#------------------------------------------------------------------------------
#$Date: 2023-03-04 19:45:42 +0200 (Sat, 04 Mar 2023) $
#$Revision: 281335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/80/1568075.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1568075
loop_
_publ_author_name
'Turley, Andrew T.'
'Hanson-Heine, Magnus W D'
'Argent, Stephen P.'
'Hu, Yaoyang'
'Jones, Thomas A.'
'Fay, Michael'
'Woodward, Simon'
_publ_section_title
;
 Catalysis enabled synthesis, structures, and reactivities of fluorinated
 S₈-corona[n]arenes (n = 8-12).
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              70
_journal_page_last               77
_journal_paper_doi               10.1039/d2sc05348a
_journal_volume                  14
_journal_year                    2022
_chemical_formula_moiety         '2(C24 H8 F8 S4)'
_chemical_formula_sum            'C56 H32 F16 O2 S8'
_chemical_formula_weight         1297.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-05-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-26 deposited with the CCDC.	2022-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                97.914(2)
_cell_angle_beta                 98.988(2)
_cell_angle_gamma                110.147(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6071(3)
_cell_length_b                   14.6029(3)
_cell_length_c                   15.3344(3)
_cell_measurement_reflns_used    14778
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5300
_cell_measurement_theta_min      4.0690
_cell_volume                     2764.52(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  10.00   0.50    1.00    --    0.00  57.00-150.00   70
  2  ω    -33.00  -1.00   0.50    1.00    --    0.00 -82.00   0.00   64
  3  ω     12.00  38.00   0.50    1.00    --    0.00 -82.00   0.00   52
  4  ω    -32.00   3.00   0.50    1.00    --    0.00  57.00 150.00   70
  5  ω     60.00  89.00   0.50    1.00    --    0.00  57.00-150.00   58
  6  ω      6.00  86.00   0.50    1.00    --    0.00  57.00 150.00  160
  7  ω    -26.00  50.00   0.50    1.00    --    0.00 -82.00  60.00  152
  8  ω     20.00  57.00   0.50    1.00    --    0.00  57.00-150.00   74
  9  ω    -30.00 108.00   0.50    4.00    --   57.50 -82.00 -60.00  276
 10  ω     14.00  40.00   0.50    4.00    --   57.50  71.00  -8.49   52
 11  ω     12.00  45.00   0.50    4.00    --   57.50  72.00-127.80   66
 12  ω     11.00 141.00   0.50    4.00    --   57.50  72.00 156.09  260
 13  ω    -16.00 102.00   0.50    4.00    --   57.50 -61.00 150.00  236
 14  ω    -24.00  98.00   0.50    4.00    --   57.50 -82.00 150.00  244
 15  ω     73.00 130.00   0.50    4.00    --   57.50  72.00  89.44  114
 16  ω     12.00 105.00   0.50    4.00    --   57.50  70.00 -58.96  186
 17  ω     11.00  47.00   0.50    4.00    --   57.50  72.00  38.57   72
 18  ω     11.00  67.00   0.50    4.00    --   57.50  72.00-114.45  112
 19  ω     60.00 144.00   0.50    4.00    --   57.50  72.00-154.81  168
 20  ω     72.00 123.00   0.50    4.00    --   57.50  72.00  38.57  102
 21  ω     13.00 119.00   0.50    4.00    --   57.50  71.00  57.70  212
 22  ω     11.00  55.00   0.50    4.00    --   57.50  72.00  89.44   88
 23  ω     11.00 142.00   0.50    4.00    --   57.50  70.00 139.20  262
 24  ω     56.00 137.00   0.50    4.00    --   57.50  72.00-127.80  162
 25  ω     12.00  46.00   0.50    4.00    --   57.50  72.00-154.81   68
 26  ω     11.00 146.00   0.50    4.00    --   57.50  70.00 -27.94  270
 27  ω     97.00 144.00   0.50    4.00    --   57.50  72.00-114.45   94
 28  ω     46.00 146.00   0.50    4.00    --   57.50  71.00  -8.49  200
 29  ω     -2.00 104.00   0.50    4.00    --   57.50 -61.00 -60.00  212
 30  ω     67.00 104.00   0.50    4.00    --   57.50 -82.00   0.00   74
 31  ω     68.00 190.00   0.50   10.00    --  115.00  63.00-105.98  244
 32  ω    110.00 204.00   0.50   10.00    --  115.00  47.00 -11.60  188
 33  ω    137.00 201.00   0.50   10.00    --  115.00  47.00  34.98  128
 34  ω     35.00  97.00   0.50   10.00    --  115.00  47.00 -11.60  124
 35  ω     62.00 132.00   0.50   10.00    --  115.00 -82.00 120.00  140
 36  ω    167.00 203.00   0.50   10.00    --  115.00  73.00 -18.06   72
 37  ω     34.00  68.00   0.50   10.00    --  115.00  47.00  34.98   68
 38  ω     67.00 131.00   0.50   10.00    --  115.00  73.00 -18.06  128
 39  ω     68.00 100.00   0.50   10.00    --  115.00  65.00-180.00   64
 40  ω    147.00 204.00   0.50   10.00    --  115.00  50.00 155.68  114
 41  ω     68.00 156.00   0.50   10.00    --  115.00  65.00-120.00  176
 42  ω     53.00 101.00   0.50   10.00    --  115.00  50.00 155.68   96
 43  ω     68.00 133.00   0.50   10.00    --  115.00  65.00  30.00  130
 44  ω     73.00 203.00   0.50   10.00    --  115.00  47.00 131.92  260
 45  ω    161.00 189.00   0.50   10.00    --  115.00  65.00-150.00   56
 46  ω     68.00 153.00   0.50   10.00    --  115.00  65.00-150.00  170
 47  ω     34.00  60.00   0.50   10.00    --  115.00  47.00 131.92   52
 48  ω     34.00 167.00   0.50   10.00    --  115.00  47.00  86.01  266
 49  ω    127.00 203.00   0.50   10.00    --  115.00  54.00  60.00  152
 50  ω     70.00  99.00   0.50   10.00    --  115.00  54.00  60.00   58
 51  ω    100.00 170.00   0.50   10.00    --  115.00  47.00 151.18  140
 52  ω    158.00 200.00   0.50   10.00    --  115.00  65.00-180.00   84
