# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   13.07527(8)
_cell_length_b                   16.18867(10)
_cell_length_c                   19.01027(12)
_cell_angle_alpha                90
_cell_angle_beta                 100.1002(6)
_cell_angle_gamma                90
_cell_volume                     3961.57(4)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.3331 0.5567 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720
0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0727 0.0534 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C48 H30 F6 O4 
# Dc =      1.32 Fooo =   1616.00 Mu =      8.62 M =    392.38
# Found Formula = C48 H30 F6 O4 
# Dc =      1.32 FOOO =   1616.00 Mu =      8.62 M =    392.38

_chemical_formula_sum            'C48 H30 F6 O4'
_chemical_formula_moiety         'C48 H30 F6 O4'
_chemical_compound_source        ?
_chemical_formula_weight         784.75


_cell_measurement_reflns_used    26323
_cell_measurement_theta_min      4
_cell_measurement_theta_max      70
_cell_measurement_temperature    105

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.250

_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    0.862

# Sheldrick geometric approximatio 0.88 0.88 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, acta cryst. (1995), a51, 33-38'
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.88
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      105
_diffrn_reflns_number            35692
_reflns_number_total             3771
_diffrn_reflns_av_R_equivalents  0.0213
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3771 
# Theoretical number of reflections is about 7531 


_diffrn_reflns_theta_min         4.388
_diffrn_reflns_theta_max         70.120
_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        70.120
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.21
_refine_diff_density_max         0.61


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     0
_refine_ls_number_parameters     262
_oxford_refine_ls_R_factor_ref   0.0485
_refine_ls_wR_factor_ref         0.0645
_refine_ls_goodness_of_fit_ref   0.9834
_refine_ls_shift/su_max          0.0004958
_refine_ls_shift/su_mean         0.0000492


# The values computed from all data 
_oxford_reflns_number_all        3754
_refine_ls_R_factor_all          0.0506
_refine_ls_wR_factor_all         0.0656

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3599
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_gt          0.0647

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 11.7 9.83 9.56 2.38 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
F1 F 0.43152(7) 0.59853(5) 0.63780(5) 0.0434 1.0000 Uani . . . . . .
F2 F 0.39843(8) 0.53138(6) 0.53901(5) 0.0479 1.0000 Uani . . . . . .
F3 F 0.31370(7) 0.50467(5) 0.62349(5) 0.0409 1.0000 Uani . . . . . .
C1 C 0.49615(10) 0.45415(8) 0.71831(7) 0.0264 1.0000 Uani . . . . . .
C2 C 0.49008(10) 0.45922(8) 0.63972(7) 0.0261 1.0000 Uani . . . . . .
C3 C 0.46115(10) 0.37908(7) 0.60532(6) 0.0257 1.0000 Uani . . . . . .
C4 C 0.43707(9) 0.31523(7) 0.57520(6) 0.0238 1.0000 Uani . . . . . .
C5 C 0.40795(9) 0.23960(7) 0.53786(7) 0.0225 1.0000 Uani . . . . . .
C6 C 0.42131(9) 0.16826(7) 0.57536(6) 0.0230 1.0000 Uani . . . . . .
C7 C 0.43377(9) 0.10150(7) 0.60781(6) 0.0223 1.0000 Uani . . . . . .
C8 C 0.44709(9) 0.02871(7) 0.64356(6) 0.0210 1.0000 Uani . . . . . .
C9 C 0.48474(9) 0.03026(7) 0.71830(7) 0.0221 1.0000 Uani . . . . . .
C57 C 0.33726(11) 0.16841(8) 0.42341(7) 0.0314 1.0000 Uani . . . . . .
C56 C 0.29640(12) 0.16946(9) 0.35162(7) 0.0345 1.0000 Uani . . . . . .
C21 C 0.40650(11) 0.52498(8) 0.60903(8) 0.0311 1.0000 Uani . . . . . .
C22 C 0.66937(12) 0.43933(10) 0.63982(9) 0.0421 1.0000 Uani . . . . . .
C51 C 0.36605(9) 0.24194(8) 0.46095(7) 0.0233 1.0000 Uani . . . . . .
C52 C 0.35387(10) 0.31613(8) 0.42323(7) 0.0282 1.0000 Uani . . . . . .
C53 C 0.31146(11) 0.31770(9) 0.35064(7) 0.0319 1.0000 Uani . . . . . .
C54 C 0.28129(10) 0.24453(9) 0.31515(7) 0.0294 1.0000 Uani . . . . . .
C55 C 0.20020(16) 0.31199(12) 0.20849(8) 0.0526 1.0000 Uani . . . . . .
C81 C 0.42209(9) -0.05183(7) 0.60786(6) 0.0220 1.0000 Uani . . . . . .
C82 C 0.39330(10) -0.05719(8) 0.53389(7) 0.0296 1.0000 Uani . . . . . .
C83 C 0.36729(11) -0.13270(10) 0.50141(8) 0.0363 1.0000 Uani . . . . . .
C84 C 0.37117(10) -0.20433(9) 0.54167(8) 0.0352 1.0000 Uani . . . . . .
C85 C 0.39867(12) -0.19982(9) 0.61530(9) 0.0378 1.0000 Uani . . . . . .
C86 C 0.42333(11) -0.12413(8) 0.64823(7) 0.0316 1.0000 Uani . . . . . .
O1 O 0.58189(7) 0.49208(6) 0.62205(5) 0.0321 1.0000 Uani . . . . . .
O2 O 0.23675(9) 0.23796(7) 0.24475(5) 0.0394 1.0000 Uani . . . . . .
H571 H 0.3450 0.1169 0.4476 0.0395 1.0000 Uiso R . . . . .
H561 H 0.2783 0.1205 0.3270 0.0412 1.0000 Uiso R . . . . .
H222 H 0.7267 0.4698 0.6277 0.0630 1.0000 Uiso R . . . . .
H221 H 0.6816 0.4278 0.6886 0.0632 1.0000 Uiso R . . . . .
H223 H 0.6605 0.3895 0.6122 0.0628 1.0000 Uiso R . . . . .
H521 H 0.3742 0.3646 0.4472 0.0335 1.0000 Uiso R . . . . .
H531 H 0.3044 0.3686 0.3262 0.0397 1.0000 Uiso R . . . . .
H551 H 0.1637 0.2961 0.1619 0.0783 1.0000 Uiso R . . . . .
H553 H 0.2591 0.3473 0.2043 0.0773 1.0000 Uiso R . . . . .
H552 H 0.1535 0.3406 0.2346 0.0784 1.0000 Uiso R . . . . .
H821 H 0.3930 -0.0099 0.5051 0.0366 1.0000 Uiso R . . . . .
H831 H 0.3473 -0.1352 0.4509 0.0443 1.0000 Uiso R . . . . .
H841 H 0.3555 -0.2564 0.5204 0.0425 1.0000 Uiso R . . . . .
H851 H 0.3996 -0.2481 0.6435 0.0448 1.0000 Uiso R . . . . .
