# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_ku81
_database_code_depnum_ccdc_archive 'CCDC 1050284'
_audit_update_record             
;
2015-02-18 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 F6 S2'
_chemical_formula_weight         536.58

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'
S S 0.1246 0.1234 '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                   10.1677(5)
_cell_length_b                   14.6615(8)
_cell_length_c                   17.0409(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.0690(10)
_cell_angle_gamma                90.00
_cell_volume                     2441.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    6609
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.42

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8962
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_process_details   
; 
 SADABS; Sheldrick 1997 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23575
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4313
_reflns_number_gt                3952
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0402P)²+2.0183P] 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         4313
_refine_ls_number_parameters     329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_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
C1 C 0.3847(2) 0.87752(15) 1.09208(13) 0.0277(5) Uani 1 1 d . . .
H1A H 0.3021 0.8696 1.1104 0.042 Uiso 1 1 calc R . .
H1B H 0.4141 0.9414 1.0991 0.042 Uiso 1 1 calc R . .
H1C H 0.4578 0.8383 1.1245 0.042 Uiso 1 1 calc R . .
C2 C 0.4784(2) 0.86372(15) 0.96941(14) 0.0265(5) Uani 1 1 d . . .
H2A H 0.5535 0.8253 1.0007 0.040 Uiso 1 1 calc R . .
H2B H 0.5070 0.9278 0.9749 0.040 Uiso 1 1 calc R . .
H2C H 0.4545 0.8461 0.9117 0.040 Uiso 1 1 calc R . .
C3 C 0.3536(2) 0.85136(13) 1.00205(12) 0.0178(4) Uani 1 1 d . . .
H3 H 0.2803 0.8933 0.9705 0.021 Uiso 1 1 calc R . .
C4 C 0.29988(19) 0.75567(13) 0.98730(11) 0.0158(4) Uani 1 1 d . . .
C5 C 0.17161(19) 0.72613(13) 0.94662(11) 0.0159(4) Uani 1 1 d . . .
C6 C 0.1596(2) 0.62723(14) 0.94538(11) 0.0169(4) Uani 1 1 d . . .
C7 C 0.0501(2) 0.57055(14) 0.90618(12) 0.0218(5) Uani 1 1 d . . .
H7 H -0.0347 0.5965 0.8766 0.026 Uiso 1 1 calc R . .
C8 C 0.0654(2) 0.47717(15) 0.91048(13) 0.0246(5) Uani 1 1 d . . .
H8 H -0.0087 0.4391 0.8832 0.029 Uiso 1 1 calc R . .
C9 C 0.1893(2) 0.43787(14) 0.95472(13) 0.0239(5) Uani 1 1 d . . .
H9 H 0.1979 0.3733 0.9575 0.029 Uiso 1 1 calc R . .
C10 C 0.2985(2) 0.49130(14) 0.99422(12) 0.0215(4) Uani 1 1 d . . .
H10 H 0.3822 0.4646 1.0248 0.026 Uiso 1 1 calc R . .
C11 C 0.2836(2) 0.58575(14) 0.98829(12) 0.0174(4) Uani 1 1 d . . .
C12 C 0.05719(19) 0.78923(13) 0.91075(11) 0.0152(4) Uani 1 1 d . . .
C13 C -0.0653(2) 0.79442(15) 0.94397(12) 0.0212(5) Uani 1 1 d . . .
C14 C -0.1430(2) 0.88050(14) 0.90541(13) 0.0208(5) Uani 1 1 d . . .
C15 C -0.0919(2) 0.89621(14) 0.83001(12) 0.0197(4) Uani 1 1 d . . .
C16 C 0.0442(2) 0.84855(13) 0.84888(12) 0.0158(4) Uani 1 1 d . . .
C17 C 0.0887(2) 0.70412(14) 0.72827(13) 0.0206(4) Uani 1 1 d . . .
H17A H 0.1217 0.6646 0.7761 0.031 Uiso 1 1 calc R . .
H17B H 0.1108 0.6765 0.6811 0.031 Uiso 1 1 calc R . .
H17C H -0.0107 0.7115 0.7164 0.031 Uiso 1 1 calc R . .
C18 C 0.1563(2) 0.79523(13) 0.74546(12) 0.0174(4) Uani 1 1 d . . .
C19 C 0.13727(19) 0.86241(13) 0.79707(12) 0.0156(4) Uani 1 1 d . . .
C20 C 0.21262(19) 0.94455(13) 0.79393(12) 0.0157(4) Uani 1 1 d . . .
