#------------------------------------------------------------------------------
#$Date: 2020-10-04 06:41:01 +0300 (Sun, 04 Oct 2020) $
#$Revision: 257152 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/87/4038743.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_4038743
loop_
_publ_author_name
'Marinova, Maya'
'Pascal, Simon'
'Guénée, Laure'
'Besnard, Céline'
'Shivachev, Boris'
'Kostova, Kalina'
'Villani, Claudio'
'Franzini, Roberta'
'Dimitrov, Vladimir'
'Lacour, Jérôme'
_publ_section_title
;
 Synthesis, Resolution, Configurational Stability, and Properties of
 Cationic Functionalized [5]Helicenes.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11908
_journal_page_last               11923
_journal_paper_doi               10.1021/acs.joc.0c01716
_journal_volume                  85
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C27 H21 Br N O2), C H2 Cl2, 2(B F4)'
_chemical_formula_sum            'C55 H44 B2 Br2 Cl2 F8 N2 O4'
_chemical_formula_weight         1201.26
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-28
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                104.972(5)
_cell_angle_beta                 95.439(4)
_cell_angle_gamma                94.459(4)
_cell_formula_units_Z            1
_cell_length_a                   7.7507(4)
_cell_length_b                   12.3048(5)
_cell_length_c                   13.5177(8)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    179.95(10)
_cell_measurement_theta_max      73.2340
_cell_measurement_theta_min      3.3730
_cell_volume                     1232.80(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004  (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4679
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -49.00   36.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365   38.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
  2 omega   66.00  131.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  178.0000 -180.0000 65

#__ type_ start__ end____ width___ exp.time_
  3 omega   59.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  178.0000 -120.0000 38

#__ type_ start__ end____ width___ exp.time_
  4 omega  118.00  172.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000 -120.0000 54

#__ type_ start__ end____ width___ exp.time_
  5 omega   86.00  129.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.9365  178.0000   30.0000 43

#__ type_ start__ end____ width___ exp.time_
  6 omega  122.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 45

#__ type_ start__ end____ width___ exp.time_
  7 omega   77.00  134.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  -60.0000 57

#__ type_ start__ end____ width___ exp.time_
  8 omega   46.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499    0.0000  -90.0000 128

#__ type_ start__ end____ width___ exp.time_
  9 omega   65.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -111.0000  -90.0000 47

#__ type_ start__ end____ width___ exp.time_
 10 omega   60.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000   30.0000 49

#__ type_ start__ end____ width___ exp.time_
 11 omega   58.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  150.0000 51

#__ type_ start__ end____ width___ exp.time_
 12 omega   31.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000    0.0000 62

#__ type_ start__ end____ width___ exp.time_
 13 omega   28.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000  -30.0000 75

#__ type_ start__ end____ width___ exp.time_
 14 omega   30.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 15 omega   24.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000   30.0000 33

#__ type_ start__ end____ width___ exp.time_
 16 omega   26.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -94.0000 -150.0000 37

#__ type_ start__ end____ width___ exp.time_
 17 omega   31.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000 -180.0000 68

#__ type_ start__ end____ width___ exp.time_
 18 omega -112.00  -15.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -57.0000 -180.0000 97

#__ type_ start__ end____ width___ exp.time_
 19 omega -119.00  -86.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365  -99.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
 20 omega -116.00  -63.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.9365 -151.0000 -102.0000 53

#__ type_ start__ end____ width___ exp.time_
 21 omega  -40.00   -5.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -77.0000 -120.0000 35

#__ type_ start__ end____ width___ exp.time_
 22 omega  -70.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -57.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 23 omega  -90.00   -3.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -77.0000    0.0000 87

#__ type_ start__ end____ width___ exp.time_
 24 omega  -51.00   -4.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -77.0000  120.0000 47

#__ type_ start__ end____ width___ exp.time_
 25 omega  -75.00   26.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615   19.0000  -90.0000 101

#__ type_ start__ end____ width___ exp.time_
 26 omega -117.00  -68.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -38.0000  -60.0000 49

#__ type_ start__ end____ width___ exp.time_
 27 omega  -32.00   -7.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -57.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 28 omega  -77.00  -50.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.0615  -57.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   50.00   76.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       39.0615 -125.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 30 omega  119.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 31 omega  117.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   60.0000 60

#__ type_ start__ end____ width___ exp.time_
 32 omega   77.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
 33 omega   74.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000    0.0000 66

#__ type_ start__ end____ width___ exp.time_
 34 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 35 omega   74.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
 36 omega   74.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   90.0000 41

#__ type_ start__ end____ width___ exp.time_
 37 omega   78.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   77.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000    0.0000 33

#__ type_ start__ end____ width___ exp.time_
 39 omega   74.00  125.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -60.0000 51

#__ type_ start__ end____ width___ exp.time_
 40 omega   74.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000   30.0000 75

#__ type_ start__ end____ width___ exp.time_
 41 omega   74.00  100.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 42 omega   77.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  120.0000 34

#__ type_ start__ end____ width___ exp.time_
 43 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 44 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
 45 omega   74.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 46 omega   74.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  150.0000 28

#__ type_ start__ end____ width___ exp.time_
 47 omega   77.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   90.0000 32

#__ type_ start__ end____ width___ exp.time_
 48 omega   78.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 49 omega   74.00  123.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  120.0000 49

#__ type_ start__ end____ width___ exp.time_
 50 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 51 omega   77.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 52 omega   74.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 53 omega   78.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   61.0000  150.0000 40