H861 H 0.4406 -0.1210 0.6981 0.0395 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F1 . C21 . 1.3272(17) yes
F2 . C21 . 1.3207(17) yes
F3 . C21 . 1.3315(17) yes
C1 . C1 6_656 1.191(3) yes
C1 . C2 . 1.4846(17) yes
C2 . C3 . 1.4720(17) yes
C2 . C21 . 1.5635(18) yes
C2 . O1 . 1.4065(15) yes
C3 . C4 . 1.1967(18) yes
C4 . C5 . 1.4330(17) yes
C5 . C6 . 1.3523(17) yes
C5 . C51 . 1.4692(17) yes
C6 . C7 . 1.2409(18) yes
C7 . C8 . 1.3561(17) yes
C8 . C9 . 1.4201(16) yes
C8 . C81 . 1.4796(16) yes
C9 . C9 6_656 1.201(3) yes
C57 . C56 . 1.3757(19) yes
C57 . C51 . 1.4049(18) yes
C57 . H571 . 0.948 no
C56 . C54 . 1.3960(19) yes
C56 . H561 . 0.929 no
C22 . O1 . 1.4200(18) yes
C22 . H222 . 0.958 no
C22 . H221 . 0.932 no
C22 . H223 . 0.958 no
C51 . C52 . 1.3935(17) yes
C52 . C53 . 1.3943(19) yes
C52 . H521 . 0.923 no
C53 . C54 . 1.386(2) yes
C53 . H531 . 0.942 no
C54 . O2 . 1.3669(17) yes
C55 . O2 . 1.4228(19) yes
C55 . H551 . 0.964 no
C55 . H553 . 0.973 no
C55 . H552 . 0.970 no
C81 . C82 . 1.3932(17) yes
C81 . C86 . 1.3982(18) yes
C82 . C83 . 1.3848(19) yes
C82 . H821 . 0.941 no
C83 . C84 . 1.386(2) yes
C83 . H831 . 0.951 no
C84 . C85 . 1.385(2) yes
C84 . H841 . 0.942 no
C85 . C86 . 1.3879(19) yes
C85 . H851 . 0.947 no
C86 . H861 . 0.937 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 6_656 C1 . C2 . 176.38(10) yes
C1 . C2 . C3 . 111.26(10) yes
C1 . C2 . C21 . 108.89(10) yes
C3 . C2 . C21 . 109.02(11) yes
C1 . C2 . O1 . 111.35(10) yes
C3 . C2 . O1 . 113.02(10) yes
C21 . C2 . O1 . 102.90(10) yes
C2 . C3 . C4 . 177.82(12) yes
C3 . C4 . C5 . 178.90(12) yes
C4 . C5 . C6 . 118.04(11) yes
C4 . C5 . C51 . 119.42(10) yes
C6 . C5 . C51 . 122.54(11) yes
C5 . C6 . C7 . 177.99(12) yes
C6 . C7 . C8 . 179.67(12) yes
C7 . C8 . C9 . 118.53(10) yes
C7 . C8 . C81 . 122.49(10) yes
C9 . C8 . C81 . 118.97(10) yes
C8 . C9 . C9 6_656 178.67(12) yes
C56 . C57 . C51 . 121.08(12) yes
C56 . C57 . H571 . 118.8 no
C51 . C57 . H571 . 120.1 no
C57 . C56 . C54 . 120.00(13) yes
C57 . C56 . H561 . 120.6 no
C54 . C56 . H561 . 119.4 no
C2 . C21 . F3 . 110.95(10) yes
C2 . C21 . F1 . 110.58(11) yes
F3 . C21 . F1 . 107.70(11) yes
C2 . C21 . F2 . 110.89(11) yes
F3 . C21 . F2 . 108.23(12) yes
F1 . C21 . F2 . 108.38(11) yes
O1 . C22 . H222 . 105.4 no
O1 . C22 . H221 . 110.3 no
H222 . C22 . H221 . 109.6 no
O1 . C22 . H223 . 111.1 no
H222 . C22 . H223 . 109.0 no
H221 . C22 . H223 . 111.1 no
C5 . C51 . C57 . 120.23(11) yes
C5 . C51 . C52 . 121.56(11) yes
C57 . C51 . C52 . 118.20(12) yes
C51 . C52 . C53 . 120.98(12) yes
C51 . C52 . H521 . 118.8 no
C53 . C52 . H521 . 120.3 no
C52 . C53 . C54 . 119.74(12) yes
C52 . C53 . H531 . 119.4 no
C54 . C53 . H531 . 120.8 no
C56 . C54 . C53 . 119.94(12) yes
C56 . C54 . O2 . 114.67(12) yes
C53 . C54 . O2 . 125.40(12) yes
O2 . C55 . H551 . 106.8 no
O2 . C55 . H553 . 109.4 no
H551 . C55 . H553 . 110.7 no
O2 . C55 . H552 . 110.0 no
H551 . C55 . H552 . 110.1 no
H553 . C55 . H552 . 109.8 no
C8 . C81 . C82 . 121.11(11) yes
C8 . C81 . C86 . 120.36(11) yes
C82 . C81 . C86 . 118.49(11) yes
C81 . C82 . C83 . 120.45(13) yes
C81 . C82 . H821 . 120.6 no
C83 . C82 . H821 . 118.9 no
C82 . C83 . C84 . 120.68(13) yes
C82 . C83 . H831 . 119.4 no
C84 . C83 . H831 . 120.0 no
C83 . C84 . C85 . 119.48(12) yes
C83 . C84 . H841 . 121.8 no
C85 . C84 . H841 . 118.7 no
C84 . C85 . C86 . 120.07(13) yes
C84 . C85 . H851 . 120.3 no
C86 . C85 . H851 . 119.6 no
C81 . C86 . C85 . 120.80(13) yes
C81 . C86 . H861 . 119.2 no
C85 . C86 . H861 . 120.0 no
C22 . O1 . C2 . 113.66(11) yes
C55 . O2 . C54 . 117.26(12) yes
_database_code_depnum_ccdc_archive 'CCDC 1003439'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H28 Cl2 F6 O2'
_chemical_formula_weight         809.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5119(17)
_cell_length_b                   12.6648(17)
_cell_length_c                   14.9565(19)
_cell_angle_alpha                70.805(5)
_cell_angle_beta                 66.621(5)
_cell_angle_gamma                67.665(5)
_cell_volume                     1967.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2560
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      21.03

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9550
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28934
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1211
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         5.12
_diffrn_reflns_theta_max         25.68
_reflns_number_total             7350
_reflns_number_gt                3141
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0870P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7350
_refine_ls_number_parameters     669
_refine_ls_number_restraints     489
_refine_ls_R_factor_all          0.1842
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1983
_refine_ls_wR_factor_gt          0.1536
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.2433(3) 0.4427(4) -0.0014(3) 0.0497(10) Uani 1 1 d D . .
C18 C 0.1054(4) 0.6131(3) 0.0670(3) 0.0482(10) Uani 1 1 d D . .