C21 C 0.2907(2) 0.93668(13) 0.74035(12) 0.0160(4) Uani 1 1 d . . .
C22 C 0.3863(2) 1.00245(14) 0.71985(11) 0.0164(4) Uani 1 1 d . . .
C23 C 0.3533(2) 1.09495(14) 0.70901(12) 0.0183(4) Uani 1 1 d . . .
H23 H 0.2690 1.1162 0.7159 0.022 Uiso 1 1 calc R . .
C24 C 0.4422(2) 1.15598(14) 0.68830(12) 0.0205(4) Uani 1 1 d . . .
H24 H 0.4188 1.2188 0.6816 0.025 Uiso 1 1 calc R . .
C25 C 0.5650(2) 1.12585(14) 0.67733(12) 0.0200(4) Uani 1 1 d . . .
H25 H 0.6254 1.1677 0.6626 0.024 Uiso 1 1 calc R . .
C26 C 0.5993(2) 1.03461(15) 0.68793(12) 0.0205(4) Uani 1 1 d . . .
H26 H 0.6836 1.0138 0.6806 0.025 Uiso 1 1 calc R . .
C27 C 0.5110(2) 0.97312(14) 0.70924(11) 0.0180(4) Uani 1 1 d . . .
H27 H 0.5357 0.9106 0.7167 0.022 Uiso 1 1 calc R . .
C28 C 0.2105(2) 1.02757(13) 0.84579(12) 0.0197(4) Uani 1 1 d . . .
H28A H 0.3013 1.0560 0.8610 0.030 Uiso 1 1 calc R . .
H28B H 0.1861 1.0094 0.8953 0.030 Uiso 1 1 calc R . .
H28C H 0.1429 1.0712 0.8148 0.030 Uiso 1 1 calc R . .
F1 F -0.03058(13) 0.79776(11) 1.02619(7) 0.0357(3) Uani 1 1 d . . .
F2 F -0.15033(12) 0.72147(8) 0.92213(8) 0.0287(3) Uani 1 1 d . . .
F3 F -0.10592(14) 0.95148(9) 0.95693(8) 0.0334(3) Uani 1 1 d . . .
F4 F -0.27950(12) 0.87184(9) 0.88795(8) 0.0285(3) Uani 1 1 d . . .
F5 F -0.08756(12) 0.98577(8) 0.81237(8) 0.0287(3) Uani 1 1 d . . .
F6 F -0.18103(12) 0.85726(9) 0.76345(7) 0.0261(3) Uani 1 1 d . . .
S1 S 0.41005(5) 0.66601(3) 1.02717(3) 0.01747(13) Uani 1 1 d . . .
S2 S 0.26869(5) 0.83106(3) 0.69305(3) 0.01780(13) 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 C3 1.527(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.530(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.501(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.367(3) . ?
C4 S1 1.7386(19) . ?
C5 C6 1.455(3) . ?
C5 C12 1.480(3) . ?
C6 C7 1.401(3) . ?
C6 C11 1.409(3) . ?
C7 C8 1.378(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.400(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.374(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(3) . ?
C10 H10 0.9500 . ?
C11 S1 1.734(2) . ?
C12 C16 1.345(3) . ?
C12 C13 1.506(3) . ?
C13 F1 1.348(2) . ?
C13 F2 1.361(2) . ?
C13 C14 1.537(3) . ?
C14 F4 1.342(2) . ?
C14 F3 1.346(2) . ?
C14 C15 1.531(3) . ?
C15 F5 1.350(2) . ?
C15 F6 1.366(2) . ?
C15 C16 1.503(3) . ?
C16 C19 1.476(3) . ?
C17 C18 1.493(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.369(3) . ?
C18 S2 1.716(2) . ?
C19 C20 1.436(3) . ?
C20 C21 1.371(3) . ?
C20 C28 1.508(3) . ?
C21 C22 1.478(3) . ?
C21 S2 1.732(2) . ?
C22 C23 1.397(3) . ?
C22 C27 1.397(3) . ?
C23 C24 1.385(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.389(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

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 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C1 111.55(16) . . ?
C4 C3 C2 110.46(17) . . ?
C1 C3 C2 111.94(18) . . ?
C4 C3 H3 107.6 . . ?
C1 C3 H3 107.6 . . ?
C2 C3 H3 107.6 . . ?
C5 C4 C3 129.26(18) . . ?
C5 C4 S1 112.32(15) . . ?
C3 C4 S1 118.42(14) . . ?
C4 C5 C6 112.82(17) . . ?