#__ type_ start__ end____ width___ exp.time_
 54 omega   74.00  145.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   77.0000  -30.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1992704000
_diffrn_orient_matrix_UB_12      -0.0296241000
_diffrn_orient_matrix_UB_13      -0.0193518000
_diffrn_orient_matrix_UB_21      -0.0110823000
_diffrn_orient_matrix_UB_22      0.0434806000
_diffrn_orient_matrix_UB_23      0.1165191000
_diffrn_orient_matrix_UB_31      -0.0220924000
_diffrn_orient_matrix_UB_32      0.1193043000
_diffrn_orient_matrix_UB_33      -0.0124785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15209
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         73.599
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
_exptl_crystal_F_000             606
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.1635
_exptl_crystal_size_min          0.0374
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
rystal is a non merohedral twin. Both components were integrated into a single HKLF5 file. No attemps was made to refine the absolute structure fron the twinned data.Hooft parameter given below.
The flack parameter on the major twin refined to -0.01(5). 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         15209
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0651
_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)+(0.1464P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.818
_reflns_Friedel_fraction_max     0.777
_reflns_number_gt                13816
_reflns_number_total             15209
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c01716_si_002.cif
_cod_data_source_block           10B
_cod_depositor_comments
'Adding full bibliography for 4038740--4038746.cif.'
_cod_original_cell_volume        1232.79(11)
_cod_database_code               4038743
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C55 H44 N2 O4 F8 B2 Br2 Cl2'
_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   0.871
_shelx_estimated_absorpt_t_min   0.434
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6504(15)
 0.3496(15)
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
 B1F-F3F \\sim B1F-F4F \\sim B1F-F2F \\sim B1F-F5F
 with sigma of 0.02
 F2F-F3F \\sim F2F-F5F \\sim F3F-F4F \\sim F3F-F5F \\sim F4F-F5F \\sim F2F-F4F
 with sigma of 0.04
 B1G-F2G \\sim B1G-F3G \\sim B1G-F4G \\sim B1G-F5G
 with sigma of 0.02
 F2G-F3G \\sim F2G-F5G \\sim F3G-F4G \\sim F3G-F5G \\sim F4G-F5G
 with sigma of 0.04
 B1I-F2I \\sim B1I-F5I \\sim B1I-F3I \\sim B1I-F4I
 with sigma of 0.02
 F2I-F3I \\sim F2I-F4I \\sim F2I-F5I \\sim F3I-F4I \\sim F3I-F5I \\sim F4I-F5I
 with sigma of 0.04
 B1H-F3H \\sim B1H-F2H \\sim B1H-F5H \\sim B1H-F4H
 with sigma of 0.02
 F3H-F2H \\sim F3H-F5H \\sim F3H-F4H \\sim F2H-F5H \\sim F2H-F4H \\sim F5H-F4H
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(B1G) = Uanis(B1F)
Uanis(B1I) = Uanis(B1H)
5. Rigid body (RIGU) restrains
 F4G, F2G, B1G, F3G, F5G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2F, F3F, B1F, F4F, F5F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5H, F3H, B1H, F2H, F4H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5I, F2I, B1I, F3I, F4I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F2G)=Sof(F3G)=Sof(B1G)=Sof(F4G)=Sof(F5G)=1-FVAR(1)
 Sof(F3F)=Sof(F4F)=Sof(B1F)=Sof(F2F)=Sof(F5F)=FVAR(1)
 Sof(F2I)=Sof(B1I)=Sof(F5I)=Sof(F3I)=Sof(F4I)=1-FVAR(2)
 Sof(F3H)=Sof(F2H)=Sof(B1H)=Sof(F5H)=Sof(F4H)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C29B(H29A,H29B), C30A(H30C,H30D), C30B(H30A,H30B), C29A(H29C,H29D), C0BA(H0BA,
 H0BB)
7.b Aromatic/amide H refined with riding coordinates:
 C24B(H24B), C22B(H22B), C13B(H13B), C8B(H8B), C22A(H22A), C24A(H24A),
 C9A(H9A), C13A(H13A), C8A(H8A), C15A(H15A), C23B(H23B), C4B(H4B), C3B(H3B),
 C15B(H15B), C7B(H7B), C7A(H7A), C14B(H14B), C9B(H9B), C23A(H23A), C4A(H4A),
 C3A(H3A), C14A(H14A)
7.c Idealised Me refined as rotating group:
 C31B(H31A,H31B,H31C), C28A(H28D,H28E,H28F), C28B(H28A,H28B,H28C), C31A(H31D,
 H31E,H31F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'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
Br1B Br 0.50799(11) 0.26138(9) 0.42768(7) 0.0469(3) Uani 1 1 d . . . . .
