 178.00   1.00   30.00    --  108.00  50.00 -30.00   92
  6  ω     36.00 178.00   1.00   30.00    --  108.00  12.00 -60.00  142
  7  ω     36.00 116.00   1.00   30.00    --  108.00-111.00 -30.00   80
  8  ω     36.00 116.00   1.00   30.00    --  108.00-111.00  30.00   80
  9  ω     57.00 151.00   1.00   30.00    --  108.00 178.00 -90.00   94
 10  ω     40.00 130.00   1.00   30.00    --  108.00 -63.00   0.00   90
 11  ω    -69.00  21.00   1.00    7.50    --    0.00 -57.00 -60.00   90
 12  ω     24.00 124.00   1.00   30.00    --   54.00  77.00 120.00  100
 13  ω     24.00 124.00   1.00   30.00    --   54.00  77.00 -60.00  100
 14  ω     24.00 124.00   1.00   30.00    --   54.00  77.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0013044000
_diffrn_orient_matrix_UB_12      0.0020379000
_diffrn_orient_matrix_UB_13      0.0414930000
_diffrn_orient_matrix_UB_21      0.1365702000
_diffrn_orient_matrix_UB_22      -0.0222655000
_diffrn_orient_matrix_UB_23      0.0066330000
_diffrn_orient_matrix_UB_31      0.0188511000
_diffrn_orient_matrix_UB_32      0.1614388000
_diffrn_orient_matrix_UB_33      0.0003909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6587
_reflns_number_total             6997
_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 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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         0.487
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         6997
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0817
_refine_ls_restrained_S_all      1.195
_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)+(0.0294P)²+13.1975P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.1774
_refine_special_details          
;
There is disorder in the perfluoronated chain, Mulitple C-F bond lengths have been restrainted to 1.34 A and multiple F-C-F bond angles have also been fixed. ADPs of mulitple C atoms in the chain and 1 F atom have been constrained using the neighbouring atoms as a template.  Full list of orders: DFIX 1.55 C22 C23B
DFIX 1.34 F7 C24
DFIX 1.34 F3BA C23B
DFIX 1.34 F6B C24B
DFIX 1.34 C28B F13B
DFIX 1.34 C29B F16B
DFIX 1.34 C29B F17B
DFIX 1.34 C29B F15B
DFIX 1.34 C29 F19
DFIX 1.34 C29 F18
DFIX 1.34 C29 F17
DANG 2.17 F7 F8
DANG 2.6 C26 C28
DANG 2.17 F6B F5B
DANG 2.17 F8B F7B
DANG 2.17 F11B F12B
EADP C22 C23B
EADP C22 C23
EADP C24 C25B C23B C24
EADP C23B C24
EADP F5B F7
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-C23B
 1.55 with sigma of 0.02
 F7-C24
 1.34 with sigma of 0.02
 F3BA-C23B
 1.34 with sigma of 0.02
 F6B-C24B
 1.34 with sigma of 0.02
 C28B-F13B
 1.34 with sigma of 0.02
 C29B-F16B
 1.34 with sigma of 0.02
 C29B-F17B
 1.34 with sigma of 0.02
 C29B-F15B
 1.34 with sigma of 0.02
 C29-F19
 1.34 with sigma of 0.02
 C29-F18
 1.34 with sigma of 0.02
 C29-F17
 1.34 with sigma of 0.02
 F7-F8
 2.17 with sigma of 0.04
 C26-C28
 2.6 with sigma of 0.04
 F6B-F5B
 2.17 with sigma of 0.04
 F8B-F7B
 2.17 with sigma of 0.04
 F11B-F12B
 2.17 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C23B)
Uanis(C22) = Uanis(C23)
Uanis(C24) = Uanis(C25B) = Uanis(C23B) = Uanis(C24)
Uanis(C23B) = Uanis(C24)
Uanis(F5B) = Uanis(F7)
4. Others
 Sof(C24B)=Sof(F14B)=Sof(F13B)=Sof(C28B)=Sof(F11B)=Sof(F12B)=Sof(C27B)=
 Sof(F9B)=Sof(F10B)=Sof(C26B)=Sof(F8B)=Sof(C25B)=Sof(F7B)=Sof(F6B)=Sof(F5B)=
 Sof(F4BA)=Sof(F3BA)=Sof(C23B)=Sof(F16B)=Sof(F15B)=Sof(C29B)=Sof(F17B)=1-FVAR(1)
 Sof(C23)=Sof(C26)=Sof(C25)=Sof(C27)=Sof(C28)=Sof(F7)=Sof(F14)=Sof(F13)=
 Sof(F6)=Sof(F9)=Sof(F10)=Sof(F12)=Sof(F11)=Sof(F8)=Sof(F5)=Sof(F16)=Sof(F15)=
 Sof(F17)=Sof(F19)=Sof(F18)=Sof(C24)=Sof(C29)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C8(H8A,H8B), C7(H7A,
 H7B), C9(H9A,H9B), C4(H4A,H4B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C1(H1A,H1B,H1C), C32(H32A,H32B,
 H32C), C31(H31A,H31B,H31C)
;
_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
F001 F 0.70734(8) 0.8073(3) 0.0514(2) 0.0485(7) Uani 1 1 d . . . . .
F1 F 0.80043(6) 0.8056(2) 0.2113(3) 0.0452(7) Uani 1 1 d . . . . .
F003 F 0.70800(8) 1.0457(3) 0.0351(2) 0.0438(6) Uani 1 1 d . . . . .
O1 O 0.60447(7) 0.3321(3) 0.3765(2) 0.0257(6) Uani 1 1 d . . . . .
F2 F 0.81220(6) 0.7383(3) 0.0357(2) 0.0476(7) Uani 1 1 d . . . . .
F3 F 0.83669(7) 0.5753(3) 0.3116(2) 0.0578(8) Uani 1 1 d . . . . .
F008 F 0.66934(7) 0.9414(4) 0.1445(3) 0.0589(8) Uani 1 1 d . . . . .
F009 F 0.72973(8) 0.9419(3) 0.2110(2) 0.0559(8) Uani 1 1 d . . . . .
N2 N 0.74830(8) 0.5867(3) 0.2054(2) 0.0216(6) Uani 1 1 d . . . . .
N1 N 0.72950(8) 0.4771(3) 0.0427(3) 0.0237(6) Uani 1 1 d . . . . .
F4 F 0.84685(8) 0.5059(3) 0.1384(3) 0.0718(11) Uani 1 1 d . . . . .
N3 N 0.76173(8) 0.5365(4) 0.0263(3) 0.0279(7) Uani 1 1 d . . . . .
C17 C 0.72081(9) 0.5059(4) 0.1500(3) 0.0208(7) Uani 1 1 d . . . . .
C14 C 0.68865(10) 0.4628(4) 0.1987(3) 0.0214(7) Uani 1 1 d . . . . .
C11 C 0.63111(9) 0.3811(4) 0.3156(3) 0.0213(7) Uani 1 1 d . . . . .
C20 C 0.77220(10) 0.6028(4) 0.1268(3) 0.0236(8) Uani 1 1 d . . . . .
C12 C 0.64850(10) 0.2815(4) 0.2534(3) 0.0223(7) Uani 1 1 d . . . . .
H12 H 0.640590 0.187955 0.249867 0.027 Uiso 1 1 calc R U . . .
O2 O 0.77924(12) 0.3074(4) 0.2443(4) 0.0736(12) Uani 1 1 d . . . . .
C10 C 0.59039(10) 0.4294(4) 0.4568(3) 0.0240(8) Uani 1 1 d . . . . .
H10A H 0.576844 0.504571 0.411598 0.029 Uiso 1 1 calc R U . . .
H10B H 0.610305 0.471601 0.510631 0.029 Uiso 1 1 calc R U . . .
C13 C 0.67746(10) 0.3210(4) 0.1970(3) 0.0219(7) Uani 1 1 d . . . . .
H13 H 0.689585 0.253451 0.157752 0.026 Uiso 1 1 calc R U . . .
C2 C 0.40308(10) 0.4702(4) 1.0273(3) 0.0251(8) Uani 1 1 d . . . . .
H2A H 0.387238 0.527598 0.970427 0.030 Uiso 1 1 calc R U . . .
H2B H 0.418671 0.533628 1.079602 0.030 Uiso 1 1 calc R U . . .
C15 C 0.66943(10) 0.5639(4) 0.2555(3) 0.0243(8) Uani 1 1 d . . . . .
H15 H 0.675983 0.658774 0.254262 0.029 Uiso 1 1 calc R U . . .
C16 C 0.64088(10) 0.5230(4) 0.3131(3) 0.0248(8) Uani 1 1 d . . . . .
H16 H 0.628122 0.590336 0.350278 0.030 Uiso 1 1 calc R U . . .
C6 C 0.50028(10) 0.4536(4) 0.7524(3) 0.0256(8) Uani 1 1 d . . . . .
H6A H 0.486210 0.521590 0.700206 0.031 Uiso 1 1 calc R U . . .
H6B H 0.517198 0.506123 0.809911 0.031 Uiso 1 1 calc R U . . .
C22 C 0.84136(10) 0.6191(4) 0.2026(3) 0.0284(7) Uani 1 1 d D . . . .
C5 C 0.47441(10) 0.3695(4) 0.8194(3) 0.0259(8) Uani 1 1 d . . . . .
H5A H 0.458305 0.313501 0.762186 0.031 Uiso 1 1 calc R U . . .
H5B H 0.488641 0.304720 0.874282 0.031 Uiso 1 1 calc R U . . .
C8 C 0.54706(10) 0.4427(4) 0.6074(3) 0.0263(8) Uani 1 1 d . . . . .
H8A H 0.532981 0.513894 0.558824 0.032 Uiso 1 1 calc R U . . .
H8B H 0.565435 0.491112 0.662957 0.032 Uiso 1 1 calc R U . . .
C7 C 0.52189(10) 0.3607(4) 0.6777(3) 0.0257(8) Uani 1 1 d . . . . .
H7A H 0.536411 0.294483 0.730443 0.031 Uiso 1 1 calc R U . . .
H7B H 0.504906 0.306089 0.622055 0.031 Uiso 1 1 calc R U . . .
C9 C 0.56572(10) 0.3479(4) 0.5271(3) 0.0243(8) Uani 1 1 d . . . . .
H9A H 0.579970 0.277183 0.575720 0.029 Uiso 1 1 calc R U . . .
H9B H 0.547350 0.298886 0.471945 0.029 Uiso 1 1 calc R U . . .
C21 C 0.80574(10) 0.6928(4) 0.1435(3) 0.0299(9) Uani 1 1 d . . . . .
C4 C 0.45135(10) 0.4620(4) 0.8898(3) 0.0246(8) Uani 1 1 d . . . . .
H4A H 0.467421 0.520519 0.945028 0.029 Uiso 1 1 calc R U . . .
H4B H 0.436432 0.524413 0.834544 0.029 Uiso 1 1 calc R U . . .
C3 C 0.42667(10) 0.3777(4) 0.9598(3) 0.0262(8) Uani 1 1 d . . . . .
H3A H 0.410991 0.317462 0.904797 0.031 Uiso 1 1 calc R U . . .
H3B H 0.441620 0.316959 1.016402 0.031 Uiso 1 1 calc R U . . .
C18 C 0.70899(11) 0.3918(5) -0.0537(3) 0.0316(9) Uani 1 1 d . . . . .
H18A H 0.710830 0.434507 -0.129634 0.047 Uiso 1 1 calc R U . . .
H18B H 0.683834 0.387368 -0.042671 0.047 Uiso 1 1 calc R U . . .
H18C H 0.718932 0.297879 -0.051529 0.047 Uiso 1 1 calc R U . . .
C19 C 0.75210(11) 0.6344(4) 0.3310(3) 0.0299(8) Uani 1 1 d . . . . .
H19A H 0.745124 0.732091 0.333450 0.045 Uiso 1 1 calc R U . . .
H19B H 0.777000 0.623881 0.367834 0.045 Uiso 1 1 calc R U . . .
H19C H 0.736639 0.578336 0.373515 0.045 Uiso 1 1 calc R U . . .
C1 C 0.37983(11) 0.3849(4) 1.1019(4) 0.0317(9) Uani 1 1 d . . . . .
H1A H 0.363570 0.324844 1.050278 0.048 Uiso 1 1 calc R U . . .
H1B H 0.365905 0.448251 1.143822 0.048 Uiso 1 1 calc R U . . .
H1C H 0.395340 0.327954 1.158549 0.048 Uiso 1 1 calc R U . . .
C23 C 0.8761(2) 0.7056(9) 0.2030(7) 0.0284(7) Uani 0.591(2) 1 d . . P A 1
C30 C 0.79557(12) 0.2015(4) 0.2241(5) 0.0419(11) Uani 1 1 d . . . . .
C24B C 0.9123(3) 0.6559(14) 0.2601(9) 0.027(3) Uani 0.409(2) 1 d D . P A 2
C32 C 0.81566(14) 0.1174(5) 0.3235(4) 0.0500(12) Uani 1 1 d . . . . .
H32A H 0.821831 0.176846 0.392454 0.075 Uiso 1 1 calc R U . . .
H32B H 0.837560 0.080232 0.299536 0.075 Uiso 1 1 calc R U . . .
H32C H 0.800594 0.040723 0.342913 0.075 Uiso 1 1 calc R U . . .
B1 B 0.70342(13) 0.9336(5) 0.1106(4) 0.0291(10) Uani 1 1 d . . . . .
C31 C 0.79556(14) 0.1463(6) 0.1008(4) 0.0552(13) Uani 1 1 d . . . . .
H31A H 0.780129 0.064463 0.088639 0.083 Uiso 1 1 calc R U . . .
H31B H 0.819952 0.120955 0.090308 0.083 Uiso 1 1 calc R U . . .
H31C H 0.786575 0.218066 0.043750 0.083 Uiso 1 1 calc R U . . .
C26 C 0.9766(2) 0.7139(8) 0.3822(7) 0.0275(16) Uani 0.591(2) 1 d D . P A 1
C25 C 0.94578(19) 0.7170(7) 0.2738(6) 0.0264(14) Uani 0.591(2) 1 d . . P A 1
C27 C 1.01573(18) 0.7192(7) 0.3488(7) 0.0258(14) Uani 0.591(2) 1 d . . P A 1
C28 C 1.0466(2) 0.7523(10) 0.4547(8) 0.037(2) Uani 0.591(2) 1 d D . P A 1
F7 F 0.9091(13) 0.5198(19) 0.304(2) 0.049(3) Uani 0.591(2) 1 d D . P A 1
F14 F 1.01684(12) 0.8190(6) 0.2676(4) 0.0585(15) Uani 0.591(2) 1 d . . P A 1
F13 F 1.02320(12) 0.5941(5) 0.3061(5) 0.0597(15) Uani 0.591(2) 1 d . . P A 1
F6 F 0.88616(11) 0.6882(6) 0.0948(3) 0.0529(14) Uani 0.591(2) 1 d . . P A 1
F9 F 0.9429(2) 0.8474(7) 0.2296(7) 0.0480(17) Uani 0.591(2) 1 d . . P A 1
F10 F 0.95659(11) 0.6374(6) 0.1866(4) 0.0485(12) Uani 0.591(2) 1 d . . P A 1
F12 F 0.97311(12) 0.5983(6) 0.4452(4) 0.0549(15) Uani 0.591(2) 1 d . . P A 1
F11 F 0.97226(13) 0.8269(6) 0.4505(5) 0.0621(15) Uani 0.591(2) 1 d . . P A 1
F8 F 0.90273(12) 0.7141(6) 0.4044(4) 0.0549(14) Uani 0.591(2) 1 d D . P A 1
F5 F 0.86946(17) 0.8423(6) 0.2194(8) 0.062(2) Uani 0.591(2) 1 d . . P A 1
F16 F 1.03939(13) 0.6874(6) 0.5514(4) 0.0599(15) Uani 0.591(2) 1 d . . P A 1
F15 F 1.04559(15) 0.8923(5) 0.4767(6) 0.0764(19) Uani 0.591(2) 1 d . . P A 1
F17 F 1.08941(12) 0.5770(5) 0.4346(5) 0.0602(14) Uani 0.591(2) 1 d D . P A 1
F19 F 1.09222(14) 0.7662(7) 0.3337(6) 0.083(2) Uani 0.591(2) 1 d D . P A 1
F18 F 1.1088(3) 0.7629(14) 0.5236(8) 0.087(3) Uani 0.591(2) 1 d D . P A 1
F14B F 1.0561(2) 0.8095(13) 0.2954(6) 0.096(4) Uani 0.409(2) 1 d . . P A 2
F13B F 1.0554(2) 0.6043(9) 0.3841(13) 0.123(5) Uani 0.409(2) 1 d D . P A 2
C28B C 1.0496(4) 0.7402(13) 0.3933(12) 0.041(3) Uani 0.409(2) 1 d D . P A 2
F11B F 1.00802(18) 0.7225(10) 0.5236(5) 0.064(2) Uani 0.409(2) 1 d D . P A 2
F12B F 1.00525(19) 0.9074(7) 0.4146(8) 0.067(2) Uani 0.409(2) 1 d D . P A 2
C27B C 1.0113(3) 0.7686(11) 0.4135(10) 0.030(2) Uani 0.409(2) 1 d . . P A 2
F9B F 0.98302(19) 0.5606(7) 0.3399(12) 0.092(4) Uani 0.409(2) 1 d . . P A 2
F10B F 0.9888(2) 0.7300(13) 0.2144(6) 0.089(3) Uani 0.409(2) 1 d . . P A 2
C26B C 0.9810(3) 0.6997(13) 0.3238(11) 0.030(3) Uani 0.409(2) 1 d . . P A 2
F8B F 0.93753(18) 0.7537(10) 0.4425(6) 0.064(2) Uani 0.409(2) 1 d D . P A 2
C25B C 0.9426(3) 0.7495(11) 0.3284(10) 0.0284(7) Uani 0.409(2) 1 d . . P A 2
F7B F 0.9382(3) 0.8802(11) 0.2862(11) 0.061(3) Uani 0.409(2) 1 d D . P A 2
F6B F 0.92187(17) 0.6206(9) 0.1534(6) 0.065(2) Uani 0.409(2) 1 d D . P A 2
F5B F 0.910(2) 0.541(3) 0.322(4) 0.049(3) Uani 0.409(2) 1 d D . P A 2
C24 C 0.9085(3) 0.6628(11) 0.2987(8) 0.0284(7) Uani 0.591(2) 1 d D . P A 1
F4BA F 0.86812(16) 0.7905(7) 0.3356(6) 0.0454(16) Uani 0.409(2) 1 d . . P A 2
F3BA F 0.8745(3) 0.8225(11) 0.1504(8) 0.055(3) Uani 0.409(2) 1 d D . P A 2
C23B C 0.8743(3) 0.7255(12) 0.2345(9) 0.0284(7) Uani 0.409(2) 1 d D . P A 2
F16B F 1.0800(2) 0.7294(12) 0.5931(8) 0.093(3) Uani 0.409(2) 1 d D . P A 2
F15B F 1.0771(2) 0.9265(8) 0.5143(9) 0.088(3) Uani 0.409(2) 1 d D . P A 2
C29 C 1.0853(2) 0.7140(9) 0.4350(8) 0.046(2) Uani 0.591(2) 1 d D . P A 1
C29B C 1.0804(3) 0.7915(12) 0.4909(11) 0.044(3) Uani 0.409(2) 1 d D . P A 2
F17B F 1.1127(3) 0.774(2) 0.4614(11) 0.075(4) Uani 0.409(2) 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F001 B1 1.386(5) . ?
F1 C21 1.344(5) . ?
F003 B1 1.386(5) . ?
O1 C11 1.366(4) . ?
O1 C10 1.443(4) . ?
F2 C21 1.346(4) . ?
F3 C22 1.334(4) . ?
F008 B1 1.376(5) . ?
F009 B1 1.384(5) . ?
N2 C17 1.351(4) . ?
N2 C20 1.353(5) . ?
N2 C19 1.476(4) . ?
N1 N3 1.358(4) . ?
N1 C17 1.328(4) . ?
N1 C18 1.472(4) . ?
F4 C22 1.325(5) . ?
N3 C20 1.305(5) . ?
C17 C14 1.444(5) . ?
C14 C13 1.402(5) . ?
C14 C15 1.402(5) . ?
C11 C12 1.390(5) . ?
C11 C16 1.390(5) . ?
C20 C21 1.496(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(5) . ?
O2 C30 1.209(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C9 1.510(5) . ?
C13 H13 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.520(5) . ?
C2 C1 1.522(5) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(5) . ?
C16 H16 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.530(5) . ?
C6 C7 1.525(5) . ?
C22 C21 1.554(5) . ?
C22 C23 1.526(9) . ?
C22 C23B 1.581(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.526(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.525(5) . ?
C8 C9 1.513(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.520(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C23 F6 1.339(8) . ?
C23 F5 1.333(10) . ?
C23 C24 1.545(14) . ?
C30 C32 1.483(6) . ?
C30 C31 1.488(7) . ?
C24B C25B 1.542(17) . ?
C24B F6B 1.348(10) . ?
C24B F5B 1.30(3) . ?
C24B C23B 1.545(19) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C26 C25 1.547(10) . ?
C26 C27 1.552(11) . ?
C26 F12 1.321(8) . ?
C26 F11 1.341(10) . ?
C25 F9 1.328(9) . ?
C25 F10 1.346(9) . ?
C25 C24 1.539(12) . ?
C27 C28 1.560(10) . ?
C27 F14 1.321(7) . ?
C27 F13 1.322(9) . ?
C28 F16 1.315(11) . ?
C28 F15 1.349(10) . ?
C28 C29 1.527(13) . ?
F7 C24 1.353(18) . ?
F8 C24 1.334(10) . ?
F17 C29 1.304(9) . ?
F19 C29 1.305(9) . ?
F18 C29 1.310(11) . ?
F14B C28B 1.337(16) . ?
F13B C28B 1.309(13) . ?
C28B C27B 1.497(18) . ?
C28B C29B 1.543(17) . ?
F11B C27B 1.341(12) . ?
F12B C27B 1.331(12) . ?
C27B C26B 1.540(15) . ?
F9B C26B 1.328(14) . ?
F10B C26B 1.341(14) . ?
C26B C25B 1.510(16) . ?
F8B C25B 1.330(13) . ?
C25B F7B 1.325(15) . ?
F4BA C23B 1.346(12) . ?
F3BA C23B 1.321(13) . ?
F16B C29B 1.297(12) . ?
F15B C29B 1.313(13) . ?
C29B F17B 1.298(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 O1 C10 117.1(3) . . ?
C17 N2 C20 106.4(3) . . ?
C17 N2 C19 125.2(3) . . ?
C20 N2 C19 128.2(3) . . ?
N3 N1 C18 119.6(3) . . ?
C17 N1 N3 112.2(3) . . ?
C17 N1 C18 128.2(3) . . ?
C20 N3 N1 103.5(3) . . ?
N2 C17 C14 126.3(3) . . ?
N1 C17 N2 105.7(3) . . ?
N1 C17 C14 128.0(3) . . ?
C13 C14 C17 121.6(3) . . ?
C13 C14 C15 119.2(3) . . ?
C15 C14 C17 119.1(3) . . ?
O1 C11 C12 116.7(3) . . ?
O1 C11 C16 123.2(3) . . ?
C12 C11 C16 120.1(3) . . ?
N2 C20 C21 126.5(3) . . ?
N3 C20 N2 112.2(3) . . ?
N3 C20 C21 121.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12 119.9 . . ?
O1 C10 H10A 110.1 . . ?
O1 C10 H10B 110.1 . . ?
O1 C10 C9 108.0(3) . . ?
H10A C10 H10B 108.4 . . ?
C9 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.1(3) . . ?
C12 C13 H13 120.0 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C3 C2 C1 112.9(3) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 H16 120.0 . . ?
C15 C16 C11 120.1(3) . . ?
C15 C16 H16 120.0 . . ?
H6A C6 H6B 107.8 . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C7 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C7 C6 C5 113.2(3) . . ?
F3 C22 C21 108.5(3) . . ?
F3 C22 C23 112.9(4) . . ?
F3 C22 C23B 100.9(5) . . ?
F4 C22 F3 107.8(4) . . ?
F4 C22 C21 108.4(3) . . ?
F4 C22 C23 103.6(4) . . ?
F4 C22 C23B 117.5(5) . . ?
C21 C22 C23B 113.0(5) . . ?
C23 C22 C21 115.1(4) . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C4 C5 C6 113.7(3) . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H8A C8 H8B 107.9 . . ?
C7 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C9 C8 C7 112.4(3) . . ?
C6 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 C6 114.1(3) . . ?
C8 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C10 C9 C8 112.3(3) . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
F1 C21 F2 108.9(3) . . ?
F1 C21 C20 109.5(3) . . ?
F1 C21 C22 107.3(3) . . ?
F2 C21 C20 108.9(3) . . ?
F2 C21 C22 106.1(3) . . ?
C20 C21 C22 115.9(3) . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C3 C4 C5 113.5(3) . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C2 C3 C4 113.3(3) . . ?
C2 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C22 C23 C24 115.5(7) . . ?
F6 C23 C22 106.3(5) . . ?
F6 C23 C24 108.3(7) . . ?
F5 C23 C22 110.2(6) . . ?
F5 C23 F6 109.2(7) . . ?
F5 C23 C24 107.3(7) . . ?
O2 C30 C32 120.7(5) . . ?
O2 C30 C31 122.4(5) . . ?
C32 C30 C31 116.9(4) . . ?
C25B C24B C23B 115.2(10) . . ?
F6B C24B C25B 108.8(9) . . ?
F6B C24B C23B 107.0(9) . . ?
F5B C24B C25B 108(3) . . ?
F5B C24B F6B 108.3(18) . . ?
F5B C24B C23B 110(3) . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
F003 B1 F001 109.3(3) . . ?
F008 B1 F001 110.3(4) . . ?
F008 B1 F003 109.4(3) . . ?
F008 B1 F009 109.5(3) . . ?
F009 B1 F001 109.4(3) . . ?
F009 B1 F003 108.9(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C26 C27 114.5(7) . . ?
F12 C26 C25 108.7(6) . . ?
F12 C26 C27 109.2(6) . . ?
F12 C26 F11 108.6(7) . . ?
F11 C26 C25 107.6(6) . . ?
F11 C26 C27 108.1(6) . . ?
F9 C25 C26 108.9(6) . . ?
F9 C25 F10 105.1(6) . . ?
F9 C25 C24 110.6(7) . . ?
F10 C25 C26 107.6(6) . . ?
F10 C25 C24 108.7(6) . . ?
C24 C25 C26 115.4(7) . . ?
C26 C27 C28 115.2(7) . . ?
F14 C27 C26 108.5(5) . . ?
F14 C27 C28 107.1(6) . . ?
F14 C27 F13 110.8(7) . . ?
F13 C27 C26 108.3(6) . . ?
F13 C27 C28 106.8(6) . . ?
F16 C28 C27 109.0(7) . . ?
F16 C28 F15 106.8(8) . . ?
F16 C28 C29 108.8(7) . . ?
F15 C28 C27 107.5(6) . . ?
F15 C28 C29 108.2(7) . . ?
C29 C28 C27 116.1(8) . . ?
F14B C28B C27B 109.2(10) . . ?
F14B C28B C29B 103.5(9) . . ?
F13B C28B F14B 111.3(13) . . ?
F13B C28B C27B 111.0(10) . . ?
F13B C28B C29B 104.6(10) . . ?
C27B C28B C29B 116.9(11) . . ?
C28B C27B C26B 116.1(11) . . ?
F11B C27B C28B 107.5(9) . . ?
F11B C27B C26B 108.4(8) . . ?
F12B C27B C28B 110.1(9) . . ?
F12B C27B F11B 105.8(10) . . ?
F12B C27B C26B 108.4(9) . . ?
F9B C26B C27B 107.9(9) . . ?
F9B C26B F10B 108.8(12) . . ?
F9B C26B C25B 109.8(9) . . ?
F10B C26B C27B 106.3(9) . . ?
F10B C26B C25B 107.3(10) . . ?
C25B C26B C27B 116.4(10) . . ?
C26B C25B C24B 115.1(10) . . ?
F8B C25B C24B 107.8(9) . . ?
F8B C25B C26B 108.2(9) . . ?
F7B C25B C24B 108.2(10) . . ?
F7B C25B C26B 110.1(10) . . ?
F7B C25B F8B 107.1(11) . . ?
C25 C24 C23 114.2(8) . . ?
F7 C24 C23 107(2) . . ?
F7 C24 C25 109(2) . . ?
F8 C24 C23 108.7(8) . . ?
F8 C24 C25 108.0(8) . . ?
F8 C24 F7 109.3(13) . . ?
C24B C23B C22 115.1(9) . . ?
F4BA C23B C22 105.2(8) . . ?
F4BA C23B C24B 107.5(9) . . ?
F3BA C23B C22 111.3(9) . . ?
F3BA C23B C24B 109.1(10) . . ?
F3BA C23B F4BA 108.3(10) . . ?
F17 C29 C28 110.4(7) . . ?
F17 C29 F19 109.5(8) . . ?
F17 C29 F18 106.7(9) . . ?
F19 C29 C28 110.4(7) . . ?
F19 C29 F18 110.0(8) . . ?
F18 C29 C28 109.7(9) . . ?
F16B C29B C28B 112.9(9) . . ?
F16B C29B F15B 104.3(12) . . ?
F16B C29B F17B 107.8(11) . . ?
F15B C29B C28B 111.6(9) . . ?
F17B C29B C28B 112.9(13) . . ?
F17B C29B F15B 106.8(12) . . ?

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
O1 C11 C12 C13 -175.3(3) . . . . ?
O1 C11 C16 C15 176.3(3) . . . . ?
O1 C10 C9 C8 -175.4(3) . . . . ?
F3 C22 C21 F1 62.1(4) . . . . ?
F3 C22 C21 F2 178.4(3) . . . . ?
F3 C22 C21 C20 -60.6(4) . . . . ?
F3 C22 C23 F6 152.8(5) . . . . ?
F3 C22 C23 F5 -89.1(7) . . . . ?
F3 C22 C23 C24 32.7(8) . . . . ?
F3 C22 C23B C24B 80.6(8) . . . . ?
F3 C22 C23B F4BA -37.5(8) . . . . ?
F3 C22 C23B F3BA -154.5(9) . . . . ?
N2 C17 C14 C13 -129.7(4) . . . . ?
N2 C17 C14 C15 46.4(5) . . . . ?
N2 C20 C21 F1 -31.1(5) . . . . ?
N2 C20 C21 F2 -150.0(3) . . . . ?
N2 C20 C21 C22 90.5(5) . . . . ?
N1 N3 C20 N2 0.5(4) . . . . ?
N1 N3 C20 C21 -175.4(3) . . . . ?
N1 C17 C14 C13 51.3(5) . . . . ?
N1 C17 C14 C15 -132.6(4) . . . . ?
F4 C22 C21 F1 178.9(3) . . . . ?
F4 C22 C21 F2 -64.8(4) . . . . ?
F4 C22 C21 C20 56.2(5) . . . . ?
F4 C22 C23 F6 36.4(7) . . . . ?
F4 C22 C23 F5 154.6(6) . . . . ?
F4 C22 C23 C24 -83.7(6) . . . . ?
F4 C22 C23B C24B -36.2(10) . . . . ?
F4 C22 C23B F4BA -154.3(6) . . . . ?
F4 C22 C23B F3BA 88.6(10) . . . . ?
N3 N1 C17 N2 0.0(4) . . . . ?
N3 N1 C17 C14 179.2(3) . . . . ?
N3 C20 C21 F1 144.2(3) . . . . ?
N3 C20 C21 F2 25.3(5) . . . . ?
N3 C20 C21 C22 -94.3(4) . . . . ?
C17 N2 C20 N3 -0.5(4) . . . . ?
C17 N2 C20 C21 175.1(3) . . . . ?
C17 N1 N3 C20 -0.4(4) . . . . ?
C17 C14 C13 C12 174.4(3) . . . . ?
C17 C14 C15 C16 -173.5(3) . . . . ?
C14 C15 C16 C11 0.3(5) . . . . ?
C11 O1 C10 C9 -171.8(3) . . . . ?
C11 C12 C13 C14 -2.2(5) . . . . ?
C20 N2 C17 N1 0.3(4) . . . . ?
C20 N2 C17 C14 -178.9(3) . . . . ?
C12 C11 C16 C15 -4.3(5) . . . . ?
C10 O1 C11 C12 170.2(3) . . . . ?
C10 O1 C11 C16 -10.4(5) . . . . ?
C13 C14 C15 C16 2.7(5) . . . . ?
C15 C14 C13 C12 -1.7(5) . . . . ?
C16 C11 C12 C13 5.2(5) . . . . ?
C6 C5 C4 C3 -177.9(3) . . . . ?
C22 C23 C24 C25 161.9(6) . . . . ?
C22 C23 C24 F7 40.7(17) . . . . ?
C22 C23 C24 F8 -77.3(9) . . . . ?
C5 C6 C7 C8 178.4(3) . . . . ?
C5 C4 C3 C2 -178.6(3) . . . . ?
C7 C6 C5 C4 -177.3(3) . . . . ?
C7 C8 C9 C10 179.5(3) . . . . ?
C9 C8 C7 C6 -175.5(3) . . . . ?
C21 C22 C23 F6 -81.9(6) . . . . ?
C21 C22 C23 F5 36.3(8) . . . . ?
C21 C22 C23 C24 158.0(6) . . . . ?
C21 C22 C23B C24B -163.7(7) . . . . ?
C21 C22 C23B F4BA 78.2(8) . . . . ?
C21 C22 C23B F3BA -38.9(11) . . . . ?
C18 N1 N3 C20 -180.0(3) . . . . ?
C18 N1 C17 N2 179.6(3) . . . . ?
C18 N1 C17 C14 -1.2(6) . . . . ?
C19 N2 C17 N1 -174.5(3) . . . . ?
C19 N2 C17 C14 6.3(6) . . . . ?
C19 N2 C20 N3 174.1(3) . . . . ?
C19 N2 C20 C21 -10.3(6) . . . . ?
C1 C2 C3 C4 -177.2(3) . . . . ?
C23 C22 C21 F1 -65.5(5) . . . . ?
C23 C22 C21 F2 50.8(5) . . . . ?
C23 C22 C21 C20 171.8(4) . . . . ?
C26 C25 C24 C23 163.3(7) . . . . ?
C26 C25 C24 F7 -76.6(16) . . . . ?
C26 C25 C24 F8 42.2(10) . . . . ?
C26 C27 C28 F16 38.5(9) . . . . ?
C26 C27 C28 F15 -76.9(8) . . . . ?
C26 C27 C28 C29 161.8(7) . . . . ?
C25 C26 C27 C28 166.1(6) . . . . ?
C25 C26 C27 F14 46.0(9) . . . . ?
C25 C26 C27 F13 -74.4(7) . . . . ?
C27 C26 C25 F9 -74.6(8) . . . . ?
C27 C26 C25 F10 38.8(8) . . . . ?
C27 C26 C25 C24 160.4(7) . . . . ?
C27 C28 C29 F17 -70.5(9) . . . . ?
C27 C28 C29 F19 50.8(10) . . . . ?
C27 C28 C29 F18 172.2(8) . . . . ?
F14 C27 C28 F16 159.4(7) . . . . ?
F14 C27 C28 F15 43.9(10) . . . . ?
F14 C27 C28 C29 -77.3(9) . . . . ?
F13 C27 C28 F16 -81.9(9) . . . . ?
F13 C27 C28 F15 162.7(7) . . . . ?
F13 C27 C28 C29 41.5(9) . . . . ?
F6 C23 C24 C25 42.9(10) . . . . ?
F6 C23 C24 F7 -78.2(17) . . . . ?
F6 C23 C24 F8 163.7(7) . . . . ?
F9 C25 C24 C23 39.1(10) . . . . ?
F9 C25 C24 F7 159.3(15) . . . . ?
F9 C25 C24 F8 -82.0(9) . . . . ?
F10 C25 C24 C23 -75.7(9) . . . . ?
F10 C25 C24 F7 44.4(16) . . . . ?
F10 C25 C24 F8 163.2(6) . . . . ?
F12 C26 C25 F9 163.0(7) . . . . ?
F12 C26 C25 F10 -83.6(8) . . . . ?
F12 C26 C25 C24 38.0(10) . . . . ?
F12 C26 C27 C28 -71.8(8) . . . . ?
F12 C26 C27 F14 168.1(6) . . . . ?
F12 C26 C27 F13 47.7(8) . . . . ?
F11 C26 C25 F9 45.6(9) . . . . ?
F11 C26 C25 F10 159.0(6) . . . . ?
F11 C26 C25 C24 -79.4(8) . . . . ?
F11 C26 C27 C28 46.2(8) . . . . ?
F11 C26 C27 F14 -73.9(8) . . . . ?
F11 C26 C27 F13 165.7(6) . . . . ?
F5 C23 C24 C25 -74.8(9) . . . . ?
F5 C23 C24 F7 164.0(16) . . . . ?
F5 C23 C24 F8 45.9(10) . . . . ?
F16 C28 C29 F17 53.0(10) . . . . ?
F16 C28 C29 F19 174.2(7) . . . . ?
F16 C28 C29 F18 -64.4(10) . . . . ?
F15 C28 C29 F17 168.7(7) . . . . ?
F15 C28 C29 F19 -70.1(10) . . . . ?
F15 C28 C29 F18 51.4(11) . . . . ?
F14B C28B C27B F11B -167.6(10) . . . . ?
F14B C28B C27B F12B -52.8(14) . . . . ?
F14B C28B C27B C26B 70.8(12) . . . . ?
F14B C28B C29B F16B -176.6(11) . . . . ?
F14B C28B C29B F15B 66.3(14) . . . . ?
F14B C28B C29B F17B -54.0(15) . . . . ?
F13B C28B C27B F11B 69.3(15) . . . . ?
F13B C28B C27B F12B -175.9(11) . . . . ?
F13B C28B C27B C26B -52.3(15) . . . . ?
F13B C28B C29B F16B -59.9(15) . . . . ?
F13B C28B C29B F15B -177.0(11) . . . . ?
F13B C28B C29B F17B 62.7(15) . . . . ?
C28B C27B C26B F9B 67.5(13) . . . . ?
C28B C27B C26B F10B -49.1(13) . . . . ?
C28B C27B C26B C25B -168.6(10) . . . . ?
F11B C27B C26B F9B -53.6(13) . . . . ?
F11B C27B C26B F10B -170.2(10) . . . . ?
F11B C27B C26B C25B 70.3(12) . . . . ?
F12B C27B C26B F9B -168.1(10) . . . . ?
F12B C27B C26B F10B 75.3(13) . . . . ?
F12B C27B C26B C25B -44.2(13) . . . . ?
C27B C28B C29B F16B 63.4(14) . . . . ?
C27B C28B C29B F15B -53.7(14) . . . . ?
C27B C28B C29B F17B -174.0(12) . . . . ?
C27B C26B C25B C24B -166.2(9) . . . . ?
C27B C26B C25B F8B -45.6(13) . . . . ?
C27B C26B C25B F7B 71.1(13) . . . . ?
F9B C26B C25B C24B -43.3(14) . . . . ?
F9B C26B C25B F8B 77.4(13) . . . . ?
F9B C26B C25B F7B -165.9(11) . . . . ?
F10B C26B C25B C24B 74.8(12) . . . . ?
F10B C26B C25B F8B -164.5(10) . . . . ?
F10B C26B C25B F7B -47.8(14) . . . . ?
C25B C24B C23B C22 -161.6(8) . . . . ?
C25B C24B C23B F4BA -44.7(12) . . . . ?
C25B C24B C23B F3BA 72.4(12) . . . . ?
F6B C24B C25B C26B -43.8(14) . . . . ?
F6B C24B C25B F8B -164.6(9) . . . . ?
F6B C24B C25B F7B 79.9(13) . . . . ?
F6B C24B C23B C22 77.4(11) . . . . ?
F6B C24B C23B F4BA -165.8(9) . . . . ?
F6B C24B C23B F3BA -48.6(13) . . . . ?
F5B C24B C25B C26B 73(3) . . . . ?
F5B C24B C25B F8B -47(3) . . . . ?
F5B C24B C25B F7B -163(3) . . . . ?
F5B C24B C23B C22 -40(2) . . . . ?
F5B C24B C23B F4BA 77(2) . . . . ?
F5B C24B C23B F3BA -166(2) . . . . ?
C23B C22 C21 F1 -48.9(6) . . . . ?
C23B C22 C21 F2 67.4(5) . . . . ?
C23B C22 C21 C20 -171.6(5) . . . . ?
C23B C24B C25B C26B -163.8(9) . . . . ?
C23B C24B C25B F8B 75.4(12) . . . . ?
C23B C24B C25B F7B -40.2(13) . . . . ?
C29B C28B C27B F11B -50.6(13) . . . . ?
C29B C28B C27B F12B 64.2(13) . . . . ?
C29B C28B C27B C26B -172.2(9) . . . . ?