 53  ω     33.00  62.00   0.50   10.00    --  115.00  47.00 151.18   58
 54  ω     79.00 144.00   0.50   10.00    --  115.00 -82.00   0.00  130
 55  ω    133.00 166.00   0.50   10.00    --  115.00 -82.00 -60.00   66
 56  ω     63.00  90.00   0.50   10.00    --  115.00  54.00  30.00   54
 57  ω    103.00 165.00   0.50   10.00    --  115.00  54.00  30.00  124
 58  ω     69.00 102.00   0.50   10.00    --  115.00  65.00  90.00   66
 59  ω    145.00 203.00   0.50   10.00    --  115.00  65.00  90.00  116
 60  ω     89.00 176.00   0.50   10.00    --  115.00  47.00-154.66  174
 61  ω     38.00  77.00   0.50   10.00    --  115.00 -82.00 -60.00   78
 62  ω     27.00  52.00   0.50   10.00    --  115.00  43.00 -60.00   50
 63  ω    178.00 203.00   0.50   10.00    --  115.00  54.00-150.00   50
 64  ω     63.00 112.00   0.50   10.00    --  115.00  54.00-150.00   98
 65  ω     34.00  70.00   0.50   10.00    --  115.00  47.00-154.66   72
 66  ω     65.00 142.00   0.50   10.00    --  115.00 -82.00  60.00  154
 67  ω     62.00 141.00   0.50   10.00    --  115.00 -82.00-150.00  158
 68  ω     30.00 152.00   0.50   10.00    --  115.00 -82.00 -90.00  244
 69  ω     75.00 201.00   0.50   10.00    --  115.00  47.00 -38.92  252
 70  ω    175.00 204.00   0.50   10.00    --  115.00  65.00 -60.00   58
 71  ω    118.00 144.00   0.50   10.00    --  115.00  65.00 -60.00   52
 72  ω    116.00 192.00   0.50   10.00    --  115.00  74.00 -96.72  152
 73  ω     68.00  94.00   0.50   10.00    --  115.00  65.00 -60.00   52
 74  ω     86.00 126.00   0.50   10.00    --  115.00 -82.00 -60.00   80
 75  ω    150.00 198.00   0.50   10.00    --  115.00  43.00 -60.00   96
 76  ω     40.00  67.00   0.50   10.00    --  115.00 -82.00   0.00   54
 77  ω     67.00  93.00   0.50   10.00    --  115.00  74.00 -96.72   52
 78  ω     33.00  59.00   0.50   10.00    --  115.00  47.00 -38.92   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0333226000
_diffrn_orient_matrix_UB_12      -0.1097039000
_diffrn_orient_matrix_UB_13      0.0091696000
_diffrn_orient_matrix_UB_21      0.0169285000
_diffrn_orient_matrix_UB_22      0.0326784000
_diffrn_orient_matrix_UB_23      0.1028865000
_diffrn_orient_matrix_UB_31      -0.1178097000
_diffrn_orient_matrix_UB_32      -0.0093432000
_diffrn_orient_matrix_UB_33      -0.0116945000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11514
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.476
_diffrn_reflns_theta_min         2.982
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       plank
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.026
_refine_diff_density_max         2.689
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.633
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11514
_refine_ls_number_restraints     534
_refine_ls_restrained_S_all      1.598
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.1245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3507
_refine_ls_wR_factor_ref         0.3658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9518
_reflns_number_total             11514
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 1.2052° 
 around [-0.94 0.30 0.16] (reciprocal) or [-1.00 -0.05 -0.01] (direct)
;
_cod_data_source_file            d2sc05348a4.cif
_cod_data_source_block           1a-THF
_cod_depositor_comments
'Adding full bibliography for 1568074--1568079.cif.'
_cod_database_code               1568075
_nottingham_internal_coll_name   OATSWJ
_nottingham_internal_coll_number 19141
_nottingham_internal_coll_client AT/SW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '1.00, 10.00, 4.00'
_nottingham_internal_coll_frame_width 0.50
_nottingham_internal_coll_user   pczspa
_nottingham_internal_coll_date   13/05/2022
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'XtalLAB PRO, A00000876'
_nottingham_internal_process_date 24/05/2022
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 25/05/2022
_nottingham_internal_solution_user pczspa
_nottingham_internal_refinement_date 25/05/2022
_nottingham_internal_refinement_user pczspa
_nottingham_internal_validation_date 25/05/2022
_nottingham_internal_validation_user pczspa
_nottingham_internal_archive_date 25/05/2022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52H30F16S8N
_chemical_oxdiff_usercomment
'OATSWJ #19141 MM-810 AT/SW fomblin oil on micromount'
_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.
;
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.395
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.592(10)
 0.408(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B), C42B(H42B), C43B(H43B),
 C45B(H45B), C46B(H46B), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A),
 C42A(H42A), C43A(H43A), C45A(H45A), C46A(H46A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.714
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1B S 0.85494(10) 0.80557(8) 1.03327(7) 0.0394(3) Uani 1 1 d . . . . .
S2B S 0.95732(9) 1.06796(8) 0.73586(7) 0.0343(3) Uani 1 1 d . . . . .
S3B S 0.87186(9) 0.74703(9) 0.38079(7) 0.0403(3) Uani 1 1 d . . . . .
S4B S 0.39076(9) 0.64105(7) 0.17695(8) 0.0363(3) Uani 1 1 d . . . . .
C11B C 0.8812(3) 0.8744(3) 0.9476(3) 0.0305(8) Uani 1 1 d . . . . .
C12B C 0.9722(4) 0.8885(3) 0.9129(3) 0.0351(9) Uani 1 1 d . . . . .
C13B C 0.9950(3) 0.9466(3) 0.8489(3) 0.0343(9) Uani 1 1 d . . . . .