C1 C 0.2101(4) 0.5713(3) -0.0168(3) 0.0429(10) Uani 0.877(2) 1 d PDU A 1
C19 C 0.3168(5) 0.6069(8) -0.0257(5) 0.0526(15) Uani 0.877(2) 1 d PDU A 1
F1 F 0.3541(2) 0.5589(2) 0.05353(19) 0.0627(7) Uani 0.877(2) 1 d PDU A 1
F2 F 0.2924(2) 0.7206(2) -0.0415(2) 0.0714(8) Uani 0.877(2) 1 d PDU A 1
F3 F 0.4140(2) 0.5724(3) -0.1036(2) 0.0721(8) Uani 0.877(2) 1 d PDU A 1
O1 O 0.1889(3) 0.6257(2) -0.10984(19) 0.0492(8) Uani 0.877(2) 1 d PDU A 1
C20 C 0.0897(5) 0.6065(5) -0.1223(4) 0.0663(14) Uani 0.877(2) 1 d PDU A 1
H20A H 0.1040 0.5226 -0.1133 0.099 Uiso 0.877(2) 1 calc PR A 1
H20B H 0.0840 0.6461 -0.1893 0.099 Uiso 0.877(2) 1 calc PR A 1
H20C H 0.0135 0.6377 -0.0726 0.099 Uiso 0.877(2) 1 calc PR A 1
C1' C 0.1709(17) 0.5687(15) -0.0276(12) 0.047(3) Uani 0.123(2) 1 d PDU A 2
C19' C 0.102(2) 0.604(2) -0.1005(16) 0.053(4) Uani 0.123(2) 1 d PDU A 2
F1' F 0.0475(16) 0.7190(14) -0.1240(13) 0.073(5) Uani 0.123(2) 1 d PDU A 2
F2' F 0.1721(17) 0.5682(16) -0.1854(12) 0.068(4) Uani 0.123(2) 1 d PDU A 2
F3' F 0.0073(15) 0.5585(15) -0.0680(14) 0.066(4) Uani 0.123(2) 1 d PDU A 2
O1' O 0.2555(18) 0.6333(16) -0.0850(15) 0.052(3) Uani 0.123(2) 1 d PDU A 2
C20' C 0.349(5) 0.609(7) -0.040(5) 0.059(5) Uani 0.123(2) 1 d PDU A 2
H20D H 0.3109 0.6300 0.0249 0.089 Uiso 0.123(2) 1 calc PR A 2
H20E H 0.4058 0.6545 -0.0837 0.089 Uiso 0.123(2) 1 calc PR A 2
H20F H 0.3931 0.5255 -0.0325 0.089 Uiso 0.123(2) 1 calc PR A 2
C3 C 0.2778(3) 0.3407(4) 0.0098(3) 0.0484(10) Uani 1 1 d D A .
C5 C 0.2578(4) 0.1491(3) 0.1122(3) 0.0476(10) Uani 1 1 d D . .
C4 C 0.3263(4) 0.2121(4) 0.0161(3) 0.0501(11) Uani 0.877(2) 1 d PDU A 1
C21 C 0.3089(7) 0.1847(5) -0.0686(4) 0.0693(15) Uani 0.877(2) 1 d PDU A 1
F4 F 0.1951(4) 0.2182(3) -0.0616(3) 0.0983(11) Uani 0.877(2) 1 d PDU A 1
F5 F 0.3672(4) 0.2448(3) -0.1573(2) 0.1111(13) Uani 0.877(2) 1 d PDU A 1
F6 F 0.3565(3) 0.0759(3) -0.0728(2) 0.1036(12) Uani 0.877(2) 1 d PDU A 1
O2 O 0.4532(3) 0.1720(3) -0.0011(2) 0.0659(9) Uani 0.877(2) 1 d PDU A 1
C22 C 0.4895(5) 0.1837(6) 0.0739(5) 0.0867(17) Uani 0.877(2) 1 d PDU A 1
H22A H 0.4627 0.2662 0.0773 0.130 Uiso 0.877(2) 1 calc PR A 1
H22B H 0.5782 0.1545 0.0572 0.130 Uiso 0.877(2) 1 calc PR A 1
H22C H 0.4524 0.1385 0.1386 0.130 Uiso 0.877(2) 1 calc PR A 1
C4' C 0.3354(18) 0.2162(15) 0.0346(16) 0.063(3) Uani 0.123(2) 1 d PDU A 2
C21' C 0.440(2) 0.203(2) 0.0685(18) 0.076(4) Uani 0.123(2) 1 d PDU A 2
F4' F 0.4958(18) 0.0945(17) 0.0885(18) 0.098(6) Uani 0.123(2) 1 d PDU A 2
F5' F 0.3979(18) 0.2489(17) 0.1521(14) 0.085(5) Uani 0.123(2) 1 d PDU A 2
F6' F 0.5063(17) 0.266(2) 0.0026(17) 0.105(6) Uani 0.123(2) 1 d PDU A 2
O2' O 0.374(2) 0.167(2) -0.0475(16) 0.073(3) Uani 0.123(2) 1 d PDU A 2
C22' C 0.290(5) 0.222(5) -0.104(4) 0.086(6) Uani 0.123(2) 1 d PDU A 2
H22D H 0.2433 0.1699 -0.0938 0.129 Uiso 0.123(2) 1 calc PR A 2
H22E H 0.3352 0.2405 -0.1753 0.129 Uiso 0.123(2) 1 calc PR A 2
H22F H 0.2342 0.2948 -0.0829 0.129 Uiso 0.123(2) 1 calc PR A 2
C6 C 0.2024(3) 0.0929(3) 0.1817(3) 0.0449(9) Uani 1 1 d . A .
C7 C 0.1342(3) 0.0201(3) 0.2604(3) 0.0444(9) Uani 1 1 d . . .
C8 C 0.0322(4) 0.0720(3) 0.3258(3) 0.0452(9) Uani 1 1 d . A .
C9 C -0.0641(4) 0.1208(3) 0.3845(3) 0.0470(10) Uani 1 1 d . . .
C10 C -0.1715(3) 0.1700(3) 0.4482(3) 0.0436(9) Uani 1 1 d . A .
C11 C -0.2034(3) 0.2921(4) 0.4423(2) 0.0470(10) Uani 1 1 d . . .
C12 C -0.2326(3) 0.3944(4) 0.4392(2) 0.0476(10) Uani 1 1 d . A .
C13 C -0.2663(3) 0.5157(3) 0.4360(3) 0.0467(10) Uani 1 1 d . . .
C14 C -0.1987(4) 0.5794(3) 0.3597(3) 0.0485(10) Uani 1 1 d . A .
C15 C -0.1362(3) 0.6381(3) 0.2894(3) 0.0487(10) Uani 1 1 d . . .
C16 C -0.0692(3) 0.7044(3) 0.2135(3) 0.0445(9) Uani 1 1 d . A .
C17 C 0.0269(4) 0.6512(3) 0.1357(3) 0.0456(10) Uani 1 1 d . A .
C23 C 0.1740(3) -0.1056(3) 0.2632(3) 0.0435(9) Uani 1 1 d . A .
C24 C 0.2823(4) -0.1541(4) 0.1950(3) 0.0580(11) Uani 1 1 d . . .
H24 H 0.3310 -0.1060 0.1473 0.070 Uiso 1 1 calc R A .
C25 C 0.3189(4) -0.2718(4) 0.1965(3) 0.0713(13) Uani 1 1 d . A .