Br1A Br 1.29147(12) 0.61032(10) 0.54756(8) 0.0503(3) Uani 1 1 d . . . . .
Cl1A Cl 0.7812(7) 0.9771(4) 0.5811(4) 0.0907(13) Uani 1 1 d . . . . .
F2G F 0.359(4) 0.795(2) 0.1527(18) 0.051(5) Uani 0.52(3) 1 d D . P A 2
O20B O 0.2129(9) 0.3391(6) 1.0789(5) 0.0351(13) Uani 1 1 d . . . . .
O27A O 0.6215(9) 0.4263(6) 0.2755(5) 0.0390(14) Uani 1 1 d . . . . .
C5B C 0.2819(10) 0.1532(8) 0.7020(6) 0.0294(17) Uani 1 1 d . . . . .
O20A O 0.6555(9) 0.2848(6) -0.0842(5) 0.0386(14) Uani 1 1 d . . . . .
N11A N 0.7830(10) 0.0406(7) 0.1310(6) 0.0352(16) Uani 1 1 d . . . . .
C17A C 0.7248(11) 0.1657(8) 0.0265(7) 0.0313(17) Uani 1 1 d . . . . .
O27B O -0.0333(9) 0.2518(7) 0.7288(5) 0.0395(15) Uani 1 1 d . . . . .
N11B N 0.2171(10) -0.0405(7) 0.8690(6) 0.0327(15) Uani 1 1 d . . . . .
C21B C 0.1349(11) 0.3691(8) 0.9956(7) 0.0327(18) Uani 1 1 d . . . . .
C12B C 0.2408(11) 0.0353(8) 0.9659(6) 0.0304(17) Uani 1 1 d . . . . .
C24B C -0.0443(12) 0.4365(9) 0.8412(8) 0.040(2) Uani 1 1 d . . . . .
H24B H -0.109866 0.460002 0.788875 0.048 Uiso 1 1 calc R U . . .
C26A C 0.6645(10) 0.3581(8) 0.1017(7) 0.0314(17) Uani 1 1 d . . . . .
C21A C 0.6269(11) 0.3675(8) 0.0000(7) 0.0334(18) Uani 1 1 d . . . . .
C10A C 0.8382(11) 0.1310(8) 0.2139(7) 0.0352(19) Uani 1 1 d . . . . .
C22B C 0.0831(13) 0.4770(9) 1.0179(8) 0.039(2) Uani 1 1 d . . . . .
H22B H 0.107229 0.526541 1.085428 0.047 Uiso 1 1 calc R U . . .
C19A C 0.8369(11) 0.2440(8) 0.2055(7) 0.0308(17) Uani 1 1 d . . . . .
C10B C 0.2251(11) -0.0028(8) 0.7830(7) 0.0325(17) Uani 1 1 d . . . . .
C12A C 0.7534(11) 0.0551(8) 0.0335(7) 0.0355(19) Uani 1 1 d . . . . .
C13B C 0.2833(12) 0.0026(9) 1.0567(7) 0.0362(19) Uani 1 1 d . . . . .
H13B H 0.297475 -0.074099 1.053737 0.043 Uiso 1 1 calc R U . . .
C16A C 0.6839(12) 0.1802(8) -0.0731(7) 0.0349(18) Uani 1 1 d . . . . .
C8B C 0.2664(14) -0.0469(8) 0.6028(7) 0.038(2) Uani 1 1 d . . . . .
H8B H 0.267949 -0.100898 0.538429 0.046 Uiso 1 1 calc R U . . .
C22A C 0.5635(13) 0.4626(9) -0.0214(8) 0.042(2) Uani 1 1 d . . . . .
H22A H 0.548164 0.468945 -0.090200 0.050 Uiso 1 1 calc R U . . .
C25A C 0.6091(11) 0.4439(8) 0.1811(7) 0.0349(18) Uani 1 1 d . . . . .
F3G F 0.314(5) 0.914(2) 0.297(2) 0.111(13) Uani 0.52(3) 1 d D . P A 2
C17B C 0.2163(10) 0.1497(8) 0.9711(6) 0.0299(17) Uani 1 1 d . . . . .
C24A C 0.5420(13) 0.5381(9) 0.1597(9) 0.042(2) Uani 1 1 d . . . . .
H24A H 0.508944 0.596047 0.213743 0.051 Uiso 1 1 calc R U . . .
C9A C 0.8985(14) 0.1114(10) 0.3107(8) 0.041(2) Uani 1 1 d . . . . .
H9A H 0.886439 0.037050 0.319350 0.050 Uiso 1 1 calc R U . . .
C6A C 0.9986(12) 0.3108(9) 0.3799(7) 0.038(2) Uani 1 1 d . . . . .
C13A C 0.7461(13) -0.0334(9) -0.0568(8) 0.041(2) Uani 1 1 d . . . . .
H13A H 0.764967 -0.107324 -0.052119 0.049 Uiso 1 1 calc R U . . .
C8A C 0.9726(14) 0.1992(10) 0.3898(8) 0.044(2) Uani 1 1 d . . . . .
H8A H 1.008619 0.185385 0.454174 0.053 Uiso 1 1 calc R U . . .
C18A C 0.7433(11) 0.2591(8) 0.1152(7) 0.0317(17) Uani 1 1 d . . . . .
C15A C 0.6797(12) 0.0945(9) -0.1607(7) 0.040(2) Uani 1 1 d . . . . .
H15A H 0.655546 0.107418 -0.226689 0.048 Uiso 1 1 calc R U . . .
C26B C 0.1139(11) 0.2951(8) 0.8958(6) 0.0291(16) Uani 1 1 d . . . . .
C23B C -0.0046(14) 0.5101(9) 0.9391(8) 0.044(2) Uani 1 1 d . . . . .
H23B H -0.038413 0.584607 0.951895 0.053 Uiso 1 1 calc R U . . .
C19B C 0.2273(10) 0.1148(8) 0.7886(6) 0.0295(16) Uani 1 1 d . . . . .
C4B C 0.3341(11) 0.2667(8) 0.7091(6) 0.0289(16) Uani 1 1 d . . . . .
H4B H 0.323292 0.322624 0.770859 0.035 Uiso 1 1 calc R U . . .
C3B C 0.4005(10) 0.2995(8) 0.6293(6) 0.0321(17) Uani 1 1 d . . . . .
H3B H 0.437273 0.376817 0.635977 0.039 Uiso 1 1 calc R U . . .
F2I F 0.902(3) 0.659(4) 0.678(3) 0.094(8) Uani 0.76(12) 1 d D . P B 4
C6B C 0.3018(11) 0.0705(8) 0.6095(6) 0.0345(18) Uani 1 1 d . . . . .
C16B C 0.2328(11) 0.2276(8) 1.0696(6) 0.0319(17) Uani 1 1 d . . . . .
C18B C 0.1853(10) 0.1861(7) 0.8814(6) 0.0281(16) Uani 1 1 d . . . . .
C15B C 0.2775(13) 0.1971(9) 1.1584(7) 0.039(2) Uani 1 1 d . . . . .
H15B H 0.290034 0.251263 1.223736 0.047 Uiso 1 1 calc R U . . .
C7B C 0.3647(12) 0.1046(9) 0.5260(7) 0.0373(19) Uani 1 1 d . . . . .
H7B H 0.373183 0.050191 0.462882 0.045 Uiso 1 1 calc R U . . .