C14B C 0.9277(3) 0.9918(3) 0.8152(3) 0.0281(8) Uani 1 1 d . . . . .
C15B C 0.8368(4) 0.9793(3) 0.8509(3) 0.0367(9) Uani 1 1 d . . . . .
C16B C 0.8132(4) 0.9206(3) 0.9145(3) 0.0358(9) Uani 1 1 d . . . . .
F17B F 1.0430(3) 0.8475(3) 0.9413(2) 0.0607(8) Uani 1 1 d . . . . .
F18B F 1.0840(2) 0.9553(3) 0.8172(2) 0.0587(8) Uani 1 1 d . . . . .
F19B F 0.7693(2) 1.0230(3) 0.8253(2) 0.0574(8) Uani 1 1 d . . . . .
F20B F 0.7257(3) 0.9123(3) 0.9475(2) 0.0632(9) Uani 1 1 d . . . . .
C21B C 0.9307(3) 0.9754(3) 0.6374(3) 0.0309(8) Uani 1 1 d . . . . .
C22B C 1.0126(3) 0.9492(3) 0.6107(3) 0.0339(9) Uani 1 1 d . . . . .
H22B H 1.083538 0.979705 0.646513 0.041 Uiso 1 1 calc R U . . .
C23B C 0.9913(3) 0.8789(3) 0.5321(3) 0.0341(9) Uani 1 1 d . . . . .
H23B H 1.047017 0.860534 0.514715 0.041 Uiso 1 1 calc R U . . .
C24B C 0.8869(3) 0.8354(3) 0.4790(3) 0.0293(8) Uani 1 1 d . . . . .
C25B C 0.8057(4) 0.8611(4) 0.5045(3) 0.0371(9) Uani 1 1 d . . . . .
H25B H 0.734653 0.830633 0.468971 0.045 Uiso 1 1 calc R U . . .
C26B C 0.8289(3) 0.9325(3) 0.5832(3) 0.0347(9) Uani 1 1 d . . . . .
H26B H 0.773358 0.951870 0.599775 0.042 Uiso 1 1 calc R U . . .
C31B C 0.7370(3) 0.7158(3) 0.3251(3) 0.0309(8) Uani 1 1 d . . . . .
C32B C 0.7122(3) 0.7580(3) 0.2523(3) 0.0322(8) Uani 1 1 d . . . . .
C33B C 0.6085(4) 0.7302(3) 0.2047(3) 0.0317(8) Uani 1 1 d . . . . .
C34B C 0.5235(3) 0.6602(3) 0.2283(3) 0.0313(8) Uani 1 1 d . . . . .
C35B C 0.5466(4) 0.6170(3) 0.2993(3) 0.0382(10) Uani 1 1 d . . . . .
C36B C 0.6528(4) 0.6435(4) 0.3466(3) 0.0403(10) Uani 1 1 d . . . . .
F37B F 0.7904(2) 0.8287(2) 0.2298(2) 0.0567(8) Uani 1 1 d . . . . .
F38B F 0.5913(2) 0.7712(2) 0.13559(18) 0.0468(7) Uani 1 1 d . . . . .
F39B F 0.4693(3) 0.5511(2) 0.3271(2) 0.0638(9) Uani 1 1 d . . . . .
F40B F 0.6715(3) 0.6003(3) 0.4158(2) 0.0681(10) Uani 1 1 d . . . . .
C41B C 0.3311(3) 0.5124(3) 0.1263(3) 0.0294(8) Uani 1 1 d . . . . .
C42B C 0.3863(3) 0.4571(3) 0.0905(3) 0.0353(9) Uani 1 1 d . . . . .
H42B H 0.461915 0.486024 0.097512 0.042 Uiso 1 1 calc R U . . .
C43B C 0.3292(4) 0.3589(3) 0.0443(3) 0.0333(9) Uani 1 1 d . . . . .
H43B H 0.365903 0.320246 0.019957 0.040 Uiso 1 1 calc R U . . .
C44B C 0.2176(3) 0.3172(3) 0.0338(3) 0.0307(8) Uani 1 1 d . . . . .
C45B C 0.1639(3) 0.3730(3) 0.0697(3) 0.0394(10) Uani 1 1 d . . . . .
H45B H 0.088084 0.344677 0.061559 0.047 Uiso 1 1 calc R U . . .
C46B C 0.2201(4) 0.4700(3) 0.1175(3) 0.0369(9) Uani 1 1 d . . . . .
H46B H 0.183475 0.507434 0.144068 0.044 Uiso 1 1 calc R U . . .
S1A S 0.47335(9) 1.07393(7) 0.74121(7) 0.0323(3) Uani 1 1 d . . . . .
S2A S 0.36894(9) 0.74834(9) 0.38237(7) 0.0416(3) Uani 1 1 d . . . . .
S3A S -0.10518(9) 0.64406(8) 0.17262(8) 0.0417(3) Uani 1 1 d . . . . .
S4A S -0.34843(9) 0.19172(7) -0.03213(6) 0.0326(3) Uani 1 1 d . . . . .
C11A C 0.4409(3) 0.9842(3) 0.6396(3) 0.0276(8) Uani 1 1 d . . . . .
C12A C 0.5160(3) 0.9512(3) 0.6115(3) 0.0300(8) Uani 1 1 d . . . . .
C13A C 0.4892(3) 0.8807(3) 0.5323(3) 0.0285(8) Uani 1 1 d . . . . .
C14A C 0.3857(3) 0.8388(3) 0.4784(3) 0.0299(8) Uani 1 1 d . . . . .
C15A C 0.3116(3) 0.8741(4) 0.5063(3) 0.0379(10) Uani 1 1 d . . . . .
C16A C 0.3385(4) 0.9457(3) 0.5854(3) 0.0358(9) Uani 1 1 d . . . . .
F17A F 0.6178(2) 0.9874(2) 0.6579(2) 0.0555(8) Uani 1 1 d . . . . .
F18A F 0.5663(2) 0.8510(2) 0.50681(19) 0.0486(7) Uani 1 1 d . . . . .
