# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

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

data_7
_database_code_depnum_ccdc_archive 'CCDC 1437230'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H12 O4'
_chemical_formula_sum            'C18 H12 O4'
_chemical_formula_weight         292.28

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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

_cell_length_a                   21.876(3)
_cell_length_b                   22.174(3)
_cell_length_c                   15.3753(18)
_cell_angle_alpha                90
_cell_angle_beta                 130.230(4)
_cell_angle_gamma                90
_cell_volume                     5694.2(12)
_cell_formula_units_Z            16
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      0.987
_cell_measurement_theta_max      0.990

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             2432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.097
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38658
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.526
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5830
_reflns_number_gt                4291
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5830
_refine_ls_number_parameters     397
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1799
_refine_ls_wR_factor_gt          0.1592
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      1.211
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001

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
O6 O 0.09720(8) 1.02446(8) -0.20247(12) 0.0218(4) Uani 1 1 d . U . . .
O8 O 0.31218(9) 1.04722(7) 0.18710(12) 0.0218(4) Uani 1 1 d . U . . .
O3 O 0.59554(9) 0.19530(8) 1.18664(12) 0.0235(4) Uani 1 1 d . U . . .
O4 O 0.41509(10) 0.34142(8) 0.89842(13) 0.0268(4) Uani 1 1 d . U . . .
O2 O 0.34323(9) 0.22732(8) 0.82016(12) 0.0244(4) Uani 1 1 d . U . . .
O1 O 0.62524(8) 0.19785(8) 1.03657(13) 0.0228(4) Uani 1 1 d . U . . .
O5 O 0.38336(9) 1.04536(9) 0.08389(13) 0.0299(4) Uani 1 1 d . U . . .
O7 O 0.15943(10) 0.90810(8) -0.12815(13) 0.0297(4) Uani 1 1 d . U . . .
C33 C 0.18552(11) 0.93212(10) -0.02646(16) 0.0158(5) Uani 1 1 d . U . . .
C5 C 0.48737(12) 0.22272(10) 0.94155(17) 0.0152(4) Uani 1 1 d . U . . .
C9 C 0.50196(12) 0.26026(10) 1.02437(17) 0.0160(5) Uani 1 1 d . U . . .
C29 C 0.29401(11) 0.98968(10) 0.14454(17) 0.0152(5) Uani 1 1 d . U . . .
C4 C 0.54597(12) 0.18140(11) 0.95902(17) 0.0168(5) Uani 1 1 d . U . . .
C14 C 0.44900(12) 0.31021(11) 0.99718(17) 0.0183(5) Uani 1 1 d . U . . .
C13 C 0.56896(12) 0.25292(11) 1.14571(17) 0.0177(5) Uani 1 1 d . U . . .
C30 C 0.33190(12) 0.94934(11) 0.23161(17) 0.0203(5) Uani 1 1 d . U . . .
H30 H 0.3291 0.9075 0.2254 0.024 Uiso 1 1 calc R U . . .
C28 C 0.23935(11) 0.98349(10) 0.02020(17) 0.0151(5) Uani 1 1 d . U . . .
C23 C 0.24000(11) 1.02355(10) -0.04762(17) 0.0153(4) Uani 1 1 d . U . . .
C24 C 0.17216(12) 1.02856(11) -0.16938(17) 0.0169(5) Uani 1 1 d . U . . .
C7 C 0.38493(13) 0.20963(11) 0.72265(18) 0.0221(5) Uani 1 1 d . U . . .
H7 H 0.4175 0.2022 0.7047 0.027 Uiso 1 1 calc R U . . .
C21 C 0.30818(13) 1.11599(11) -0.04727(17) 0.0226(5) Uani 1 1 d . U . . .
H21 H 0.2641 1.1370 -0.1089 0.027 Uiso 1 1 calc R U . . .
C6 C 0.40908(12) 0.22003(10) 0.82816(17) 0.0168(5) Uani 1 1 d . U . . .
C32 C 0.36310(13) 1.04190(12) 0.30351(18) 0.0229(5) Uani 1 1 d . U . . .
H32 H 0.3850 1.0742 0.3539 0.028 Uiso 1 1 calc R U . . .
C2 C 0.61863(14) 0.10807(12) 0.9655(2) 0.0261(5) Uani 1 1 d . U . . .
H2 H 0.6335 0.0724 0.9519 0.031 Uiso 1 1 calc R U . . .
C22 C 0.30727(12) 1.06276(11) -0.00640(17) 0.0182(5) Uani 1 1 d . U . . .
C25 C 0.16582(13) 1.03683(12) -0.26242(18) 0.0247(5) Uani 1 1 d . U . . .
H25 H 0.2077 1.0417 -0.2632 0.030 Uiso 1 1 calc R U . . .
C31 C 0.37694(13) 0.98373(12) 0.33462(18) 0.0229(5) Uani 1 1 d . U . . .
H31 H 0.4094 0.9687 0.4086 0.028 Uiso 1 1 calc R U . . .
C3 C 0.53962(13) 0.12693(11) 0.91275(18) 0.0216(5) Uani 1 1 d . U . . .
H3 H 0.4926 0.1062 0.8573 0.026 Uiso 1 1 calc R U . . .
C1 C 0.66795(13) 0.15193(12) 1.0392(2) 0.0264(6) Uani 1 1 d . U . . .
H1 H 0.7235 0.1510 1.0855 0.032 Uiso 1 1 calc R U . . .
C8 C 0.29957(14) 0.21242(12) 0.64514(18) 0.0274(6) Uani 1 1 d . U . . .
H8 H 0.2657 0.2080 0.5664 0.033 Uiso 1 1 calc R U . . .
C27 C 0.04372(13) 1.02910(12) -0.31890(17) 0.0243(5) Uani 1 1 d . U . . .
H27 H -0.0116 1.0273 -0.3638 0.029 Uiso 1 1 calc R U . . .
C26 C 0.08232(14) 1.03651(13) -0.35868(19) 0.0276(6) Uani 1 1 d . U . . .
H26 H 0.0592 1.0407 -0.4346 0.033 Uiso 1 1 calc R U . . .
C34 C 0.15551(13) 0.90087(13) 0.0144(2) 0.0298(6) Uani 1 1 d . U . . .
H34 H 0.1638 0.9073 0.0811 0.036 Uiso 1 1 calc R U . . .
C10 C 0.65664(14) 0.20058(12) 1.30220(18) 0.0296(6) Uani 1 1 d . U . . .
H10 H 0.6858 0.1685 1.3515 0.036 Uiso 1 1 calc R U . . .
C12 C 0.61137(14) 0.29289(12) 1.23331(19) 0.0278(6) Uani 1 1 d . U . . .
H12 H 0.6047 0.3345 1.2288 0.033 Uiso 1 1 calc R U . . .
C19 C 0.43271(14) 1.09075(15) 0.09978(19) 0.0351(7) Uani 1 1 d . U . . .
H19 H 0.4881 1.0913 0.1565 0.042 Uiso 1 1 calc R U . . .
C15 C 0.42272(13) 0.33303(12) 1.04967(19) 0.0278(6) Uani 1 1 d . U . . .
H15 H 0.4374 0.3203 1.1186 0.033 Uiso 1 1 calc R U . . .
C17 C 0.36530(14) 0.38354(12) 0.8893(2) 0.0323(6) Uani 1 1 d . U . . .
H17 H 0.3339 0.4106 0.8293 0.039 Uiso 1 1 calc R U . . .
C18 C 0.27754(13) 0.22258(12) 0.70730(19) 0.0280(6) Uani 1 1 d . U . . .
H18 H 0.2248 0.2259 0.6778 0.034 Uiso 1 1 calc R U . . .
C16 C 0.36823(14) 0.38028(13) 0.9786(2) 0.0339(7) Uani 1 1 d . U . . .
H16 H 0.3401 0.4042 0.9919 0.041 Uiso 1 1 calc R U . . .
C11 C 0.66808(16) 0.25824(13) 1.33343(19) 0.0353(7) Uani 1 1 d . U . . .
H11 H 0.7060 0.2732 1.4070 0.042 Uiso 1 1 calc R U . . .
C20 C 0.38958(17) 1.13371(14) 0.0222(2) 0.0387(7) Uani 1 1 d . U . . .
H20 H 0.4092 1.1688 0.0149 0.046 Uiso 1 1 calc R U . . .
C35 C 0.10591(14) 0.85351(13) -0.0744(2) 0.0391(7) Uani 1 1 d . U . . .
H35 H 0.0763 0.8239 -0.0735 0.047 Uiso 1 1 calc R U . . .
C36 C 0.11125(15) 0.86081(13) -0.1535(2) 0.0365(7) Uani 1 1 d . U . . .
H36 H 0.0856 0.8369 -0.2182 0.044 Uiso 1 1 calc R U . . .


_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
O6 C27 1.371(2) . ?
O6 C24 1.370(2) . ?
O8 C29 1.370(3) . ?
O8 C32 1.372(2) . ?
O3 C13 1.376(3) . ?
O3 C10 1.375(3) . ?
O4 C14 1.371(3) . ?
O4 C17 1.372(3) . ?
O2 C6 1.374(3) . ?
O2 C18 1.366(3) . ?
O1 C1 1.365(3) . ?
O1 C4 1.375(2) . ?
O5 C22 1.365(2) . ?
O5 C19 1.378(3) . ?
O7 C36 1.354(3) . ?
O7 C33 1.379(2) . ?
C33 C34 1.356(3) . ?
C33 C28 1.452(3) . ?
C5 C9 1.375(3) . ?
C5 C4 1.453(3) . ?
C5 C6 1.456(3) . ?
C9 C14 1.455(3) . ?
C9 C13 1.457(3) . ?
C29 C30 1.359(3) . ?
C29 C28 1.467(3) . ?
C4 C3 1.363(3) . ?
C14 C15 1.355(3) . ?
C13 C12 1.359(3) . ?
C30 C31 1.430(3) . ?
C28 C23 1.377(3) . ?
C23 C22 1.456(3) . ?
C23 C24 1.460(3) . ?
C24 C25 1.358(3) . ?
C7 C6 1.363(3) . ?
C7 C8 1.427(3) . ?
C21 C22 1.343(3) . ?
C21 C20 1.417(3) . ?
C32 C31 1.341(4) . ?
C2 C1 1.347(4) . ?
C2 C3 1.417(3) . ?
C25 C26 1.427(3) . ?
C8 C18 1.338(4) . ?
C27 C26 1.335(3) . ?
C34 C35 1.494(4) . ?
C10 C11 1.332(4) . ?
C12 C11 1.426(3) . ?
C19 C20 1.329(4) . ?
C15 C16 1.425(4) . ?
C17 C16 1.334(4) . ?
C35 C36 1.305(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C27 O6 C24 106.70(16) . . ?
C29 O8 C32 106.47(17) . . ?
C13 O3 C10 106.44(18) . . ?
C14 O4 C17 106.40(18) . . ?
C6 O2 C18 106.65(17) . . ?
C1 O1 C4 106.48(18) . . ?
C22 O5 C19 106.0(2) . . ?
C36 O7 C33 107.5(2) . . ?
C34 C33 O7 111.0(2) . . ?
C34 C33 C28 130.7(2) . . ?
O7 C33 C28 118.23(18) . . ?
C9 C5 C4 124.14(18) . . ?
C9 C5 C6 121.58(19) . . ?
C4 C5 C6 114.25(18) . . ?
C5 C9 C14 121.94(18) . . ?
C5 C9 C13 123.9(2) . . ?
C14 C9 C13 114.13(19) . . ?
C30 C29 O8 109.77(18) . . ?
C30 C29 C28 133.4(2) . . ?
O8 C29 C28 116.77(18) . . ?
C3 C4 O1 109.51(19) . . ?
C3 C4 C5 133.0(2) . . ?
O1 C4 C5 117.46(19) . . ?
C15 C14 O4 109.7(2) . . ?
C15 C14 C9 132.7(2) . . ?
O4 C14 C9 117.59(18) . . ?
C12 C13 O3 109.63(19) . . ?
C12 C13 C9 132.4(2) . . ?
O3 C13 C9 117.90(19) . . ?
C29 C30 C31 106.6(2) . . ?
C23 C28 C33 122.26(18) . . ?
C23 C28 C29 121.9(2) . . ?
C33 C28 C29 115.84(18) . . ?
C28 C23 C22 123.90(18) . . ?
C28 C23 C24 121.41(19) . . ?
C22 C23 C24 114.68(18) . . ?
C25 C24 O6 109.53(18) . . ?
C25 C24 C23 133.55(19) . . ?
O6 C24 C23 116.92(18) . . ?
C6 C7 C8 106.2(2) . . ?
C22 C21 C20 106.4(2) . . ?
C7 C6 O2 109.60(18) . . ?
C7 C6 C5 133.2(2) . . ?
O2 C6 C5 117.18(18) . . ?
C31 C32 O8 110.7(2) . . ?
C1 C2 C3 106.6(2) . . ?
C21 C22 O5 110.3(2) . . ?
C21 C22 C23 129.6(2) . . ?
O5 C22 C23 120.0(2) . . ?
C24 C25 C26 106.5(2) . . ?
C32 C31 C30 106.4(2) . . ?
C4 C3 C2 106.7(2) . . ?
C2 C1 O1 110.7(2) . . ?
C18 C8 C7 106.9(2) . . ?
C26 C27 O6 110.41(19) . . ?
C27 C26 C25 106.9(2) . . ?
C33 C34 C35 102.6(2) . . ?
C11 C10 O3 110.3(2) . . ?
C13 C12 C11 106.2(2) . . ?
C20 C19 O5 110.1(2) . . ?
C14 C15 C16 106.5(2) . . ?
C16 C17 O4 110.6(2) . . ?
C8 C18 O2 110.6(2) . . ?
C17 C16 C15 106.8(2) . . ?
C10 C11 C12 107.4(2) . . ?
C19 C20 C21 107.2(2) . . ?
C36 C35 C34 108.4(2) . . ?
C35 C36 O7 110.5(2) . . ?