_olex2_date_sample_data_collection 2016-11-09
_olex2_date_sample_submission    2016-11-07
_olex2_exptl_crystal_mounting_method 'oil on micromount 200 micrometres'
_olex2_submission_original_sample_id ALR17
_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 1.838
_oxdiff_exptl_absorpt_empirical_full_min 0.691
####################################################################### 
# 
# 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_dwb1670
_database_code_depnum_ccdc_archive 'CCDC 2177832'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H31 F7 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C25 H31 F13 N4 O5 S2'
_chemical_formula_weight         778.66
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25 H31 F13 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio NV 2566'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.8452(4)
_cell_length_b                   8.4550(4)
_cell_length_c                   56.345(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3261.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11708
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.6740
_cell_measurement_theta_min      5.2760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0159
0 0 1 0.0219
-4 1 2 0.0993
1 0 -1 0.1070
0 -1 1 0.0812
0 1 -1 0.0823
-1 -5 3 0.0823

_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.038
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
0.0000 -0.0001 -0.9999 -0.0013 -0.0272 -0.0026
-0.0000 0.0001 0.9999 0.0013 0.0272 0.0026
-3.9956 1.0000 2.0058 -0.5692 0.0145 0.7214
0.9989 0.0000 -1.0003 0.1012 -0.0132 -0.2022
0.0002 -1.0001 0.9956 0.1632 0.0113 0.0848
-0.0002 1.0001 -0.9956 -0.1632 -0.0113 -0.0848
-0.9980 -5.0008 2.9788 0.7111 -0.0118 0.6183

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            29641
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         4.709
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  21.00   1.00    1.00    --    0.00 -57.00  90.00   90
  2  ω    -69.00  21.00   1.00    1.00    --    0.00 -57.00 150.00   90
  3  ω     33.00 123.00   1.00    2.00    --   54.00  57.00  90.00   90
  4  ω     33.00 123.00   1.00    2.00    --   54.00  57.00 -30.00   90
  5  ω    -16.00  84.00   1.00    2.00    --   54.00 -77.00-150.00  100
  6  ω     33.00 123.00   1.00    2.00    --   54.00  57.00   0.00   90
  7  ω     86.00 178.00   1.00    4.00    --  108.00  50.00  90.00   92
  8  ω     38.00 130.00   1.00    4.00    --  108.00 -50.00-180.00   92
  9  ω     38.00 130.00   1.00    4.00    --  108.00 -50.00 -60.00   92
 10  ω     35.00 142.00   1.00    4.00    --  108.00 -25.00  90.00  107
 11  ω     36.00 116.00   1.00    4.00    --  108.00-111.00-120.00   80
 12  ω    100.00 178.00   1.00    4.00    --  108.00 111.00  30.00   78
 13  ω     40.00 130.00   1.00    4.00    --  108.00 -63.00 -60.00   90
 14  ω    -55.00   1.00   1.00    1.00    --    0.00 122.00 -52.00   56
 15  ω    -69.00  21.00   1.00    1.00    --    0.00 -57.00  30.00   90
 16  ω     10.00 127.00   1.00    2.00    --   54.00  19.00-120.00  117
 17  ω    -15.00  75.00   1.00    2.00    --   54.00 -57.00 -60.00   90
 18  ω    -15.00  75.00   1.00    2.00    --   54.00 -57.00  60.00   90
 19  ω     33.00 123.00   1.00    2.00    --   54.00  57.00 -90.00   90
 20  ω     82.00 178.00   1.00    4.00    --  108.00  37.00 -90.00   96
 21  ω     40.00 130.00   1.00    4.00    --  108.00 -63.00  60.00   90
 22  ω     86.00 178.00   1.00    4.00    --  108.00  50.00-150.00   92
 23  ω     74.00 178.00   1.00    4.00    --  108.00  25.00   0.00  104
 24  ω     36.00 116.00   1.00    4.00    --  108.00-111.00 120.00   80
 25  ω     74.00 178.00   1.00    4.00    --  108.00  25.00-180.00  104
 26  ω    -30.00  70.00   1.00    1.00    --    0.00  77.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1026224000
_diffrn_orient_matrix_UB_12      -0.1618751000
_diffrn_orient_matrix_UB_13      0.0013431000
_diffrn_orient_matrix_UB_21      0.0139626000
_diffrn_orient_matrix_UB_22      0.0157606000
_diffrn_orient_matrix_UB_23      0.0271765000
_diffrn_orient_matrix_UB_31      -0.1998329000
_diffrn_orient_matrix_UB_32      -0.0822180000
_diffrn_orient_matrix_UB_33      0.0025742000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5708
_reflns_number_total             5800
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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         0.306
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(4)
_refine_ls_extinction_coef       0.00016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5800
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      1.186
_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)+9.4610P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1171
_refine_special_details          
;
The crystal was a racemic twin with refined BASF of 0.44(4).
The structure exhibited disorder with the perfluoropropyl
group modelled in two position althought the site of the terminal
carbon was common to both conformers.  The refined occupancies of
the two forms were 0.672:0.328(6).  Withing the disordered chain:
The ADP of closely proximate atoms were constrained to be equal 
(C12 & C12A, C13 & C13A, C14 & C14A, F1 & F1A, F2 & F3A, F2A & F3
F4 & F4A, F5 & F5A, F6 & F6A, F7 & F7A).  
Equivalent pairs of C-C distances were restrained to be equal 
(C9-C12 & C9-C12A, C12-C13 & C12A-C13A, C13-C14 & C13A-C14A)
Several C-F bond lengths were restrained to be 1.35 angstroms
(C-12-F1, F12A-F1A, C12A-F2A, C14-F5, C14-F6, C14-F7, 
C14A-F5A, C14A-F6A, C14A-F7A)
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.56(4)
 0.44(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 F1A-C12A = F1-C12 = F2A-C12A
 1.35 with sigma of 0.02
 F7A-C14A = F7-C14 = F6-C14 = F6A-C14A = F5A-C14A = F5-C14
 1.35 with sigma of 0.01
 C9-C12A \\sim C9-C12
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C13A)
Uanis(C12A) = Uanis(C12)
Uanis(C14) = Uanis(C14A)
Uanis(F2A) = Uanis(F3)
Uanis(F4A) = Uanis(F4)
Uanis(F6) = Uanis(F6A)
Uanis(F5) = Uanis(F5A)
Uanis(F7) = Uanis(F7A)
Uanis(F1A) = Uanis(F1)
Uanis(F3A) = Uanis(F2)
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(C12A)=
 Sof(C13A)=Sof(C14A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(C12)=Sof(C13)=
 Sof(C14)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C)
;
_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
F1 F 1.139(4) 0.672(4) 0.4740(6) 0.033(4) Uani 0.672(6) 1 d D . P A 1
F1A F 1.164(10) 0.676(8) 0.4770(13) 0.033(4) Uani 0.328(6) 1 d D . P A 2
F2 F 1.0622(15) 0.4179(14) 0.47925(12) 0.0333(18) Uani 0.672(6) 1 d . . P A 1
F2A F 1.472(3) 0.626(3) 0.4684(3) 0.0314(17) Uani 0.328(6) 1 d D . P A 2
F3 F 1.5186(12) 0.6014(11) 0.47600(13) 0.0314(17) Uani 0.672(6) 1 d . . P A 1
F3A F 1.082(4) 0.394(3) 0.4869(3) 0.0333(18) Uani 0.328(6) 1 d . . P A 2
F4 F 1.4594(11) 0.3456(8) 0.47636(11) 0.0304(15) Uani 0.672(6) 1 d . . P A 1
F4A F 1.363(2) 0.3034(18) 0.4758(2) 0.0304(15) Uani 0.328(6) 1 d . . P A 2
F5 F 1.3169(19) 0.619(2) 0.5180(4) 0.034(3) Uani 0.672(6) 1 d D . P A 1
F5A F 1.269(5) 0.602(5) 0.5193(9) 0.034(3) Uani 0.328(6) 1 d D . P A 2
F6 F 1.279(3) 0.363(2) 0.5183(2) 0.038(2) Uani 0.672(6) 1 d D . P A 1
F6A F 1.307(7) 0.354(6) 0.5241(6) 0.038(2) Uani 0.328(6) 1 d D . P A 2
F7 F 1.5664(11) 0.4764(11) 0.51839(11) 0.0394(16) Uani 0.672(6) 1 d D . P A 1
F7A F 1.547(3) 0.465(3) 0.5090(2) 0.0394(16) Uani 0.328(6) 1 d D . P A 2
O1 O 0.6393(6) 0.4252(5) 0.32676(7) 0.0275(10) Uani 1 1 d . . . . .
N1 N 1.3012(7) 0.4524(5) 0.40826(8) 0.0180(10) Uani 1 1 d . . . . .
N2 N 1.0545(7) 0.5150(6) 0.42960(8) 0.0231(11) Uani 1 1 d . . . . .
N8 N 1.3717(8) 0.4678(6) 0.43086(9) 0.0255(12) Uani 1 1 d . . . . .
C1 C 0.7560(8) 0.4512(6) 0.34608(9) 0.0187(12) Uani 1 1 d . . . . .
C2 C 0.8390(9) 0.3153(7) 0.35555(11) 0.0250(14) Uani 1 1 d . . . . .
H2 H 0.815733 0.215721 0.348268 0.030 Uiso 1 1 calc R U . . .
C3 C 0.9556(9) 0.3246(7) 0.37560(11) 0.0246(14) Uani 1 1 d . . . . .
H3 H 1.013155 0.231973 0.382103 0.030 Uiso 1 1 calc R U . . .
C4 C 0.9872(8) 0.4712(7) 0.38605(9) 0.0172(12) Uani 1 1 d . . . . .
C5 C 0.9062(8) 0.6091(7) 0.37636(10) 0.0194(12) Uani 1 1 d . . . . .
H5 H 0.930478 0.709006 0.383485 0.023 Uiso 1 1 calc R U . . .
C6 C 0.7897(8) 0.5978(7) 0.35613(10) 0.0192(12) Uani 1 1 d . . . . .
H6 H 0.733871 0.690087 0.349322 0.023 Uiso 1 1 calc R U . . .
C7 C 1.1118(8) 0.4799(7) 0.40726(9) 0.0177(11) Uani 1 1 d . . . . .
C9 C 1.2194(10) 0.5066(8) 0.44313(10) 0.0317(15) Uani 1 1 d D . . . .
C10 C 1.4346(8) 0.4080(8) 0.38923(10) 0.0233(13) Uani 1 1 d . . . . .
H10A H 1.531685 0.491866 0.386994 0.035 Uiso 1 1 calc R U . . .
H10B H 1.360835 0.393093 0.374496 0.035 Uiso 1 1 calc R U . . .
H10C H 1.501044 0.309168 0.393416 0.035 Uiso 1 1 calc R U . . .
C11 C 0.8538(10) 0.5538(8) 0.43707(11) 0.0333(16) Uani 1 1 d . . . . .
H11A H 0.849309 0.663152 0.442795 0.050 Uiso 1 1 calc R U . . .
H11B H 0.813719 0.482064 0.449837 0.050 Uiso 1 1 calc R U . . .
H11C H 0.765018 0.541850 0.423546 0.050 Uiso 1 1 calc R U . . .
C12 C 1.1967(13) 0.5194(10) 0.47034(15) 0.0219(19) Uani 0.672(6) 1 d D . P A 1
C12A C 1.290(3) 0.571(2) 0.4672(3) 0.0219(19) Uani 0.328(6) 1 d D . P A 2
C13 C 1.3916(12) 0.4894(10) 0.48279(14) 0.0193(16) Uani 0.672(6) 1 d D . P A 1
C13A C 1.272(3) 0.433(2) 0.4844(3) 0.0193(16) Uani 0.328(6) 1 d D . P A 2
C14 C 1.3867(16) 0.482(3) 0.5101(2) 0.031(2) Uani 0.672(6) 1 d D . P A 1
C14A C 1.352(3) 0.474(5) 0.5096(4) 0.031(2) Uani 0.328(6) 1 d D . P A 2
C15 C 0.4918(9) 0.5410(7) 0.32108(10) 0.0233(14) Uani 1 1 d . . . . .
H15A H 0.551484 0.635871 0.313761 0.028 Uiso 1 1 calc R U . . .
H15B H 0.420105 0.573623 0.335540 0.028 Uiso 1 1 calc R U . . .
C16 C 0.3563(9) 0.4597(7) 0.30378(10) 0.0241(13) Uani 1 1 d . . . . .
H16A H 0.305329 0.362271 0.311310 0.029 Uiso 1 1 calc R U . . .
H16B H 0.432729 0.427528 0.289672 0.029 Uiso 1 1 calc R U . . .
C17 C 0.1839(9) 0.5596(7) 0.29559(10) 0.0215(13) Uani 1 1 d . . . . .
H17A H 0.102477 0.587637 0.309481 0.026 Uiso 1 1 calc R U . . .
H17B H 0.233169 0.658958 0.288486 0.026 Uiso 1 1 calc R U . . .
C18 C 0.0592(9) 0.4731(7) 0.27752(10) 0.0234(13) Uani 1 1 d . . . . .
H18A H 0.010922 0.373936 0.284783 0.028 Uiso 1 1 calc R U . . .
H18B H 0.142567 0.443769 0.263851 0.028 Uiso 1 1 calc R U . . .
C19 C -0.1149(9) 0.5667(7) 0.26839(10) 0.0211(12) Uani 1 1 d . . . . .
H19A H -0.067795 0.668875 0.261984 0.025 Uiso 1 1 calc R U . . .
H19B H -0.203022 0.590140 0.281869 0.025 Uiso 1 1 calc R U . . .
C20 C -0.2306(9) 0.4818(7) 0.24920(10) 0.0237(12) Uani 1 1 d . . . . .
H20A H -0.143103 0.460936 0.235570 0.028 Uiso 1 1 calc R U . . .
H20B H -0.274342 0.378359 0.255483 0.028 Uiso 1 1 calc R U . . .
C21 C -0.4081(9) 0.5724(7) 0.24039(10) 0.0217(12) Uani 1 1 d . . . . .
H21A H -0.495369 0.593658 0.254038 0.026 Uiso 1 1 calc R U . . .
H21B H -0.364327 0.675701 0.234061 0.026 Uiso 1 1 calc R U . . .
C22 C -0.5238(8) 0.4881(7) 0.22140(10) 0.0210(12) Uani 1 1 d . . . . .
H22A H -0.564251 0.383427 0.227547 0.025 Uiso 1 1 calc R U . . .
H22B H -0.437781 0.469839 0.207544 0.025 Uiso 1 1 calc R U . . .
C23 C -0.7046(9) 0.5769(7) 0.21316(10) 0.0239(13) Uani 1 1 d . . . . .
H23A H -0.663996 0.680225 0.206538 0.029 Uiso 1 1 calc R U . . .
H23B H -0.789022 0.597940 0.227075 0.029 Uiso 1 1 calc R U . . .
C24 C -0.8232(9) 0.4887(8) 0.19455(11) 0.0307(15) Uani 1 1 d . . . . .
H24A H -0.742553 0.471144 0.180422 0.046 Uiso 1 1 calc R U . . .
H24B H -0.938159 0.551544 0.190241 0.046 Uiso 1 1 calc R U . . .
H24C H -0.865336 0.386570 0.200992 0.046 Uiso 1 1 calc R U . . .
S1 S 0.2302(2) 1.00058(18) 0.41980(2) 0.0240(3) Uani 1 1 d . . . . .
S2 S 0.3962(2) 0.91424(17) 0.37600(3) 0.0219(3) Uani 1 1 d . . . . .
F8 F 0.4034(7) 0.9642(6) 0.46077(6) 0.0512(12) Uani 1 1 d . . . . .
F9 F 0.5573(6) 1.1161(5) 0.43643(7) 0.0443(11) Uani 1 1 d . . . . .
F10 F 0.5588(7) 0.8635(5) 0.43105(7) 0.0486(12) Uani 1 1 d . . . . .
F11 F 0.2702(7) 0.8656(5) 0.33314(6) 0.0447(11) Uani 1 1 d . . . . .
F12 F 0.0499(5) 0.9518(4) 0.35707(6) 0.0310(9) Uani 1 1 d . . . . .
F13 F 0.2683(6) 1.1115(4) 0.34361(6) 0.0345(9) Uani 1 1 d . . . . .
O2 O 0.1330(7) 1.1392(5) 0.42800(7) 0.0290(10) Uani 1 1 d . . . . .
O3 O 0.1349(8) 0.8514(5) 0.42231(8) 0.0349(11) Uani 1 1 d . . . . .
O4 O 0.5866(7) 0.9565(5) 0.36787(9) 0.0348(11) Uani 1 1 d . . . . .
O5 O 0.3560(7) 0.7523(5) 0.38098(7) 0.0259(10) Uani 1 1 d . . . . .
N3 N 0.3214(8) 1.0383(5) 0.39467(8) 0.0224(11) Uani 1 1 d . . . . .
C25 C 0.4521(10) 0.9855(9) 0.43812(11) 0.0351(16) Uani 1 1 d . . . . .
C26 C 0.2360(10) 0.9653(7) 0.35110(10) 0.0261(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C12 1.36(2) . ?
F1A C12A 1.36(3) . ?
F2 C12 1.355(13) . ?
F2A C12A 1.34(2) . ?
F3 C13 1.341(12) . ?
F3A C13A 1.35(3) . ?
F4 C13 1.351(11) . ?
F4A C13A 1.35(2) . ?
F5 C14 1.327(10) . ?
F5A C14A 1.341(13) . ?
F6 C14 1.330(10) . ?
F6A C14A 1.343(13) . ?
F7 C14 1.317(9) . ?
F7A C14A 1.340(14) . ?
O1 C1 1.367(6) . ?
O1 C15 1.443(7) . ?
N1 N8 1.368(6) . ?
N1 C7 1.318(7) . ?
N1 C10 1.458(7) . ?
N2 C7 1.351(7) . ?
N2 C9 1.364(8) . ?
N2 C11 1.474(8) . ?
N8 C9 1.293(8) . ?
C1 C2 1.389(8) . ?
C1 C6 1.382(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(8) . ?
C4 C5 1.402(8) . ?
C4 C7 1.470(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.395(8) . ?
C6 H6 0.9500 . ?
C9 C12 1.545(10) . ?
C9 C12A 1.537(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.529(12) . ?
C12A C13A 1.52(2) . ?
C13 C14 1.540(13) . ?
C13A C14A 1.56(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.511(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.522(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.516(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.520(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.521(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.520(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.510(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.520(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.522(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
S1 O2 1.425(4) . ?
S1 O3 1.427(5) . ?
S1 N3 1.580(5) . ?
S1 C25 1.841(7) . ?
S2 O4 1.427(5) . ?
S2 O5 1.424(4) . ?
S2 N3 1.571(5) . ?
S2 C26 1.832(6) . ?
F8 C25 1.331(7) . ?
F9 C25 1.321(9) . ?
F10 C25 1.325(8) . ?
F11 C26 1.337(7) . ?
F12 C26 1.323(8) . ?
F13 C26 1.325(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C15 118.4(4) . . ?
N8 N1 C10 119.2(5) . . ?
C7 N1 N8 111.7(5) . . ?
C7 N1 C10 129.1(5) . . ?
C7 N2 C9 105.6(5) . . ?
C7 N2 C11 125.8(5) . . ?
C9 N2 C11 128.6(5) . . ?
C9 N8 N1 103.7(5) . . ?
O1 C1 C2 114.3(5) . . ?
O1 C1 C6 124.6(5) . . ?
C6 C1 C2 121.1(5) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.2(6) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.1(6) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 121.0(5) . . ?
C3 C4 C7 118.7(5) . . ?
C5 C4 C7 120.3(5) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.2(5) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C5 119.5(5) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N1 C7 N2 106.5(5) . . ?
N1 C7 C4 126.6(5) . . ?
N2 C7 C4 126.9(5) . . ?
N2 C9 C12 117.9(6) . . ?
N2 C9 C12A 137.2(9) . . ?
N8 C9 N2 112.4(5) . . ?
N8 C9 C12 129.0(6) . . ?
N8 C9 C12A 108.0(9) . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
F1 C12 C9 104.3(16) . . ?
F1 C12 C13 109.9(14) . . ?
F2 C12 F1 110.2(19) . . ?
F2 C12 C9 113.1(7) . . ?
F2 C12 C13 108.5(7) . . ?
C13 C12 C9 110.9(7) . . ?
F1A C12A C9 113(3) . . ?
F1A C12A C13A 101(4) . . ?
F2A C12A F1A 110(4) . . ?
F2A C12A C9 117.3(15) . . ?
F2A C12A C13A 108.1(16) . . ?
C13A C12A C9 105.7(12) . . ?
F3 C13 F4 109.6(8) . . ?
F3 C13 C12 108.5(7) . . ?
F3 C13 C14 109.1(9) . . ?
F4 C13 C12 109.0(7) . . ?
F4 C13 C14 103.9(10) . . ?
C12 C13 C14 116.5(8) . . ?
F3A C13A F4A 106.3(19) . . ?
F3A C13A C12A 109.1(16) . . ?
F3A C13A C14A 107.3(17) . . ?
F4A C13A C12A 110.8(14) . . ?
F4A C13A C14A 110.5(19) . . ?
C12A C13A C14A 113(2) . . ?
F5 C14 F6 110.0(15) . . ?
F5 C14 C13 108.0(16) . . ?
F6 C14 C13 113.0(11) . . ?
F7 C14 F5 104.5(14) . . ?
F7 C14 F6 111.4(15) . . ?
F7 C14 C13 109.6(9) . . ?
F5A C14A F6A 105(4) . . ?
F5A C14A C13A 114(3) . . ?
F6A C14A C13A 108(2) . . ?
F7A C14A F5A 119(3) . . ?
F7A C14A F6A 101(3) . . ?
F7A C14A C13A 108.4(18) . . ?
O1 C15 H15A 110.7 . . ?
O1 C15 H15B 110.7 . . ?
O1 C15 C16 105.3(5) . . ?
H15A C15 H15B 108.8 . . ?
C16 C15 H15A 110.7 . . ?
C16 C15 H15B 110.7 . . ?
C15 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
C15 C16 C17 114.8(5) . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C16 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C18 C17 C16 111.9(5) . . ?
C18 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
C17 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
C17 C18 C19 114.7(5) . . ?
H18A C18 H18B 107.6 . . ?
C19 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C18 C19 C20 113.8(5) . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C19 C20 H20A 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
C21 C20 C19 114.3(5) . . ?
C21 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C20 C21 H21A 108.7 . . ?
C20 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 C20 114.4(5) . . ?
C22 C21 H21A 108.7 . . ?
C22 C21 H21B 108.7 . . ?
C21 C22 H22A 108.7 . . ?
C21 C22 H22B 108.7 . . ?
C21 C22 C23 114.2(5) . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C22 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
C22 C23 C24 113.8(5) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 S1 O3 118.8(3) . . ?
O2 S1 N3 108.0(3) . . ?
O2 S1 C25 105.1(3) . . ?
O3 S1 N3 116.6(3) . . ?
O3 S1 C25 105.1(3) . . ?
N3 S1 C25 101.0(3) . . ?
O4 S2 N3 110.2(3) . . ?
O4 S2 C26 104.0(3) . . ?
O5 S2 O4 118.7(3) . . ?
O5 S2 N3 116.5(3) . . ?
O5 S2 C26 105.2(3) . . ?
N3 S2 C26 99.2(3) . . ?
S2 N3 S1 126.4(3) . . ?
F8 C25 S1 109.9(5) . . ?
F9 C25 S1 110.6(5) . . ?
F9 C25 F8 108.6(6) . . ?
F9 C25 F10 109.2(6) . . ?
F10 C25 S1 109.9(5) . . ?
F10 C25 F8 108.7(6) . . ?
F11 C26 S2 109.0(4) . . ?
F12 C26 S2 111.2(4) . . ?
F12 C26 F11 107.9(5) . . ?
F12 C26 F13 108.8(5) . . ?
F13 C26 S2 111.3(4) . . ?
F13 C26 F11 108.5(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
F1 C12 C13 F3 -52(2) . . . . ?
F1 C12 C13 F4 -171.8(19) . . . . ?
F1 C12 C13 C14 71(2) . . . . ?
F1A C12A C13A F3A 53(4) . . . . ?
F1A C12A C13A F4A 170(3) . . . . ?
F1A C12A C13A C14A -66(4) . . . . ?
F2 C12 C13 F3 -172.9(8) . . . . ?
F2 C12 C13 F4 67.7(9) . . . . ?
F2 C12 C13 C14 -49.5(13) . . . . ?
F2A C12A C13A F3A 168.5(19) . . . . ?
F2A C12A C13A F4A -74.8(19) . . . . ?
F2A C12A C13A C14A 50(2) . . . . ?
F3 C13 C14 F5 64.5(11) . . . . ?
F3 C13 C14 F6 -173.6(13) . . . . ?
F3 C13 C14 F7 -48.7(17) . . . . ?
F3A C13A C14A F5A -64(3) . . . . ?
F3A C13A C14A F6A 52(3) . . . . ?
F3A C13A C14A F7A 161(3) . . . . ?
F4 C13 C14 F5 -178.6(9) . . . . ?
F4 C13 C14 F6 -56.7(15) . . . . ?
F4 C13 C14 F7 68.1(15) . . . . ?
F4A C13A C14A F5A -180(3) . . . . ?
F4A C13A C14A F6A -63(3) . . . . ?
F4A C13A C14A F7A 46(4) . . . . ?
O1 C1 C2 C3 -178.0(6) . . . . ?
O1 C1 C6 C5 177.7(5) . . . . ?
O1 C15 C16 C17 178.7(5) . . . . ?
N1 N8 C9 N2 0.7(7) . . . . ?
N1 N8 C9 C12 171.0(7) . . . . ?
N1 N8 C9 C12A -164.9(9) . . . . ?
N2 C9 C12 F1 -68.2(17) . . . . ?
N2 C9 C12 F2 51.6(10) . . . . ?
N2 C9 C12 C13 173.7(7) . . . . ?
N2 C9 C12A F1A -8(5) . . . . ?
N2 C9 C12A F2A -137.5(15) . . . . ?
N2 C9 C12A C13A 101.9(16) . . . . ?
N8 N1 C7 N2 0.2(7) . . . . ?
N8 N1 C7 C4 -178.8(5) . . . . ?
N8 C9 C12 F1 122.0(17) . . . . ?
N8 C9 C12 F2 -118.3(10) . . . . ?
N8 C9 C12 C13 3.9(12) . . . . ?
N8 C9 C12A F1A 152(5) . . . . ?
N8 C9 C12A F2A 22.6(19) . . . . ?
N8 C9 C12A C13A -98.0(13) . . . . ?
C1 O1 C15 C16 -165.0(5) . . . . ?
C1 C2 C3 C4 0.3(10) . . . . ?
C2 C1 C6 C5 -1.1(9) . . . . ?
C2 C3 C4 C5 -1.2(9) . . . . ?
C2 C3 C4 C7 -179.8(6) . . . . ?
C3 C4 C5 C6 1.1(9) . . . . ?
C3 C4 C7 N1 67.3(8) . . . . ?
C3 C4 C7 N2 -111.6(7) . . . . ?
C4 C5 C6 C1 0.1(8) . . . . ?
C5 C4 C7 N1 -111.3(7) . . . . ?
C5 C4 C7 N2 69.9(8) . . . . ?
C6 C1 C2 C3 0.9(10) . . . . ?
C7 N1 N8 C9 -0.6(7) . . . . ?
C7 N2 C9 N8 -0.6(8) . . . . ?
C7 N2 C9 C12 -172.1(6) . . . . ?
C7 N2 C9 C12A 159.0(13) . . . . ?
C7 C4 C5 C6 179.6(5) . . . . ?
C9 N2 C7 N1 0.2(7) . . . . ?
C9 N2 C7 C4 179.2(6) . . . . ?
C9 C12 C13 F3 62.3(9) . . . . ?
C9 C12 C13 F4 -57.1(9) . . . . ?
C9 C12 C13 C14 -174.2(11) . . . . ?
C9 C12A C13A F3A -65.0(19) . . . . ?
C9 C12A C13A F4A 51.7(18) . . . . ?
C9 C12A C13A C14A 175.9(15) . . . . ?
C10 N1 N8 C9 -179.8(5) . . . . ?
C10 N1 C7 N2 179.3(5) . . . . ?
C10 N1 C7 C4 0.3(10) . . . . ?
C11 N2 C7 N1 -179.8(6) . . . . ?
C11 N2 C7 C4 -0.8(10) . . . . ?
C11 N2 C9 N8 179.4(6) . . . . ?
C11 N2 C9 C12 7.9(10) . . . . ?
C11 N2 C9 C12A -21.0(17) . . . . ?
C12 C13 C14 F5 -58.7(13) . . . . ?
C12 C13 C14 F6 63.2(17) . . . . ?
C12 C13 C14 F7 -171.9(11) . . . . ?
C12A C13A C14A F5A 56(3) . . . . ?
C12A C13A C14A F6A 172(3) . . . . ?
C12A C13A C14A F7A -79(3) . . . . ?
C15 O1 C1 C2 156.9(5) . . . . ?
C15 O1 C1 C6 -22.0(9) . . . . ?
C15 C16 C17 C18 177.6(5) . . . . ?
C16 C17 C18 C19 -179.5(5) . . . . ?
C17 C18 C19 C20 176.5(5) . . . . ?
C18 C19 C20 C21 178.5(5) . . . . ?
C19 C20 C21 C22 -179.8(5) . . . . ?
C20 C21 C22 C23 178.3(5) . . . . ?
C21 C22 C23 C24 -178.3(5) . . . . ?
O2 S1 N3 S2 -163.8(4) . . . . ?
O2 S1 C25 F8 63.5(6) . . . . ?
O2 S1 C25 F9 -56.4(5) . . . . ?
O2 S1 C25 F10 -176.9(5) . . . . ?
O3 S1 N3 S2 -27.0(5) . . . . ?
O3 S1 C25 F8 -62.6(6) . . . . ?
O3 S1 C25 F9 177.5(4) . . . . ?
O3 S1 C25 F10 57.0(5) . . . . ?
O4 S2 N3 S1 -130.9(4) . . . . ?
O4 S2 C26 F11 69.3(5) . . . . ?
O4 S2 C26 F12 -171.9(4) . . . . ?
O4 S2 C26 F13 -50.4(5) . . . . ?
O5 S2 N3 S1 8.3(5) . . . . ?
O5 S2 C26 F11 -56.2(5) . . . . ?
O5 S2 C26 F12 62.6(5) . . . . ?
O5 S2 C26 F13 -175.9(4) . . . . ?
N3 S1 C25 F8 175.8(5) . . . . ?
N3 S1 C25 F9 55.9(5) . . . . ?
N3 S1 C25 F10 -64.7(5) . . . . ?
N3 S2 C26 F11 -177.0(4) . . . . ?
N3 S2 C26 F12 -58.2(5) . . . . ?
N3 S2 C26 F13 63.3(5) . . . . ?
C25 S1 N3 S2 86.2(5) . . . . ?
C26 S2 N3 S1 120.4(4) . . . . ?

_olex2_date_sample_data_collection 2016-11-08
_olex2_date_sample_submission    2016-11-07
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id NV2566
_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 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.791
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.56(4)
2 0.44(4)
####################################################################### 
# 
# 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_dwb1679b
_database_code_depnum_ccdc_archive 'CCDC 2177837'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H35 F19 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C33 H35 F25 N4 O5 S2'
_chemical_formula_weight         1106.77
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H35 F25 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio Riccobono ALR15 rpt at 220K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   6.7752(8)
_cell_length_b                   8.6424(9)
_cell_length_c                   74.967(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.731(11)
_cell_angle_gamma                90
_cell_volume                     4389.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3213
_cell_measurement_temperature    220.00(14)
_cell_measurement_theta_max      70.2100
_cell_measurement_theta_min      5.1360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.514
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0059
-1 1 0 0.1714
1 1 -1 0.1590
3 0 -5 0.2056
-3 -2 5 0.1959
0 -1 0 0.0430
0 1 0 0.0210
0 0 1 0.0069

_exptl_crystal_recrystallization_method 'evaporation of acetone/hexane'
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.013
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
-0.0001 -0.0002 -1.0001 -0.0173 -0.0111 0.0009
-1.0009 0.9987 0.0042 0.1522 -0.2368 0.0654
0.9998 1.0000 -1.0080 -0.0757 0.1072 0.2579
3.0009 0.0012 -5.0185 -0.4024 0.4772 0.2919
-2.9998 -2.0000 5.0223 0.3086 -0.3587 -0.6143
0.0005 -0.9994 0.0019 -0.0469 0.0592 -0.1612
-0.0005 0.9994 -0.0019 0.0469 -0.0592 0.1612
0.0001 0.0002 1.0001 0.0173 0.0111 -0.0009

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            13874
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.538
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -86.00 -36.50   0.75   10.00    --    0.00-178.00   0.00   66
  2  ω     37.00  68.50   0.75   10.00    --    0.00  57.00  60.00   42
  3  ω     14.00  44.00   0.75   10.00    --    0.00 -99.00  30.00   40
  4  ω   -115.00 -64.00   0.75   40.00    --  -56.36-141.00-175.00   68
  5  ω   -118.00 -88.00   0.75   40.00    --  -56.36 -94.00  30.00   40
  6  ω   -132.00 -81.00   0.75   40.00    --  -56.36 -94.00   0.00   68
  7  ω   -133.00 -94.00   0.75   40.00    --  -56.36 -94.00  60.00   52
  8  ω    -95.00 -44.75   0.75   40.00    --  -56.36 125.00-120.00   67
  9  ω   -125.00 -80.00   0.75   40.00    --  -56.36 -94.00  90.00   60
 10  ω   -118.00 -79.75   0.75   40.00    --  -56.36 -94.00 -60.00   51
 11  ω   -120.00 -87.00   0.75   40.00    --  -56.36 -94.00 -30.00   44
 12  ω    -15.00  84.00   0.75   40.00    --   56.36 -61.00 -30.00  132
 13  ω     35.00 107.00   0.75   50.00    --  112.72-111.00 -90.00   96
 14  ω    121.00 160.00   0.75   50.00    --  112.72  63.00-120.00   52
 15  ω    104.00 130.25   0.75   50.00    --  112.72 111.00-180.00   35
 16  ω     57.00 146.25   0.75   50.00    --  112.72 178.00 150.00  119
 17  ω     35.00 151.25   0.75   50.00    --  112.72 -91.00  90.00  155
 18  ω    141.00 173.25   0.75   50.00    --  112.72 111.00  60.00   43
 19  ω     56.00 175.25   0.75   50.00    --  112.72  25.00-180.00  159
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1052459000
_diffrn_orient_matrix_UB_12      0.0468871000
_diffrn_orient_matrix_UB_13      0.0172591000
_diffrn_orient_matrix_UB_21      0.1776343000
_diffrn_orient_matrix_UB_22      -0.0591577000
_diffrn_orient_matrix_UB_23      0.0111240000
_diffrn_orient_matrix_UB_31      0.0955999000
_diffrn_orient_matrix_UB_32      0.1613354000
_diffrn_orient_matrix_UB_33      -0.0009600000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4771
_reflns_number_total             7800
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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         0.428
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.00035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.1044
_refine_ls_restrained_S_all      1.069
_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)+(0.0568P)²+22.5275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2323
_refine_ls_wR_factor_ref         0.2616
_refine_special_details          
;
The perfluoroalkyl chain of the anion exhibited disorder.  The terminal
 trifluoromethyl group and the next 3 difluoromethylene groups were 
modelled in two positions, each group having its own refined occupancy.  
For the trifluoromethyl group the occupancies were 0.708:0.292(12).  
The occupancies of the minor form decreased going down the chain as 
follows: 0.722:0.278(12), 0.794:0.216(6) and 0.85:0.15(3).  For the 
trifluoromethyl and adjacent difluoromethylene, the carbons were also 
modelled over two sites.  The ADP of several pairs of atoms were 
constrained to be equal namely: C18 & C18A, C19 & C19A, F13 & F13A, 
F14 & F14A, F16 & F16A, F18 & F19A, F18A & F19.  The C-F distances 
for the minor trifluoromethyl were restrained to be equal as were
the terminal C-C bonds (C18-C19 and C18A-C19A) and the next 
methylene-methylene C-C bonds (C17-C18 & C17A-C18A).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F17A-C19A \\sim F19A-C19A \\sim F18A-C19A
 with sigma of 0.01
 C18A-C17 \\sim C18-C17
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F19) = Uanis(F18A)
Uanis(F19A) = Uanis(F18)
Uanis(C19) = Uanis(C19A)
Uanis(F16A) = Uanis(F16)
Uanis(C18) = Uanis(C18A)
Uanis(F13A) = Uanis(F13)
Uanis(F14) = Uanis(F14A)
4. Others
 Sof(C19A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=1-FVAR(1)
 Sof(C19)=Sof(F17)=Sof(F18)=Sof(F19)=FVAR(1)
 Sof(C18A)=Sof(F15A)=Sof(F16A)=1-FVAR(2)
 Sof(C18)=Sof(F15)=Sof(F16)=FVAR(2)
 Sof(F13A)=Sof(F14A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=FVAR(3)
 Sof(F11A)=Sof(F12A)=1-FVAR(4)
 Sof(F11)=Sof(F12)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C)
;
_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
C1 C 1.1129(9) 0.1074(8) 0.33277(9) 0.0431(16) Uani 1 1 d . . . . .
C2 C 1.0806(9) 0.2518(8) 0.33982(9) 0.0466(17) Uani 1 1 d . . . . .
H2 H 1.136708 0.338595 0.334577 0.056 Uiso 1 1 calc R U . . .
C3 C 0.9643(9) 0.2676(8) 0.35473(9) 0.0457(16) Uani 1 1 d . . . . .
H3 H 0.941238 0.365569 0.359403 0.055 Uiso 1 1 calc R U . . .
C4 C 0.8820(8) 0.1396(8) 0.36278(8) 0.0388(15) Uani 1 1 d . . . . .
C5 C 0.9096(10) -0.0048(9) 0.35519(9) 0.0521(18) Uani 1 1 d . . . . .
H5 H 0.848284 -0.090982 0.360064 0.063 Uiso 1 1 calc R U . . .
C6 C 1.0271(10) -0.0214(9) 0.34048(10) 0.0554(19) Uani 1 1 d . . . . .
H6 H 1.049072 -0.119197 0.335713 0.066 Uiso 1 1 calc R U . . .
C7 C 0.7688(9) 0.1521(8) 0.37916(9) 0.0410(15) Uani 1 1 d . . . . .
C8 C 0.6843(9) 0.1833(8) 0.40651(8) 0.0415(15) Uani 1 1 d . . . . .
C9 C 1.0441(9) 0.2391(11) 0.39952(10) 0.067(2) Uani 1 1 d . . . . .
H9A H 1.106386 0.158271 0.406336 0.100 Uiso 1 1 calc R U . . .
H9B H 1.044695 0.333098 0.406339 0.100 Uiso 1 1 calc R U . . .
H9C H 1.114827 0.254768 0.388655 0.100 Uiso 1 1 calc R U . . .
C10 C 0.4358(9) 0.0726(8) 0.36777(8) 0.0438(16) Uani 1 1 d . . . . .
H10A H 0.375714 -0.022948 0.371323 0.066 Uiso 1 1 calc R U . . .
H10B H 0.500491 0.058464 0.356565 0.066 Uiso 1 1 calc R U . . .
H10C H 0.336112 0.150945 0.366522 0.066 Uiso 1 1 calc R U . . .
C11 C 0.7050(10) 0.2137(9) 0.42628(9) 0.0490(18) Uani 1 1 d . . . . .
C12 C 0.5141(10) 0.2019(9) 0.43692(9) 0.0465(17) Uani 1 1 d . . . . .
C13 C 0.5334(10) 0.2546(9) 0.45663(9) 0.0489(17) Uani 1 1 d . . . . .
C14 C 0.3638(10) 0.2034(9) 0.46852(9) 0.0484(17) Uani 1 1 d . . . . .
C15 C 0.3542(11) 0.2803(9) 0.48710(9) 0.0500(17) Uani 1 1 d . . . . .
C16 C 0.2098(12) 0.2087(10) 0.50015(10) 0.0551(19) Uani 1 1 d . . . . .
C17 C 0.1812(11) 0.2908(10) 0.51799(10) 0.0541(19) Uani 1 1 d D . . . .
C18 C 0.029(3) 0.221(2) 0.53027(16) 0.075(6) Uani 0.722(12) 1 d D . P A 1
C18A C 0.082(10) 0.232(8) 0.5347(4) 0.075(6) Uani 0.278(12) 1 d D . P A 2
C19 C 0.012(2) 0.291(2) 0.5484(2) 0.069(4) Uani 0.708(12) 1 d D . P A 1
C19A C -0.054(5) 0.301(5) 0.5480(5) 0.069(4) Uani 0.292(12) 1 d D . P A 2
C20 C 1.3791(10) 0.1903(9) 0.31399(9) 0.0524(18) Uani 1 1 d . . . . .
H20A H 1.451910 0.224761 0.324480 0.063 Uiso 1 1 calc R U . . .
H20B H 1.317830 0.279424 0.308324 0.063 Uiso 1 1 calc R U . . .
C21 C 1.5139(11) 0.1089(9) 0.30122(10) 0.058(2) Uani 1 1 d . . . . .
H21A H 1.436716 0.073432 0.291030 0.069 Uiso 1 1 calc R U . . .
H21B H 1.569372 0.018501 0.307085 0.069 Uiso 1 1 calc R U . . .
C22 C 1.6826(10) 0.2107(9) 0.29460(10) 0.0519(18) Uani 1 1 d . . . . .
H22A H 1.628427 0.302534 0.288929 0.062 Uiso 1 1 calc R U . . .
H22B H 1.763579 0.243466 0.304670 0.062 Uiso 1 1 calc R U . . .
C23 C 1.8099(10) 0.1237(9) 0.28135(10) 0.0548(19) Uani 1 1 d . . . . .
H23A H 1.865971 0.033830 0.287271 0.066 Uiso 1 1 calc R U . . .
H23B H 1.725944 0.086826 0.271670 0.066 Uiso 1 1 calc R U . . .
C24 C 1.9760(10) 0.2177(9) 0.27352(10) 0.0544(19) Uani 1 1 d . . . . .
H24A H 2.063738 0.251085 0.283101 0.065 Uiso 1 1 calc R U . . .
H24B H 1.921143 0.309639 0.267928 0.065 Uiso 1 1 calc R U . . .
C25 C 2.0950(10) 0.1293(9) 0.25984(10) 0.0567(19) Uani 1 1 d . . . . .
H25A H 2.146424 0.035918 0.265375 0.068 Uiso 1 1 calc R U . . .
H25B H 2.007491 0.098207 0.250146 0.068 Uiso 1 1 calc R U . . .
C26 C 2.2658(10) 0.2202(9) 0.25217(10) 0.0524(18) Uani 1 1 d . . . . .
H26A H 2.353971 0.250710 0.261841 0.063 Uiso 1 1 calc R U . . .
H26B H 2.214679 0.313799 0.246671 0.063 Uiso 1 1 calc R U . . .
C27 C 2.3832(11) 0.1305(9) 0.23840(10) 0.057(2) Uani 1 1 d . . . . .
H27A H 2.433831 0.036659 0.243887 0.069 Uiso 1 1 calc R U . . .
H27B H 2.295105 0.100310 0.228708 0.069 Uiso 1 1 calc R U . . .
C28 C 2.5531(10) 0.2202(9) 0.23083(10) 0.0561(19) Uani 1 1 d . . . . .
H28A H 2.640039 0.251562 0.240553 0.067 Uiso 1 1 calc R U . . .
H28B H 2.502073 0.313371 0.225228 0.067 Uiso 1 1 calc R U . . .
C29 C 2.6735(11) 0.1308(9) 0.21718(10) 0.058(2) Uani 1 1 d . . . . .
H29A H 2.721482 0.035941 0.222631 0.070 Uiso 1 1 calc R U . . .
H29B H 2.588038 0.102480 0.207227 0.070 Uiso 1 1 calc R U . . .
C30 C 2.8475(11) 0.2212(10) 0.21019(11) 0.063(2) Uani 1 1 d . . . . .
H30A H 2.932289 0.249921 0.220179 0.076 Uiso 1 1 calc R U . . .
H30B H 2.799124 0.315941 0.204743 0.076 Uiso 1 1 calc R U . . .
C31 C 2.9697(13) 0.1339(11) 0.19662(11) 0.075(3) Uani 1 1 d . . . . .
H31A H 2.890394 0.113246 0.186187 0.113 Uiso 1 1 calc R U . . .
H31B H 3.014135 0.037885 0.201717 0.113 Uiso 1 1 calc R U . . .
H31C H 3.081771 0.195287 0.193389 0.113 Uiso 1 1 calc R U . . .
F1 F 0.8350(6) 0.1077(7) 0.43286(5) 0.0787(15) Uani 1 1 d . . . . .
F2 F 0.7843(6) 0.3535(6) 0.42913(5) 0.0684(13) Uani 1 1 d . . . . .
F3 F 0.4494(7) 0.0572(5) 0.43619(5) 0.0669(13) Uani 1 1 d . . . . .
F4 F 0.3787(6) 0.2923(6) 0.42887(5) 0.0636(12) Uani 1 1 d . . . . .
F5 F 0.7033(6) 0.2067(7) 0.46341(5) 0.0771(15) Uani 1 1 d . . . . .
F6 F 0.5366(7) 0.4101(5) 0.45669(6) 0.0744(14) Uani 1 1 d . . . . .
F7 F 0.3865(8) 0.0493(5) 0.47113(6) 0.0801(15) Uani 1 1 d . . . . .
F8 F 0.1931(6) 0.2222(7) 0.45999(5) 0.0749(15) Uani 1 1 d . . . . .
F9 F 0.5348(6) 0.2791(7) 0.49443(6) 0.0830(16) Uani 1 1 d . . . . .
F10 F 0.3027(9) 0.4273(6) 0.48456(6) 0.0885(17) Uani 1 1 d . . . . .
F11 F 0.254(3) 0.0642(9) 0.50321(12) 0.087(5) Uani 0.85(3) 1 d . . P B 1
F11A F 0.376(8) 0.101(7) 0.5088(6) 0.059(16) Uani 0.15(3) 1 d . . P B 2
F12 F 0.0279(12) 0.212(2) 0.49182(9) 0.080(5) Uani 0.85(3) 1 d . . P B 1
F12A F 0.094(7) 0.113(5) 0.4943(4) 0.048(14) Uani 0.15(3) 1 d . . P B 2
F13 F 0.3614(9) 0.2803(10) 0.52669(8) 0.083(2) Uani 0.794(6) 1 d . . P A 1
F13A F -0.008(4) 0.363(4) 0.5105(3) 0.083(2) Uani 0.206(6) 1 d . . P A 2
F14 F 0.1459(12) 0.4411(7) 0.51606(8) 0.079(2) Uani 0.794(6) 1 d . . P A 1
F14A F 0.300(5) 0.398(3) 0.5207(4) 0.079(2) Uani 0.206(6) 1 d . . P A 2
F15 F -0.1506(10) 0.2456(10) 0.52231(9) 0.085(3) Uani 0.722(12) 1 d . . P A 1
F15A F 0.268(3) 0.168(3) 0.5422(2) 0.120(11) Uani 0.278(12) 1 d . . P A 2
F16 F 0.057(3) 0.0670(18) 0.5325(2) 0.081(4) Uani 0.722(12) 1 d . . P A 1
F16A F 0.015(10) 0.102(6) 0.5289(7) 0.081(4) Uani 0.278(12) 1 d . . P A 2
F17 F 0.1707(14) 0.2777(17) 0.55822(10) 0.129(5) Uani 0.708(12) 1 d . . P A 1
F17A F -0.212(3) 0.302(3) 0.5405(3) 0.124(11) Uani 0.292(12) 1 d D . P A 2
F18 F -0.125(2) 0.2207(18) 0.55777(16) 0.131(6) Uani 0.708(12) 1 d . . P A 1
F18A F -0.052(7) 0.230(4) 0.5619(4) 0.113(5) Uani 0.292(12) 1 d D . P A 2
F19 F -0.030(2) 0.4452(12) 0.54745(15) 0.113(5) Uani 0.708(12) 1 d . . P A 1
F19A F 0.050(7) 0.410(6) 0.5519(4) 0.131(6) Uani 0.292(12) 1 d D . P A 2
N1 N 0.8400(7) 0.1949(7) 0.39529(7) 0.0414(13) Uani 1 1 d . . . . .
N2 N 0.5801(7) 0.1202(6) 0.38126(7) 0.0388(12) Uani 1 1 d . . . . .
N3 N 0.5235(7) 0.1394(6) 0.39843(7) 0.0413(13) Uani 1 1 d . . . . .
O1 O 1.2322(7) 0.0774(6) 0.31874(6) 0.0597(14) Uani 1 1 d . . . . .
C32 C 0.4426(16) 0.6702(14) 0.40574(15) 0.087(3) Uani 1 1 d . . . . .
C33 C 0.6010(14) 0.6244(10) 0.33946(11) 0.066(2) Uani 1 1 d . . . . .
F20 F 0.3377(10) 0.7991(8) 0.40531(9) 0.115(2) Uani 1 1 d . . . . .
F21 F 0.3198(10) 0.5553(8) 0.40231(9) 0.122(2) Uani 1 1 d . . . . .
F22 F 0.5101(12) 0.6519(9) 0.42220(8) 0.134(3) Uani 1 1 d . . . . .
F23 F 0.5639(9) 0.7645(6) 0.33333(7) 0.0888(16) Uani 1 1 d . . . . .
F24 F 0.5618(11) 0.5257(7) 0.32622(7) 0.112(2) Uani 1 1 d . . . . .
F25 F 0.7896(8) 0.6164(6) 0.34333(7) 0.0829(15) Uani 1 1 d . . . . .
N4 N 0.5269(11) 0.7023(7) 0.37207(9) 0.0648(18) Uani 1 1 d . . . . .
O2 O 0.7494(9) 0.8106(7) 0.39436(8) 0.0790(18) Uani 1 1 d . . . . .
O3 O 0.7376(10) 0.5268(7) 0.39164(8) 0.0863(19) Uani 1 1 d . . . . .
O4 O 0.2558(8) 0.6128(8) 0.35255(10) 0.094(2) Uani 1 1 d . . . . .
O5 O 0.4954(9) 0.4188(6) 0.36253(8) 0.0754(17) Uani 1 1 d . . . . .
S1 S 0.6422(3) 0.6739(3) 0.38990(3) 0.0674(6) Uani 1 1 d . . . . .
S2 S 0.4484(3) 0.5778(2) 0.35848(3) 0.0652(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.374(9) . ?
C1 C6 1.386(9) . ?
C1 O1 1.360(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.383(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.381(9) . ?
C4 C5 1.385(9) . ?
C4 C7 1.459(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.376(9) . ?
C6 H6 0.9300 . ?
C7 N1 1.348(8) . ?
C7 N2 1.319(7) . ?
C8 C11 1.510(9) . ?
C8 N1 1.361(7) . ?
C8 N3 1.297(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 N1 1.465(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N2 1.457(8) . ?
C11 C12 1.532(9) . ?
C11 F1 1.359(8) . ?
C11 F2 1.338(8) . ?
C12 C13 1.550(9) . ?
C12 F3 1.326(8) . ?
C12 F4 1.343(8) . ?
C13 C14 1.529(9) . ?
C13 F5 1.319(8) . ?
C13 F6 1.343(8) . ?
C14 C15 1.545(9) . ?
C14 F7 1.354(8) . ?
C14 F8 1.324(8) . ?
C15 C16 1.524(10) . ?
C15 F9 1.335(8) . ?
C15 F10 1.330(9) . ?
C16 C17 1.529(10) . ?
C16 F11 1.303(11) . ?
C16 F11A 1.59(3) . ?
C16 F12 1.375(12) . ?
C16 F12A 1.22(3) . ?
C17 C18 1.517(12) . ?
C17 C18A 1.518(14) . ?
C17 F13 1.379(9) . ?
C17 F13A 1.52(3) . ?
C17 F14 1.328(10) . ?
C17 F14A 1.24(3) . ?
C18 C19 1.493(15) . ?
C18 F15 1.36(2) . ?
C18 F16 1.36(3) . ?
C18A C19A 1.49(2) . ?
C18A F15A 1.48(8) . ?
C18A F16A 1.29(8) . ?
C19 F17 1.299(18) . ?
C19 F18 1.321(15) . ?
C19 F19 1.362(18) . ?
C19A F17A 1.21(2) . ?
C19A F18A 1.21(2) . ?
C19A F19A 1.21(2) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.505(9) . ?
C20 O1 1.442(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.530(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.522(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.513(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.519(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.518(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.524(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.505(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.527(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.513(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.521(10) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
N2 N3 1.358(7) . ?
C32 F20 1.321(12) . ?
C32 F21 1.319(11) . ?
C32 F22 1.320(12) . ?
C32 S1 1.811(10) . ?
C33 F23 1.318(10) . ?
C33 F24 1.333(9) . ?
C33 F25 1.309(9) . ?
C33 S2 1.817(9) . ?
N4 S1 1.559(7) . ?
N4 S2 1.569(7) . ?
O2 S1 1.425(6) . ?
O3 S1 1.431(6) . ?
O4 S2 1.406(6) . ?
O5 S2 1.442(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 120.0(6) . . ?
O1 C1 C2 124.7(6) . . ?
O1 C1 C6 115.2(6) . . ?
C1 C2 H2 120.1 . . ?
C1 C2 C3 119.7(6) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(6) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 119.0(6) . . ?
C3 C4 C7 121.8(6) . . ?
C5 C4 C7 119.2(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(7) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.0(7) . . ?
C5 C6 H6 120.0 . . ?
N1 C7 C4 126.1(5) . . ?
N2 C7 C4 127.2(6) . . ?
N2 C7 N1 106.6(5) . . ?
N1 C8 C11 122.1(6) . . ?
N3 C8 C11 125.2(6) . . ?
N3 C8 N1 112.7(6) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
C8 C11 C12 115.5(6) . . ?
F1 C11 C8 106.9(6) . . ?
F1 C11 C12 108.3(6) . . ?
F2 C11 C8 110.3(6) . . ?
F2 C11 C12 108.5(6) . . ?
F2 C11 F1 107.1(6) . . ?
C11 C12 C13 114.5(6) . . ?
F3 C12 C11 108.8(6) . . ?
F3 C12 C13 109.9(6) . . ?
F3 C12 F4 107.9(6) . . ?
F4 C12 C11 107.7(6) . . ?
F4 C12 C13 107.8(6) . . ?
C14 C13 C12 114.6(6) . . ?
F5 C13 C12 109.7(6) . . ?
F5 C13 C14 110.0(6) . . ?
F5 C13 F6 107.4(6) . . ?
F6 C13 C12 107.4(6) . . ?
F6 C13 C14 107.4(6) . . ?
C13 C14 C15 116.2(6) . . ?
F7 C14 C13 106.5(6) . . ?
F7 C14 C15 107.4(6) . . ?
F8 C14 C13 109.9(6) . . ?
F8 C14 C15 109.6(6) . . ?
F8 C14 F7 106.7(6) . . ?
C16 C15 C14 116.0(6) . . ?
F9 C15 C14 108.6(6) . . ?
F9 C15 C16 109.0(6) . . ?
F10 C15 C14 107.2(6) . . ?
F10 C15 C16 108.1(6) . . ?
F10 C15 F9 107.7(6) . . ?
C15 C16 C17 117.6(6) . . ?
C15 C16 F11A 92.3(16) . . ?
C17 C16 F11A 90.7(19) . . ?
F11 C16 C15 110.8(8) . . ?
F11 C16 C17 108.8(7) . . ?
F11 C16 F12 107.6(8) . . ?
F12 C16 C15 106.2(7) . . ?
F12 C16 C17 105.3(7) . . ?
F12A C16 C15 117.6(15) . . ?
F12A C16 C17 122.7(17) . . ?
F12A C16 F11A 101(2) . . ?
C18 C17 C16 116.2(8) . . ?
C18A C17 C16 129(2) . . ?
C18A C17 F13A 94(3) . . ?
F13 C17 C16 105.2(6) . . ?
F13 C17 C18 107.0(10) . . ?
F13A C17 C16 89.1(10) . . ?
F14 C17 C16 112.5(7) . . ?
F14 C17 C18 109.3(11) . . ?
F14 C17 F13 105.9(7) . . ?
F14A C17 C16 113.7(13) . . ?
F14A C17 C18A 114(2) . . ?
F14A C17 F13A 107(2) . . ?
C19 C18 C17 116.7(10) . . ?
F15 C18 C17 106.4(12) . . ?
F15 C18 C19 105.0(16) . . ?
F16 C18 C17 111.7(18) . . ?
F16 C18 C19 107.4(15) . . ?
F16 C18 F15 109.2(14) . . ?
C19A C18A C17 135(5) . . ?
F15A C18A C17 93(3) . . ?
F15A C18A C19A 115(3) . . ?
F16A C18A C17 100(4) . . ?
F16A C18A C19A 111(4) . . ?
F16A C18A F15A 95(6) . . ?
F17 C19 C18 114.1(14) . . ?
F17 C19 F18 103.7(14) . . ?
F17 C19 F19 106.9(15) . . ?
F18 C19 C18 110.9(12) . . ?
F18 C19 F19 109.3(16) . . ?
F19 C19 C18 111.6(17) . . ?
F17A C19A C18A 104(4) . . ?
F17A C19A F18A 114(4) . . ?
F17A C19A F19A 128(5) . . ?
F18A C19A C18A 112(3) . . ?
F18A C19A F19A 101(3) . . ?
F19A C19A C18A 96(4) . . ?
H20A C20 H20B 108.8 . . ?
C21 C20 H20A 110.6 . . ?
C21 C20 H20B 110.6 . . ?
O1 C20 H20A 110.6 . . ?
O1 C20 H20B 110.6 . . ?
O1 C20 C21 105.5(6) . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
C20 C21 C22 113.5(6) . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C21 C22 H22A 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 C21 111.1(6) . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C22 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.7(6) . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C23 C24 C25 113.3(6) . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
C24 C25 H25A 108.7 . . ?
C24 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 C24 114.1(6) . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
C25 C26 C27 113.6(6) . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C26 C27 H27A 108.8 . . ?
C26 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 C26 113.7(7) . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
C27 C28 C29 114.2(6) . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C28 C29 H29A 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C30 C29 C28 113.3(6) . . ?
C30 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C29 C30 H30A 108.7 . . ?
C29 C30 H30B 108.7 . . ?
C29 C30 C31 114.1(7) . . ?
H30A C30 H30B 107.6 . . ?
C31 C30 H30A 108.7 . . ?
C31 C30 H30B 108.7 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C7 N1 C8 105.3(5) . . ?
C7 N1 C9 126.2(5) . . ?
C8 N1 C9 128.5(5) . . ?
C7 N2 C10 128.2(5) . . ?
C7 N2 N3 111.9(5) . . ?
N3 N2 C10 119.8(5) . . ?
C8 N3 N2 103.4(5) . . ?
C1 O1 C20 118.8(5) . . ?
F20 C32 S1 112.0(7) . . ?
F21 C32 F20 107.0(9) . . ?
F21 C32 F22 107.6(9) . . ?
F21 C32 S1 111.1(8) . . ?
F22 C32 F20 107.7(9) . . ?
F22 C32 S1 111.3(8) . . ?
F23 C33 F24 107.0(7) . . ?
F23 C33 S2 111.7(6) . . ?
F24 C33 S2 109.4(6) . . ?
F25 C33 F23 107.9(7) . . ?
F25 C33 F24 108.4(8) . . ?
F25 C33 S2 112.2(6) . . ?
S1 N4 S2 127.6(4) . . ?
N4 S1 C32 101.2(5) . . ?
O2 S1 C32 104.1(5) . . ?
O2 S1 N4 108.6(4) . . ?
O2 S1 O3 119.1(4) . . ?
O3 S1 C32 105.3(5) . . ?
O3 S1 N4 116.0(4) . . ?
N4 S2 C33 99.6(4) . . ?
O4 S2 C33 103.8(4) . . ?
O4 S2 N4 111.3(4) . . ?
O4 S2 O5 118.2(4) . . ?
O5 S2 C33 104.5(4) . . ?
O5 S2 N4 116.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.8(10) . . . . ?
C2 C1 C6 C5 0.0(11) . . . . ?
C2 C1 O1 C20 19.2(10) . . . . ?
C2 C3 C4 C5 -3.1(10) . . . . ?
C2 C3 C4 C7 176.2(6) . . . . ?
C3 C4 C5 C6 3.9(11) . . . . ?
C3 C4 C7 N1 -65.9(10) . . . . ?
C3 C4 C7 N2 116.1(8) . . . . ?
C4 C5 C6 C1 -2.4(11) . . . . ?
C4 C7 N1 C8 -177.4(7) . . . . ?
C4 C7 N1 C9 0.8(12) . . . . ?
C4 C7 N2 C10 -3.4(11) . . . . ?
C4 C7 N2 N3 177.8(6) . . . . ?
C5 C4 C7 N1 113.4(8) . . . . ?
C5 C4 C7 N2 -64.6(10) . . . . ?
C6 C1 C2 C3 0.8(10) . . . . ?
C6 C1 O1 C20 -158.2(7) . . . . ?
C7 C4 C5 C6 -175.4(6) . . . . ?
C7 N2 N3 C8 -0.1(7) . . . . ?
C8 C11 C12 C13 -172.3(6) . . . . ?
C8 C11 C12 F3 64.3(8) . . . . ?
C8 C11 C12 F4 -52.3(8) . . . . ?
C10 N2 N3 C8 -179.0(6) . . . . ?
C11 C8 N1 C7 176.8(6) . . . . ?
C11 C8 N1 C9 -1.3(11) . . . . ?
C11 C8 N3 N2 -177.1(7) . . . . ?
C11 C12 C13 C14 -164.2(7) . . . . ?
C11 C12 C13 F5 -39.9(9) . . . . ?
C11 C12 C13 F6 76.5(8) . . . . ?
C12 C13 C14 C15 -167.9(6) . . . . ?
C12 C13 C14 F7 72.5(8) . . . . ?
C12 C13 C14 F8 -42.7(9) . . . . ?
C13 C14 C15 C16 -169.2(7) . . . . ?
C13 C14 C15 F9 -46.1(9) . . . . ?
C13 C14 C15 F10 70.0(8) . . . . ?
C14 C15 C16 C17 -174.2(7) . . . . ?
C14 C15 C16 F11 59.9(11) . . . . ?
C14 C15 C16 F11A 94(3) . . . . ?
C14 C15 C16 F12 -56.7(11) . . . . ?
C14 C15 C16 F12A -10(3) . . . . ?
C15 C16 C17 C18 176.9(13) . . . . ?
C15 C16 C17 C18A -167(4) . . . . ?
C15 C16 C17 F13 -64.9(10) . . . . ?
C15 C16 C17 F13A 99.6(13) . . . . ?
C15 C16 C17 F14 49.8(10) . . . . ?
C15 C16 C17 F14A -9(2) . . . . ?
C16 C17 C18 C19 174.6(15) . . . . ?
C16 C17 C18 F15 -68.6(17) . . . . ?
C16 C17 C18 F16 50.5(19) . . . . ?
C16 C17 C18A C19A -138(4) . . . . ?
C16 C17 C18A F15A 90(3) . . . . ?
C16 C17 C18A F16A -6(7) . . . . ?
C17 C18 C19 F17 -63(2) . . . . ?
C17 C18 C19 F18 -179.8(18) . . . . ?
C17 C18 C19 F19 58(2) . . . . ?
C17 C18A C19A F17A 76(6) . . . . ?
C17 C18A C19A F18A -160(5) . . . . ?
C17 C18A C19A F19A -55(7) . . . . ?
C20 C21 C22 C23 -178.3(7) . . . . ?
C21 C20 O1 C1 167.2(6) . . . . ?
C21 C22 C23 C24 177.7(7) . . . . ?
C22 C23 C24 C25 -177.8(7) . . . . ?
C23 C24 C25 C26 -178.5(7) . . . . ?
C24 C25 C26 C27 -179.7(7) . . . . ?
C25 C26 C27 C28 -179.8(7) . . . . ?
C26 C27 C28 C29 179.3(7) . . . . ?
C27 C28 C29 C30 -178.1(7) . . . . ?
C28 C29 C30 C31 179.8(7) . . . . ?
F1 C11 C12 C13 67.9(8) . . . . ?
F1 C11 C12 F3 -55.5(7) . . . . ?
F1 C11 C12 F4 -172.2(5) . . . . ?
F2 C11 C12 C13 -47.9(8) . . . . ?
F2 C11 C12 F3 -171.3(5) . . . . ?
F2 C11 C12 F4 72.0(7) . . . . ?
F3 C12 C13 C14 -41.4(8) . . . . ?
F3 C12 C13 F5 82.9(7) . . . . ?
F3 C12 C13 F6 -160.7(6) . . . . ?
F4 C12 C13 C14 75.9(8) . . . . ?
F4 C12 C13 F5 -159.7(6) . . . . ?
F4 C12 C13 F6 -43.3(7) . . . . ?
F5 C13 C14 C15 67.9(8) . . . . ?
F5 C13 C14 F7 -51.7(8) . . . . ?
F5 C13 C14 F8 -166.9(6) . . . . ?
F6 C13 C14 C15 -48.7(8) . . . . ?
F6 C13 C14 F7 -168.3(6) . . . . ?
F6 C13 C14 F8 76.5(7) . . . . ?
F7 C14 C15 C16 -50.1(9) . . . . ?
F7 C14 C15 F9 73.0(8) . . . . ?
F7 C14 C15 F10 -170.9(6) . . . . ?
F8 C14 C15 C16 65.5(9) . . . . ?
F8 C14 C15 F9 -171.5(6) . . . . ?
F8 C14 C15 F10 -55.4(8) . . . . ?
F9 C15 C16 C17 62.9(9) . . . . ?
F9 C15 C16 F11 -63.0(11) . . . . ?
F9 C15 C16 F11A -29(3) . . . . ?
F9 C15 C16 F12 -179.6(9) . . . . ?
F9 C15 C16 F12A -133(3) . . . . ?
F10 C15 C16 C17 -53.8(9) . . . . ?
F10 C15 C16 F11 -179.8(10) . . . . ?
F10 C15 C16 F11A -146(3) . . . . ?
F10 C15 C16 F12 63.7(10) . . . . ?
F10 C15 C16 F12A 110(3) . . . . ?
F11 C16 C17 C18 -56.2(16) . . . . ?
F11 C16 C17 F13 62.0(11) . . . . ?
F11 C16 C17 F14 176.7(10) . . . . ?
F11A C16 C17 C18A -74(5) . . . . ?
F11A C16 C17 F13A -167(3) . . . . ?
F11A C16 C17 F14A 84(3) . . . . ?
F12 C16 C17 C18 59.0(15) . . . . ?
F12 C16 C17 F13 177.1(9) . . . . ?
F12 C16 C17 F14 -68.1(11) . . . . ?
F12A C16 C17 C18A 31(5) . . . . ?
F12A C16 C17 F13A -63(4) . . . . ?
F12A C16 C17 F14A -171(4) . . . . ?
F13 C17 C18 C19 57(2) . . . . ?
F13 C17 C18 F15 174.3(10) . . . . ?
F13 C17 C18 F16 -66.6(16) . . . . ?
F13A C17 C18A C19A -47(6) . . . . ?
F13A C17 C18A F15A -178(3) . . . . ?
F13A C17 C18A F16A 86(5) . . . . ?
F14 C17 C18 C19 -57(2) . . . . ?
F14 C17 C18 F15 60.1(13) . . . . ?
F14 C17 C18 F16 179.2(14) . . . . ?
F14A C17 C18A C19A 64(7) . . . . ?
F14A C17 C18A F15A -67(4) . . . . ?
F14A C17 C18A F16A -164(4) . . . . ?
F15 C18 C19 F17 179.2(13) . . . . ?
F15 C18 C19 F18 62.6(19) . . . . ?
F15 C18 C19 F19 -59.5(15) . . . . ?
F15A C18A C19A F17A -160(4) . . . . ?
F15A C18A C19A F18A -36(5) . . . . ?
F15A C18A C19A F19A 68(4) . . . . ?
F16 C18 C19 F17 63(2) . . . . ?
F16 C18 C19 F18 -54(2) . . . . ?
F16 C18 C19 F19 -175.7(17) . . . . ?
F16A C18A C19A F17A -53(6) . . . . ?
F16A C18A C19A F18A 71(6) . . . . ?
F16A C18A C19A F19A 175(6) . . . . ?
N1 C7 N2 C10 178.2(6) . . . . ?
N1 C7 N2 N3 -0.5(7) . . . . ?
N1 C8 C11 C12 177.7(6) . . . . ?
N1 C8 C11 F1 -61.7(9) . . . . ?
N1 C8 C11 F2 54.3(9) . . . . ?
N1 C8 N3 N2 0.8(8) . . . . ?
N2 C7 N1 C8 0.9(7) . . . . ?
N2 C7 N1 C9 179.1(7) . . . . ?
N3 C8 C11 C12 -4.7(11) . . . . ?
N3 C8 C11 F1 115.9(7) . . . . ?
N3 C8 C11 F2 -128.1(7) . . . . ?
N3 C8 N1 C7 -1.1(8) . . . . ?
N3 C8 N1 C9 -179.2(7) . . . . ?
O1 C1 C2 C3 -176.5(6) . . . . ?
O1 C1 C6 C5 177.6(6) . . . . ?
O1 C20 C21 C22 -179.8(6) . . . . ?
F20 C32 S1 N4 -57.4(9) . . . . ?
F20 C32 S1 O2 55.3(9) . . . . ?
F20 C32 S1 O3 -178.6(8) . . . . ?
F21 C32 S1 N4 62.2(9) . . . . ?
F21 C32 S1 O2 174.9(8) . . . . ?
F21 C32 S1 O3 -59.0(9) . . . . ?
F22 C32 S1 N4 -178.0(8) . . . . ?
F22 C32 S1 O2 -65.3(9) . . . . ?
F22 C32 S1 O3 60.8(9) . . . . ?
F23 C33 S2 N4 -63.9(7) . . . . ?
F23 C33 S2 O4 51.0(7) . . . . ?
F23 C33 S2 O5 175.5(6) . . . . ?
F24 C33 S2 N4 177.8(7) . . . . ?
F24 C33 S2 O4 -67.4(7) . . . . ?
F24 C33 S2 O5 57.2(7) . . . . ?
F25 C33 S2 N4 57.4(7) . . . . ?
F25 C33 S2 O4 172.3(6) . . . . ?
F25 C33 S2 O5 -63.2(7) . . . . ?
S1 N4 S2 C33 -114.4(6) . . . . ?
S1 N4 S2 O4 136.6(6) . . . . ?
S1 N4 S2 O5 -2.9(7) . . . . ?
S2 N4 S1 C32 -93.3(7) . . . . ?
S2 N4 S1 O2 157.5(5) . . . . ?
S2 N4 S1 O3 20.1(8) . . . . ?