C4 C5 C12 122.83(18) . . ?
C6 C5 C12 124.31(17) . . ?
C7 C6 C11 118.04(19) . . ?
C7 C6 C5 130.59(19) . . ?
C11 C6 C5 111.29(17) . . ?
C8 C7 C6 120.1(2) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.6(2) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 120.9(2) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 118.3(2) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C10 C11 C6 122.05(19) . . ?
C10 C11 S1 126.32(16) . . ?
C6 C11 S1 111.60(15) . . ?
C16 C12 C5 128.59(18) . . ?
C16 C12 C13 110.49(17) . . ?
C5 C12 C13 120.92(17) . . ?
F1 C13 F2 106.06(16) . . ?
F1 C13 C12 112.75(16) . . ?
F2 C13 C12 112.74(17) . . ?
F1 C13 C14 111.74(17) . . ?
F2 C13 C14 108.43(16) . . ?
C12 C13 C14 105.16(16) . . ?
F4 C14 F3 107.66(16) . . ?
F4 C14 C15 113.49(17) . . ?
F3 C14 C15 109.39(17) . . ?
F4 C14 C13 113.25(17) . . ?
F3 C14 C13 109.76(17) . . ?
C15 C14 C13 103.22(16) . . ?
F5 C15 F6 106.07(16) . . ?
F5 C15 C16 114.52(17) . . ?
F6 C15 C16 110.07(16) . . ?
F5 C15 C14 111.88(17) . . ?
F6 C15 C14 109.43(16) . . ?
C16 C15 C14 104.87(16) . . ?
C12 C16 C19 128.16(18) . . ?
C12 C16 C15 110.69(18) . . ?
C19 C16 C15 120.83(17) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C17 129.08(18) . . ?
C19 C18 S2 110.29(15) . . ?
C17 C18 S2 120.53(15) . . ?
C18 C19 C20 114.07(18) . . ?
C18 C19 C16 120.85(18) . . ?
C20 C19 C16 125.07(17) . . ?
C21 C20 C19 111.56(18) . . ?
C21 C20 C28 124.27(18) . . ?
C19 C20 C28 124.12(17) . . ?
C20 C21 C22 129.99(18) . . ?
C20 C21 S2 111.18(15) . . ?
C22 C21 S2 118.83(15) . . ?
C23 C22 C27 118.34(18) . . ?
C23 C22 C21 121.01(18) . . ?
C27 C22 C21 120.63(18) . . ?
C24 C23 C22 120.75(19) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 120.30(19) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C26 C25 C24 119.68(19) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 120.32(19) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C22 120.61(19) . . ?
C26 C27 H27 119.7 . . ?
C22 C27 H27 119.7 . . ?
C20 C28 H28A 109.5 . . ?
C20 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C20 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C11 S1 C4 91.97(10) . . ?
C18 S2 C21 92.89(10) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.056

####################################################################### 
# 
# 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_ku82
_database_code_depnum_ccdc_archive 'CCDC 1050285'
_audit_update_record             
;
2015-02-18 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H22 F6 S2'
_chemical_formula_weight         536.58

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'
S S 0.1246 0.1234 '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                   21.9703(11)
_cell_length_b                   10.0662(5)
_cell_length_c                   21.3000(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0920(10)
_cell_angle_gamma                90.00
_cell_volume                     4703.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    7016
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.79

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8926
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_process_details   
; 
 SADABS; Sheldrick 1997 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33939
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         0.93
_diffrn_reflns_theta_max         25.03
_reflns_number_total             8281
_reflns_number_gt                7263
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0400P)²+4.3369P] 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         8281
_refine_ls_number_parameters     657
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.1006
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_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
C51 C 0.22966(10) 0.2312(2) 0.64180(10) 0.0146(5) Uani 1 1 d . . .
C1 C 0.15159(11) -0.1392(3) 0.80215(12) 0.0202(6) Uani 1 1 d . . .
H1A H 0.1614 -0.1456 0.7579 0.030 Uiso 1 1 calc R . .
H1B H 0.1079 -0.1546 0.8058 0.030 Uiso 1 1 calc R . .
H1C H 0.1748 -0.2062 0.8267 0.030 Uiso 1 1 calc R . .
C2 C 0.16820(11) -0.0012(2) 0.82706(11) 0.0151(5) Uani 1 1 d . . .
H2 H 0.1427 0.0633 0.8014 0.018 Uiso 1 1 calc R . .
C3 C 0.23447(11) 0.0272(3) 0.81321(12) 0.0223(6) Uani 1 1 d . . .