H25 H 0.3928 -0.3042 0.1495 0.086 Uiso 1 1 calc R . .
C26 C 0.2507(4) -0.3418(4) 0.2644(3) 0.0677(12) Uani 1 1 d . . .
H26 H 0.2769 -0.4229 0.2650 0.081 Uiso 1 1 calc R A .
C27 C 0.1433(4) -0.2950(4) 0.3326(3) 0.0635(12) Uani 1 1 d . A .
H27 H 0.0951 -0.3437 0.3798 0.076 Uiso 1 1 calc R . .
C28 C 0.1057(4) -0.1770(3) 0.3323(3) 0.0531(10) Uani 1 1 d . . .
H28 H 0.0323 -0.1453 0.3801 0.064 Uiso 1 1 calc R A .
C29 C -0.2546(3) 0.1026(3) 0.5191(3) 0.0454(9) Uani 1 1 d . . .
C30 C -0.2407(4) -0.0068(4) 0.5078(3) 0.0645(12) Uani 1 1 d . A .
H30 H -0.1740 -0.0399 0.4563 0.077 Uiso 1 1 calc R . .
C31 C -0.3221(5) -0.0674(4) 0.5703(4) 0.0779(14) Uani 1 1 d . . .
H31 H -0.3123 -0.1414 0.5606 0.094 Uiso 1 1 calc R A .
C32 C -0.4170(4) -0.0234(4) 0.6463(3) 0.0704(13) Uani 1 1 d . A .
H32 H -0.4735 -0.0660 0.6889 0.084 Uiso 1 1 calc R . .
C33 C -0.4301(4) 0.0821(4) 0.6605(3) 0.0745(14) Uani 1 1 d . . .
H33 H -0.4950 0.1128 0.7141 0.089 Uiso 1 1 calc R A .
C34 C -0.3486(4) 0.1452(4) 0.5967(3) 0.0608(12) Uani 1 1 d . A .
H34 H -0.3584 0.2188 0.6072 0.073 Uiso 1 1 calc R . .
C35 C -0.3715(3) 0.5674(3) 0.5141(3) 0.0460(10) Uani 1 1 d . A .
C36 C -0.4398(4) 0.5012(4) 0.5917(3) 0.0662(12) Uani 1 1 d . . .
H36 H -0.4191 0.4200 0.5946 0.079 Uiso 1 1 calc R A .
C37 C -0.5373(4) 0.5504(4) 0.6649(3) 0.0706(13) Uani 1 1 d . A .
H37 H -0.5829 0.5029 0.7178 0.085 Uiso 1 1 calc R . .
C38 C -0.5696(4) 0.6678(4) 0.6624(3) 0.0642(12) Uani 1 1 d . . .
H38 H -0.6361 0.7017 0.7136 0.077 Uiso 1 1 calc R A .
C39 C -0.5046(4) 0.7336(4) 0.5855(3) 0.0663(12) Uani 1 1 d . A .
H39 H -0.5274 0.8151 0.5821 0.080 Uiso 1 1 calc R . .
C40 C -0.4062(4) 0.6857(4) 0.5119(3) 0.0632(12) Uani 1 1 d . . .
H40 H -0.3617 0.7341 0.4591 0.076 Uiso 1 1 calc R A .
C41 C -0.0961(3) 0.8295(3) 0.2062(3) 0.0445(9) Uani 1 1 d . . .
C42 C -0.2013(4) 0.8896(4) 0.2682(3) 0.0640(12) Uani 1 1 d . A .
H42 H -0.2571 0.8492 0.3170 0.077 Uiso 1 1 calc R . .
C43 C -0.2260(4) 1.0071(4) 0.2599(4) 0.0781(14) Uani 1 1 d . . .
H43 H -0.2995 1.0477 0.3021 0.094 Uiso 1 1 calc R A .
C44 C -0.1458(5) 1.0664(4) 0.1914(3) 0.0663(12) Uani 1 1 d . A .
H44 H -0.1631 1.1476 0.1865 0.080 Uiso 1 1 calc R . .
C45 C -0.0407(4) 1.0081(4) 0.1302(3) 0.0615(12) Uani 1 1 d . . .
H45 H 0.0155 1.0487 0.0827 0.074 Uiso 1 1 calc R A .
C46 C -0.0159(4) 0.8907(3) 0.1369(3) 0.0525(10) Uani 1 1 d . A .
H46 H 0.0571 0.8511 0.0936 0.063 Uiso 1 1 calc R . .
C47 C 0.1271(12) 0.3422(13) 0.3337(11) 0.125(3) Uani 0.581(5) 1 d PDU B 1
H47A H 0.0645 0.3934 0.3012 0.150 Uiso 0.581(5) 1 calc PR B 1
H47B H 0.1248 0.2609 0.3478 0.150 Uiso 0.581(5) 1 calc PR B 1
Cl1 Cl 0.2681(4) 0.3528(2) 0.25276(17) 0.1283(19) Uani 0.581(5) 1 d PDU B 1
Cl2 Cl 0.0928(5) 0.3796(7) 0.4418(5) 0.130(2) Uani 0.581(5) 1 d PDU B 1
C47' C 0.0803(16) 0.3241(18) 0.3953(13) 0.107(3) Uani 0.419(5) 1 d PDU B 2
H47C H 0.1008 0.2379 0.4123 0.128 Uiso 0.419(5) 1 calc PR B 2
H47D H -0.0092 0.3554 0.4209 0.128 Uiso 0.419(5) 1 calc PR B 2
Cl1' Cl 0.1255(7) 0.3683(5) 0.2707(3) 0.150(3) Uani 0.419(5) 1 d PDU B 2
Cl2' Cl 0.1435(7) 0.3665(9) 0.4535(6) 0.108(2) Uani 0.419(5) 1 d PDU B 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 C3 1.172(5) . ?
C2 C1 1.481(6) . ?
C2 C1' 1.514(17) . ?
C18 C17 1.190(5) . ?
C18 C1 1.475(5) . ?
C18 C1' 1.498(17) . ?
C1 O1 1.416(5) . ?
C1 C19 1.510(7) . ?
C19 F2 1.312(10) . ?
C19 F1 1.319(7) . ?
C19 F3 1.354(8) . ?
O1 C20 1.442(6) . ?
C1' O1' 1.415(17) . ?
C1' C19' 1.503(18) . ?
C19' F2' 1.33(2) . ?
C19' F1' 1.348(19) . ?
C19' F3' 1.36(2) . ?
O1' C20' 1.45(2) . ?
C3 C4' 1.451(17) . ?
C3 C4 1.492(6) . ?
C5 C6 1.177(5) . ?
C5 C4' 1.448(17) . ?
C5 C4 1.492(6) . ?
C4 O2 1.412(5) . ?
C4 C21 1.528(9) . ?
C21 F6 1.289(6) . ?
C21 F4 1.293(8) . ?
C21 F5 1.364(7) . ?
O2 C22 1.432(7) . ?
C4' O2' 1.393(18) . ?
C4' C21' 1.513(19) . ?
C21' F6' 1.277(19) . ?
C21' F4' 1.282(19) . ?
C21' F5' 1.377(19) . ?
O2' C22' 1.44(2) . ?