_olex2_date_sample_data_collection 2017-07-19
_olex2_date_sample_submission    2016-11-24
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre 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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.782
####################################################################### 
# 
# 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_dwb1681b
_database_code_depnum_ccdc_archive 'CCDC 2177839'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H39 F7 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C29 H39 F13 N4 O5 S2'
_chemical_formula_weight         834.76
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H39 F13 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio NV2586 repeat 220K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   6.8348(3)
_cell_length_b                   8.5999(4)
_cell_length_c                   63.658(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.931(5)
_cell_angle_gamma                90
_cell_volume                     3741.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6763
_cell_measurement_temperature    220.00(14)
_cell_measurement_theta_max      70.4280
_cell_measurement_theta_min      5.1850
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.555
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1720
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0083
0 0 -1 0.0163
-1 0 0 0.1503
1 0 0 0.1433
0 1 0 0.0767
0 -1 0 0.0767

_exptl_crystal_recrystallization_method 'Evaporation of acetone/hexane'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.025
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
-0.0001 0.0000 0.9999 0.0100 0.0220 -0.0006
0.0001 -0.0000 -0.9999 -0.0100 -0.0220 0.0006
-0.9999 0.0002 0.0010 0.1932 -0.0888 0.0749
0.9999 -0.0002 -0.0010 -0.1932 0.0888 -0.0749
-0.0001 1.0005 -0.0016 -0.0525 0.0284 0.1690
0.0001 -1.0005 0.0016 0.0525 -0.0284 -0.1690

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            21029
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.472
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -37.00  74.00   0.75    2.00    --    0.00  77.00-120.00  148
  2  ω      1.00  49.00   0.75    2.00    --    0.00 -99.00 -60.00   64
  3  ω   -133.00 -73.00   0.75    8.00    --  -56.36-125.00-180.00   80
  4  ω   -136.00 -80.50   0.75    8.00    --  -56.36 -94.00 120.00   74
  5  ω   -136.00 -80.50   0.75    8.00    --  -56.36 -94.00-150.00   74
  6  ω   -136.00 -80.50   0.75    8.00    --  -56.36 -94.00 150.00   74
  7  ω   -133.00 -73.00   0.75    8.00    --  -56.36-125.00 -30.00   80
  8  ω    -19.00  92.00   0.75    8.00    --   56.36 -77.00  60.00  148
  9  ω     26.00 128.00   0.75    8.00    --   56.36  61.00-180.00  136
 10  ω     36.00 153.00   0.75   20.00    --  112.72 -37.00 -90.00  156
 11  ω     34.00 115.00   0.75   20.00    --  112.72-111.00   0.00  108
 12  ω     72.00 177.00   0.75   20.00    --  112.72  37.00  90.00  140
 13  ω    100.00 178.00   0.75   20.00    --  112.72 111.00  30.00  104
 14  ω     38.00 143.00   0.75   20.00    --  112.72 -50.00   0.00  140
 15  ω     41.00 143.00   0.75   20.00    --  112.72 -63.00 -90.00  136
 16  ω     34.00 115.00   0.75   20.00    --  112.72-111.00-150.00  108
 17  ω     57.00 150.00   0.75   20.00    --  112.72 178.00 -60.00  124
 18  ω    -86.00 -35.00   0.75    2.00    --    0.00-178.00  60.00   68
 19  ω    -86.00 -35.00   0.75    2.00    --    0.00-178.00 -30.00   68
 20  ω   -132.00 -21.00   0.75    8.00    --  -56.36 -77.00  60.00  148
 21  ω     26.00 128.00   0.75    8.00    --   56.36  61.00 -30.00  136
 22  ω     20.00 126.50   0.75    8.00    --   56.36  77.00-120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1931869000
_diffrn_orient_matrix_UB_12      -0.0524545000
_diffrn_orient_matrix_UB_13      0.0099482000
_diffrn_orient_matrix_UB_21      0.0888023000
_diffrn_orient_matrix_UB_22      0.0284391000
_diffrn_orient_matrix_UB_23      0.0220577000
_diffrn_orient_matrix_UB_31      -0.0748424000
_diffrn_orient_matrix_UB_32      0.1689114000
_diffrn_orient_matrix_UB_33      -0.0006246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                9347
_reflns_number_total             10458
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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         0.503
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         10458
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0980
_refine_ls_restrained_S_all      1.065
_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)+(0.1510P)²+11.3268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2747
_refine_ls_wR_factor_ref         0.2810
_refine_special_details          
;
The crystal was both pseudomerohedrally and racemically twinned which 
was modelled using a twin matrix (-1 0 0 0 -1 0 0 0 1) and 3 
weightings which refined to 0.00(3), 0.11(5) and 0.16(3).
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.75(7)
 -0.02(3) 0.11(5) 0.16(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O5)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C41(H41A,H41B),
  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C29(H29), C30(H30), C32(H32), C33(H33)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C54(H54A,H54B,H54C)
;
_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
C1 C -0.0233(19) 0.6894(17) 0.1105(2) 0.046(3) Uani 1 1 d . . . . .
C2 C -0.107(2) 0.5582(16) 0.1194(2) 0.047(3) Uani 1 1 d . . . . .
H2 H -0.082550 0.459949 0.113478 0.057 Uiso 1 1 calc R U . . .
C3 C -0.225(2) 0.5700(17) 0.1367(2) 0.051(4) Uani 1 1 d . . . . .
H3 H -0.288210 0.482286 0.142197 0.061 Uiso 1 1 calc R U . . .
C4 C -0.2462(14) 0.7146(13) 0.14566(17) 0.031(2) Uani 1 1 d . . . . .
C5 C -0.1673(17) 0.8462(13) 0.1373(2) 0.039(3) Uani 1 1 d . . . . .
H5 H -0.192052 0.943925 0.143282 0.047 Uiso 1 1 calc R U . . .
C6 C -0.046(2) 0.8336(14) 0.11920(19) 0.042(3) Uani 1 1 d . . . . .
H6 H 0.014884 0.921474 0.113488 0.050 Uiso 1 1 calc R U . . .
C7 C -0.3672(17) 0.7232(14) 0.16508(18) 0.035(2) Uani 1 1 d . . . . .
C8 C -0.466(2) 0.7483(18) 0.1973(2) 0.052(3) Uani 1 1 d . . . . .
C9 C -0.105(2) 0.797(3) 0.1909(2) 0.068(5) Uani 1 1 d . . . . .
H9A H -0.018060 0.786233 0.179127 0.102 Uiso 1 1 calc R U . . .
H9B H -0.065342 0.725892 0.202000 0.102 Uiso 1 1 calc R U . . .
H9C H -0.099417 0.902946 0.196139 0.102 Uiso 1 1 calc R U . . .
C10 C -0.6933(18) 0.6479(15) 0.14983(19) 0.041(3) Uani 1 1 d . . . . .
H10A H -0.750714 0.548039 0.153205 0.061 Uiso 1 1 calc R U . . .
H10B H -0.626039 0.640450 0.136565 0.061 Uiso 1 1 calc R U . . .
H10C H -0.795726 0.725730 0.148703 0.061 Uiso 1 1 calc R U . . .
C11 C -0.461(2) 0.765(3) 0.2207(3) 0.072(5) Uani 1 1 d . . . . .
C12 C -0.647(2) 0.762(2) 0.2326(3) 0.062(4) Uani 1 1 d . . . . .
C13 C -0.634(3) 0.774(3) 0.2553(3) 0.071(5) Uani 1 1 d . . . . .
C14 C 0.2403(19) 0.7772(16) 0.0881(2) 0.046(3) Uani 1 1 d . . . . .
H14A H 0.314493 0.810722 0.100579 0.055 Uiso 1 1 calc R U . . .
H14B H 0.179459 0.868290 0.081436 0.055 Uiso 1 1 calc R U . . .
C15 C 0.370(2) 0.6935(17) 0.0730(2) 0.048(3) Uani 1 1 d . . . . .
H15A H 0.290564 0.656038 0.061070 0.057 Uiso 1 1 calc R U . . .
H15B H 0.427846 0.602723 0.080012 0.057 Uiso 1 1 calc R U . . .
C16 C 0.536(2) 0.7974(17) 0.0646(2) 0.047(3) Uani 1 1 d . . . . .
H16A H 0.479469 0.889448 0.057797 0.056 Uiso 1 1 calc R U . . .
H16B H 0.618849 0.832506 0.076412 0.056 Uiso 1 1 calc R U . . .
C17 C 0.659(2) 0.7107(16) 0.0492(2) 0.047(3) Uani 1 1 d . . . . .
H17A H 0.575569 0.677842 0.037331 0.056 Uiso 1 1 calc R U . . .
H17B H 0.710417 0.616514 0.055970 0.056 Uiso 1 1 calc R U . . .
C18 C 0.833(2) 0.8040(17) 0.0405(2) 0.047(3) Uani 1 1 d . . . . .
H18A H 0.783720 0.900385 0.034104 0.056 Uiso 1 1 calc R U . . .
H18B H 0.921320 0.832562 0.052131 0.056 Uiso 1 1 calc R U . . .
C19 C 0.9475(18) 0.7159(16) 0.02434(19) 0.042(3) Uani 1 1 d . . . . .
H19A H 0.858351 0.685355 0.012854 0.050 Uiso 1 1 calc R U . . .
H19B H 0.998739 0.620562 0.030812 0.050 Uiso 1 1 calc R U . . .
C20 C 1.1178(18) 0.8070(17) 0.0152(2) 0.044(3) Uani 1 1 d . . . . .
H20A H 1.205924 0.839355 0.026649 0.053 Uiso 1 1 calc R U . . .
H20B H 1.066537 0.901302 0.008400 0.053 Uiso 1 1 calc R U . . .
C21 C 1.235(2) 0.7144(17) -0.0009(2) 0.048(3) Uani 1 1 d . . . . .
H21A H 1.286363 0.619908 0.005784 0.057 Uiso 1 1 calc R U . . .
H21B H 1.147664 0.682642 -0.012488 0.057 Uiso 1 1 calc R U . . .
C22 C 1.4022(19) 0.8043(15) -0.0097(2) 0.042(3) Uani 1 1 d . . . . .
H22A H 1.487615 0.837990 0.001922 0.050 Uiso 1 1 calc R U . . .
H22B H 1.350157 0.897976 -0.016582 0.050 Uiso 1 1 calc R U . . .
C23 C 1.527(2) 0.7135(18) -0.0258(2) 0.050(3) Uani 1 1 d . . . . .
H23A H 1.583493 0.621708 -0.018862 0.060 Uiso 1 1 calc R U . . .
H23B H 1.441733 0.677100 -0.037287 0.060 Uiso 1 1 calc R U . . .
C24 C 1.689(2) 0.8070(16) -0.0348(2) 0.047(3) Uani 1 1 d . . . . .
H24A H 1.775167 0.842833 -0.023387 0.056 Uiso 1 1 calc R U . . .
H24B H 1.632963 0.899122 -0.041737 0.056 Uiso 1 1 calc R U . . .
C25 C 1.811(2) 0.7159(19) -0.0509(2) 0.050(3) Uani 1 1 d . . . . .
H25A H 1.859047 0.619822 -0.044305 0.060 Uiso 1 1 calc R U . . .
H25B H 1.727193 0.687220 -0.062877 0.060 Uiso 1 1 calc R U . . .
C26 C 1.983(2) 0.8098(18) -0.0585(2) 0.051(3) Uani 1 1 d . . . . .
H26A H 2.068464 0.836731 -0.046552 0.061 Uiso 1 1 calc R U . . .
H26B H 1.935440 0.906791 -0.064846 0.061 Uiso 1 1 calc R U . . .
C27 C 2.104(2) 0.719(2) -0.0750(3) 0.062(4) Uani 1 1 d . . . . .
H27A H 2.019321 0.689898 -0.086713 0.093 Uiso 1 1 calc R U . . .
H27B H 2.158519 0.626235 -0.068529 0.093 Uiso 1 1 calc R U . . .
H27C H 2.208997 0.784491 -0.079961 0.093 Uiso 1 1 calc R U . . .
F1 F -0.3716(15) 0.9100(14) 0.22433(14) 0.079(3) Uani 1 1 d . . . . .
F2 F -0.3391(17) 0.6561(18) 0.22982(17) 0.103(4) Uani 1 1 d . . . . .
F3 F -0.7509(15) 0.8704(13) 0.22275(14) 0.070(3) Uani 1 1 d . . . . .
F4 F -0.7255(17) 0.6209(13) 0.22771(14) 0.078(3) Uani 1 1 d . . . . .
F5 F -0.556(2) 0.9078(17) 0.26093(15) 0.104(5) Uani 1 1 d . . . . .
F6 F -0.8256(16) 0.7860(19) 0.26180(18) 0.103(4) Uani 1 1 d . . . . .
F7 F -0.5537(19) 0.6599(18) 0.26511(15) 0.099(4) Uani 1 1 d . . . . .
N1 N -0.3058(14) 0.7610(14) 0.18407(15) 0.041(2) Uani 1 1 d . . . . .
N2 N -0.5562(14) 0.6918(12) 0.16614(15) 0.036(2) Uani 1 1 d . . . . .
N3 N -0.6200(14) 0.7080(13) 0.18610(16) 0.039(2) Uani 1 1 d . . . . .
O1 O 0.0912(14) 0.6599(12) 0.09357(14) 0.053(2) Uani 1 1 d . . . . .
C28 C 0.4482(19) 0.2362(16) 0.38972(18) 0.041(3) Uani 1 1 d . . . . .
C29 C 0.4134(16) 0.3806(15) 0.38106(19) 0.037(3) Uani 1 1 d . . . . .
H29 H 0.470429 0.468862 0.387353 0.045 Uiso 1 1 calc R U . . .
C30 C 0.2940(18) 0.3986(15) 0.3630(2) 0.042(3) Uani 1 1 d . . . . .
H30 H 0.270770 0.497055 0.357009 0.050 Uiso 1 1 calc R U . . .
C31 C 0.2103(15) 0.2624(14) 0.35407(17) 0.033(2) Uani 1 1 d . . . . .
C32 C 0.238(2) 0.1184(14) 0.3635(2) 0.046(3) Uani 1 1 d . . . . .
H32 H 0.173902 0.030460 0.358022 0.055 Uiso 1 1 calc R U . . .
C33 C 0.3596(18) 0.1032(16) 0.3808(2) 0.047(3) Uani 1 1 d . . . . .
H33 H 0.383415 0.004523 0.386646 0.057 Uiso 1 1 calc R U . . .
C34 C 0.0844(15) 0.2745(14) 0.33533(17) 0.033(2) Uani 1 1 d . . . . .
C35 C -0.0322(18) 0.3098(17) 0.3038(2) 0.046(3) Uani 1 1 d . . . . .
C36 C 0.335(2) 0.358(2) 0.3090(3) 0.062(4) Uani 1 1 d . . . . .
H36A H 0.341239 0.469771 0.307101 0.093 Uiso 1 1 calc R U . . .
H36B H 0.364699 0.306633 0.295868 0.093 Uiso 1 1 calc R U . . .
H36C H 0.430641 0.326869 0.319681 0.093 Uiso 1 1 calc R U . . .
C37 C -0.237(2) 0.1975(17) 0.3511(2) 0.050(3) Uani 1 1 d . . . . .
H37A H -0.334302 0.278162 0.352863 0.075 Uiso 1 1 calc R U . . .
H37B H -0.163652 0.183472 0.364111 0.075 Uiso 1 1 calc R U . . .
H37C H -0.301247 0.100744 0.347256 0.075 Uiso 1 1 calc R U . . .
C38 C -0.061(3) 0.352(2) 0.2812(2) 0.073(5) Uani 1 1 d . . . . .
C39 C -0.045(4) 0.214(3) 0.2665(3) 0.091(7) Uani 1 1 d . . . . .
C40 C -0.090(6) 0.250(4) 0.2428(4) 0.121(11) Uani 1 1 d . . . . .
C41 C 0.7111(18) 0.3247(17) 0.41207(19) 0.045(3) Uani 1 1 d . . . . .
H41A H 0.652625 0.416980 0.418454 0.054 Uiso 1 1 calc R U . . .
H41B H 0.782031 0.356528 0.399527 0.054 Uiso 1 1 calc R U . . .
C42 C 0.848(2) 0.2433(18) 0.4277(2) 0.049(3) Uani 1 1 d . . . . .
H42A H 0.773287 0.211127 0.439930 0.059 Uiso 1 1 calc R U . . .
H42B H 0.900489 0.149356 0.421098 0.059 Uiso 1 1 calc R U . . .
C43 C 1.0162(17) 0.3460(17) 0.4348(2) 0.043(3) Uani 1 1 d . . . . .
H43A H 0.964901 0.440759 0.441260 0.051 Uiso 1 1 calc R U . . .
H43B H 1.093911 0.376215 0.422677 0.051 Uiso 1 1 calc R U . . .
C44 C 1.1463(17) 0.2592(16) 0.4508(2) 0.045(3) Uani 1 1 d . . . . .
H44A H 1.064410 0.224581 0.462357 0.054 Uiso 1 1 calc R U . . .
H44B H 1.198076 0.166072 0.443947 0.054 Uiso 1 1 calc R U . . .
C45 C 1.3183(16) 0.3519(16) 0.45996(19) 0.039(3) Uani 1 1 d . . . . .
H45A H 1.402497 0.384611 0.448457 0.047 Uiso 1 1 calc R U . . .
H45B H 1.267431 0.446102 0.466610 0.047 Uiso 1 1 calc R U . . .
C46 C 1.4408(18) 0.2640(17) 0.47591(19) 0.042(3) Uani 1 1 d . . . . .
H46A H 1.356380 0.232250 0.487444 0.050 Uiso 1 1 calc R U . . .
H46B H 1.489887 0.169247 0.469273 0.050 Uiso 1 1 calc R U . . .
C47 C 1.6101(16) 0.3516(15) 0.48489(19) 0.037(3) Uani 1 1 d . . . . .
H47A H 1.561359 0.447146 0.491358 0.044 Uiso 1 1 calc R U . . .
H47B H 1.695771 0.381912 0.473397 0.044 Uiso 1 1 calc R U . . .
C48 C 1.7309(18) 0.2627(17) 0.5012(2) 0.044(3) Uani 1 1 d . . . . .
H48A H 1.777090 0.165674 0.494910 0.052 Uiso 1 1 calc R U . . .
H48B H 1.646802 0.235290 0.512963 0.052 Uiso 1 1 calc R U . . .
C49 C 1.9095(17) 0.3552(17) 0.5098(2) 0.043(3) Uani 1 1 d . . . . .
H49A H 1.994216 0.382707 0.498048 0.051 Uiso 1 1 calc R U . . .
H49B H 1.863946 0.452000 0.516164 0.051 Uiso 1 1 calc R U . . .
C50 C 2.0277(19) 0.2625(16) 0.5260(2) 0.046(3) Uani 1 1 d . . . . .
H50A H 1.942459 0.233810 0.537630 0.055 Uiso 1 1 calc R U . . .
H50B H 2.074682 0.166423 0.519553 0.055 Uiso 1 1 calc R U . . .
C51 C 2.2022(18) 0.3542(17) 0.5347(2) 0.045(3) Uani 1 1 d . . . . .
H51A H 2.286944 0.383013 0.523053 0.054 Uiso 1 1 calc R U . . .
H51B H 2.154816 0.450340 0.541120 0.054 Uiso 1 1 calc R U . . .
C52 C 2.3213(19) 0.2643(17) 0.5509(2) 0.045(3) Uani 1 1 d . . . . .
H52A H 2.365318 0.166554 0.544576 0.054 Uiso 1 1 calc R U . . .
H52B H 2.237740 0.238355 0.562719 0.054 Uiso 1 1 calc R U . . .
C53 C 2.498(2) 0.3542(19) 0.5589(2) 0.056(4) Uani 1 1 d . . . . .
H53A H 2.579060 0.382338 0.546923 0.068 Uiso 1 1 calc R U . . .
H53B H 2.452984 0.450955 0.565347 0.068 Uiso 1 1 calc R U . . .
C54 C 2.623(2) 0.270(2) 0.5745(2) 0.067(5) Uani 1 1 d . . . . .
H54A H 2.660330 0.170271 0.568717 0.100 Uiso 1 1 calc R U . . .
H54B H 2.549754 0.254040 0.587238 0.100 Uiso 1 1 calc R U . . .
H54C H 2.738824 0.330995 0.577612 0.100 Uiso 1 1 calc R U . . .
F8 F 0.0582(15) 0.4640(11) 0.27576(13) 0.067(3) Uani 1 1 d . . . . .
F9 F -0.2651(16) 0.4024(15) 0.27759(18) 0.088(3) Uani 1 1 d . . . . .
F10 F 0.1447(19) 0.178(2) 0.2695(2) 0.117(5) Uani 1 1 d . . . . .
F11 F -0.178(3) 0.1093(16) 0.27199(17) 0.144(8) Uani 1 1 d . . . . .
F12 F -0.024(4) 0.377(2) 0.2363(2) 0.167(9) Uani 1 1 d . . . . .
F13 F -0.271(4) 0.273(3) 0.2405(3) 0.171(9) Uani 1 1 d . . . . .
F14 F -0.037(3) 0.1295(19) 0.23242(19) 0.124(5) Uani 1 1 d . . . . .
N4 N 0.1367(14) 0.3131(13) 0.31574(17) 0.041(2) Uani 1 1 d . . . . .
N5 N -0.1827(15) 0.2649(14) 0.31493(17) 0.046(3) Uani 1 1 d . . . . .
N6 N -0.1029(14) 0.2428(13) 0.33440(15) 0.037(2) Uani 1 1 d . . . . .
O2 O 0.5615(14) 0.2110(12) 0.40671(14) 0.050(2) Uani 1 1 d . . . . .
C57 C 0.486(3) 1.206(2) 0.1161(2) 0.063(4) Uani 1 1 d . . . . .
C58 C 0.326(4) 1.230(3) 0.1942(3) 0.095(7) Uani 1 1 d . . . . .
F21 F 0.6683(15) 1.1904(13) 0.12121(16) 0.076(3) Uani 1 1 d . . . . .
F22 F 0.4497(19) 1.3457(10) 0.10958(15) 0.079(3) Uani 1 1 d . . . . .
F23 F 0.446(2) 1.1033(13) 0.10064(16) 0.098(4) Uani 1 1 d . . . . .
F24 F 0.206(2) 1.3584(16) 0.1935(2) 0.113(5) Uani 1 1 d . . . . .
F25 F 0.1938(19) 1.1162(15) 0.18878(19) 0.100(4) Uani 1 1 d . . . . .
F26 F 0.381(3) 1.2119(19) 0.21359(17) 0.130(6) Uani 1 1 d . . . . .
N8 N 0.410(2) 1.2811(14) 0.15489(19) 0.061(3) Uani 1 1 d . . . . .
O7 O 0.1450(16) 1.1965(17) 0.1319(3) 0.092(4) Uani 1 1 d . . . . .
O8 O 0.3735(18) 0.9963(12) 0.14307(19) 0.065(3) Uani 1 1 d . . . . .
O9 O 0.6249(17) 1.3807(14) 0.18219(19) 0.071(3) Uani 1 1 d . . . . .
O10 O 0.620(3) 1.0948(15) 0.1777(2) 0.091(4) Uani 1 1 d . . . . .
S3 S 0.3318(5) 1.1562(4) 0.13859(6) 0.0537(9) Uani 1 1 d . . . . .
S4 S 0.5177(7) 1.2440(4) 0.17600(6) 0.0600(10) Uani 1 1 d . . . . .
C55 C 0.769(3) 0.788(3) 0.3050(2) 0.076(5) Uani 1 1 d . . . . .
C56 C 0.944(3) 0.7474(17) 0.3836(2) 0.058(4) Uani 1 1 d . . . . .
F15 F 0.6520(16) 0.9072(16) 0.30630(18) 0.086(3) Uani 1 1 d . . . . .
F16 F 0.818(2) 0.7636(16) 0.28634(15) 0.095(4) Uani 1 1 d . . . . .
F17 F 0.6464(18) 0.6619(14) 0.31025(16) 0.086(3) Uani 1 1 d . . . . .
F18 F 0.9202(18) 0.8915(12) 0.39088(15) 0.077(3) Uani 1 1 d . . . . .
F19 F 0.922(2) 0.6523(14) 0.39951(15) 0.097(4) Uani 1 1 d . . . . .
F20 F 1.1346(14) 0.7389(12) 0.37894(15) 0.071(3) Uani 1 1 d . . . . .
N7 N 0.860(2) 0.8270(13) 0.34513(18) 0.054(3) Uani 1 1 d . . . . .
O3 O 1.0597(19) 0.9357(13) 0.31803(18) 0.070(3) Uani 1 1 d . . . . .
O4 O 1.0769(15) 0.6542(13) 0.32258(19) 0.067(3) Uani 1 1 d . . . . .
O5 O 0.6026(17) 0.7418(12) 0.3692(2) 0.070(2) Uani 1 1 d . . . . .
O6 O 0.8288(18) 0.5426(12) 0.3571(2) 0.070(2) Uani 1 1 d . . . . .
S1 S 0.9679(6) 0.7960(4) 0.32396(6) 0.0520(8) Uani 1 1 d . . . . .
S2 S 0.7894(5) 0.7029(4) 0.36140(6) 0.0486(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.388(18) . ?
C1 C6 1.368(18) . ?
C1 O1 1.367(15) . ?
C2 H2 0.9400 . ?
C2 C3 1.381(18) . ?
C3 H3 0.9400 . ?
C3 C4 1.377(18) . ?
C4 C5 1.367(16) . ?
C4 C7 1.500(15) . ?
C5 H5 0.9400 . ?
C5 C6 1.430(18) . ?
C6 H6 0.9400 . ?
C7 N1 1.314(15) . ?
C7 N2 1.323(15) . ?
C8 C11 1.50(2) . ?
C8 N1 1.395(16) . ?
C8 N3 1.308(18) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C9 N1 1.465(17) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C10 N2 1.438(15) . ?
C11 C12 1.49(2) . ?
C11 F1 1.40(2) . ?
C11 F2 1.38(2) . ?
C12 C13 1.45(2) . ?
C12 F3 1.326(19) . ?
C12 F4 1.361(19) . ?
C13 F5 1.32(2) . ?
C13 F6 1.38(2) . ?
C13 F7 1.28(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 C15 1.502(18) . ?
C14 O1 1.480(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 C16 1.545(18) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 C17 1.504(18) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 C18 1.544(19) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 C19 1.504(18) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C20 1.527(17) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 C21 1.535(19) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 C22 1.493(18) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C23 1.556(18) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 C24 1.488(19) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 C25 1.542(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 C26 1.516(19) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 C27 1.55(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
N2 N3 1.357(13) . ?
C28 C29 1.377(18) . ?
C28 C33 1.410(17) . ?
C28 O2 1.338(14) . ?
C29 H29 0.9400 . ?
C29 C30 1.410(17) . ?
C30 H30 0.9400 . ?
C30 C31 1.417(17) . ?
C31 C32 1.389(17) . ?
C31 C34 1.463(13) . ?
C32 H32 0.9400 . ?
C32 C33 1.372(16) . ?
C33 H33 0.9400 . ?
C34 N4 1.344(15) . ?
C34 N6 1.309(14) . ?
C35 C38 1.492(19) . ?
C35 N4 1.371(14) . ?
C35 N5 1.315(17) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 H36C 0.9700 . ?
C36 N4 1.482(18) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C37 H37C 0.9700 . ?
C37 N6 1.465(16) . ?
C38 C39 1.52(3) . ?
C38 F8 1.32(2) . ?
C38 F9 1.47(2) . ?
C39 C40 1.56(3) . ?
C39 F10 1.34(3) . ?
C39 F11 1.33(2) . ?
C40 F12 1.26(3) . ?
C40 F13 1.26(4) . ?
C40 F14 1.28(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 C42 1.523(18) . ?
C41 O2 1.451(14) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 C43 1.515(17) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 C44 1.532(16) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 C45 1.529(16) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 C46 1.508(16) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 C47 1.487(16) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 C48 1.522(16) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 C49 1.549(16) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 C50 1.528(16) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 C51 1.525(16) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 C52 1.514(17) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 C53 1.518(18) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 C54 1.48(2) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 H54C 0.9700 . ?
N5 N6 1.359(14) . ?
C57 F21 1.29(2) . ?
C57 F22 1.29(2) . ?
C57 F23 1.350(18) . ?
C57 S3 1.840(16) . ?
C58 F24 1.38(3) . ?
C58 F25 1.37(2) . ?
C58 F26 1.29(2) . ?
C58 S4 1.77(2) . ?
N8 S3 1.581(13) . ?
N8 S4 1.554(14) . ?
O7 S3 1.383(12) . ?
O8 S3 1.432(11) . ?
O9 S4 1.437(11) . ?
O10 S4 1.463(14) . ?
C55 F15 1.30(2) . ?
C55 F16 1.258(18) . ?
C55 F17 1.41(2) . ?
C55 S1 1.805(18) . ?
C56 F18 1.334(18) . ?
C56 F19 1.313(17) . ?
C56 F20 1.34(2) . ?
C56 S2 1.791(17) . ?
N7 S1 1.569(13) . ?
N7 S2 1.569(13) . ?
O3 S1 1.410(12) . ?
O4 S1 1.432(10) . ?
O5 S2 1.418(12) . ?
O6 S2 1.432(11) . ?