H3A H 0.2616 -0.0213 0.8432 0.033 Uiso 1 1 calc R . .
H3B H 0.2424 0.1227 0.8172 0.033 Uiso 1 1 calc R . .
H3C H 0.2419 -0.0016 0.7703 0.033 Uiso 1 1 calc R . .
C4 C 0.15071(10) 0.0178(2) 0.89769(11) 0.0136(5) Uani 1 1 d . . .
C5 C 0.08318(10) -0.0190(2) 0.90023(10) 0.0130(5) Uani 1 1 d . . .
C6 C 0.07456(11) -0.1542(2) 0.92283(11) 0.0148(5) Uani 1 1 d . . .
C7 C 0.02193(11) -0.2331(2) 0.91876(11) 0.0187(5) Uani 1 1 d . . .
H7 H -0.0152 -0.1981 0.9009 0.022 Uiso 1 1 calc R . .
C8 C 0.02448(12) -0.3623(3) 0.94100(12) 0.0210(6) Uani 1 1 d . . .
H8 H -0.0111 -0.4161 0.9379 0.025 Uiso 1 1 calc R . .
C9 C 0.07839(11) -0.4141(2) 0.96770(11) 0.0203(6) Uani 1 1 d . . .
H9 H 0.0792 -0.5029 0.9829 0.024 Uiso 1 1 calc R . .
C10 C 0.13092(11) -0.3385(2) 0.97259(11) 0.0179(5) Uani 1 1 d . . .
H10 H 0.1677 -0.3740 0.9912 0.021 Uiso 1 1 calc R . .
C11 C 0.12870(11) -0.2090(2) 0.94949(11) 0.0148(5) Uani 1 1 d . . .
C12 C 0.13114(11) 0.1775(2) 0.98971(11) 0.0159(5) Uani 1 1 d . . .
H12A H 0.1403 0.2672 1.0055 0.024 Uiso 1 1 calc R . .
H12B H 0.1500 0.1119 1.0187 0.024 Uiso 1 1 calc R . .
H12C H 0.0869 0.1643 0.9867 0.024 Uiso 1 1 calc R . .
C13 C 0.13406(11) 0.4705(2) 0.81360(11) 0.0176(5) Uani 1 1 d . . .
H13A H 0.1084 0.5333 0.8354 0.026 Uiso 1 1 calc R . .
H13B H 0.1101 0.4291 0.7788 0.026 Uiso 1 1 calc R . .
H13C H 0.1688 0.5179 0.7971 0.026 Uiso 1 1 calc R . .
C14 C 0.15676(10) 0.1606(2) 0.92400(11) 0.0130(5) Uani 1 1 d . . .
C15 C 0.12142(10) 0.2528(2) 0.87804(10) 0.0128(5) Uani 1 1 d . . .
C16 C 0.15696(11) 0.3651(2) 0.85882(11) 0.0150(5) Uani 1 1 d . . .
C17 C 0.21606(10) 0.3589(2) 0.88208(11) 0.0141(5) Uani 1 1 d . . .
C18 C 0.26726(10) 0.4499(2) 0.86989(11) 0.0148(5) Uani 1 1 d . . .
C19 C 0.26422(11) 0.5847(2) 0.88276(11) 0.0175(5) Uani 1 1 d . . .
H19 H 0.2279 0.6214 0.8978 0.021 Uiso 1 1 calc R . .
C20 C 0.31388(12) 0.6662(3) 0.87371(12) 0.0217(6) Uani 1 1 d . . .
H20 H 0.3117 0.7580 0.8836 0.026 Uiso 1 1 calc R . .
C21 C 0.36646(11) 0.6148(3) 0.85044(12) 0.0212(6) Uani 1 1 d . . .
H21 H 0.4002 0.6711 0.8439 0.025 Uiso 1 1 calc R . .
C22 C 0.36946(11) 0.4810(3) 0.83681(12) 0.0217(6) Uani 1 1 d . . .
H22 H 0.4053 0.4456 0.8201 0.026 Uiso 1 1 calc R . .
C23 C 0.32089(11) 0.3982(2) 0.84724(12) 0.0190(5) Uani 1 1 d . . .
H23 H 0.3240 0.3057 0.8390 0.023 Uiso 1 1 calc R . .
C24 C 0.04352(10) 0.0770(2) 0.88044(10) 0.0137(5) Uani 1 1 d . . .
C25 C -0.02422(11) 0.0685(2) 0.87206(11) 0.0164(5) Uani 1 1 d . . .