C6 C7 1.432(5) . ?
C7 C8 1.346(5) . ?
C7 C23 1.467(5) . ?
C8 C9 1.247(5) . ?
C9 C10 1.357(5) . ?
C10 C11 1.423(5) . ?
C10 C29 1.462(5) . ?
C11 C12 1.196(5) . ?
C12 C13 1.419(5) . ?
C13 C14 1.347(5) . ?
C13 C35 1.467(5) . ?
C14 C15 1.243(5) . ?
C15 C16 1.360(5) . ?
C16 C17 1.430(5) . ?
C16 C41 1.464(5) . ?
C23 C28 1.375(5) . ?
C23 C24 1.392(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.357(5) . ?
C26 C27 1.379(6) . ?
C27 C28 1.384(5) . ?
C29 C34 1.367(5) . ?
C29 C30 1.388(5) . ?
C30 C31 1.366(5) . ?
C31 C32 1.361(6) . ?
C32 C33 1.361(6) . ?
C33 C34 1.390(5) . ?
C35 C36 1.378(5) . ?
C35 C40 1.385(5) . ?
C36 C37 1.374(5) . ?
C37 C38 1.376(6) . ?
C38 C39 1.350(5) . ?
C39 C40 1.376(5) . ?
C41 C42 1.381(5) . ?
C41 C46 1.385(5) . ?
C42 C43 1.374(5) . ?
C43 C44 1.368(6) . ?
C44 C45 1.365(6) . ?
C45 C46 1.376(5) . ?
C47 Cl2 1.679(12) . ?
C47 Cl1 1.725(15) . ?
C47' Cl1' 1.681(16) . ?
C47' Cl2' 1.687(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C1 175.2(4) . . ?
C3 C2 C1' 161.7(8) . . ?
C17 C18 C1 174.4(4) . . ?
C17 C18 C1' 162.3(8) . . ?
O1 C1 C18 112.4(3) . . ?
O1 C1 C2 110.5(3) . . ?
C18 C1 C2 110.6(3) . . ?
O1 C1 C19 103.9(4) . . ?
C18 C1 C19 109.3(4) . . ?
C2 C1 C19 109.9(4) . . ?
F2 C19 F1 108.6(6) . . ?
F2 C19 F3 106.3(5) . . ?
F1 C19 F3 105.9(5) . . ?
F2 C19 C1 112.1(5) . . ?
F1 C19 C1 112.6(5) . . ?
F3 C19 C1 110.9(6) . . ?
C1 O1 C20 115.9(3) . . ?
O1' C1' C18 105.2(14) . . ?
O1' C1' C19' 97.6(15) . . ?
C18 C1' C19' 117.3(14) . . ?
O1' C1' C2 107.1(14) . . ?
C18 C1' C2 107.6(10) . . ?
C19' C1' C2 119.9(14) . . ?
F2' C19' F1' 107.5(18) . . ?
F2' C19' F3' 104.4(17) . . ?
F1' C19' F3' 101.7(17) . . ?
F2' C19' C1' 112.3(16) . . ?
F1' C19' C1' 115.3(17) . . ?
F3' C19' C1' 114.5(18) . . ?
C1' O1' C20' 113(2) . . ?
C2 C3 C4' 168.1(10) . . ?
C2 C3 C4 175.7(4) . . ?
C6 C5 C4' 172.6(10) . . ?
C6 C5 C4 172.5(4) . . ?
O2 C4 C3 111.9(4) . . ?
O2 C4 C5 112.9(4) . . ?
C3 C4 C5 110.5(3) . . ?
O2 C4 C21 104.7(4) . . ?
C3 C4 C21 108.5(4) . . ?
C5 C4 C21 108.0(4) . . ?
F6 C21 F4 110.8(6) . . ?
F6 C21 F5 106.1(5) . . ?
F4 C21 F5 107.4(6) . . ?
F6 C21 C4 112.4(5) . . ?
F4 C21 C4 110.8(5) . . ?
F5 C21 C4 109.1(6) . . ?
C4 O2 C22 113.9(4) . . ?
O2' C4' C5 103.9(16) . . ?
O2' C4' C3 110.3(16) . . ?
C5 C4' C3 115.4(13) . . ?
O2' C4' C21' 112.6(19) . . ?
C5 C4' C21' 108.5(15) . . ?
C3 C4' C21' 106.2(14) . . ?
F6' C21' F4' 114(2) . . ?
F6' C21' F5' 104.0(19) . . ?
F4' C21' F5' 109(2) . . ?
F6' C21' C4' 109.4(18) . . ?
F4' C21' C4' 108.6(18) . . ?
F5' C21' C4' 111.1(18) . . ?
C4' O2' C22' 111(2) . . ?
C5 C6 C7 175.1(4) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C23 123.0(3) . . ?
C6 C7 C23 119.1(3) . . ?
C9 C8 C7 178.2(4) . . ?
C8 C9 C10 177.0(4) . . ?
C9 C10 C11 117.5(3) . . ?
C9 C10 C29 122.2(3) . . ?
C11 C10 C29 120.2(3) . . ?
C12 C11 C10 178.5(4) . . ?
C11 C12 C13 179.5(5) . . ?
C14 C13 C12 117.6(3) . . ?
C14 C13 C35 122.4(3) . . ?
C12 C13 C35 120.0(3) . . ?
C15 C14 C13 179.9(4) . . ?
C14 C15 C16 178.7(4) . . ?
C15 C16 C17 118.7(3) . . ?
C15 C16 C41 122.3(3) . . ?
C17 C16 C41 118.9(3) . . ?
C18 C17 C16 176.2(4) . . ?
C28 C23 C24 119.0(4) . . ?
C28 C23 C7 121.0(3) . . ?
C24 C23 C7 120.0(3) . . ?
C25 C24 C23 120.1(4) . . ?
C26 C25 C24 120.7(4) . . ?
C25 C26 C27 119.8(4) . . ?
C26 C27 C28 120.1(4) . . ?
C23 C28 C27 120.3(4) . . ?
C34 C29 C30 118.1(4) . . ?
C34 C29 C10 121.7(3) . . ?
C30 C29 C10 120.2(3) . . ?
C31 C30 C29 120.5(4) . . ?
C32 C31 C30 121.1(4) . . ?
C33 C32 C31 119.3(4) . . ?
C32 C33 C34 120.2(4) . . ?
C29 C34 C33 120.8(4) . . ?
C36 C35 C40 117.4(3) . . ?
C36 C35 C13 121.7(3) . . ?
C40 C35 C13 120.8(3) . . ?
C37 C36 C35 121.2(4) . . ?
C36 C37 C38 120.6(4) . . ?
C39 C38 C37 118.5(4) . . ?
C38 C39 C40 121.6(4) . . ?
C39 C40 C35 120.6(4) . . ?
C42 C41 C46 118.1(4) . . ?
C42 C41 C16 121.1(3) . . ?
C46 C41 C16 120.7(3) . . ?
C43 C42 C41 120.5(4) . . ?
C44 C43 C42 120.7(4) . . ?
C45 C44 C43 119.5(4) . . ?
C44 C45 C46 120.3(4) . . ?
