#------------------------------------------------------------------------------
#$Date: 2026-03-05 14:13:11 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304961 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/65/1576560.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_1576560
loop_
_publ_author_name
'Pociecha, D.'
'Thornborrow, Z.'
'Karcz, J.'
'Bakiera, M.'
'Herman, J.'
'Makal, A.'
'Szydłowska, J'
'Górecka, E'
_publ_section_title
;
 Helical vs. non-helical nematic and lamellar proper ferroelectric
 liquid crystal phases.
;
_journal_issue                   9
_journal_name_full               'Soft matter'
_journal_page_first              1973
_journal_page_last               1978
_journal_paper_doi               10.1039/d5sm01265a
_journal_volume                  22
_journal_year                    2026
_chemical_formula_moiety         'C33 H20 F10 O3'
_chemical_formula_sum            'C33 H20 F10 O3'
_chemical_formula_weight         654.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.07.13 svn.rb7424ae for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-19 deposited with the CCDC.	2026-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.416(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0779(2)
_cell_length_b                   15.6905(3)
_cell_length_c                   17.9427(3)
_cell_measurement_reflns_used    7073
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      72.3280
_cell_measurement_theta_min      2.5410
_cell_volume                     2747.90(9)
_computing_cell_refinement       'CrysAlisPro 1.171.44.85 (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.144a 64-bit (release 23-01-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.85 (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00 -23.00   0.50    2.00    --    0.00 -77.00 129.00  122
  2  ω     -3.00  23.00   0.50    2.00    --    0.00  77.00-104.00   52
  3  ω    -40.00 -15.00   0.50    2.00    --    0.00  77.00-104.00   50
  4  ω    -13.00  20.00   0.50    8.00    --   56.40 -77.00 129.00   66
  5  ω     68.00  94.00   0.50    8.00    --   56.40  77.00-104.00   52
  6  ω     23.00  77.00   0.50    8.00    --   56.40 -77.00 129.00  108
  7  ω     72.00 176.00   0.50   10.00    --  112.80  77.00-104.00  208
  8  ω     57.00 124.00   0.50   10.00    --  112.80 -77.00 129.00  134
  9  ω      4.00  33.00   0.50    2.00    --    0.00 -99.00 -90.00   58
 10  ω    -84.00 -56.00   0.50    2.00    --    0.00-178.00-150.00   56
 11  ω    -75.00 -43.00   0.50    2.00    --    0.00-178.00  30.00   64
 12  ω    -73.00 -48.00   0.50    2.00    --    0.00-178.00-120.00   50
 13  ω   -137.00 -86.00   0.50    8.00    --  -54.00 -99.00 -30.00  102
 14  ω   -142.00 -91.00   0.50    8.00    --  -54.00 -99.00-150.00  102
 15  ω   -134.00 -20.00   0.50    8.00    --  -54.00 -57.00  30.00  228
 16  ω   -134.00 -21.00   0.50    8.00    --  -54.00 -57.00  60.00  226
 17  ω   -142.00-114.00   0.50    8.00    --  -54.00 -99.00  60.00   56
 18  ω   -140.00 -87.00   0.50    8.00    --  -54.00 -99.00  30.00  106
 19  ω    -35.00 -10.00   0.50    8.00    --  -54.00  77.00-104.00   50
 20  ω   -142.00 -86.00   0.50    8.00    --  -54.00 -99.00 150.00  112
 21  ω   -100.00 -75.00   0.50    8.00    --  -54.00 -77.00 129.00   50
 22  ω    -81.00 -15.00   0.50    8.00    --  -54.00 125.00-150.00  132
 23  ω   -137.00 -87.00   0.50    8.00    --  -54.00 -99.00 -90.00  100
 24  ω     45.00 105.00   0.50    8.00    --   56.40-125.00  60.00  120
 25  ω     34.00  98.00   0.50    8.00    --   56.40-125.00 150.00  128
 26  ω     54.00  79.00   0.50    8.00    --   56.40 -99.00-180.00   50
 27  ω     23.00  90.00   0.50   10.00    --  112.80 -94.00-150.00  134
 28  ω    118.00 144.00   0.50   10.00    --  112.80  61.00-120.00   52
 29  ω     29.00  89.00   0.50   10.00    --  112.80-111.00 -30.00  120
 30  ω     29.00  85.00   0.50   10.00    --  112.80-111.00 -90.00  112
 31  ω    105.00 141.00   0.50   10.00    --  112.80 -61.00  30.00   72
 32  ω    103.00 177.00   0.50   10.00    --  112.80 111.00 120.00  148
 33  ω     64.00  90.00   0.50   10.00    --  112.80 178.00 150.00   52
 34  ω     51.00 101.00   0.50   10.00    --  112.80 -61.00  30.00  100
 35  ω     69.00 157.00   0.50   10.00    --  112.80  45.00  30.00  176
 36  ω     79.00 105.00   0.50   10.00    --  112.80  61.00 -30.00   52
 37  ω    134.00 178.00   0.50   10.00    --  112.80  61.00 -30.00   88
 38  ω    116.00 170.00   0.50   10.00    --  112.80  61.00 -60.00  108
 39  ω    105.00 131.00   0.50   10.00    --  112.80 111.00 -60.00   52
 40  ω     81.00 106.00   0.50   10.00    --  112.80  61.00 -60.00   50
 41  ω     79.00 178.00   0.50   10.00    --  112.80  61.00-180.00  198
 42  ω     69.00 124.00   0.50   10.00    --  112.80  45.00-120.00  110
 43  ω     24.00 106.00   0.50   10.00    --  112.80 -94.00 120.00  164
 44  ω     30.00 103.00   0.50   10.00    --  112.80-111.00  60.00  146
 45  ω    134.00 168.00   0.50   10.00    --  112.80  45.00-120.00   68
 46  ω     71.00 151.00   0.50   10.00    --  112.80 -45.00-180.00  160
 47  ω     29.00  58.00   0.50   10.00    --  112.80 -45.00-180.00   58
 48  ω     72.00 166.00   0.50   10.00    --  112.80  77.00 -60.00  188
 49  ω     90.00 174.00   0.50   10.00    --  112.80  45.00   0.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.920
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.85 (Rigaku Oxford Diffraction, 2024)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.30(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         10908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0460
_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)+(0.0686P)²+0.0875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1180
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                8918
_reflns_number_total             10908
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sm01265a2.cif
_cod_data_source_block           proces1_abs
_cod_depositor_comments
'Adding full bibliography for 1576557--1576560.cif.'