_refine_diff_density_max         0.990
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.064

_shelxl_version_number           2013-3



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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1437235'
_audit_update_record             
;
2015-11-16 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C98 H14 F10 O4'
_chemical_formula_weight         1445.09

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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   35.203(6)
_cell_length_b                   55.389(9)
_cell_length_c                   12.2274(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     23842(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5346
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      23.04

_exptl_crystal_description       rectangle
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_F_000             11584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.120
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'Multi-Scan absorbtion correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85545
_diffrn_reflns_av_unetI/netI     0.1141
_diffrn_reflns_av_R_equivalents  0.1202
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_k_max       74
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.371
_diffrn_reflns_theta_max         28.430
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             14492
_reflns_number_gt                8805
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.850
_reflns_Friedel_fraction_max     0.930
_reflns_Friedel_fraction_full    0.952

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0783P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2681 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.7(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14492
_refine_ls_number_parameters     1009
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1573
_refine_ls_wR_factor_gt          0.1396
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.972
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.51457(17) 0.46155(11) 0.5758(6) 0.0404(18) Uani 1 1 d . . . . .
C2 C 0.52400(17) 0.47014(11) 0.6769(6) 0.0377(16) Uani 1 1 d . . . . .
C3 C 0.51831(17) 0.45645(10) 0.7661(6) 0.0363(16) Uani 1 1 d . . . . .
C4 C 0.50370(16) 0.43345(10) 0.7551(5) 0.0287(13) Uani 1 1 d . . . . .
C5 C 0.49870(16) 0.43802(10) 0.5653(5) 0.0284(13) Uani 1 1 d . . . . .
C6 C 0.49342(14) 0.42351(8) 0.6554(5) 0.0218(11) Uani 1 1 d . . . . .
C7 C 0.47689(13) 0.39880(8) 0.6468(4) 0.0157(10) Uani 1 1 d . . . . .
C8 C 0.50409(13) 0.37989(7) 0.6318(4) 0.0136(9) Uani 1 1 d . . . . .
C9 C 0.54179(14) 0.38180(8) 0.6035(4) 0.0171(10) Uani 1 1 d . . . . .
H9 H 0.5553 0.3963 0.5885 0.021 Uiso 1 1 calc R U . . .
C10 C 0.55654(14) 0.35831(8) 0.6012(4) 0.0157(10) Uani 1 1 d . . . . .
H10 H 0.5821 0.3539 0.5855 0.019 Uiso 1 1 calc R U . . .
C11 C 0.52728(13) 0.34275(8) 0.6259(4) 0.0134(10) Uani 1 1 d . . . . .
C12 C 0.52821(12) 0.31700(7) 0.6355(4) 0.0120(9) Uani 1 1 d . . . . .
C13 C 0.49922(13) 0.30093(8) 0.6477(4) 0.0146(9) Uani 1 1 d . . . . .
C14 C 0.50232(15) 0.27593(8) 0.6697(4) 0.0213(12) Uani 1 1 d . . . . .
H14 H 0.5253 0.2673 0.6818 0.026 Uiso 1 1 calc R U . . .
C15 C 0.46706(14) 0.26632(9) 0.6707(4) 0.0211(11) Uani 1 1 d . . . . .
H15 H 0.4609 0.2498 0.6830 0.025 Uiso 1 1 calc R U . . .
C16 C 0.44082(13) 0.28528(8) 0.6501(4) 0.0162(10) Uani 1 1 d . . . . .
C17 C 0.40224(13) 0.28360(8) 0.6398(4) 0.0161(10) Uani 1 1 d . . . . .
C18 C 0.37497(14) 0.30236(8) 0.6256(4) 0.0165(10) Uani 1 1 d . . . . .
C19 C 0.33676(14) 0.30050(9) 0.6041(4) 0.0199(11) Uani 1 1 d . . . . .
H19 H 0.3228 0.2861 0.5919 0.024 Uiso 1 1 calc R U . . .
C20 C 0.32238(15) 0.32424(9) 0.6036(4) 0.0211(11) Uani 1 1 d . . . . .
H20 H 0.2967 0.3288 0.5918 0.025 Uiso 1 1 calc R U . . .
C21 C 0.35214(13) 0.33943(8) 0.6232(4) 0.0155(10) Uani 1 1 d . . . . .
C22 C 0.35215(13) 0.36477(8) 0.6312(4) 0.0161(10) Uani 1 1 d . . . . .
H22 H 0.3275 0.3717 0.6282 0.019 Uiso 1 1 calc R U . . .
C23 C 0.38045(13) 0.38140(8) 0.6423(4) 0.0171(10) Uani 1 1 d . . . . .
C24 C 0.37646(14) 0.40703(8) 0.6539(4) 0.0179(10) Uani 1 1 d . . . . .
H24 H 0.3533 0.4158 0.6556 0.021 Uiso 1 1 calc R U . . .
C25 C 0.41164(15) 0.41640(9) 0.6619(4) 0.0205(11) Uani 1 1 d . . . . .
H25 H 0.4175 0.4330 0.6722 0.025 Uiso 1 1 calc R U . . .
C26 C 0.43842(13) 0.39736(8) 0.6525(4) 0.0143(9) Uani 1 1 d . . . . .
C27 C 0.38638(13) 0.25859(8) 0.6400(4) 0.0165(9) Uani 1 1 d . . . . .
C28 C 0.36355(14) 0.25025(9) 0.7241(4) 0.0182(10) Uani 1 1 d . . . . .
C29 C 0.34874(15) 0.22735(9) 0.7254(4) 0.0225(11) Uani 1 1 d . . . . .
C30 C 0.35659(15) 0.21166(8) 0.6408(5) 0.0244(11) Uani 1 1 d . . . . .
C31 C 0.37932(15) 0.21907(9) 0.5556(4) 0.0231(12) Uani 1 1 d . . . . .
C32 C 0.39352(15) 0.24212(9) 0.5553(4) 0.0197(11) Uani 1 1 d . . . . .
C33 C 0.56713(13) 0.30599(8) 0.6256(4) 0.0174(10) Uani 1 1 d . . . . .
C34 C 0.57556(15) 0.29100(9) 0.5380(4) 0.0220(11) Uani 1 1 d . . . . .
H34 H 0.5569 0.2881 0.4834 0.026 Uiso 1 1 calc R U . . .
C35 C 0.61087(16) 0.28022(9) 0.5295(5) 0.0281(13) Uani 1 1 d . . . . .
H35 H 0.6164 0.2701 0.4689 0.034 Uiso 1 1 calc R U . . .
C36 C 0.63801(16) 0.28410(10) 0.6081(5) 0.0299(14) Uani 1 1 d . . . . .
H36 H 0.6622 0.2766 0.6020 0.036 Uiso 1 1 calc R U . . .
C37 C 0.63010(16) 0.29905(10) 0.6967(6) 0.0328(14) Uani 1 1 d . . . . .
H37 H 0.6489 0.3019 0.7510 0.039 Uiso 1 1 calc R U . . .
C38 C 0.59449(15) 0.30988(9) 0.7055(5) 0.0227(11) Uani 1 1 d . . . . .
H38 H 0.5889 0.3200 0.7663 0.027 Uiso 1 1 calc R U . . .
C39 C 0.4424(3) 0.28066(11) 0.0301(6) 0.049(2) Uani 1 1 d . . . . .
C40 C 0.44720(19) 0.29518(10) -0.0665(4) 0.0312(14) Uani 1 1 d . . . . .
C41 C 0.53032(16) 0.31185(11) 0.0822(5) 0.0340(14) Uani 1 1 d . . . . .
C42 C 0.41728(18) 0.30985(10) -0.1043(5) 0.0332(14) Uani 1 1 d . . . . .
C43 C 0.46613(17) 0.36886(9) 0.3887(4) 0.0282(12) Uani 1 1 d . . . . .
C44 C 0.51776(17) 0.34481(11) 0.3294(5) 0.0328(14) Uani 1 1 d . . . . .
C45 C 0.53672(16) 0.33680(12) 0.2370(5) 0.0334(14) Uani 1 1 d . . . . .
C46 C 0.37882(19) 0.38218(12) 0.2562(5) 0.0383(16) Uani 1 1 d . . . . .
C47 C 0.50501(19) 0.29648(11) 0.0286(5) 0.0331(15) Uani 1 1 d . U . . .
C48 C 0.53098(17) 0.31228(11) 0.2002(5) 0.0337(14) Uani 1 1 d . . . . .
C49 C 0.48514(18) 0.30489(11) -0.0666(4) 0.0315(14) Uani 1 1 d . . . . .
C50 C 0.43620(19) 0.38223(11) -0.0704(5) 0.0359(15) Uani 1 1 d . . . . .
C51 C 0.4737(2) 0.39813(11) 0.0799(5) 0.0434(19) Uani 1 1 d . . . . .
C52 C 0.35373(18) 0.36668(13) 0.2035(5) 0.0402(16) Uani 1 1 d . . . . .
C53 C 0.35301(18) 0.36614(12) 0.0858(5) 0.0379(16) Uani 1 1 d . . . . .
C54 C 0.4366(2) 0.38301(10) 0.3527(5) 0.0376(16) Uani 1 1 d . . . . .
C55 C 0.50145(19) 0.36878(11) 0.3317(5) 0.0388(16) Uani 1 1 d . . . . .
C56 C 0.49134(18) 0.32856(11) -0.1034(5) 0.0358(15) Uani 1 1 d . . . . .
C57 C 0.46544(18) 0.36859(10) -0.1040(5) 0.0330(14) Uani 1 1 d . . . . .
C58 C 0.41800(19) 0.31000(10) 0.3898(5) 0.0345(14) Uani 1 1 d . . . . .
C59 C 0.38217(18) 0.30975(13) -0.0449(6) 0.0415(17) Uani 1 1 d . . . . .
C60 C 0.5010(2) 0.36865(11) -0.0488(6) 0.0411(17) Uani 1 1 d . . . . .
C61 C 0.4799(2) 0.28158(11) 0.0912(6) 0.0435(17) Uani 1 1 d . . . . .
C62 C 0.39266(19) 0.34963(12) 0.3896(5) 0.0407(16) Uani 1 1 d . . . . .
C63 C 0.39824(19) 0.37369(12) 0.3527(5) 0.0380(16) Uani 1 1 d . . . . .
C64 C 0.4482(2) 0.29621(11) 0.3556(5) 0.0398(16) Uani 1 1 d . . . . .
C65 C 0.4592(2) 0.34318(11) -0.1394(5) 0.0379(16) Uani 1 1 d . . . . .
