# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_eileen64
_database_code_depnum_ccdc_archive 'CCDC 1052442'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H45 F3 N2 O3 S Si'
_chemical_formula_weight         610.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   9.71654(13)
_cell_length_b                   22.4084(2)
_cell_length_c                   15.65661(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0178(12)
_cell_angle_gamma                90.00
_cell_volume                     3321.34(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    37763
_cell_measurement_theta_min      3.9380
_cell_measurement_theta_max      76.5810

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.51691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            67865
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.51
_diffrn_reflns_theta_max         76.98
_reflns_number_total             7001
_reflns_number_gt                6406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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)+(0.0429P)²+1.5267P] 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         7001
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Si Si 0.82826(3) 0.451620(14) 0.73385(2) 0.01804(8) Uani 1 1 d . . .
N1 N 0.58490(10) 0.37164(4) 0.72754(6) 0.0162(2) Uani 1 1 d . . .
N2 N 0.77686(11) 0.33215(4) 0.80193(6) 0.0167(2) Uani 1 1 d . . .
C1 C 0.72438(12) 0.38274(5) 0.75905(7) 0.0157(2) Uani 1 1 d . . .
C2 C 0.55226(13) 0.31440(5) 0.74970(8) 0.0202(2) Uani 1 1 d . . .
H2 H 0.4619 0.2960 0.7349 0.024 Uiso 1 1 calc R . .
C3 C 0.67205(13) 0.28969(5) 0.79604(8) 0.0206(2) Uani 1 1 d . . .
H3 H 0.6826 0.2506 0.8201 0.025 Uiso 1 1 calc R . .
C4 C 0.47689(12) 0.41291(5) 0.68264(8) 0.0166(2) Uani 1 1 d . . .
C5 C 0.42820(12) 0.40732(5) 0.59185(8) 0.0180(2) Uani 1 1 d . . .
C6 C 0.31585(13) 0.44421(6) 0.55220(8) 0.0216(3) Uani 1 1 d . . .
H6 H 0.2791 0.4416 0.4907 0.026 Uiso 1 1 calc R . .
C7 C 0.25733(14) 0.48444(6) 0.60105(9) 0.0235(3) Uani 1 1 d . . .
H7 H 0.1807 0.5089 0.5728 0.028 Uiso 1 1 calc R . .
C8 C 0.30928(14) 0.48938(6) 0.69072(9) 0.0224(3) Uani 1 1 d . . .
H8 H 0.2692 0.5178 0.7230 0.027 Uiso 1 1 calc R . .
C9 C 0.41969(13) 0.45313(5) 0.73414(8) 0.0186(2) Uani 1 1 d . . .
C10 C 0.48538(13) 0.36170(6) 0.53707(8) 0.0217(3) Uani 1 1 d . . .
H10 H 0.5812 0.3490 0.5702 0.026 Uiso 1 1 calc R . .
C11 C 0.49890(15) 0.38660(7) 0.44809(9) 0.0291(3) Uani 1 1 d . . .
H11A H 0.4045 0.3932 0.4110 0.044 Uiso 1 1 calc R . .
H11B H 0.5502 0.3580 0.4195 0.044 Uiso 1 1 calc R . .
H11C H 0.5506 0.4245 0.4569 0.044 Uiso 1 1 calc R . .
C12 C 0.38896(16) 0.30671(6) 0.52228(10) 0.0307(3) Uani 1 1 d . . .
H12A H 0.3856 0.2890 0.5790 0.046 Uiso 1 1 calc R . .
H12B H 0.4261 0.2774 0.4868 0.046 Uiso 1 1 calc R . .
H12C H 0.2936 0.3186 0.4916 0.046 Uiso 1 1 calc R . .
C13 C 0.47226(14) 0.45679(6) 0.83324(8) 0.0226(3) Uani 1 1 d . . .
H13 H 0.5756 0.4476 0.8473 0.027 Uiso 1 1 calc R . .
C14 C 0.45357(18) 0.51911(7) 0.86895(10) 0.0341(3) Uani 1 1 d . . .
H14A H 0.4916 0.5490 0.8348 0.051 Uiso 1 1 calc R . .
H14B H 0.5042 0.5214 0.9305 0.051 Uiso 1 1 calc R . .
H14C H 0.3529 0.5268 0.8645 0.051 Uiso 1 1 calc R . .
C15 C 0.39938(15) 0.41000(7) 0.87965(9) 0.0284(3) Uani 1 1 d . . .
H15A H 0.2985 0.4192 0.8699 0.043 Uiso 1 1 calc R . .
H15B H 0.4417 0.4106 0.9427 0.043 Uiso 1 1 calc R . .
H15C H 0.4115 0.3703 0.8560 0.043 Uiso 1 1 calc R . .
C16 C 0.91891(13) 0.32160(5) 0.85355(8) 0.0183(2) Uani 1 1 d . . .