C7A C 1.0994(12) 0.3960(10) 0.4588(7) 0.040(2) Uani 1 1 d . . . . .
H7A H 1.138796 0.380767 0.522072 0.048 Uiso 1 1 calc R U . . .
C29B C 0.1895(12) -0.1632(8) 0.8607(7) 0.0366(19) Uani 1 1 d . . . . .
H29A H 0.108334 -0.200506 0.797881 0.044 Uiso 1 1 calc R U . . .
H29B H 0.133604 -0.173919 0.920844 0.044 Uiso 1 1 calc R U . . .
C30A C 0.9251(13) -0.1342(9) 0.1380(9) 0.044(2) Uani 1 1 d . . . . .
H30C H 0.974467 -0.131973 0.073562 0.053 Uiso 1 1 calc R U . . .
H30D H 1.012056 -0.093299 0.196920 0.053 Uiso 1 1 calc R U . . .
C14B C 0.3042(13) 0.0836(9) 1.1504(7) 0.040(2) Uani 1 1 d . . . . .
H14B H 0.337772 0.061927 1.211348 0.048 Uiso 1 1 calc R U . . .
C2A C 1.1411(12) 0.5012(9) 0.4444(7) 0.039(2) Uani 1 1 d . . . . .
C30B C 0.3562(13) -0.2207(9) 0.8559(8) 0.042(2) Uani 1 1 d . . . . .
H30A H 0.414666 -0.209176 0.796892 0.050 Uiso 1 1 calc R U . . .
H30B H 0.436379 -0.186416 0.919873 0.050 Uiso 1 1 calc R U . . .
C9B C 0.2309(14) -0.0832(9) 0.6856(8) 0.041(2) Uani 1 1 d . . . . .
H9B H 0.209649 -0.161931 0.679311 0.049 Uiso 1 1 calc R U . . .
C31B C 0.3163(16) -0.3459(9) 0.8440(9) 0.049(2) Uani 1 1 d . . . . .
H31A H 0.239821 -0.380136 0.779627 0.073 Uiso 1 1 calc R U . . .
H31B H 0.257978 -0.357153 0.902399 0.073 Uiso 1 1 calc R U . . .
H31C H 0.425092 -0.381514 0.842320 0.073 Uiso 1 1 calc R U . . .
C23A C 0.5234(14) 0.5471(10) 0.0588(9) 0.048(2) Uani 1 1 d . . . . .
H23A H 0.482205 0.613080 0.045112 0.057 Uiso 1 1 calc R U . . .
C25B C 0.0103(11) 0.3293(9) 0.8189(7) 0.0332(18) Uani 1 1 d . . . . .
B1G B 0.366(3) 0.811(2) 0.257(2) 0.038(4) Uani 0.52(3) 1 d D . P A 2
C2B C 0.4128(11) 0.2160(9) 0.5373(6) 0.037(2) Uani 1 1 d . . . . .
C28A C 0.6013(17) 0.5197(11) 0.3610(9) 0.054(3) Uani 1 1 d . . . . .
H28D H 0.481139 0.538959 0.355272 0.082 Uiso 1 1 calc R U . . .
H28E H 0.681538 0.585105 0.360536 0.082 Uiso 1 1 calc R U . . .
H28F H 0.627508 0.498741 0.425578 0.082 Uiso 1 1 calc R U . . .
C4A C 0.9847(11) 0.4419(9) 0.2749(7) 0.0348(18) Uani 1 1 d . . . . .
H4A H 0.946654 0.458053 0.211874 0.042 Uiso 1 1 calc R U . . .
C3A C 1.0864(12) 0.5240(9) 0.3505(7) 0.038(2) Uani 1 1 d . . . . .
H3A H 1.119515 0.595501 0.339539 0.046 Uiso 1 1 calc R U . . .
C29A C 0.7589(12) -0.0760(8) 0.1433(8) 0.039(2) Uani 1 1 d . . . . .
H29C H 0.668681 -0.121830 0.088454 0.047 Uiso 1 1 calc R U . . .
H29D H 0.715893 -0.072874 0.210537 0.047 Uiso 1 1 calc R U . . .
C14A C 0.7120(14) -0.0140(9) -0.1513(8) 0.042(2) Uani 1 1 d . . . . .
H14A H 0.710025 -0.074469 -0.211689 0.050 Uiso 1 1 calc R U . . .
C28B C -0.1510(16) 0.2808(12) 0.6539(8) 0.053(3) Uani 1 1 d . . . . .
H28A H -0.186515 0.213962 0.595718 0.079 Uiso 1 1 calc R U . . .
H28B H -0.092947 0.340735 0.629370 0.079 Uiso 1 1 calc R U . . .
H28C H -0.254053 0.307460 0.685421 0.079 Uiso 1 1 calc R U . . .
C31A C 0.889(2) -0.2563(10) 0.1410(11) 0.060(3) Uani 1 1 d . . . . .
H31D H 0.807550 -0.297840 0.080563 0.090 Uiso 1 1 calc R U . . .
H31E H 0.836996 -0.258580 0.203934 0.090 Uiso 1 1 calc R U . . .
H31F H 0.997996 -0.291399 0.140361 0.090 Uiso 1 1 calc R U . . .
C5A C 0.9349(11) 0.3345(8) 0.2877(7) 0.0316(17) Uani 1 1 d . . . . .
F4G F 0.532(2) 0.808(2) 0.2969(15) 0.087(8) Uani 0.52(3) 1 d D . P A 2
F5G F 0.262(3) 0.726(2) 0.275(2) 0.096(8) Uani 0.52(3) 1 d D . P A 2
C0BA C 0.761(2) 0.8357(15) 0.5069(12) 0.075(4) Uani 1 1 d . . . . .
H0BA H 0.775389 0.785213 0.552828 0.091 Uiso 1 1 calc R U . . .
H0BB H 0.643786 0.815386 0.467292 0.091 Uiso 1 1 calc R U . . .
Cl0B Cl 0.9204(6) 0.8174(5) 0.4219(3) 0.0905(14) Uani 1 1 d . . . . .
B1I B 0.752(3) 0.656(2) 0.724(3) 0.049(4) Uani 0.76(12) 1 d D . P B 4
F5I F 0.675(5) 0.547(2) 0.703(4) 0.090(10) Uani 0.76(12) 1 d D . P B 4
F3I F 0.639(4) 0.724(2) 0.691(2) 0.052(4) Uani 0.76(12) 1 d D . P B 4
F4I F 0.796(5) 0.696(4) 0.831(2) 0.062(6) Uani 0.76(12) 1 d D . P B 4
F3F F 0.519(3) 0.913(3) 0.3216(16) 0.100(10) Uani 0.48(3) 1 d D . P A 1
F4F F 0.361(6) 0.802(4) 0.180(2) 0.077(10) Uani 0.48(3) 1 d D . P A 1
B1F B 0.377(3) 0.837(2) 0.283(2) 0.038(4) Uani 0.48(3) 1 d D . P A 1
F2F F 0.248(3) 0.901(3) 0.315(2) 0.089(10) Uani 0.48(3) 1 d D . P A 1
F5F F 0.373(5) 0.750(2) 0.324(2) 0.105(11) Uani 0.48(3) 1 d D . P A 1