_cod_database_code               1576560
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C33 H20 F10 O3'
_chemical_oxdiff_usercomment     '100  K'
_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.
;
_cell_oxdiff_angle_alpha         89.998(2)
_cell_oxdiff_angle_beta          104.3888(19)
_cell_oxdiff_angle_gamma         89.9985(19)
_cell_oxdiff_length_a            10.0765(2)
_cell_oxdiff_length_b            15.6932(4)
_cell_oxdiff_length_c            17.9399(4)
_cell_oxdiff_measurement_reflns_used 7073
_cell_oxdiff_volume              2747.88(11)
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.70(14)
 0.30(14)
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.a Ternary CH refined with riding coordinates:
 C62(H62), C31(H31), C29(H29), C64(H64)
3.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C61(H61A,H61B), C28(H28A,H28B), C30(H30A,H30B), C63(H63A,
 H63B), C65(H65A,H65B)
3.c Aromatic/amide H refined with riding coordinates:
 C59(H59), C47(H47), C45(H45), C17(H17), C38(H38), C41(H41), C55(H55),
 C50(H50), C51(H51), C22(H22), C12(H12), C26(H26), C1(H1), C8(H8), C34(H34),
 C14(H14), C5(H5), C18(H18)
3.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C66(H66A,H66B,H66C)
;
_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 1.250
_oxdiff_exptl_absorpt_empirical_full_min 0.832
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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
F20 F -0.7716(3) 0.30884(18) 0.84518(15) 0.0307(6) Uani 1 1 d . . . . .
F9 F 1.0075(2) 0.55392(19) -0.07173(15) 0.0310(6) Uani 1 1 d . . . . .
F17 F -0.1063(3) 0.42839(19) 0.44864(14) 0.0327(6) Uani 1 1 d . . . . .
F6 F 0.2870(2) 0.69553(18) 0.32622(16) 0.0314(6) Uani 1 1 d . . . . .
F8 F 0.9208(3) 0.6441(2) 0.37383(15) 0.0320(6) Uani 1 1 d . . . . .
F14 F 0.2461(3) 0.28636(18) 0.50936(17) 0.0342(6) Uani 1 1 d . . . . .
F16 F 0.2326(2) 0.30538(18) 0.64854(15) 0.0308(6) Uani 1 1 d . . . . .
F19 F -0.4771(2) 0.44989(19) 1.05216(14) 0.0305(6) Uani 1 1 d . . . . .
F2 F 0.0370(3) 0.5539(2) 0.72904(16) 0.0328(7) Uani 1 1 d . . . . .
F3 F 0.2924(3) 0.48970(19) 0.75400(15) 0.0330(6) Uani 1 1 d . . . . .
F12 F 0.4926(3) 0.44819(18) 0.25004(16) 0.0333(6) Uani 1 1 d . . . . .
F18 F -0.3981(2) 0.36484(19) 0.60480(15) 0.0323(6) Uani 1 1 d . . . . .
F7 F 0.6288(3) 0.5800(2) 0.52918(15) 0.0336(6) Uani 1 1 d . . . . .
F10 F 1.2978(3) 0.69995(19) 0.13329(15) 0.0334(6) Uani 1 1 d . . . . .
F15 F 0.0680(3) 0.31419(19) 0.41852(16) 0.0352(6) Uani 1 1 d . . . . .
F13 F 0.2386(3) 0.51535(18) 0.22584(15) 0.0340(6) Uani 1 1 d . . . . .
F11 F 0.6079(3) 0.3709(2) 0.38538(17) 0.0382(7) Uani 1 1 d . . . . .
F1 F -0.0832(3) 0.6271(2) 0.59309(17) 0.0375(7) Uani 1 1 d . . . . .
F5 F 0.4492(3) 0.6950(2) 0.55544(17) 0.0407(7) Uani 1 1 d . . . . .
O4 O 0.2050(3) 0.4217(2) 0.47166(18) 0.0252(7) Uani 1 1 d . . . . .
F4 F 0.2694(3) 0.71422(19) 0.46431(18) 0.0411(7) Uani 1 1 d . . . . .
O5 O -0.8944(3) 0.3528(2) 1.14097(17) 0.0266(7) Uani 1 1 d . . . . .
O1 O 0.3229(3) 0.5818(2) 0.50751(17) 0.0247(7) Uani 1 1 d . . . . .
O2 O 1.4221(3) 0.6530(2) -0.16124(18) 0.0261(7) Uani 1 1 d . . . . .
O3 O 1.5886(3) 0.6608(2) -0.04486(18) 0.0282(7) Uani 1 1 d . . . . .
O6 O -1.0590(3) 0.3471(2) 1.02377(17) 0.0289(7) Uani 1 1 d . . . . .
C49 C -0.1929(5) 0.3907(3) 0.7010(3) 0.0258(10) Uani 1 1 d . . . . .
C25 C 1.1302(5) 0.5904(3) -0.0398(3) 0.0247(10) Uani 1 1 d . . . . .
C11 C 0.4160(5) 0.6653(3) 0.3545(3) 0.0266(10) Uani 1 1 d . . . . .
C48 C -0.3347(4) 0.3792(3) 0.6794(2) 0.0220(9) Uani 1 1 d . . . . .
C39 C 0.2777(4) 0.4235(3) 0.4140(2) 0.0227(9) Uani 1 1 d . . . . .
C46 C -0.1051(4) 0.3836(3) 0.6465(3) 0.0215(9) Uani 1 1 d . . . . .
C3 C 0.1070(5) 0.5617(3) 0.6751(3) 0.0251(10) Uani 1 1 d . . . . .
C62 C -0.9408(4) 0.3881(3) 1.0670(3) 0.0237(10) Uani 1 1 d . . . . .
H62 H -0.962168 0.449734 1.072164 0.028 Uiso 1 1 calc R U . . .
C10 C 0.4569(5) 0.6443(3) 0.4327(3) 0.0245(9) Uani 1 1 d . . . . .
C21 C 1.0466(5) 0.6254(3) 0.0756(3) 0.0234(10) Uani 1 1 d . . . . .
C20 C 0.9696(5) 0.6226(3) 0.1164(3) 0.0233(10) Uani 1 1 d . . . . .
C27 C 1.3583(4) 0.6244(3) -0.0456(3) 0.0227(9) Uani 1 1 d . . . . .