C26 C -0.04512(11) 0.2101(3) 0.85504(11) 0.0175(5) Uani 1 1 d . . .
C27 C 0.01118(11) 0.2771(2) 0.82817(11) 0.0158(5) Uani 1 1 d . . .
C28 C 0.06389(10) 0.2101(2) 0.86209(11) 0.0138(5) Uani 1 1 d . . .
C29 C 0.34524(12) 0.8304(3) 0.70493(12) 0.0209(6) Uani 1 1 d . . .
H29A H 0.3377 0.8384 0.7497 0.031 Uiso 1 1 calc R . .
H29B H 0.3208 0.8964 0.6810 0.031 Uiso 1 1 calc R . .
H29C H 0.3886 0.8458 0.6988 0.031 Uiso 1 1 calc R . .
C30 C 0.32767(11) 0.6912(2) 0.68202(11) 0.0162(5) Uani 1 1 d . . .
H30 H 0.3538 0.6277 0.7075 0.019 Uiso 1 1 calc R . .
C31 C 0.26189(11) 0.6645(3) 0.69852(12) 0.0238(6) Uani 1 1 d . . .
H31A H 0.2339 0.7086 0.6678 0.036 Uiso 1 1 calc R . .
H31B H 0.2554 0.6993 0.7406 0.036 Uiso 1 1 calc R . .
H31C H 0.2542 0.5686 0.6978 0.036 Uiso 1 1 calc R . .
C32 C 0.34273(11) 0.6690(2) 0.61116(11) 0.0147(5) Uani 1 1 d . . .
C33 C 0.40997(10) 0.7056(2) 0.60574(10) 0.0140(5) Uani 1 1 d . . .
C34 C 0.41755(11) 0.8402(2) 0.58187(11) 0.0148(5) Uani 1 1 d . . .
C35 C 0.46922(11) 0.9211(2) 0.58510(11) 0.0190(5) Uani 1 1 d . . .
H35 H 0.5064 0.8888 0.6043 0.023 Uiso 1 1 calc R . .
C36 C 0.46641(12) 1.0482(2) 0.56041(12) 0.0213(6) Uani 1 1 d . . .
H36 H 0.5015 1.1036 0.5634 0.026 Uiso 1 1 calc R . .
C37 C 0.41277(12) 1.0951(3) 0.53129(12) 0.0220(6) Uani 1 1 d . . .
H37 H 0.4117 1.1816 0.5134 0.026 Uiso 1 1 calc R . .
C38 C 0.36072(12) 1.0176(2) 0.52786(11) 0.0195(5) Uani 1 1 d . . .
H38 H 0.3240 1.0501 0.5079 0.023 Uiso 1 1 calc R . .
C39 C 0.36329(11) 0.8915(2) 0.55411(11) 0.0164(5) Uani 1 1 d . . .
C40 C 0.45042(10) 0.6098(2) 0.62365(11) 0.0140(5) Uani 1 1 d . . .
C41 C 0.51850(11) 0.6174(3) 0.62669(11) 0.0188(5) Uani 1 1 d . . .
C42 C 0.53957(11) 0.4746(3) 0.64066(12) 0.0215(6) Uani 1 1 d . . .
C43 C 0.48643(11) 0.4099(2) 0.67319(11) 0.0164(5) Uani 1 1 d . . .
C44 C 0.43167(10) 0.4772(2) 0.64347(11) 0.0144(5) Uani 1 1 d . . .
C45 C 0.35692(11) 0.5045(2) 0.51948(11) 0.0176(5) Uani 1 1 d . . .
H45A H 0.3508 0.4115 0.5071 0.026 Uiso 1 1 calc R . .
H45B H 0.4003 0.5269 0.5184 0.026 Uiso 1 1 calc R . .
H45C H 0.3332 0.5621 0.4903 0.026 Uiso 1 1 calc R . .
C46 C 0.36507(11) 0.2115(2) 0.69316(11) 0.0170(5) Uani 1 1 d . . .
H46A H 0.3888 0.1489 0.6690 0.025 Uiso 1 1 calc R . .
H46B H 0.3315 0.1642 0.7118 0.025 Uiso 1 1 calc R . .
H46C H 0.3915 0.2512 0.7266 0.025 Uiso 1 1 calc R . .
C47 C 0.33564(10) 0.5250(2) 0.58684(11) 0.0147(5) Uani 1 1 d . . .
C48 C 0.37362(11) 0.4338(2) 0.63089(11) 0.0139(5) Uani 1 1 d . . .