F3H F 0.674(15) 0.723(9) 0.688(9) 0.07(2) Uani 0.24(12) 1 d D . P B 3
F2H F 0.912(7) 0.636(5) 0.709(8) 0.058(16) Uani 0.24(12) 1 d D . P B 3
B1H B 0.750(8) 0.653(6) 0.741(6) 0.049(4) Uani 0.24(12) 1 d D . P B 3
F5H F 0.649(12) 0.551(8) 0.717(9) 0.065(16) Uani 0.24(12) 1 d D . P B 3
F4H F 0.766(15) 0.703(10) 0.846(6) 0.059(17) Uani 0.24(12) 1 d D . P B 3
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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_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 0 1 0.0187 -0.0002 -0.0005 1.0006 -0.0193 0.1166 -0.0125
0 0 -1 0.0187 0.0002 0.0005 -1.0006 0.0193 -0.1166 0.0125
0 1 0 0.0738 0.0000 0.9995 0.0002 -0.0296 0.0435 0.1192
0 -1 0 0.0738 -0.0000 -0.9995 -0.0002 0.0296 -0.0435 -0.1192
1 -1 1 0.0700 0.9998 -1.0005 1.0013 -0.1890 0.0621 -0.1539
-1 0 1 0.0952 -1.0002 0.0000 0.9996 0.1800 0.1276 0.0096
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
C16B O20B C21B 118.7(7) . . ?
C25A O27A C28A 117.6(8) . . ?
C4B C5B C19B 122.9(8) . . ?
C4B C5B C6B 118.2(8) . . ?
C6B C5B C19B 118.5(8) . . ?
C21A O20A C16A 119.2(7) . . ?
C10A N11A C12A 120.6(8) . . ?
C10A N11A C29A 121.0(8) . . ?
C12A N11A C29A 118.3(8) . . ?
C16A C17A C12A 117.4(9) . . ?
C16A C17A C18A 120.9(8) . . ?
C18A C17A C12A 121.6(8) . . ?
C25B O27B C28B 117.1(8) . . ?
C12B N11B C29B 118.9(7) . . ?
C10B N11B C12B 120.4(8) . . ?
C10B N11B C29B 120.7(8) . . ?
O20B C21B C22B 114.9(8) . . ?
O20B C21B C26B 121.6(8) . . ?
C22B C21B C26B 123.6(9) . . ?
N11B C12B C13B 122.8(8) . . ?
N11B C12B C17B 117.0(8) . . ?
C13B C12B C17B 120.2(8) . . ?
C23B C24B H24B 119.6 . . ?
C25B C24B H24B 119.6 . . ?
C25B C24B C23B 120.8(9) . . ?
C21A C26A C25A 116.1(8) . . ?
C21A C26A C18A 117.8(8) . . ?
C25A C26A C18A 126.0(8) . . ?
O20A C21A C26A 122.2(8) . . ?
O20A C21A C22A 115.2(8) . . ?
C22A C21A C26A 122.6(9) . . ?
N11A C10A C19A 121.1(8) . . ?
N11A C10A C9A 119.2(9) . . ?
C19A C10A C9A 119.7(9) . . ?
C21B C22B H22B 121.1 . . ?
C23B C22B C21B 117.9(9) . . ?
C23B C22B H22B 121.1 . . ?
C10A C19A C5A 118.1(8) . . ?
C18A C19A C10A 116.9(8) . . ?
C18A C19A C5A 125.0(9) . . ?
N11B C10B C19B 121.1(8) . . ?
N11B C10B C9B 119.1(9) . . ?
C19B C10B C9B 119.8(8) . . ?
N11A C12A C17A 116.9(8) . . ?
N11A C12A C13A 123.4(9) . . ?
C13A C12A C17A 119.7(9) . . ?
C12B C13B H13B 120.5 . . ?
C14B C13B C12B 119.1(9) . . ?
C14B C13B H13B 120.5 . . ?
O20A C16A C17A 119.7(8) . . ?
C15A C16A O20A 117.5(8) . . ?
C15A C16A C17A 122.6(9) . . ?
C6B C8B H8B 119.2 . . ?
C9B C8B H8B 119.2 . . ?
C9B C8B C6B 121.7(9) . . ?
C21A C22A H22A 120.7 . . ?
C23A C22A C21A 118.7(10) . . ?
C23A C22A H22A 120.7 . . ?
O27A C25A C26A 116.0(8) . . ?
O27A C25A C24A 123.1(9) . . ?
C24A C25A C26A 120.9(9) . . ?
C16B C17B C12B 118.0(8) . . ?
C18B C17B C12B 121.3(8) . . ?
C18B C17B C16B 120.6(8) . . ?
C25A C24A H24A 120.1 . . ?
C23A C24A C25A 119.7(10) . . ?
C23A C24A H24A 120.1 . . ?
C10A C9A H9A 120.2 . . ?
C8A C9A C10A 119.7(10) . . ?
C8A C9A H9A 120.2 . . ?
C7A C6A C8A 120.2(9) . . ?
C5A C6A C8A 119.7(9) . . ?
C5A C6A C7A 119.9(10) . . ?
C12A C13A H13A 119.7 . . ?
C14A C13A C12A 120.5(10) . . ?
C14A C13A H13A 119.7 . . ?
C9A C8A C6A 122.4(9) . . ?
C9A C8A H8A 118.8 . . ?
C6A C8A H8A 118.8 . . ?
C17A C18A C26A 115.5(8) . . ?
C17A C18A C19A 116.2(8) . . ?
C19A C18A C26A 128.3(8) . . ?
C16A C15A H15A 120.7 . . ?
C16A C15A C14A 118.6(9) . . ?
C14A C15A H15A 120.7 . . ?
C21B C26B C18B 118.1(8) . . ?
C21B C26B C25B 116.2(8) . . ?
C25B C26B C18B 125.4(8) . . ?
C24B C23B H23B 119.5 . . ?
C22B C23B C24B 121.0(10) . . ?
C22B C23B H23B 119.5 . . ?
C10B C19B C5B 118.2(8) . . ?
C18B C19B C5B 125.0(8) . . ?
C18B C19B C10B 116.7(8) . . ?
C5B C4B H4B 119.1 . . ?
C3B C4B C5B 121.8(8) . . ?
C3B C4B H4B 119.1 . . ?
C4B C3B H3B 120.7 . . ?
C4B C3B C2B 118.6(9) . . ?
C2B C3B H3B 120.7 . . ?
C5B C6B C8B 120.0(8) . . ?
C7B C6B C5B 119.9(9) . . ?
C7B C6B C8B 120.0(8) . . ?
O20B C16B C17B 120.4(8) . . ?
O20B C16B C15B 117.2(8) . . ?
C15B C16B C17B 122.3(9) . . ?
C17B C18B C26B 115.4(7) . . ?
C17B C18B C19B 117.0(8) . . ?
C19B C18B C26B 127.7(7) . . ?
C16B C15B H15B 120.9 . . ?
C16B C15B C14B 118.2(9) . . ?
C14B C15B H15B 120.9 . . ?
C6B C7B H7B 120.4 . . ?