C45 C46 C41 120.8(4) . . ?
Cl2 C47 Cl1 113.1(7) . . ?
Cl1' C47' Cl2' 113.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.047


#===END
_database_code_depnum_ccdc_archive 'CCDC 951896'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H25 Cl3 F12 O2'
_chemical_formula_weight         980.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.8182(16)
_cell_length_b                   35.815(5)
_cell_length_c                   9.7626(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.841(6)
_cell_angle_gamma                90.00
_cell_volume                     4476.4(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2244
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      19.94

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9434
_exptl_absorpt_correction_T_max  0.9883
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59064
_diffrn_reflns_av_R_equivalents  0.1994
_diffrn_reflns_av_sigmaI/netI    0.1503
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         24.71
_reflns_number_total             7551
_reflns_number_gt                3302
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0921P)²+5.9849P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7551
_refine_ls_number_parameters     653
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.2077
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.2414
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.8620(4) 0.04173(12) 1.1537(5) 0.0524(13) Uani 1 1 d . . .
O2 O 0.4946(3) 0.02854(12) 0.8506(5) 0.0510(12) Uani 1 1 d . . .
F1 F 0.7823(3) 0.05758(12) 1.3924(4) 0.0697(12) Uani 1 1 d . . .
F2 F 0.6812(3) 0.02287(12) 1.2691(4) 0.0747(13) Uani 1 1 d . . .
F3 F 0.6411(3) 0.07960(13) 1.2990(4) 0.0708(13) Uani 1 1 d . . .
F4 F 0.6675(3) -0.00588(11) 0.7736(4) 0.0704(12) Uani 1 1 d . . .
F5 F 0.7221(3) 0.04237(11) 0.6728(4) 0.0648(12) Uani 1 1 d . . .
F6 F 0.5776(4) 0.01772(12) 0.6051(4) 0.0769(13) Uani 1 1 d . . .
C1 C 0.7783(5) 0.06817(16) 1.1541(6) 0.0335(15) Uani 1 1 d . . .
C2 C 0.7073(4) 0.06466(15) 1.0301(6) 0.0318(14) Uani 1 1 d . . .
C3 C 0.6506(4) 0.05942(15) 0.9341(6) 0.0301(14) Uani 1 1 d . . .
C4 C 0.5781(5) 0.05122(17) 0.8138(6) 0.0356(15) Uani 1 1 d . . .
C5 C 0.5463(4) 0.08592(18) 0.7429(6) 0.0346(15) Uani 1 1 d . . .
C6 C 0.5172(5) 0.11372(18) 0.6829(6) 0.0349(15) Uani 1 1 d . . .
C7 C 0.4796(4) 0.14578(17) 0.6093(6) 0.0325(15) Uani 1 1 d . . .
C8 C 0.5079(4) 0.18047(17) 0.6562(6) 0.0300(14) Uani 1 1 d . . .
C9 C 0.5347(4) 0.21190(18) 0.6977(6) 0.0296(14) Uani 1 1 d . . .
C10 C 0.5625(4) 0.24669(16) 0.7349(6) 0.0288(14) Uani 1 1 d . . .
C11 C 0.6357(4) 0.25230(15) 0.8479(6) 0.0267(13) Uani 1 1 d . . .
C12 C 0.6977(4) 0.25781(15) 0.9405(6) 0.0281(14) Uani 1 1 d . . .
C13 C 0.7717(4) 0.26281(16) 1.0532(5) 0.0274(14) Uani 1 1 d . . .
C14 C 0.8184(4) 0.23098(17) 1.1070(6) 0.0292(14) Uani 1 1 d . . .
C15 C 0.8564(4) 0.20296(16) 1.1621(6) 0.0286(14) Uani 1 1 d . . .
C16 C 0.8947(4) 0.17280(15) 1.2302(6) 0.0269(14) Uani 1 1 d . . .
C17 C 0.8549(4) 0.13662(17) 1.1947(6) 0.0306(14) Uani 1 1 d . . .
C18 C 0.8187(5) 0.10674(18) 1.1736(6) 0.0349(15) Uani 1 1 d . . .
C19 C 0.7212(6) 0.05684(18) 1.2770(7) 0.0439(17) Uani 1 1 d . . .
C20 C 0.9264(6) 0.0468(2) 1.0377(9) 0.071(2) Uani 1 1 d . . .
H20A H 0.8916 0.0356 0.9559 0.106 Uiso 1 1 calc R . .
H20B H 0.9941 0.0346 1.0564 0.106 Uiso 1 1 calc R . .
H20C H 0.9371 0.0735 1.0220 0.106 Uiso 1 1 calc R . .
C21 C 0.6356(6) 0.02617(18) 0.7148(7) 0.0488(19) Uani 1 1 d . . .
C22 C 0.4257(5) 0.0479(2) 0.9385(8) 0.066(2) Uani 1 1 d . . .
H22A H 0.4670 0.0609 1.0110 0.099 Uiso 1 1 calc R . .
H22B H 0.3791 0.0299 0.9800 0.099 Uiso 1 1 calc R . .
H22C H 0.3841 0.0661 0.8845 0.099 Uiso 1 1 calc R . .
C23 C 0.4097(4) 0.14032(17) 0.4867(6) 0.0327(15) Uani 1 1 d . . .
C24 C 0.3615(5) 0.17039(19) 0.4185(7) 0.0449(17) Uani 1 1 d . . .
H24 H 0.3769 0.1950 0.4496 0.054 Uiso 1 1 calc R . .
C25 C 0.2927(5) 0.1656(2) 0.3085(7) 0.0469(18) Uani 1 1 d . . .
H25 H 0.2604 0.1865 0.2646 0.056 Uiso 1 1 calc R . .
C26 C 0.2705(5) 0.1297(2) 0.2615(6) 0.0431(17) Uani 1 1 d . A .
C27 C 0.3199(6) 0.0998(2) 0.3255(7) 0.058(2) Uani 1 1 d . . .
H27 H 0.3064 0.0753 0.2918 0.069 Uiso 1 1 calc R . .
C28 C 0.3878(5) 0.10461(19) 0.4360(7) 0.0511(19) Uani 1 1 d . . .
H28 H 0.4204 0.0835 0.4787 0.061 Uiso 1 1 calc R . .
C29 C 0.1944(6) 0.1232(3) 0.1428(8) 0.067(2) Uani 1 1 d D . .
F10 F 0.1446(13) 0.1548(3) 0.1022(17) 0.086(3) Uani 0.75(4) 1 d PDU A 1
F11 F 0.2383(10) 0.1103(6) 0.0325(13) 0.085(4) Uani 0.75(4) 1 d PDU A 1
F12 F 0.1164(14) 0.1004(7) 0.173(2) 0.097(5) Uani 0.75(4) 1 d PDU A 1
F10' F 0.107(4) 0.109(2) 0.189(7) 0.098(8) Uani 0.25(4) 1 d PDU A 2
F11' F 0.177(3) 0.1516(10) 0.060(3) 0.085(5) Uani 0.25(4) 1 d PDU A 2
F12' F 0.227(3) 0.0949(12) 0.065(4) 0.086(6) Uani 0.25(4) 1 d PDU A 2
C30 C 0.5213(4) 0.27974(15) 0.6581(6) 0.0277(14) Uani 1 1 d . . .