F19A F 0.2118(3) 0.8436(3) 0.4588(2) 0.0779(12) Uani 1 1 d . . . . .
F20A F 0.2634(2) 0.9758(3) 0.6095(2) 0.0621(9) Uani 1 1 d . . . . .
C21A C 0.2345(3) 0.7158(3) 0.3233(3) 0.0332(9) Uani 1 1 d . . . . .
C22A C 0.2156(4) 0.7608(3) 0.2513(3) 0.0358(9) Uani 1 1 d . . . . .
H22A H 0.273242 0.809045 0.235075 0.043 Uiso 1 1 calc R U . . .
C23A C 0.1104(4) 0.7334(3) 0.2038(3) 0.0351(9) Uani 1 1 d . . . . .
H23A H 0.095970 0.763918 0.155040 0.042 Uiso 1 1 calc R U . . .
C24A C 0.0270(3) 0.6622(3) 0.2267(3) 0.0324(9) Uani 1 1 d . . . . .
C25A C 0.0461(4) 0.6162(4) 0.2975(4) 0.0448(11) Uani 1 1 d . . . . .
H25A H -0.011721 0.568876 0.314315 0.054 Uiso 1 1 calc R U . . .
C26A C 0.1511(4) 0.6405(4) 0.3433(3) 0.0444(11) Uani 1 1 d . . . . .
H26A H 0.165879 0.605632 0.388335 0.053 Uiso 1 1 calc R U . . .
C31A C -0.1644(3) 0.5166(3) 0.1227(3) 0.0325(9) Uani 1 1 d . . . . .
C32A C -0.1113(3) 0.4590(3) 0.0871(3) 0.0339(9) Uani 1 1 d . . . . .
C33A C -0.1673(3) 0.3593(3) 0.0438(3) 0.0278(8) Uani 1 1 d . . . . .
C34A C -0.2783(3) 0.3151(3) 0.0310(3) 0.0278(8) Uani 1 1 d . . . . .
C35A C -0.3308(3) 0.3734(3) 0.0642(3) 0.0333(9) Uani 1 1 d . . . . .
C36A C -0.2756(4) 0.4707(3) 0.1100(3) 0.0319(8) Uani 1 1 d . . . . .
F37A F -0.0054(2) 0.4972(2) 0.0912(2) 0.0540(8) Uani 1 1 d . . . . .
F38A F -0.1114(2) 0.3087(2) 0.0114(2) 0.0530(7) Uani 1 1 d . . . . .
F39A F -0.4365(2) 0.3367(2) 0.0553(2) 0.0614(9) Uani 1 1 d . . . . .
F40A F -0.3298(2) 0.5252(2) 0.1414(2) 0.0569(8) Uani 1 1 d . . . . .
C41A C -0.3784(3) 0.1253(3) 0.0557(3) 0.0286(8) Uani 1 1 d . . . . .
C42A C -0.4748(3) 0.1103(3) 0.0832(3) 0.0329(9) Uani 1 1 d . . . . .
H42A H -0.521646 0.140270 0.058670 0.040 Uiso 1 1 calc R U . . .
C43A C -0.5029(3) 0.0510(3) 0.1472(3) 0.0321(8) Uani 1 1 d . . . . .
H43A H -0.568402 0.041254 0.166046 0.038 Uiso 1 1 calc R U . . .
C44A C -0.4342(3) 0.0068(3) 0.1827(3) 0.0281(8) Uani 1 1 d . . . . .
C45A C -0.3383(4) 0.0214(3) 0.1548(3) 0.0372(9) Uani 1 1 d . . . . .
H45A H -0.292257 -0.009798 0.178277 0.045 Uiso 1 1 calc R U . . .
C46A C -0.3096(3) 0.0812(3) 0.0929(3) 0.0335(9) Uani 1 1 d . . . . .
H46A H -0.242982 0.092332 0.075700 0.040 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0289
0 1 0 0.0289
0 0 1 0.0039
0 0 -1 0.0219
5 -2 -1 0.1462
-5 2 1 0.1462
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11B S1B C44B 100.35(18) . 2_666 ?
C14B S2B C21B 100.02(19) . . ?
C31B S3B C24B 102.81(19) . . ?
C34B S4B C41B 104.9(2) . . ?
C12B C11B S1B 121.8(3) . . ?
C12B C11B C16B 116.9(4) . . ?
C16B C11B S1B 121.2(3) . . ?
C11B C12B C13B 121.5(4) . . ?
F17B C12B C11B 121.1(4) . . ?
F17B C12B C13B 117.4(4) . . ?
C14B C13B C12B 122.0(4) . . ?
F18B C13B C12B 118.0(4) . . ?
F18B C13B C14B 120.0(4) . . ?
C13B C14B S2B 122.4(3) . . ?
C13B C14B C15B 116.9(4) . . ?
C15B C14B S2B 120.6(3) . . ?
C16B C15B C14B 121.3(4) . . ?
F19B C15B C14B 121.4(4) . . ?
F19B C15B C16B 117.3(4) . . ?
C15B C16B C11B 121.3(4) . . ?
F20B C16B C11B 119.7(4) . . ?
F20B C16B C15B 118.8(4) . . ?
C22B C21B S2B 121.2(3) . . ?
C26B C21B S2B 119.8(3) . . ?
C26B C21B C22B 118.9(4) . . ?
C21B C22B H22B 119.7 . . ?
C23B C22B C21B 120.6(4) . . ?
C23B C22B H22B 119.7 . . ?
C22B C23B H23B 120.3 . . ?
C22B C23B C24B 119.4(4) . . ?
C24B C23B H23B 120.3 . . ?
C23B C24B S3B 114.3(3) . . ?
C25B C24B S3B 125.3(3) . . ?
C25B C24B C23B 120.4(4) . . ?
C24B C25B H25B 120.3 . . ?
C24B C25B C26B 119.3(4) . . ?
C26B C25B H25B 120.3 . . ?
C21B C26B C25B 121.3(4) . . ?
C21B C26B H26B 119.3 . . ?