C2B C7B C6B 119.2(8) . . ?
C2B C7B H7B 120.4 . . ?
C6A C7A H7A 119.9 . . ?
C2A C7A C6A 120.2(9) . . ?
C2A C7A H7A 119.9 . . ?
N11B C29B H29A 108.8 . . ?
N11B C29B H29B 108.8 . . ?
N11B C29B C30B 113.7(8) . . ?
H29A C29B H29B 107.7 . . ?
C30B C29B H29A 108.8 . . ?
C30B C29B H29B 108.8 . . ?
H30C C30A H30D 108.1 . . ?
C29A C30A H30C 109.5 . . ?
C29A C30A H30D 109.5 . . ?
C31A C30A H30C 109.5 . . ?
C31A C30A H30D 109.5 . . ?
C31A C30A C29A 110.7(9) . . ?
C13B C14B C15B 122.2(8) . . ?
C13B C14B H14B 118.9 . . ?
C15B C14B H14B 118.9 . . ?
C7A C2A Br1A 119.2(7) . . ?
C7A C2A C3A 120.4(9) . . ?
C3A C2A Br1A 120.1(8) . . ?
C29B C30B H30A 109.6 . . ?
C29B C30B H30B 109.6 . . ?
H30A C30B H30B 108.1 . . ?
C31B C30B C29B 110.4(9) . . ?
C31B C30B H30A 109.6 . . ?
C31B C30B H30B 109.6 . . ?
C10B C9B H9B 120.0 . . ?
C8B C9B C10B 120.0(10) . . ?
C8B C9B H9B 120.0 . . ?
C30B C31B H31A 109.5 . . ?
C30B C31B H31B 109.5 . . ?
C30B C31B H31C 109.5 . . ?
H31A C31B H31B 109.5 . . ?
H31A C31B H31C 109.5 . . ?
H31B C31B H31C 109.5 . . ?
C22A C23A C24A 121.4(10) . . ?
C22A C23A H23A 119.3 . . ?
C24A C23A H23A 119.3 . . ?
O27B C25B C24B 123.9(8) . . ?
O27B C25B C26B 116.2(8) . . ?
C24B C25B C26B 119.8(9) . . ?
F3G B1G F2G 108(2) . . ?
F4G B1G F2G 110(2) . . ?
F4G B1G F3G 110(2) . . ?
F5G B1G F2G 109(2) . . ?
F5G B1G F3G 112(2) . . ?
F5G B1G F4G 109(2) . . ?
C3B C2B Br1B 118.5(8) . . ?
C7B C2B Br1B 119.3(7) . . ?
C7B C2B C3B 122.2(8) . . ?
O27A C28A H28D 109.5 . . ?
O27A C28A H28E 109.5 . . ?
O27A C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
C3A C4A H4A 119.0 . . ?
C3A C4A C5A 122.1(9) . . ?
C5A C4A H4A 119.0 . . ?
C2A C3A H3A 120.4 . . ?
C4A C3A C2A 119.2(10) . . ?
C4A C3A H3A 120.4 . . ?
N11A C29A C30A 113.2(8) . . ?
N11A C29A H29C 108.9 . . ?
N11A C29A H29D 108.9 . . ?
C30A C29A H29C 108.9 . . ?
C30A C29A H29D 108.9 . . ?
H29C C29A H29D 107.7 . . ?
C13A C14A C15A 121.0(9) . . ?
C13A C14A H14A 119.5 . . ?
C15A C14A H14A 119.5 . . ?
O27B C28B H28A 109.5 . . ?
O27B C28B H28B 109.5 . . ?
O27B C28B H28C 109.5 . . ?
H28A C28B H28B 109.5 . . ?
H28A C28B H28C 109.5 . . ?
H28B C28B H28C 109.5 . . ?
C30A C31A H31D 109.5 . . ?
C30A C31A H31E 109.5 . . ?
C30A C31A H31F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C6A C5A C19A 119.0(9) . . ?
C6A C5A C4A 118.0(9) . . ?
C4A C5A C19A 122.6(8) . . ?
Cl1A C0BA H0BA 109.7 . . ?
Cl1A C0BA H0BB 109.7 . . ?
H0BA C0BA H0BB 108.2 . . ?
Cl0B C0BA Cl1A 109.8(10) . . ?
Cl0B C0BA H0BA 109.7 . . ?
Cl0B C0BA H0BB 109.7 . . ?
F2I B1I F5I 110.3(18) . . ?
F2I B1I F3I 109.6(16) . . ?
F2I B1I F4I 108.4(15) . . ?
F5I B1I F3I 110.5(15) . . ?
F5I B1I F4I 108.1(18) . . ?
F3I B1I F4I 109.8(16) . . ?
F4F B1F F3F 112(3) . . ?
F4F B1F F2F 110(2) . . ?
F2F B1F F3F 101(2) . . ?
F5F B1F F3F 113(2) . . ?
F5F B1F F4F 111(2) . . ?
F5F B1F F2F 109(3) . . ?
F3H B1H F2H 108(3) . . ?
F3H B1H F4H 110(4) . . ?
F5H B1H F3H 109(4) . . ?
F5H B1H F2H 109(3) . . ?
F5H B1H F4H 110(4) . . ?
F4H B1H F2H 110(3) . . ?
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
Br1B C2B 1.903(9) . ?
Br1A C2A 1.894(9) . ?
Cl1A C0BA 1.756(17) . ?
F2G B1G 1.363(19) . ?
O20B C21B 1.375(10) . ?
O20B C16B 1.366(12) . ?
O27A C25A 1.344(12) . ?
O27A C28A 1.434(12) . ?
C5B C19B 1.457(12) . ?
C5B C4B 1.400(13) . ?
C5B C6B 1.423(12) . ?
O20A C21A 1.365(11) . ?
O20A C16A 1.365(12) . ?
N11A C10A 1.366(13) . ?
N11A C12A 1.375(12) . ?
N11A C29A 1.487(12) . ?
C17A C12A 1.421(13) . ?
C17A C16A 1.414(12) . ?
C17A C18A 1.417(12) . ?
O27B C25B 1.333(12) . ?
O27B C28B 1.430(11) . ?
N11B C12B 1.384(11) . ?
N11B C10B 1.362(12) . ?
N11B C29B 1.482(12) . ?
C21B C22B 1.383(14) . ?
C21B C26B 1.406(12) . ?
C12B C13B 1.406(12) . ?
C12B C17B 1.420(13) . ?
C24B H24B 0.9500 . ?
C24B C23B 1.388(16) . ?
C24B C25B 1.384(14) . ?
C26A C21A 1.414(12) . ?
C26A C25A 1.422(13) . ?
C26A C18A 1.449(13) . ?
C21A C22A 1.390(14) . ?
C10A C19A 1.424(14) . ?
C10A C9A 1.434(13) . ?
C22B H22B 0.9500 . ?
C22B C23B 1.376(15) . ?
C19A C18A 1.422(12) . ?
C19A C5A 1.456(12) . ?
C10B C19B 1.428(13) . ?
C10B C9B 1.435(13) . ?
C12A C13A 1.404(14) . ?
C13B H13B 0.9500 . ?
C13B C14B 1.380(15) . ?
C16A C15A 1.363(13) . ?
C8B H8B 0.9500 . ?
C8B C6B 1.426(14) . ?
C8B C9B 1.352(15) . ?