C66 C 0.3784(2) 0.29426(14) 0.0500(7) 0.054(2) Uani 1 1 d . . . . .
C67 C 0.49174(19) 0.32927(12) 0.3887(5) 0.0399(15) Uani 1 1 d . . . . .
C68 C 0.5056(2) 0.38349(12) 0.0435(6) 0.0461(19) Uani 1 1 d . . . . .
C69 C 0.34817(18) 0.34258(15) 0.2432(5) 0.0481(19) Uani 1 1 d . . . . .
C70 C 0.50609(19) 0.29737(11) 0.2575(5) 0.0376(16) Uani 1 1 d . . . . .
C71 C 0.5055(2) 0.38381(12) 0.2377(6) 0.0431(18) Uani 1 1 d . . . . .
C72 C 0.4037(2) 0.39718(11) 0.1948(6) 0.0439(18) Uani 1 1 d . . . . .
C73 C 0.4406(2) 0.39733(11) 0.0234(6) 0.049(2) Uani 1 1 d . . . . .
C74 C 0.3977(2) 0.37243(15) -0.0675(6) 0.051(2) Uani 1 1 d . . . . .
C75 C 0.4865(2) 0.30636(13) 0.3546(5) 0.0437(17) Uani 1 1 d . . . . .
C76 C 0.38295(19) 0.30971(12) 0.3345(5) 0.0398(16) Uani 1 1 d . . . . .
C77 C 0.3779(2) 0.38080(13) 0.0289(6) 0.0437(18) Uani 1 1 d . . . . .
C78 C 0.4244(2) 0.33504(12) 0.4266(5) 0.0418(17) Uani 1 1 d . . . . .
C79 C 0.4246(2) 0.33398(11) -0.1398(4) 0.0388(16) Uani 1 1 d . U . . .
C80 C 0.4742(3) 0.39808(11) 0.2011(6) 0.052(2) Uani 1 1 d . . . . .
C81 C 0.4099(2) 0.28027(11) 0.2055(5) 0.0439(18) Uani 1 1 d . . . . .
C82 C 0.54030(15) 0.35216(12) 0.1427(6) 0.0419(16) Uani 1 1 d . . . . .
C83 C 0.37829(19) 0.29497(14) 0.2407(6) 0.047(2) Uani 1 1 d . . . . .
C84 C 0.4040(2) 0.39687(12) 0.0843(7) 0.053(2) Uani 1 1 d . . . . .
C85 C 0.4591(2) 0.34432(12) 0.4258(5) 0.0412(17) Uani 1 1 d . . . . .
C86 C 0.53632(17) 0.33621(13) 0.0415(6) 0.0432(17) Uani 1 1 d . . . . .
C87 C 0.3668(2) 0.33400(14) 0.3339(6) 0.0492(19) Uani 1 1 d . . . . .
C88 C 0.4438(2) 0.28133(10) 0.2620(6) 0.0403(17) Uani 1 1 d . . . . .
C89 C 0.3917(2) 0.34946(13) -0.1026(5) 0.0460(17) Uani 1 1 d . . . . .
C90 C 0.34741(17) 0.34168(14) 0.0484(6) 0.0441(18) Uani 1 1 d . . . . .
C91 C 0.4095(2) 0.28018(11) 0.0857(6) 0.0493(19) Uani 1 1 d . . . . .
C92 C 0.5171(2) 0.34427(13) -0.0474(6) 0.0445(18) Uani 1 1 d . . . . .
C93 C 0.36661(18) 0.33353(13) -0.0442(5) 0.0412(17) Uani 1 1 d . . . . .
C94 C 0.4415(3) 0.39782(10) 0.2564(6) 0.0471(19) Uani 1 1 d . . . . .
C95 C 0.34380(17) 0.32619(14) 0.1443(8) 0.057(2) Uani 1 1 d . . . . .
C96 C 0.52540(18) 0.37486(12) 0.1423(6) 0.0457(17) Uani 1 1 d . . . . .
C97 C 0.4802(2) 0.28179(11) 0.2021(6) 0.0500(19) Uani 1 1 d . . . . .
C98 C 0.3589(2) 0.30387(15) 0.1447(7) 0.058(2) Uani 1 1 d . . . . .
F1 F 0.48891(10) 0.42999(6) 0.4662(3) 0.0396(9) Uani 1 1 d . . . . .
F2 F 0.51822(12) 0.47488(6) 0.4847(4) 0.0618(13) Uani 1 1 d . . . . .
F3 F 0.53785(10) 0.49242(5) 0.6852(4) 0.0574(13) Uani 1 1 d . . . . .
F4 F 0.52613(11) 0.46561(6) 0.8662(4) 0.0557(12) Uani 1 1 d . . . . .
F5 F 0.49887(11) 0.42063(6) 0.8473(3) 0.0405(9) Uani 1 1 d . . . . .
F6 F 0.41458(9) 0.24885(5) 0.4701(3) 0.0305(7) Uani 1 1 d . . . . .
F7 F 0.38645(10) 0.20386(5) 0.4740(3) 0.0354(8) Uani 1 1 d . . . . .
F8 F 0.34209(9) 0.18932(5) 0.6446(3) 0.0357(8) Uani 1 1 d . . . . .
F9 F 0.32628(10) 0.22038(5) 0.8092(3) 0.0319(8) Uani 1 1 d . . . . .
F10 F 0.35622(9) 0.26490(5) 0.8090(2) 0.0249(7) Uani 1 1 d . . . . .
O1 O 0.41871(8) 0.37579(5) 0.6415(3) 0.0152(7) Uani 1 1 d . . . . .
O2 O 0.38496(8) 0.32600(5) 0.6372(3) 0.0144(7) Uani 1 1 d . . . . .
O3 O 0.46064(9) 0.30670(5) 0.6406(3) 0.0147(7) Uani 1 1 d . . . . .
O4 O 0.49447(9) 0.35576(5) 0.6452(3) 0.0150(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 F2 1.342(7) . ?
C1 C2 1.366(10) . ?
C1 C5 1.424(9) . ?
C2 F3 1.331(7) . ?
C2 C3 1.343(9) . ?
C3 F4 1.353(7) . ?
C3 C4 1.380(8) . ?
C4 F5 1.343(7) . ?
C4 C6 1.385(8) . ?
C5 F1 1.336(7) . ?
C5 C6 1.377(8) . ?
C6 C7 1.491(6) . ?
C7 C26 1.358(7) . ?
C7 C8 1.431(6) . ?
C8 C9 1.375(7) . ?
C8 O4 1.388(5) . ?
C9 C10 1.401(7) . ?
C10 C11 1.376(6) . ?
C11 O4 1.382(5) . ?
C11 C12 1.431(6) . ?
C12 C13 1.362(6) . ?
C12 C33 1.504(6) . ?
C13 O3 1.398(5) . ?
C13 C14 1.415(6) . ?
C14 C15 1.351(7) . ?
C15 C16 1.421(7) . ?
C16 C17 1.367(7) . ?
C16 O3 1.381(5) . ?
C17 C18 1.425(7) . ?
C17 C27 1.494(6) . ?
C18 O2 1.363(5) . ?
C18 C19 1.375(7) . ?
C19 C20 1.409(7) . ?
C20 C21 1.365(7) . ?
C21 O2 1.385(5) . ?
C21 C22 1.407(6) . ?
C22 C23 1.364(7) . ?
C23 O1 1.382(5) . ?
C23 C24 1.433(6) . ?
C24 C25 1.347(7) . ?
C25 C26 1.420(7) . ?
C26 O1 1.388(5) . ?
C27 C28 1.385(7) . ?
C27 C32 1.402(7) . ?
C28 F10 1.343(6) . ?
C28 C29 1.371(7) . ?
C29 F9 1.350(6) . ?
C29 C30 1.379(8) . ?
C30 F8 1.339(5) . ?
C30 C31 1.377(8) . ?
C31 F7 1.329(6) . ?
C31 C32 1.371(7) . ?
C32 F6 1.332(6) . ?
C33 C34 1.387(7) . ?
C33 C38 1.389(7) . ?
C34 C35 1.383(7) . ?
C35 C36 1.372(8) . ?
C36 C37 1.392(9) . ?
C37 C38 1.394(8) . ?
C39 C91 1.345(11) . ?
C39 C40 1.438(9) . ?
C39 C61 1.517(11) . ?
C40 C42 1.408(8) . ?
C40 C49 1.440(9) . ?
C41 C47 1.396(9) . ?
C41 C48 1.443(8) . ?
C41 C86 1.453(9) . ?
C42 C79 1.429(8) . ?
C42 C59 1.434(9) . ?
C43 C54 1.374(8) . ?
C43 C55 1.425(9) . ?
C43 C85 1.454(8) . ?
C44 C45 1.385(9) . ?
C44 C55 1.447(9) . ?
C44 C67 1.451(9) . ?
C45 C82 1.438(9) . ?
C45 C48 1.445(9) . ?
C46 C52 1.390(10) . ?
C46 C72 1.423(10) . ?
C46 C63 1.442(9) . ?
C47 C61 1.431(9) . ?
C47 C49 1.436(8) . ?
C48 C70 1.393(9) . ?
C49 C56 1.404(8) . ?
C50 C57 1.341(9) . ?
C50 C73 1.428(10) . ?
C50 C74 1.461(10) . ?
C51 C73 1.354(11) . ?
C51 C68 1.457(11) . ?
C51 C80 1.482(9) . ?
C52 C69 1.434(10) . ?
C52 C53 1.439(9) . ?
C53 C77 1.381(10) . ?
C53 C90 1.443(9) . ?
C54 C94 1.446(9) . ?
C54 C63 1.446(10) . ?
C55 C71 1.427(10) . ?
C56 C92 1.430(10) . ?
C56 C65 1.460(9) . ?
C57 C60 1.422(10) . ?
C57 C65 1.489(8) . ?
C58 C64 1.374(9) . ?
C58 C76 1.407(9) . ?
C58 C78 1.475(9) . ?
C59 C93 1.426(10) . ?
C59 C66 1.449(11) . ?
C60 C68 1.405(11) . ?
C60 C92 1.465(9) . ?
C61 C97 1.356(9) . ?
C62 C63 1.420(9) . ?
C62 C87 1.429(10) . ?
C62 C78 1.451(9) . ?
C64 C88 1.419(9) . ?
C64 C75 1.461(10) . ?
C65 C79 1.319(10) . ?
C66 C91 1.412(11) . ?
C66 C98 1.448(12) . ?
C67 C75 1.348(9) . ?
C67 C85 1.491(10) . ?
C68 C96 1.474(10) . ?
C69 C87 1.373(10) . ?
C69 C95 1.520(11) . ?
C70 C97 1.426(10) . ?
C70 C75 1.461(10) . ?
C71 C80 1.430(11) . ?
C71 C96 1.448(10) . ?
C72 C84 1.351(10) . ?
C72 C94 1.529(11) . ?
C73 C84 1.491(11) . ?
C74 C89 1.359(10) . ?
C74 C77 1.446(10) . ?
C76 C83 1.418(10) . ?
C76 C87 1.461(10) . ?
C77 C84 1.448(11) . ?
C78 C85 1.324(10) . ?
C79 C89 1.512(10) . ?
C80 C94 1.333(11) . ?
C81 C88 1.381(10) . ?
C81 C83 1.445(11) . ?
C81 C91 1.464(9) . ?
C82 C96 1.362(9) . ?
C82 C86 1.527(11) . ?
C83 C98 1.445(10) . ?
C86 C92 1.356(10) . ?
C88 C97 1.474(10) . ?
C89 C93 1.438(10) . ?
C90 C93 1.394(10) . ?
C90 C95 1.459(11) . ?
C95 C98 1.345(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 C1 C2 122.4(6) . . ?
F2 C1 C5 117.8(7) . . ?
C2 C1 C5 119.7(6) . . ?
F3 C2 C3 121.1(6) . . ?
F3 C2 C1 118.8(6) . . ?
C3 C2 C1 120.1(5) . . ?
C2 C3 F4 119.5(5) . . ?
C2 C3 C4 119.8(6) . . ?
F4 C3 C4 120.7(6) . . ?
F5 C4 C3 117.0(5) . . ?
F5 C4 C6 119.7(5) . . ?
C3 C4 C6 123.3(6) . . ?
F1 C5 C6 119.8(5) . . ?
F1 C5 C1 119.2(5) . . ?
C6 C5 C1 121.0(6) . . ?
C5 C6 C4 115.9(5) . . ?
C5 C6 C7 122.1(5) . . ?
C4 C6 C7 121.9(5) . . ?
C26 C7 C8 129.1(4) . . ?
C26 C7 C6 116.1(4) . . ?
C8 C7 C6 114.8(4) . . ?
C9 C8 O4 109.8(4) . . ?
C9 C8 C7 128.4(4) . . ?
O4 C8 C7 121.7(4) . . ?
C8 C9 C10 106.9(4) . . ?
C11 C10 C9 107.5(4) . . ?
C10 C11 O4 109.6(4) . . ?
C10 C11 C12 128.7(4) . . ?
O4 C11 C12 121.7(4) . . ?
C13 C12 C11 130.0(4) . . ?
C13 C12 C33 115.2(4) . . ?
C11 C12 C33 114.7(4) . . ?
C12 C13 O3 124.9(4) . . ?
C12 C13 C14 127.1(4) . . ?
O3 C13 C14 108.1(4) . . ?
C15 C14 C13 108.5(4) . . ?
C14 C15 C16 107.7(4) . . ?
C17 C16 O3 123.5(4) . . ?
C17 C16 C15 127.7(4) . . ?