C56 C -0.7485(4) 0.3435(3) 0.9164(3) 0.0246(9) Uani 1 1 d . . . . .
C31 C 1.6578(4) 0.6841(3) -0.1641(3) 0.0244(10) Uani 1 1 d . . . . .
H31 H 1.644350 0.747197 -0.162422 0.029 Uiso 1 1 calc R U . . .
C60 C -0.8280(4) 0.3812(3) 1.0257(2) 0.0224(9) Uani 1 1 d . . . . .
C57 C -0.6180(4) 0.3781(3) 0.9473(3) 0.0233(10) Uani 1 1 d . . . . .
C9 C 0.5863(5) 0.6077(3) 0.4556(3) 0.0273(11) Uani 1 1 d . . . . .
C19 C 0.8841(5) 0.6182(3) 0.1694(3) 0.0257(10) Uani 1 1 d . . . . .
C59 C -0.6992(5) 0.4158(3) 1.0601(3) 0.0223(10) Uani 1 1 d . . . . .
H59 H -0.681224 0.440182 1.110111 0.027 Uiso 1 1 calc R U . . .
C47 C -0.4154(5) 0.3778(3) 0.7301(3) 0.0267(11) Uani 1 1 d . . . . .
H47 H -0.511417 0.369198 0.712119 0.032 Uiso 1 1 calc R U . . .
C45 C 0.0257(4) 0.3475(3) 0.6711(3) 0.0249(10) Uani 1 1 d . . . . .
H45 H 0.058511 0.329612 0.723045 0.030 Uiso 1 1 calc R U . . .
C4 C 0.0481(5) 0.6007(3) 0.6051(3) 0.0273(11) Uani 1 1 d . . . . .
C17 C 0.6638(5) 0.6000(3) 0.1977(3) 0.0250(10) Uani 1 1 d . . . . .
H17 H 0.568714 0.588024 0.180121 0.030 Uiso 1 1 calc R U . . .
C52 C -0.3564(4) 0.3890(3) 0.8092(3) 0.0221(9) Uani 1 1 d . . . . .
C6 C 0.2513(5) 0.5805(3) 0.5639(3) 0.0214(10) Uani 1 1 d . . . . .
C38 C 0.4092(5) 0.3909(3) 0.4289(3) 0.0262(10) Uani 1 1 d . . . . .
H38 H 0.449457 0.363107 0.476136 0.031 Uiso 1 1 calc R U . . .
C40 C 0.1492(4) 0.3460(3) 0.4850(3) 0.0244(9) Uani 1 1 d . . . . .
C24 C 1.1475(4) 0.6273(3) 0.0325(3) 0.0235(9) Uani 1 1 d . . . . .
C41 C -0.1467(5) 0.4114(3) 0.5697(3) 0.0257(11) Uani 1 1 d . . . . .
H41 H -0.232937 0.438607 0.551405 0.031 Uiso 1 1 calc R U . . .
C55 C -0.8512(5) 0.3436(3) 0.9533(3) 0.0228(10) Uani 1 1 d . . . . .
H55 H -0.937377 0.318506 0.930062 0.027 Uiso 1 1 calc R U . . .
C50 C -0.1360(4) 0.4041(3) 0.7802(3) 0.0261(10) Uani 1 1 d . . . . .
H50 H -0.040269 0.414002 0.797615 0.031 Uiso 1 1 calc R U . . .
C51 C -0.2138(5) 0.4033(3) 0.8331(3) 0.0252(10) Uani 1 1 d . . . . .
H51 H -0.171474 0.412366 0.886047 0.030 Uiso 1 1 calc R U . . .
C2 C 0.2392(5) 0.5314(3) 0.6871(3) 0.0272(11) Uani 1 1 d . . . . .
C15 C 0.8596(5) 0.6293(3) 0.2978(3) 0.0264(11) Uani 1 1 d . . . . .
C22 C 1.3816(5) 0.6628(3) 0.0268(3) 0.0266(10) Uani 1 1 d . . . . .
H22 H 1.467675 0.687922 0.050151 0.032 Uiso 1 1 calc R U . . .
C44 C 0.1065(4) 0.3379(3) 0.6203(3) 0.0222(9) Uani 1 1 d . . . . .
C12 C 0.4974(4) 0.6566(3) 0.3051(3) 0.0245(9) Uani 1 1 d . . . . .
H12 H 0.465054 0.673937 0.252969 0.029 Uiso 1 1 calc R U . . .
C32 C 1.7696(5) 0.6664(3) -0.2062(3) 0.0282(10) Uani 1 1 d . . . . .
H32A H 1.777755 0.604027 -0.212271 0.034 Uiso 1 1 calc R U . . .
H32B H 1.858368 0.687434 -0.174428 0.034 Uiso 1 1 calc R U . . .
C26 C 1.2307(4) 0.5887(3) -0.0793(3) 0.0261(10) Uani 1 1 d . . . . .
H26 H 1.213547 0.563451 -0.128971 0.031 Uiso 1 1 calc R U . . .
C1 C 0.3131(4) 0.5399(3) 0.6328(3) 0.0241(9) Uani 1 1 d . . . . .
H1 H 0.404042 0.518686 0.642016 0.029 Uiso 1 1 calc R U . . .
C29 C 1.4709(4) 0.6180(3) -0.0876(2) 0.0236(9) Uani 1 1 d . . . . .
H29 H 1.493743 0.556627 -0.092635 0.028 Uiso 1 1 calc R U . . .
C61 C -0.9958(5) 0.3633(3) 1.1840(3) 0.0276(10) Uani 1 1 d . . . . .
H61A H -1.010594 0.424783 1.191375 0.033 Uiso 1 1 calc R U . . .
H61B H -0.962793 0.336906 1.235436 0.033 Uiso 1 1 calc R U . . .
C13 C 0.6303(5) 0.6218(3) 0.3311(3) 0.0247(10) Uani 1 1 d . . . . .
C8 C 0.6731(4) 0.5957(3) 0.4077(3) 0.0261(10) Uani 1 1 d . . . . .
H8 H 0.760406 0.569997 0.426602 0.031 Uiso 1 1 calc R U . . .
C42 C -0.0633(4) 0.3994(3) 0.5218(3) 0.0240(9) Uani 1 1 d . . . . .
C23 C 1.2764(5) 0.6632(3) 0.0634(3) 0.0262(10) Uani 1 1 d . . . . .