C22A H22A 0.9500 . ?
C22A C23A 1.373(16) . ?
C25A C24A 1.392(15) . ?
F3G B1G 1.36(2) . ?
C17B C16B 1.413(12) . ?
C17B C18B 1.403(11) . ?
C24A H24A 0.9500 . ?
C24A C23A 1.392(16) . ?
C9A H9A 0.9500 . ?
C9A C8A 1.352(16) . ?
C6A C8A 1.415(15) . ?
C6A C7A 1.408(14) . ?
C6A C5A 1.405(13) . ?
C13A H13A 0.9500 . ?
C13A C14A 1.364(15) . ?
C8A H8A 0.9500 . ?
C15A H15A 0.9500 . ?
C15A C14A 1.412(16) . ?
C26B C18B 1.464(13) . ?
C26B C25B 1.423(12) . ?
C23B H23B 0.9500 . ?
C19B C18B 1.416(11) . ?
C4B H4B 0.9500 . ?
C4B C3B 1.375(12) . ?
C3B H3B 0.9500 . ?
C3B C2B 1.411(13) . ?
F2I B1I 1.373(19) . ?
C6B C7B 1.416(13) . ?
C16B C15B 1.370(12) . ?
C15B H15B 0.9500 . ?
C15B C14B 1.406(16) . ?
C7B H7B 0.9500 . ?
C7B C2B 1.358(15) . ?
C7A H7A 0.9500 . ?
C7A C2A 1.377(16) . ?
C29B H29A 0.9900 . ?
C29B H29B 0.9900 . ?
C29B C30B 1.519(13) . ?
C30A H30C 0.9900 . ?
C30A H30D 0.9900 . ?
C30A C29A 1.520(13) . ?
C30A C31A 1.519(16) . ?
C14B H14B 0.9500 . ?
C2A C3A 1.403(13) . ?
C30B H30A 0.9900 . ?
C30B H30B 0.9900 . ?
C30B C31B 1.510(15) . ?
C9B H9B 0.9500 . ?
C31B H31A 0.9800 . ?
C31B H31B 0.9800 . ?
C31B H31C 0.9800 . ?
C23A H23A 0.9500 . ?
B1G F4G 1.36(2) . ?
B1G F5G 1.35(2) . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?
C4A H4A 0.9500 . ?
C4A C3A 1.369(13) . ?
C4A C5A 1.406(14) . ?
C3A H3A 0.9500 . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C14A H14A 0.9500 . ?
C28B H28A 0.9800 . ?
C28B H28B 0.9800 . ?
C28B H28C 0.9800 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C0BA H0BA 0.9900 . ?
C0BA H0BB 0.9900 . ?
C0BA Cl0B 1.753(17) . ?
B1I F5I 1.38(2) . ?
B1I F3I 1.379(19) . ?
B1I F4I 1.40(2) . ?
F3F B1F 1.35(2) . ?
F4F B1F 1.34(2) . ?
B1F F2F 1.35(2) . ?
B1F F5F 1.33(2) . ?
F3H B1H 1.38(4) . ?
F2H B1H 1.38(4) . ?
B1H F5H 1.38(4) . ?
B1H F4H 1.38(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
Br1A C2A C3A C4A 176.8(7) . . . . ?
O20B C21B C22B C23B -176.5(8) . . . . ?
O20B C21B C26B C18B -3.0(12) . . . . ?
O20B C21B C26B C25B 171.6(8) . . . . ?
O20B C16B C15B C14B -178.0(8) . . . . ?
O27A C25A C24A C23A -176.1(9) . . . . ?
C5B C19B C18B C17B -150.3(8) . . . . ?
C5B C19B C18B C26B 29.1(13) . . . . ?
C5B C4B C3B C2B 1.2(12) . . . . ?
C5B C6B C7B C2B 3.0(13) . . . . ?
O20A C21A C22A C23A 176.9(9) . . . . ?
O20A C16A C15A C14A 178.8(8) . . . . ?
N11A C10A C19A C18A 12.8(12) . . . . ?
N11A C10A C19A C5A -165.4(8) . . . . ?
N11A C10A C9A C8A 172.1(9) . . . . ?
N11A C12A C13A C14A 178.4(9) . . . . ?
C17A C12A C13A C14A 0.1(14) . . . . ?
C17A C16A C15A C14A 2.1(14) . . . . ?
N11B C12B C13B C14B -179.9(8) . . . . ?
N11B C12B C17B C16B 177.5(7) . . . . ?
N11B C12B C17B C18B -5.6(11) . . . . ?
N11B C10B C19B C5B 163.9(8) . . . . ?
N11B C10B C19B C18B -12.5(12) . . . . ?
N11B C10B C9B C8B -169.5(9) . . . . ?
N11B C29B C30B C31B -178.1(8) . . . . ?
C21B O20B C16B C17B 16.2(11) . . . . ?
C21B O20B C16B C15B -167.1(8) . . . . ?
C21B C22B C23B C24B 1.9(14) . . . . ?
C21B C26B C18B C17B 20.2(11) . . . . ?
C21B C26B C18B C19B -159.2(8) . . . . ?
C21B C26B C25B O27B -169.5(8) . . . . ?
C21B C26B C25B C24B 8.2(12) . . . . ?
C12B N11B C10B C19B -11.1(13) . . . . ?
C12B N11B C10B C9B 169.1(8) . . . . ?
C12B N11B C29B C30B -92.9(10) . . . . ?
C12B C13B C14B C15B 2.6(14) . . . . ?
C12B C17B C16B O20B 179.1(7) . . . . ?
C12B C17B C16B C15B 2.5(12) . . . . ?
C12B C17B C18B C26B 163.2(7) . . . . ?
C12B C17B C18B C19B -17.3(11) . . . . ?
C26A C21A C22A C23A -5.0(14) . . . . ?
C26A C25A C24A C23A 2.1(14) . . . . ?
C21A O20A C16A C17A -15.1(12) . . . . ?
C21A O20A C16A C15A 168.1(8) . . . . ?
C21A C26A C25A O27A 170.6(8) . . . . ?
C21A C26A C25A C24A -7.7(13) . . . . ?
C21A C26A C18A C17A -19.2(11) . . . . ?
C21A C26A C18A C19A 160.5(9) . . . . ?
C21A C22A C23A C24A -1.2(16) . . . . ?
C10A N11A C12A C17A -20.7(12) . . . . ?
C10A N11A C12A C13A 161.1(9) . . . . ?
C10A N11A C29A C30A -86.4(11) . . . . ?
C10A C19A C18A C17A -25.9(11) . . . . ?
C10A C19A C18A C26A 154.4(8) . . . . ?
C10A C19A C5A C6A -11.9(12) . . . . ?
C10A C19A C5A C4A 161.2(8) . . . . ?
C10A C9A C8A C6A -2.0(16) . . . . ?
C22B C21B C26B C18B 175.8(8) . . . . ?
C22B C21B C26B C25B -9.6(13) . . . . ?
C19A C10A C9A C8A -7.8(14) . . . . ?