O3 C16 C15 108.7(4) . . ?
C16 C17 C18 129.1(4) . . ?
C16 C17 C27 115.7(4) . . ?
C18 C17 C27 115.1(4) . . ?
O2 C18 C19 110.2(4) . . ?
O2 C18 C17 120.9(4) . . ?
C19 C18 C17 128.9(4) . . ?
C18 C19 C20 106.4(4) . . ?
C21 C20 C19 107.4(4) . . ?
C20 C21 O2 109.3(4) . . ?
C20 C21 C22 128.8(4) . . ?
O2 C21 C22 121.8(4) . . ?
C23 C22 C21 132.9(4) . . ?
C22 C23 O1 124.0(4) . . ?
C22 C23 C24 127.4(4) . . ?
O1 C23 C24 108.6(4) . . ?
C25 C24 C23 107.4(4) . . ?
C24 C25 C26 108.6(4) . . ?
C7 C26 O1 123.0(4) . . ?
C7 C26 C25 128.5(4) . . ?
O1 C26 C25 108.4(4) . . ?
C28 C27 C32 115.8(4) . . ?
C28 C27 C17 121.8(4) . . ?
C32 C27 C17 122.3(4) . . ?
F10 C28 C29 118.5(5) . . ?
F10 C28 C27 119.0(4) . . ?
C29 C28 C27 122.5(5) . . ?
F9 C29 C28 119.7(5) . . ?
F9 C29 C30 120.4(4) . . ?
C28 C29 C30 119.9(5) . . ?
F8 C30 C31 121.5(5) . . ?
F8 C30 C29 118.7(5) . . ?
C31 C30 C29 119.8(4) . . ?
F7 C31 C32 121.3(5) . . ?
F7 C31 C30 119.3(4) . . ?
C32 C31 C30 119.4(5) . . ?
F6 C32 C31 117.7(4) . . ?
F6 C32 C27 119.7(4) . . ?
C31 C32 C27 122.6(5) . . ?
C34 C33 C38 119.2(5) . . ?
C34 C33 C12 120.0(4) . . ?
C38 C33 C12 120.8(4) . . ?
C35 C34 C33 120.6(5) . . ?
C36 C35 C34 120.4(5) . . ?
C35 C36 C37 119.9(5) . . ?
C36 C37 C38 119.7(6) . . ?
C33 C38 C37 120.2(5) . . ?
C91 C39 C40 121.8(7) . . ?
C91 C39 C61 120.1(6) . . ?
C40 C39 C61 106.5(6) . . ?
C42 C40 C39 120.3(6) . . ?
C42 C40 C49 118.6(5) . . ?
C39 C40 C49 108.5(6) . . ?
C47 C41 C48 119.3(6) . . ?
C47 C41 C86 119.9(6) . . ?
C48 C41 C86 109.0(6) . . ?
C40 C42 C79 120.2(6) . . ?
C40 C42 C59 118.5(6) . . ?
C79 C42 C59 108.3(6) . . ?
C54 C43 C55 120.3(6) . . ?
C54 C43 C85 120.3(6) . . ?
C55 C43 C85 107.4(5) . . ?
C45 C44 C55 120.1(6) . . ?
C45 C44 C67 121.5(6) . . ?
C55 C44 C67 106.5(6) . . ?
C44 C45 C82 120.4(6) . . ?
C44 C45 C48 119.2(6) . . ?
C82 C45 C48 108.6(6) . . ?
C52 C46 C72 120.5(6) . . ?
C52 C46 C63 118.6(6) . . ?
C72 C46 C63 109.3(6) . . ?
C41 C47 C61 119.7(6) . . ?
C41 C47 C49 119.6(6) . . ?
C61 C47 C49 108.7(6) . . ?
C70 C48 C41 118.9(6) . . ?
C70 C48 C45 119.3(6) . . ?
C41 C48 C45 109.2(6) . . ?
C56 C49 C47 119.2(6) . . ?
C56 C49 C40 119.6(5) . . ?
C47 C49 C40 109.3(5) . . ?
C57 C50 C73 119.5(6) . . ?
C57 C50 C74 120.7(6) . . ?
C73 C50 C74 107.4(6) . . ?
C73 C51 C68 119.3(6) . . ?
C73 C51 C80 121.4(8) . . ?
C68 C51 C80 107.2(7) . . ?
C46 C52 C69 120.3(6) . . ?
C46 C52 C53 119.2(7) . . ?
C69 C52 C53 108.5(6) . . ?
C77 C53 C52 118.7(7) . . ?
C77 C53 C90 118.6(6) . . ?
C52 C53 C90 109.8(6) . . ?
C43 C54 C94 119.6(7) . . ?
C43 C54 C63 120.2(6) . . ?
C94 C54 C63 108.3(6) . . ?
C43 C55 C71 118.7(6) . . ?
C43 C55 C44 111.0(6) . . ?
C71 C55 C44 118.7(6) . . ?
C49 C56 C92 120.9(6) . . ?
C49 C56 C65 119.6(6) . . ?
C92 C56 C65 107.3(6) . . ?
C50 C57 C60 121.9(6) . . ?
C50 C57 C65 120.5(6) . . ?
C60 C57 C65 105.7(5) . . ?
C64 C58 C76 121.7(6) . . ?
C64 C58 C78 119.8(6) . . ?
C76 C58 C78 106.9(6) . . ?
C93 C59 C42 109.3(6) . . ?
C93 C59 C66 120.5(6) . . ?
C42 C59 C66 119.1(6) . . ?
C68 C60 C57 119.0(6) . . ?
C68 C60 C92 119.0(7) . . ?
C57 C60 C92 110.1(6) . . ?
C97 C61 C47 121.7(7) . . ?
C97 C61 C39 119.9(7) . . ?
C47 C61 C39 107.0(6) . . ?
C63 C62 C87 120.3(6) . . ?
C63 C62 C78 121.0(6) . . ?
C87 C62 C78 107.5(6) . . ?
C62 C63 C46 120.0(6) . . ?
C62 C63 C54 117.6(6) . . ?
C46 C63 C54 109.1(6) . . ?
C58 C64 C88 119.0(6) . . ?
C58 C64 C75 120.2(6) . . ?
C88 C64 C75 108.5(6) . . ?
C79 C65 C56 120.1(6) . . ?
C79 C65 C57 120.2(6) . . ?
C56 C65 C57 108.8(6) . . ?
C91 C66 C98 108.9(7) . . ?
C91 C66 C59 120.3(7) . . ?
C98 C66 C59 117.8(7) . . ?
C75 C67 C44 119.4(6) . . ?
C75 C67 C85 121.0(6) . . ?
C44 C67 C85 107.9(5) . . ?
C60 C68 C51 118.8(6) . . ?
C60 C68 C96 121.6(7) . . ?
C51 C68 C96 107.1(7) . . ?
C87 C69 C52 122.0(7) . . ?
C87 C69 C95 119.0(7) . . ?
C52 C69 C95 107.5(6) . . ?
C48 C70 C97 121.5(6) . . ?
C48 C70 C75 120.3(6) . . ?
C97 C70 C75 106.9(6) . . ?
C55 C71 C80 119.8(7) . . ?
C55 C71 C96 119.9(6) . . ?
C80 C71 C96 108.0(6) . . ?
C84 C72 C46 121.6(8) . . ?
C84 C72 C94 119.2(7) . . ?
C46 C72 C94 106.9(6) . . ?
C51 C73 C50 121.6(7) . . ?
C51 C73 C84 119.3(7) . . ?
C50 C73 C84 107.2(7) . . ?
C89 C74 C77 118.9(7) . . ?
C89 C74 C50 118.9(7) . . ?
C77 C74 C50 110.4(7) . . ?
C67 C75 C64 119.1(7) . . ?
C67 C75 C70 120.5(6) . . ?
C64 C75 C70 108.1(6) . . ?
C58 C76 C83 119.8(6) . . ?
C58 C76 C87 109.5(6) . . ?
C83 C76 C87 118.8(6) . . ?
C53 C77 C74 121.8(7) . . ?
C53 C77 C84 121.8(6) . . ?
C74 C77 C84 105.8(7) . . ?
C85 C78 C62 119.4(6) . . ?
C85 C78 C58 120.2(6) . . ?
C62 C78 C58 108.1(6) . . ?
C65 C79 C42 121.8(6) . . ?
C65 C79 C89 119.1(6) . . ?
C42 C79 C89 107.5(6) . . ?
C94 C80 C71 120.0(7) . . ?
C94 C80 C51 119.8(8) . . ?
C71 C80 C51 108.9(8) . . ?
C88 C81 C83 119.5(6) . . ?
C88 C81 C91 120.7(7) . . ?
C83 C81 C91 107.0(7) . . ?
C96 C82 C45 121.0(7) . . ?
C96 C82 C86 119.7(6) . . ?
C45 C82 C86 107.4(5) . . ?
C76 C83 C98 121.1(7) . . ?
C76 C83 C81 118.5(6) . . ?
C98 C83 C81 108.3(7) . . ?
C72 C84 C77 118.2(8) . . ?
C72 C84 C73 120.3(8) . . ?
C77 C84 C73 109.0(7) . . ?
C78 C85 C43 121.5(7) . . ?
C78 C85 C67 119.7(6) . . ?
C43 C85 C67 107.2(6) . . ?
C92 C86 C41 120.5(7) . . ?
C92 C86 C82 120.3(6) . . ?
C41 C86 C82 105.8(6) . . ?
C69 C87 C62 118.7(7) . . ?
C69 C87 C76 120.6(7) . . ?
C62 C87 C76 107.9(6) . . ?
C81 C88 C64 121.5(6) . . ?
C81 C88 C97 120.2(6) . . ?
C64 C88 C97 107.3(7) . . ?
C74 C89 C93 120.8(7) . . ?
C74 C89 C79 120.5(6) . . ?
C93 C89 C79 105.8(6) . . ?
C93 C90 C53 119.7(6) . . ?
C93 C90 C95 120.3(7) . . ?
C53 C90 C95 108.0(6) . . ?
C39 C91 C66 120.0(7) . . ?
C39 C91 C81 119.8(8) . . ?
C66 C91 C81 108.4(8) . . ?
C86 C92 C56 120.0(6) . . ?
C86 C92 C60 120.4(7) . . ?
C56 C92 C60 108.1(6) . . ?
C90 C93 C59 119.3(6) . . ?
C90 C93 C89 120.1(7) . . ?
C59 C93 C89 109.1(6) . . ?
C80 C94 C54 121.5(7) . . ?
C80 C94 C72 120.0(6) . . ?
C54 C94 C72 106.5(7) . . ?
C98 C95 C90 120.6(8) . . ?
C98 C95 C69 120.4(8) . . ?
C90 C95 C69 106.2(6) . . ?
C82 C96 C71 120.0(6) . . ?
C82 C96 C68 118.9(7) . . ?
C71 C96 C68 108.8(6) . . ?
C61 C97 C70 119.0(7) . . ?
C61 C97 C88 119.4(8) . . ?
C70 C97 C88 109.2(6) . . ?
C95 C98 C83 120.2(8) . . ?
C95 C98 C66 121.5(8) . . ?
C83 C98 C66 107.4(7) . . ?
C23 O1 C26 107.0(3) . . ?
C18 O2 C21 106.7(3) . . ?
C16 O3 C13 106.8(3) . . ?
C11 O4 C8 106.1(3) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.137 269 84 ' '
2 0.000 0.248 0.407 16 1 ' '
3 0.000 0.252 0.907 16 1 ' '
4 0.000 0.500 0.637 269 84 ' '
5 0.000 0.748 0.907 16 1 ' '
6 0.000 0.752 0.407 16 1 ' '
7 0.058 0.161 0.142 24 1 ' '
8 0.058 0.661 0.642 24 1 ' '
9 0.250 0.250 0.387 269 84 ' '
10 0.250 0.750 0.887 269 84 ' '
11 0.192 0.411 0.392 24 1 ' '
12 0.192 0.911 0.892 24 1 ' '
13 0.250 -0.002 0.157 16 1 ' '
14 0.250 0.002 0.657 16 1 ' '
15 0.250 0.498 0.657 16 1 ' '
16 0.250 0.502 0.157 16 1 ' '
17 0.308 0.089 0.392 24 1 ' '
18 0.308 0.589 0.892 24 1 ' '
19 0.500 0.500 0.137 269 84 ' '
20 0.500 1.000 0.637 269 84 ' '
21 0.442 0.339 0.142 24 1 ' '
22 0.442 0.839 0.642 24 1 ' '
23 0.500 0.248 0.907 16 1 ' '
24 0.500 0.252 0.407 16 1 ' '
25 0.500 0.748 0.407 16 1 ' '
26 0.500 0.752 0.907 16 1 ' '
27 0.558 0.161 0.642 24 1 ' '
28 0.558 0.661 0.142 24 1 ' '
29 0.750 0.250 0.887 269 84 ' '
30 0.750 0.750 0.387 269 84 ' '
31 0.692 0.411 0.892 24 1 ' '
32 0.692 0.911 0.392 24 1 ' '
33 0.750 -0.002 0.657 16 1 ' '
34 0.750 0.002 0.157 16 1 ' '
35 0.750 0.498 0.157 16 1 ' '
36 0.750 0.502 0.657 16 1 ' '
37 0.808 0.089 0.892 24 1 ' '
38 0.808 0.589 0.392 24 1 ' '
39 0.942 0.339 0.642 24 1 ' '
40 0.942 0.839 0.142 24 1 ' '
_platon_squeeze_details          
;
;