C25B C26B H26B 119.3 . . ?
C32B C31B S3B 120.8(3) . . ?
C36B C31B S3B 121.8(3) . . ?
C36B C31B C32B 117.2(4) . . ?
C33B C32B C31B 121.6(4) . . ?
F37B C32B C31B 119.4(4) . . ?
F37B C32B C33B 119.0(4) . . ?
C32B C33B C34B 121.2(4) . . ?
F38B C33B C32B 118.4(4) . . ?
F38B C33B C34B 120.4(4) . . ?
C33B C34B S4B 119.5(3) . . ?
C35B C34B S4B 122.1(4) . . ?
C35B C34B C33B 118.0(4) . . ?
C34B C35B C36B 120.9(4) . . ?
F39B C35B C34B 121.4(4) . . ?
F39B C35B C36B 117.6(4) . . ?
C31B C36B C35B 121.0(4) . . ?
F40B C36B C31B 120.0(4) . . ?
F40B C36B C35B 118.9(4) . . ?
C42B C41B S4B 124.2(3) . . ?
C42B C41B C46B 120.8(4) . . ?
C46B C41B S4B 114.8(3) . . ?
C41B C42B H42B 120.4 . . ?
C41B C42B C43B 119.2(4) . . ?
C43B C42B H42B 120.4 . . ?
C42B C43B H43B 120.0 . . ?
C42B C43B C44B 120.0(4) . . ?
C44B C43B H43B 120.0 . . ?
C43B C44B S1B 119.0(3) . 2_666 ?
C45B C44B S1B 120.7(3) . 2_666 ?
C45B C44B C43B 120.2(4) . . ?
C44B C45B H45B 119.8 . . ?
C44B C45B C46B 120.4(4) . . ?
C46B C45B H45B 119.8 . . ?
C41B C46B H46B 120.3 . . ?
C45B C46B C41B 119.4(4) . . ?
C45B C46B H46B 120.3 . . ?
C11A S1A C44A 100.01(18) . 2_566 ?
C14A S2A C21A 104.7(2) . . ?
C31A S3A C24A 104.7(2) . . ?
C34A S4A C41A 101.02(17) . . ?
C12A C11A S1A 121.6(3) . . ?
C12A C11A C16A 117.4(4) . . ?
C16A C11A S1A 121.0(3) . . ?
C11A C12A C13A 120.9(4) . . ?
F17A C12A C11A 121.4(4) . . ?
F17A C12A C13A 117.7(4) . . ?
C12A C13A C14A 122.4(4) . . ?
F18A C13A C12A 118.8(4) . . ?
F18A C13A C14A 118.9(4) . . ?
C13A C14A S2A 114.7(3) . . ?
C15A C14A S2A 129.1(3) . . ?
C15A C14A C13A 116.2(4) . . ?
C14A C15A C16A 121.5(4) . . ?
F19A C15A C14A 122.0(4) . . ?
F19A C15A C16A 116.4(4) . . ?
C11A C16A C15A 121.5(4) . . ?
F20A C16A C11A 119.7(4) . . ?
F20A C16A C15A 118.8(4) . . ?
C22A C21A S2A 118.7(3) . . ?
C26A C21A S2A 120.5(4) . . ?
C26A C21A C22A 120.6(4) . . ?
C21A C22A H22A 120.7 . . ?
C23A C22A C21A 118.6(4) . . ?
C23A C22A H22A 120.7 . . ?
C22A C23A H23A 119.7 . . ?
C24A C23A C22A 120.6(4) . . ?
C24A C23A H23A 119.7 . . ?
C23A C24A S3A 117.4(3) . . ?
C23A C24A C25A 120.8(4) . . ?
C25A C24A S3A 121.4(4) . . ?
C24A C25A H25A 120.5 . . ?
C26A C25A C24A 119.0(5) . . ?
C26A C25A H25A 120.5 . . ?
C21A C26A H26A 119.9 . . ?
C25A C26A C21A 120.2(4) . . ?
C25A C26A H26A 119.9 . . ?
C32A C31A S3A 125.5(3) . . ?
C32A C31A C36A 116.8(4) . . ?
C36A C31A S3A 117.5(3) . . ?
C31A C32A C33A 121.0(4) . . ?
F37A C32A C31A 121.7(4) . . ?
F37A C32A C33A 117.3(4) . . ?
C34A C33A C32A 121.5(4) . . ?
F38A C33A C32A 117.7(4) . . ?
F38A C33A C34A 120.8(4) . . ?
C33A C34A S4A 120.5(3) . . ?
C35A C34A S4A 122.1(3) . . ?
C35A C34A C33A 117.2(4) . . ?
C36A C35A C34A 121.6(4) . . ?
F39A C35A C34A 121.0(4) . . ?
F39A C35A C36A 117.4(4) . . ?
C35A C36A C31A 121.9(4) . . ?
F40A C36A C31A 118.3(4) . . ?
F40A C36A C35A 119.8(4) . . ?
C42A C41A S4A 120.1(3) . . ?
C42A C41A C46A 119.3(4) . . ?
C46A C41A S4A 120.5(3) . . ?
C41A C42A H42A 119.8 . . ?
C41A C42A C43A 120.3(4) . . ?
C43A C42A H42A 119.8 . . ?
C42A C43A H43A 120.2 . . ?
C44A C43A C42A 119.6(4) . . ?
C44A C43A H43A 120.2 . . ?
C43A C44A S1A 119.6(3) . 2_566 ?
C45A C44A S1A 120.4(3) . 2_566 ?
C45A C44A C43A 119.9(4) . . ?
C44A C45A H45A 119.7 . . ?
C46A C45A C44A 120.5(4) . . ?
C46A C45A H45A 119.7 . . ?
C41A C46A H46A 119.9 . . ?
C45A C46A C41A 120.3(4) . . ?
C45A C46A H46A 119.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1B C11B 1.768(4) . ?
S1B C44B 1.790(4) 2_666 ?
S2B C14B 1.760(4) . ?
S2B C21B 1.780(4) . ?
S3B C24B 1.778(4) . ?