C49 C 0.33977(11) 0.3189(2) 0.65033(11) 0.0149(5) Uani 1 1 d . . .
C50 C 0.27994(11) 0.3246(2) 0.63037(11) 0.0149(5) Uani 1 1 d . . .
C52 C 0.23329(11) 0.0974(2) 0.62609(11) 0.0178(5) Uani 1 1 d . . .
H52 H 0.2697 0.0630 0.6102 0.021 Uiso 1 1 calc R . .
C53 C 0.18393(11) 0.0142(3) 0.63356(12) 0.0211(6) Uani 1 1 d . . .
H53 H 0.1865 -0.0770 0.6224 0.025 Uiso 1 1 calc R . .
C54 C 0.13093(11) 0.0632(3) 0.65721(12) 0.0208(6) Uani 1 1 d . . .
H54 H 0.0972 0.0059 0.6621 0.025 Uiso 1 1 calc R . .
C55 C 0.12720(11) 0.1957(3) 0.67363(12) 0.0202(6) Uani 1 1 d . . .
H55 H 0.0911 0.2292 0.6906 0.024 Uiso 1 1 calc R . .
C56 C 0.17600(11) 0.2794(3) 0.66536(11) 0.0186(5) Uani 1 1 d . . .
H56 H 0.1729 0.3708 0.6759 0.022 Uiso 1 1 calc R . .
F1 F -0.05246(6) 0.02511(14) 0.92323(7) 0.0230(3) Uani 1 1 d . . .
F2 F -0.04291(6) -0.01549(14) 0.82418(7) 0.0230(3) Uani 1 1 d . . .
F3 F -0.05825(7) 0.27509(15) 0.90779(7) 0.0276(4) Uani 1 1 d . . .
F4 F -0.09492(6) 0.21336(15) 0.81574(7) 0.0275(4) Uani 1 1 d . . .
F5 F 0.00809(6) 0.41005(13) 0.83528(7) 0.0230(3) Uani 1 1 d . . .
F6 F 0.00891(6) 0.25431(15) 0.76473(6) 0.0226(3) Uani 1 1 d . . .
F7 F 0.54254(6) 0.66250(14) 0.57319(7) 0.0246(3) Uani 1 1 d . . .
F8 F 0.54127(7) 0.69880(15) 0.67356(7) 0.0278(4) Uani 1 1 d . . .
F9 F 0.54648(7) 0.41014(15) 0.58577(7) 0.0322(4) Uani 1 1 d . . .
F10 F 0.59308(6) 0.46851(16) 0.67401(8) 0.0353(4) Uani 1 1 d . . .
F11 F 0.48887(6) 0.27590(14) 0.66648(7) 0.0240(3) Uani 1 1 d . . .
F12 F 0.49390(6) 0.43378(15) 0.73644(6) 0.0247(3) Uani 1 1 d . . .
S1 S 0.19233(3) -0.10300(6) 0.94859(3) 0.01498(14) Uani 1 1 d . . .
S2 S 0.23526(3) 0.22421(6) 0.93093(3) 0.01483(14) Uani 1 1 d . . .
S3 S 0.29988(3) 0.78531(6) 0.55860(3) 0.01611(14) Uani 1 1 d . . .
S4 S 0.25749(3) 0.46167(6) 0.58497(3) 0.01517(14) 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
C51 C52 1.391(3) . ?
C51 C56 1.393(3) . ?
C51 C50 1.481(3) . ?
C1 C2 1.525(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.528(3) . ?
C2 C4 1.584(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.533(3) . ?
C4 C14 1.546(3) . ?
C4 S1 1.839(2) . ?
C5 C24 1.353(3) . ?
C5 C6 1.459(3) . ?
C6 C7 1.402(3) . ?
C6 C11 1.403(3) . ?
C7 C8 1.385(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.381(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.394(3) . ?
C10 H10 0.9500 . ?
C11 S1 1.759(2) . ?
C12 C14 1.546(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C16 1.501(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.530(3) . ?
C14 S2 1.838(2) . ?
C15 C28 1.361(3) . ?
C15 C16 1.446(3) . ?
C16 C17 1.366(3) . ?
C17 C18 1.484(3) . ?
C17 S2 1.747(2) . ?
C18 C19 1.387(3) . ?
C18 C23 1.398(3) . ?
C19 C20 1.387(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(3) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C28 1.472(3) . ?
C24 C25 1.492(3) . ?
C25 F1 1.355(3) . ?
C25 F2 1.371(3) . ?
C25 C26 1.535(3) . ?