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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1437308'
_audit_update_record             
;
2015-11-17 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84.86 H11.14 F8.57 O3.43'
_chemical_formula_sum            'C84.86 H11.14 F8.57 O3.43'
_chemical_formula_weight         1248.08

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'

_space_group_crystal_system      cubic
_space_group_IT_number           203
_space_group_name_H-M_alt        'F d -3'
_space_group_name_Hall           '-F 2uv 2vw 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'z, x, y'
'y, z, x'
'-y+1/4, -z+1/4, x'
'z, -x+1/4, -y+1/4'
'-y+1/4, z, -x+1/4'
'-z+1/4, -x+1/4, y'
'-z+1/4, x, -y+1/4'
'y, -z+1/4, -x+1/4'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'-x+1/4, -y+1/4, z'
'x, y+1/2, z+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y+1/4, -z+3/4, x+1/2'
'z, -x+3/4, -y+3/4'
'-y+1/4, z+1/2, -x+3/4'
'-z+1/4, -x+3/4, y+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, -z+3/4, -x+3/4'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'-x+1/4, -y+3/4, z+1/2'
'x+1/2, y, z+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+3/4, -z+1/4, x+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-y+3/4, z, -x+3/4'
'-z+3/4, -x+1/4, y+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, -z+1/4, -x+3/4'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, y+1/2, z'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+3/4, -z+3/4, x'
'z+1/2, -x+3/4, -y+1/4'
'-y+3/4, z+1/2, -x+1/4'
'-z+3/4, -x+3/4, y'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, -z+3/4, -x+1/4'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x+3/4, -y+3/4, z'
'-x, -y, -z'
'-z, -x, -y'
'-y, -z, -x'
'y-1/4, z-1/4, -x'
'-z, x-1/4, y-1/4'
'y-1/4, -z, x-1/4'
'z-1/4, x-1/4, -y'
'z-1/4, -x, y-1/4'
'-y, z-1/4, x-1/4'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'x-1/4, y-1/4, -z'
'-x, -y+1/2, -z+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y-1/4, z+1/4, -x+1/2'
'-z, x+1/4, y+1/4'
'y-1/4, -z+1/2, x+1/4'
'z-1/4, x+1/4, -y+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, z+1/4, x+1/4'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'x-1/4, y+1/4, -z+1/2'
'-x+1/2, -y, -z+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/4, z-1/4, -x+1/2'
'-z+1/2, x-1/4, y+1/4'
'y+1/4, -z, x+1/4'
'z+1/4, x-1/4, -y+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, z-1/4, x+1/4'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, -y+1/2, -z'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/4, z+1/4, -x'
'-z+1/2, x+1/4, y-1/4'
'y+1/4, -z+1/2, x-1/4'
'z+1/4, x+1/4, -y'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, z+1/4, x-1/4'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
'x+1/4, y+1/4, -z'

_cell_length_a                   57.756(6)
_cell_length_b                   57.756(6)
_cell_length_c                   57.756(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     192656(58)
_cell_formula_units_Z            112
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9626
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      19.75