C34 C 0.2178(5) 0.4655(3) 0.3462(3) 0.0254(10) Uani 1 1 d . . . . .
H34 H 0.127748 0.488025 0.337294 0.031 Uiso 1 1 calc R U . . .
C36 C 0.4233(5) 0.4403(3) 0.3036(3) 0.0256(10) Uani 1 1 d . . . . .
C14 C 0.9418(4) 0.6316(3) 0.2475(3) 0.0236(9) Uani 1 1 d . . . . .
H14 H 1.037249 0.642242 0.265646 0.028 Uiso 1 1 calc R U . . .
C54 C -0.5171(5) 0.3812(3) 0.9036(3) 0.0238(11) Uani 1 1 d . . . . .
C35 C 0.2918(5) 0.4737(3) 0.2924(3) 0.0250(10) Uani 1 1 d . . . . .
C5 C 0.1176(4) 0.6102(3) 0.5492(3) 0.0243(9) Uani 1 1 d . . . . .
H5 H 0.075443 0.636448 0.501444 0.029 Uiso 1 1 calc R U . . .
C28 C 1.6981(4) 0.6508(3) -0.0823(3) 0.0282(10) Uani 1 1 d . . . . .
H28A H 1.722482 0.589764 -0.082790 0.034 Uiso 1 1 calc R U . . .
H28B H 1.779793 0.682088 -0.052884 0.034 Uiso 1 1 calc R U . . .
C18 C 0.7422(4) 0.6011(3) 0.1451(3) 0.0256(10) Uani 1 1 d . . . . .
H18 H 0.700886 0.590455 0.092348 0.031 Uiso 1 1 calc R U . . .
C53 C -0.4401(5) 0.3852(3) 0.8622(3) 0.0255(11) Uani 1 1 d . . . . .
C43 C 0.0644(5) 0.3597(3) 0.5428(3) 0.0250(10) Uani 1 1 d . . . . .
C7 C 0.3734(5) 0.6579(3) 0.4900(3) 0.0295(11) Uani 1 1 d . . . . .
C30 C 1.5225(4) 0.6435(3) -0.2051(3) 0.0272(10) Uani 1 1 d . . . . .
H30A H 1.488296 0.670554 -0.256156 0.033 Uiso 1 1 calc R U . . .
H30B H 1.536941 0.582189 -0.213298 0.033 Uiso 1 1 calc R U . . .
C37 C 0.4799(4) 0.4003(3) 0.3728(3) 0.0263(10) Uani 1 1 d . . . . .
C58 C -0.6001(4) 0.4137(3) 1.0204(2) 0.0220(9) Uani 1 1 d . . . . .
C64 C -1.1316(4) 0.3218(3) 1.1418(3) 0.0261(10) Uani 1 1 d . . . . .
H64 H -1.116967 0.258978 1.138858 0.031 Uiso 1 1 calc R U . . .
C16 C 0.7183(4) 0.6156(3) 0.2763(3) 0.0224(9) Uani 1 1 d . . . . .
C63 C -1.1698(5) 0.3577(4) 1.0605(3) 0.0314(11) Uani 1 1 d . . . . .
H63A H -1.252320 0.328130 1.030039 0.038 Uiso 1 1 calc R U . . .
H63B H -1.191759 0.419047 1.062365 0.038 Uiso 1 1 calc R U . . .
C33 C 1.7410(5) 0.7085(4) -0.2856(3) 0.0346(11) Uani 1 1 d . . . . .
H33A H 1.657180 0.684425 -0.318815 0.052 Uiso 1 1 calc R U . . .
H33B H 1.818102 0.698014 -0.308590 0.052 Uiso 1 1 calc R U . . .
H33C H 1.729362 0.770027 -0.280266 0.052 Uiso 1 1 calc R U . . .
C65 C -1.2443(5) 0.3373(3) 1.1839(3) 0.0301(11) Uani 1 1 d . . . . .
H65A H -1.253779 0.399398 1.190771 0.036 Uiso 1 1 calc R U . . .
H65B H -1.332402 0.316038 1.151485 0.036 Uiso 1 1 calc R U . . .
C66 C -1.2165(5) 0.2940(4) 1.2623(3) 0.0380(12) Uani 1 1 d . . . . .
H66A H -1.197550 0.233423 1.256758 0.057 Uiso 1 1 calc R U . . .
H66B H -1.296901 0.300033 1.283378 0.057 Uiso 1 1 calc R U . . .
H66C H -1.137137 0.320845 1.297310 0.057 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'
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'
O O 0.0492 0.0322 '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 -7 -8 0.0274
-7 1 3 0.0606
7 -1 -3 0.0632
0 7 9 0.0105
4 -3 -10 0.0507
-4 1 11 0.0318
0 -8 7 0.0102
0 8 -7 0.0184
0 1 -11 0.0149
0 -1 11 0.0010
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
C40 O4 C39 117.5(3) . . ?
C62 O5 C61 110.4(3) . . ?
C7 O1 C6 118.3(3) . . ?
C29 O2 C30 110.2(3) . . ?
C29 O3 C28 109.5(3) . . ?
C62 O6 C63 110.0(3) . . ?
C48 C49 C46 123.1(4) . . ?
C48 C49 C50 115.6(4) . . ?
C50 C49 C46 121.2(4) . . ?
F9 C25 C24 117.4(4) . . ?
F9 C25 C26 119.1(4) . . ?
C26 C25 C24 123.5(4) . . ?
F6 C11 C10 118.2(4) . . ?
C12 C11 F6 117.9(4) . . ?
C12 C11 C10 123.9(4) . . ?
F18 C48 C49 119.8(4) . . ?
F18 C48 C47 116.4(4) . . ?
C47 C48 C49 123.7(4) . . ?
C38 C39 O4 119.9(4) . . ?
C34 C39 O4 117.6(4) . . ?
C34 C39 C38 122.2(4) . . ?
C45 C46 C49 119.5(4) . . ?
C45 C46 C41 117.6(4) . . ?
C41 C46 C49 122.9(4) . . ?
F2 C3 C4 120.6(4) . . ?
F2 C3 C2 121.2(4) . . ?
C2 C3 C4 118.2(4) . . ?
O5 C62 H62 108.8 . . ?
O5 C62 C60 108.8(4) . . ?
O6 C62 O5 112.2(4) . . ?
O6 C62 H62 108.8 . . ?
O6 C62 C60 109.6(4) . . ?