C26 F4 1.342(3) . ?
C26 F3 1.345(3) . ?
C26 C27 1.545(3) . ?
C27 F5 1.349(3) . ?
C27 F6 1.369(3) . ?
C27 C28 1.492(3) . ?
C29 C30 1.527(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.529(3) . ?
C30 C32 1.578(3) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.533(3) . ?
C32 C47 1.545(3) . ?
C32 S3 1.843(2) . ?
C33 C40 1.353(3) . ?
C33 C34 1.460(3) . ?
C34 C35 1.396(3) . ?
C34 C39 1.400(3) . ?
C35 C36 1.384(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.383(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.387(3) . ?
C38 H38 0.9500 . ?
C39 S3 1.762(2) . ?
C40 C44 1.466(3) . ?
C40 C41 1.495(3) . ?
C41 F7 1.360(3) . ?
C41 F8 1.366(3) . ?
C41 C42 1.534(4) . ?
C42 F10 1.342(3) . ?
C42 F9 1.353(3) . ?
C42 C43 1.535(3) . ?
C43 F11 1.358(3) . ?
C43 F12 1.370(3) . ?
C43 C44 1.492(3) . ?
C44 C48 1.361(3) . ?
C45 C47 1.547(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C49 1.502(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.528(3) . ?
C47 S4 1.830(2) . ?
C48 C49 1.448(3) . ?
C49 C50 1.361(3) . ?
C50 S4 1.741(2) . ?
C52 C53 1.387(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.384(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.382(3) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?

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
C52 C51 C56 119.0(2) . . ?
C52 C51 C50 121.5(2) . . ?
C56 C51 C50 119.4(2) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 C3 108.4(2) . . ?
C1 C2 C4 111.99(19) . . ?
C3 C2 C4 116.3(2) . . ?
C1 C2 H2 106.5 . . ?
C3 C2 H2 106.5 . . ?
C4 C2 H2 106.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C14 106.05(18) . . ?
C5 C4 C2 106.81(18) . . ?
C14 C4 C2 115.83(19) . . ?
C5 C4 S1 105.70(15) . . ?
C14 C4 S1 111.76(16) . . ?
C2 C4 S1 109.99(15) . . ?
C24 C5 C6 132.5(2) . . ?
C24 C5 C4 115.1(2) . . ?
C6 C5 C4 112.3(2) . . ?
C7 C6 C11 118.7(2) . . ?
C7 C6 C5 129.0(2) . . ?
C11 C6 C5 112.2(2) . . ?
C8 C7 C6 119.6(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 120.7(2) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 121.0(2) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 118.4(2) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C10 C11 C6 121.6(2) . . ?
C10 C11 S1 123.94(19) . . ?
C6 C11 S1 114.46(18) . . ?
C14 C12 H12A 109.5 . . ?
C14 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C14 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C16 C13 H13A 109.5 . . ?
C16 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C16 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C4 107.55(18) . . ?
C15 C14 C12 108.37(18) . . ?
C4 C14 C12 113.74(19) . . ?
C15 C14 S2 106.35(15) . . ?
C4 C14 S2 114.53(16) . . ?
C12 C14 S2 105.94(15) . . ?
C28 C15 C16 133.2(2) . . ?
C28 C15 C14 113.6(2) . . ?
C16 C15 C14 113.11(19) . . ?
C17 C16 C15 112.2(2) . . ?
C17 C16 C13 123.0(2) . . ?
C15 C16 C13 124.5(2) . . ?
C16 C17 C18 128.5(2) . . ?
C16 C17 S2 116.50(18) . . ?
C18 C17 S2 114.97(17) . . ?
C19 C18 C23 118.9(2) . . ?
C19 C18 C17 121.6(2) . . ?
C23 C18 C17 119.5(2) . . ?
C20 C19 C18 120.3(2) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 120.5(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 119.4(2) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 120.6(2) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C18 120.2(2) . . ?
C22 C23 H23 119.9 . . ?
C18 C23 H23 119.9 . . ?
C5 C24 C28 122.2(2) . . ?
C5 C24 C25 128.2(2) . . ?
C28 C24 C25 109.6(2) . . ?
F1 C25 F2 105.53(18) . . ?
F1 C25 C24 114.79(19) . . ?
F2 C25 C24 112.42(19) . . ?
F1 C25 C26 110.19(19) . . ?
F2 C25 C26 108.87(19) . . ?
C24 C25 C26 105.00(19) . . ?
F4 C26 F3 107.75(19) . . ?