_exptl_crystal_description       CUBE
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             69984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.089
_shelx_estimated_absorpt_T_min   0.965
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_process_details   'MULTI-SCAN Absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            754013
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.1793
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_theta_min         0.611
_diffrn_reflns_theta_max         25.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14973
_reflns_number_gt                8582
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 Structure factors included contributions from the .fab file.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2100P)²+0.5883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14973
_refine_ls_number_parameters     1019
_refine_ls_number_restraints     121
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.1296
_refine_ls_wR_factor_ref         0.4364
_refine_ls_wR_factor_gt          0.3647
_refine_ls_goodness_of_fit_ref   1.557
_refine_ls_restrained_S_all      1.659
_refine_ls_shift/su_max          0.155
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.61484(9) 0.80885(9) 0.07060(9) 0.0398(12) Uani 1 1 d . . . . .
C2 C 0.63381(9) 0.80048(9) 0.08428(9) 0.0432(13) Uani 1 1 d . . . . .
H2 H 0.6419 0.7864 0.0817 0.052 Uiso 1 1 calc R U . . .
C3 C 0.63837(9) 0.81558(9) 0.10117(9) 0.0410(12) Uani 1 1 d . . . . .
H3 H 0.6502 0.8142 0.1125 0.049 Uiso 1 1 calc R U . . .
C4 C 0.62221(8) 0.83431(9) 0.09911(8) 0.0356(11) Uani 1 1 d . . . . .
C5 C 0.61853(8) 0.85209(8) 0.11387(8) 0.0341(11) Uani 1 1 d . . . . .
C6 C 0.60303(8) 0.87173(9) 0.11084(8) 0.0359(11) Uani 1 1 d . . . . .
C7 C 0.59458(9) 0.88643(9) 0.12701(9) 0.0405(12) Uani 1 1 d . . . . .
H7 H 0.5965 0.8852 0.1433 0.049 Uiso 1 1 calc R U . . .
C8 C 0.58243(8) 0.90376(9) 0.11519(9) 0.0393(12) Uani 1 1 d . . . . .
H8 H 0.5745 0.9165 0.1219 0.047 Uiso 1 1 calc R U . . .
C9 C 0.58404(8) 0.89888(8) 0.09226(9) 0.0374(11) Uani 1 1 d . . . . .
C10 C 0.57515(8) 0.91161(8) 0.07249(8) 0.0345(11) Uani 1 1 d . . . . .
C11 C 0.56858(8) 0.90346(8) 0.05178(8) 0.0347(11) Uani 1 1 d . . . . .
C12 C 0.55913(8) 0.91601(9) 0.03242(9) 0.0380(12) Uani 1 1 d . . . . .
H12 H 0.5570 0.9323 0.0315 0.046 Uiso 1 1 calc R U . . .
C13 C 0.55383(9) 0.90036(9) 0.01585(9) 0.0394(12) Uani 1 1 d . . . . .
H13 H 0.5470 0.9038 0.0013 0.047 Uiso 1 1 calc R U . . .
C14 C 0.56018(8) 0.87789(8) 0.02384(8) 0.0309(10) Uani 1 1 d . . . . .
C15 C 0.55818(8) 0.85732(9) 0.01258(8) 0.0333(11) Uani 1 1 d . . . . .
C16 C 0.56594(8) 0.83456(8) 0.01944(8) 0.0330(11) Uani 1 1 d . . . . .
C17 C 0.55955(9) 0.81366(9) 0.01099(8) 0.0378(12) Uani 1 1 d . . . . .
H17 H 0.5484 0.8109 -0.0008 0.045 Uiso 1 1 calc R U . . .
C18 C 0.57222(9) 0.79702(9) 0.02256(8) 0.0376(11) Uani 1 1 d . . . . .
H18 H 0.5713 0.7808 0.0203 0.045 Uiso 1 1 calc R U . . .
C19 C 0.58617(9) 0.80813(8) 0.03779(8) 0.0369(12) Uani 1 1 d . . . . .
C20 C 0.60387(9) 0.79890(8) 0.05277(8) 0.0361(11) Uani 1 1 d . . . . .
C21 C 0.57220(9) 0.93682(9) 0.07708(9) 0.0396(12) Uani 1 1 d . . . . .
C22 C 0.59104(10) 0.95059(9) 0.08367(10) 0.0478(14) Uani 1 1 d . . . . .
C23 C 0.58892(12) 0.97369(11) 0.08858(12) 0.0606(17) Uani 1 1 d . . . . .
C24 C 0.56729(12) 0.98421(9) 0.08725(12) 0.0587(17) Uani 1 1 d . . . . .
C25 C 0.54847(11) 0.97125(10) 0.08103(11) 0.0549(16) Uani 1 1 d . . . . .
C26 C 0.55077(9) 0.94764(9) 0.07628(9) 0.0417(12) Uani 1 1 d . . . . .
C27 C 0.54530(8) 0.85748(9) -0.00974(8) 0.0355(11) Uani 1 1 d . . . . .
C28 C 0.55680(9) 0.85325(9) -0.03071(8) 0.0378(12) Uani 1 1 d . . . . .
H28 H 0.5731 0.8509 -0.0309 0.045 Uiso 1 1 calc R U . . .
C29 C 0.54445(10) 0.85259(9) -0.05102(9) 0.0451(13) Uani 1 1 d . . . . .
H29 H 0.5524 0.8493 -0.0651 0.054 Uiso 1 1 calc R U . . .
C30 C 0.52097(10) 0.85651(10) -0.05158(10) 0.0501(14) Uani 1 1 d . . . . .
H30 H 0.5128 0.8561 -0.0658 0.060 Uiso 1 1 calc R U . . .
C31 C 0.50946(10) 0.86112(12) -0.03113(11) 0.0585(16) Uani 1 1 d . . . . .
H31 H 0.4932 0.8638 -0.0312 0.070 Uiso 1 1 calc R U . . .
C32 C 0.52158(9) 0.86178(10) -0.01049(10) 0.0481(14) Uani 1 1 d . . . . .
H32 H 0.5136 0.8652 0.0035 0.058 Uiso 1 1 calc R U . . .
C33 C 0.61059(10) 0.77401(9) 0.04786(9) 0.0443(13) Uani 1 1 d . . . . .
C34 C 0.59611(13) 0.75608(11) 0.05367(13) 0.0666(18) Uani 1 1 d . . . . .
C35 C 0.60197(17) 0.73313(13) 0.04942(17) 0.094(3) Uani 1 1 d . . . . .
C36 C 0.62284(16) 0.72829(12) 0.03968(13) 0.077(2) Uani 1 1 d . . . . .
C37 C 0.63784(13) 0.74571(12) 0.03371(10) 0.0623(18) Uani 1 1 d . . . . .
C38 C 0.63133(11) 0.76817(10) 0.03717(10) 0.0502(14) Uani 1 1 d . . . . .
C40 C 0.6392(2) 0.84102(16) 0.0017(2) 0.113(3) Uani 1 1 d . . . . .
C41 C 0.64143(17) 0.9408(2) 0.0205(4) 0.179(8) Uani 1 1 d . . . . .
C42 C 0.6607(3) 0.8798(3) -0.05390(13) 0.118(4) Uani 1 1 d . . . . .
C43 C 0.70283(17) 0.84022(19) -0.0079(3) 0.152(7) Uani 1 1 d . . . . .
C44 C 0.6274(3) 0.9342(2) 0.0029(3) 0.141(4) Uani 1 1 d . U . . .
C45 C 0.7266(2) 0.8657(4) -0.0071(3) 0.200(10) Uani 1 1 d . . . . .
C46 C 0.6480(3) 0.8617(2) -0.04237(19) 0.134(5) Uani 1 1 d . . . . .
C47 C 0.71823(18) 0.92909(18) 0.0177(2) 0.119(5) Uani 1 1 d . . . . .
C48 C 0.71443(13) 0.91768(12) 0.04025(14) 0.070(2) Uani 1 1 d . . . . .
C49 C 0.69537(15) 0.92251(14) 0.05190(13) 0.076(2) Uani 1 1 d . . . . .
C50 C 0.68313(15) 0.90413(17) 0.06319(11) 0.079(2) Uani 1 1 d . . . . .
C51 C 0.6430(3) 0.84303(18) 0.02721(16) 0.114(5) Uani 1 1 d . . . . .
C52 C 0.67938(16) 0.93874(14) 0.04257(15) 0.077(2) Uani 1 1 d . . . . .
C53 C 0.6723(3) 0.86304(15) 0.05871(12) 0.110(4) Uani 1 1 d . . . . .
C54 C 0.7116(2) 0.87610(15) 0.0487(2) 0.104(4) Uani 1 1 d . . . . .
C55 C 0.73066(14) 0.9099(2) 0.00073(16) 0.102(3) Uani 1 1 d . . . . .
C56 C 0.69171(17) 0.8806(2) 0.06148(12) 0.092(3) Uani 1 1 d . . . . .
C57 C 0.63569(19) 0.8594(3) 0.04170(17) 0.122(5) Uani 1 1 d . . . . .
C58 C 0.72292(13) 0.89408(15) 0.03909(17) 0.086(3) Uani 1 1 d . . . . .
C59 C 0.65073(16) 0.8734(2) 0.05848(12) 0.093(3) Uani 1 1 d . U . . .
C60 C 0.6647(2) 0.8443(2) -0.0329(2) 0.126(5) Uani 1 1 d . . . . .
C61 C 0.73239(12) 0.8894(2) 0.0153(2) 0.108(4) Uani 1 1 d . . . . .
C62 C 0.61951(19) 0.91800(19) 0.0174(2) 0.117(3) Uani 1 1 d D U . . .
C63 C 0.69672(14) 0.9023(3) -0.05024(13) 0.097(3) Uani 1 1 d . . . . .
C64 C 0.7237(3) 0.8592(3) 0.0102(3) 0.159(5) Uani 1 1 d . U . . .
C65 C 0.6635(3) 0.95130(14) 0.0051(3) 0.171(7) Uani 1 1 d . . . . .
C66 C 0.6543(2) 0.8985(3) 0.06199(15) 0.133(4) Uani 1 1 d . U . . .
C67 C 0.6512(3) 0.9387(2) -0.0273(2) 0.126(4) Uani 1 1 d . U . . .
C68 C 0.6865(4) 0.8797(3) -0.05309(17) 0.161(7) Uani 1 1 d . . . . .
C69 C 0.6516(2) 0.9027(3) -0.05135(15) 0.107(4) Uani 1 1 d . . . . .
C70 C 0.63162(15) 0.92880(18) -0.02125(18) 0.093(3) Uani 1 1 d . . . . .