S3B C31B 1.770(4) . ?
S4B C34B 1.763(4) . ?
S4B C41B 1.773(4) . ?
C11B C12B 1.384(6) . ?
C11B C16B 1.395(7) . ?
C12B C13B 1.387(7) . ?
C12B F17B 1.348(5) . ?
C13B C14B 1.379(6) . ?
C13B F18B 1.347(5) . ?
C14B C15B 1.395(6) . ?
C15B C16B 1.390(7) . ?
C15B F19B 1.328(5) . ?
C16B F20B 1.338(5) . ?
C21B C22B 1.395(6) . ?
C21B C26B 1.379(6) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.391(6) . ?
C23B H23B 0.9500 . ?
C23B C24B 1.400(6) . ?
C24B C25B 1.376(6) . ?
C25B H25B 0.9500 . ?
C25B C26B 1.396(6) . ?
C26B H26B 0.9500 . ?
C31B C32B 1.397(6) . ?
C31B C36B 1.385(6) . ?
C32B C33B 1.375(6) . ?
C32B F37B 1.332(5) . ?
C33B C34B 1.389(6) . ?
C33B F38B 1.316(5) . ?
C34B C35B 1.379(6) . ?
C35B C36B 1.405(7) . ?
C35B F39B 1.330(5) . ?
C36B F40B 1.340(6) . ?
C41B C42B 1.392(6) . ?
C41B C46B 1.397(6) . ?
C42B H42B 0.9500 . ?
C42B C43B 1.394(6) . ?
C43B H43B 0.9500 . ?
C43B C44B 1.401(6) . ?
C44B C45B 1.382(6) . ?
C45B H45B 0.9500 . ?
C45B C46B 1.387(6) . ?
C46B H46B 0.9500 . ?
S1A C11A 1.778(4) . ?
S1A C44A 1.782(4) 2_566 ?
S2A C14A 1.766(4) . ?
S2A C21A 1.776(4) . ?
S3A C24A 1.772(4) . ?
S3A C31A 1.756(4) . ?
S4A C34A 1.772(4) . ?
S4A C41A 1.783(4) . ?
C11A C12A 1.373(6) . ?
C11A C16A 1.385(6) . ?
C12A C13A 1.388(6) . ?
C12A F17A 1.338(5) . ?
C13A C14A 1.394(6) . ?
C13A F18A 1.355(5) . ?
C14A C15A 1.378(6) . ?
C15A C16A 1.395(6) . ?
C15A F19A 1.326(5) . ?
C16A F20A 1.326(5) . ?
C21A C22A 1.393(7) . ?
C21A C26A 1.391(7) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.393(6) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.380(6) . ?
C24A C25A 1.389(7) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.388(7) . ?
C26A H26A 0.9500 . ?
C31A C32A 1.393(6) . ?
C31A C36A 1.396(6) . ?
C32A C33A 1.398(6) . ?
C32A F37A 1.341(5) . ?
C33A C34A 1.392(6) . ?
C33A F38A 1.332(5) . ?
C34A C35A 1.382(6) . ?
C35A C36A 1.379(6) . ?
C35A F39A 1.327(5) . ?
C36A F40A 1.348(5) . ?
C41A C42A 1.395(6) . ?
C41A C46A 1.403(6) . ?
C42A H42A 0.9500 . ?
C42A C43A 1.407(6) . ?
C43A H43A 0.9500 . ?
C43A C44A 1.394(6) . ?
C44A C45A 1.392(6) . ?
C45A H45A 0.9500 . ?
C45A C46A 1.387(6) . ?
C46A H46A 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C22B H22B F18B 0.95 2.69 3.143(6) 110.0 . yes
C22B H22B F37B 0.95 2.93 3.669(5) 135.6 2_776 yes
C22B H22B F20A 0.95 2.61 3.302(5) 129.6 1_655 yes
C23B H23B F19A 0.95 2.60 3.536(5) 169.0 1_655 yes
C23B H23B F20A 0.95 2.86 3.417(5) 118.4 1_655 yes
C25B H25B F40B 0.95 3.12 3.563(6) 110.2 . yes
C25B H25B F18A 0.95 2.55 3.216(5) 127.2 . yes
C25B H25B F20A 0.95 3.21 3.433(6) 95.2 2_676 yes
C26B H26B F17A 0.95 2.60 3.545(5) 172.5 . yes
C26B H26B F18A 0.95 2.73 3.306(5) 119.9 . yes
C26B H26B F19A 0.95 3.19 3.624(7) 110.1 2_676 yes
C42B H42B F39A 0.95 3.01 3.502(6) 113.9 1_655 yes
C42B H42B F40A 0.95 2.65 3.567(5) 163.8 1_655 yes
C43B H43B F38B 0.95 2.81 3.646(5) 147.2 2_665 yes
C43B H43B F39A 0.95 2.58 3.296(6) 132.6 1_655 yes
C45B H45B F17B 0.95 2.75 3.432(5) 129.6 2_666 yes
C45B H45B F37A 0.95 2.94 3.414(6) 112.3 . yes
C45B H45B F38A 0.95 2.55 3.466(5) 162.7 . yes
C46B H46B F37A 0.95 2.52 3.199(6) 128.8 . yes
C22A H22A F19B 0.95 2.94 3.471(6) 116.6 2_676 yes
C22A H22A F17A 0.95 2.93 3.530(5) 122.3 2_676 yes
C23A H23A S2B 0.95 3.13 3.390(5) 97.4 2_676 yes
C23A H23A F19B 0.95 2.96 3.492(6) 116.5 2_676 yes
C23A H23A F38A 0.95 2.69 3.275(5) 120.1 2_565 yes
C42A H42A F20B 0.95 2.60 3.266(5) 127.9 2_566 yes
C42A H42A F39A 0.95 2.71 3.265(6) 117.9 . yes
C43A H43A F19B 0.95 2.60 3.520(5) 163.6 2_566 yes
C43A H43A F20B 0.95 2.87 3.397(6) 116.2 2_566 yes
C43A H43A F17A 0.95 2.93 3.607(5) 129.1 2_566 yes
C45A H45A F18B 0.95 2.65 3.311(6) 126.8 2_666 yes
C45A H45A F38B 0.95 2.96 3.400(5) 109.5 1_445 yes
C45A H45A F20A 0.95 3.16 3.590(6) 109.2 2_566 yes
C46A H46A F17B 0.95 2.62 3.558(5) 168.0 2_666 yes
C46A H46A F18B 0.95 2.85 3.408(6) 118.8 2_666 yes
C46A H46A F20B 0.95 2.92 3.305(6) 105.9 1_444 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1B C11B C12B C13B -176.8(3) . . . . ?