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
C6 C1 C2 121.5(12) . . ?
O1 C1 C2 114.4(12) . . ?
O1 C1 C6 124.0(12) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 C1 120.9(13) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 121.2 . . ?
C4 C3 C2 117.7(12) . . ?
C4 C3 H3 121.2 . . ?
C3 C4 C7 116.7(11) . . ?
C5 C4 C3 122.7(11) . . ?
C5 C4 C7 120.5(11) . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(11) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C5 117.8(12) . . ?
C1 C6 H6 121.1 . . ?
C5 C6 H6 121.1 . . ?
N1 C7 C4 126.8(10) . . ?
N1 C7 N2 107.5(10) . . ?
N2 C7 C4 125.7(10) . . ?
N1 C8 C11 126.0(13) . . ?
N3 C8 C11 124.8(12) . . ?
N3 C8 N1 109.0(11) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
C12 C11 C8 120.0(13) . . ?
F1 C11 C8 104.6(15) . . ?
F1 C11 C12 108.0(14) . . ?
F2 C11 C8 110.8(15) . . ?
F2 C11 C12 106.7(16) . . ?
F2 C11 F1 106.0(13) . . ?
C13 C12 C11 117.9(14) . . ?
F3 C12 C11 101.7(14) . . ?
F3 C12 C13 116.3(16) . . ?
F3 C12 F4 108.1(12) . . ?
F4 C12 C11 103.9(15) . . ?
F4 C12 C13 107.9(14) . . ?
F5 C13 C12 110.5(14) . . ?
F5 C13 F6 103.6(17) . . ?
F6 C13 C12 105.3(14) . . ?
F7 C13 C12 116.8(18) . . ?
F7 C13 F5 111.4(16) . . ?
F7 C13 F6 108.2(14) . . ?
H14A C14 H14B 109.0 . . ?
C15 C14 H14A 111.0 . . ?
C15 C14 H14B 111.0 . . ?
O1 C14 H14A 111.0 . . ?
O1 C14 H14B 111.0 . . ?
O1 C14 C15 104.0(10) . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C14 C15 C16 112.8(11) . . ?
H15A C15 H15B 107.8 . . ?
C16 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C15 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 C15 111.2(11) . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C16 C17 H17A 108.6 . . ?
C16 C17 H17B 108.6 . . ?
C16 C17 C18 114.8(12) . . ?
H17A C17 H17B 107.5 . . ?
C18 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
C17 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
H18A C18 H18B 107.8 . . ?
C19 C18 C17 113.2(11) . . ?
C19 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
C18 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
C18 C19 C20 114.2(11) . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.6(11) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 C20 113.1(12) . . ?
C22 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
C21 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C21 C22 C23 114.7(11) . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 H22A 108.6 . . ?
C23 C22 H22B 108.6 . . ?
C22 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 C22 113.7(12) . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
C23 C24 C25 113.2(12) . . ?
H24A C24 H24B 107.8 . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
C24 C25 H25A 109.2 . . ?
C24 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 C24 112.0(12) . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
C25 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
C25 C26 C27 112.0(12) . . ?
H26A C26 H26B 107.9 . . ?
C27 C26 H26A 109.2 . . ?
C27 C26 H26B 109.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C7 N1 C8 107.0(11) . . ?
C7 N1 C9 127.5(11) . . ?
C8 N1 C9 125.3(11) . . ?
C7 N2 C10 130.0(10) . . ?
C7 N2 N3 110.8(9) . . ?
N3 N2 C10 119.2(10) . . ?
C8 N3 N2 105.5(9) . . ?
C1 O1 C14 117.7(10) . . ?
C29 C28 C33 120.0(11) . . ?
O2 C28 C29 124.3(11) . . ?
O2 C28 C33 115.7(11) . . ?
C28 C29 H29 119.3 . . ?
C28 C29 C30 121.3(11) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 H30 121.3 . . ?
C29 C30 C31 117.4(12) . . ?
C31 C30 H30 121.3 . . ?
C30 C31 C34 119.7(11) . . ?
C32 C31 C30 120.8(10) . . ?
C32 C31 C34 119.5(10) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(11) . . ?
C33 C32 H32 119.7 . . ?
C28 C33 H33 120.1 . . ?
C32 C33 C28 119.7(12) . . ?
C32 C33 H33 120.1 . . ?
N4 C34 C31 127.7(10) . . ?
N6 C34 C31 125.7(11) . . ?
N6 C34 N4 106.5(9) . . ?
N4 C35 C38 128.7(14) . . ?
N5 C35 C38 119.7(12) . . ?
N5 C35 N4 111.6(11) . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C36 H36A 109.5 . . ?
N4 C36 H36B 109.5 . . ?
N4 C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N6 C37 H37A 109.5 . . ?
N6 C37 H37B 109.5 . . ?
N6 C37 H37C 109.5 . . ?
C35 C38 C39 113.5(16) . . ?
F8 C38 C35 111.1(14) . . ?
F8 C38 C39 110.8(16) . . ?
F8 C38 F9 109.2(15) . . ?
F9 C38 C35 109.6(15) . . ?
F9 C38 C39 102.4(16) . . ?
C38 C39 C40 115(2) . . ?
F10 C39 C38 100.0(16) . . ?
F10 C39 C40 111(2) . . ?
F11 C39 C38 107.9(19) . . ?
F11 C39 C40 105.1(18) . . ?
F11 C39 F10 118(2) . . ?
F12 C40 C39 115(2) . . ?
F12 C40 F13 100(4) . . ?
F12 C40 F14 115(2) . . ?
F13 C40 C39 109(2) . . ?
F13 C40 F14 111(3) . . ?
F14 C40 C39 107(3) . . ?
H41A C41 H41B 108.8 . . ?
C42 C41 H41A 110.6 . . ?
C42 C41 H41B 110.6 . . ?
O2 C41 H41A 110.6 . . ?
O2 C41 H41B 110.6 . . ?
O2 C41 C42 105.5(11) . . ?
C41 C42 H42A 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C43 C42 C41 112.6(12) . . ?
C43 C42 H42A 109.1 . . ?
C43 C42 H42B 109.1 . . ?
C42 C43 H43A 109.6 . . ?
C42 C43 H43B 109.6 . . ?
C42 C43 C44 110.2(11) . . ?
H43A C43 H43B 108.1 . . ?
C44 C43 H43A 109.6 . . ?
C44 C43 H43B 109.6 . . ?
C43 C44 H44A 108.3 . . ?
C43 C44 H44B 108.3 . . ?
H44A C44 H44B 107.4 . . ?
C45 C44 C43 115.7(11) . . ?
C45 C44 H44A 108.3 . . ?
C45 C44 H44B 108.3 . . ?
C44 C45 H45A 108.7 . . ?
C44 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
C46 C45 C44 114.3(11) . . ?
C46 C45 H45A 108.7 . . ?
C46 C45 H45B 108.7 . . ?
C45 C46 H46A 108.5 . . ?
C45 C46 H46B 108.5 . . ?
H46A C46 H46B 107.5 . . ?
C47 C46 C45 115.2(11) . . ?
C47 C46 H46A 108.5 . . ?
C47 C46 H46B 108.5 . . ?
C46 C47 H47A 108.6 . . ?
C46 C47 H47B 108.6 . . ?
C46 C47 C48 114.7(11) . . ?
H47A C47 H47B 107.6 . . ?
C48 C47 H47A 108.6 . . ?
C48 C47 H47B 108.6 . . ?
C47 C48 H48A 108.9 . . ?
C47 C48 H48B 108.9 . . ?
C47 C48 C49 113.4(11) . . ?
H48A C48 H48B 107.7 . . ?
C49 C48 H48A 108.9 . . ?
C49 C48 H48B 108.9 . . ?
C48 C49 H49A 109.2 . . ?
C48 C49 H49B 109.2 . . ?
H49A C49 H49B 107.9 . . ?
C50 C49 C48 112.1(11) . . ?
C50 C49 H49A 109.2 . . ?
C50 C49 H49B 109.2 . . ?
C49 C50 H50A 109.2 . . ?
C49 C50 H50B 109.2 . . ?
H50A C50 H50B 107.9 . . ?
C51 C50 C49 112.2(11) . . ?
C51 C50 H50A 109.2 . . ?
C51 C50 H50B 109.2 . . ?
C50 C51 H51A 109.0 . . ?
C50 C51 H51B 109.0 . . ?
H51A C51 H51B 107.8 . . ?
C52 C51 C50 113.0(11) . . ?
C52 C51 H51A 109.0 . . ?
C52 C51 H51B 109.0 . . ?
C51 C52 H52A 109.0 . . ?
C51 C52 H52B 109.0 . . ?
C51 C52 C53 112.8(12) . . ?
H52A C52 H52B 107.8 . . ?
C53 C52 H52A 109.0 . . ?
C53 C52 H52B 109.0 . . ?
C52 C53 H53A 108.5 . . ?
C52 C53 H53B 108.5 . . ?
H53A C53 H53B 107.5 . . ?
C54 C53 C52 115.0(14) . . ?
C54 C53 H53A 108.5 . . ?
C54 C53 H53B 108.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C34 N4 C35 105.9(10) . . ?
C34 N4 C36 126.3(10) . . ?
C35 N4 C36 127.8(11) . . ?
C35 N5 N6 103.0(9) . . ?
C34 N6 C37 130.1(10) . . ?
C34 N6 N5 112.9(10) . . ?
N5 N6 C37 116.8(10) . . ?
C28 O2 C41 118.5(10) . . ?
F21 C57 F22 110.9(15) . . ?
F21 C57 F23 107.4(15) . . ?
F21 C57 S3 110.2(12) . . ?
F22 C57 F23 109.6(14) . . ?
F22 C57 S3 111.0(12) . . ?
F23 C57 S3 107.6(12) . . ?
F24 C58 S4 111.7(14) . . ?
F25 C58 F24 100(2) . . ?
F25 C58 S4 112.1(14) . . ?
F26 C58 F24 106.9(18) . . ?
F26 C58 F25 109.9(18) . . ?
F26 C58 S4 115(2) . . ?
S4 N8 S3 125.4(9) . . ?
N8 S3 C57 99.1(7) . . ?
O7 S3 C57 103.9(9) . . ?
O7 S3 N8 109.5(9) . . ?
O7 S3 O8 118.8(8) . . ?
O8 S3 C57 105.3(8) . . ?
O8 S3 N8 117.2(7) . . ?
N8 S4 C58 103.7(11) . . ?
O9 S4 C58 104.9(9) . . ?
O9 S4 N8 107.5(7) . . ?
O9 S4 O10 117.2(8) . . ?
O10 S4 C58 104.3(10) . . ?
O10 S4 N8 117.5(7) . . ?
F15 C55 F17 102.9(15) . . ?
F15 C55 S1 112.5(13) . . ?
F16 C55 F15 111.4(17) . . ?
F16 C55 F17 105.3(15) . . ?
F16 C55 S1 115.2(15) . . ?
F17 C55 S1 108.4(13) . . ?
F18 C56 F20 104.6(13) . . ?
F18 C56 S2 113.6(12) . . ?
F19 C56 F18 107.0(13) . . ?
F19 C56 F20 104.9(14) . . ?
F19 C56 S2 113.8(12) . . ?
F20 C56 S2 112.2(11) . . ?
S2 N7 S1 127.3(8) . . ?
N7 S1 C55 102.8(8) . . ?
O3 S1 C55 100.8(8) . . ?
O3 S1 N7 107.6(7) . . ?
O3 S1 O4 118.3(7) . . ?
O4 S1 C55 108.3(9) . . ?
O4 S1 N7 116.7(7) . . ?
N7 S2 C56 101.0(7) . . ?
O5 S2 C56 101.3(8) . . ?
O5 S2 N7 111.1(7) . . ?
O5 S2 O6 117.9(7) . . ?
O6 S2 C56 104.3(7) . . ?
O6 S2 N7 117.8(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -4(2) . . . . ?
C2 C1 C6 C5 -3(2) . . . . ?
C2 C1 O1 C14 -157.9(12) . . . . ?
C2 C3 C4 C5 5(2) . . . . ?
C2 C3 C4 C7 -177.1(12) . . . . ?
C3 C4 C5 C6 -4.2(18) . . . . ?
C3 C4 C7 N1 114.8(15) . . . . ?
C3 C4 C7 N2 -64.2(16) . . . . ?
C4 C5 C6 C1 3.1(18) . . . . ?
C4 C7 N1 C8 -177.9(12) . . . . ?
C4 C7 N1 C9 -3(2) . . . . ?
C4 C7 N2 C10 -2(2) . . . . ?
C4 C7 N2 N3 178.8(11) . . . . ?
C5 C4 C7 N1 -66.9(17) . . . . ?
C5 C4 C7 N2 114.1(14) . . . . ?
C6 C1 C2 C3 3(2) . . . . ?
C6 C1 O1 C14 18(2) . . . . ?
C7 C4 C5 C6 177.6(10) . . . . ?
C7 N2 N3 C8 -0.7(14) . . . . ?
C8 C11 C12 C13 178.0(18) . . . . ?
C8 C11 C12 F3 -54(2) . . . . ?
C8 C11 C12 F4 59(2) . . . . ?
C10 N2 N3 C8 -179.8(12) . . . . ?
C11 C8 N1 C7 173.8(16) . . . . ?
C11 C8 N1 C9 -1(3) . . . . ?
C11 C8 N3 N2 -174.2(15) . . . . ?
C11 C12 C13 F5 62(2) . . . . ?
C11 C12 C13 F6 173.1(17) . . . . ?
C11 C12 C13 F7 -67(2) . . . . ?
C14 C15 C16 C17 -178.5(12) . . . . ?
C15 C14 O1 C1 166.1(12) . . . . ?
C15 C16 C17 C18 -178.2(12) . . . . ?
C16 C17 C18 C19 -177.4(11) . . . . ?
C17 C18 C19 C20 178.8(11) . . . . ?
C18 C19 C20 C21 178.9(11) . . . . ?
C19 C20 C21 C22 -179.7(11) . . . . ?
C20 C21 C22 C23 178.9(11) . . . . ?
C21 C22 C23 C24 178.2(12) . . . . ?
C22 C23 C24 C25 -179.7(11) . . . . ?
C23 C24 C25 C26 -175.7(12) . . . . ?
C24 C25 C26 C27 -178.9(12) . . . . ?
F1 C11 C12 C13 -62(2) . . . . ?
F1 C11 C12 F3 66.0(16) . . . . ?
F1 C11 C12 F4 178.3(13) . . . . ?
F2 C11 C12 C13 51(2) . . . . ?
F2 C11 C12 F3 179.5(13) . . . . ?
F2 C11 C12 F4 -68.2(16) . . . . ?
F3 C12 C13 F5 -59(2) . . . . ?
F3 C12 C13 F6 52(2) . . . . ?
F3 C12 C13 F7 172.0(14) . . . . ?
F4 C12 C13 F5 179.1(15) . . . . ?
F4 C12 C13 F6 -69.7(19) . . . . ?
F4 C12 C13 F7 50(2) . . . . ?
N1 C7 N2 C10 178.6(12) . . . . ?
N1 C7 N2 N3 -0.4(14) . . . . ?
N1 C8 C11 C12 174.9(16) . . . . ?
N1 C8 C11 F1 54(2) . . . . ?
N1 C8 C11 F2 -60(2) . . . . ?
N1 C8 N3 N2 1.5(15) . . . . ?
N2 C7 N1 C8 1.3(15) . . . . ?
N2 C7 N1 C9 176.5(15) . . . . ?
N3 C8 C11 C12 -10(3) . . . . ?
N3 C8 C11 F1 -131.4(15) . . . . ?
N3 C8 C11 F2 114.8(17) . . . . ?
N3 C8 N1 C7 -1.8(16) . . . . ?
N3 C8 N1 C9 -177.1(15) . . . . ?
O1 C1 C2 C3 179.4(13) . . . . ?
O1 C1 C6 C5 -178.4(12) . . . . ?
O1 C14 C15 C16 178.6(11) . . . . ?
C28 C29 C30 C31 0.3(19) . . . . ?
C29 C28 C33 C32 0(2) . . . . ?
C29 C28 O2 C41 -23(2) . . . . ?
C29 C30 C31 C32 2.9(19) . . . . ?
C29 C30 C31 C34 179.7(11) . . . . ?
C30 C31 C32 C33 -5(2) . . . . ?
C30 C31 C34 N4 68.8(18) . . . . ?
C30 C31 C34 N6 -114.2(14) . . . . ?
C31 C32 C33 C28 3(2) . . . . ?
C31 C34 N4 C35 -179.5(13) . . . . ?
C31 C34 N4 C36 -2(2) . . . . ?
C31 C34 N6 C37 4(2) . . . . ?
C31 C34 N6 N5 179.9(12) . . . . ?
C32 C31 C34 N4 -114.4(15) . . . . ?
C32 C31 C34 N6 62.6(18) . . . . ?
C33 C28 C29 C30 -2(2) . . . . ?
C33 C28 O2 C41 157.4(12) . . . . ?
C34 C31 C32 C33 178.4(13) . . . . ?
C35 C38 C39 C40 175(2) . . . . ?
C35 C38 C39 F10 -65(2) . . . . ?
C35 C38 C39 F11 58(2) . . . . ?
C35 N5 N6 C34 1.0(15) . . . . ?
C35 N5 N6 C37 177.5(12) . . . . ?
C38 C35 N4 C34 176.2(16) . . . . ?
C38 C35 N4 C36 -1(3) . . . . ?
C38 C35 N5 N6 -177.9(14) . . . . ?
C38 C39 C40 F12 40(4) . . . . ?
C38 C39 C40 F13 -71(3) . . . . ?
C38 C39 C40 F14 169(2) . . . . ?
C41 C42 C43 C44 178.9(12) . . . . ?
C42 C41 O2 C28 -164.3(12) . . . . ?
C42 C43 C44 C45 -177.8(12) . . . . ?
C43 C44 C45 C46 178.8(11) . . . . ?
C44 C45 C46 C47 179.4(11) . . . . ?
C45 C46 C47 C48 179.1(11) . . . . ?
C46 C47 C48 C49 178.3(11) . . . . ?
C47 C48 C49 C50 -179.8(11) . . . . ?
C48 C49 C50 C51 -179.2(11) . . . . ?
C49 C50 C51 C52 -180.0(12) . . . . ?
C50 C51 C52 C53 178.2(13) . . . . ?
C51 C52 C53 C54 -178.8(13) . . . . ?
F8 C38 C39 C40 -59(3) . . . . ?
F8 C38 C39 F10 60(2) . . . . ?
F8 C38 C39 F11 -175.9(17) . . . . ?
F9 C38 C39 C40 58(2) . . . . ?
F9 C38 C39 F10 176.7(15) . . . . ?
F9 C38 C39 F11 -60(2) . . . . ?
F10 C39 C40 F12 -73(4) . . . . ?
F10 C39 C40 F13 176(3) . . . . ?
F10 C39 C40 F14 56(3) . . . . ?
F11 C39 C40 F12 159(3) . . . . ?
F11 C39 C40 F13 47(3) . . . . ?
F11 C39 C40 F14 -72(3) . . . . ?
N4 C34 N6 C37 -178.6(12) . . . . ?
N4 C34 N6 N5 -2.6(15) . . . . ?
N4 C35 C38 C39 93(2) . . . . ?
N4 C35 C38 F8 -32(3) . . . . ?
N4 C35 C38 F9 -153.2(15) . . . . ?
N4 C35 N5 N6 1.1(15) . . . . ?
N5 C35 C38 C39 -88(2) . . . . ?
N5 C35 C38 F8 146.3(16) . . . . ?
N5 C35 C38 F9 26(2) . . . . ?
N5 C35 N4 C34 -2.6(16) . . . . ?
N5 C35 N4 C36 -179.7(14) . . . . ?
N6 C34 N4 C35 3.1(14) . . . . ?
N6 C34 N4 C36 -179.8(13) . . . . ?
O2 C28 C29 C30 179.2(12) . . . . ?
O2 C28 C33 C32 179.0(13) . . . . ?
O2 C41 C42 C43 179.4(11) . . . . ?
F21 C57 S3 N8 59.9(13) . . . . ?
F21 C57 S3 O7 172.8(12) . . . . ?
F21 C57 S3 O8 -61.7(13) . . . . ?
F22 C57 S3 N8 -63.3(14) . . . . ?
F22 C57 S3 O7 49.5(15) . . . . ?
F22 C57 S3 O8 175.1(12) . . . . ?
F23 C57 S3 N8 176.7(13) . . . . ?
F23 C57 S3 O7 -70.4(15) . . . . ?
F23 C57 S3 O8 55.2(15) . . . . ?
F24 C58 S4 N8 -52.4(18) . . . . ?
F24 C58 S4 O9 60.3(18) . . . . ?
F24 C58 S4 O10 -175.9(16) . . . . ?
F25 C58 S4 N8 59.2(19) . . . . ?
F25 C58 S4 O9 171.8(16) . . . . ?
F25 C58 S4 O10 -64.3(19) . . . . ?
F26 C58 S4 N8 -174.4(15) . . . . ?
F26 C58 S4 O9 -61.7(18) . . . . ?
F26 C58 S4 O10 62.1(18) . . . . ?
S3 N8 S4 C58 -89.9(12) . . . . ?
S3 N8 S4 O9 159.4(10) . . . . ?
S3 N8 S4 O10 24.6(15) . . . . ?
S4 N8 S3 C57 -116.5(11) . . . . ?
S4 N8 S3 O7 135.1(11) . . . . ?
S4 N8 S3 O8 -4.0(14) . . . . ?
F15 C55 S1 N7 50.8(15) . . . . ?
F15 C55 S1 O3 -60.2(14) . . . . ?
F15 C55 S1 O4 174.9(12) . . . . ?
F16 C55 S1 N7 -180.0(16) . . . . ?
F16 C55 S1 O3 69.0(19) . . . . ?
F16 C55 S1 O4 -55.9(19) . . . . ?
F17 C55 S1 N7 -62.3(15) . . . . ?
F17 C55 S1 O3 -173.4(13) . . . . ?
F17 C55 S1 O4 61.7(14) . . . . ?
F18 C56 S2 N7 60.9(13) . . . . ?
F18 C56 S2 O5 -53.4(13) . . . . ?
F18 C56 S2 O6 -176.4(12) . . . . ?
F19 C56 S2 N7 -176.3(12) . . . . ?
F19 C56 S2 O5 69.4(14) . . . . ?
F19 C56 S2 O6 -53.6(15) . . . . ?
F20 C56 S2 N7 -57.4(12) . . . . ?
F20 C56 S2 O5 -171.8(10) . . . . ?
F20 C56 S2 O6 65.3(12) . . . . ?
S1 N7 S2 C56 114.1(11) . . . . ?
S1 N7 S2 O5 -139.1(10) . . . . ?
S1 N7 S2 O6 1.3(14) . . . . ?
S2 N7 S1 C55 93.2(12) . . . . ?
S2 N7 S1 O3 -160.8(10) . . . . ?
S2 N7 S1 O4 -25.0(14) . . . . ?

_olex2_date_sample_data_collection 2017-07-26
_olex2_date_sample_submission    2017-12-05
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id NV2568
_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.736
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.75(7)
2 -0.02(3)
3 0.11(5)
4 0.16(3)
####################################################################### 
# 
# 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_dwb1684
_database_code_depnum_ccdc_archive 'CCDC 2177840'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2017-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H39 F19 N3 O, C F3 O3 S, C3 H6 O'
_chemical_formula_sum            'C37 H45 F22 N3 O5 S'
_chemical_formula_weight         1061.82
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C37 H45 F22 N3 O5 S'
_chemical_oxdiff_usercomment     'Alessio ALR13'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   6.23099(17)
_cell_length_b                   9.1796(4)
_cell_length_c                   39.4248(14)
_cell_angle_alpha                95.565(3)
_cell_angle_beta                 92.989(3)
_cell_angle_gamma                92.795(3)
_cell_volume                     2238.04(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4530
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.5570
_cell_measurement_theta_min      4.5070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0069
4 -1 1 0.1233
0 0 1 0.0069
0 -5 2 0.0344
-1 0 0 0.1366
-3 -4 2 0.1029
0 5 -2 0.0344

_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.014
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
-0.0000 0.0001 -1.0004 -0.0393 -0.0007 -0.0000
4.0008 -1.0004 1.0007 0.0960 -0.9891 -0.1072
0.0000 -0.0001 1.0004 0.0393 0.0007 0.0000
0.0021 -4.9985 2.0032 -0.0021 -0.1906 0.8179
-1.0001 0.0002 0.0001 -0.0182 0.2379 0.0677
-2.9986 -3.9983 2.0029 -0.0405 0.5613 0.8574
-0.0021 4.9985 -2.0032 0.0021 0.1906 -0.8179

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            13942
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.385
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  28.00   1.00    5.00    --    0.00  57.00 120.00   49
  2  ω    -13.00  12.00   1.00    5.00    --    0.00 -37.00 -30.00   25
  3  ω     32.00  69.00   1.00    5.00    --    0.00  57.00 120.00   37
  4  ω    -53.00 -27.00   1.00    5.00    --    0.00 -37.00 -30.00   26
  5  ω     35.00 110.00   1.00   20.00    --   54.00-125.00 -90.00   75
  6  ω    -19.00  51.00   1.00   20.00    --   54.00 -19.00-180.00   70
  7  ω     94.00 122.00   1.00   20.00    --   54.00  57.00-180.00   28
  8  ω     18.00  73.00   1.00   20.00    --   54.00 -57.00 -60.00   55
  9  ω      1.00  68.00   1.00   20.00    --   54.00 -57.00  30.00   67
 10  ω     26.00 103.00   1.00   20.00    --   54.00  77.00 150.00   77
 11  ω     45.00 113.00   1.00   20.00    --   54.00  57.00 -60.00   68
 12  ω     46.00  84.00   1.00   20.00    --  108.00 -50.00  60.00   38
 13  ω     87.00 155.00   1.00   20.00    --  108.00  63.00  30.00   68
 14  ω    100.00 126.00   1.00   20.00    --  108.00 -50.00  60.00   26
 15  ω     62.00 114.00   1.00   20.00    --  108.00-111.00  30.00   52
 16  ω    150.00 176.00   1.00   20.00    --  108.00  63.00 -30.00   26
 17  ω    124.00 151.00   1.00   20.00    --  108.00 178.00 -60.00   27
 18  ω     41.00 176.00   1.00   20.00    --  108.00 -12.00   0.00  135
 19  ω     57.00 109.00   1.00   20.00    --  108.00 178.00 -60.00   52
 20  ω    100.00 126.00   1.00   20.00    --  108.00 -50.00-120.00   26
 21  ω     73.00 120.00   1.00   20.00    --  108.00 -77.00  30.00   47
 22  ω     89.00 115.00   1.00   20.00    --  108.00  63.00 -30.00   26
 23  ω     45.00 133.00   1.00   20.00    --  108.00 -37.00-180.00   88
 24  ω     41.00 125.00   1.00   20.00    --  108.00 -50.00 -30.00   84
 25  ω     40.00  76.00   1.00   20.00    --  108.00 -63.00 120.00   36
 26  ω     97.00 122.00   1.00   20.00    --  108.00 -63.00 120.00   25
 27  ω     63.00  89.00   1.00   20.00    --  108.00 -50.00-120.00   26
 28  ω     49.00 145.00   1.00   20.00    --  108.00 -91.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0182078000
_diffrn_orient_matrix_UB_12      0.0161774000
_diffrn_orient_matrix_UB_13      0.0393198000
_diffrn_orient_matrix_UB_21      -0.2378206000
_diffrn_orient_matrix_UB_22      0.0383080000
_diffrn_orient_matrix_UB_23      0.0006665000
_diffrn_orient_matrix_UB_31      -0.0677147000
_diffrn_orient_matrix_UB_32      -0.1636676000
_diffrn_orient_matrix_UB_33      -0.0000057000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6458
_reflns_number_total             7968
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         7968
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0880
_refine_ls_restrained_S_all      1.146
_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)+(0.0436P)²+15.9904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2198
_refine_ls_wR_factor_ref         0.2274
_refine_special_details          
;
The crystal showed evidence of non-merohedral twinning but a
suitable model could not be obtained using Crysalis.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C33(H33A,H33B,H33C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C)
;
_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
C1 C 1.1166(9) 0.8652(7) 0.67584(15) 0.0268(13) Uani 1 1 d . . . . .
C2 C 1.1318(10) 0.7211(7) 0.68412(15) 0.0281(13) Uani 1 1 d . . . . .
H2 H 1.0518 0.6449 0.6713 0.034 Uiso 1 1 calc R . . . .
C3 C 1.2656(9) 0.6922(6) 0.71139(14) 0.0243(12) Uani 1 1 d . . . . .
H3 H 1.2772 0.5962 0.7166 0.029 Uiso 1 1 calc R . . . .
C4 C 1.3839(9) 0.8062(6) 0.73116(15) 0.0213(12) Uani 1 1 d . . . . .
C5 C 1.3734(9) 0.9499(6) 0.72226(15) 0.0238(12) Uani 1 1 d . . . . .
H5 H 1.4540 1.0260 0.7350 0.029 Uiso 1 1 calc R . . . .
C6 C 1.2428(9) 0.9784(7) 0.69441(16) 0.0265(13) Uani 1 1 d . . . . .
H6 H 1.2392 1.0733 0.6881 0.032 Uiso 1 1 calc R . . . .
C7 C 1.5072(8) 0.7813(6) 0.76235(14) 0.0183(11) Uani 1 1 d . . . . .
C8 C 1.6023(8) 0.7166(6) 0.81206(14) 0.0192(11) Uani 1 1 d . . . . .
C9 C 1.8542(9) 0.9208(7) 0.75423(16) 0.0276(13) Uani 1 1 d . . . . .
H9A H 1.8167 1.0213 0.7556 0.041 Uiso 1 1 calc GR . . . .
H9B H 1.8496 0.8814 0.7307 0.041 Uiso 1 1 calc GR . . . .
H9C H 1.9968 0.9151 0.7643 0.041 Uiso 1 1 calc GR . . . .
C10 C 1.2240(8) 0.6289(6) 0.78827(16) 0.0236(12) Uani 1 1 d . . . . .
H10A H 1.1245 0.6722 0.7733 0.035 Uiso 1 1 calc GR . . . .
H10B H 1.1768 0.6404 0.8111 0.035 Uiso 1 1 calc GR . . . .
H10C H 1.2304 0.5265 0.7809 0.035 Uiso 1 1 calc GR . . . .
C11 C 1.6079(9) 0.6469(6) 0.84521(15) 0.0219(12) Uani 1 1 d . . . . .
C12 C 1.5106(9) 0.7423(6) 0.87440(15) 0.0214(12) Uani 1 1 d . . . . .
C13 C 1.4547(9) 0.6602(6) 0.90585(15) 0.0220(12) Uani 1 1 d . . . . .
C14 C 1.4166(9) 0.7644(6) 0.93804(15) 0.0212(12) Uani 1 1 d . . . . .
C15 C 1.2792(9) 0.6940(6) 0.96464(15) 0.0238(12) Uani 1 1 d . . . . .
C16 C 1.2902(8) 0.7826(6) 0.99998(15) 0.0219(12) Uani 1 1 d . . . . .
C17 C 1.1219(8) 0.7325(6) 1.02505(15) 0.0225(12) Uani 1 1 d . . . . .
C18 C 1.1269(8) 0.8302(6) 1.05947(15) 0.0228(12) Uani 1 1 d . . . . .
C19 C 0.9863(9) 0.7704(7) 1.08656(16) 0.0273(13) Uani 1 1 d . . . . .
C20 C 0.8057(10) 0.8061(7) 0.63791(16) 0.0317(14) Uani 1 1 d . . . . .
H20A H 0.7267 0.7741 0.6567 0.038 Uiso 1 1 calc R . . . .
H20B H 0.8594 0.7204 0.6254 0.038 Uiso 1 1 calc R . . . .
C21 C 0.6601(10) 0.8824(7) 0.61476(17) 0.0336(14) Uani 1 1 d . . . . .
H21A H 0.7428 0.9187 0.5969 0.040 Uiso 1 1 calc R . . . .
H21B H 0.6040 0.9660 0.6277 0.040 Uiso 1 1 calc R . . . .
C22 C 0.4725(10) 0.7819(7) 0.59854(16) 0.0324(14) Uani 1 1 d . . . . .
H22A H 0.5291 0.6959 0.5866 0.039 Uiso 1 1 calc R . . . .
H22B H 0.3863 0.7494 0.6165 0.039 Uiso 1 1 calc R . . . .
C23 C 0.3290(11) 0.8545(7) 0.57365(17) 0.0350(15) Uani 1 1 d . . . . .
H23A H 0.4164 0.8910 0.5563 0.042 Uiso 1 1 calc R . . . .
H23B H 0.2673 0.9380 0.5858 0.042 Uiso 1 1 calc R . . . .
C24 C 0.1472(10) 0.7521(7) 0.55621(17) 0.0335(14) Uani 1 1 d . . . . .
H24A H 0.2089 0.6668 0.5448 0.040 Uiso 1 1 calc R . . . .
H24B H 0.0569 0.7186 0.5735 0.040 Uiso 1 1 calc R . . . .
C25 C 0.0075(10) 0.8222(7) 0.53024(17) 0.0319(14) Uani 1 1 d . . . . .
H25A H 0.0963 0.8517 0.5123 0.038 Uiso 1 1 calc R . . . .
H25B H -0.0494 0.9099 0.5413 0.038 Uiso 1 1 calc R . . . .
C26 C -0.1791(10) 0.7213(7) 0.51417(16) 0.0317(14) Uani 1 1 d . . . . .
H26A H -0.1223 0.6330 0.5034 0.038 Uiso 1 1 calc R . . . .
H26B H -0.2691 0.6930 0.5320 0.038 Uiso 1 1 calc R . . . .
C27 C -0.3166(10) 0.7902(7) 0.48794(17) 0.0328(14) Uani 1 1 d . . . . .
H27A H -0.2272 0.8178 0.4699 0.039 Uiso 1 1 calc R . . . .
H27B H -0.3729 0.8788 0.4987 0.039 Uiso 1 1 calc R . . . .
C28 C -0.5050(10) 0.6877(7) 0.47214(17) 0.0333(14) Uani 1 1 d . . . . .
H28A H -0.4480 0.5984 0.4619 0.040 Uiso 1 1 calc R . . . .
H28B H -0.5948 0.6614 0.4902 0.040 Uiso 1 1 calc R . . . .
C29 C -0.6442(11) 0.7526(7) 0.44527(17) 0.0344(15) Uani 1 1 d . . . . .
H29A H -0.7017 0.8417 0.4555 0.041 Uiso 1 1 calc R . . . .
H29B H -0.5545 0.7792 0.4272 0.041 Uiso 1 1 calc R . . . .
C30 C -0.8290(11) 0.6511(7) 0.42972(17) 0.0335(14) Uani 1 1 d . . . . .
H30A H -0.9180 0.6246 0.4479 0.040 Uiso 1 1 calc R . . . .
H30B H -0.7708 0.5618 0.4196 0.040 Uiso 1 1 calc R . . . .
C31 C -0.9715(11) 0.7124(7) 0.40263(17) 0.0352(15) Uani 1 1 d . . . . .
H31A H -1.0244 0.8044 0.4122 0.042 Uiso 1 1 calc R . . . .
H31B H -0.8854 0.7331 0.3837 0.042 Uiso 1 1 calc R . . . .
C32 C -1.1611(11) 0.6104(8) 0.38931(18) 0.0410(17) Uani 1 1 d . . . . .
H32A H -1.1076 0.5180 0.3802 0.049 Uiso 1 1 calc R . . . .
H32B H -1.2476 0.5910 0.4083 0.049 Uiso 1 1 calc R . . . .
C33 C -1.3038(12) 0.6671(10) 0.3620(2) 0.053(2) Uani 1 1 d . . . . .
H33A H -1.2222 0.6812 0.3425 0.080 Uiso 1 1 calc GR . . . .
H33B H -1.3579 0.7587 0.3707 0.080 Uiso 1 1 calc GR . . . .
H33C H -1.4221 0.5973 0.3555 0.080 Uiso 1 1 calc GR . . . .
F1 F 1.4941(5) 0.5158(3) 0.84053(8) 0.0263(7) Uani 1 1 d . . . . .
F2 F 1.8119(5) 0.6225(4) 0.85447(9) 0.0288(8) Uani 1 1 d . . . . .
F3 F 1.3317(5) 0.7976(4) 0.86206(9) 0.0321(8) Uani 1 1 d . . . . .
F4 F 1.6553(6) 0.8535(4) 0.88487(9) 0.0326(8) Uani 1 1 d . . . . .
F5 F 1.2721(6) 0.5764(4) 0.89685(9) 0.0339(8) Uani 1 1 d . . . . .
F6 F 1.6119(6) 0.5730(4) 0.91325(9) 0.0355(9) Uani 1 1 d . . . . .
F7 F 1.3172(6) 0.8812(4) 0.92856(9) 0.0353(9) Uani 1 1 d . . . . .
F8 F 1.6092(5) 0.8104(4) 0.95314(9) 0.0356(9) Uani 1 1 d . . . . .
F9 F 1.0744(5) 0.6801(5) 0.95188(9) 0.0381(9) Uani 1 1 d . . . . .
F10 F 1.3469(7) 0.5592(4) 0.96835(9) 0.0379(9) Uani 1 1 d . . . . .
F11 F 1.2641(6) 0.9231(4) 0.99598(9) 0.0333(8) Uani 1 1 d . . . . .
F12 F 1.4866(5) 0.7708(5) 1.01487(9) 0.0374(9) Uani 1 1 d . . . . .
F13 F 0.9245(5) 0.7367(5) 1.01039(9) 0.0403(10) Uani 1 1 d . . . . .
F14 F 1.1579(6) 0.5954(4) 1.03110(9) 0.0379(9) Uani 1 1 d . . . . .
F15 F 1.0567(6) 0.9613(4) 1.05382(10) 0.0398(9) Uani 1 1 d . . . . .
F16 F 1.3291(5) 0.8498(4) 1.07313(9) 0.0362(9) Uani 1 1 d . . . . .
F17 F 0.7880(6) 0.7379(5) 1.07455(10) 0.0449(10) Uani 1 1 d . . . . .
F18 F 1.0676(7) 0.6523(4) 1.09802(10) 0.0430(10) Uani 1 1 d . . . . .
F19 F 0.9829(6) 0.8718(4) 1.11300(9) 0.0392(9) Uani 1 1 d . . . . .
N1 N 1.7019(7) 0.8367(5) 0.77244(12) 0.0204(10) Uani 1 1 d . . . . .
N2 N 1.7649(7) 0.8000(5) 0.80425(12) 0.0195(10) Uani 1 1 d . . . . .
N3 N 1.4377(7) 0.7015(5) 0.78745(11) 0.0179(9) Uani 1 1 d . . . . .
O1 O 0.9822(7) 0.9058(5) 0.65089(11) 0.0327(10) Uani 1 1 d . . . . .
C34 C 0.7991(10) 0.3223(7) 0.71061(18) 0.0361(15) Uani 1 1 d . . . . .
F20 F 0.7937(9) 0.4282(6) 0.68955(14) 0.0704(15) Uani 1 1 d . . . . .
F21 F 0.7081(7) 0.2015(5) 0.69254(11) 0.0515(11) Uani 1 1 d . . . . .
F22 F 1.0033(6) 0.2989(6) 0.71715(12) 0.0618(14) Uani 1 1 d . . . . .
O2 O 0.4461(7) 0.3896(5) 0.73687(14) 0.0432(12) Uani 1 1 d . . . . .
O3 O 0.7808(8) 0.4976(6) 0.76469(16) 0.0576(16) Uani 1 1 d . . . . .
O4 O 0.6818(8) 0.2424(5) 0.76731(12) 0.0441(12) Uani 1 1 d . . . . .
S1 S 0.6616(2) 0.36993(16) 0.74895(4) 0.0278(3) Uani 1 1 d . . . . .
C35 C 0.3384(9) 0.1179(6) 0.81827(15) 0.0243(12) Uani 1 1 d . . . . .
C36 C 0.1833(10) 0.2309(7) 0.81072(18) 0.0332(14) Uani 1 1 d . . . . .
H36A H 0.2231 0.2751 0.7907 0.050 Uiso 1 1 calc GR . . . .
H36B H 0.1860 0.3048 0.8297 0.050 Uiso 1 1 calc GR . . . .
H36C H 0.0409 0.1854 0.8069 0.050 Uiso 1 1 calc GR . . . .
C37 C 0.5318(10) 0.1645(7) 0.84141(17) 0.0342(15) Uani 1 1 d . . . . .
H37A H 0.4870 0.1996 0.8635 0.051 Uiso 1 1 calc GR . . . .
H37B H 0.6129 0.2415 0.8321 0.051 Uiso 1 1 calc GR . . . .
H37C H 0.6200 0.0826 0.8434 0.051 Uiso 1 1 calc GR . . . .
O5 O 0.3120(7) -0.0079(4) 0.80559(11) 0.0313(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.399(9) . ?
C1 C6 1.395(9) . ?
C1 O1 1.351(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.380(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.397(8) . ?
C4 C5 1.401(8) . ?
C4 C7 1.458(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.386(8) . ?
C6 H6 0.9300 . ?
C7 N1 1.319(7) . ?
C7 N3 1.363(7) . ?
C8 C11 1.509(8) . ?
C8 N2 1.308(7) . ?
C8 N3 1.367(7) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9 N1 1.456(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N3 1.463(7) . ?
C11 C12 1.545(7) . ?
C11 F1 1.358(6) . ?
C11 F2 1.340(6) . ?
C12 C13 1.558(8) . ?
C12 F3 1.335(6) . ?
C12 F4 1.348(6) . ?
C13 C14 1.549(8) . ?
C13 F5 1.353(6) . ?
C13 F6 1.333(6) . ?
C14 C15 1.556(8) . ?
C14 F7 1.339(6) . ?
C14 F8 1.342(6) . ?
C15 C16 1.540(8) . ?
C15 F9 1.342(7) . ?
C15 F10 1.346(7) . ?
C16 C17 1.561(8) . ?
C16 F11 1.332(7) . ?
C16 F12 1.343(6) . ?
C17 C18 1.551(8) . ?
C17 F13 1.335(6) . ?
C17 F14 1.330(7) . ?
C18 C19 1.541(8) . ?
C18 F15 1.335(7) . ?
C18 F16 1.341(6) . ?
C19 F17 1.310(7) . ?
C19 F18 1.327(7) . ?
C19 F19 1.331(7) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.499(9) . ?
C20 O1 1.436(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.526(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.516(9) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.527(9) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 C25 1.520(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.521(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.513(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.534(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.519(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 C30 1.510(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.521(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.510(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.507(10) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
N1 N2 1.373(7) . ?
C34 F20 1.339(8) . ?
C34 F21 1.342(8) . ?
C34 F22 1.317(8) . ?
C34 S1 1.804(7) . ?
O2 S1 1.427(5) . ?
O3 S1 1.427(5) . ?
O4 S1 1.442(5) . ?
C35 C36 1.492(8) . ?
C35 C37 1.492(9) . ?
C35 O5 1.213(7) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?