C71 C 0.70703(19) 0.93351(19) -0.0222(3) 0.130(5) Uani 1 1 d . . . . .
C72 C 0.62090(15) 0.8745(2) 0.03160(14) 0.102(3) Uani 1 1 d . . . . .
C73 C 0.61428(10) 0.87322(13) 0.00878(13) 0.0657(19) Uani 1 1 d . . . . .
C74 C 0.68467(18) 0.94825(15) 0.0222(3) 0.114(4) Uani 1 1 d . . . . .
C75 C 0.61259(12) 0.89206(18) -0.0044(2) 0.104(4) Uani 1 1 d . . . . .
C76 C 0.7062(3) 0.9419(3) 0.0077(2) 0.179(8) Uani 1 1 d . . . . .
C77 C 0.6920(3) 0.9450(2) -0.0170(2) 0.127(4) Uani 1 1 d . U . . .
C78 C 0.6323(2) 0.9048(2) -0.0387(2) 0.136(5) Uani 1 1 d . . . . .
C79 C 0.62460(16) 0.85537(18) -0.00596(19) 0.101(3) Uani 1 1 d . U . . .
C80 C 0.6798(3) 0.8450(3) 0.0447(3) 0.137(4) Uani 1 1 d . U . . .
C81 C 0.6692(4) 0.8355(2) 0.0273(4) 0.205(10) Uani 1 1 d . . . . .
C82 C 0.62231(19) 0.8885(2) -0.0295(2) 0.130(5) Uani 1 1 d . . . . .
C83 C 0.6954(3) 0.8483(3) -0.0321(2) 0.152(6) Uani 1 1 d . . . . .
C84 C 0.6541(3) 0.93365(19) 0.0446(2) 0.138(5) Uani 1 1 d . . . . .
C85 C 0.6663(2) 0.9235(2) -0.04671(19) 0.115(3) Uani 1 1 d . U . . .
C86 C 0.6709(3) 0.9445(3) -0.0242(3) 0.167(5) Uani 1 1 d . U . . .
C87 C 0.6470(3) 0.9160(4) 0.0517(3) 0.182(6) Uani 1 1 d . U . . .
C88 C 0.62346(15) 0.9093(2) 0.03656(16) 0.091(3) Uani 1 1 d . U . . .
C89 C 0.6262(3) 0.8918(3) 0.0448(3) 0.150(5) Uani 1 1 d . U . . .
C90 C 0.6176(3) 0.9122(3) -0.0053(3) 0.162(5) Uani 1 1 d D U . . .
C91 C 0.72191(13) 0.87498(18) -0.02733(17) 0.086(3) Uani 1 1 d . . . . .
C92 C 0.62922(18) 0.8658(2) -0.02994(16) 0.096(3) Uani 1 1 d . . . . .
C93 C 0.7230(3) 0.8972(3) -0.0282(3) 0.175(5) Uani 1 1 d . U . . .
C94 C 0.6947(5) 0.8618(3) -0.0435(3) 0.235(13) Uani 1 1 d . . . . .
C95 C 0.6796(4) 0.83138(15) 0.0050(2) 0.154(7) Uani 1 1 d . . . . .
C96 C 0.65934(16) 0.83430(14) -0.0123(3) 0.103(4) Uani 1 1 d . . . . .
C97 C 0.7182(2) 0.9158(2) -0.0266(2) 0.128(4) Uani 1 1 d . U . . .
C98 C 0.6848(3) 0.9191(2) -0.04828(18) 0.117(4) Uani 1 1 d . U . . .
C99 C 0.6986(4) 0.8465(3) 0.0364(3) 0.166(5) Uani 1 1 d . U . . .
C100 C 0.71399(17) 0.85518(17) 0.0303(2) 0.102(3) Uani 1 1 d . U . . .
F1 F 0.61217(5) 0.94125(6) 0.08520(6) 0.0581(9) Uani 1 1 d . . . . .
F2 F 0.60739(7) 0.98610(7) 0.09475(8) 0.0838(13) Uani 1 1 d . . . . .
F3 F 0.56500(8) 1.00666(6) 0.09187(9) 0.0905(14) Uani 1 1 d . . . . .
F4 F 0.52745(7) 0.98132(6) 0.07937(7) 0.0716(11) Uani 1 1 d . . . . .
F5 F 0.53177(5) 0.93576(5) 0.07113(5) 0.0483(8) Uani 1 1 d . . . . .
F6 F 0.57587(8) 0.76053(7) 0.06444(9) 0.0905(14) Uani 1 1 d . . . . .
F7 F 0.58765(11) 0.71631(8) 0.05572(13) 0.140(2) Uani 1 1 d . . . . .
F8 F 0.62874(11) 0.70622(7) 0.03579(10) 0.122(2) Uani 1 1 d . . . . .
F9 F 0.65770(8) 0.74054(7) 0.02384(7) 0.0910(15) Uani 1 1 d . . . . .
F10 F 0.64578(6) 0.78487(6) 0.03061(6) 0.0673(10) Uani 1 1 d . . . . .
O1 O 0.60870(6) 0.83062(5) 0.07956(5) 0.0349(8) Uani 1 1 d . . . . .
O2 O 0.59656(5) 0.87878(5) 0.08900(5) 0.0304(7) Uani 1 1 d . . . . .
O3 O 0.56988(5) 0.88012(5) 0.04600(5) 0.0333(8) Uani 1 1 d . . . . .
O4 O 0.58238(5) 0.83141(5) 0.03639(5) 0.0330(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C20 1.339(7) . ?
C1 O1 1.405(6) . ?
C1 C2 1.435(7) . ?
C2 C3 1.335(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.434(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.351(7) . ?
C4 O1 1.389(6) . ?
C5 C6 1.455(7) . ?
C5 C5 1.487(9) 11_655 ?
C6 C7 1.353(7) . ?
C6 O2 1.377(5) . ?
C7 C8 1.400(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.357(7) . ?
C8 H8 0.9500 . ?
C9 O2 1.380(6) . ?
C9 C10 1.452(7) . ?
C10 C11 1.340(7) . ?
C10 C21 1.490(7) . ?
C11 O3 1.391(6) . ?
C11 C12 1.440(7) . ?
C12 C13 1.352(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.425(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.360(7) . ?
C14 O3 1.403(5) . ?
C15 C16 1.444(7) . ?
C15 C27 1.488(6) . ?
C16 C17 1.353(7) . ?
C16 O4 1.376(6) . ?
C17 C18 1.381(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.354(7) . ?
C18 H18 0.9500 . ?
C19 O4 1.365(6) . ?
C19 C20 1.442(7) . ?
C20 C33 1.516(7) . ?
C21 C26 1.387(7) . ?
C21 C22 1.400(8) . ?
C22 F1 1.337(7) . ?
C22 C23 1.370(8) . ?
C23 F2 1.334(7) . ?
C23 C24 1.391(9) . ?
C24 F3 1.330(7) . ?
C24 C25 1.368(9) . ?
C25 F4 1.350(7) . ?
C25 C26 1.397(8) . ?
C26 F5 1.328(6) . ?
C27 C32 1.393(7) . ?
C27 C28 1.402(7) . ?
C28 C29 1.373(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(8) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.373(9) . ?
C33 C38 1.389(8) . ?
C34 F6 1.349(8) . ?
C34 C35 1.390(10) . ?
C35 F7 1.327(10) . ?
C35 C36 1.359(12) . ?
C36 F8 1.338(7) . ?
C36 C37 1.372(11) . ?
C37 F9 1.316(8) . ?
C37 C38 1.365(8) . ?
C38 F10 1.331(7) . ?
C40 C79 1.265(13) . ?
C40 C96 1.468(15) . ?
C40 C51 1.493(14) . ?
C41 C44 1.355(19) . ?
C41 C84 1.63(2) . ?
C41 C65 1.67(2) . ?
C41 C62 1.836(17) . ?
C42 C69 1.434(17) . ?
C42 C46 1.442(16) . ?
C42 C68 1.49(2) . ?
C43 C83 1.54(2) . ?
C43 C95 1.62(2) . ?
C43 C64 1.93(2) . ?
C43 C45 2.01(2) . ?
C44 C62 1.335(16) . ?
C44 C70 1.452(17) . ?
C44 C90 1.47(2) . ?
C45 C64 1.078(17) . ?
C45 C91 1.316(16) . ?
C45 C61 1.91(2) . ?
C46 C92 1.321(18) . ?
C46 C60 1.498(18) . ?
C47 C76 1.167(19) . ?
C47 C48 1.477(13) . ?
C47 C55 1.643(16) . ?
C48 C49 1.320(11) . ?
C48 C58 1.450(11) . ?
C49 C52 1.422(11) . ?
C49 C50 1.432(12) . ?
C50 C56 1.449(13) . ?
C50 C66 1.697(16) . ?
C51 C57 1.334(16) . ?
C51 C81 1.57(2) . ?
C52 C74 1.333(15) . ?
C52 C84 1.493(16) . ?
C53 C59 1.385(15) . ?
C53 C80 1.388(18) . ?
C53 C56 1.519(14) . ?
C54 C58 1.346(13) . ?
C54 C56 1.391(14) . ?
C54 C100 1.618(15) . ?
C54 C99 2.00(2) . ?
C55 C61 1.457(15) . ?
C55 C97 1.769(18) . ?
C55 C93 1.88(2) . ?
C57 C72 1.351(16) . ?
C57 C59 1.532(13) . ?
C57 C89 1.96(2) . ?
C58 C61 1.504(14) . ?
C59 C66 1.474(16) . ?
C59 C89 1.94(2) . ?
C60 C96 1.359(17) . ?
C60 C83 1.79(2) . ?
C61 C64 1.84(2) . ?
C62 C88 1.236(14) . ?
C62 C90 1.356(14) . ?
C62 C75 1.999(18) . ?
C63 C98 1.198(15) . ?
C63 C68 1.438(18) . ?
C63 C93 2.00(2) . ?
C63 C97 2.004(17) . ?
C64 C100 1.308(17) . ?
C65 C74 1.582(17) . ?
C65 C86 1.79(2) . ?
C66 C87 1.25(2) . ?
C66 C89 1.94(2) . ?
C67 C86 1.205(18) . ?
C67 C70 1.313(16) . ?
C67 C85 1.671(19) . ?
C68 C94 1.265(19) . ?
C69 C78 1.338(17) . ?
C69 C85 1.496(16) . ?
C70 C90 1.56(2) . ?
C70 C78 1.713(18) . ?
C71 C77 1.133(16) . ?
C71 C97 1.235(15) . ?
C71 C76 1.796(19) . ?
C72 C89 1.296(17) . ?
C72 C73 1.374(11) . ?
C72 C88 2.036(18) . ?
C73 C75 1.332(11) . ?
C73 C79 1.464(13) . ?
C74 C76 1.54(2) . ?
C75 C90 1.200(19) . ?
C75 C82 1.567(17) . ?
C76 C77 1.657(19) . ?
C77 C86 1.286(19) . ?
C78 C82 1.225(14) . ?
C79 C92 1.534(14) . ?
C80 C99 1.192(19) . ?
C80 C81 1.30(2) . ?
C81 C95 1.44(3) . ?
C81 C99 1.89(3) . ?
C82 C92 1.371(15) . ?
C82 C90 1.98(2) . ?
C83 C94 1.019(18) . ?
C84 C87 1.17(2) . ?
C85 C98 1.098(15) . ?
C85 C86 1.80(2) . ?
C87 C88 1.66(2) . ?
C87 C89 1.88(3) . ?
C88 C89 1.129(16) . ?
C91 C93 1.288(17) . ?
C91 C94 1.98(3) . ?
C93 C97 1.114(17) . ?
C95 C96 1.549(19) . ?
C99 C100 1.079(19) . ?