S1B C11B C12B F17B 2.1(6) . . . . ?
S1B C11B C16B C15B 176.3(3) . . . . ?
S1B C11B C16B F20B -0.5(6) . . . . ?
S1B C44B C45B C46B -176.5(4) 2_666 . . . ?
S2B C14B C15B C16B -179.1(3) . . . . ?
S2B C14B C15B F19B 1.1(6) . . . . ?
S2B C21B C22B C23B -178.1(3) . . . . ?
S2B C21B C26B C25B 178.7(4) . . . . ?
S3B C24B C25B C26B -179.5(3) . . . . ?
S3B C31B C32B C33B 176.1(3) . . . . ?
S3B C31B C32B F37B -5.7(6) . . . . ?
S3B C31B C36B C35B -177.6(4) . . . . ?
S3B C31B C36B F40B 5.1(7) . . . . ?
S4B C34B C35B C36B -171.7(4) . . . . ?
S4B C34B C35B F39B 6.5(7) . . . . ?
S4B C41B C42B C43B -173.6(3) . . . . ?
S4B C41B C46B C45B 172.7(4) . . . . ?
C11B C12B C13B C14B -1.2(7) . . . . ?
C11B C12B C13B F18B -178.8(4) . . . . ?
C12B C11B C16B C15B -1.0(6) . . . . ?
C12B C11B C16B F20B -177.9(4) . . . . ?
C12B C13B C14B S2B 178.5(3) . . . . ?
C12B C13B C14B C15B 2.2(6) . . . . ?
C13B C14B C15B C16B -2.7(6) . . . . ?
C13B C14B C15B F19B 177.4(4) . . . . ?
C14B S2B C21B C22B -94.5(4) . . . . ?
C14B S2B C21B C26B 89.3(4) . . . . ?
C14B C15B C16B C11B 2.2(7) . . . . ?
C14B C15B C16B F20B 179.1(4) . . . . ?
C16B C11B C12B C13B 0.6(6) . . . . ?
C16B C11B C12B F17B 179.5(4) . . . . ?
F17B C12B C13B C14B 179.8(4) . . . . ?
F17B C12B C13B F18B 2.2(6) . . . . ?
F18B C13B C14B S2B -3.9(6) . . . . ?
F18B C13B C14B C15B 179.8(4) . . . . ?
F19B C15B C16B C11B -177.9(4) . . . . ?
F19B C15B C16B F20B -1.0(6) . . . . ?
C21B S2B C14B C13B 74.1(4) . . . . ?
C21B S2B C14B C15B -109.7(4) . . . . ?
C21B C22B C23B C24B 1.0(7) . . . . ?
C22B C21B C26B C25B 2.4(7) . . . . ?
C22B C23B C24B S3B 180.0(3) . . . . ?
C22B C23B C24B C25B -0.6(7) . . . . ?
C23B C24B C25B C26B 1.1(7) . . . . ?
C24B S3B C31B C32B 100.5(4) . . . . ?
C24B S3B C31B C36B -84.6(4) . . . . ?
C24B C25B C26B C21B -2.1(7) . . . . ?
C26B C21B C22B C23B -1.8(7) . . . . ?
C31B S3B C24B C23B -174.9(3) . . . . ?
C31B S3B C24B C25B 5.7(5) . . . . ?
C31B C32B C33B C34B 1.3(7) . . . . ?
C31B C32B C33B F38B -178.3(4) . . . . ?
C32B C31B C36B C35B -2.5(7) . . . . ?
C32B C31B C36B F40B -179.9(4) . . . . ?
C32B C33B C34B S4B 170.3(3) . . . . ?
C32B C33B C34B C35B -1.9(6) . . . . ?
C33B C34B C35B C36B 0.3(7) . . . . ?
C33B C34B C35B F39B 178.4(4) . . . . ?
C34B S4B C41B C42B -32.7(4) . . . . ?
C34B S4B C41B C46B 152.5(3) . . . . ?
C34B C35B C36B C31B 2.0(8) . . . . ?
C34B C35B C36B F40B 179.3(5) . . . . ?
C36B C31B C32B C33B 0.9(7) . . . . ?
C36B C31B C32B F37B 179.1(4) . . . . ?
F37B C32B C33B C34B -176.9(4) . . . . ?
F37B C32B C33B F38B 3.5(6) . . . . ?
F38B C33B C34B S4B -10.2(6) . . . . ?
F38B C33B C34B C35B 177.7(4) . . . . ?
F39B C35B C36B C31B -176.3(5) . . . . ?
F39B C35B C36B F40B 1.1(7) . . . . ?
C41B S4B C34B C33B 122.8(3) . . . . ?
C41B S4B C34B C35B -65.3(4) . . . . ?
C41B C42B C43B C44B 0.5(7) . . . . ?
C42B C41B C46B C45B -2.3(7) . . . . ?
C42B C43B C44B S1B 175.2(3) . . . 2_666 ?
C42B C43B C44B C45B -0.5(7) . . . . ?
C43B C44B C45B C46B -1.0(7) . . . . ?
C44B S1B C11B C12B -88.9(4) 2_666 . . . ?
C44B S1B C11B C16B 93.9(4) 2_666 . . . ?
C44B C45B C46B C41B 2.4(7) . . . . ?
C46B C41B C42B C43B 0.9(7) . . . . ?
S1A C11A C12A C13A 179.7(3) . . . . ?