C31 C 0.5716(5) 0.31356(17) 0.6672(7) 0.0405(16) Uani 1 1 d . . .
H31 H 0.6317 0.3163 0.7271 0.049 Uiso 1 1 calc R . .
C32 C 0.5354(5) 0.34377(18) 0.5897(7) 0.0489(18) Uani 1 1 d . . .
H32 H 0.5708 0.3671 0.5966 0.059 Uiso 1 1 calc R . .
C33 C 0.4482(5) 0.33994(19) 0.5026(7) 0.0496(18) Uani 1 1 d . . .
H33 H 0.4240 0.3605 0.4484 0.059 Uiso 1 1 calc R . .
C34 C 0.3961(5) 0.30647(19) 0.4941(7) 0.0471(18) Uani 1 1 d . . .
H34 H 0.3347 0.3041 0.4363 0.056 Uiso 1 1 calc R . .
C35 C 0.4335(5) 0.27596(18) 0.5703(6) 0.0389(16) Uani 1 1 d . . .
H35 H 0.3988 0.2526 0.5621 0.047 Uiso 1 1 calc R . .
C36 C 0.7928(4) 0.30006(15) 1.1121(6) 0.0288(14) Uani 1 1 d . . .
C37 C 0.8488(4) 0.30375(16) 1.2363(6) 0.0343(15) Uani 1 1 d . . .
H37 H 0.8771 0.2823 1.2815 0.041 Uiso 1 1 calc R . .
C38 C 0.8637(5) 0.33866(17) 1.2948(7) 0.0450(17) Uani 1 1 d . . .
H38 H 0.9007 0.3411 1.3811 0.054 Uiso 1 1 calc R . .
C39 C 0.8251(5) 0.36967(18) 1.2284(8) 0.0480(18) Uani 1 1 d . . .
H39 H 0.8368 0.3937 1.2676 0.058 Uiso 1 1 calc R . .
C40 C 0.7695(5) 0.36627(17) 1.1053(7) 0.0420(16) Uani 1 1 d . . .
H40 H 0.7418 0.3879 1.0605 0.050 Uiso 1 1 calc R . .
C41 C 0.7535(4) 0.33187(16) 1.0467(6) 0.0341(15) Uani 1 1 d . . .
H41 H 0.7154 0.3298 0.9610 0.041 Uiso 1 1 calc R . .
C42 C 0.9715(4) 0.17759(16) 1.3479(6) 0.0277(14) Uani 1 1 d . . .
C43 C 0.9983(4) 0.14715(17) 1.4325(6) 0.0344(15) Uani 1 1 d . . .
H43 H 0.9706 0.1231 1.4111 0.041 Uiso 1 1 calc R . .
C44 C 1.0648(5) 0.15181(17) 1.5466(6) 0.0374(16) Uani 1 1 d . . .
H44 H 1.0819 0.1312 1.6049 0.045 Uiso 1 1 calc R . .
C45 C 1.1065(4) 0.18689(17) 1.5753(6) 0.0340(15) Uani 1 1 d . . .
C46 C 1.0822(5) 0.21692(17) 1.4918(7) 0.0406(16) Uani 1 1 d . . .
H46 H 1.1113 0.2408 1.5121 0.049 Uiso 1 1 calc R . .
C47 C 1.0152(4) 0.21201(16) 1.3785(6) 0.0336(15) Uani 1 1 d . . .
H47 H 0.9988 0.2327 1.3203 0.040 Uiso 1 1 calc R . .
C48 C 1.1733(5) 0.1923(2) 1.7035(7) 0.0492(18) Uani 1 1 d U . .
F7 F 1.2417(4) 0.21950(15) 1.6942(5) 0.1007(18) Uani 1 1 d U . .
F8 F 1.1208(3) 0.19937(14) 1.8122(4) 0.0796(15) Uani 1 1 d U . .
F9 F 1.2310(4) 0.16249(14) 1.7369(5) 0.0896(16) Uani 1 1 d U . .
C49 C 0.0961(5) 0.0342(2) 0.6534(8) 0.073(2) Uani 1 1 d DU . .
H49 H 0.1313 0.0094 0.6627 0.088 Uiso 1 1 calc R B 1
Cl1 Cl -0.0388(11) 0.0271(6) 0.6612(19) 0.106(5) Uani 0.277(12) 1 d PDU C 1
Cl2 Cl 0.1594(18) 0.0641(6) 0.761(2) 0.141(6) Uani 0.277(12) 1 d PDU C 1
Cl3 Cl 0.096(2) 0.0479(4) 0.4743(14) 0.141(5) Uani 0.277(12) 1 d PDU C 1
Cl1' Cl -0.0317(5) 0.0447(2) 0.6115(10) 0.122(3) Uani 0.723(12) 1 d PDU C 2
Cl2' Cl 0.1278(5) 0.05876(19) 0.8085(5) 0.0890(17) Uani 0.723(12) 1 d PDU C 2
Cl3' Cl 0.1764(6) 0.04843(15) 0.5305(7) 0.129(3) Uani 0.723(12) 1 d PDU C 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.432(7) . ?
O1 C20 1.445(9) . ?
O2 C4 1.405(7) . ?
O2 C22 1.440(8) . ?
F1 C19 1.340(7) . ?
F2 C19 1.321(7) . ?
F3 C19 1.337(8) . ?
F4 C21 1.338(7) . ?
F5 C21 1.334(8) . ?
F6 C21 1.309(7) . ?
C1 C2 1.483(8) . ?
C1 C18 1.485(8) . ?
C1 C19 1.492(9) . ?
C2 C3 1.173(7) . ?
C3 C4 1.490(8) . ?
C4 C5 1.470(9) . ?
C4 C21 1.534(9) . ?
C5 C6 1.205(8) . ?
C6 C7 1.426(9) . ?
C7 C8 1.367(8) . ?
C7 C23 1.472(8) . ?
C8 C9 1.239(8) . ?
C9 C10 1.341(8) . ?
C10 C11 1.427(8) . ?
C10 C30 1.484(8) . ?
C11 C12 1.190(7) . ?
C12 C13 1.428(8) . ?
C13 C14 1.379(8) . ?
C13 C36 1.472(8) . ?
C14 C15 1.228(8) . ?
C15 C16 1.348(8) . ?
C16 C17 1.429(8) . ?
C16 C42 1.486(7) . ?
C17 C18 1.180(8) . ?
C23 C24 1.394(8) . ?
C23 C28 1.395(8) . ?
C24 C25 1.366(8) . ?
C25 C26 1.388(9) . ?
C26 C27 1.379(9) . ?
C26 C29 1.496(9) . ?
C27 C28 1.363(9) . ?
C29 F11' 1.31(2) . ?
C29 F11 1.324(12) . ?
C29 F10' 1.330(19) . ?
C29 F12 1.337(12) . ?
C29 F10 1.347(13) . ?
C29 F12' 1.35(2) . ?
C30 C31 1.373(8) . ?
C30 C35 1.387(8) . ?
C31 C32 1.386(8) . ?
C32 C33 1.377(9) . ?