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
C6 C1 C2 119.9(6) . . ?
O1 C1 C2 124.4(6) . . ?
O1 C1 C6 115.7(5) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.5(5) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 119.6(5) . . ?
C3 C4 C7 121.6(5) . . ?
C5 C4 C7 118.7(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.9(6) . . ?
C6 C5 H5 120.0 . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.2(6) . . ?
C5 C6 H6 119.9 . . ?
N1 C7 C4 126.9(5) . . ?
N1 C7 N3 106.9(5) . . ?
N3 C7 C4 126.1(5) . . ?
N2 C8 C11 120.8(5) . . ?
N2 C8 N3 113.0(5) . . ?
N3 C8 C11 126.2(5) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
C8 C11 C12 112.8(4) . . ?
F1 C11 C8 109.2(5) . . ?
F1 C11 C12 108.2(4) . . ?
F2 C11 C8 109.3(4) . . ?
F2 C11 C12 109.1(5) . . ?
F2 C11 F1 108.2(4) . . ?
C11 C12 C13 114.8(4) . . ?
F3 C12 C11 108.6(5) . . ?
F3 C12 C13 108.6(4) . . ?
F3 C12 F4 108.8(4) . . ?
F4 C12 C11 107.4(4) . . ?
F4 C12 C13 108.5(5) . . ?
C14 C13 C12 113.4(4) . . ?
F5 C13 C12 107.0(5) . . ?
F5 C13 C14 108.8(4) . . ?
F6 C13 C12 109.8(4) . . ?
F6 C13 C14 109.0(5) . . ?
F6 C13 F5 108.7(5) . . ?
C13 C14 C15 114.5(4) . . ?
F7 C14 C13 109.1(5) . . ?
F7 C14 C15 108.0(4) . . ?
F7 C14 F8 108.4(4) . . ?
F8 C14 C13 108.1(4) . . ?
F8 C14 C15 108.6(5) . . ?
C16 C15 C14 114.1(5) . . ?
F9 C15 C14 107.6(5) . . ?
F9 C15 C16 109.5(4) . . ?
F9 C15 F10 108.3(5) . . ?
F10 C15 C14 108.7(4) . . ?
F10 C15 C16 108.6(5) . . ?
C15 C16 C17 115.4(5) . . ?
F11 C16 C15 109.1(5) . . ?
F11 C16 C17 108.2(4) . . ?
F11 C16 F12 108.5(5) . . ?
F12 C16 C15 108.1(4) . . ?
F12 C16 C17 107.4(5) . . ?
C18 C17 C16 114.1(5) . . ?
F13 C17 C16 109.0(5) . . ?
F13 C17 C18 106.9(4) . . ?
F14 C17 C16 108.3(4) . . ?
F14 C17 C18 109.2(5) . . ?
F14 C17 F13 109.3(5) . . ?
C19 C18 C17 114.9(5) . . ?
F15 C18 C17 109.0(5) . . ?
F15 C18 C19 106.9(5) . . ?
F15 C18 F16 108.2(5) . . ?
F16 C18 C17 110.1(4) . . ?
F16 C18 C19 107.5(5) . . ?
F17 C19 C18 111.7(5) . . ?
F17 C19 F18 109.2(5) . . ?
F17 C19 F19 108.4(5) . . ?
F18 C19 C18 110.9(5) . . ?
F18 C19 F19 107.5(5) . . ?
F19 C19 C18 109.0(5) . . ?
H20A C20 H20B 108.3 . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
O1 C20 H20A 109.9 . . ?
O1 C20 H20B 109.9 . . ?
O1 C20 C21 108.9(5) . . ?
C20 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C20 C21 C22 112.4(5) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C21 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 C21 113.4(6) . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C22 C23 C24 113.5(6) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.9 . . ?
C24 C23 H23B 108.9 . . ?
C23 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 C23 113.9(5) . . ?
C25 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
C24 C25 H25A 108.9 . . ?
C24 C25 H25B 108.9 . . ?
C24 C25 C26 113.4(5) . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
C25 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 C25 113.5(5) . . ?
C27 C26 H26A 108.9 . . ?
C27 C26 H26B 108.9 . . ?
C26 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
C26 C27 C28 112.9(5) . . ?
H27A C27 H27B 107.8 . . ?
C28 C27 H27A 109.0 . . ?
C28 C27 H27B 109.0 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 C27 114.3(5) . . ?
C29 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C28 C29 H29A 108.7 . . ?
C28 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C30 C29 C28 114.1(5) . . ?
C30 C29 H29A 108.7 . . ?
C30 C29 H29B 108.7 . . ?
C29 C30 H30A 108.4 . . ?
C29 C30 H30B 108.4 . . ?
C29 C30 C31 115.5(6) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.4 . . ?
C31 C30 H30B 108.4 . . ?
C30 C31 H31A 108.9 . . ?
C30 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 C30 113.5(6) . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C31 C32 H32A 108.6 . . ?
C31 C32 H32B 108.6 . . ?
H32A C32 H32B 107.5 . . ?
C33 C32 C31 114.8(7) . . ?
C33 C32 H32A 108.6 . . ?
C33 C32 H32B 108.6 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C7 N1 C9 129.5(5) . . ?
C7 N1 N2 112.0(4) . . ?
N2 N1 C9 118.5(5) . . ?
C8 N2 N1 103.1(4) . . ?
C7 N3 C8 104.9(4) . . ?
C7 N3 C10 126.0(5) . . ?
C8 N3 C10 128.9(5) . . ?
C1 O1 C20 118.2(5) . . ?
F20 C34 F21 105.8(6) . . ?
F20 C34 S1 111.9(5) . . ?
F21 C34 S1 111.9(4) . . ?
F22 C34 F20 106.9(6) . . ?
F22 C34 F21 107.7(6) . . ?
F22 C34 S1 112.2(5) . . ?
O2 S1 C34 104.0(3) . . ?
O2 S1 O3 116.4(3) . . ?
O2 S1 O4 113.3(3) . . ?
O3 S1 C34 103.9(3) . . ?
O3 S1 O4 114.1(4) . . ?
O4 S1 C34 103.0(3) . . ?
C36 C35 C37 118.1(5) . . ?
O5 C35 C36 121.5(6) . . ?
O5 C35 C37 120.4(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_olex2_date_sample_data_collection 2016-12-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id ALR13
_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 1.307
_oxdiff_exptl_absorpt_empirical_full_min 0.734
####################################################################### 
# 
# 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_dwb1683a
_database_code_depnum_ccdc_archive 'CCDC 2177843'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_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         'C31 H39 F15 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C33 H39 F21 N4 O5 S2'
_chemical_formula_weight         1034.80
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H39 F21 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio Riccobono NV 2520'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   6.67080(17)
_cell_length_b                   8.5688(2)
_cell_length_c                   74.9335(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4283.27(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4701
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      71.5020
_cell_measurement_theta_min      4.7250
_shelx_estimated_absorpt_T_max   0.947
_shelx_estimated_absorpt_T_min   0.478
_exptl_absorpt_coefficient_mu    2.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2104
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0191
0 0 1 0.0035
-1 0 0 0.1776
1 0 1 0.1820
0 1 1 0.0710
0 -1 -1 0.0749

_exptl_crystal_recrystallization_method 
'crystallisation from acetone and hexane'
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.023
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
0.0001 -0.0002 -1.0003 -0.0205 -0.0001 -0.0017
-0.0001 0.0002 1.0003 0.0205 0.0001 0.0017
-1.0002 -0.0002 0.0000 0.0076 -0.2172 -0.0778
1.0002 0.0004 1.0003 0.0129 0.2174 0.0794
0.0007 0.9999 0.9972 0.0075 -0.0606 0.1703
-0.0007 -0.9999 -0.9972 -0.0075 0.0606 -0.1703

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -88
_diffrn_reflns_number            14579
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        66.577
_diffrn_reflns_theta_max         66.577
_diffrn_reflns_theta_min         3.539
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     27.00  64.50   0.75    0.75    --    0.00  77.00  30.00   50
  2  ω    -82.00 -56.50   0.75    0.75    --    0.00 178.00-150.00   34
  3  ω    -32.00  17.50   0.75    0.75    --    0.00  77.00  30.00   66
  4  ω    -79.00 -40.00   0.75    0.75    --    0.00 178.00 -30.00   52
  5  ω     -8.00  80.50   0.75    2.25    --   56.00 -61.00 -60.00  118
  6  ω     69.00  95.25   0.75    2.25    --   56.00-125.00  60.00   35
  7  ω     69.00  95.25   0.75    2.25    --   56.00  61.00  90.00   35
  8  ω     72.00 114.75   0.75    2.25    --   56.00-124.00 140.00   57
  9  ω     29.00 128.00   0.75    2.25    --   56.00  45.00-180.00  132
 10  ω    -10.00  72.50   0.75    2.25    --   56.00 -61.00  30.00  110
 11  ω     39.00 152.25   0.75    4.50    --  112.00 -91.00  30.00  151
 12  ω     46.00 115.00   0.75    4.50    --  112.00-111.00-150.00   92
 13  ω     92.00 170.00   0.75    4.50    --  112.00  50.00-180.00  104
 14  ω    102.00 128.25   0.75    4.50    --  112.00 111.00 -60.00   35
 15  ω    131.00 176.00   0.75    4.50    --  112.00 111.00 120.00   60
 16  ω     86.00 113.00   0.75    4.50    --  112.00-111.00 -30.00   36
 17  ω     72.00 176.25   0.75    4.50    --  112.00  12.00 120.00  139
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0076116000
_diffrn_orient_matrix_UB_12      -0.0129303000
_diffrn_orient_matrix_UB_13      0.0205088000
_diffrn_orient_matrix_UB_21      0.2172056000
_diffrn_orient_matrix_UB_22      -0.0608542000
_diffrn_orient_matrix_UB_23      0.0001366000
_diffrn_orient_matrix_UB_31      0.0777211000
_diffrn_orient_matrix_UB_32      0.1686594000
_diffrn_orient_matrix_UB_33      0.0016300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.682
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                7043
_reflns_number_total             7399
_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 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 
;
 Flack x determined using 2379 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.1076
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+65.3063P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2579
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(C26) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002
Uanis(O5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(F2)
\\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C)
;
_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
C1 C 0.5741(19) 0.3681(15) 0.34273(16) 0.019(3) Uani 1 1 d . . . . .
C2 C 0.605(2) 0.2239(15) 0.35012(17) 0.022(3) Uani 1 1 d . . . . .
H2 H 0.546131 0.133379 0.344967 0.027 Uiso 1 1 calc R U . . .
C3 C 0.7258(18) 0.2125(15) 0.36568(16) 0.021(3) Uani 1 1 d . U . . .
H3 H 0.751778 0.113315 0.370859 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8058(17) 0.3454(15) 0.37327(16) 0.018(3) Uani 1 1 d . U . . .
C5 C 0.775(2) 0.4884(16) 0.36542(17) 0.026(3) Uani 1 1 d . U . . .
H5 H 0.833713 0.578603 0.370613 0.032 Uiso 1 1 calc R U . . .
C6 C 0.6616(18) 0.5040(14) 0.35032(18) 0.020(3) Uani 1 1 d . . . . .
H6 H 0.641715 0.603483 0.345011 0.025 Uiso 1 1 calc R U . . .
C7 C 0.9308(19) 0.3301(14) 0.38940(16) 0.018(3) Uani 1 1 d . U . . .
C8 C 1.0498(17) 0.2929(14) 0.41587(16) 0.017(2) Uani 1 1 d . U . . .
C9 C 0.670(2) 0.2392(18) 0.4113(2) 0.032(3) Uani 1 1 d . . . . .
H9A H 0.665340 0.125958 0.413083 0.048 Uiso 1 1 calc R U . . .
H9B H 0.575058 0.268698 0.401899 0.048 Uiso 1 1 calc R U . . .
H9C H 0.634129 0.292142 0.422424 0.048 Uiso 1 1 calc R U . . .
C10 C 1.262(2) 0.4142(16) 0.37600(17) 0.024(3) Uani 1 1 d . . . . .
H10A H 1.372930 0.339371 0.375077 0.036 Uiso 1 1 calc R U . . .
H10B H 1.315899 0.517717 0.378872 0.036 Uiso 1 1 calc R U . . .
H10C H 1.190349 0.418797 0.364616 0.036 Uiso 1 1 calc R U . . .
C11 C 1.069(2) 0.2487(16) 0.43518(18) 0.026(3) Uani 1 1 d . . . . .
C12 C 1.045(2) 0.3911(15) 0.44776(18) 0.025(3) Uani 1 1 d . U . . .
C13 C 1.036(2) 0.3552(16) 0.46779(18) 0.023(3) Uani 1 1 d . U . . .
C14 C 1.089(2) 0.4952(17) 0.48028(19) 0.030(3) Uani 1 1 d . U . . .
C15 C 1.022(2) 0.4681(16) 0.49990(19) 0.025(3) Uani 1 1 d . . . . .
C16 C 1.128(3) 0.5828(18) 0.5133(2) 0.039(4) Uani 1 1 d . . . . .
C17 C 1.038(3) 0.5840(19) 0.5321(2) 0.045(5) Uani 1 1 d . . . . .
C18 C 0.3047(19) 0.2835(15) 0.32396(17) 0.022(3) Uani 1 1 d . . . . .
H18A H 0.231939 0.251678 0.334889 0.026 Uiso 1 1 calc R U . . .
H18B H 0.364626 0.189418 0.318447 0.026 Uiso 1 1 calc R U . . .
C19 C 0.164(2) 0.3622(15) 0.31110(18) 0.023(3) Uani 1 1 d . . . . .
H19A H 0.242847 0.395424 0.300537 0.028 Uiso 1 1 calc R U . . .
H19B H 0.111690 0.457754 0.316853 0.028 Uiso 1 1 calc R U . . .
C20 C -0.0123(17) 0.2654(14) 0.30467(16) 0.015(2) Uani 1 1 d . U . . .
H20A H 0.038258 0.168122 0.299151 0.018 Uiso 1 1 calc R U . . .
H20B H -0.096076 0.236112 0.315045 0.018 Uiso 1 1 calc R U . . .
C21 C -0.1410(19) 0.3522(14) 0.29120(18) 0.021(3) Uani 1 1 d . . . . .
H21A H -0.196099 0.446965 0.296948 0.026 Uiso 1 1 calc R U . . .
H21B H -0.054966 0.386377 0.281162 0.026 Uiso 1 1 calc R U . . .
C22 C -0.3129(17) 0.2564(14) 0.28382(16) 0.015(2) Uani 1 1 d . U . . .
H22A H -0.400685 0.223170 0.293779 0.019 Uiso 1 1 calc R U . . .
H22B H -0.258776 0.161255 0.278075 0.019 Uiso 1 1 calc R U . . .
C23 C -0.4385(17) 0.3484(14) 0.27008(15) 0.014(2) Uani 1 1 d . U . . .
H23A H -0.489866 0.444389 0.275843 0.017 Uiso 1 1 calc R U . . .
H23B H -0.350112 0.380582 0.260130 0.017 Uiso 1 1 calc R U . . .
C24 C -0.6139(17) 0.2579(14) 0.26253(16) 0.016(2) Uani 1 1 d . U . . .
H24A H -0.701397 0.224932 0.272509 0.019 Uiso 1 1 calc R U . . .
H24B H -0.562178 0.162329 0.256706 0.019 Uiso 1 1 calc R U . . .
C25 C -0.7411(19) 0.3490(14) 0.24893(16) 0.018(3) Uani 1 1 d . U . . .
H25A H -0.792408 0.444722 0.254743 0.022 Uiso 1 1 calc R U . . .
H25B H -0.653605 0.381700 0.238934 0.022 Uiso 1 1 calc R U . . .
C26 C -0.9160(18) 0.2592(14) 0.24144(15) 0.017(2) Uani 1 1 d . U . . .
H26A H -1.006139 0.229330 0.251362 0.020 Uiso 1 1 calc R U . . .
H26B H -0.865519 0.161951 0.235900 0.020 Uiso 1 1 calc R U . . .
C27 C -1.0354(17) 0.3490(14) 0.22772(16) 0.015(2) Uani 1 1 d . U . . .
H27A H -0.945784 0.377000 0.217684 0.018 Uiso 1 1 calc R U . . .
H27B H -1.083386 0.447286 0.233187 0.018 Uiso 1 1 calc R U . . .
C28 C -1.2143(19) 0.2603(15) 0.22039(17) 0.022(3) Uani 1 1 d . U . . .
H28A H -1.303074 0.232146 0.230477 0.026 Uiso 1 1 calc R U . . .
H28B H -1.165596 0.161850 0.215000 0.026 Uiso 1 1 calc R U . . .
C29 C -1.3379(19) 0.3472(15) 0.20653(18) 0.022(3) Uani 1 1 d . . . . .
H29A H -1.250983 0.373545 0.196250 0.027 Uiso 1 1 calc R U . . .
H29B H -1.386405 0.446262 0.211781 0.027 Uiso 1 1 calc R U . . .
C30 C -1.5173(19) 0.2535(15) 0.19987(17) 0.022(3) Uani 1 1 d . . . . .
H30A H -1.469020 0.154877 0.194486 0.026 Uiso 1 1 calc R U . . .
H30B H -1.603968 0.226387 0.210137 0.026 Uiso 1 1 calc R U . . .
C31 C -1.640(2) 0.3424(18) 0.18616(19) 0.030(3) Uani 1 1 d . . . . .
H31A H -1.561665 0.354960 0.175200 0.044 Uiso 1 1 calc R U . . .
H31B H -1.675079 0.445376 0.190924 0.044 Uiso 1 1 calc R U . . .
H31C H -1.763103 0.284195 0.183509 0.044 Uiso 1 1 calc R U . . .
F1 F 0.9266(13) 0.1442(9) 0.44026(10) 0.0321(19) Uani 1 1 d . . . . .
F2 F 1.2500(13) 0.1880(11) 0.43778(11) 0.039(2) Uani 1 1 d . U . . .
F3 F 0.8803(12) 0.4709(9) 0.44279(11) 0.0324(19) Uani 1 1 d . . . . .
F4 F 1.2028(14) 0.4859(11) 0.44477(11) 0.039(2) Uani 1 1 d . . . . .
F5 F 0.8443(13) 0.3096(10) 0.47144(11) 0.036(2) Uani 1 1 d . . . . .
F6 F 1.1549(14) 0.2360(9) 0.47146(11) 0.036(2) Uani 1 1 d . . . . .
F7 F 0.9989(15) 0.6216(9) 0.47394(11) 0.039(2) Uani 1 1 d . . . . .
F8 F 1.2912(12) 0.5125(11) 0.47979(11) 0.038(2) Uani 1 1 d . . . . .
F9 F 0.8254(14) 0.4905(11) 0.50120(11) 0.038(2) Uani 1 1 d . . . . .
F10 F 1.0676(13) 0.3197(9) 0.50486(10) 0.0326(19) Uani 1 1 d . . . . .
F11 F 1.1246(19) 0.7253(10) 0.50664(12) 0.054(3) Uani 1 1 d . . . . .
F12 F 1.3219(15) 0.5363(11) 0.51505(12) 0.044(2) Uani 1 1 d . . . . .
F13 F 0.8557(18) 0.6440(14) 0.53195(14) 0.063(3) Uani 1 1 d . . . . .
F14 F 1.0363(16) 0.4442(11) 0.53915(11) 0.045(2) Uani 1 1 d . . . . .
F15 F 1.150(2) 0.6747(14) 0.54249(13) 0.072(4) Uani 1 1 d . . . . .
N1 N 0.8788(15) 0.2864(12) 0.40582(14) 0.018(2) Uani 1 1 d . U . . .
N2 N 1.1242(15) 0.3644(12) 0.39017(13) 0.017(2) Uani 1 1 d . U . . .
N3 N 1.2006(17) 0.3387(14) 0.40675(14) 0.025(2) Uani 1 1 d . . . . .
O1 O 0.4576(14) 0.3951(10) 0.32821(12) 0.023(2) Uani 1 1 d . . . . .
C32 C 0.750(3) 0.6853(18) 0.5840(2) 0.051(5) Uani 1 1 d . . . . .
C33 C 0.581(2) 0.6443(16) 0.65063(18) 0.028(3) Uani 1 1 d . U . . .
F16 F 0.875(2) 0.5654(12) 0.58787(16) 0.069(4) Uani 1 1 d . . . . .
F17 F 0.684(2) 0.6686(12) 0.56754(14) 0.080(4) Uani 1 1 d . . . . .
F18 F 0.8629(17) 0.8132(13) 0.58455(15) 0.061(3) Uani 1 1 d . . . . .
F19 F 0.6127(14) 0.7851(9) 0.65681(12) 0.037(2) Uani 1 1 d . . . . .
F20 F 0.6084(15) 0.5395(9) 0.66365(12) 0.041(2) Uani 1 1 d . . . . .
F21 F 0.3840(13) 0.6348(10) 0.64619(12) 0.036(2) Uani 1 1 d . . . . .
N4 N 0.6590(19) 0.7245(13) 0.61790(15) 0.027(3) Uani 1 1 d . U . . .
O2 O 0.443(2) 0.5519(12) 0.59800(16) 0.047(3) Uani 1 1 d . . . . .
O3 O 0.4457(18) 0.8356(11) 0.59508(14) 0.037(3) Uani 1 1 d . . . . .
O4 O 0.6895(14) 0.4383(10) 0.62729(13) 0.026(2) Uani 1 1 d . U . . .
O5 O 0.9313(15) 0.6308(12) 0.63770(14) 0.035(2) Uani 1 1 d . U . . .
S1 S 0.5467(6) 0.6960(4) 0.59979(5) 0.0308(8) Uani 1 1 d . . . . .
S2 S 0.7352(5) 0.5968(4) 0.63145(5) 0.0260(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.369(17) . ?
C1 C6 1.421(17) . ?
C1 O1 1.357(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.422(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(18) . ?
C4 C5 1.375(19) . ?
C4 C7 1.475(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.368(18) . ?
C6 H6 0.9500 . ?
C7 N1 1.332(16) . ?
C7 N2 1.324(16) . ?
C8 C11 1.501(18) . ?
C8 N1 1.368(15) . ?
C8 N3 1.278(16) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 N1 1.506(16) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N2 1.469(16) . ?
C11 C12 1.551(18) . ?
C11 F1 1.361(16) . ?
C11 F2 1.327(16) . ?
C12 C13 1.533(18) . ?
C12 F3 1.345(15) . ?
C12 F4 1.349(16) . ?
C13 C14 1.562(19) . ?
C13 F5 1.363(16) . ?
C13 F6 1.323(15) . ?
C14 C15 1.554(19) . ?
C14 F7 1.325(16) . ?
C14 F8 1.360(18) . ?
C15 C16 1.58(2) . ?
C15 F9 1.329(16) . ?
C15 F10 1.359(16) . ?
C16 C17 1.53(2) . ?
C16 F11 1.321(17) . ?
C16 F12 1.36(2) . ?
C17 F13 1.32(2) . ?
C17 F14 1.309(18) . ?
C17 F15 1.33(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.503(17) . ?
C18 O1 1.434(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.520(16) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.519(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.515(16) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.544(15) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.513(15) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.539(15) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.506(16) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.511(16) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.517(16) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.521(17) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.525(16) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.519(18) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N2 N3 1.361(14) . ?
C32 F16 1.35(2) . ?
C32 F17 1.32(2) . ?
C32 F18 1.33(2) . ?
C32 S1 1.800(19) . ?
C33 F19 1.310(16) . ?
C33 F20 1.339(16) . ?
C33 F21 1.356(17) . ?
C33 S2 1.815(14) . ?
N4 S1 1.570(12) . ?
N4 S2 1.577(12) . ?
O2 S1 1.423(12) . ?
O3 S1 1.418(10) . ?
O4 S2 1.427(9) . ?
O5 S2 1.419(10) . ?

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
C2 C1 C6 121.1(11) . . ?
O1 C1 C2 124.3(11) . . ?
O1 C1 C6 114.6(11) . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.6(12) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.1(12) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C7 118.9(11) . . ?
C5 C4 C3 120.1(11) . . ?
C5 C4 C7 121.0(12) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.6(12) . . ?
C6 C5 H5 119.2 . . ?
C1 C6 H6 120.7 . . ?
C5 C6 C1 118.6(11) . . ?
C5 C6 H6 120.7 . . ?
N1 C7 C4 129.4(12) . . ?
N2 C7 C4 124.5(12) . . ?
N2 C7 N1 106.0(11) . . ?
N1 C8 C11 126.3(11) . . ?
N3 C8 C11 121.6(11) . . ?
N3 C8 N1 112.0(11) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
C8 C11 C12 112.2(11) . . ?
F1 C11 C8 112.0(11) . . ?
F1 C11 C12 105.9(11) . . ?
F2 C11 C8 108.6(11) . . ?
F2 C11 C12 108.3(11) . . ?
F2 C11 F1 109.7(11) . . ?
C13 C12 C11 116.2(11) . . ?
F3 C12 C11 108.5(11) . . ?
F3 C12 C13 109.9(11) . . ?
F3 C12 F4 106.6(10) . . ?
F4 C12 C11 106.9(11) . . ?
F4 C12 C13 108.3(11) . . ?
C12 C13 C14 115.1(11) . . ?
F5 C13 C12 106.9(11) . . ?
F5 C13 C14 108.2(11) . . ?
F6 C13 C12 109.5(11) . . ?
F6 C13 C14 109.4(11) . . ?
F6 C13 F5 107.5(11) . . ?
C15 C14 C13 112.8(11) . . ?
F7 C14 C13 108.1(11) . . ?
F7 C14 C15 109.4(12) . . ?
F7 C14 F8 110.5(13) . . ?
F8 C14 C13 107.0(12) . . ?
F8 C14 C15 109.0(12) . . ?
C14 C15 C16 112.5(12) . . ?
F9 C15 C14 109.3(12) . . ?
F9 C15 C16 107.9(12) . . ?
F9 C15 F10 109.6(12) . . ?
F10 C15 C14 109.5(11) . . ?
F10 C15 C16 108.0(11) . . ?
C17 C16 C15 114.4(14) . . ?
F11 C16 C15 108.9(13) . . ?
F11 C16 C17 109.6(14) . . ?
F11 C16 F12 109.0(15) . . ?
F12 C16 C15 107.8(13) . . ?
F12 C16 C17 107.0(14) . . ?
F13 C17 C16 111.1(15) . . ?
F13 C17 F15 107.2(15) . . ?
F14 C17 C16 111.6(14) . . ?
F14 C17 F13 110.7(16) . . ?
F14 C17 F15 107.5(14) . . ?
F15 C17 C16 108.5(15) . . ?
H18A C18 H18B 108.6 . . ?
C19 C18 H18A 110.4 . . ?
C19 C18 H18B 110.4 . . ?
O1 C18 H18A 110.4 . . ?
O1 C18 H18B 110.4 . . ?
O1 C18 C19 106.6(10) . . ?
C18 C19 H19A 108.2 . . ?
C18 C19 H19B 108.2 . . ?
C18 C19 C20 116.2(10) . . ?
H19A C19 H19B 107.4 . . ?
C20 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 C19 112.4(10) . . ?
C21 C20 H20A 109.1 . . ?
C21 C20 H20B 109.1 . . ?
C20 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 C20 113.9(10) . . ?
C22 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
C21 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C21 C22 C23 112.2(10) . . ?
H22A C22 H22B 107.9 . . ?
C23 C22 H22A 109.2 . . ?
C23 C22 H22B 109.2 . . ?
C22 C23 H23A 108.7 . . ?
C22 C23 H23B 108.7 . . ?
H23A C23 H23B 107.6 . . ?
C24 C23 C22 114.0(9) . . ?
C24 C23 H23A 108.7 . . ?
C24 C23 H23B 108.7 . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
C23 C24 C25 114.5(10) . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 108.6 . . ?
C24 C25 H25B 108.6 . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 C24 114.5(10) . . ?
C26 C25 H25A 108.6 . . ?
C26 C25 H25B 108.6 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
C25 C26 C27 113.7(10) . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C26 C27 H27A 108.8 . . ?
C26 C27 H27B 108.8 . . ?
C26 C27 C28 113.9(10) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C27 C28 H28A 108.4 . . ?
C27 C28 H28B 108.4 . . ?
C27 C28 C29 115.3(11) . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
C28 C29 H29A 109.0 . . ?
C28 C29 H29B 109.0 . . ?
C28 C29 C30 113.0(11) . . ?
H29A C29 H29B 107.8 . . ?
C30 C29 H29A 109.0 . . ?
C30 C29 H29B 109.0 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C31 C30 C29 112.4(11) . . ?
C31 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C7 N1 C8 106.2(10) . . ?
C7 N1 C9 124.6(11) . . ?
C8 N1 C9 129.2(11) . . ?
C7 N2 C10 130.1(11) . . ?
C7 N2 N3 111.7(10) . . ?
N3 N2 C10 118.1(10) . . ?
C8 N3 N2 104.0(10) . . ?
C1 O1 C18 118.1(9) . . ?
F16 C32 S1 111.2(11) . . ?
F17 C32 F16 108.8(14) . . ?
F17 C32 F18 107.7(13) . . ?
F17 C32 S1 111.8(16) . . ?
F18 C32 F16 105.6(18) . . ?
F18 C32 S1 111.4(11) . . ?
F19 C33 F20 109.7(11) . . ?
F19 C33 F21 107.5(11) . . ?
F19 C33 S2 113.2(11) . . ?
F20 C33 F21 105.8(12) . . ?
F20 C33 S2 110.4(10) . . ?
F21 C33 S2 110.0(9) . . ?
S1 N4 S2 127.1(7) . . ?
N4 S1 C32 102.5(9) . . ?
O2 S1 C32 105.2(8) . . ?
O2 S1 N4 116.7(7) . . ?
O3 S1 C32 103.7(7) . . ?
O3 S1 N4 108.1(6) . . ?
O3 S1 O2 118.5(7) . . ?
N4 S2 C33 99.9(6) . . ?
O4 S2 C33 105.4(7) . . ?
O4 S2 N4 116.8(6) . . ?
O5 S2 C33 102.5(7) . . ?
O5 S2 N4 111.6(7) . . ?
O5 S2 O4 117.7(6) . . ?

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
C1 C2 C3 C4 1.6(19) . . . . ?
C2 C1 C6 C5 -1.1(19) . . . . ?
C2 C1 O1 C18 22.7(18) . . . . ?
C2 C3 C4 C5 -2.5(19) . . . . ?
C2 C3 C4 C7 180.0(12) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C3 C4 C7 N1 -67.5(18) . . . . ?
C3 C4 C7 N2 114.9(14) . . . . ?
C4 C5 C6 C1 0(2) . . . . ?
C4 C7 N1 C8 -179.5(12) . . . . ?
C4 C7 N1 C9 1(2) . . . . ?
C4 C7 N2 C10 -4(2) . . . . ?
C4 C7 N2 N3 -179.9(11) . . . . ?
C5 C4 C7 N1 115.0(16) . . . . ?
C5 C4 C7 N2 -62.6(18) . . . . ?
C6 C1 C2 C3 0.2(19) . . . . ?
C6 C1 O1 C18 -155.8(11) . . . . ?
C7 C4 C5 C6 179.1(12) . . . . ?
C7 N2 N3 C8 -1.6(14) . . . . ?
C8 C11 C12 C13 172.5(11) . . . . ?
C8 C11 C12 F3 48.1(15) . . . . ?
C8 C11 C12 F4 -66.5(14) . . . . ?
C10 N2 N3 C8 -178.0(11) . . . . ?
C11 C8 N1 C7 -177.7(12) . . . . ?
C11 C8 N1 C9 2(2) . . . . ?
C11 C8 N3 N2 178.9(11) . . . . ?
C11 C12 C13 C14 158.8(12) . . . . ?
C11 C12 C13 F5 -81.1(14) . . . . ?
C11 C12 C13 F6 35.1(16) . . . . ?
C12 C13 C14 C15 164.2(12) . . . . ?
C12 C13 C14 F7 43.1(16) . . . . ?
C12 C13 C14 F8 -75.9(14) . . . . ?
C13 C14 C15 C16 163.2(12) . . . . ?
C13 C14 C15 F9 -77.0(15) . . . . ?
C13 C14 C15 F10 43.1(16) . . . . ?
C14 C15 C16 C17 168.1(14) . . . . ?
C14 C15 C16 F11 45.1(18) . . . . ?
C14 C15 C16 F12 -73.1(15) . . . . ?
C15 C16 C17 F13 -67.5(17) . . . . ?
C15 C16 C17 F14 57(2) . . . . ?
C15 C16 C17 F15 174.8(14) . . . . ?
C18 C19 C20 C21 -177.8(11) . . . . ?
C19 C18 O1 C1 164.1(11) . . . . ?
C19 C20 C21 C22 177.2(11) . . . . ?
C20 C21 C22 C23 -179.5(10) . . . . ?
C21 C22 C23 C24 -179.2(10) . . . . ?
C22 C23 C24 C25 179.5(10) . . . . ?
C23 C24 C25 C26 -179.8(10) . . . . ?
C24 C25 C26 C27 -178.3(10) . . . . ?
C25 C26 C27 C28 -178.8(10) . . . . ?
C26 C27 C28 C29 -180.0(11) . . . . ?
C27 C28 C29 C30 -179.1(11) . . . . ?
C28 C29 C30 C31 179.5(11) . . . . ?
F1 C11 C12 C13 50.0(15) . . . . ?
F1 C11 C12 F3 -74.3(13) . . . . ?
F1 C11 C12 F4 171.1(10) . . . . ?
F2 C11 C12 C13 -67.6(15) . . . . ?
F2 C11 C12 F3 168.0(11) . . . . ?
F2 C11 C12 F4 53.4(14) . . . . ?
F3 C12 C13 C14 -77.5(15) . . . . ?
F3 C12 C13 F5 42.6(14) . . . . ?
F3 C12 C13 F6 158.8(11) . . . . ?
F4 C12 C13 C14 38.6(15) . . . . ?
F4 C12 C13 F5 158.7(10) . . . . ?
F4 C12 C13 F6 -85.2(13) . . . . ?
F5 C13 C14 C15 44.8(15) . . . . ?
F5 C13 C14 F7 -76.3(14) . . . . ?
F5 C13 C14 F8 164.7(11) . . . . ?
F6 C13 C14 C15 -72.0(15) . . . . ?
F6 C13 C14 F7 166.9(11) . . . . ?
F6 C13 C14 F8 47.9(14) . . . . ?
F7 C14 C15 C16 -76.4(16) . . . . ?
F7 C14 C15 F9 43.4(16) . . . . ?
F7 C14 C15 F10 163.5(12) . . . . ?
F8 C14 C15 C16 44.5(16) . . . . ?
F8 C14 C15 F9 164.3(12) . . . . ?
F8 C14 C15 F10 -75.6(15) . . . . ?
F9 C15 C16 C17 47.5(18) . . . . ?
F9 C15 C16 F11 -75.5(17) . . . . ?
F9 C15 C16 F12 166.3(11) . . . . ?
F10 C15 C16 C17 -70.9(17) . . . . ?
F10 C15 C16 F11 166.0(13) . . . . ?
F10 C15 C16 F12 47.9(15) . . . . ?
F11 C16 C17 F13 55(2) . . . . ?
F11 C16 C17 F14 179.2(16) . . . . ?
F11 C16 C17 F15 -63(2) . . . . ?
F12 C16 C17 F13 173.2(13) . . . . ?
F12 C16 C17 F14 -62.7(19) . . . . ?
F12 C16 C17 F15 55.6(18) . . . . ?
N1 C7 N2 C10 177.9(12) . . . . ?
N1 C7 N2 N3 2.0(14) . . . . ?
N1 C8 C11 C12 -94.2(15) . . . . ?
N1 C8 C11 F1 24.8(18) . . . . ?
N1 C8 C11 F2 146.1(12) . . . . ?
N1 C8 N3 N2 0.5(14) . . . . ?
N2 C7 N1 C8 -1.5(14) . . . . ?
N2 C7 N1 C9 179.0(12) . . . . ?
N3 C8 C11 C12 87.7(15) . . . . ?
N3 C8 C11 F1 -153.4(12) . . . . ?
N3 C8 C11 F2 -32.1(17) . . . . ?
N3 C8 N1 C7 0.6(15) . . . . ?
N3 C8 N1 C9 -179.9(13) . . . . ?
O1 C1 C2 C3 -178.1(12) . . . . ?
O1 C1 C6 C5 177.4(12) . . . . ?
O1 C18 C19 C20 -179.8(11) . . . . ?
F16 C32 S1 N4 61.2(15) . . . . ?
F16 C32 S1 O2 -61.3(15) . . . . ?
F16 C32 S1 O3 173.6(13) . . . . ?
F17 C32 S1 N4 -177.0(11) . . . . ?
F17 C32 S1 O2 60.5(12) . . . . ?
F17 C32 S1 O3 -64.6(12) . . . . ?
F18 C32 S1 N4 -56.4(14) . . . . ?
F18 C32 S1 O2 -178.8(12) . . . . ?
F18 C32 S1 O3 56.0(15) . . . . ?
F19 C33 S2 N4 -61.9(11) . . . . ?
F19 C33 S2 O4 176.6(10) . . . . ?
F19 C33 S2 O5 52.9(11) . . . . ?
F20 C33 S2 N4 174.6(10) . . . . ?
F20 C33 S2 O4 53.2(12) . . . . ?
F20 C33 S2 O5 -70.5(11) . . . . ?
F21 C33 S2 N4 58.3(11) . . . . ?
F21 C33 S2 O4 -63.2(11) . . . . ?
F21 C33 S2 O5 173.1(9) . . . . ?
S1 N4 S2 C33 -116.1(10) . . . . ?
S1 N4 S2 O4 -3.2(13) . . . . ?
S1 N4 S2 O5 136.2(10) . . . . ?
S2 N4 S1 C32 -91.0(11) . . . . ?
S2 N4 S1 O2 23.3(13) . . . . ?
S2 N4 S1 O3 159.8(9) . . . . ?

_olex2_date_sample_data_collection 2016-12-16
_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 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.632
####################################################################### 
# 
# 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_dwb1707
_database_code_depnum_ccdc_archive 'CCDC 2177841'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H31 F7 N3 O, B F4, C3 H6 O'
_chemical_formula_sum            'C26 H37 B F11 N3 O2'
_chemical_formula_weight         643.39
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C23 H31 B F11 N3 O'
_chemical_oxdiff_usercomment     'Alessio Riccobono NV2570'
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'
B B 0.0090 0.0039 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   29.5005(5)
_cell_length_b                   9.28574(14)
_cell_length_c                   11.08372(17)
_cell_angle_alpha                90
_cell_angle_beta                 98.6889(15)
_cell_angle_gamma                90
_cell_volume                     3001.36(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.8910
_cell_measurement_theta_min      4.5370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 5 0.1350
1 5 -1 0.1190
1 -5 -2 0.1410
1 0 0 0.0363
-1 0 0 0.0294
3 0 -5 0.1469
1 -5 -1 0.1494
2 -5 -3 0.1357
5 -2 -1 0.1167
5 -2 0 0.1317
5 0 1 0.0774
5 0 -1 0.0796
-5 -1 0 0.0778
-5 -1 -1 0.0973
5 1 0 0.0780
-5 1 1 0.1289

_exptl_crystal_recrystallization_method acetone/hexane
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.066
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
-2.9995 -0.0000 5.0000 0.0147 -0.0557 0.6941
1.0003 5.0000 -1.0000 -0.0399 -0.8157 -0.2054
0.9994 -5.0000 -2.0000 0.0205 0.8494 -0.2117
1.0000 0.0000 0.0000 -0.0527 0.0012 -0.0028
-1.0000 -0.0000 -0.0000 0.0527 -0.0012 0.0028
2.9995 0.0000 -5.0000 -0.0147 0.0557 -0.6941
0.9995 -5.0000 -1.0000 -0.0082 0.8390 -0.0745
1.9993 -5.0000 -3.0000 -0.0036 0.8610 -0.3516
4.9997 -2.0000 -1.0000 -0.2287 0.3475 -0.1250
4.9999 -2.0000 -0.0000 -0.2574 0.3371 0.0122
5.0001 -0.0000 1.0000 -0.2924 -0.0042 0.1232
4.9999 0.0000 -1.0000 -0.2350 0.0166 -0.1511
-5.0001 -1.0000 -0.0000 0.2669 0.1593 0.0271
-5.0002 -1.0000 -1.0000 0.2956 0.1697 -0.1101
5.0001 1.0000 0.0000 -0.2669 -0.1593 -0.0271
-4.9998 1.0000 1.0000 0.2318 -0.1821 0.1380

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22329
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.143
_diffrn_reflns_theta_min         4.549
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  44.00   1.00    2.00    --    0.00 -19.00  90.00  117
  2  ω    -21.00  69.00   1.00    2.00    --    0.00  57.00 -60.00   90
  3  ω     33.00 123.00   1.00    8.00    --   54.00  57.00 150.00   90
  4  ω     33.00 123.00   1.00    8.00    --   54.00  57.00-150.00   90
  5  ω    -18.00  80.00   1.00    8.00    --   54.00 -37.00-120.00   98
  6  ω     26.00 113.00   1.00    8.00    --   54.00-128.00 141.00   87
  7  ω      1.00  96.00   1.00    8.00    --   54.00 -99.00   0.00   95
  8  ω     36.00 116.00   1.00   25.00    --  108.00-111.00  30.00   80
  9  ω     36.00 134.00   1.00   25.00    --  108.00 -37.00-180.00   98
 10  ω     82.00 178.00   1.00   25.00    --  108.00  37.00 120.00   96
 11  ω     86.00 178.00   1.00   25.00    --  108.00  50.00   0.00   92
 12  ω     36.00 116.00   1.00   25.00    --  108.00-111.00-120.00   80
 13  ω     86.00 176.00   1.00   25.00    --  108.00  63.00  90.00   90
 14  ω    100.00 178.00   1.00   25.00    --  108.00 111.00 -60.00   78
 15  ω     36.00 146.00   1.00   25.00    --  108.00 -91.00  30.00  110
 16  ω    -71.00 -13.00   1.00    2.00    --    0.00 147.00 113.00   58
 17  ω    -30.00  70.00   1.00    2.00    --    0.00  77.00  90.00  100
 18  ω     28.00 126.00   1.00    8.00    --   54.00  37.00 -30.00   98
 19  ω     24.00 124.00   1.00    8.00    --   54.00  77.00-120.00  100
 20  ω    -18.00  55.00   1.00    8.00    --   54.00 -37.00  90.00   73
 21  ω     24.00 124.00   1.00    8.00    --   54.00  77.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0527379000
_diffrn_orient_matrix_UB_12      -0.0031602000
_diffrn_orient_matrix_UB_13      -0.0286926000
_diffrn_orient_matrix_UB_21      0.0012399000
_diffrn_orient_matrix_UB_22      -0.1654661000
_diffrn_orient_matrix_UB_23      -0.0104054000
_diffrn_orient_matrix_UB_31      -0.0027950000
_diffrn_orient_matrix_UB_32      -0.0130814000
_diffrn_orient_matrix_UB_33      0.1371527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4863
_reflns_number_total             5746
_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 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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    
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5746
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0392
_refine_ls_restrained_S_all      1.008
_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)+(0.0478P)²+1.5484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1016
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.71766(5) 0.49163(15) -0.07990(13) 0.0172(3) Uani 1 1 d . . . . .
C2 C 0.75890(5) 0.53385(16) 0.00253(13) 0.0177(3) Uani 1 1 d . . . . .
C3 C 0.77355(5) 0.67762(16) 0.00897(13) 0.0182(3) Uani 1 1 d . . . . .
H3 H 0.758779 0.745626 -0.044746 0.022 Uiso 1 1 calc R U . . .
C4 C 0.81010(5) 0.71770(16) 0.09563(13) 0.0181(3) Uani 1 1 d . . . . .
H4 H 0.820409 0.812467 0.099191 0.022 Uiso 1 1 calc R U . . .
C5 C 0.83156(5) 0.61576(16) 0.17794(13) 0.0179(3) Uani 1 1 d . . . . .
C6 C 0.81830(5) 0.47220(17) 0.16770(14) 0.0213(3) Uani 1 1 d . . . . .
H6 H 0.833748 0.403655 0.219629 0.026 Uiso 1 1 calc R U . . .
C7 C 0.78207(5) 0.43130(16) 0.08013(14) 0.0205(3) Uani 1 1 d . . . . .
H7 H 0.773197 0.335180 0.073149 0.025 Uiso 1 1 calc R U . . .
C8 C 0.88277(5) 0.56681(16) 0.36201(13) 0.0203(3) Uani 1 1 d . . . . .
H8A H 0.899212 0.489026 0.329375 0.024 Uiso 1 1 calc R U . . .
H8B H 0.857841 0.525788 0.398649 0.024 Uiso 1 1 calc R U . . .
C9 C 0.91468(5) 0.65036(16) 0.45614(13) 0.0200(3) Uani 1 1 d . . . . .
H9A H 0.897243 0.722580 0.492635 0.024 Uiso 1 1 calc R U . . .
H9B H 0.937308 0.699830 0.416278 0.024 Uiso 1 1 calc R U . . .
C10 C 0.93915(5) 0.55319(17) 0.55614(14) 0.0212(3) Uani 1 1 d . . . . .
H10A H 0.956956 0.481855 0.519808 0.025 Uiso 1 1 calc R U . . .
H10B H 0.916522 0.502655 0.595236 0.025 Uiso 1 1 calc R U . . .
C11 C 0.97086(5) 0.63809(17) 0.65217(13) 0.0208(3) Uani 1 1 d . . . . .
H11A H 0.991516 0.695418 0.611518 0.025 Uiso 1 1 calc R U . . .
H11B H 0.952494 0.703863 0.692631 0.025 Uiso 1 1 calc R U . . .
C12 C 0.99919(5) 0.54444(16) 0.74837(14) 0.0207(3) Uani 1 1 d . . . . .
H12A H 1.017177 0.477404 0.708002 0.025 Uiso 1 1 calc R U . . .
H12B H 0.978591 0.488584 0.790404 0.025 Uiso 1 1 calc R U . . .
C13 C 1.03136(5) 0.63059(17) 0.84215(14) 0.0212(3) Uani 1 1 d . . . . .
H13A H 1.051205 0.689072 0.799814 0.025 Uiso 1 1 calc R U . . .
H13B H 1.013260 0.695226 0.884465 0.025 Uiso 1 1 calc R U . . .
C14 C 1.06092(5) 0.53738(17) 0.93578(14) 0.0210(3) Uani 1 1 d . . . . .
H14A H 1.079709 0.474968 0.893527 0.025 Uiso 1 1 calc R U . . .
H14B H 1.041044 0.476512 0.976004 0.025 Uiso 1 1 calc R U . . .
C15 C 1.09214(5) 0.62255(16) 1.03264(14) 0.0213(3) Uani 1 1 d . . . . .
H15A H 1.112059 0.683464 0.992619 0.026 Uiso 1 1 calc R U . . .
H15B H 1.073407 0.684758 1.075245 0.026 Uiso 1 1 calc R U . . .
C16 C 1.12157(5) 0.52766(16) 1.12557(14) 0.0210(3) Uani 1 1 d . . . . .
H16A H 1.101809 0.463760 1.163339 0.025 Uiso 1 1 calc R U . . .
H16B H 1.141431 0.468635 1.083732 0.025 Uiso 1 1 calc R U . . .
C17 C 1.15081(6) 0.61489(17) 1.22439(15) 0.0255(3) Uani 1 1 d . . . . .
H17A H 1.172046 0.673056 1.188162 0.038 Uiso 1 1 calc R U . . .
H17B H 1.167431 0.550746 1.283042 0.038 Uiso 1 1 calc R U . . .
H17C H 1.131391 0.675909 1.264321 0.038 Uiso 1 1 calc R U . . .
C18 C 0.65151(5) 0.40296(16) -0.15245(14) 0.0195(3) Uani 1 1 d . . . . .
C19 C 0.60545(5) 0.32980(17) -0.16576(14) 0.0235(3) Uani 1 1 d . . . . .
C20 C 0.56564(5) 0.43269(19) -0.15069(15) 0.0279(4) Uani 1 1 d . . . . .
C21 C 0.51755(6) 0.3652(3) -0.1640(2) 0.0455(5) Uani 1 1 d . . . . .
C22 C 0.73422(5) 0.59728(19) -0.27716(14) 0.0256(3) Uani 1 1 d . . . . .
H22A H 0.724132 0.695623 -0.284267 0.038 Uiso 1 1 calc R U . . .
H22B H 0.730149 0.553498 -0.356526 0.038 Uiso 1 1 calc R U . . .
H22C H 0.766060 0.594226 -0.242519 0.038 Uiso 1 1 calc R U . . .
C23 C 0.67652(6) 0.37392(18) 0.07703(13) 0.0239(3) Uani 1 1 d . . . . .
H23A H 0.697098 0.428982 0.134727 0.036 Uiso 1 1 calc R U . . .
H23B H 0.683400 0.273303 0.088042 0.036 Uiso 1 1 calc R U . . .
H23C H 0.645511 0.391352 0.089722 0.036 Uiso 1 1 calc R U . . .
F1 F 0.59627(3) 0.27181(12) -0.27845(9) 0.0359(3) Uani 1 1 d . . . . .
F2 F 0.60572(3) 0.22288(11) -0.08364(10) 0.0348(2) Uani 1 1 d . . . . .
F3 F 0.56427(4) 0.53783(12) -0.23296(11) 0.0428(3) Uani 1 1 d . . . . .
F4 F 0.57422(4) 0.49175(13) -0.03899(10) 0.0418(3) Uani 1 1 d . . . . .
F5 F 0.50604(4) 0.3074(2) -0.27224(16) 0.0817(6) Uani 1 1 d . . . . .
F6 F 0.48711(4) 0.46638(16) -0.15030(13) 0.0586(4) Uani 1 1 d . . . . .
F7 F 0.51524(5) 0.2671(2) -0.0809(2) 0.0937(6) Uani 1 1 d . . . . .
N1 N 0.70729(4) 0.51884(14) -0.19823(11) 0.0186(3) Uani 1 1 d . . . . .
N2 N 0.66571(4) 0.46403(14) -0.24550(11) 0.0207(3) Uani 1 1 d . . . . .
N3 N 0.68196(4) 0.41714(13) -0.04799(11) 0.0176(3) Uani 1 1 d . . . . .
O1 O 0.86498(4) 0.66605(11) 0.26575(9) 0.0212(2) Uani 1 1 d . . . . .
B15 B 0.73870(7) 0.4251(2) 0.39720(16) 0.0248(4) Uani 1 1 d . . . . .
F8 F 0.74011(4) 0.29891(10) 0.33062(9) 0.0336(2) Uani 1 1 d . . . . .
F9 F 0.77817(4) 0.43856(13) 0.48155(10) 0.0439(3) Uani 1 1 d . . . . .
F10 F 0.73441(3) 0.54382(10) 0.31968(9) 0.0300(2) Uani 1 1 d . . . . .
F11 F 0.70081(4) 0.42015(13) 0.45913(10) 0.0433(3) Uani 1 1 d . . . . .
C24 C 0.62692(6) 0.6344(2) 0.29280(17) 0.0384(4) Uani 1 1 d . . . . .
H24A H 0.635550 0.534655 0.295629 0.058 Uiso 1 1 calc R U . . .
H24B H 0.648082 0.688628 0.252939 0.058 Uiso 1 1 calc R U . . .
H24C H 0.596550 0.644513 0.248243 0.058 Uiso 1 1 calc R U . . .
C25 C 0.62781(6) 0.68952(18) 0.41955(17) 0.0309(4) Uani 1 1 d . . . . .
C26 C 0.59700(7) 0.6172(2) 0.49637(17) 0.0383(4) Uani 1 1 d . . . . .
H26A H 0.590949 0.681693 0.559762 0.057 Uiso 1 1 calc R U . . .
H26B H 0.611616 0.531819 0.532259 0.057 Uiso 1 1 calc R U . . .
H26C H 0.568659 0.591832 0.446405 0.057 Uiso 1 1 calc R U . . .
O2 O 0.65277(5) 0.78673(15) 0.45978(15) 0.0487(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.4603(19) . ?
C1 N1 1.3252(19) . ?
C1 N3 1.3509(19) . ?
C2 C3 1.402(2) . ?
C2 C7 1.392(2) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.398(2) . ?
C5 C6 1.389(2) . ?
C5 O1 1.3592(17) . ?
C6 H6 0.9300 . ?
C6 C7 1.384(2) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.510(2) . ?
C8 O1 1.4469(17) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.524(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.526(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.524(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.524(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.521(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.526(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.523(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.521(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.506(2) . ?
C18 N2 1.300(2) . ?
C18 N3 1.3604(18) . ?
C19 C20 1.542(2) . ?
C19 F1 1.3495(18) . ?
C19 F2 1.3461(19) . ?
C20 C21 1.537(2) . ?
C20 F3 1.332(2) . ?
C20 F4 1.343(2) . ?
C21 F5 1.311(3) . ?
C21 F6 1.324(2) . ?
C21 F7 1.305(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 N1 1.462(2) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 N3 1.4746(19) . ?
N1 N2 1.3577(17) . ?
B15 F8 1.389(2) . ?
B15 F9 1.384(2) . ?
B15 F10 1.392(2) . ?
B15 F11 1.398(2) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.492(3) . ?
C25 C26 1.495(3) . ?
C25 O2 1.207(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?