S1A C11A C12A F17A -2.1(6) . . . . ?
S1A C11A C16A C15A -179.0(4) . . . . ?
S1A C11A C16A F20A -0.1(6) . . . . ?
S1A C44A C45A C46A 177.6(3) 2_566 . . . ?
S2A C14A C15A C16A 179.2(4) . . . . ?
S2A C14A C15A F19A -2.0(8) . . . . ?
S2A C21A C22A C23A 178.5(3) . . . . ?
S2A C21A C26A C25A 179.3(4) . . . . ?
S3A C24A C25A C26A -173.8(4) . . . . ?
S3A C31A C32A C33A -176.1(3) . . . . ?
S3A C31A C32A F37A 2.5(7) . . . . ?
S3A C31A C36A C35A 174.1(4) . . . . ?
S3A C31A C36A F40A -3.8(6) . . . . ?
S4A C34A C35A C36A -177.2(3) . . . . ?
S4A C34A C35A F39A 4.7(6) . . . . ?
S4A C41A C42A C43A 174.7(3) . . . . ?
S4A C41A C46A C45A -173.6(3) . . . . ?
C11A C12A C13A C14A -1.2(6) . . . . ?
C11A C12A C13A F18A 179.4(4) . . . . ?
C12A C11A C16A C15A 1.5(7) . . . . ?
C12A C11A C16A F20A -179.6(4) . . . . ?
C12A C13A C14A S2A -178.4(3) . . . . ?
C12A C13A C14A C15A 2.6(6) . . . . ?
C13A C14A C15A C16A -1.9(7) . . . . ?
C13A C14A C15A F19A 176.9(5) . . . . ?
C14A S2A C21A C22A 97.9(4) . . . . ?
C14A S2A C21A C26A -87.9(4) . . . . ?
C14A C15A C16A C11A -0.1(8) . . . . ?
C14A C15A C16A F20A -179.0(5) . . . . ?
C16A C11A C12A C13A -0.8(6) . . . . ?
C16A C11A C12A F17A 177.4(4) . . . . ?
F17A C12A C13A C14A -179.5(4) . . . . ?
F17A C12A C13A F18A 1.2(6) . . . . ?
F18A C13A C14A S2A 1.0(5) . . . . ?
F18A C13A C14A C15A -178.1(4) . . . . ?
F19A C15A C16A C11A -178.9(5) . . . . ?
F19A C15A C16A F20A 2.1(7) . . . . ?
C21A S2A C14A C13A -175.7(3) . . . . ?
C21A S2A C14A C15A 3.2(5) . . . . ?
C21A C22A C23A C24A -0.9(7) . . . . ?
C22A C21A C26A C25A -6.5(8) . . . . ?
C22A C23A C24A S3A 171.9(3) . . . . ?
C22A C23A C24A C25A -0.2(7) . . . . ?
C23A C24A C25A C26A -2.0(8) . . . . ?
C24A S3A C31A C32A -33.6(4) . . . . ?
C24A S3A C31A C36A 152.5(4) . . . . ?
C24A C25A C26A C21A 5.3(8) . . . . ?
C26A C21A C22A C23A 4.2(7) . . . . ?
C31A S3A C24A C23A 124.1(4) . . . . ?
C31A S3A C24A C25A -63.8(5) . . . . ?
C31A C32A C33A C34A 2.9(7) . . . . ?
C31A C32A C33A F38A 180.0(4) . . . . ?
C32A C31A C36A C35A -0.3(7) . . . . ?
C32A C31A C36A F40A -178.2(4) . . . . ?
C32A C33A C34A S4A 174.8(3) . . . . ?
C32A C33A C34A C35A -1.1(6) . . . . ?
C33A C34A C35A C36A -1.4(6) . . . . ?
C33A C34A C35A F39A -179.5(4) . . . . ?
C34A S4A C41A C42A 91.5(3) . . . . ?
C34A S4A C41A C46A -93.4(3) . . . . ?
C34A C35A C36A C31A 2.1(7) . . . . ?
C34A C35A C36A F40A -180.0(4) . . . . ?
C36A C31A C32A C33A -2.2(7) . . . . ?
C36A C31A C32A F37A 176.4(4) . . . . ?
F37A C32A C33A C34A -175.7(4) . . . . ?
F37A C32A C33A F38A 1.4(6) . . . . ?
F38A C33A C34A S4A -2.2(5) . . . . ?
F38A C33A C34A C35A -178.0(4) . . . . ?
F39A C35A C36A C31A -179.7(4) . . . . ?
F39A C35A C36A F40A -1.8(7) . . . . ?
C41A S4A C34A C33A 104.9(3) . . . . ?
C41A S4A C34A C35A -79.4(4) . . . . ?
C41A C42A C43A C44A -0.4(6) . . . . ?
C42A C41A C46A C45A 1.5(6) . . . . ?
C42A C43A C44A S1A -176.5(3) . . . 2_566 ?
C42A C43A C44A C45A 0.0(6) . . . . ?
C43A C44A C45A C46A 1.1(6) . . . . ?
C44A S1A C11A C12A -94.1(4) 2_566 . . . ?
C44A S1A C11A C16A 86.5(4) 2_566 . . . ?
C44A C45A C46A C41A -1.9(7) . . . . ?
C46A C41A C42A C43A -0.4(6) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.592(10) 422 43765 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.408(10) 254 43765 nmt 0.9999 0.0034 -0.0012 0.0048 1.0001 0.0182 -0.0083
-0.0237 0.9969
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0009 -1.0006 -0.0045 0.1097 -0.0331 0.0093
-0.0009 1.0006 0.0045 -0.1097 0.0331 -0.0093
0.0000 -0.0035 1.0012 0.0096 0.1029 -0.0117
-0.0000 0.0035 -1.0012 -0.0096 -0.1029 0.0117
5.0040 -2.0055 -1.0005 0.0441 -0.0838 -0.5591
-5.0040 2.0055 1.0005 -0.0441 0.0838 0.5591
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.275 0.500 0.500 742.0 195.7 '4 C4H8O'