C33 C34 1.372(9) . ?
C34 C35 1.393(8) . ?
C36 C37 1.384(8) . ?
C36 C41 1.388(8) . ?
C37 C38 1.384(8) . ?
C38 C39 1.366(9) . ?
C39 C40 1.372(9) . ?
C40 C41 1.369(8) . ?
C42 C47 1.381(8) . ?
C42 C43 1.400(8) . ?
C43 C44 1.379(8) . ?
C44 C45 1.389(8) . ?
C45 C46 1.376(8) . ?
C45 C48 1.493(8) . ?
C46 C47 1.377(8) . ?
C48 F8 1.310(8) . ?
C48 F7 1.318(8) . ?
C48 F9 1.329(8) . ?
C49 Cl2 1.683(15) . ?
C49 Cl3' 1.697(8) . ?
C49 Cl1' 1.710(10) . ?
C49 Cl1 1.753(14) . ?
C49 Cl2' 1.780(9) . ?
C49 Cl3 1.816(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C20 112.2(5) . . ?
C4 O2 C22 111.8(5) . . ?
O1 C1 C2 111.8(5) . . ?
O1 C1 C18 111.0(5) . . ?
C2 C1 C18 112.3(5) . . ?
O1 C1 C19 102.7(5) . . ?
C2 C1 C19 109.2(5) . . ?
C18 C1 C19 109.4(5) . . ?
C3 C2 C1 175.6(6) . . ?
C2 C3 C4 177.8(6) . . ?
O2 C4 C5 114.4(5) . . ?
O2 C4 C3 111.4(5) . . ?
C5 C4 C3 110.6(5) . . ?
O2 C4 C21 102.7(5) . . ?
C5 C4 C21 109.2(5) . . ?
C3 C4 C21 108.1(5) . . ?
C6 C5 C4 177.7(6) . . ?
C5 C6 C7 177.7(6) . . ?
C8 C7 C6 119.0(5) . . ?
C8 C7 C23 122.3(5) . . ?
C6 C7 C23 118.7(5) . . ?
C9 C8 C7 179.2(7) . . ?
C8 C9 C10 176.5(6) . . ?
C9 C10 C11 119.7(5) . . ?
C9 C10 C30 121.4(5) . . ?
C11 C10 C30 118.8(5) . . ?
C12 C11 C10 178.3(6) . . ?
C11 C12 C13 177.6(6) . . ?
C14 C13 C12 116.7(5) . . ?
C14 C13 C36 122.2(5) . . ?
C12 C13 C36 121.1(5) . . ?
C15 C14 C13 176.0(6) . . ?
C14 C15 C16 176.1(7) . . ?
C15 C16 C17 119.4(5) . . ?
C15 C16 C42 120.0(5) . . ?
C17 C16 C42 120.5(5) . . ?
C18 C17 C16 175.5(7) . . ?
C17 C18 C1 176.2(6) . . ?
F2 C19 F3 105.8(6) . . ?
F2 C19 F1 106.1(5) . . ?
F3 C19 F1 106.0(6) . . ?
F2 C19 C1 114.0(6) . . ?
F3 C19 C1 112.0(5) . . ?
F1 C19 C1 112.4(6) . . ?
F6 C21 F5 107.2(6) . . ?
F6 C21 F4 107.5(5) . . ?
F5 C21 F4 105.3(6) . . ?
F6 C21 C4 112.3(6) . . ?
F5 C21 C4 111.8(5) . . ?
F4 C21 C4 112.2(6) . . ?
C24 C23 C28 117.5(5) . . ?
C24 C23 C7 121.5(5) . . ?
C28 C23 C7 120.9(6) . . ?
C25 C24 C23 122.0(6) . . ?
C24 C25 C26 119.4(6) . . ?
C27 C26 C25 119.1(6) . . ?
C27 C26 C29 119.9(7) . . ?
C25 C26 C29 121.0(7) . . ?
C28 C27 C26 121.4(6) . . ?
C27 C28 C23 120.4(6) . . ?
F11' C29 F11 80.5(16) . . ?
F11' C29 F10' 113(4) . . ?
F11 C29 F10' 123(3) . . ?
F11' C29 F12 121(2) . . ?
F11 C29 F12 108.7(13) . . ?
F11 C29 F10 105.6(9) . . ?
F10' C29 F10 91(4) . . ?
F12 C29 F10 103.3(14) . . ?
F11' C29 F12' 106.5(18) . . ?
F10' C29 F12' 101(3) . . ?
F12 C29 F12' 86(3) . . ?
F10 C29 F12' 128.6(19) . . ?
F11' C29 C26 116.1(17) . . ?
F11 C29 C26 113.4(8) . . ?
F10' C29 C26 109(4) . . ?
F12 C29 C26 112.8(13) . . ?
F10 C29 C26 112.3(8) . . ?
F12' C29 C26 110.0(18) . . ?
C31 C30 C35 119.3(5) . . ?
C31 C30 C10 121.1(5) . . ?
C35 C30 C10 119.5(5) . . ?
C30 C31 C32 120.7(6) . . ?
C33 C32 C31 119.9(6) . . ?
C34 C33 C32 120.1(6) . . ?
C33 C34 C35 120.0(6) . . ?
C30 C35 C34 120.0(6) . . ?
C37 C36 C41 119.0(5) . . ?
C37 C36 C13 120.4(5) . . ?
C41 C36 C13 120.6(5) . . ?
C38 C37 C36 120.2(6) . . ?
C39 C38 C37 120.0(6) . . ?
C38 C39 C40 120.2(6) . . ?
C41 C40 C39 120.4(6) . . ?
C40 C41 C36 120.2(6) . . ?
C47 C42 C43 118.9(5) . . ?
C47 C42 C16 121.1(5) . . ?
C43 C42 C16 120.0(5) . . ?
C44 C43 C42 120.4(6) . . ?
C43 C44 C45 119.3(6) . . ?
C46 C45 C44 120.9(5) . . ?
C46 C45 C48 120.0(6) . . ?
C44 C45 C48 119.0(6) . . ?
C45 C46 C47 119.4(6) . . ?
C46 C47 C42 121.2(6) . . ?
F8 C48 F7 106.4(6) . . ?
F8 C48 F9 105.0(6) . . ?
F7 C48 F9 104.3(6) . . ?
F8 C48 C45 114.1(6) . . ?
F7 C48 C45 113.1(6) . . ?
F9 C48 C45 113.0(6) . . ?
Cl2 C49 Cl3' 87.8(9) . . ?
Cl2 C49 Cl1' 115.9(10) . . ?
Cl3' C49 Cl1' 111.9(5) . . ?
Cl2 C49 Cl1 120.8(12) . . ?
Cl3' C49 Cl1 135.1(7) . . ?
Cl3' C49 Cl2' 109.4(5) . . ?
Cl1' C49 Cl2' 105.7(5) . . ?
Cl1 C49 Cl2' 102.7(7) . . ?
Cl2 C49 Cl3 114.2(9) . . ?
Cl1' C49 Cl3 75.7(8) . . ?
Cl1 C49 Cl3 97.2(9) . . ?
Cl2' C49 Cl3 132.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 951897'