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
N1 C1 C2 127.88(14) . . ?
N1 C1 N3 106.51(12) . . ?
N3 C1 C2 125.61(13) . . ?
C3 C2 C1 120.60(13) . . ?
C7 C2 C1 119.21(13) . . ?
C7 C2 C3 120.09(13) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.61(13) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.00(14) . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.15(13) . . ?
O1 C5 C4 116.27(13) . . ?
O1 C5 C6 123.58(13) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 119.92(14) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 H7 120.0 . . ?
C6 C7 C2 120.06(14) . . ?
C6 C7 H7 120.0 . . ?
H8A C8 H8B 108.5 . . ?
C9 C8 H8A 110.2 . . ?
C9 C8 H8B 110.2 . . ?
O1 C8 H8A 110.2 . . ?
O1 C8 H8B 110.2 . . ?
O1 C8 C9 107.52(12) . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C8 C9 C10 112.07(13) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C9 C10 C11 112.00(13) . . ?
H10A C10 H10B 107.9 . . ?
C11 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C10 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 C10 114.01(13) . . ?
C12 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
C11 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C11 C12 C13 113.38(13) . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C12 C13 H13A 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 C12 113.60(13) . . ?
C14 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C13 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
C13 C14 C15 114.08(13) . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
C14 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C14 113.44(13) . . ?
C16 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C15 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 C15 112.47(13) . . ?
C17 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 120.86(13) . . ?
N2 C18 N3 112.47(13) . . ?
N3 C18 C19 126.65(14) . . ?
C18 C19 C20 113.60(13) . . ?
F1 C19 C18 108.81(13) . . ?
F1 C19 C20 107.33(13) . . ?
F2 C19 C18 110.69(13) . . ?
F2 C19 C20 108.09(13) . . ?
F2 C19 F1 108.15(13) . . ?
C21 C20 C19 116.35(15) . . ?
F3 C20 C19 108.95(13) . . ?
F3 C20 C21 107.49(15) . . ?
F3 C20 F4 108.28(14) . . ?
F4 C20 C19 108.20(13) . . ?
F4 C20 C21 107.33(15) . . ?
F5 C21 C20 111.26(17) . . ?
F5 C21 F6 108.03(18) . . ?
F6 C21 C20 109.39(17) . . ?
F7 C21 C20 111.25(17) . . ?
F7 C21 F5 109.0(2) . . ?
F7 C21 F6 107.79(19) . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
C1 N1 C22 128.47(13) . . ?
C1 N1 N2 111.74(12) . . ?
N2 N1 C22 119.78(12) . . ?
C18 N2 N1 103.76(12) . . ?
C1 N3 C18 105.51(12) . . ?
C1 N3 C23 125.82(12) . . ?
C18 N3 C23 128.45(13) . . ?
C5 O1 C8 116.88(11) . . ?
F8 B15 F10 110.34(13) . . ?
F8 B15 F11 108.89(14) . . ?
F9 B15 F8 110.21(15) . . ?
F9 B15 F10 109.51(14) . . ?
F9 B15 F11 108.94(14) . . ?
F10 B15 F11 108.91(15) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C24 C25 C26 117.17(16) . . ?
O2 C25 C24 121.84(18) . . ?
O2 C25 C26 120.98(18) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 173.92(13) . . . . ?
C1 C2 C7 C6 -173.20(14) . . . . ?
C1 N1 N2 C18 -0.16(16) . . . . ?
C2 C1 N1 C22 0.2(3) . . . . ?
C2 C1 N1 N2 -179.41(14) . . . . ?
C2 C1 N3 C18 179.66(14) . . . . ?
C2 C1 N3 C23 4.7(2) . . . . ?
C2 C3 C4 C5 -1.4(2) . . . . ?
C3 C2 C7 C6 3.0(2) . . . . ?
C3 C4 C5 C6 4.4(2) . . . . ?
C3 C4 C5 O1 -175.36(13) . . . . ?
C4 C5 C6 C7 -3.6(2) . . . . ?
C4 C5 O1 C8 171.13(13) . . . . ?
C5 C6 C7 C2 -0.1(2) . . . . ?
C6 C5 O1 C8 -8.6(2) . . . . ?
C7 C2 C3 C4 -2.3(2) . . . . ?
C8 C9 C10 C11 -179.17(13) . . . . ?
C9 C8 O1 C5 -173.04(12) . . . . ?
C9 C10 C11 C12 -175.08(13) . . . . ?
C10 C11 C12 C13 178.87(13) . . . . ?
C11 C12 C13 C14 -177.99(13) . . . . ?
C12 C13 C14 C15 -178.10(13) . . . . ?
C13 C14 C15 C16 -179.90(13) . . . . ?
C14 C15 C16 C17 -177.43(13) . . . . ?
C18 C19 C20 C21 179.60(15) . . . . ?
C18 C19 C20 F3 57.96(18) . . . . ?
C18 C19 C20 F4 -59.55(18) . . . . ?
C19 C18 N2 N1 179.05(13) . . . . ?
C19 C18 N3 C1 -179.04(14) . . . . ?
C19 C18 N3 C23 -4.3(2) . . . . ?
C19 C20 C21 F5 -60.0(2) . . . . ?
C19 C20 C21 F6 -179.27(16) . . . . ?
C19 C20 C21 F7 61.8(2) . . . . ?
C22 N1 N2 C18 -179.84(13) . . . . ?
F1 C19 C20 C21 59.3(2) . . . . ?
F1 C19 C20 F3 -62.36(17) . . . . ?
F1 C19 C20 F4 -179.88(13) . . . . ?
F2 C19 C20 C21 -57.15(19) . . . . ?
F2 C19 C20 F3 -178.79(12) . . . . ?
F2 C19 C20 F4 63.69(16) . . . . ?
F3 C20 C21 F5 62.4(2) . . . . ?
F3 C20 C21 F6 -56.9(2) . . . . ?
F3 C20 C21 F7 -175.83(18) . . . . ?
F4 C20 C21 F5 178.70(17) . . . . ?
F4 C20 C21 F6 59.4(2) . . . . ?
F4 C20 C21 F7 -59.5(2) . . . . ?
N1 C1 C2 C3 51.8(2) . . . . ?
N1 C1 C2 C7 -132.00(16) . . . . ?
N1 C1 N3 C18 0.36(16) . . . . ?
N1 C1 N3 C23 -174.59(13) . . . . ?
N2 C18 C19 C20 -86.51(18) . . . . ?
N2 C18 C19 F1 33.0(2) . . . . ?
N2 C18 C19 F2 151.67(14) . . . . ?
N2 C18 N3 C1 -0.50(17) . . . . ?
N2 C18 N3 C23 174.27(14) . . . . ?
N3 C1 C2 C3 -127.36(16) . . . . ?
N3 C1 C2 C7 48.9(2) . . . . ?
N3 C1 N1 C22 179.51(14) . . . . ?
N3 C1 N1 N2 -0.13(16) . . . . ?
N3 C18 C19 C20 91.92(19) . . . . ?
N3 C18 C19 F1 -148.60(15) . . . . ?
N3 C18 C19 F2 -29.9(2) . . . . ?
N3 C18 N2 N1 0.41(17) . . . . ?
O1 C5 C6 C7 176.10(14) . . . . ?
O1 C8 C9 C10 -174.39(12) . . . . ?

_olex2_date_sample_data_collection 2017-03-21
_olex2_date_sample_submission    2017-03-08
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id 'NV 2570'
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.820
####################################################################### 
# 
# 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_dwb1715
_database_code_depnum_ccdc_archive 'CCDC 2177844'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-05-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H31 F7 N3 O, C F3 O3 S'
_chemical_formula_sum            'C24 H31 F10 N3 O4 S'
_chemical_formula_weight         647.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H31 F10 N3 O4 S1'
_chemical_oxdiff_usercomment     'Alessio NV2554'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.2841(3)
_cell_length_b                   14.1569(5)
_cell_length_c                   34.4881(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.596(3)
_cell_angle_gamma                90
_cell_volume                     5997.3(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4390
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      69.6540
_cell_measurement_theta_min      4.7410
_shelx_estimated_absorpt_T_max   0.982
_shelx_estimated_absorpt_T_min   0.598
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 -1 0.0628
0 0 1 0.0073
0 0 -1 0.0063
-5 5 -1 0.1003
4 5 1 0.1179
0 -1 0 0.1496
5 0 1 0.0770

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.01
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
-4.9991 0.0119 -1.0490 -0.0845 -0.0181 -0.6235
-0.0006 -0.0014 1.0010 -0.0018 -0.0444 0.0052
0.0006 0.0014 -1.0010 0.0018 0.0444 -0.0052
-5.0016 5.0120 -0.8805 -0.6230 0.0074 -0.5519
3.9967 4.9903 1.2079 -0.4714 0.0312 0.5714
0.0005 -1.0000 -0.0337 0.1077 -0.0051 -0.0143
4.9991 -0.0119 1.0490 0.0845 0.0181 0.6235

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            21199
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         3.375
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  68.00   1.00   10.00    --    0.00  57.00 -30.00   89
  2  ω     84.00 114.00   1.00   40.00    --   54.00 156.00 -73.00   30
  3  ω      9.00  79.00   1.00   40.00    --   54.00 -19.00  60.00   70
  4  ω      1.00  84.00   1.00   40.00    --   54.00 -99.00 -30.00   83
  5  ω     25.00 122.00   1.00   40.00    --   54.00  77.00  60.00   97
  6  ω     48.00 116.00   1.00   60.00    --  108.00-111.00 120.00   68
  7  ω    101.00 174.00   1.00   60.00    --  108.00 111.00  30.00   73
  8  ω    132.00 176.00   1.00   60.00    --  108.00  63.00  90.00   44
  9  ω     94.00 131.00   1.00   60.00    --  108.00 -37.00  30.00   37
 10  ω     37.00  64.00   1.00   60.00    --  108.00 -37.00  30.00   27
 11  ω     62.00 130.00   1.00   60.00    --  108.00 -63.00  60.00   68
 12  ω     44.00 116.00   1.00   60.00    --  108.00-111.00-120.00   72
 13  ω     82.00 178.00   1.00   60.00    --  108.00  37.00-150.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0170485000
_diffrn_orient_matrix_UB_12      -0.1076376000
_diffrn_orient_matrix_UB_13      -0.0019405000
_diffrn_orient_matrix_UB_21      0.0129433000
_diffrn_orient_matrix_UB_22      0.0066057000
_diffrn_orient_matrix_UB_23      -0.0443110000
_diffrn_orient_matrix_UB_31      0.1236283000
_diffrn_orient_matrix_UB_32      0.0141946000
_diffrn_orient_matrix_UB_33      0.0053363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8220
_reflns_number_total             10655
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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         1.291
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         10655
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.1130
_refine_ls_restrained_S_all      1.047
_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)+(0.0426P)²+70.6624P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2752
_refine_special_details          
;
The diffraction was weak and smeared in certain directions presumably due 
to slippage of layers within the crystal.  This led to the low quality of 
the result.   Both of the decyl chains were disordered.  For one terminal 
propyl chain was modelled in two positions with refined occupancies of
0.725:0.275(17).  For the other, the terminal hexyl chain was modelled in 
two positions with refined occupancies of 0.723:0.277(8).
For the disordered chains, the C-C bond lengths were restrained to be 
1.52 angstroms and the C-C-C distances restrained to be 2.48 angstroms.  
The ADP of disordered pairs of atoms were constrained to be equal.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.939(2)
 0.061(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C37A-C36 = C38A-C37A = C38A-C39A
 1.52 with sigma of 0.01
 C38A-C39A = C39A-C40A = C41A-C40A = C41A-C42A = C43A-C42A
 1.52 with sigma of 0.01
 C18A-C17 = C18-C17 = C19-C18 = C19A-C18A = C20-C19 = C20A-C19A
 1.52 with sigma of 0.01
 C38A-C40A = C41A-C43A = C39A-C41A = C40A-C42A
 2.48 with sigma of 0.01
 C17-C19 = C17-C19A = C18A-C20A = C18-C20
 2.48 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C18A)
Uanis(C19A) = Uanis(C19)
Uanis(C20A) = Uanis(C20)
Uanis(C43) = Uanis(C43A)
Uanis(C40A) = Uanis(C40)
Uanis(C39) = Uanis(C39A)
Uanis(C38) = Uanis(C38A)
Uanis(C41A) = Uanis(C41)
Uanis(C37) = Uanis(C37A)
Uanis(C42) = Uanis(C42A)
Uanis(C7) = Uanis(C8)
Uanis(C10) = Uanis(C9)
Uanis(C33) = Uanis(C32)
5. Others
 Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38C)=
 Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=
 Sof(C41A)=Sof(H41C)=Sof(H41D)=Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43A)=
 Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37C)=Sof(H37D)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=
 FVAR(1)
 Sof(H17C)=Sof(H17D)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=
 Sof(H19D)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
6.a Riding coordinates:
 C43A(H43D,H43E,H43F)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C16(H16A,H16B), C17(H17A,H17B), C17(H17C,H17D), C18(H18A,H18B),
 C18A(H18C,H18D), C19(H19A,H19B), C19A(H19C,H19D), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C36(H36C,H36D), C37A(H37A,H37B), C37(H37C,H37D),
 C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D), C40(H40A,
 H40B), C40A(H40C,H40D), C41(H41A,H41B), C41A(H41C,H41D), C42(H42A,H42B),
 C42A(H42C,H42D)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C25(H25), C26(H26), C28(H28), C29(H29)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C20A(H20D,H20E,
 H20F), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   mixed
_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
C1 C 0.9729(6) 0.5212(6) 0.6290(2) 0.0385(19) Uani 1 1 d . . . . .
C2 C 0.9659(6) 0.5773(6) 0.6613(2) 0.0380(18) Uani 1 1 d . . . . .
H2 H 1.004904 0.635213 0.662400 0.046 Uiso 1 1 calc R U . . .
C3 C 0.9026(6) 0.5505(6) 0.6924(2) 0.0380(18) Uani 1 1 d . . . . .
H3 H 0.896716 0.590691 0.714341 0.046 Uiso 1 1 calc R U . . .
C4 C 0.8471(5) 0.4641(5) 0.6915(2) 0.0311(16) Uani 1 1 d . . . . .
C5 C 0.8574(6) 0.4063(6) 0.6593(2) 0.0413(19) Uani 1 1 d . . . . .
H5 H 0.822005 0.346649 0.658823 0.050 Uiso 1 1 calc R U . . .
C6 C 0.9182(7) 0.4345(6) 0.6282(3) 0.0421(19) Uani 1 1 d . . . . .
H6 H 0.923174 0.395033 0.605981 0.050 Uiso 1 1 calc R U . . .
C7 C 0.7835(5) 0.4378(5) 0.7254(2) 0.0304(11) Uani 1 1 d . . . . .
C8 C 0.7316(6) 0.3752(5) 0.7793(2) 0.0304(11) Uani 1 1 d . . . . .
C9 C 0.9167(6) 0.3201(6) 0.7530(2) 0.0362(13) Uani 1 1 d . . . . .
H9A H 0.943730 0.312616 0.779675 0.054 Uiso 1 1 calc R U . . .
H9B H 0.970811 0.354125 0.737706 0.054 Uiso 1 1 calc R U . . .
H9C H 0.903614 0.257792 0.741545 0.054 Uiso 1 1 calc R U . . .
C10 C 0.6190(6) 0.5401(5) 0.7153(2) 0.0362(13) Uani 1 1 d . . . . .
H10A H 0.543541 0.517863 0.713712 0.054 Uiso 1 1 calc R U . . .
H10B H 0.646754 0.550281 0.689100 0.054 Uiso 1 1 calc R U . . .
H10C H 0.621871 0.599566 0.729816 0.054 Uiso 1 1 calc R U . . .
C11 C 1.0945(7) 0.6280(6) 0.5976(3) 0.044(2) Uani 1 1 d . . . . .
H11A H 1.149190 0.626324 0.618823 0.053 Uiso 1 1 calc R U . . .
H11B H 1.046196 0.683086 0.601517 0.053 Uiso 1 1 calc R U . . .
C12 C 1.1494(8) 0.6345(7) 0.5591(3) 0.056(3) Uani 1 1 d . . . . .
H12A H 1.190819 0.575546 0.554688 0.067 Uiso 1 1 calc R U . . .
H12B H 1.202248 0.687248 0.559949 0.067 Uiso 1 1 calc R U . . .
C13 C 1.0721(8) 0.6499(7) 0.5248(3) 0.056(2) Uani 1 1 d . . . . .
H13A H 1.013418 0.602033 0.525819 0.067 Uiso 1 1 calc R U . . .
H13B H 1.112507 0.640023 0.500471 0.067 Uiso 1 1 calc R U . . .
C14 C 1.0205(7) 0.7491(7) 0.5241(3) 0.051(2) Uani 1 1 d . . . . .
H14A H 0.982701 0.759784 0.548937 0.061 Uiso 1 1 calc R U . . .
H14B H 1.079198 0.796712 0.522159 0.061 Uiso 1 1 calc R U . . .
C15 C 0.9403(7) 0.7645(7) 0.4912(3) 0.051(2) Uani 1 1 d . . . . .
H15A H 0.881103 0.717344 0.493311 0.061 Uiso 1 1 calc R U . . .
H15B H 0.977845 0.752849 0.466344 0.061 Uiso 1 1 calc R U . . .
C16 C 0.8903(7) 0.8622(7) 0.4899(3) 0.053(2) Uani 1 1 d . . . . .
H16A H 0.949046 0.909694 0.487482 0.063 Uiso 1 1 calc R U . . .
H16B H 0.852461 0.874262 0.514653 0.063 Uiso 1 1 calc R U . . .
C17 C 0.8096(7) 0.8744(7) 0.4564(3) 0.058(3) Uani 1 1 d D . . . .
H17A H 0.848706 0.861392 0.431962 0.070 Uiso 0.725(17) 1 calc R U P A 1
H17B H 0.752684 0.825338 0.458924 0.070 Uiso 0.725(17) 1 calc R U P A 1
H17C H 0.847184 0.870318 0.431146 0.070 Uiso 0.275(17) 1 calc R U P A 2
H17D H 0.752338 0.825240 0.457197 0.070 Uiso 0.275(17) 1 calc R U P A 2
C18 C 0.7534(17) 0.9689(10) 0.4521(5) 0.068(4) Uani 0.725(17) 1 d D . P A 1
H18A H 0.808319 1.018958 0.447836 0.082 Uiso 0.725(17) 1 calc R U P A 1
H18B H 0.713905 0.983979 0.476212 0.082 Uiso 0.725(17) 1 calc R U P A 1
C18A C 0.761(4) 0.972(2) 0.4621(15) 0.068(4) Uani 0.275(17) 1 d D . P A 2
H18C H 0.819961 1.018268 0.467100 0.082 Uiso 0.275(17) 1 calc R U P A 2
H18D H 0.712557 0.971461 0.484868 0.082 Uiso 0.275(17) 1 calc R U P A 2
C19 C 0.6738(13) 0.9662(10) 0.4180(4) 0.069(5) Uani 0.725(17) 1 d D . P A 1
H19A H 0.714017 0.957875 0.393549 0.083 Uiso 0.725(17) 1 calc R U P A 1
H19B H 0.623414 0.912069 0.420949 0.083 Uiso 0.725(17) 1 calc R U P A 1
C19A C 0.697(3) 1.001(2) 0.4261(14) 0.069(5) Uani 0.275(17) 1 d D . P A 2
H19C H 0.705693 1.069340 0.421401 0.083 Uiso 0.275(17) 1 calc R U P A 2
H19D H 0.724134 0.966283 0.403258 0.083 Uiso 0.275(17) 1 calc R U P A 2
C20 C 0.6096(15) 1.0576(11) 0.4167(5) 0.093(6) Uani 0.725(17) 1 d D . P A 1
H20A H 0.565074 1.059406 0.392951 0.139 Uiso 0.725(17) 1 calc R U P A 1
H20B H 0.660064 1.111257 0.416873 0.139 Uiso 0.725(17) 1 calc R U P A 1
H20C H 0.562302 1.061314 0.439326 0.139 Uiso 0.725(17) 1 calc R U P A 1
C20A C 0.577(3) 0.978(4) 0.4320(15) 0.093(6) Uani 0.275(17) 1 d D . P A 2
H20D H 0.536684 0.989795 0.407769 0.139 Uiso 0.275(17) 1 calc R U P A 2
H20E H 0.547989 1.018330 0.452530 0.139 Uiso 0.275(17) 1 calc R U P A 2
H20F H 0.569385 0.911625 0.439321 0.139 Uiso 0.275(17) 1 calc R U P A 2
C21 C 0.7267(6) 0.3174(6) 0.8159(2) 0.0359(18) Uani 1 1 d . . . . .
C22 C 0.7789(6) 0.3699(6) 0.8509(2) 0.0396(19) Uani 1 1 d . . . . .
C23 C 0.7767(8) 0.3170(7) 0.8903(3) 0.050(2) Uani 1 1 d . . . . .
F1 F 0.7769(4) 0.2344(3) 0.81137(14) 0.0401(11) Uani 1 1 d . . . . .
F2 F 0.6207(3) 0.3009(3) 0.82412(14) 0.0400(11) Uani 1 1 d . . . . .
F3 F 0.8845(3) 0.3864(4) 0.84252(14) 0.0427(11) Uani 1 1 d . . . . .
F4 F 0.7282(4) 0.4528(3) 0.85551(14) 0.0454(11) Uani 1 1 d . . . . .
F5 F 0.8274(6) 0.2360(5) 0.88757(17) 0.078(2) Uani 1 1 d . . . . .
F6 F 0.6751(5) 0.3010(5) 0.90070(16) 0.0676(17) Uani 1 1 d . . . . .
F7 F 0.8242(5) 0.3697(5) 0.91712(16) 0.0685(17) Uani 1 1 d . . . . .
N1 N 0.8137(4) 0.3744(4) 0.75325(18) 0.0297(13) Uani 1 1 d . . . . .
N2 N 0.6865(5) 0.4686(4) 0.73532(18) 0.0307(14) Uani 1 1 d . . . . .
N3 N 0.6531(5) 0.4332(4) 0.76934(19) 0.0337(14) Uani 1 1 d . . . . .
O1 O 1.0316(5) 0.5413(4) 0.59686(17) 0.0448(14) Uani 1 1 d . . . . .
C24 C 0.4839(6) 0.5105(6) 0.8735(2) 0.0354(17) Uani 1 1 d . . . . .
C25 C 0.4658(6) 0.5756(5) 0.8441(2) 0.0381(18) Uani 1 1 d . . . . .
H25 H 0.497817 0.636654 0.845299 0.046 Uiso 1 1 calc R U . . .
C26 C 0.3997(6) 0.5500(5) 0.8128(2) 0.0357(17) Uani 1 1 d . . . . .
H26 H 0.385336 0.594421 0.792719 0.043 Uiso 1 1 calc R U . . .
C27 C 0.3552(5) 0.4612(5) 0.8106(2) 0.0301(16) Uani 1 1 d . . . . .
C28 C 0.3744(6) 0.3946(6) 0.8400(2) 0.0373(18) Uani 1 1 d . . . . .
H28 H 0.344167 0.332891 0.838345 0.045 Uiso 1 1 calc R U . . .
C29 C 0.4384(6) 0.4207(6) 0.8718(2) 0.0384(18) Uani 1 1 d . . . . .
H29 H 0.451024 0.377076 0.892269 0.046 Uiso 1 1 calc R U . . .
C30 C 0.2881(6) 0.4349(5) 0.7766(2) 0.0317(16) Uani 1 1 d . . . . .
C31 C 0.2296(6) 0.3789(5) 0.7221(2) 0.0316(16) Uani 1 1 d . . . . .
C32 C 0.4186(6) 0.3231(6) 0.7457(2) 0.0366(13) Uani 1 1 d . . . . .
H32A H 0.406791 0.257928 0.754276 0.055 Uiso 1 1 calc R U . . .
H32B H 0.472848 0.353317 0.762675 0.055 Uiso 1 1 calc R U . . .
H32C H 0.444810 0.323062 0.718991 0.055 Uiso 1 1 calc R U . . .
C33 C 0.1246(6) 0.5356(6) 0.7893(2) 0.0366(13) Uani 1 1 d . . . . .
H33A H 0.128414 0.597775 0.776869 0.055 Uiso 1 1 calc R U . . .
H33B H 0.153018 0.540079 0.815889 0.055 Uiso 1 1 calc R U . . .
H33C H 0.048719 0.514337 0.789781 0.055 Uiso 1 1 calc R U . . .
C34 C 0.6068(6) 0.6158(6) 0.9070(3) 0.0416(19) Uani 1 1 d . . . . .
H34A H 0.555948 0.669143 0.910935 0.050 Uiso 1 1 calc R U . . .
H34B H 0.646458 0.626305 0.882570 0.050 Uiso 1 1 calc R U . . .
C35 C 0.6862(7) 0.6089(7) 0.9408(3) 0.050(2) Uani 1 1 d . . . . .
H35A H 0.739699 0.558256 0.935639 0.059 Uiso 1 1 calc R U . . .
H35B H 0.646152 0.591665 0.964579 0.059 Uiso 1 1 calc R U . . .
C36 C 0.7467(7) 0.7021(8) 0.9476(3) 0.057(3) Uani 1 1 d D . . . .
H36A H 0.696355 0.749267 0.958795 0.069 Uiso 0.722(8) 1 calc R U P B 1
H36B H 0.773230 0.726992 0.922630 0.069 Uiso 0.722(8) 1 calc R U P B 1
H36C H 0.770996 0.727157 0.922363 0.069 Uiso 0.278(8) 1 calc R U P B 2
H36D H 0.695605 0.748576 0.958846 0.069 Uiso 0.278(8) 1 calc R U P B 2
C37A C 0.845(15) 0.693(7) 0.975(7) 0.110(7) Uani 0.278(8) 1 d D . P B 2
H37A H 0.832497 0.642584 0.994047 0.132 Uiso 0.278(8) 1 calc R U P B 2
H37B H 0.910760 0.676321 0.959582 0.132 Uiso 0.278(8) 1 calc R U P B 2
C37 C 0.845(6) 0.686(3) 0.976(3) 0.110(7) Uani 0.722(8) 1 d . . P B 1
H37C H 0.816545 0.667395 1.001634 0.132 Uiso 0.722(8) 1 calc R U P B 1
H37D H 0.888943 0.632559 0.966244 0.132 Uiso 0.722(8) 1 calc R U P B 1
C38 C 0.9193(13) 0.7683(14) 0.9818(5) 0.075(5) Uani 0.722(8) 1 d . . P B 1
H38A H 0.881923 0.818295 0.996741 0.090 Uiso 0.722(8) 1 calc R U P B 1
H38B H 0.940389 0.794818 0.956439 0.090 Uiso 0.722(8) 1 calc R U P B 1
C38A C 0.859(2) 0.788(4) 0.9941(12) 0.075(5) Uani 0.278(8) 1 d D . P B 2
H38C H 0.792609 0.802536 1.009230 0.090 Uiso 0.278(8) 1 calc R U P B 2
H38D H 0.866438 0.837618 0.974030 0.090 Uiso 0.278(8) 1 calc R U P B 2
C39 C 1.0201(11) 0.7345(15) 1.0040(6) 0.082(5) Uani 0.722(8) 1 d . . P B 1
H39A H 1.060782 0.688380 0.988108 0.099 Uiso 0.722(8) 1 calc R U P B 1
H39B H 0.998450 0.703019 1.028351 0.099 Uiso 0.722(8) 1 calc R U P B 1
C39A C 0.958(2) 0.789(4) 1.0209(9) 0.082(5) Uani 0.278(8) 1 d D . P B 2
H39C H 0.970414 0.725680 1.031894 0.099 Uiso 0.278(8) 1 calc R U P B 2
H39D H 0.946153 0.834078 1.042490 0.099 Uiso 0.278(8) 1 calc R U P B 2
C40 C 1.1015(14) 0.8314(16) 1.0143(6) 0.086(5) Uani 0.722(8) 1 d . . P B 1
H40A H 1.173416 0.809674 1.023972 0.103 Uiso 0.722(8) 1 calc R U P B 1
H40B H 1.113114 0.868270 0.990284 0.103 Uiso 0.722(8) 1 calc R U P B 1
C40A C 1.056(2) 0.820(3) 0.9971(8) 0.086(5) Uani 0.278(8) 1 d D . P B 2
H40C H 1.076226 0.769267 0.978806 0.103 Uiso 0.278(8) 1 calc R U P B 2
H40D H 1.037829 0.877334 0.981967 0.103 Uiso 0.278(8) 1 calc R U P B 2
C41 C 1.0519(12) 0.8900(12) 1.0427(5) 0.071(4) Uani 0.722(8) 1 d . . P B 1
H41A H 1.028930 0.851600 1.065201 0.085 Uiso 0.722(8) 1 calc R U P B 1
H41B H 0.986967 0.921822 1.031605 0.085 Uiso 0.722(8) 1 calc R U P B 1
C41A C 1.151(2) 0.840(2) 1.0245(11) 0.071(4) Uani 0.278(8) 1 d D . P B 2
H41C H 1.209457 0.793934 1.020265 0.085 Uiso 0.278(8) 1 calc R U P B 2
H41D H 1.126250 0.834545 1.051692 0.085 Uiso 0.278(8) 1 calc R U P B 2
C42 C 1.1422(17) 0.9675(13) 1.0561(6) 0.088(5) Uani 0.722(8) 1 d . . P B 1
H42A H 1.209843 0.934777 1.064336 0.105 Uiso 0.722(8) 1 calc R U P B 1
H42B H 1.159777 1.008911 1.033905 0.105 Uiso 0.722(8) 1 calc R U P B 1
C42A C 1.193(4) 0.940(2) 1.0173(11) 0.088(5) Uani 0.278(8) 1 d D . P B 2
H42C H 1.236821 0.940942 0.993427 0.105 Uiso 0.278(8) 1 calc R U P B 2
H42D H 1.131105 0.984020 1.013916 0.105 Uiso 0.278(8) 1 calc R U P B 2
C43 C 1.0998(18) 1.0282(16) 1.0899(6) 0.105(6) Uani 0.722(8) 1 d . . P B 1
H43A H 1.029054 1.055431 1.082738 0.157 Uiso 0.722(8) 1 calc R U P B 1
H43B H 1.151663 1.079103 1.095512 0.157 Uiso 0.722(8) 1 calc R U P B 1
H43C H 1.091625 0.988550 1.113016 0.157 Uiso 0.722(8) 1 calc R U P B 1
C43A C 1.263(4) 0.970(3) 1.0519(13) 0.105(6) Uani 0.278(8) 1 d D . P B 2
H43D H 1.317978 1.014863 1.043428 0.157 Uiso 0.278(8) 1 d R U P B 2
H43E H 1.298188 0.914593 1.063568 0.157 Uiso 0.278(8) 1 d R U P B 2
H43F H 1.215658 0.999933 1.071088 0.157 Uiso 0.278(8) 1 d R U P B 2
C44 C 0.2210(6) 0.3268(5) 0.6839(2) 0.0346(17) Uani 1 1 d . . . . .
C45 C 0.2685(6) 0.3844(6) 0.6502(2) 0.0397(19) Uani 1 1 d . . . . .
C46 C 0.2616(8) 0.3398(8) 0.6098(3) 0.059(3) Uani 1 1 d . . . . .
F8 F 0.1154(3) 0.3094(3) 0.67623(14) 0.0430(11) Uani 1 1 d . . . . .
F9 F 0.2739(4) 0.2438(3) 0.68608(14) 0.0400(11) Uani 1 1 d . . . . .
F10 F 0.2159(4) 0.4680(3) 0.64856(14) 0.0471(12) Uani 1 1 d . . . . .
F11 F 0.3749(4) 0.4003(3) 0.65826(14) 0.0448(11) Uani 1 1 d . . . . .
F12 F 0.1598(5) 0.3202(5) 0.59993(17) 0.0729(18) Uani 1 1 d . . . . .
F13 F 0.3197(5) 0.2610(5) 0.60889(17) 0.0756(19) Uani 1 1 d . . . . .
F14 F 0.3020(6) 0.3994(6) 0.58401(17) 0.083(2) Uani 1 1 d . . . . .
N4 N 0.3153(4) 0.3758(4) 0.74761(18) 0.0294(13) Uani 1 1 d . . . . .
N5 N 0.1897(5) 0.4680(4) 0.76743(19) 0.0313(14) Uani 1 1 d . . . . .
N6 N 0.1531(5) 0.4356(4) 0.73318(19) 0.0319(14) Uani 1 1 d . . . . .
O2 O 0.5480(4) 0.5282(4) 0.90534(16) 0.0406(13) Uani 1 1 d . . . . .
C47 C 0.3902(6) 0.6941(7) 0.6631(3) 0.045(2) Uani 1 1 d . . . . .
F15 F 0.3600(5) 0.6431(6) 0.63272(16) 0.078(2) Uani 1 1 d . . . . .
F16 F 0.3757(5) 0.7852(4) 0.6541(2) 0.085(2) Uani 1 1 d . . . . .
F17 F 0.4989(3) 0.6827(4) 0.66675(15) 0.0463(12) Uani 1 1 d . . . . .
O3 O 0.2073(4) 0.6778(4) 0.69698(17) 0.0413(13) Uani 1 1 d . . . . .
O4 O 0.3515(4) 0.5662(4) 0.71335(17) 0.0401(13) Uani 1 1 d . . . . .
O5 O 0.3649(5) 0.7287(4) 0.73532(19) 0.0504(16) Uani 1 1 d . . . . .
S1 S 0.32002(14) 0.66287(13) 0.70696(6) 0.0321(4) Uani 1 1 d . . . . .
C48 C -0.0947(6) 0.6872(6) 0.8413(2) 0.0392(19) Uani 1 1 d . . . . .
F18 F -0.1191(4) 0.6249(4) 0.86923(14) 0.0525(13) Uani 1 1 d . . . . .
F19 F -0.1152(4) 0.7733(4) 0.85466(17) 0.0582(15) Uani 1 1 d . . . . .
F20 F 0.0104(3) 0.6802(4) 0.83439(14) 0.0441(12) Uani 1 1 d . . . . .
O6 O -0.1370(4) 0.7331(4) 0.77018(18) 0.0447(14) Uani 1 1 d . . . . .
O7 O -0.2868(4) 0.6768(4) 0.80931(18) 0.0438(14) Uani 1 1 d . . . . .
O8 O -0.1472(4) 0.5671(4) 0.78775(16) 0.0381(13) Uani 1 1 d . . . . .
S2 S -0.17626(14) 0.66287(13) 0.79712(6) 0.0318(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.373(12) . ?
C1 C6 1.398(12) . ?
C1 O1 1.359(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.400(11) . ?
C4 C5 1.384(11) . ?
C4 C7 1.464(10) . ?
C5 H5 0.9500 . ?
C5 C6 1.376(11) . ?
C6 H6 0.9500 . ?
C7 N1 1.362(10) . ?
C7 N2 1.317(9) . ?
C8 C21 1.508(11) . ?
C8 N1 1.357(9) . ?
C8 N3 1.309(9) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 N1 1.480(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N2 1.475(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.499(12) . ?
C11 O1 1.451(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.522(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.542(13) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.511(12) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.515(13) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.526(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 H17C 0.9900 . ?
C17 H17D 0.9900 . ?
C17 C18 1.513(9) . ?
C17 C18A 1.519(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.522(9) . ?
C18A H18C 0.9900 . ?
C18A H18D 0.9900 . ?
C18A C19A 1.521(10) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(9) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C19A C20A 1.519(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21 C22 1.551(12) . ?
C21 F1 1.336(9) . ?
C21 F2 1.355(8) . ?
C22 C23 1.551(12) . ?
C22 F3 1.352(9) . ?
C22 F4 1.338(9) . ?
C23 F5 1.308(11) . ?
C23 F6 1.321(10) . ?
C23 F7 1.321(11) . ?
N2 N3 1.344(9) . ?
C24 C25 1.387(11) . ?
C24 C29 1.390(11) . ?
C24 O2 1.368(9) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(11) . ?
C26 H26 0.9500 . ?
C26 C27 1.373(10) . ?
C27 C28 1.405(11) . ?
C27 C30 1.475(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.391(11) . ?
C29 H29 0.9500 . ?
C30 N4 1.347(10) . ?
C30 N5 1.331(9) . ?
C31 C44 1.511(11) . ?
C31 N4 1.367(9) . ?
C31 N6 1.297(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 N4 1.474(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 N5 1.462(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.516(11) . ?
C34 O2 1.437(10) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.532(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 H36C 0.9900 . ?
C36 H36D 0.9900 . ?
C36 C37A 1.520(11) . ?
C36 C37 1.57(2) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C37A C38A 1.520(10) . ?
C37 H37C 0.9900 . ?
C37 H37D 0.9900 . ?
C37 C38 1.49(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.53(2) . ?
C38A H38C 0.9900 . ?
C38A H38D 0.9900 . ?
C38A C39A 1.523(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.73(3) . ?
C39A H39C 0.9900 . ?
C39A H39D 0.9900 . ?
C39A C40A 1.528(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C40 C41 1.43(2) . ?
C40A H40C 0.9900 . ?
C40A H40D 0.9900 . ?
C40A C41A 1.516(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.63(2) . ?
C41A H41C 0.9900 . ?
C41A H41D 0.9900 . ?
C41A C42A 1.522(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C43 1.54(3) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C42A C43A 1.521(10) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43A H43D 0.9799 . ?
C43A H43E 0.9798 . ?
C43A H43F 0.9797 . ?
C44 C45 1.541(11) . ?
C44 F8 1.344(8) . ?
C44 F9 1.344(8) . ?
C45 C46 1.531(13) . ?
C45 F10 1.349(9) . ?
C45 F11 1.352(9) . ?
C46 F12 1.321(11) . ?
C46 F13 1.325(12) . ?
C46 F14 1.326(13) . ?
N5 N6 1.340(9) . ?
C47 F15 1.322(11) . ?
C47 F16 1.338(10) . ?
C47 F17 1.350(9) . ?
C47 S1 1.804(9) . ?
O3 S1 1.439(5) . ?
O4 S1 1.438(6) . ?
O5 S1 1.455(6) . ?
C48 F18 1.342(10) . ?
C48 F19 1.329(9) . ?
C48 F20 1.319(9) . ?
C48 S2 1.847(8) . ?
O6 S2 1.447(6) . ?
O7 S2 1.439(5) . ?
O8 S2 1.439(6) . ?