C60 C62 H62 108.8 . . ?
C11 C10 C7 125.4(4) . . ?
C9 C10 C11 114.4(4) . . ?
C9 C10 C7 120.2(4) . . ?
C20 C21 C24 175.2(5) . . ?
C21 C20 C19 176.5(5) . . ?
C22 C27 C29 121.1(4) . . ?
C26 C27 C22 120.0(4) . . ?
C26 C27 C29 118.8(4) . . ?
F20 C56 C57 116.9(4) . . ?
F20 C56 C55 119.1(4) . . ?
C55 C56 C57 124.0(4) . . ?
C32 C31 H31 108.5 . . ?
C28 C31 H31 108.5 . . ?
C28 C31 C32 111.3(4) . . ?
C28 C31 C30 108.4(4) . . ?
C30 C31 H31 108.5 . . ?
C30 C31 C32 111.5(4) . . ?
C59 C60 C62 119.0(4) . . ?
C55 C60 C62 121.1(4) . . ?
C55 C60 C59 119.9(4) . . ?
C56 C57 C54 121.4(4) . . ?
C58 C57 C56 114.5(4) . . ?
C58 C57 C54 123.9(4) . . ?
F7 C9 C10 117.8(4) . . ?
F7 C9 C8 117.8(4) . . ?
C8 C9 C10 124.4(4) . . ?
C14 C19 C20 119.3(4) . . ?
C14 C19 C18 118.4(4) . . ?
C18 C19 C20 122.3(4) . . ?
C60 C59 H59 120.7 . . ?
C58 C59 C60 118.6(4) . . ?
C58 C59 H59 120.7 . . ?
C48 C47 H47 120.0 . . ?
C48 C47 C52 119.9(4) . . ?
C52 C47 H47 120.0 . . ?
C46 C45 H45 120.0 . . ?
C44 C45 C46 120.1(4) . . ?
C44 C45 H45 120.0 . . ?
F1 C4 C3 117.4(4) . . ?
F1 C4 C5 120.7(4) . . ?
C5 C4 C3 121.9(4) . . ?
C18 C17 H17 118.6 . . ?
C18 C17 C16 122.7(4) . . ?
C16 C17 H17 118.6 . . ?
C47 C52 C51 118.1(4) . . ?
C47 C52 C53 119.8(4) . . ?
C51 C52 C53 122.1(4) . . ?
O1 C6 C1 117.2(4) . . ?
O1 C6 C5 121.0(4) . . ?
C5 C6 C1 121.4(4) . . ?
C39 C38 H38 121.2 . . ?
C37 C38 C39 117.6(4) . . ?
C37 C38 H38 121.2 . . ?
F14 C40 F15 105.0(4) . . ?
F14 C40 O4 111.5(3) . . ?
F14 C40 C43 111.4(4) . . ?
F15 C40 C43 109.5(3) . . ?
O4 C40 F15 110.5(4) . . ?
O4 C40 C43 109.0(4) . . ?
C25 C24 C21 123.9(4) . . ?
C25 C24 C23 115.2(4) . . ?
C23 C24 C21 120.9(4) . . ?
C46 C41 H41 120.1 . . ?
C42 C41 C46 119.8(4) . . ?
C42 C41 H41 120.1 . . ?
C56 C55 C60 118.9(4) . . ?
C56 C55 H55 120.6 . . ?
C60 C55 H55 120.6 . . ?
C49 C50 H50 118.8 . . ?
C51 C50 C49 122.4(4) . . ?
C51 C50 H50 118.8 . . ?
C52 C51 H51 119.9 . . ?
C50 C51 C52 120.3(4) . . ?
C50 C51 H51 119.9 . . ?
F3 C2 C3 117.3(4) . . ?
F3 C2 C1 120.7(4) . . ?
C1 C2 C3 121.9(4) . . ?
F8 C15 C14 117.1(4) . . ?
F8 C15 C16 118.5(4) . . ?
C14 C15 C16 124.4(4) . . ?
C27 C22 H22 120.9 . . ?
C23 C22 C27 118.2(4) . . ?
C23 C22 H22 120.9 . . ?
F16 C44 C45 116.9(4) . . ?
F16 C44 C43 119.6(4) . . ?
C45 C44 C43 123.5(4) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(4) . . ?
C13 C12 H12 120.0 . . ?
C31 C32 H32A 109.0 . . ?
C31 C32 H32B 109.0 . . ?
C31 C32 C33 112.9(4) . . ?
H32A C32 H32B 107.8 . . ?
C33 C32 H32A 109.0 . . ?
C33 C32 H32B 109.0 . . ?
C25 C26 C27 119.1(4) . . ?
C25 C26 H26 120.5 . . ?
C27 C26 H26 120.5 . . ?
C6 C1 H1 120.9 . . ?
C2 C1 C6 118.2(4) . . ?
C2 C1 H1 120.9 . . ?
O2 C29 O3 112.1(4) . . ?
O2 C29 C27 108.2(3) . . ?
O2 C29 H29 109.0 . . ?
O3 C29 C27 109.4(3) . . ?
O3 C29 H29 109.0 . . ?
C27 C29 H29 109.0 . . ?
O5 C61 H61A 109.5 . . ?
O5 C61 H61B 109.5 . . ?
O5 C61 C64 110.6(4) . . ?
H61A C61 H61B 108.1 . . ?
C64 C61 H61A 109.5 . . ?
C64 C61 H61B 109.5 . . ?
C12 C13 C16 118.7(4) . . ?
C8 C13 C12 118.3(4) . . ?
C8 C13 C16 123.0(4) . . ?
C9 C8 C13 118.9(4) . . ?
C9 C8 H8 120.5 . . ?
C13 C8 H8 120.5 . . ?
F17 C42 C41 117.9(4) . . ?
F17 C42 C43 117.5(4) . . ?
C41 C42 C43 124.6(4) . . ?
F10 C23 C24 117.3(4) . . ?
F10 C23 C22 118.8(4) . . ?
C22 C23 C24 124.0(4) . . ?
C39 C34 H34 120.9 . . ?
C35 C34 C39 118.1(4) . . ?
C35 C34 H34 120.9 . . ?
F12 C36 C35 120.9(4) . . ?
F12 C36 C37 121.3(4) . . ?
C37 C36 C35 117.8(4) . . ?
C19 C14 H14 120.3 . . ?
C15 C14 C19 119.3(4) . . ?
C15 C14 H14 120.3 . . ?