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
C20 C1 O1 123.2(5) . . ?
C20 C1 C2 129.8(5) . . ?
O1 C1 C2 106.9(4) . . ?
C3 C2 C1 109.4(5) . . ?
C3 C2 H2 125.3 . . ?
C1 C2 H2 125.3 . . ?
C2 C3 C4 107.7(5) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
C5 C4 O1 122.8(4) . . ?
C5 C4 C3 128.6(5) . . ?
O1 C4 C3 108.5(4) . . ?
C4 C5 C6 127.8(4) . . ?
C4 C5 C5 117.8(4) . 11_655 ?
C6 C5 C5 114.4(3) . 11_655 ?
C7 C6 O2 110.4(4) . . ?
C7 C6 C5 128.9(4) . . ?
O2 C6 C5 120.5(4) . . ?
C6 C7 C8 107.0(4) . . ?
C6 C7 H7 126.5 . . ?
C8 C7 H7 126.5 . . ?
C9 C8 C7 107.1(4) . . ?
C9 C8 H8 126.5 . . ?
C7 C8 H8 126.5 . . ?
C8 C9 O2 110.1(4) . . ?
C8 C9 C10 129.6(5) . . ?
O2 C9 C10 120.3(4) . . ?
C11 C10 C9 128.6(4) . . ?
C11 C10 C21 118.0(4) . . ?
C9 C10 C21 113.3(4) . . ?
C10 C11 O3 122.6(4) . . ?
C10 C11 C12 128.6(5) . . ?
O3 C11 C12 108.8(4) . . ?
C13 C12 C11 107.4(4) . . ?
C13 C12 H12 126.3 . . ?
C11 C12 H12 126.3 . . ?
C12 C13 C14 108.8(4) . . ?
C12 C13 H13 125.6 . . ?
C14 C13 H13 125.6 . . ?
C15 C14 O3 123.4(4) . . ?
C15 C14 C13 128.2(4) . . ?
O3 C14 C13 108.3(4) . . ?
C14 C15 C16 129.6(4) . . ?
C14 C15 C27 116.8(4) . . ?
C16 C15 C27 113.5(4) . . ?
C17 C16 O4 109.1(4) . . ?
C17 C16 C15 128.9(4) . . ?
O4 C16 C15 122.0(4) . . ?
C16 C17 C18 107.6(4) . . ?
C16 C17 H17 126.2 . . ?
C18 C17 H17 126.2 . . ?
C19 C18 C17 107.4(5) . . ?
C19 C18 H18 126.3 . . ?
C17 C18 H18 126.3 . . ?
C18 C19 O4 109.5(4) . . ?
C18 C19 C20 129.5(5) . . ?
O4 C19 C20 120.9(4) . . ?
C1 C20 C19 129.7(5) . . ?
C1 C20 C33 115.5(5) . . ?
C19 C20 C33 114.8(4) . . ?
C26 C21 C22 116.5(5) . . ?
C26 C21 C10 122.4(5) . . ?
C22 C21 C10 121.0(5) . . ?
F1 C22 C23 117.4(5) . . ?
F1 C22 C21 119.9(5) . . ?
C23 C22 C21 122.7(6) . . ?
F2 C23 C22 120.5(6) . . ?
F2 C23 C24 119.9(5) . . ?
C22 C23 C24 119.6(6) . . ?
F3 C24 C25 120.5(6) . . ?
F3 C24 C23 120.3(6) . . ?
C25 C24 C23 119.2(5) . . ?
F4 C25 C24 119.8(5) . . ?
F4 C25 C26 119.5(6) . . ?
C24 C25 C26 120.7(6) . . ?
F5 C26 C21 120.8(4) . . ?
F5 C26 C25 118.0(5) . . ?
C21 C26 C25 121.2(5) . . ?
C32 C27 C28 118.0(5) . . ?
C32 C27 C15 121.3(4) . . ?
C28 C27 C15 120.7(4) . . ?
C29 C28 C27 119.8(5) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 121.8(5) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C29 C30 C31 119.1(5) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C32 C31 C30 119.9(5) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C27 121.3(5) . . ?
C31 C32 H32 119.3 . . ?
C27 C32 H32 119.3 . . ?
C34 C33 C38 116.8(5) . . ?
C34 C33 C20 120.9(5) . . ?
C38 C33 C20 122.3(5) . . ?
F6 C34 C33 119.8(5) . . ?
F6 C34 C35 118.3(7) . . ?
C33 C34 C35 121.8(7) . . ?
F7 C35 C36 121.1(7) . . ?
F7 C35 C34 119.9(9) . . ?
C36 C35 C34 119.0(8) . . ?
F8 C36 C35 119.4(8) . . ?
F8 C36 C37 119.7(8) . . ?
C35 C36 C37 120.9(6) . . ?
F9 C37 C38 121.3(7) . . ?
F9 C37 C36 119.6(6) . . ?
C38 C37 C36 119.1(7) . . ?
F10 C38 C37 118.3(6) . . ?
F10 C38 C33 119.4(5) . . ?
C37 C38 C33 122.2(6) . . ?
C79 C40 C96 120.5(12) . . ?
C79 C40 C51 113.2(12) . . ?
C96 C40 C51 116.7(12) . . ?
C44 C41 C84 147.1(14) . . ?
C44 C41 C65 99.3(16) . . ?
C84 C41 C65 101.8(8) . . ?
C44 C41 C62 46.5(8) . . ?
C84 C41 C62 102.2(13) . . ?
C65 C41 C62 137.4(11) . . ?
C69 C42 C46 115.7(14) . . ?
C69 C42 C68 111.5(12) . . ?
C46 C42 C68 119.7(16) . . ?
C83 C43 C95 106.4(10) . . ?
C83 C43 C64 119.6(13) . . ?
C95 C43 C64 116.6(13) . . ?
C83 C43 C45 89.4(13) . . ?
C95 C43 C45 141.9(10) . . ?
C64 C43 C45 31.6(6) . . ?
C62 C44 C41 86.1(14) . . ?
C62 C44 C70 120.6(13) . . ?
C41 C44 C70 132.8(14) . . ?
C62 C44 C90 57.6(9) . . ?
C41 C44 C90 135.6(13) . . ?
C70 C44 C90 64.4(11) . . ?
C64 C45 C91 158.8(13) . . ?
C64 C45 C61 69.6(16) . . ?
C91 C45 C61 110.1(14) . . ?
C64 C45 C43 70.2(16) . . ?
C91 C45 C43 97.9(13) . . ?
C61 C45 C43 131.2(10) . . ?
C92 C46 C42 122.6(15) . . ?
C92 C46 C60 116.9(11) . . ?
C42 C46 C60 108.9(16) . . ?
C76 C47 C48 129.1(15) . . ?
C76 C47 C55 113.1(14) . . ?
C48 C47 C55 106.9(8) . . ?
C49 C48 C58 120.3(8) . . ?
C49 C48 C47 118.7(8) . . ?
C58 C48 C47 109.2(9) . . ?
C48 C49 C52 119.2(8) . . ?
C48 C49 C50 119.2(8) . . ?
C52 C49 C50 109.9(8) . . ?
C49 C50 C56 119.7(8) . . ?
C49 C50 C66 127.5(8) . . ?
C56 C50 C66 98.7(8) . . ?
C57 C51 C40 128.9(12) . . ?
C57 C51 C81 120.0(11) . . ?
C40 C51 C81 97.0(13) . . ?
C74 C52 C49 117.2(9) . . ?
C74 C52 C84 112.0(10) . . ?
C49 C52 C84 118.4(9) . . ?
C59 C53 C80 126.9(12) . . ?
C59 C53 C56 112.0(8) . . ?
C80 C53 C56 109.4(13) . . ?
C58 C54 C56 118.4(9) . . ?
C58 C54 C100 105.2(11) . . ?
C56 C54 C100 123.9(9) . . ?
C58 C54 C99 133.9(10) . . ?
C56 C54 C99 92.2(9) . . ?
C100 C54 C99 32.5(6) . . ?
C61 C55 C47 103.6(8) . . ?
C61 C55 C97 134.4(9) . . ?
C47 C55 C97 103.0(9) . . ?
C61 C55 C93 102.2(10) . . ?
C47 C55 C93 133.7(9) . . ?
C97 C55 C93 35.4(6) . . ?
C54 C56 C50 119.6(9) . . ?
C54 C56 C53 115.4(10) . . ?
C50 C56 C53 112.4(9) . . ?
C51 C57 C72 112.8(10) . . ?
C51 C57 C59 126.3(12) . . ?
C72 C57 C59 107.0(12) . . ?
C51 C57 C89 145.7(9) . . ?
C72 C57 C89 41.3(8) . . ?
C59 C57 C89 66.1(9) . . ?
C54 C58 C48 122.8(9) . . ?
C54 C58 C61 114.5(9) . . ?
C48 C58 C61 109.6(8) . . ?
C53 C59 C66 107.3(8) . . ?
C53 C59 C57 106.7(11) . . ?
C66 C59 C57 133.2(11) . . ?
C53 C59 C89 154.1(7) . . ?
C66 C59 C89 67.8(9) . . ?
C57 C59 C89 67.5(8) . . ?
C96 C60 C46 117.1(11) . . ?
C96 C60 C83 105.0(12) . . ?
C46 C60 C83 124.3(12) . . ?
C55 C61 C58 110.8(8) . . ?
C55 C61 C64 131.4(10) . . ?
C58 C61 C64 102.6(10) . . ?
C55 C61 C45 100.5(10) . . ?
C58 C61 C45 133.0(9) . . ?
C64 C61 C45 33.3(6) . . ?
C88 C62 C44 141.6(15) . . ?
C88 C62 C90 141.1(13) . . ?
C44 C62 C90 66.2(11) . . ?
C88 C62 C41 94.5(12) . . ?
C44 C62 C41 47.4(11) . . ?
C90 C62 C41 109.1(13) . . ?
C88 C62 C75 107.2(9) . . ?
C44 C62 C75 101.5(11) . . ?
C90 C62 C75 35.9(10) . . ?
C41 C62 C75 137.5(9) . . ?
C98 C63 C68 120.7(13) . . ?
C98 C63 C93 119.7(12) . . ?
C68 C63 C93 104.5(12) . . ?
C98 C63 C97 88.6(12) . . ?
C68 C63 C97 133.3(11) . . ?
C93 C63 C97 32.3(5) . . ?
C45 C64 C100 161.4(13) . . ?
C45 C64 C61 77.0(17) . . ?
C100 C64 C61 98.3(12) . . ?
C45 C64 C43 78.1(17) . . ?
C100 C64 C43 96.4(14) . . ?
C61 C64 C43 142.5(9) . . ?
C74 C65 C41 102.6(11) . . ?
C74 C65 C86 112.3(14) . . ?
C41 C65 C86 127.5(12) . . ?
C87 C66 C59 133.0(16) . . ?
C87 C66 C50 101.4(15) . . ?
C59 C66 C50 109.4(8) . . ?
C87 C66 C89 68.5(13) . . ?
C59 C66 C89 67.5(10) . . ?
C50 C66 C89 151.5(7) . . ?
C86 C67 C70 153.7(13) . . ?
C86 C67 C85 75.5(14) . . ?
C70 C67 C85 113.6(11) . . ?
C94 C68 C63 123(2) . . ?
C94 C68 C42 113(2) . . ?
C63 C68 C42 114.2(12) . . ?
C78 C69 C42 116.5(11) . . ?
C78 C69 C85 107.7(13) . . ?
C42 C69 C85 123.4(12) . . ?
C67 C70 C44 107.9(12) . . ?
C67 C70 C90 150.8(9) . . ?
C44 C70 C90 58.3(9) . . ?
C67 C70 C78 100.1(10) . . ?
C44 C70 C78 138.1(9) . . ?
C90 C70 C78 82.1(10) . . ?
C77 C71 C97 160.1(11) . . ?
C77 C71 C76 64.3(13) . . ?
C97 C71 C76 115.8(14) . . ?
C89 C72 C57 95.2(12) . . ?
C89 C72 C73 132.3(14) . . ?
C57 C72 C73 123.8(11) . . ?
C89 C72 C88 30.4(9) . . ?
C57 C72 C88 121.9(8) . . ?
C73 C72 C88 102.0(8) . . ?
C75 C73 C72 121.7(9) . . ?
C75 C73 C79 105.8(9) . . ?
C72 C73 C79 118.8(9) . . ?
C52 C74 C76 124.4(11) . . ?
C52 C74 C65 114.8(11) . . ?
C76 C74 C65 108.2(13) . . ?
C90 C75 C73 142.9(13) . . ?
C90 C75 C82 90.1(12) . . ?
C73 C75 C82 113.4(10) . . ?
C90 C75 C62 41.4(9) . . ?
C73 C75 C62 103.7(9) . . ?
C82 C75 C62 127.5(7) . . ?
C47 C76 C74 111.2(12) . . ?
C47 C76 C77 142.1(17) . . ?
C74 C76 C77 92.5(14) . . ?
C47 C76 C71 106.8(18) . . ?
C74 C76 C71 127.4(12) . . ?
C77 C76 C71 38.1(6) . . ?
C71 C77 C86 128.8(18) . . ?
C71 C77 C76 77.6(14) . . ?
C86 C77 C76 138.0(14) . . ?
C82 C78 C69 124.0(17) . . ?
C82 C78 C70 110.8(14) . . ?
C69 C78 C70 114.4(10) . . ?
C40 C79 C73 122.0(10) . . ?
C40 C79 C92 117.3(11) . . ?
C73 C79 C92 108.6(9) . . ?
C99 C80 C81 99(2) . . ?
C99 C80 C53 117.9(19) . . ?
C81 C80 C53 128.6(17) . . ?
C80 C81 C95 124(2) . . ?
C80 C81 C51 110(2) . . ?
C95 C81 C51 116.3(15) . . ?
C80 C81 C99 38.6(10) . . ?
C95 C81 C99 85.9(17) . . ?
C51 C81 C99 140.6(14) . . ?
C78 C82 C92 126.1(16) . . ?
C78 C82 C75 118.0(14) . . ?
C92 C82 C75 104.2(9) . . ?
C78 C82 C90 80.8(12) . . ?
C92 C82 C90 135.6(10) . . ?
C75 C82 C90 37.4(7) . . ?
C94 C83 C43 146(2) . . ?
C94 C83 C60 92(2) . . ?
C43 C83 C60 105.1(11) . . ?
C87 C84 C52 122.9(17) . . ?
C87 C84 C41 111.2(18) . . ?
C52 C84 C41 108.8(11) . . ?
C98 C85 C69 110.6(15) . . ?
C98 C85 C67 133.2(14) . . ?
C69 C85 C67 104.1(11) . . ?
C98 C85 C86 94.1(13) . . ?
C69 C85 C86 139.0(10) . . ?
C67 C85 C86 40.4(7) . . ?
C67 C86 C77 162.3(13) . . ?
C67 C86 C65 88.5(14) . . ?
C77 C86 C65 85.4(15) . . ?
C67 C86 C85 64.1(13) . . ?
C77 C86 C85 112.8(15) . . ?
C65 C86 C85 142.7(11) . . ?
C84 C87 C66 139(2) . . ?
C84 C87 C88 108(2) . . ?
C66 C87 C88 109.8(18) . . ?
C84 C87 C89 143(2) . . ?
C66 C87 C89 73.4(15) . . ?
C88 C87 C89 36.5(7) . . ?
C89 C88 C62 140.3(15) . . ?
C89 C88 C87 82.5(14) . . ?
C62 C88 C87 121.8(13) . . ?
C89 C88 C72 35.5(11) . . ?
C62 C88 C72 105.2(9) . . ?
C87 C88 C72 111.4(10) . . ?
C88 C89 C72 114.1(18) . . ?
C88 C89 C87 61.0(12) . . ?
C72 C89 C87 148.1(11) . . ?
C88 C89 C66 99.1(13) . . ?
C72 C89 C66 130.8(13) . . ?
C87 C89 C66 38.1(8) . . ?
C88 C89 C59 140.0(14) . . ?
C72 C89 C59 89.5(11) . . ?
C87 C89 C59 81.8(10) . . ?
C66 C89 C59 44.7(6) . . ?
C88 C89 C57 148.9(13) . . ?
C72 C89 C57 43.5(8) . . ?
C87 C89 C57 123.5(11) . . ?
C66 C89 C57 90.2(9) . . ?
C59 C89 C57 46.4(6) . . ?
C75 C90 C62 102.7(17) . . ?
C75 C90 C44 156.8(16) . . ?
C62 C90 C44 56.2(10) . . ?
C75 C90 C70 138.2(16) . . ?
C62 C90 C70 112.3(15) . . ?
C44 C90 C70 57.3(10) . . ?
C75 C90 C82 52.5(10) . . ?
C62 C90 C82 147.6(13) . . ?
C44 C90 C82 140.8(14) . . ?
C70 C90 C82 86.2(10) . . ?
C93 C91 C45 115.7(14) . . ?
C93 C91 C94 113.8(12) . . ?
C45 C91 C94 115.2(12) . . ?
C46 C92 C82 114.9(11) . . ?
C46 C92 C79 124.2(11) . . ?
C82 C92 C79 108.0(11) . . ?
C97 C93 C91 161.2(13) . . ?
C97 C93 C55 66.9(14) . . ?
C91 C93 C55 111.4(12) . . ?
C97 C93 C63 73.9(14) . . ?
C91 C93 C63 97.6(13) . . ?
C55 C93 C63 133.3(10) . . ?
C83 C94 C68 157(2) . . ?
C83 C94 C91 88(2) . . ?
C68 C94 C91 100.8(18) . . ?
C81 C95 C96 104.1(17) . . ?
C81 C95 C43 134.8(15) . . ?
C96 C95 C43 107.3(10) . . ?
C60 C96 C40 123.5(11) . . ?
C60 C96 C95 116.0(11) . . ?
C40 C96 C95 105.7(12) . . ?
C93 C97 C71 161.0(12) . . ?
C93 C97 C55 77.7(15) . . ?
C71 C97 C55 100.9(12) . . ?
C93 C97 C63 73.8(13) . . ?
C71 C97 C63 98.0(13) . . ?
C55 C97 C63 141.6(8) . . ?
C85 C98 C63 138.9(16) . . ?
C100 C99 C80 156(2) . . ?
C100 C99 C81 143.7(15) . . ?
C80 C99 C81 42.8(14) . . ?
C100 C99 C54 53.8(13) . . ?
C80 C99 C54 104.9(16) . . ?
C81 C99 C54 136.4(12) . . ?
C99 C100 C64 136.4(17) . . ?
C99 C100 C54 93.7(15) . . ?
C64 C100 C54 119.2(11) . . ?
C4 O1 C1 107.2(4) . . ?
C6 O2 C9 105.4(4) . . ?
C11 O3 C14 106.6(3) . . ?
C19 O4 C16 106.4(4) . . ?

_refine_diff_density_max         1.315
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.148