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
C2 C1 C6 119.4(7) . . ?
O1 C1 C2 125.5(8) . . ?
O1 C1 C6 115.2(8) . . ?
C1 C2 H2 119.6 . . ?
C1 C2 C3 120.7(8) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.9(8) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C7 117.9(7) . . ?
C5 C4 C3 119.1(7) . . ?
C5 C4 C7 123.0(7) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(8) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.2(8) . . ?
C5 C6 H6 119.9 . . ?
N1 C7 C4 126.0(6) . . ?
N2 C7 C4 127.9(7) . . ?
N2 C7 N1 106.1(6) . . ?
N1 C8 C21 125.9(6) . . ?
N3 C8 C21 121.7(7) . . ?
N3 C8 N1 112.4(7) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H11A C11 H11B 108.6 . . ?
C12 C11 H11A 110.5 . . ?
C12 C11 H11B 110.5 . . ?
O1 C11 H11A 110.5 . . ?
O1 C11 H11B 110.5 . . ?
O1 C11 C12 106.4(8) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C11 C12 C13 114.4(8) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
C12 C13 H13A 108.9 . . ?
C12 C13 H13B 108.9 . . ?
C12 C13 C14 113.3(9) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
C13 C14 H14A 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 C13 114.1(9) . . ?
C15 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
C14 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C14 C15 C16 114.4(8) . . ?
H15A C15 H15B 107.6 . . ?
C16 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C15 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C15 C16 C17 112.6(8) . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 H16A 109.1 . . ?
C17 C16 H16B 109.1 . . ?
C16 C17 H17A 107.9 . . ?
C16 C17 H17B 107.9 . . ?
C16 C17 H17C 110.8 . . ?
C16 C17 H17D 110.8 . . ?
H17A C17 H17B 107.2 . . ?
H17C C17 H17D 108.9 . . ?
C18 C17 C16 117.7(9) . . ?
C18 C17 H17A 107.9 . . ?
C18 C17 H17B 107.9 . . ?
C18A C17 C16 104.8(13) . . ?
C18A C17 H17C 110.8 . . ?
C18A C17 H17D 110.8 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
C17 C18 C19 109.9(8) . . ?
H18A C18 H18B 108.2 . . ?
C19 C18 H18A 109.7 . . ?
C19 C18 H18B 109.7 . . ?
C17 C18A H18C 109.7 . . ?
C17 C18A H18D 109.7 . . ?
C17 C18A C19A 109.8(10) . . ?
H18C C18A H18D 108.2 . . ?
C19A C18A H18C 109.7 . . ?
C19A C18A H18D 109.7 . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.3 . . ?
C20 C19 C18 109.4(8) . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C18A C19A H19C 109.8 . . ?
C18A C19A H19D 109.8 . . ?
H19C C19A H19D 108.3 . . ?
C20A C19A C18A 109.3(10) . . ?
C20A C19A H19C 109.8 . . ?
C20A C19A H19D 109.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19A C20A H20D 109.5 . . ?
C19A C20A H20E 109.5 . . ?
C19A C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
C8 C21 C22 111.8(7) . . ?
F1 C21 C8 110.9(6) . . ?
F1 C21 C22 109.0(6) . . ?
F1 C21 F2 108.6(6) . . ?
F2 C21 C8 108.4(6) . . ?
F2 C21 C22 108.1(6) . . ?
C23 C22 C21 116.0(7) . . ?
F3 C22 C21 107.8(6) . . ?
F3 C22 C23 107.2(7) . . ?
F4 C22 C21 108.9(6) . . ?
F4 C22 C23 107.9(7) . . ?
F4 C22 F3 108.8(7) . . ?
F5 C23 C22 110.4(7) . . ?
F5 C23 F6 108.8(9) . . ?
F5 C23 F7 109.8(8) . . ?
F6 C23 C22 110.2(7) . . ?
F7 C23 C22 109.1(8) . . ?
F7 C23 F6 108.5(8) . . ?
C7 N1 C9 124.4(6) . . ?
C8 N1 C7 105.2(6) . . ?
C8 N1 C9 130.5(6) . . ?
C7 N2 C10 127.8(7) . . ?
C7 N2 N3 112.8(6) . . ?
N3 N2 C10 119.3(6) . . ?
C8 N3 N2 103.4(6) . . ?
C1 O1 C11 116.8(7) . . ?
C25 C24 C29 121.0(7) . . ?
O2 C24 C25 123.5(7) . . ?
O2 C24 C29 115.4(7) . . ?
C24 C25 H25 120.6 . . ?
C24 C25 C26 118.8(7) . . ?
C26 C25 H25 120.6 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.7(7) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C28 120.8(7) . . ?
C26 C27 C30 119.6(7) . . ?
C28 C27 C30 119.6(7) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.7(7) . . ?
C29 C28 H28 120.7 . . ?
C24 C29 C28 120.1(8) . . ?
C24 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
N4 C30 C27 127.3(6) . . ?
N5 C30 C27 126.7(7) . . ?
N5 C30 N4 106.0(6) . . ?
N4 C31 C44 126.3(6) . . ?
N6 C31 C44 121.0(6) . . ?
N6 C31 N4 112.6(7) . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
N4 C32 H32C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N5 C33 H33A 109.5 . . ?
N5 C33 H33B 109.5 . . ?
N5 C33 H33C 109.5 . . ?
H34A C34 H34B 108.5 . . ?
C35 C34 H34A 110.3 . . ?
C35 C34 H34B 110.3 . . ?
O2 C34 H34A 110.3 . . ?
O2 C34 H34B 110.3 . . ?
O2 C34 C35 107.2(7) . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
C34 C35 C36 111.7(8) . . ?
H35A C35 H35B 107.9 . . ?
C36 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C35 C36 H36A 109.7 . . ?
C35 C36 H36B 109.7 . . ?
C35 C36 H36C 108.9 . . ?
C35 C36 H36D 108.9 . . ?
C35 C36 C37 110(2) . . ?
H36A C36 H36B 108.2 . . ?
H36C C36 H36D 107.7 . . ?
C37A C36 C35 113(6) . . ?
C37A C36 H36C 108.9 . . ?
C37A C36 H36D 108.9 . . ?
C37 C36 H36A 109.7 . . ?
C37 C36 H36B 109.7 . . ?
C36 C37A H37A 110.6 . . ?
C36 C37A H37B 110.6 . . ?
H37A C37A H37B 108.7 . . ?
C38A C37A C36 106(2) . . ?
C38A C37A H37A 110.6 . . ?
C38A C37A H37B 110.6 . . ?
C36 C37 H37C 108.3 . . ?
C36 C37 H37D 108.3 . . ?
H37C C37 H37D 107.4 . . ?
C38 C37 C36 116(4) . . ?
C38 C37 H37C 108.3 . . ?
C38 C37 H37D 108.3 . . ?
C37 C38 H38A 110.1 . . ?
C37 C38 H38B 110.1 . . ?
C37 C38 C39 108.2(18) . . ?
H38A C38 H38B 108.4 . . ?
C39 C38 H38A 110.1 . . ?
C39 C38 H38B 110.1 . . ?
C37A C38A H38C 109.4 . . ?
C37A C38A H38D 109.4 . . ?
C37A C38A C39A 111(3) . . ?
H38C C38A H38D 108.0 . . ?
C39A C38A H38C 109.4 . . ?
C39A C38A H38D 109.4 . . ?
C38 C39 H39A 110.0 . . ?
C38 C39 H39B 110.0 . . ?
C38 C39 C40 108.5(15) . . ?
H39A C39 H39B 108.4 . . ?
C40 C39 H39A 110.0 . . ?
C40 C39 H39B 110.0 . . ?
C38A C39A H39C 110.1 . . ?
C38A C39A H39D 110.1 . . ?
C38A C39A C40A 108.1(9) . . ?
H39C C39A H39D 108.4 . . ?
C40A C39A H39C 110.1 . . ?
C40A C39A H39D 110.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
C41 C40 C39 110.6(15) . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
C39A C40A H40C 109.9 . . ?
C39A C40A H40D 109.9 . . ?
H40C C40A H40D 108.3 . . ?
C41A C40A C39A 108.9(10) . . ?
C41A C40A H40C 109.9 . . ?
C41A C40A H40D 109.9 . . ?
C40 C41 H41A 110.3 . . ?
C40 C41 H41B 110.3 . . ?
C40 C41 C42 107.0(15) . . ?
H41A C41 H41B 108.6 . . ?
C42 C41 H41A 110.3 . . ?
C42 C41 H41B 110.3 . . ?
C40A C41A H41C 109.8 . . ?
C40A C41A H41D 109.8 . . ?
C40A C41A C42A 109.6(10) . . ?
H41C C41A H41D 108.2 . . ?
C42A C41A H41C 109.8 . . ?
C42A C41A H41D 109.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 108.1 . . ?
C43 C42 C41 110.8(17) . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
C41A C42A H42C 109.9 . . ?
C41A C42A H42D 109.9 . . ?
H42C C42A H42D 108.3 . . ?
C43A C42A C41A 108.7(10) . . ?
C43A C42A H42C 109.9 . . ?
C43A C42A H42D 109.9 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42A C43A H43D 109.6 . . ?
C42A C43A H43E 110.1 . . ?
C42A C43A H43F 108.7 . . ?
H43D C43A H43E 109.5 . . ?
H43D C43A H43F 109.5 . . ?
H43E C43A H43F 109.5 . . ?
C31 C44 C45 112.0(7) . . ?
F8 C44 C31 108.6(6) . . ?
F8 C44 C45 108.7(6) . . ?
F9 C44 C31 110.4(6) . . ?
F9 C44 C45 108.5(6) . . ?
F9 C44 F8 108.4(6) . . ?
C46 C45 C44 116.8(8) . . ?
F10 C45 C44 108.1(6) . . ?
F10 C45 C46 107.6(7) . . ?
F10 C45 F11 108.9(7) . . ?
F11 C45 C44 107.8(6) . . ?
F11 C45 C46 107.5(7) . . ?
F12 C46 C45 111.3(8) . . ?
F12 C46 F13 109.0(10) . . ?
F12 C46 F14 108.7(8) . . ?
F13 C46 C45 110.1(8) . . ?
F13 C46 F14 108.3(8) . . ?
F14 C46 C45 109.2(9) . . ?
C30 N4 C31 105.2(6) . . ?
C30 N4 C32 124.5(6) . . ?
C31 N4 C32 130.2(6) . . ?
C30 N5 C33 127.5(7) . . ?
C30 N5 N6 112.6(6) . . ?
N6 N5 C33 119.9(6) . . ?
C31 N6 N5 103.6(6) . . ?
C24 O2 C34 118.4(6) . . ?
F15 C47 F16 107.8(8) . . ?
F15 C47 F17 106.2(7) . . ?
F15 C47 S1 113.5(6) . . ?
F16 C47 F17 105.4(7) . . ?
F16 C47 S1 111.6(7) . . ?
F17 C47 S1 111.9(6) . . ?
O3 S1 C47 103.3(4) . . ?
O3 S1 O5 115.0(4) . . ?
O4 S1 C47 103.4(4) . . ?
O4 S1 O3 115.7(3) . . ?
O4 S1 O5 114.0(4) . . ?
O5 S1 C47 103.1(4) . . ?
F18 C48 S2 110.3(5) . . ?
F19 C48 F18 108.0(7) . . ?
F19 C48 S2 110.7(6) . . ?
F20 C48 F18 107.9(7) . . ?
F20 C48 F19 108.7(7) . . ?
F20 C48 S2 111.2(6) . . ?
O6 S2 C48 102.7(4) . . ?
O7 S2 C48 103.8(4) . . ?
O7 S2 O6 114.5(4) . . ?
O7 S2 O8 115.6(3) . . ?
O8 S2 C48 103.1(4) . . ?
O8 S2 O6 114.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 1.7(12) . . . . ?
C2 C1 C6 C5 0.5(12) . . . . ?
C2 C1 O1 C11 2.1(11) . . . . ?
C2 C3 C4 C5 0.5(11) . . . . ?
C2 C3 C4 C7 178.4(7) . . . . ?
C3 C4 C5 C6 -2.1(12) . . . . ?
C3 C4 C7 N1 -102.6(9) . . . . ?
C3 C4 C7 N2 78.2(10) . . . . ?
C4 C5 C6 C1 1.6(13) . . . . ?
C4 C7 N1 C8 178.1(7) . . . . ?
C4 C7 N1 C9 -1.1(12) . . . . ?
C4 C7 N2 C10 -2.3(13) . . . . ?
C4 C7 N2 N3 -177.2(7) . . . . ?
C5 C4 C7 N1 75.3(10) . . . . ?
C5 C4 C7 N2 -103.9(10) . . . . ?
C6 C1 C2 C3 -2.2(12) . . . . ?
C6 C1 O1 C11 -176.6(7) . . . . ?
C7 C4 C5 C6 -180.0(7) . . . . ?
C7 N2 N3 C8 -2.9(8) . . . . ?
C8 C21 C22 C23 179.2(6) . . . . ?
C8 C21 C22 F3 -60.6(8) . . . . ?
C8 C21 C22 F4 57.3(8) . . . . ?
C10 N2 N3 C8 -178.3(6) . . . . ?
C11 C12 C13 C14 70.3(11) . . . . ?
C12 C11 O1 C1 -179.1(7) . . . . ?
C12 C13 C14 C15 -177.8(8) . . . . ?
C13 C14 C15 C16 -179.2(8) . . . . ?
C14 C15 C16 C17 -179.8(8) . . . . ?
C15 C16 C17 C18 179.6(14) . . . . ?
C15 C16 C17 C18A 175(3) . . . . ?
C16 C17 C18 C19 -178.1(13) . . . . ?
C16 C17 C18A C19A 168(3) . . . . ?
C17 C18 C19 C20 174.1(18) . . . . ?
C17 C18A C19A C20A 96(4) . . . . ?
C21 C8 N1 C7 -179.4(7) . . . . ?
C21 C8 N1 C9 -0.3(12) . . . . ?
C21 C8 N3 N2 -178.6(7) . . . . ?
C21 C22 C23 F5 58.9(10) . . . . ?
C21 C22 C23 F6 -61.3(10) . . . . ?
C21 C22 C23 F7 179.7(7) . . . . ?
F1 C21 C22 C23 -57.9(9) . . . . ?
F1 C21 C22 F3 62.3(8) . . . . ?
F1 C21 C22 F4 -179.8(6) . . . . ?
F2 C21 C22 C23 60.0(9) . . . . ?
F2 C21 C22 F3 -179.8(6) . . . . ?
F2 C21 C22 F4 -61.9(8) . . . . ?
F3 C22 C23 F5 -61.6(10) . . . . ?
F3 C22 C23 F6 178.2(7) . . . . ?
F3 C22 C23 F7 59.2(9) . . . . ?
F4 C22 C23 F5 -178.7(7) . . . . ?
F4 C22 C23 F6 61.1(10) . . . . ?
F4 C22 C23 F7 -57.9(9) . . . . ?
N1 C7 N2 C10 178.4(7) . . . . ?
N1 C7 N2 N3 3.5(8) . . . . ?
N1 C8 C21 C22 89.8(9) . . . . ?
N1 C8 C21 F1 -32.0(10) . . . . ?
N1 C8 C21 F2 -151.1(7) . . . . ?
N1 C8 N3 N2 1.2(8) . . . . ?
N2 C7 N1 C8 -2.6(8) . . . . ?
N2 C7 N1 C9 178.2(6) . . . . ?
N3 C8 C21 C22 -90.5(8) . . . . ?
N3 C8 C21 F1 147.7(7) . . . . ?
N3 C8 C21 F2 28.6(10) . . . . ?
N3 C8 N1 C7 0.9(8) . . . . ?
N3 C8 N1 C9 180.0(7) . . . . ?
O1 C1 C2 C3 179.3(7) . . . . ?
O1 C1 C6 C5 179.2(8) . . . . ?
O1 C11 C12 C13 67.4(10) . . . . ?
C24 C25 C26 C27 -1.4(12) . . . . ?
C25 C24 C29 C28 0.6(12) . . . . ?
C25 C24 O2 C34 -5.2(11) . . . . ?
C25 C26 C27 C28 0.7(12) . . . . ?
C25 C26 C27 C30 -178.3(7) . . . . ?
C26 C27 C28 C29 0.7(11) . . . . ?
C26 C27 C30 N4 107.5(9) . . . . ?
C26 C27 C30 N5 -69.4(11) . . . . ?
C27 C28 C29 C24 -1.3(12) . . . . ?
C27 C30 N4 C31 -176.4(7) . . . . ?
C27 C30 N4 C32 2.4(12) . . . . ?
C27 C30 N5 C33 -1.8(13) . . . . ?
C27 C30 N5 N6 175.4(7) . . . . ?
C28 C27 C30 N4 -71.4(11) . . . . ?
C28 C27 C30 N5 111.7(9) . . . . ?
C29 C24 C25 C26 0.8(12) . . . . ?
C29 C24 O2 C34 173.5(7) . . . . ?
C30 C27 C28 C29 179.6(7) . . . . ?
C30 N5 N6 C31 2.3(8) . . . . ?
C31 C44 C45 C46 -178.4(7) . . . . ?
C31 C44 C45 F10 -57.1(8) . . . . ?
C31 C44 C45 F11 60.5(8) . . . . ?
C33 N5 N6 C31 179.7(7) . . . . ?
C34 C35 C36 C37A -166(12) . . . . ?
C34 C35 C36 C37 -167(4) . . . . ?
C35 C34 O2 C24 -169.4(7) . . . . ?
C35 C36 C37A C38A -152(11) . . . . ?
C35 C36 C37 C38 173(5) . . . . ?
C36 C37A C38A C39A -178(11) . . . . ?
C36 C37 C38 C39 -170(5) . . . . ?
C37A C38A C39A C40A 89(13) . . . . ?
C37 C38 C39 C40 -175(4) . . . . ?
C38 C39 C40 C41 70(2) . . . . ?
C38A C39A C40A C41A 169(3) . . . . ?
C39 C40 C41 C42 170.0(13) . . . . ?
C39A C40A C41A C42A -125(4) . . . . ?
C40 C41 C42 C43 -174.3(16) . . . . ?
C40A C41A C42A C43A 163(4) . . . . ?
C44 C31 N4 C30 178.3(7) . . . . ?
C44 C31 N4 C32 -0.5(13) . . . . ?
C44 C31 N6 N5 -179.6(7) . . . . ?
C44 C45 C46 F12 57.6(11) . . . . ?
C44 C45 C46 F13 -63.5(10) . . . . ?
C44 C45 C46 F14 177.7(7) . . . . ?
F8 C44 C45 C46 -58.4(9) . . . . ?
F8 C44 C45 F10 63.0(8) . . . . ?
F8 C44 C45 F11 -179.4(6) . . . . ?
F9 C44 C45 C46 59.4(9) . . . . ?
F9 C44 C45 F10 -179.2(6) . . . . ?
F9 C44 C45 F11 -61.7(8) . . . . ?
F10 C45 C46 F12 -64.0(11) . . . . ?
F10 C45 C46 F13 174.9(8) . . . . ?
F10 C45 C46 F14 56.1(9) . . . . ?
F11 C45 C46 F12 178.8(8) . . . . ?
F11 C45 C46 F13 57.7(11) . . . . ?
F11 C45 C46 F14 -61.1(9) . . . . ?
N4 C30 N5 C33 -179.3(7) . . . . ?
N4 C30 N5 N6 -2.1(9) . . . . ?
N4 C31 C44 C45 -88.9(9) . . . . ?
N4 C31 C44 F8 151.0(7) . . . . ?
N4 C31 C44 F9 32.2(10) . . . . ?
N4 C31 N6 N5 -1.6(8) . . . . ?
N5 C30 N4 C31 1.0(8) . . . . ?
N5 C30 N4 C32 179.9(6) . . . . ?
N6 C31 C44 C45 88.8(8) . . . . ?
N6 C31 C44 F8 -31.3(10) . . . . ?
N6 C31 C44 F9 -150.1(7) . . . . ?
N6 C31 N4 C30 0.4(9) . . . . ?
N6 C31 N4 C32 -178.4(7) . . . . ?
O2 C24 C25 C26 179.4(7) . . . . ?
O2 C24 C29 C28 -178.2(7) . . . . ?
O2 C34 C35 C36 -175.0(7) . . . . ?
F15 C47 S1 O3 -58.8(7) . . . . ?
F15 C47 S1 O4 62.1(7) . . . . ?
F15 C47 S1 O5 -178.9(6) . . . . ?
F16 C47 S1 O3 63.2(7) . . . . ?
F16 C47 S1 O4 -175.9(6) . . . . ?
F16 C47 S1 O5 -56.8(7) . . . . ?
F17 C47 S1 O3 -178.9(6) . . . . ?
F17 C47 S1 O4 -58.0(7) . . . . ?
F17 C47 S1 O5 61.0(7) . . . . ?
F18 C48 S2 O6 -177.9(5) . . . . ?
F18 C48 S2 O7 62.5(6) . . . . ?
F18 C48 S2 O8 -58.4(6) . . . . ?
F19 C48 S2 O6 62.6(6) . . . . ?
F19 C48 S2 O7 -57.0(7) . . . . ?
F19 C48 S2 O8 -177.9(6) . . . . ?
F20 C48 S2 O6 -58.3(7) . . . . ?
F20 C48 S2 O7 -177.9(6) . . . . ?
F20 C48 S2 O8 61.2(7) . . . . ?

_olex2_date_sample_data_collection 2017-04-21
_olex2_date_sample_submission    2017-06-08
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id NV2554
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.629
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.939(2)
2 0.061(2)


### END
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_dwb1680b
_database_code_depnum_ccdc_archive 'CCDC 2177838'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2022-02-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H35 F15 N3 O, C2 F6 N O4 S2'
_chemical_formula_sum            'C31 H35 F21 N4 O5 S2'
_chemical_formula_weight         1006.75
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C31 H35 F21 N4 O5 S2'
_chemical_oxdiff_usercomment     'Alessio NV2434 repeat at 220K'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   6.7404(7)
_cell_length_b                   8.6592(7)
_cell_length_c                   71.960(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4200.0(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3996
_cell_measurement_temperature    220.00(14)
_cell_measurement_theta_max      70.2180
_cell_measurement_theta_min      4.9200
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.612
_exptl_absorpt_coefficient_mu    2.421
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0062
0 0 -1 0.0022
4 0 3 0.1121
-4 0 -3 0.1121
0 1 -1 0.1021
0 -1 1 0.1021

_exptl_crystal_recrystallization_method 'evaporation of acetone/hexane solution'
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.008
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
-0.0001 -0.0002 1.0000 0.0093 0.0192 -0.0010
0.0001 0.0002 -1.0000 -0.0093 -0.0192 0.0010
4.0012 -0.0024 3.0033 -0.6599 0.4161 0.4813
-4.0012 0.0024 -3.0033 0.6599 -0.4161 -0.4813
-0.0001 1.0001 -0.9992 0.0784 -0.0545 0.1517
0.0001 -1.0001 0.9992 -0.0784 0.0545 -0.1517

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            13238
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.685
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     36.00  71.25   0.75    2.50    --    0.00  57.00 -90.00   47
  2  ω      2.00  85.25   0.75   10.00    --   56.36 -61.00 -90.00  111
  3  ω     38.00 127.25   0.75   25.00    --  112.72 -77.00 -90.00  119
  4  ω     59.00 152.00   0.75   25.00    --  112.72 -37.00-120.00  124
  5  ω     84.00 178.50   0.75   25.00    --  112.72  63.00  30.00  126
  6  ω    138.00 175.50   0.75   25.00    --  112.72 111.00   0.00   50
  7  ω    118.00 144.25   0.75   25.00    --  112.72 111.00-150.00   35
  8  ω     49.00 142.00   0.75   25.00    --  112.72 -50.00  90.00  124
  9  ω     37.00 126.25   0.75   25.00    --  112.72 -77.00  90.00  119
 10  ω    -84.00 -33.75   0.75    2.50    --    0.00 178.00  90.00   67
 11  ω    -79.00  -7.00   0.75   10.00    --  -56.36 125.00  30.00   96
 12  ω   -119.00 -74.75   0.75   10.00    --  -56.36 -78.00 -89.00   59
 13  ω   -107.00 -80.00   0.75   10.00    --  -56.36 -94.00-180.00   36
 14  ω   -127.00 -91.75   0.75   10.00    --  -56.36-125.00 -90.00   47
 15  ω   -127.00 -79.75   0.75   10.00    --  -56.36 -94.00   0.00   63
 16  ω   -114.00 -82.50   0.75   10.00    --  -56.36-125.00  60.00   42
 17  ω   -109.00 -76.75   0.75   10.00    --  -56.36-125.00 150.00   43
 18  ω   -111.00 -84.75   0.75   10.00    --  -56.36 -94.00 150.00   35
 19  ω    -85.00 -60.25   0.75    2.50    --    0.00-178.00-120.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1718972000
_diffrn_orient_matrix_UB_12      0.0877403000
_diffrn_orient_matrix_UB_13      0.0093459000
_diffrn_orient_matrix_UB_21      0.0895391000
_diffrn_orient_matrix_UB_22      -0.0352292000
_diffrn_orient_matrix_UB_23      0.0192434000
_diffrn_orient_matrix_UB_31      0.1210786000
_diffrn_orient_matrix_UB_32      0.1507160000
_diffrn_orient_matrix_UB_33      -0.0009375000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_special_details          
;
Long unit cell required detector to be moved back to 55 mm. 
Phase change at 110 K so sample collected at 220 K
;
_reflns_Friedel_coverage         0.590
_reflns_Friedel_fraction_full    0.819
_reflns_Friedel_fraction_max     0.819
_reflns_number_gt                5965
_reflns_number_total             6861
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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         0.444
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Flack x determined using 1650 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.00012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         6861
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0867
_refine_ls_restrained_S_all      1.166
_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)+17.6707P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1837
_refine_special_details          
;
The perfluoroheptyl chain exhibited disorder with the last 5 carbons
and associated fluorines being modelled in two positions with refined 
occupancies of 0.899:0.101(5).  The C-C bonds in the disordered 
section were restrained to be equal.  The C-F bond lengths in the 
minor form were restrained to be 1.34 angstroms for the
difluoromethylene groups and 1.32 angstroms for the trifluoromethyl 
group.  The ADP of pairs of disordered carbons were constrained to 
be equal (e.g. C14 & C14A).  Similarly, the ADP of pairs of 
disordered fluorines were constained to be equal (e.g. F5 & F5A, 
F6 & F6A).
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F14A-C17A = F13A-C17A = F15A-C17A
 1.32 with sigma of 0.01
 F8A-C14A = F7A-C14A
 1.34 with sigma of 0.01
 F9A-C15A = F10A-C15A = F11A-C16A = C16A-F12A = C13A-F5A = C13A-F6A
 1.34 with sigma of 0.01
 F10A-F9A = F5A-F6A = F7A-F8A
 2.15 with sigma of 0.01
 F15A-C17A \\sim C17A-F14A \\sim C17A-F13A
 with sigma of 0.01
 F13A-F14A \\sim F14A-F15A \\sim F13A-F15A
 with sigma of 0.02
 C13-C12 \\sim C13A-C12
 with sigma of 0.05
 C16-C17 \\sim C16A-C17A
 with sigma of 0.05
 C16-F13 \\sim C16-F14 \\sim C16-F15 \\sim C16A-F13A \\sim C16A-F14A \\sim
C16A-F15A
 with sigma of 0.05
 C15A-C16A \\sim C15-C16 \\sim C15A-C14A \\sim C15-C14 \\sim C14A-C13A \\sim
C14-C13
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) = Uanis(C17)
Uanis(F13A) = Uanis(F14)
Uanis(F15A) = Uanis(F13)
Uanis(F10A) = Uanis(F10)
Uanis(F9) = Uanis(F9A)
Uanis(F14A) = Uanis(F15)
Uanis(C15) = Uanis(C15A)
Uanis(F6) = Uanis(F5A)
Uanis(C13) = Uanis(C13A)
Uanis(C14A) = Uanis(C14)
Uanis(F7A) = Uanis(F7)
Uanis(F6A) = Uanis(F6)
Uanis(F8A) = Uanis(F8)
Uanis(F5) = Uanis(F5A)
Uanis(C16) = Uanis(C16A)
Uanis(F11A) = Uanis(F11)
Uanis(F12A) = Uanis(F12)
4. Others
 Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(C16A)=Sof(C17A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=
 Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=
 1-FVAR(1)
 Sof(C13)=Sof(C14)=Sof(C15)=Sof(C16)=Sof(C17)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=
 Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C)
;
_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
C1 C 0.0975(14) 0.6167(10) 0.66321(11) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.0131(15) 0.4857(11) 0.65516(13) 0.041(2) Uani 1 1 d . . . . .
H2 H 0.035315 0.387973 0.660439 0.050 Uiso 1 1 calc R U . . .
C3 C -0.1026(15) 0.4996(11) 0.63948(13) 0.042(2) Uani 1 1 d . . . . .
H3 H -0.162728 0.412132 0.634167 0.050 Uiso 1 1 calc R U . . .
C4 C -0.1292(14) 0.6443(10) 0.63166(12) 0.034(2) Uani 1 1 d . . . . .
C5 C -0.0533(13) 0.7755(10) 0.63990(12) 0.034(2) Uani 1 1 d . . . . .
H5 H -0.081199 0.873542 0.634934 0.040 Uiso 1 1 calc R U . . .
C6 C 0.0658(14) 0.7609(11) 0.65579(12) 0.036(2) Uani 1 1 d . . . . .
H6 H 0.123314 0.848565 0.661288 0.043 Uiso 1 1 calc R U . . .
C7 C -0.2553(14) 0.6598(9) 0.61502(12) 0.032(2) Uani 1 1 d . . . . .
C8 C -0.3697(14) 0.7023(11) 0.58757(12) 0.035(2) Uani 1 1 d . . . . .
C9 C 0.0002(16) 0.7502(15) 0.59254(16) 0.061(3) Uani 1 1 d . . . . .
H9A H 0.010318 0.861904 0.592350 0.091 Uiso 1 1 calc R U . . .
H9B H 0.029255 0.709688 0.580271 0.091 Uiso 1 1 calc R U . . .
H9C H 0.094297 0.708595 0.601423 0.091 Uiso 1 1 calc R U . . .
C10 C -0.5794(15) 0.5769(11) 0.62885(12) 0.037(2) Uani 1 1 d . . . . .
H10A H -0.668760 0.660154 0.632181 0.056 Uiso 1 1 calc R U . . .
H10B H -0.501363 0.547593 0.639612 0.056 Uiso 1 1 calc R U . . .
H10C H -0.655723 0.488709 0.624603 0.056 Uiso 1 1 calc R U . . .
C11 C -0.3930(17) 0.7444(12) 0.56712(13) 0.044(2) Uani 1 1 d . . . . .
C12 C -0.3721(17) 0.6035(12) 0.55432(14) 0.044(2) Uani 1 1 d D . . . .
C13 C -0.3573(18) 0.6398(14) 0.53326(16) 0.043(3) Uani 0.899(5) 1 d D . P A 1
C13A C -0.423(10) 0.637(7) 0.5333(8) 0.043(3) Uani 0.101(5) 1 d D . P A 2
C14 C -0.414(2) 0.5049(13) 0.52042(15) 0.048(3) Uani 0.899(5) 1 d D . P A 1
C14A C -0.334(11) 0.531(9) 0.5181(11) 0.048(3) Uani 0.101(5) 1 d D . P A 2
C15 C -0.349(2) 0.5286(16) 0.49979(16) 0.053(4) Uani 0.899(5) 1 d D . P A 1
C15A C -0.424(10) 0.544(11) 0.4984(11) 0.053(4) Uani 0.101(5) 1 d D . P A 2
C16 C -0.451(3) 0.4178(19) 0.48593(18) 0.074(5) Uani 0.899(5) 1 d D . P A 1
C16A C -0.345(11) 0.416(14) 0.4852(12) 0.074(5) Uani 0.101(5) 1 d D . P A 2
C17 C -0.358(4) 0.416(2) 0.4662(2) 0.082(6) Uani 0.899(5) 1 d D . P A 1
C17A C -0.433(11) 0.410(8) 0.4651(13) 0.082(6) Uani 0.101(5) 1 d D . P A 2
C18 C 0.3630(16) 0.7000(12) 0.68325(12) 0.043(2) Uani 1 1 d . . . . .
H18A H 0.300521 0.788845 0.689320 0.052 Uiso 1 1 calc R U . . .
H18B H 0.434309 0.736350 0.672213 0.052 Uiso 1 1 calc R U . . .
C19 C 0.5030(17) 0.6202(11) 0.69640(14) 0.047(3) Uani 1 1 d . . . . .
H19A H 0.559330 0.529964 0.690093 0.057 Uiso 1 1 calc R U . . .
H19B H 0.426921 0.582613 0.707085 0.057 Uiso 1 1 calc R U . . .
C20 C 0.6727(14) 0.7203(11) 0.70351(13) 0.038(2) Uani 1 1 d . . . . .
H20A H 0.753848 0.754152 0.692971 0.045 Uiso 1 1 calc R U . . .
H20B H 0.618032 0.812449 0.709525 0.045 Uiso 1 1 calc R U . . .
C21 C 0.8025(16) 0.6340(11) 0.71725(14) 0.043(2) Uani 1 1 d . . . . .
H21A H 0.718405 0.596123 0.727381 0.052 Uiso 1 1 calc R U . . .
H21B H 0.858898 0.543694 0.710972 0.052 Uiso 1 1 calc R U . . .
C22 C 0.9693(14) 0.7259(11) 0.72553(13) 0.039(2) Uani 1 1 d . . . . .
H22A H 0.913712 0.817746 0.731547 0.047 Uiso 1 1 calc R U . . .
H22B H 1.056110 0.761193 0.715464 0.047 Uiso 1 1 calc R U . . .
C23 C 1.0931(14) 0.6395(11) 0.73955(13) 0.039(2) Uani 1 1 d . . . . .
H23A H 1.006168 0.605107 0.749646 0.047 Uiso 1 1 calc R U . . .
H23B H 1.147040 0.547005 0.733543 0.047 Uiso 1 1 calc R U . . .
C24 C 1.2619(15) 0.7291(11) 0.74782(13) 0.040(2) Uani 1 1 d . . . . .
H24A H 1.208508 0.822133 0.753742 0.048 Uiso 1 1 calc R U . . .
H24B H 1.350130 0.762353 0.737767 0.048 Uiso 1 1 calc R U . . .
C25 C 1.3837(16) 0.6406(11) 0.76209(13) 0.042(2) Uani 1 1 d . . . . .
H25A H 1.296163 0.610428 0.772344 0.050 Uiso 1 1 calc R U . . .
H25B H 1.432817 0.545592 0.756288 0.050 Uiso 1 1 calc R U . . .
C26 C 1.5573(16) 0.7271(11) 0.77000(14) 0.045(2) Uani 1 1 d . . . . .
H26A H 1.508109 0.822777 0.775634 0.054 Uiso 1 1 calc R U . . .
H26B H 1.645339 0.756239 0.759737 0.054 Uiso 1 1 calc R U . . .
C27 C 1.6785(15) 0.6412(11) 0.78438(13) 0.041(2) Uani 1 1 d . . . . .
H27A H 1.725771 0.544399 0.778890 0.049 Uiso 1 1 calc R U . . .
H27B H 1.592000 0.614624 0.794851 0.049 Uiso 1 1 calc R U . . .
C28 C 1.8555(17) 0.7305(12) 0.79171(15) 0.052(3) Uani 1 1 d . . . . .
H28A H 1.941104 0.758692 0.781237 0.063 Uiso 1 1 calc R U . . .
H28B H 1.808308 0.826360 0.797442 0.063 Uiso 1 1 calc R U . . .
C29 C 1.977(2) 0.6423(15) 0.80578(16) 0.068(4) Uani 1 1 d . . . . .
H29A H 2.016348 0.543659 0.800553 0.102 Uiso 1 1 calc R U . . .
H29B H 1.898375 0.625033 0.816879 0.102 Uiso 1 1 calc R U . . .
H29C H 2.094456 0.701412 0.808958 0.102 Uiso 1 1 calc R U . . .
C30 C 0.590(2) 0.1283(12) 0.65661(16) 0.056(3) Uani 1 1 d . . . . .
C31 C 0.414(3) 0.1803(18) 0.5873(2) 0.098(6) Uani 1 1 d . . . . .
F1 F -0.5717(10) 0.8059(9) 0.56466(8) 0.070(2) Uani 1 1 d . . . . .
F2 F -0.2544(11) 0.8489(7) 0.56224(8) 0.0594(18) Uani 1 1 d . . . . .
F3 F -0.2083(13) 0.5270(8) 0.55915(9) 0.078(2) Uani 1 1 d . . . . .
F4 F -0.5252(12) 0.5110(9) 0.55741(9) 0.078(2) Uani 1 1 d . . . . .
F5 F -0.4785(14) 0.7601(10) 0.52965(10) 0.0698(17) Uani 0.899(5) 1 d . . P A 1
F5A F -0.334(10) 0.768(9) 0.5278(9) 0.0698(17) Uani 0.101(5) 1 d D . P A 2
F6 F -0.1748(14) 0.6862(10) 0.52987(9) 0.0698(17) Uani 0.899(5) 1 d . . P A 1
F6A F -0.618(9) 0.659(8) 0.5312(8) 0.0698(17) Uani 0.101(5) 1 d D . P A 2
F7 F -0.6091(13) 0.4880(11) 0.52080(10) 0.077(3) Uani 0.899(5) 1 d . . P A 1
F7A F -0.135(10) 0.527(9) 0.5176(9) 0.077(3) Uani 0.101(5) 1 d D . P A 2
F8 F -0.3252(17) 0.3756(11) 0.5266(2) 0.075(3) Uani 0.899(5) 1 d . . P A 1
F8A F -0.393(13) 0.400(12) 0.526(2) 0.075(3) Uani 0.101(5) 1 d D . P A 2
F9 F -0.385(2) 0.6724(12) 0.4945(5) 0.067(3) Uani 0.899(5) 1 d . . P A 1
F9A F -0.41(2) 0.696(13) 0.495(5) 0.067(3) Uani 0.101(5) 1 d D . P A 2
F10 F -0.1528(13) 0.5094(10) 0.49869(10) 0.070(2) Uani 0.899(5) 1 d . . P A 1
F10A F -0.616(11) 0.508(9) 0.5000(9) 0.070(2) Uani 0.101(5) 1 d D . P A 2
F11 F -0.6414(17) 0.4600(12) 0.48414(12) 0.091(3) Uani 0.899(5) 1 d . . P A 1
F11A F -0.149(12) 0.423(11) 0.4823(10) 0.091(3) Uani 0.101(5) 1 d D . P A 2
F12 F -0.437(7) 0.275(2) 0.4928(3) 0.105(6) Uani 0.899(5) 1 d . . P A 1
F12A F -0.41(7) 0.27(2) 0.489(3) 0.105(6) Uani 0.101(5) 1 d D . P A 2
F13 F -0.470(2) 0.3292(15) 0.45534(14) 0.140(6) Uani 0.899(5) 1 d D . P A 1
F13A F -0.371(15) 0.279(10) 0.4577(11) 0.088(3) Uani 0.101(5) 1 d D . P A 2
F14 F -0.362(2) 0.5565(12) 0.45919(13) 0.088(3) Uani 0.899(5) 1 d D . P A 1
F14A F -0.629(11) 0.414(12) 0.4662(11) 0.135(5) Uani 0.101(5) 1 d D . P A 2
F15 F -0.176(2) 0.3647(16) 0.46646(14) 0.135(5) Uani 0.899(5) 1 d D . P A 1
F15A F -0.36(2) 0.531(11) 0.4561(16) 0.140(6) Uani 0.101(5) 1 d D . P A 2
F16 F 0.7804(12) 0.1220(9) 0.65225(11) 0.077(2) Uani 1 1 d . . . . .
F17 F 0.5580(16) 0.0303(9) 0.67028(10) 0.097(3) Uani 1 1 d . . . . .
F18 F 0.5561(13) 0.2695(8) 0.66305(9) 0.076(2) Uani 1 1 d . . . . .
F19 F 0.3102(16) 0.3068(12) 0.58812(14) 0.117(4) Uani 1 1 d . . . . .
F20 F 0.2994(19) 0.0593(11) 0.59082(14) 0.133(4) Uani 1 1 d . . . . .
F21 F 0.489(2) 0.1643(11) 0.57046(11) 0.142(5) Uani 1 1 d . . . . .
N1 N -0.2017(11) 0.7053(10) 0.59795(10) 0.0387(19) Uani 1 1 d . . . . .
N2 N -0.4486(12) 0.6277(8) 0.61416(10) 0.0321(17) Uani 1 1 d . . . . .
N3 N -0.5225(11) 0.6552(9) 0.59672(10) 0.0359(18) Uani 1 1 d . . . . .
N4 N 0.5050(17) 0.2099(9) 0.62274(12) 0.059(3) Uani 1 1 d . . . . .
O1 O 0.2172(12) 0.5882(8) 0.67821(9) 0.052(2) Uani 1 1 d . . . . .
O2 O 0.4799(13) -0.0703(8) 0.63245(12) 0.064(2) Uani 1 1 d . . . . .
O3 O 0.2391(13) 0.1192(10) 0.64333(14) 0.081(3) Uani 1 1 d . . . . .
O4 O 0.7160(17) 0.0398(9) 0.60203(12) 0.084(3) Uani 1 1 d . . . . .
O5 O 0.7220(15) 0.3224(9) 0.59968(11) 0.071(3) Uani 1 1 d . . . . .
S1 S 0.4330(5) 0.0842(3) 0.63685(4) 0.0518(7) Uani 1 1 d . . . . .
S2 S 0.6189(6) 0.1843(3) 0.60412(4) 0.0590(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.395(12) . ?
C1 C6 1.374(12) . ?
C1 O1 1.370(10) . ?
C2 H2 0.9400 . ?
C2 C3 1.377(13) . ?
C3 H3 0.9400 . ?
C3 C4 1.385(12) . ?
C4 C5 1.380(12) . ?
C4 C7 1.475(12) . ?
C5 H5 0.9400 . ?
C5 C6 1.403(12) . ?
C6 H6 0.9400 . ?
C7 N1 1.340(11) . ?
C7 N2 1.334(12) . ?
C8 C11 1.524(12) . ?
C8 N1 1.357(11) . ?
C8 N3 1.289(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C9 N1 1.468(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C10 N2 1.445(11) . ?
C11 C12 1.535(13) . ?
C11 F1 1.329(12) . ?
C11 F2 1.348(12) . ?
C12 C13 1.551(14) . ?
C12 C13A 1.58(6) . ?
C12 F3 1.333(12) . ?
C12 F4 1.326(12) . ?
C13 C14 1.538(13) . ?
C13 F5 1.349(14) . ?
C13 F6 1.317(14) . ?
C13A C14A 1.55(2) . ?
C13A F5A 1.345(14) . ?
C13A F6A 1.339(14) . ?
C14 C15 1.561(13) . ?
C14 F7 1.323(17) . ?
C14 F8 1.346(14) . ?
C14A C15A 1.55(2) . ?
C14A F7A 1.340(14) . ?
C14A F8A 1.340(14) . ?
C15 C16 1.545(15) . ?
C15 F9 1.323(17) . ?
C15 F10 1.335(16) . ?
C15A C16A 1.54(2) . ?
C15A F9A 1.339(14) . ?
C15A F10A 1.340(14) . ?
C16 C17 1.55(2) . ?
C16 F11 1.34(2) . ?
C16 F12 1.34(3) . ?
C16A C17A 1.56(6) . ?
C16A F11A 1.341(14) . ?
C16A F12A 1.340(16) . ?
C17 F13 1.32(2) . ?
C17 F14 1.321(19) . ?
C17 F15 1.30(2) . ?
C17A F13A 1.321(10) . ?
C17A F14A 1.321(10) . ?
C17A F15A 1.321(11) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 C19 1.504(13) . ?
C18 O1 1.426(12) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C20 1.523(13) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 C21 1.517(12) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 C22 1.501(13) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 C23 1.507(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 C24 1.500(12) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 C25 1.522(12) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 C26 1.502(13) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 C27 1.514(12) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 C28 1.517(14) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 C29 1.510(14) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C30 F16 1.321(15) . ?
C30 F17 1.317(12) . ?
C30 F18 1.328(12) . ?
C30 S1 1.814(13) . ?
C31 F19 1.301(19) . ?
C31 F20 1.327(18) . ?
C31 F21 1.323(19) . ?
C31 S2 1.835(17) . ?
N2 N3 1.371(10) . ?
N4 S1 1.566(9) . ?
N4 S2 1.560(10) . ?
O2 S1 1.411(7) . ?
O3 S1 1.420(9) . ?
O4 S2 1.420(9) . ?
O5 S2 1.419(8) . ?

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
C6 C1 C2 120.9(8) . . ?
O1 C1 C2 114.9(8) . . ?
O1 C1 C6 124.1(8) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(9) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(9) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C7 119.1(8) . . ?
C5 C4 C3 121.5(8) . . ?
C5 C4 C7 119.2(8) . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.2(8) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 C5 119.2(8) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N1 C7 C4 128.0(9) . . ?
N2 C7 C4 125.6(8) . . ?
N2 C7 N1 106.4(8) . . ?
N1 C8 C11 127.8(9) . . ?
N3 C8 C11 119.1(9) . . ?
N3 C8 N1 113.0(8) . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
C8 C11 C12 112.3(8) . . ?
F1 C11 C8 108.5(9) . . ?
F1 C11 C12 108.8(9) . . ?
F1 C11 F2 108.9(8) . . ?
F2 C11 C8 109.9(8) . . ?
F2 C11 C12 108.3(9) . . ?
C11 C12 C13 115.5(9) . . ?
C11 C12 C13A 114(3) . . ?
F3 C12 C11 108.4(9) . . ?
F3 C12 C13 107.6(9) . . ?
F3 C12 C13A 121(3) . . ?
F4 C12 C11 107.9(9) . . ?
F4 C12 C13 109.6(9) . . ?
F4 C12 C13A 96(3) . . ?
F4 C12 F3 107.5(9) . . ?
C14 C13 C12 114.7(9) . . ?
F5 C13 C12 107.8(10) . . ?
F5 C13 C14 108.7(10) . . ?
F6 C13 C12 107.6(9) . . ?
F6 C13 C14 110.7(11) . . ?
F6 C13 F5 107.1(10) . . ?
C14A C13A C12 119(5) . . ?
F5A C13A C12 110(5) . . ?
F5A C13A C14A 97(6) . . ?
F6A C13A C12 110(5) . . ?
F6A C13A C14A 113(6) . . ?
F6A C13A F5A 106.3(15) . . ?
C13 C14 C15 113.7(10) . . ?
F7 C14 C13 108.6(11) . . ?
F7 C14 C15 108.3(11) . . ?
F7 C14 F8 110.1(12) . . ?
F8 C14 C13 108.8(11) . . ?
F8 C14 C15 107.4(12) . . ?
C15A C14A C13A 117(5) . . ?
F7A C14A C13A 115(7) . . ?
F7A C14A C15A 111(6) . . ?
F8A C14A C13A 94(8) . . ?
F8A C14A C15A 111(10) . . ?
F8A C14A F7A 106.7(15) . . ?
C16 C15 C14 114.0(12) . . ?
F9 C15 C14 110.1(16) . . ?
F9 C15 C16 108.5(18) . . ?
F9 C15 F10 106.4(13) . . ?
F10 C15 C14 108.6(11) . . ?
F10 C15 C16 108.9(13) . . ?
C16A C15A C14A 112(7) . . ?
F9A C15A C14A 102(10) . . ?
F9A C15A C16A 126(10) . . ?
F9A C15A F10A 106.8(15) . . ?
F10A C15A C14A 106(7) . . ?
F10A C15A C16A 103(7) . . ?
C15 C16 C17 114.7(14) . . ?
F11 C16 C15 108.5(14) . . ?
F11 C16 C17 107.7(14) . . ?
F12 C16 C15 107.7(18) . . ?
F12 C16 C17 107.5(17) . . ?
F12 C16 F11 111(2) . . ?
C15A C16A C17A 118(6) . . ?
F11A C16A C15A 114(8) . . ?
F11A C16A C17A 103(6) . . ?
F12A C16A C15A 115(10) . . ?
F12A C16A C17A 92(10) . . ?
F12A C16A F11A 113(10) . . ?
F13 C17 C16 108.5(16) . . ?
F14 C17 C16 109.3(15) . . ?
F14 C17 F13 106.3(16) . . ?
F15 C17 C16 111.9(16) . . ?
F15 C17 F13 110.7(18) . . ?
F15 C17 F14 109.9(18) . . ?
F13A C17A C16A 107(5) . . ?
F13A C17A F15A 111(4) . . ?
F14A C17A C16A 109(5) . . ?
F14A C17A F13A 111(4) . . ?
F14A C17A F15A 111(4) . . ?
F15A C17A C16A 107(5) . . ?
H18A C18 H18B 108.7 . . ?
C19 C18 H18A 110.5 . . ?
C19 C18 H18B 110.5 . . ?
O1 C18 H18A 110.5 . . ?
O1 C18 H18B 110.5 . . ?
O1 C18 C19 106.3(8) . . ?
C18 C19 H19A 108.5 . . ?
C18 C19 H19B 108.5 . . ?
C18 C19 C20 114.9(8) . . ?
H19A C19 H19B 107.5 . . ?
C20 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C19 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C21 C20 C19 111.8(8) . . ?
C21 C20 H20A 109.2 . . ?
C21 C20 H20B 109.2 . . ?
C20 C21 H21A 108.4 . . ?
C20 C21 H21B 108.4 . . ?
H21A C21 H21B 107.5 . . ?
C22 C21 C20 115.5(8) . . ?
C22 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
C21 C22 H22A 108.6 . . ?
C21 C22 H22B 108.6 . . ?
C21 C22 C23 114.7(8) . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 H22A 108.6 . . ?
C23 C22 H22B 108.6 . . ?
C22 C23 H23A 108.4 . . ?
C22 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
C24 C23 C22 115.4(8) . . ?
C24 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
C23 C24 H24A 108.6 . . ?
C23 C24 H24B 108.6 . . ?
C23 C24 C25 114.6(8) . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 H24A 108.6 . . ?
C25 C24 H24B 108.6 . . ?
C24 C25 H25A 108.5 . . ?
C24 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 C24 115.1(8) . . ?
C26 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
C25 C26 H26A 108.4 . . ?
C25 C26 H26B 108.4 . . ?
C25 C26 C27 115.7(8) . . ?
H26A C26 H26B 107.4 . . ?
C27 C26 H26A 108.4 . . ?
C27 C26 H26B 108.4 . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
C26 C27 C28 114.3(8) . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C29 C28 C27 113.7(10) . . ?
C29 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
F16 C30 F18 106.8(10) . . ?
F16 C30 S1 111.8(8) . . ?
F17 C30 F16 108.2(12) . . ?
F17 C30 F18 107.7(10) . . ?
F17 C30 S1 110.7(8) . . ?
F18 C30 S1 111.4(9) . . ?
F19 C31 F20 110.0(18) . . ?
F19 C31 F21 109.6(13) . . ?
F19 C31 S2 111.1(10) . . ?
F20 C31 S2 109.2(10) . . ?
F21 C31 F20 108.3(13) . . ?
F21 C31 S2 108.5(15) . . ?
C7 N1 C8 105.9(8) . . ?
C7 N1 C9 124.8(8) . . ?
C8 N1 C9 129.2(8) . . ?
C7 N2 C10 128.7(8) . . ?
C7 N2 N3 111.2(8) . . ?
N3 N2 C10 120.1(8) . . ?
C8 N3 N2 103.5(7) . . ?
S2 N4 S1 127.7(5) . . ?
C1 O1 C18 119.0(7) . . ?
N4 S1 C30 100.4(5) . . ?
O2 S1 C30 104.2(6) . . ?
O2 S1 N4 116.4(5) . . ?
O2 S1 O3 118.8(6) . . ?
O3 S1 C30 103.6(6) . . ?
O3 S1 N4 110.5(6) . . ?
N4 S2 C31 101.4(8) . . ?
O4 S2 C31 105.1(7) . . ?
O4 S2 N4 116.3(5) . . ?
O5 S2 C31 103.6(6) . . ?
O5 S2 N4 108.3(5) . . ?
O5 S2 O4 119.6(6) . . ?