C53 C54 C57 175.2(5) . . ?
F13 C35 C34 120.3(4) . . ?
F13 C35 C36 117.7(4) . . ?
C34 C35 C36 122.0(4) . . ?
C4 C5 C6 118.3(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
O3 C28 C31 111.3(4) . . ?
O3 C28 H28A 109.4 . . ?
O3 C28 H28B 109.4 . . ?
C31 C28 H28A 109.4 . . ?
C31 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C19 C18 H18 119.9 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C54 C53 C52 176.3(4) . . ?
C44 C43 C40 124.4(4) . . ?
C44 C43 C42 114.2(4) . . ?
C42 C43 C40 121.3(4) . . ?
F5 C7 O1 109.6(4) . . ?
F5 C7 C10 111.3(4) . . ?
F4 C7 F5 103.6(4) . . ?
F4 C7 O1 110.2(4) . . ?
F4 C7 C10 112.2(4) . . ?
O1 C7 C10 109.8(4) . . ?
O2 C30 C31 111.2(4) . . ?
O2 C30 H30A 109.4 . . ?
O2 C30 H30B 109.4 . . ?
C31 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
F11 C37 C38 119.5(4) . . ?
F11 C37 C36 118.3(4) . . ?
C38 C37 C36 122.2(4) . . ?
F19 C58 C57 117.0(4) . . ?
F19 C58 C59 118.9(4) . . ?
C59 C58 C57 124.1(4) . . ?
C61 C64 H64 108.6 . . ?
C63 C64 C61 107.3(4) . . ?
C63 C64 H64 108.6 . . ?
C63 C64 C65 111.8(4) . . ?
C65 C64 C61 111.7(4) . . ?
C65 C64 H64 108.6 . . ?
C17 C16 C13 122.0(4) . . ?
C15 C16 C17 115.0(4) . . ?
C15 C16 C13 122.9(4) . . ?
O6 C63 C64 110.9(4) . . ?
O6 C63 H63A 109.5 . . ?
O6 C63 H63B 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
H63A C63 H63B 108.1 . . ?
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 . . ?
C64 C65 H65A 108.9 . . ?
C64 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
C66 C65 C64 113.3(4) . . ?
C66 C65 H65A 108.9 . . ?
C66 C65 H65B 108.9 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
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
F20 C56 1.354(5) . ?
F9 C25 1.354(5) . ?
F17 C42 1.355(5) . ?
F6 C11 1.359(5) . ?
F8 C15 1.369(5) . ?
F14 C40 1.345(5) . ?
F16 C44 1.346(5) . ?
F19 C58 1.354(5) . ?
F2 C3 1.338(5) . ?
F3 C2 1.355(5) . ?
F12 C36 1.327(5) . ?
F18 C48 1.350(5) . ?
F7 C9 1.354(5) . ?
F10 C23 1.349(5) . ?
F15 C40 1.363(5) . ?
F13 C35 1.350(5) . ?
F11 C37 1.335(5) . ?
F1 C4 1.351(5) . ?
F5 C7 1.362(6) . ?
O4 C39 1.409(5) . ?
O4 C40 1.361(6) . ?
F4 C7 1.360(6) . ?
O5 C62 1.407(5) . ?
O5 C61 1.436(5) . ?
O1 C6 1.381(5) . ?
O1 C7 1.365(6) . ?
O2 C29 1.403(5) . ?
O2 C30 1.436(5) . ?
O3 C29 1.411(5) . ?
O3 C28 1.436(5) . ?
O6 C62 1.405(5) . ?
O6 C63 1.440(5) . ?
C49 C48 1.396(6) . ?
C49 C46 1.479(6) . ?
C49 C50 1.409(6) . ?
C25 C24 1.391(6) . ?
C25 C26 1.374(6) . ?
C11 C10 1.399(7) . ?
C11 C12 1.357(6) . ?
C48 C47 1.364(6) . ?
C39 C38 1.384(6) . ?
C39 C34 1.383(7) . ?
C46 C45 1.402(6) . ?
C46 C41 1.406(6) . ?
C3 C4 1.390(7) . ?
C3 C2 1.379(6) . ?
C62 H62 1.0000 . ?
C62 C60 1.507(6) . ?
C10 C9 1.391(6) . ?
C10 C7 1.496(7) . ?
C21 C20 1.192(6) . ?
C21 C24 1.422(6) . ?
C20 C19 1.436(7) . ?
C27 C22 1.398(6) . ?
C27 C26 1.395(6) . ?
C27 C29 1.513(6) . ?
C56 C57 1.403(6) . ?
C56 C55 1.361(6) . ?
C31 H31 1.0000 . ?
C31 C32 1.530(6) . ?
C31 C28 1.516(6) . ?
C31 C30 1.519(6) . ?
C60 C59 1.401(6) . ?
C60 C55 1.392(6) . ?
C57 C54 1.431(7) . ?
C57 C58 1.396(6) . ?
C9 C8 1.385(6) . ?
C19 C14 1.394(7) . ?
C19 C18 1.412(6) . ?
C59 H59 0.9500 . ?
C59 C58 1.364(6) . ?
C47 H47 0.9500 . ?
C47 C52 1.406(6) . ?
C45 H45 0.9500 . ?
C45 C44 1.374(6) . ?
C4 C5 1.367(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.373(6) . ?
C17 C16 1.401(6) . ?
C52 C51 1.411(6) . ?
C52 C53 1.422(6) . ?
C6 C1 1.392(6) . ?
C6 C5 1.388(6) . ?
C38 H38 0.9500 . ?
C38 C37 1.378(6) . ?
C40 C43 1.513(6) . ?
C24 C23 1.398(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.356(6) . ?
C55 H55 0.9500 . ?
C50 H50 0.9500 . ?
C50 C51 1.374(6) . ?
C51 H51 0.9500 . ?
C2 C1 1.372(6) . ?
C15 C14 1.370(6) . ?
C15 C16 1.397(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.379(6) . ?
C44 C43 1.392(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.414(6) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.532(7) . ?
C26 H26 0.9500 . ?
C1 H1 0.9500 . ?
C29 H29 1.0000 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C64 1.534(6) . ?
C13 C8 1.396(7) . ?
C13 C16 1.482(6) . ?
C8 H8 0.9500 . ?
C42 C43 1.394(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.364(7) . ?
C36 C35 1.392(7) . ?
C36 C37 1.381(7) . ?