F4 C26 C25 113.2(2) . . ?
F3 C26 C25 109.22(19) . . ?
F4 C26 C27 113.60(19) . . ?
F3 C26 C27 108.0(2) . . ?
C25 C26 C27 104.91(19) . . ?
F5 C27 F6 106.11(18) . . ?
F5 C27 C28 115.9(2) . . ?
F6 C27 C28 112.86(19) . . ?
F5 C27 C26 110.18(19) . . ?
F6 C27 C26 107.77(19) . . ?
C28 C27 C26 103.85(19) . . ?
C15 C28 C24 120.9(2) . . ?
C15 C28 C27 131.6(2) . . ?
C24 C28 C27 107.5(2) . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C29 C30 C31 108.3(2) . . ?
C29 C30 C32 111.89(19) . . ?
C31 C30 C32 116.4(2) . . ?
C29 C30 H30 106.6 . . ?
C31 C30 H30 106.6 . . ?
C32 C30 H30 106.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 C32 C47 106.30(18) . . ?
C33 C32 C30 106.90(18) . . ?
C47 C32 C30 115.51(19) . . ?
C33 C32 S3 105.32(15) . . ?
C47 C32 S3 110.70(16) . . ?
C30 C32 S3 111.38(16) . . ?
C40 C33 C34 132.4(2) . . ?
C40 C33 C32 115.4(2) . . ?
C34 C33 C32 112.2(2) . . ?
C35 C34 C39 118.5(2) . . ?
C35 C34 C33 129.2(2) . . ?
C39 C34 C33 112.2(2) . . ?
C36 C35 C34 120.1(2) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C37 120.3(2) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C38 C37 C36 120.8(2) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 118.7(2) . . ?
C37 C38 H38 120.7 . . ?
C39 C38 H38 120.7 . . ?
C38 C39 C34 121.5(2) . . ?
C38 C39 S3 124.2(2) . . ?
C34 C39 S3 114.28(18) . . ?
C33 C40 C44 122.7(2) . . ?
C33 C40 C41 128.0(2) . . ?
C44 C40 C41 109.3(2) . . ?
F7 C41 F8 105.57(19) . . ?
F7 C41 C40 114.4(2) . . ?
F8 C41 C40 112.86(19) . . ?
F7 C41 C42 110.4(2) . . ?
F8 C41 C42 109.0(2) . . ?
C40 C41 C42 104.6(2) . . ?
F10 C42 F9 107.4(2) . . ?
F10 C42 C41 113.1(2) . . ?
F9 C42 C41 109.2(2) . . ?
F10 C42 C43 114.1(2) . . ?
F9 C42 C43 108.1(2) . . ?
C41 C42 C43 104.86(19) . . ?
F11 C43 F12 105.94(18) . . ?
F11 C43 C44 116.2(2) . . ?
F12 C43 C44 112.88(19) . . ?
F11 C43 C42 109.82(19) . . ?
F12 C43 C42 108.40(19) . . ?
C44 C43 C42 103.37(19) . . ?
C48 C44 C40 120.7(2) . . ?
C48 C44 C43 131.6(2) . . ?
C40 C44 C43 107.6(2) . . ?
C47 C45 H45A 109.5 . . ?
C47 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C47 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C49 C46 H46A 109.5 . . ?
C49 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C49 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C32 108.42(19) . . ?
C48 C47 C45 107.89(19) . . ?
C32 C47 C45 113.97(19) . . ?
C48 C47 S4 106.56(16) . . ?
C32 C47 S4 114.31(16) . . ?
C45 C47 S4 105.28(16) . . ?
C44 C48 C49 133.7(2) . . ?
C44 C48 C47 113.8(2) . . ?
C49 C48 C47 112.6(2) . . ?
C50 C49 C48 112.3(2) . . ?
C50 C49 C46 122.7(2) . . ?
C48 C49 C46 124.7(2) . . ?
C49 C50 C51 129.7(2) . . ?
C49 C50 S4 116.56(18) . . ?
C51 C50 S4 113.78(17) . . ?
C53 C52 C51 120.2(2) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C54 C53 C52 120.3(2) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C55 C54 C53 119.9(2) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C56 C55 C54 119.9(2) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C55 C56 C51 120.7(2) . . ?
C55 C56 H56 119.7 . . ?
C51 C56 H56 119.7 . . ?
C11 S1 C4 92.13(11) . . ?
C17 S2 C14 91.56(11) . . ?
C39 S3 C32 92.21(11) . . ?
C50 S4 C47 91.52(11) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.059