C10B N11B C12B C13B -161.4(8) . . . . ?
C10B N11B C12B C17B 20.0(12) . . . . ?
C10B N11B C29B C30B 84.8(11) . . . . ?
C10B C19B C18B C17B 25.9(11) . . . . ?
C10B C19B C18B C26B -154.7(8) . . . . ?
C12A N11A C10A C19A 11.3(13) . . . . ?
C12A N11A C10A C9A -168.5(8) . . . . ?
C12A N11A C29A C30A 91.7(10) . . . . ?
C12A C17A C16A O20A -179.8(8) . . . . ?
C12A C17A C16A C15A -3.3(13) . . . . ?
C12A C17A C18A C26A -163.3(8) . . . . ?
C12A C17A C18A C19A 16.9(12) . . . . ?
C12A C13A C14A C15A -1.4(15) . . . . ?
C13B C12B C17B C16B -1.2(12) . . . . ?
C13B C12B C17B C18B 175.7(8) . . . . ?
C16A O20A C21A C26A 14.9(12) . . . . ?
C16A O20A C21A C22A -167.0(8) . . . . ?
C16A C17A C12A N11A -176.3(8) . . . . ?
C16A C17A C12A C13A 2.1(12) . . . . ?
C16A C17A C18A C26A 19.3(11) . . . . ?
C16A C17A C18A C19A -160.5(8) . . . . ?
C16A C15A C14A C13A 0.3(15) . . . . ?
C8B C6B C7B C2B -174.0(8) . . . . ?
C25A C26A C21A O20A -172.7(8) . . . . ?
C25A C26A C21A C22A 9.3(13) . . . . ?
C25A C26A C18A C17A 155.8(8) . . . . ?
C25A C26A C18A C19A -24.4(14) . . . . ?
C25A C24A C23A C22A 2.7(16) . . . . ?
C17B C12B C13B C14B -1.3(13) . . . . ?
C17B C16B C15B C14B -1.2(13) . . . . ?
C9A C10A C19A C18A -167.3(8) . . . . ?
C9A C10A C19A C5A 14.5(12) . . . . ?
C6A C7A C2A Br1A -175.3(7) . . . . ?
C6A C7A C2A C3A -1.2(14) . . . . ?
C8A C6A C7A C2A 172.7(9) . . . . ?
C8A C6A C5A C19A 2.5(13) . . . . ?
C8A C6A C5A C4A -170.9(9) . . . . ?
C18A C17A C12A N11A 6.3(12) . . . . ?
C18A C17A C12A C13A -175.4(8) . . . . ?
C18A C17A C16A O20A -2.4(13) . . . . ?
C18A C17A C16A C15A 174.2(9) . . . . ?
C18A C26A C21A O20A 2.8(12) . . . . ?
C18A C26A C21A C22A -175.1(8) . . . . ?
C18A C26A C25A O27A -4.6(13) . . . . ?
C18A C26A C25A C24A 177.1(9) . . . . ?
C18A C19A C5A C6A 170.1(8) . . . . ?
C18A C19A C5A C4A -16.8(13) . . . . ?
C26B C21B C22B C23B 4.7(14) . . . . ?
C23B C24B C25B O27B 175.2(9) . . . . ?
C23B C24B C25B C26B -2.3(14) . . . . ?
C19B C5B C4B C3B 173.8(8) . . . . ?
C19B C5B C6B C8B 0.8(12) . . . . ?
C19B C5B C6B C7B -176.2(8) . . . . ?
C19B C10B C9B C8B 10.7(14) . . . . ?
C4B C5B C19B C10B -162.3(8) . . . . ?
C4B C5B C19B C18B 13.9(13) . . . . ?
C4B C5B C6B C8B 173.9(8) . . . . ?
C4B C5B C6B C7B -3.1(12) . . . . ?
C4B C3B C2B Br1B -179.1(6) . . . . ?
C4B C3B C2B C7B -1.4(13) . . . . ?
C6B C5B C19B C10B 10.5(11) . . . . ?
C6B C5B C19B C18B -173.4(8) . . . . ?
C6B C5B C4B C3B 1.0(12) . . . . ?
C6B C8B C9B C10B 1.0(16) . . . . ?
C6B C7B C2B Br1B 177.0(6) . . . . ?
C6B C7B C2B C3B -0.7(13) . . . . ?
C16B O20B C21B C22B 165.5(8) . . . . ?
C16B O20B C21B C26B -15.6(12) . . . . ?
C16B C17B C18B C26B -20.0(11) . . . . ?
C16B C17B C18B C19B 159.5(8) . . . . ?
C16B C15B C14B C13B -1.4(14) . . . . ?
C18B C17B C16B O20B 2.2(12) . . . . ?
C18B C17B C16B C15B -174.4(8) . . . . ?
C18B C26B C25B O27B 4.6(13) . . . . ?
C18B C26B C25B C24B -177.7(8) . . . . ?
C7A C6A C8A C9A -170.4(10) . . . . ?
C7A C6A C5A C19A 177.5(8) . . . . ?
C7A C6A C5A C4A 4.1(13) . . . . ?
C7A C2A C3A C4A 2.8(13) . . . . ?
C29B N11B C12B C13B 16.4(12) . . . . ?
C29B N11B C12B C17B -162.2(7) . . . . ?
C29B N11B C10B C19B 171.2(8) . . . . ?
C29B N11B C10B C9B -8.6(13) . . . . ?
C9B C10B C19B C5B -16.3(12) . . . . ?
C9B C10B C19B C18B 167.3(8) . . . . ?
C9B C8B C6B C5B -6.8(14) . . . . ?
C9B C8B C6B C7B 170.2(9) . . . . ?
C25B C24B C23B C22B -3.0(15) . . . . ?
C25B C26B C18B C17B -153.8(8) . . . . ?
C25B C26B C18B C19B 26.8(14) . . . . ?
C28A O27A C25A C26A 167.6(9) . . . . ?
C28A O27A C25A C24A -14.2(13) . . . . ?
C3A C4A C5A C19A -175.7(8) . . . . ?
C3A C4A C5A C6A -2.6(13) . . . . ?
C29A N11A C10A C19A -170.7(8) . . . . ?
C29A N11A C10A C9A 9.5(13) . . . . ?
C29A N11A C12A C17A 161.3(8) . . . . ?
C29A N11A C12A C13A -17.0(13) . . . . ?
C28B O27B C25B C24B -3.4(14) . . . . ?
C28B O27B C25B C26B 174.2(9) . . . . ?
C31A C30A C29A N11A -174.7(9) . . . . ?
C5A C19A C18A C17A 152.2(8) . . . . ?
C5A C19A C18A C26A -27.5(14) . . . . ?
C5A C6A C8A C9A 4.6(15) . . . . ?
C5A C6A C7A C2A -2.3(13) . . . . ?
C5A C4A C3A C2A -0.9(14) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6504(15)
2 0.3496(15)
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6389 10987 5784
2 0.3611 10946 5784