C14 H14 0.9500 . ?
C54 C53 1.201(6) . ?
C5 H5 0.9500 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C18 H18 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C64 H64 1.0000 . ?
C64 C63 1.521(7) . ?
C64 C65 1.532(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C65 C66 1.525(7) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
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
F20 C56 C57 C54 3.6(7) . . . . ?
F20 C56 C57 C58 179.4(4) . . . . ?
F20 C56 C55 C60 -178.4(4) . . . . ?
F9 C25 C24 C21 2.9(7) . . . . ?
F9 C25 C24 C23 179.2(4) . . . . ?
F9 C25 C26 C27 -178.4(4) . . . . ?
F17 C42 C43 C40 -2.7(6) . . . . ?
F17 C42 C43 C44 175.0(4) . . . . ?
F6 C11 C10 C9 175.2(4) . . . . ?
F6 C11 C10 C7 -4.5(7) . . . . ?
F6 C11 C12 C13 -177.2(4) . . . . ?
F8 C15 C14 C19 -179.2(4) . . . . ?
F8 C15 C16 C17 -179.2(4) . . . . ?
F8 C15 C16 C13 4.1(7) . . . . ?
F14 C40 C43 C44 20.8(6) . . . . ?
F14 C40 C43 C42 -161.8(4) . . . . ?
F16 C44 C43 C40 2.8(7) . . . . ?
F16 C44 C43 C42 -174.8(4) . . . . ?
F2 C3 C4 F1 -2.3(7) . . . . ?
F2 C3 C4 C5 179.4(4) . . . . ?
F2 C3 C2 F3 3.2(7) . . . . ?
F2 C3 C2 C1 -179.1(4) . . . . ?
F3 C2 C1 C6 177.6(4) . . . . ?
F12 C36 C35 F13 -1.1(7) . . . . ?
F12 C36 C35 C34 179.2(4) . . . . ?
F12 C36 C37 F11 1.4(7) . . . . ?
F12 C36 C37 C38 -179.5(4) . . . . ?
F18 C48 C47 C52 177.6(4) . . . . ?
F7 C9 C8 C13 178.5(4) . . . . ?
F15 C40 C43 C44 136.5(5) . . . . ?
F15 C40 C43 C42 -46.1(6) . . . . ?
F1 C4 C5 C6 -178.9(4) . . . . ?
O4 C39 C38 C37 -175.0(4) . . . . ?
O4 C39 C34 C35 174.8(4) . . . . ?
O4 C40 C43 C44 -102.6(5) . . . . ?
O4 C40 C43 C42 74.8(5) . . . . ?
O5 C62 C60 C59 -55.1(5) . . . . ?
O5 C62 C60 C55 126.9(4) . . . . ?
O5 C61 C64 C63 -53.3(5) . . . . ?
O5 C61 C64 C65 -176.2(4) . . . . ?
O1 C6 C1 C2 -174.5(4) . . . . ?
O1 C6 C5 C4 174.5(4) . . . . ?
O6 C62 C60 C59 -178.1(4) . . . . ?
O6 C62 C60 C55 4.0(6) . . . . ?
C49 C48 C47 C52 0.5(7) . . . . ?
C49 C46 C45 C44 177.8(4) . . . . ?
C49 C46 C41 C42 -177.0(4) . . . . ?
C49 C50 C51 C52 -0.2(7) . . . . ?
C25 C24 C23 F10 179.8(4) . . . . ?
C25 C24 C23 C22 -0.4(7) . . . . ?
C11 C10 C9 F7 -175.3(4) . . . . ?
C11 C10 C9 C8 2.9(7) . . . . ?
C11 C10 C7 F5 -132.8(5) . . . . ?
C11 C10 C7 F4 -17.3(6) . . . . ?
C11 C10 C7 O1 105.6(5) . . . . ?
C11 C12 C13 C8 1.2(7) . . . . ?
C11 C12 C13 C16 -178.2(4) . . . . ?
C48 C49 C46 C45 -143.2(5) . . . . ?
C48 C49 C46 C41 36.6(7) . . . . ?
C48 C49 C50 C51 1.9(7) . . . . ?
C48 C47 C52 C51 1.3(7) . . . . ?
C48 C47 C52 C53 -178.3(4) . . . . ?
C39 O4 C40 F14 62.2(5) . . . . ?
C39 O4 C40 F15 -54.0(5) . . . . ?
C39 O4 C40 C43 -174.4(3) . . . . ?
C39 C38 C37 F11 178.9(4) . . . . ?
C39 C38 C37 C36 -0.1(7) . . . . ?
C39 C34 C35 F13 -178.9(4) . . . . ?
C39 C34 C35 C36 0.8(7) . . . . ?
C46 C49 C48 F18 -3.3(7) . . . . ?
C46 C49 C48 C47 173.7(4) . . . . ?
C46 C49 C50 C51 -174.0(4) . . . . ?
C46 C45 C44 F16 177.8(4) . . . . ?
C46 C45 C44 C43 -2.3(7) . . . . ?
C46 C41 C42 F17 -178.9(4) . . . . ?
C46 C41 C42 C43 0.5(7) . . . . ?
C3 C4 C5 C6 -0.6(7) . . . . ?
C3 C2 C1 C6 0.0(7) . . . . ?
C62 O5 C61 C64 57.8(5) . . . . ?
C62 O6 C63 C64 -58.5(5) . . . . ?
C62 C60 C59 C58 -176.2(4) . . . . ?
C62 C60 C55 C56 176.1(4) . . . . ?
C10 C11 C12 C13 2.3(7) . . . . ?
C10 C9 C8 C13 0.3(7) . . . . ?
C21 C24 C23 F10 -3.7(7) . . . . ?
C21 C24 C23 C22 176.1(5) . . . . ?
C20 C19 C14 C15 178.5(4) . . . . ?
C20 C19 C18 C17 -178.1(4) . . . . ?
C27 C22 C23 F10 179.9(4) . . . . ?
C27 C22 C23 C24 0.1(7) . . . . ?
C56 C57 C58 F19 -178.5(4) . . . . ?
C56 C57 C58 C59 -0.1(7) . . . . ?
C60 C59 C58 F19 177.5(4) . . . . ?
C60 C59 C58 C57 -0.8(7) . . . . ?
C57 C56 C55 C60 0.9(7) . . . . ?
C9 C10 C7 F5 47.5(6) . . . . ?