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
C1 C2 C3 C4 1.6(16) . . . . ?
C2 C1 C6 C5 0.1(15) . . . . ?
C2 C1 O1 C18 157.7(9) . . . . ?
C2 C3 C4 C5 -4.3(15) . . . . ?
C2 C3 C4 C7 -179.2(9) . . . . ?
C3 C4 C5 C6 4.9(14) . . . . ?
C3 C4 C7 N1 -116.2(11) . . . . ?
C3 C4 C7 N2 62.6(13) . . . . ?
C4 C5 C6 C1 -2.7(14) . . . . ?
C4 C7 N1 C8 -179.4(9) . . . . ?
C4 C7 N1 C9 -0.2(16) . . . . ?
C4 C7 N2 C10 2.3(14) . . . . ?
C4 C7 N2 N3 179.7(8) . . . . ?
C5 C4 C7 N1 68.9(13) . . . . ?
C5 C4 C7 N2 -112.3(10) . . . . ?
C6 C1 C2 C3 0.5(16) . . . . ?
C6 C1 O1 C18 -19.7(14) . . . . ?
C7 C4 C5 C6 179.7(8) . . . . ?
C7 N2 N3 C8 0.4(10) . . . . ?
C8 C11 C12 C13 -169.8(9) . . . . ?
C8 C11 C12 C13A 172(3) . . . . ?
C8 C11 C12 F3 -49.1(12) . . . . ?
C8 C11 C12 F4 67.1(11) . . . . ?
C10 N2 N3 C8 178.0(8) . . . . ?
C11 C8 N1 C7 179.6(9) . . . . ?
C11 C8 N1 C9 0.6(18) . . . . ?
C11 C8 N3 N2 179.7(8) . . . . ?
C11 C12 C13 C14 -158.2(11) . . . . ?
C11 C12 C13 F5 -37.0(14) . . . . ?
C11 C12 C13 F6 78.2(13) . . . . ?
C11 C12 C13A C14A 157(5) . . . . ?
C11 C12 C13A F5A 46(5) . . . . ?
C11 C12 C13A F6A -71(5) . . . . ?
C12 C13 C14 C15 -165.6(11) . . . . ?
C12 C13 C14 F7 73.9(13) . . . . ?
C12 C13 C14 F8 -46.0(16) . . . . ?
C12 C13A C14A C15A 166(6) . . . . ?
C12 C13A C14A F7A -60(8) . . . . ?
C12 C13A C14A F8A 51(8) . . . . ?
C13 C14 C15 C16 -164.7(13) . . . . ?
C13 C14 C15 F9 -42(2) . . . . ?
C13 C14 C15 F10 73.7(14) . . . . ?
C13A C14A C15A C16A -172(7) . . . . ?
C13A C14A C15A F9A 52(10) . . . . ?
C13A C14A C15A F10A -60(10) . . . . ?
C14 C15 C16 C17 -167.9(15) . . . . ?
C14 C15 C16 F11 71.7(16) . . . . ?
C14 C15 C16 F12 -48(3) . . . . ?
C14A C15A C16A C17A 176(7) . . . . ?
C14A C15A C16A F11A -62(12) . . . . ?
C14A C15A C16A F12A 69(24) . . . . ?
C15 C16 C17 F13 -173.7(16) . . . . ?
C15 C16 C17 F14 -58(2) . . . . ?
C15 C16 C17 F15 64(2) . . . . ?
C15A C16A C17A F13A -170(8) . . . . ?
C15A C16A C17A F14A -49(8) . . . . ?
C15A C16A C17A F15A 71(8) . . . . ?
C18 C19 C20 C21 177.7(9) . . . . ?
C19 C18 O1 C1 -165.2(9) . . . . ?
C19 C20 C21 C22 -177.8(9) . . . . ?
C20 C21 C22 C23 178.4(9) . . . . ?
C21 C22 C23 C24 179.4(8) . . . . ?
C22 C23 C24 C25 179.3(9) . . . . ?
C23 C24 C25 C26 178.0(9) . . . . ?
C24 C25 C26 C27 179.3(9) . . . . ?
C25 C26 C27 C28 178.6(9) . . . . ?
C26 C27 C28 C29 -178.9(10) . . . . ?
F1 C11 C12 C13 70.0(12) . . . . ?
F1 C11 C12 C13A 52(3) . . . . ?
F1 C11 C12 F3 -169.3(8) . . . . ?
F1 C11 C12 F4 -53.1(10) . . . . ?
F2 C11 C12 C13 -48.3(13) . . . . ?
F2 C11 C12 C13A -66(3) . . . . ?
F2 C11 C12 F3 72.5(10) . . . . ?
F2 C11 C12 F4 -171.4(8) . . . . ?
F3 C12 C13 C14 80.7(13) . . . . ?
F3 C12 C13 F5 -158.2(9) . . . . ?
F3 C12 C13 F6 -42.9(13) . . . . ?
F3 C12 C13A C14A 24(7) . . . . ?
F3 C12 C13A F5A -87(4) . . . . ?
F3 C12 C13A F6A 157(4) . . . . ?
F4 C12 C13 C14 -36.0(14) . . . . ?
F4 C12 C13 F5 85.2(11) . . . . ?
F4 C12 C13 F6 -159.6(10) . . . . ?
F4 C12 C13A C14A -91(6) . . . . ?
F4 C12 C13A F5A 159(4) . . . . ?
F4 C12 C13A F6A 42(5) . . . . ?
F5 C13 C14 C15 73.7(15) . . . . ?
F5 C13 C14 F7 -46.8(12) . . . . ?
F5 C13 C14 F8 -166.6(11) . . . . ?
F5A C13A C14A C15A -76(8) . . . . ?
F5A C13A C14A F7A 58(6) . . . . ?
F5A C13A C14A F8A 168(7) . . . . ?
F6 C13 C14 C15 -43.6(15) . . . . ?
F6 C13 C14 F7 -164.2(10) . . . . ?
F6 C13 C14 F8 76.0(13) . . . . ?
F6A C13A C14A C15A 35(9) . . . . ?
F6A C13A C14A F7A 168(6) . . . . ?
F6A C13A C14A F8A -81(6) . . . . ?
F7 C14 C15 C16 -44.0(17) . . . . ?
F7 C14 C15 F9 78.3(17) . . . . ?
F7 C14 C15 F10 -165.6(11) . . . . ?
F7A C14A C15A C16A 53(10) . . . . ?
F7A C14A C15A F9A -83(8) . . . . ?
F7A C14A C15A F10A 165(7) . . . . ?
F8 C14 C15 C16 74.9(18) . . . . ?
F8 C14 C15 F9 -162.9(15) . . . . ?
F8 C14 C15 F10 -46.7(15) . . . . ?
F8A C14A C15A C16A -65(9) . . . . ?
F8A C14A C15A F9A 158(9) . . . . ?
F8A C14A C15A F10A 47(9) . . . . ?
F9 C15 C16 C17 69(2) . . . . ?
F9 C15 C16 F11 -51.4(17) . . . . ?
F9 C15 C16 F12 -171(2) . . . . ?
F9A C15A C16A C17A -60(14) . . . . ?
F9A C15A C16A F11A 62(16) . . . . ?
F9A C15A C16A F12A -167(25) . . . . ?
F10 C15 C16 C17 -46.4(19) . . . . ?
F10 C15 C16 F11 -166.9(11) . . . . ?
F10 C15 C16 F12 73(2) . . . . ?
F10A C15A C16A C17A 62(9) . . . . ?
F10A C15A C16A F11A -176(9) . . . . ?
F10A C15A C16A F12A -45(24) . . . . ?
F11 C16 C17 F13 -53(2) . . . . ?
F11 C16 C17 F14 63(2) . . . . ?
F11 C16 C17 F15 -175.2(15) . . . . ?
F11A C16A C17A F13A 64(9) . . . . ?
F11A C16A C17A F14A -176(9) . . . . ?
F11A C16A C17A F15A -56(9) . . . . ?
F12 C16 C17 F13 67(3) . . . . ?
F12 C16 C17 F14 -178(2) . . . . ?
F12 C16 C17 F15 -56(3) . . . . ?
F12A C16A C17A F13A -50(19) . . . . ?
F12A C16A C17A F14A 70(19) . . . . ?
F12A C16A C17A F15A -169(19) . . . . ?
F16 C30 S1 N4 -57.3(9) . . . . ?
F16 C30 S1 O2 63.6(9) . . . . ?
F16 C30 S1 O3 -171.5(8) . . . . ?
F17 C30 S1 N4 -177.9(9) . . . . ?
F17 C30 S1 O2 -57.1(11) . . . . ?
F17 C30 S1 O3 67.8(10) . . . . ?
F18 C30 S1 N4 62.2(9) . . . . ?
F18 C30 S1 O2 -176.9(8) . . . . ?
F18 C30 S1 O3 -52.0(9) . . . . ?
F19 C31 S2 N4 57.3(14) . . . . ?
F19 C31 S2 O4 178.8(12) . . . . ?
F19 C31 S2 O5 -55.0(14) . . . . ?
F20 C31 S2 N4 -64.2(14) . . . . ?
F20 C31 S2 O4 57.3(14) . . . . ?
F20 C31 S2 O5 -176.5(12) . . . . ?
F21 C31 S2 N4 177.9(10) . . . . ?
F21 C31 S2 O4 -60.6(12) . . . . ?
F21 C31 S2 O5 65.6(12) . . . . ?
N1 C7 N2 C10 -178.7(8) . . . . ?
N1 C7 N2 N3 -1.3(10) . . . . ?
N1 C8 C11 C12 92.8(13) . . . . ?
N1 C8 C11 F1 -146.8(10) . . . . ?
N1 C8 C11 F2 -27.8(14) . . . . ?
N1 C8 N3 N2 0.7(11) . . . . ?
N2 C7 N1 C8 1.6(10) . . . . ?
N2 C7 N1 C9 -179.2(10) . . . . ?
N3 C8 C11 C12 -86.0(12) . . . . ?
N3 C8 C11 F1 34.4(12) . . . . ?
N3 C8 C11 F2 153.4(9) . . . . ?
N3 C8 N1 C7 -1.5(12) . . . . ?
N3 C8 N1 C9 179.4(11) . . . . ?
O1 C1 C2 C3 -177.0(9) . . . . ?
O1 C1 C6 C5 177.3(9) . . . . ?
O1 C18 C19 C20 179.8(8) . . . . ?
S1 N4 S2 C31 94.4(10) . . . . ?
S1 N4 S2 O4 -18.9(12) . . . . ?
S1 N4 S2 O5 -156.9(8) . . . . ?
S2 N4 S1 C30 113.0(9) . . . . ?
S2 N4 S1 O2 1.4(11) . . . . ?
S2 N4 S1 O3 -138.0(8) . . . . ?

_olex2_date_sample_data_collection 2017-07-24
_olex2_date_sample_submission    2016-12-03
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id NV2434
_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 1.209
_oxdiff_exptl_absorpt_empirical_full_min 0.834
####################################################################### 
# 
# 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_dwb1717
_database_code_depnum_ccdc_archive 'CCDC 2177842'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2022-06-08 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_audit_creation_date             2017-05-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H39 F19 N3 O, B F4, C3 H6 O'
_chemical_formula_sum            'C36 H45 B F23 N3 O2'
_chemical_formula_weight         999.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C33 H39 B F23 N3 O'
_chemical_oxdiff_usercomment     'Alessio Riccobono ALR19'
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'
B B 0.0090 0.0039 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   40.3423(12)
_cell_length_b                   9.4231(3)
_cell_length_c                   11.2821(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.753(3)
_cell_angle_gamma                90
_cell_volume                     4283.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15671
_cell_measurement_temperature    110.00(14)
_cell_measurement_theta_max      70.9880
_cell_measurement_theta_min      5.4770
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.573
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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       block
_exptl_crystal_F_000             2040
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 6 0 0.1470
-3 0 -5 0.2527
2 -2 5 0.2603
3 1 5 0.2246
3 5 5 0.1852
-1 0 0 0.0364
1 0 0 0.0484
-1 -5 0 0.1682
5 0 1 0.1398
5 1 1 0.1304
-5 2 -1 0.1673
-5 -1 -1 0.2071
5 -2 1 0.1999
5 0 -2 0.2097
5 2 -2 0.2114
26 0 1 0.0554
24 2 1 0.0690
25 0 -2 0.0985
24 3 -1 0.0881

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method acetone/hexane
_exptl_crystal_size_max          0.518
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.085
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
1.0037 5.9946 0.0078 0.0043 -0.0117 -0.9806
-3.0015 0.0074 -5.0003 -0.1760 -0.6759 0.0121
2.0003 -2.0054 4.9978 0.1491 0.6809 0.3156
3.0021 0.9918 5.0017 0.1703 0.6743 -0.1753
3.0045 4.9884 5.0069 0.1477 0.6675 -0.8282
-1.0000 0.0003 0.0001 -0.0382 0.0016 0.0012
1.0000 -0.0003 -0.0001 0.0382 -0.0016 -0.0012
-1.0031 -4.9955 -0.0065 -0.0100 0.0100 0.8174
5.0005 -0.0028 0.9998 0.2032 0.1282 -0.0079
5.0011 0.9964 1.0011 0.1976 0.1265 -0.1711
-4.9993 2.0011 -0.9972 -0.2145 -0.1316 -0.3185
-5.0011 -0.9964 -1.0011 -0.1976 -0.1265 0.1711
4.9993 -2.0011 0.9972 0.2145 0.1316 0.3185
4.9997 0.0011 -2.0005 0.1664 -0.2802 -0.0029
5.0009 1.9994 -1.9979 0.1551 -0.2836 -0.3293
26.0016 -0.0089 0.9986 1.0053 0.0949 -0.0342
24.0027 1.9900 1.0014 0.9176 0.0947 -0.3581
25.0007 -0.0047 -2.0016 0.9302 -0.3120 -0.0279
24.0027 2.9917 -0.9975 0.8874 -0.1793 -0.5180

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            39137
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.366
_diffrn_reflns_theta_min         4.389
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  69.00   1.00    1.00    --    0.00  57.00-150.00   90
  2  ω    -30.00  70.00   1.00    1.00    --    0.00  77.00  90.00  100
  3  ω    -16.00  84.00   1.00    4.00    --   54.00 -77.00 120.00  100
  4  ω     28.00 126.00   1.00    4.00    --   54.00  37.00 -90.00   98
  5  ω     27.00 114.00   1.00    4.00    --   54.00-129.00 -39.00   87
  6  ω    -18.00  80.00   1.00    4.00    --   54.00 -37.00  90.00   98
  7  ω     40.00 130.00   1.00    8.00    --  108.00 -63.00   0.00   90
  8  ω     57.00 151.00   1.00    8.00    --  108.00 178.00  60.00   94
  9  ω     74.00 178.00   1.00    8.00    --  108.00  25.00-180.00  104
 10  ω     74.00 178.00   1.00    8.00    --  108.00  25.00 -90.00  104
 11  ω     36.00 116.00   1.00    8.00    --  108.00-111.00  30.00   80
 12  ω     38.00 130.00   1.00    8.00    --  108.00 -50.00-180.00   92
 13  ω     86.00 176.00   1.00    8.00    --  108.00  63.00 -30.00   90
 14  ω    -30.00  70.00   1.00    1.00    --    0.00  77.00 -90.00  100
 15  ω    -73.00  73.00   1.00    1.00    --    0.00   3.00 -75.00  146
 16  ω    -15.00  75.00   1.00    4.00    --   54.00 -57.00 -30.00   90
 17  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 -30.00  100
 18  ω     24.00 124.00   1.00    4.00    --   54.00  77.00 150.00  100
 19  ω     28.00 126.00   1.00    4.00    --   54.00  37.00  90.00   98
 20  ω     74.00 178.00   1.00    8.00    --  108.00  25.00  60.00  104
 21  ω     86.00 178.00   1.00    8.00    --  108.00  50.00 -60.00   92
 22  ω     78.00 178.00   1.00    8.00    --  108.00  77.00  90.00  100
 23  ω     86.00 178.00   1.00    8.00    --  108.00  50.00-150.00   92
 24  ω     36.00 116.00   1.00    8.00    --  108.00-111.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0381888000
_diffrn_orient_matrix_UB_12      -0.0056893000
_diffrn_orient_matrix_UB_13      0.0122590000
_diffrn_orient_matrix_UB_21      -0.0015797000
_diffrn_orient_matrix_UB_22      -0.0018685000
_diffrn_orient_matrix_UB_23      0.1361256000
_diffrn_orient_matrix_UB_31      -0.0012975000
_diffrn_orient_matrix_UB_32      -0.1633564000
_diffrn_orient_matrix_UB_33      -0.0018850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7338
_reflns_number_total             8204
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.65
_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 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         8204
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.088
_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)+(0.0395P)²+7.3765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1398
_refine_special_details          
'Most of the C9F19 chain was disordered and modelled in two positions. The ADPs of a number of disordered atoms were restrained to be approx. isotropic.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A)
\\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F11A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F16A)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(C27A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(C32A)=Sof(C33A)=
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=
 Sof(F11A)=Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(F16A)=Sof(F17A)=
 Sof(F18A)=Sof(F19A)=1-FVAR(1)
 Sof(C27)=Sof(C28)=Sof(C29)=Sof(C30)=Sof(C31)=Sof(C32)=Sof(C33)=Sof(F3)=
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=Sof(F19)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C)
;
_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
C1 C 0.74523(5) 0.5053(2) 1.16644(19) 0.0215(5) Uani 1 1 d . . . . .
C2 C 0.71568(5) 0.4632(2) 1.09619(18) 0.0201(4) Uani 1 1 d . . . . .
C3 C 0.69843(6) 0.5648(2) 1.0284(2) 0.0239(5) Uani 1 1 d . . . . .
H3 H 0.7045 0.6598 1.0350 0.029 Uiso 1 1 calc R . . . .
C4 C 0.67239(6) 0.5258(2) 0.9515(2) 0.0233(5) Uani 1 1 d . . . . .
H4 H 0.6610 0.5941 0.9061 0.028 Uiso 1 1 calc R . . . .
C5 C 0.66323(5) 0.3837(2) 0.94225(19) 0.0206(4) Uani 1 1 d . . . . .
C6 C 0.67905(5) 0.2823(2) 1.01544(19) 0.0210(4) Uani 1 1 d . . . . .
H6 H 0.6718 0.1886 1.0131 0.025 Uiso 1 1 calc R . . . .
C7 C 0.70541(5) 0.3212(2) 1.09122(19) 0.0202(4) Uani 1 1 d . . . . .
H7 H 0.7163 0.2534 1.1387 0.024 Uiso 1 1 calc R . . . .
C8 C 0.62648(5) 0.4339(2) 0.7751(2) 0.0231(5) Uani 1 1 d . . . . .
H8A H 0.6446 0.4758 0.7340 0.028 Uiso 1 1 calc R . . . .
H8B H 0.6143 0.5094 0.8121 0.028 Uiso 1 1 calc R . . . .
C9 C 0.60386(5) 0.3535(2) 0.6887(2) 0.0223(5) Uani 1 1 d . . . . .
H9A H 0.5872 0.3043 0.7322 0.027 Uiso 1 1 calc R . . . .
H9B H 0.6167 0.2828 0.6486 0.027 Uiso 1 1 calc R . . . .
C10 C 0.58672(5) 0.4499(2) 0.5967(2) 0.0225(5) Uani 1 1 d . . . . .
H10A H 0.6034 0.4994 0.5535 0.027 Uiso 1 1 calc R . . . .
H10B H 0.5738 0.5204 0.6369 0.027 Uiso 1 1 calc R . . . .
C11 C 0.56396(5) 0.3684(2) 0.50908(19) 0.0224(5) Uani 1 1 d . . . . .
H11A H 0.5774 0.3040 0.4644 0.027 Uiso 1 1 calc R . . . .
H11B H 0.5488 0.3113 0.5534 0.027 Uiso 1 1 calc R . . . .
C12 C 0.54370(5) 0.4608(2) 0.42206(19) 0.0221(5) Uani 1 1 d . . . . .
H12A H 0.5587 0.5170 0.3764 0.027 Uiso 1 1 calc R . . . .
H12B H 0.5303 0.5258 0.4662 0.027 Uiso 1 1 calc R . . . .
C13 C 0.52106(5) 0.3751(2) 0.33706(19) 0.0223(5) Uani 1 1 d . . . . .
H13A H 0.5065 0.3176 0.3832 0.027 Uiso 1 1 calc R . . . .
H13B H 0.5346 0.3112 0.2925 0.027 Uiso 1 1 calc R . . . .
C14 C 0.49992(5) 0.4646(2) 0.2498(2) 0.0221(5) Uani 1 1 d . . . . .
H14A H 0.4860 0.5274 0.2940 0.026 Uiso 1 1 calc R . . . .
H14B H 0.5144 0.5232 0.2041 0.026 Uiso 1 1 calc R . . . .
C15 C 0.47799(5) 0.3759(2) 0.1648(2) 0.0227(5) Uani 1 1 d . . . . .
H15A H 0.4920 0.3133 0.1207 0.027 Uiso 1 1 calc R . . . .
H15B H 0.4636 0.3170 0.2107 0.027 Uiso 1 1 calc R . . . .
C16 C 0.45662(5) 0.4635(2) 0.0773(2) 0.0221(5) Uani 1 1 d . . . . .
H16A H 0.4710 0.5221 0.0313 0.027 Uiso 1 1 calc R . . . .
H16B H 0.4427 0.5265 0.1216 0.027 Uiso 1 1 calc R . . . .
C17 C 0.43449(5) 0.3754(2) -0.0075(2) 0.0234(5) Uani 1 1 d . . . . .
H17A H 0.4204 0.3154 0.0384 0.028 Uiso 1 1 calc R . . . .
H17B H 0.4483 0.3141 -0.0533 0.028 Uiso 1 1 calc R . . . .
C18 C 0.41272(5) 0.4650(2) -0.0925(2) 0.0226(5) Uani 1 1 d . . . . .
H18A H 0.3988 0.5255 -0.0464 0.027 Uiso 1 1 calc R . . . .
H18B H 0.4269 0.5262 -0.1372 0.027 Uiso 1 1 calc R . . . .
C19 C 0.39066(5) 0.3799(2) -0.1796(2) 0.0235(5) Uani 1 1 d . . . . .
H19A H 0.4046 0.3202 -0.2267 0.028 Uiso 1 1 calc R . . . .
H19B H 0.3765 0.3181 -0.1353 0.028 Uiso 1 1 calc R . . . .
C20 C 0.36896(5) 0.4713(2) -0.2626(2) 0.0232(5) Uani 1 1 d . . . . .
H20A H 0.3830 0.5351 -0.3054 0.028 Uiso 1 1 calc R . . . .
H20B H 0.3545 0.5286 -0.2160 0.028 Uiso 1 1 calc R . . . .
C21 C 0.34794(6) 0.3843(3) -0.3515(2) 0.0299(5) Uani 1 1 d . . . . .
H21A H 0.3354 0.4469 -0.4038 0.045 Uiso 1 1 calc GR . . . .
H21B H 0.3330 0.3252 -0.3098 0.045 Uiso 1 1 calc GR . . . .
H21C H 0.3621 0.3258 -0.3969 0.045 Uiso 1 1 calc GR . . . .
C22 C 0.73418(6) 0.3927(3) 1.3631(2) 0.0321(6) Uani 1 1 d . . . . .
H22A H 0.7418 0.2962 1.3634 0.048 Uiso 1 1 calc GR . . . .
H22B H 0.7110 0.3954 1.3391 0.048 Uiso 1 1 calc GR . . . .
H22C H 0.7373 0.4318 1.4415 0.048 Uiso 1 1 calc GR . . . .
C23 C 0.77380(6) 0.6327(3) 1.0045(2) 0.0301(5) Uani 1 1 d . . . . .
H23A H 0.7587 0.5803 0.9528 0.045 Uiso 1 1 calc GR . . . .
H23B H 0.7961 0.6160 0.9822 0.045 Uiso 1 1 calc GR . . . .
H23C H 0.7689 0.7321 0.9980 0.045 Uiso 1 1 calc GR . . . .
C24 C 0.79194(5) 0.6019(3) 1.2231(2) 0.0250(5) Uani 1 1 d . . . . .
C25 C 0.82274(6) 0.6922(3) 1.2279(2) 0.0291(5) Uani 1 1 d . . . . .
C26 C 0.85490(6) 0.6179(3) 1.1913(2) 0.0257(5) Uani 1 1 d . . . . .
C27 C 0.8865(3) 0.7055(13) 1.2161(8) 0.029(2) Uani 0.6218(15) 1 d . U P A 1
C27A C 0.8853(5) 0.723(2) 1.1800(12) 0.025(3) Uani 0.3782(15) 1 d . U P A 2
C28 C 0.91637(16) 0.6592(8) 1.1418(5) 0.0239(13) Uani 0.6218(15) 1 d . U P A 1
C28A C 0.9196(3) 0.6604(14) 1.1838(9) 0.028(3) Uani 0.3782(15) 1 d . U P A 2
C29 C 0.95052(11) 0.7183(5) 1.1917(5) 0.0260(10) Uani 0.6218(15) 1 d . . P A 1
C29A C 0.94686(19) 0.7496(9) 1.1325(8) 0.0314(17) Uani 0.3782(15) 1 d . . P A 2
C30 C 0.97847(11) 0.7145(5) 1.1036(5) 0.0270(10) Uani 0.6218(15) 1 d . . P A 1
C30A C 0.98242(18) 0.6982(9) 1.1645(8) 0.0306(17) Uani 0.3782(15) 1 d . . P A 2
C31 C 1.01388(10) 0.7188(5) 1.1608(4) 0.0263(8) Uani 0.6218(15) 1 d . . P A 1
C31A C 1.00995(16) 0.7687(7) 1.0943(7) 0.0253(13) Uani 0.3782(15) 1 d . . P A 2
C32 C 1.04161(13) 0.7532(6) 1.0770(5) 0.0357(11) Uani 0.6218(15) 1 d . . P A 1
C32A C 1.0458(2) 0.7405(11) 1.1401(9) 0.041(2) Uani 0.3782(15) 1 d . . P A 2
C33 C 1.07692(12) 0.7145(6) 1.1221(6) 0.0466(12) Uani 0.6218(15) 1 d . . P A 1
C33A C 1.07304(18) 0.7914(11) 1.0597(9) 0.044(2) Uani 0.3782(15) 1 d . . P A 2
F1 F 0.81785(4) 0.80518(16) 1.15641(18) 0.0464(4) Uani 1 1 d . . . . .
F2 F 0.82858(4) 0.7377(2) 1.34014(15) 0.0490(5) Uani 1 1 d . . . . .
F3 F 0.85751(13) 0.4922(6) 1.2455(5) 0.0402(11) Uani 0.6218(15) 1 d . . P A 1
F3A F 0.8640(2) 0.5274(10) 1.2841(8) 0.0408(18) Uani 0.3782(15) 1 d . . P A 2
F4 F 0.8520(2) 0.5877(9) 1.0710(7) 0.0365(13) Uani 0.6218(15) 1 d . . P A 1
F4A F 0.8490(4) 0.5506(14) 1.0973(11) 0.040(3) Uani 0.3782(15) 1 d . . P A 2
F5 F 0.88060(10) 0.8416(5) 1.1966(5) 0.0634(15) Uani 0.6218(15) 1 d . . P A 1
F5A F 0.87938(10) 0.7904(5) 1.0770(4) 0.0460(12) Uani 0.3782(15) 1 d . . P A 2
F6 F 0.89567(6) 0.6858(4) 1.3297(2) 0.0581(10) Uani 0.6218(15) 1 d . . P A 1
F6A F 0.88496(17) 0.8233(9) 1.2659(6) 0.054(2) Uani 0.3782(15) 1 d . . P A 2
F7 F 0.9165(3) 0.5297(14) 1.1213(9) 0.043(2) Uani 0.6218(15) 1 d . . P A 1
F7A F 0.92809(10) 0.6224(6) 1.2957(4) 0.0557(14) Uani 0.3782(15) 1 d . . P A 2
F8 F 0.91116(7) 0.7137(4) 1.0322(2) 0.0584(9) Uani 0.6218(15) 1 d . . P A 1
F8A F 0.9189(6) 0.524(2) 1.1489(17) 0.064(5) Uani 0.3782(15) 1 d . U P A 2
F9 F 0.94729(10) 0.8478(4) 1.2330(4) 0.0498(11) Uani 0.6218(15) 1 d . . P A 1
F9A F 0.94256(10) 0.7523(7) 1.0154(4) 0.0639(17) Uani 0.3782(15) 1 d . . P A 2
F10 F 0.95987(6) 0.6353(4) 1.2850(2) 0.0497(8) Uani 0.6218(15) 1 d . . P A 1
F10A F 0.94286(18) 0.8820(8) 1.1693(8) 0.059(2) Uani 0.3782(15) 1 d . . P A 2
F11 F 0.97518(7) 0.5970(4) 1.0378(3) 0.0591(10) Uani 0.6218(15) 1 d . . P A 1
F11A F 0.98899(12) 0.7335(9) 1.2788(4) 0.084(2) Uani 0.3782(15) 1 d . U P A 2
F12 F 0.97459(7) 0.8267(4) 1.0310(3) 0.0629(10) Uani 0.6218(15) 1 d . . P A 1
F12A F 0.98388(11) 0.5615(5) 1.1517(7) 0.0734(19) Uani 0.3782(15) 1 d . U P A 2
F13 F 1.01463(6) 0.8181(4) 1.2450(3) 0.0612(10) Uani 0.6218(15) 1 d . . P A 1
F13A F 1.00672(10) 0.7220(7) 0.9824(4) 0.0608(16) Uani 0.3782(15) 1 d . . P A 2
F14 F 1.02061(7) 0.5926(3) 1.2095(3) 0.0587(9) Uani 0.6218(15) 1 d . . P A 1
F14A F 1.00426(11) 0.9086(5) 1.0872(5) 0.0582(15) Uani 0.3782(15) 1 d . . P A 2
F15 F 1.03572(7) 0.6867(4) 0.9743(2) 0.0630(10) Uani 0.6218(15) 1 d . . P A 1
F15A F 1.05021(12) 0.8140(9) 1.2419(4) 0.083(2) Uani 0.3782(15) 1 d . . P A 2
F16 F 1.04107(8) 0.8933(4) 1.0550(4) 0.0788(12) Uani 0.6218(15) 1 d . . P A 1
F16A F 1.04955(12) 0.6043(6) 1.1547(7) 0.090(2) Uani 0.3782(15) 1 d . U P A 2
F17 F 1.08314(8) 0.7667(5) 1.2288(4) 0.0841(13) Uani 0.6218(15) 1 d . . P A 1
F17A F 1.07252(13) 0.7277(8) 0.9606(6) 0.091(2) Uani 0.3782(15) 1 d . . P A 2
F18 F 1.08123(7) 0.5766(3) 1.1253(3) 0.0589(8) Uani 0.6218(15) 1 d . . P A 1
F18A F 1.06990(13) 0.9276(6) 1.0372(7) 0.082(2) Uani 0.3782(15) 1 d . . P A 2
F19 F 1.09899(14) 0.7642(9) 1.0501(5) 0.0864(18) Uani 0.6218(15) 1 d . U P A 1
F19A F 1.1016(2) 0.7768(14) 1.1149(7) 0.074(2) Uani 0.3782(15) 1 d . U P A 2
N1 N 0.75312(4) 0.4764(2) 1.27979(16) 0.0241(4) Uani 1 1 d . . . . .
N2 N 0.78234(5) 0.5353(2) 1.31703(17) 0.0271(4) Uani 1 1 d . . . . .
N3 N 0.77026(4) 0.5860(2) 1.12835(16) 0.0212(4) Uani 1 1 d . . . . .
O1 O 0.63920(4) 0.33544(16) 0.86402(14) 0.0233(3) Uani 1 1 d . . . . .
B1 B 0.72895(7) 0.5670(3) 0.6950(2) 0.0289(6) Uani 1 1 d . . . . .
F20 F 0.69845(4) 0.5572(2) 0.63604(16) 0.0553(5) Uani 1 1 d . . . . .
F21 F 0.73186(5) 0.69421(16) 0.75697(14) 0.0469(4) Uani 1 1 d . . . . .
F22 F 0.73320(4) 0.45433(16) 0.77306(14) 0.0411(4) Uani 1 1 d . . . . .
F23 F 0.75371(4) 0.5622(2) 0.61308(15) 0.0529(5) Uani 1 1 d . . . . .
C34 C 0.81335(7) 0.2993(3) 0.6396(3) 0.0402(7) Uani 1 1 d . . . . .
C35 C 0.81294(8) 0.3545(4) 0.7622(3) 0.0533(8) Uani 1 1 d . . . . .
H35A H 0.8030 0.2856 0.8120 0.080 Uiso 1 1 calc GR . . . .
H35B H 0.8003 0.4409 0.7627 0.080 Uiso 1 1 calc GR . . . .
H35C H 0.8353 0.3731 0.7915 0.080 Uiso 1 1 calc GR . . . .
C36 C 0.83237(8) 0.3822(4) 0.5536(3) 0.0494(8) Uani 1 1 d . . . . .
H36A H 0.8199 0.4647 0.5290 0.074 Uiso 1 1 calc GR . . . .
H36B H 0.8363 0.3244 0.4856 0.074 Uiso 1 1 calc GR . . . .
H36C H 0.8532 0.4111 0.5906 0.074 Uiso 1 1 calc GR . . . .
O2 O 0.79815(7) 0.1935(3) 0.6079(3) 0.0698(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.455(3) . ?
C1 N1 1.331(3) . ?
C1 N3 1.350(3) . ?
C2 C3 1.390(3) . ?
C2 C7 1.401(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.380(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.391(3) . ?
C5 C6 1.397(3) . ?
C5 O1 1.358(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.381(3) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.506(3) . ?
C8 O1 1.442(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.520(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.524(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.521(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.524(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.526(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.523(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.522(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.523(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 C18 1.524(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.522(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 C20 1.519(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C21 1.521(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C22 N1 1.469(3) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C23 N3 1.479(3) . ?
C24 C25 1.504(3) . ?
C24 N2 1.306(3) . ?
C24 N3 1.357(3) . ?
C25 C26 1.547(3) . ?
C25 F1 1.345(3) . ?
C25 F2 1.347(3) . ?
C26 C27 1.534(13) . ?
C26 C27A 1.586(19) . ?
C26 F3 1.335(6) . ?
C26 F3A 1.387(10) . ?
C26 F4 1.387(9) . ?
C26 F4A 1.249(15) . ?
C27 C28 1.562(12) . ?
C27 F5 1.321(13) . ?
C27 F6 1.329(9) . ?
C27A C28A 1.50(2) . ?
C27A F5A 1.336(14) . ?
C27A F6A 1.36(2) . ?
C28 C29 1.566(8) . ?
C28 F7 1.242(15) . ?
C28 F8 1.345(7) . ?
C28A C29A 1.520(15) . ?
C28A F7A 1.340(11) . ?
C28A F8A 1.34(2) . ?
C29 C30 1.539(6) . ?
C29 F9 1.315(6) . ?
C29 F10 1.351(6) . ?
C29A C30A 1.541(11) . ?
C29A F9A 1.325(10) . ?
C29A F10A 1.327(11) . ?
C30 C31 1.539(6) . ?
C30 F11 1.336(5) . ?
C30 F12 1.343(6) . ?
C30A C31A 1.545(10) . ?
C30A F11A 1.346(10) . ?
C30A F12A 1.297(10) . ?
C31 C32 1.534(6) . ?
C31 F13 1.332(5) . ?
C31 F14 1.333(5) . ?
C31A C32A 1.536(11) . ?
C31A F13A 1.338(8) . ?
C31A F14A 1.339(8) . ?
C32 C33 1.533(8) . ?
C32 F15 1.329(7) . ?
C32 F16 1.344(6) . ?
C32A C33A 1.535(13) . ?
C32A F15A 1.345(12) . ?
C32A F16A 1.303(12) . ?
C33 F17 1.313(6) . ?
C33 F18 1.311(7) . ?
C33 F19 1.320(8) . ?
C33A F17A 1.268(10) . ?
C33A F18A 1.313(12) . ?
C33A F19A 1.290(13) . ?
N1 N2 1.352(3) . ?
B1 F20 1.373(3) . ?
B1 F21 1.390(3) . ?
B1 F22 1.384(3) . ?
B1 F23 1.394(3) . ?
C34 C35 1.479(5) . ?
C34 C36 1.488(4) . ?
C34 O2 1.215(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

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
N1 C1 C2 128.3(2) . . ?
N1 C1 N3 105.8(2) . . ?
N3 C1 C2 125.9(2) . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 C7 119.8(2) . . ?
C7 C2 C1 121.0(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.7(2) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.1(2) . . ?
O1 C5 C4 123.4(2) . . ?
O1 C5 C6 116.5(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.1(2) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 H7 120.2 . . ?
C6 C7 C2 119.7(2) . . ?
C6 C7 H7 120.2 . . ?
H8A C8 H8B 108.4 . . ?
C9 C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
O1 C8 H8A 110.1 . . ?
O1 C8 H8B 110.1 . . ?
O1 C8 C9 108.12(18) . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C8 C9 C10 112.54(19) . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C9 C10 H10B 109.1 . . ?
C9 C10 C11 112.48(19) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C10 C11 H11A 108.6 . . ?
C10 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C12 C11 C10 114.74(19) . . ?
C12 C11 H11A 108.6 . . ?
C12 C11 H11B 108.6 . . ?
C11 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
C11 C12 C13 112.97(19) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C12 C13 H13A 108.7 . . ?
C12 C13 H13B 108.7 . . ?
C12 C13 C14 114.41(19) . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 C13 113.12(19) . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C14 113.83(19) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C15 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
C15 C16 C17 114.10(19) . . ?
H16A C16 H16B 107.6 . . ?
C17 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C16 C17 H17A 108.9 . . ?
C16 C17 H17B 108.9 . . ?
C16 C17 C18 113.34(19) . . ?
H17A C17 H17B 107.7 . . ?
C18 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C17 C18 H18A 108.6 . . ?
C17 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C19 C18 C17 114.57(19) . . ?
C19 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 C18 113.64(19) . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C19 C20 C21 112.77(19) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
N2 C24 C25 121.3(2) . . ?
N2 C24 N3 112.4(2) . . ?
N3 C24 C25 126.2(2) . . ?
C24 C25 C26 115.9(2) . . ?
F1 C25 C24 109.2(2) . . ?
F1 C25 C26 107.39(19) . . ?
F1 C25 F2 109.0(2) . . ?
F2 C25 C24 108.70(19) . . ?
F2 C25 C26 106.5(2) . . ?
C25 C26 C27A 113.7(8) . . ?
C27 C26 C25 114.2(5) . . ?
F3 C26 C25 109.2(3) . . ?
F3 C26 C27 110.3(5) . . ?
F3 C26 F4 105.5(4) . . ?
F3A C26 C25 105.8(5) . . ?
F3A C26 C27A 105.4(7) . . ?
F4 C26 C25 108.8(5) . . ?
F4 C26 C27 108.6(5) . . ?
F4A C26 C25 109.2(8) . . ?
F4A C26 C27A 111.4(7) . . ?
F4A C26 F3A 111.2(7) . . ?
C26 C27 C28 114.0(8) . . ?
F5 C27 C26 110.4(8) . . ?
F5 C27 C28 108.7(8) . . ?
F5 C27 F6 109.6(9) . . ?
F6 C27 C26 106.9(7) . . ?
F6 C27 C28 107.1(8) . . ?
C28A C27A C26 117.9(13) . . ?
F5A C27A C26 105.0(12) . . ?
F5A C27A C28A 109.8(12) . . ?
F5A C27A F6A 106.4(14) . . ?
F6A C27A C26 110.0(11) . . ?
F6A C27A C28A 107.1(13) . . ?
C27 C28 C29 113.2(6) . . ?
F7 C28 C27 112.7(8) . . ?
F7 C28 C29 113.8(8) . . ?
F7 C28 F8 101.9(7) . . ?
F8 C28 C27 107.2(6) . . ?
F8 C28 C29 106.9(5) . . ?
C27A C28A C29A 117.0(11) . . ?
F7A C28A C27A 108.9(9) . . ?
F7A C28A C29A 110.5(9) . . ?
F7A C28A F8A 91.2(13) . . ?
F8A C28A C27A 111.1(15) . . ?
F8A C28A C29A 115.0(13) . . ?
C30 C29 C28 114.8(4) . . ?
F9 C29 C28 110.9(4) . . ?
F9 C29 C30 109.8(4) . . ?
F9 C29 F10 106.8(4) . . ?
F10 C29 C28 106.4(4) . . ?
F10 C29 C30 107.7(4) . . ?
C28A C29A C30A 114.8(8) . . ?
F9A C29A C28A 109.2(7) . . ?
F9A C29A C30A 108.4(7) . . ?
F9A C29A F10A 106.3(8) . . ?
F10A C29A C28A 107.4(8) . . ?
F10A C29A C30A 110.4(7) . . ?
C29 C30 C31 115.0(4) . . ?
F11 C30 C29 108.8(4) . . ?
F11 C30 C31 108.7(4) . . ?
F11 C30 F12 107.9(4) . . ?
F12 C30 C29 107.9(4) . . ?
F12 C30 C31 108.3(4) . . ?
C29A C30A C31A 115.4(7) . . ?
F11A C30A C29A 106.5(7) . . ?
F11A C30A C31A 105.7(6) . . ?
F12A C30A C29A 109.4(6) . . ?
F12A C30A C31A 109.4(7) . . ?
F12A C30A F11A 110.1(8) . . ?
C32 C31 C30 115.9(4) . . ?
F13 C31 C30 107.9(3) . . ?
F13 C31 C32 107.4(4) . . ?
F13 C31 F14 109.6(4) . . ?
F14 C31 C30 108.4(4) . . ?
F14 C31 C32 107.6(3) . . ?
C32A C31A C30A 116.2(7) . . ?
F13A C31A C30A 107.6(6) . . ?
F13A C31A C32A 107.9(6) . . ?
F13A C31A F14A 105.0(7) . . ?
F14A C31A C30A 109.2(5) . . ?
F14A C31A C32A 110.3(6) . . ?
C31 C32 C33 116.0(5) . . ?
F15 C32 C31 109.5(4) . . ?
F15 C32 C33 107.6(4) . . ?
F15 C32 F16 107.5(5) . . ?
F16 C32 C31 108.4(4) . . ?
F16 C32 C33 107.6(4) . . ?
C33A C32A C31A 115.9(8) . . ?
F15A C32A C31A 106.4(7) . . ?
F15A C32A C33A 106.0(7) . . ?
F16A C32A C31A 108.4(7) . . ?
F16A C32A C33A 107.5(8) . . ?
F16A C32A F15A 112.9(9) . . ?
F17 C33 C32 110.4(4) . . ?
F17 C33 F19 109.1(5) . . ?
F18 C33 C32 111.4(4) . . ?
F18 C33 F17 109.1(6) . . ?
F18 C33 F19 106.0(5) . . ?
F19 C33 C32 110.8(6) . . ?
F17A C33A C32A 113.0(7) . . ?
F17A C33A F18A 107.2(10) . . ?
F17A C33A F19A 110.6(8) . . ?
F18A C33A C32A 110.8(7) . . ?
F19A C33A C32A 109.2(9) . . ?
F19A C33A F18A 105.9(9) . . ?
C1 N1 C22 128.1(2) . . ?
C1 N1 N2 112.30(18) . . ?
N2 N1 C22 119.60(19) . . ?
C24 N2 N1 103.50(19) . . ?
C1 N3 C23 125.2(2) . . ?
C1 N3 C24 105.97(18) . . ?
C24 N3 C23 128.60(19) . . ?
C5 O1 C8 117.11(17) . . ?
F20 B1 F21 110.7(2) . . ?
F20 B1 F22 109.7(2) . . ?
F20 B1 F23 109.3(2) . . ?
F21 B1 F23 108.4(2) . . ?
F22 B1 F21 109.7(2) . . ?
F22 B1 F23 109.1(2) . . ?
C35 C34 C36 117.0(3) . . ?
O2 C34 C35 122.4(3) . . ?
O2 C34 C36 120.6(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

_olex2_date_sample_data_collection 2017-05-09
_olex2_date_sample_submission    2017-05-09
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id ALR19
_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 1.609
_oxdiff_exptl_absorpt_empirical_full_min 0.540