C9 C10 C7 F4 163.0(4) . . . . ?
C9 C10 C7 O1 -74.0(5) . . . . ?
C59 C60 C55 C56 -1.8(7) . . . . ?
C47 C52 C51 C50 -1.4(7) . . . . ?
C45 C46 C41 C42 2.8(7) . . . . ?
C45 C44 C43 C40 -177.1(4) . . . . ?
C45 C44 C43 C42 5.3(7) . . . . ?
C4 C3 C2 F3 -176.6(4) . . . . ?
C4 C3 C2 C1 1.0(7) . . . . ?
C6 O1 C7 F5 52.7(5) . . . . ?
C6 O1 C7 F4 -60.6(5) . . . . ?
C6 O1 C7 C10 175.3(4) . . . . ?
C38 C39 C34 C35 0.7(7) . . . . ?
C40 O4 C39 C38 -77.3(5) . . . . ?
C40 O4 C39 C34 108.4(5) . . . . ?
C24 C25 C26 C27 1.0(7) . . . . ?
C41 C46 C45 C44 -2.0(7) . . . . ?
C41 C42 C43 C40 177.9(4) . . . . ?
C41 C42 C43 C44 -4.5(7) . . . . ?
C55 C56 C57 C54 -175.7(4) . . . . ?
C55 C56 C57 C58 0.1(7) . . . . ?
C55 C60 C59 C58 1.8(7) . . . . ?
C50 C49 C48 F18 -179.1(4) . . . . ?
C50 C49 C48 C47 -2.1(7) . . . . ?
C50 C49 C46 C45 32.4(6) . . . . ?
C50 C49 C46 C41 -147.8(5) . . . . ?
C2 C3 C4 F1 177.6(4) . . . . ?
C2 C3 C4 C5 -0.7(7) . . . . ?
C22 C27 C26 C25 -1.3(7) . . . . ?
C22 C27 C29 O2 -126.5(4) . . . . ?
C22 C27 C29 O3 -4.2(6) . . . . ?
C12 C11 C10 C9 -4.3(7) . . . . ?
C12 C11 C10 C7 176.0(4) . . . . ?
C12 C13 C8 C9 -2.4(7) . . . . ?
C12 C13 C16 C17 -33.5(6) . . . . ?
C12 C13 C16 C15 143.0(5) . . . . ?
C32 C31 C28 O3 -175.0(4) . . . . ?
C32 C31 C30 O2 174.1(4) . . . . ?
C26 C25 C24 C21 -176.5(4) . . . . ?
C26 C25 C24 C23 -0.1(7) . . . . ?
C26 C27 C22 C23 0.7(7) . . . . ?
C26 C27 C29 O2 55.5(5) . . . . ?
C26 C27 C29 O3 177.8(4) . . . . ?
C1 C6 C5 C4 1.7(7) . . . . ?
C29 O2 C30 C31 -56.8(5) . . . . ?
C29 O3 C28 C31 57.6(5) . . . . ?
C29 C27 C22 C23 -177.3(4) . . . . ?
C29 C27 C26 C25 176.8(4) . . . . ?
C61 O5 C62 O6 -62.4(5) . . . . ?
C61 O5 C62 C60 176.2(3) . . . . ?
C61 C64 C63 O6 53.7(5) . . . . ?
C61 C64 C65 C66 -65.8(6) . . . . ?
C8 C13 C16 C17 147.2(5) . . . . ?
C8 C13 C16 C15 -36.3(7) . . . . ?
C34 C39 C38 C37 -1.1(7) . . . . ?
C14 C19 C18 C17 1.4(7) . . . . ?
C14 C15 C16 C17 2.8(7) . . . . ?
C14 C15 C16 C13 -173.9(4) . . . . ?
C54 C57 C58 F19 -2.8(7) . . . . ?
C54 C57 C58 C59 175.5(4) . . . . ?
C35 C36 C37 F11 -177.5(4) . . . . ?
C35 C36 C37 C38 1.6(7) . . . . ?
C5 C6 C1 C2 -1.4(7) . . . . ?
C28 O3 C29 O2 -63.2(5) . . . . ?
C28 O3 C29 C27 176.8(4) . . . . ?
C28 C31 C32 C33 -173.0(4) . . . . ?
C28 C31 C30 O2 51.2(5) . . . . ?
C18 C19 C14 C15 -1.1(7) . . . . ?
C18 C17 C16 C15 -2.4(7) . . . . ?
C18 C17 C16 C13 174.4(4) . . . . ?
C53 C52 C51 C50 178.1(4) . . . . ?
C7 O1 C6 C1 -110.8(5) . . . . ?
C7 O1 C6 C5 76.1(5) . . . . ?
C7 C10 C9 F7 4.5(7) . . . . ?
C7 C10 C9 C8 -177.4(4) . . . . ?
C30 O2 C29 O3 63.0(4) . . . . ?
C30 O2 C29 C27 -176.3(4) . . . . ?
C30 C31 C32 C33 65.8(5) . . . . ?
C30 C31 C28 O3 -51.9(5) . . . . ?
C37 C36 C35 F13 177.8(4) . . . . ?
C37 C36 C35 C34 -1.9(7) . . . . ?
C16 C17 C18 C19 0.4(7) . . . . ?
C16 C15 C14 C19 -1.1(7) . . . . ?
C16 C13 C8 C9 176.9(4) . . . . ?
C63 O6 C62 O5 62.5(5) . . . . ?
C63 O6 C62 C60 -176.6(4) . . . . ?
C63 C64 C65 C66 173.9(4) . . . . ?
C65 C64 C63 O6 176.5(4) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.70(14)
2 0.30(14)
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 -7.0000 -8.0000 0.2000 0.5925 0.7643
-7.0000 1.0000 3.0000 0.1924 0.7684 -0.7263
7.0000 -1.0000 -3.0000 -0.1924 -0.7684 0.7263
-0.0000 7.0000 9.0000 -0.1546 -0.6510 -0.8131
4.0000 -3.0000 -10.0000 -0.2905 0.0887 0.9491
-4.0000 1.0000 11.0000 0.4967 -0.1115 -0.8911
0.0000 -8.0000 7.0000 0.9609 -0.2669 0.0857
-0.0000 8.0000 -7.0000 -0.9609 0.2669 -0.0857
-0.0000 1.0000 -11.0000 -0.5795 0.6254 0.4834
0.0000 -1.0000 11.0000 0.5795 -0.6254 -0.4834