C17 C 1.01140(14) 0.28834(6) 0.81589(8) 0.0222(3) Uani 1 1 d . . .
C18 C 1.14442(14) 0.27540(7) 0.86883(9) 0.0285(3) Uani 1 1 d . . .
H18 H 1.2103 0.2528 0.8457 0.034 Uiso 1 1 calc R . .
C19 C 1.18057(15) 0.29530(7) 0.95447(10) 0.0323(3) Uani 1 1 d . . .
H19 H 1.2708 0.2858 0.9898 0.039 Uiso 1 1 calc R . .
C20 C 1.08717(16) 0.32888(6) 0.98951(9) 0.0301(3) Uani 1 1 d . . .
H20 H 1.1150 0.3426 1.0483 0.036 Uiso 1 1 calc R . .
C21 C 0.95249(15) 0.34304(5) 0.93997(8) 0.0227(3) Uani 1 1 d . . .
C22 C 0.97334(16) 0.26608(7) 0.72173(9) 0.0293(3) Uani 1 1 d . . .
H22 H 0.8829 0.2857 0.6917 0.035 Uiso 1 1 calc R . .
C23 C 1.0865(2) 0.28292(9) 0.67189(11) 0.0453(4) Uani 1 1 d . . .
H23A H 1.1026 0.3261 0.6759 0.068 Uiso 1 1 calc R . .
H23B H 1.0547 0.2714 0.6102 0.068 Uiso 1 1 calc R . .
H23C H 1.1747 0.2620 0.6977 0.068 Uiso 1 1 calc R . .
C24 C 0.9491(2) 0.19849(7) 0.71886(10) 0.0407(4) Uani 1 1 d . . .
H24A H 1.0368 0.1782 0.7473 0.061 Uiso 1 1 calc R . .
H24B H 0.9201 0.1854 0.6577 0.061 Uiso 1 1 calc R . .
H24C H 0.8748 0.1887 0.7498 0.061 Uiso 1 1 calc R . .
C25 C 0.84928(17) 0.37960(6) 0.97836(9) 0.0296(3) Uani 1 1 d . . .
H25 H 0.7860 0.4014 0.9289 0.036 Uiso 1 1 calc R . .
C26 C 0.9242(2) 0.42639(7) 1.04424(11) 0.0456(4) Uani 1 1 d . . .
H26A H 0.9710 0.4066 1.0989 0.068 Uiso 1 1 calc R . .
H26B H 0.8547 0.4550 1.0563 0.068 Uiso 1 1 calc R . .
H26C H 0.9947 0.4475 1.0197 0.068 Uiso 1 1 calc R . .
C27 C 0.75572(17) 0.34032(7) 1.02201(10) 0.0337(3) Uani 1 1 d . . .
H27A H 0.7078 0.3104 0.9800 0.051 Uiso 1 1 calc R . .
H27B H 0.6852 0.3652 1.0409 0.051 Uiso 1 1 calc R . .
H27C H 0.8143 0.3202 1.0730 0.051 Uiso 1 1 calc R . .
C28 C 0.74301(16) 0.52121(6) 0.75954(12) 0.0338(3) Uani 1 1 d . . .
H28A H 0.7450 0.5225 0.8224 0.051 Uiso 1 1 calc R . .
H28B H 0.6448 0.5223 0.7260 0.051 Uiso 1 1 calc R . .
H28C H 0.7941 0.5557 0.7438 0.051 Uiso 1 1 calc R . .
C29 C 0.82727(17) 0.44509(8) 0.61595(9) 0.0354(3) Uani 1 1 d . . .
H29A H 0.8880 0.4760 0.5998 0.053 Uiso 1 1 calc R . .
H29B H 0.7306 0.4501 0.5812 0.053 Uiso 1 1 calc R . .
H29C H 0.8626 0.4057 0.6043 0.053 Uiso 1 1 calc R . .
C30 C 1.01217(14) 0.44801(6) 0.79900(9) 0.0245(3) Uani 1 1 d . . .
H30A H 1.0582 0.4122 0.7828 0.037 Uiso 1 1 calc R . .
H30B H 1.0119 0.4465 0.8615 0.037 Uiso 1 1 calc R . .
H30C H 1.0639 0.4835 0.7872 0.037 Uiso 1 1 calc R . .
S S 0.47805(3) 0.144864(13) 0.80185(2) 0.02387(9) Uani 1 1 d . . .
O1 O 0.39665(12) 0.19386(5) 0.75694(7) 0.0340(2) Uani 1 1 d . . .
O2 O 0.62950(11) 0.15182(4) 0.81744(8) 0.0331(2) Uani 1 1 d . . .
O3 O 0.42680(13) 0.08632(5) 0.77411(9) 0.0460(3) Uani 1 1 d . . .
C31 C 0.44617(16) 0.15095(7) 0.91109(10) 0.0327(3) Uani 1 1 d . . .
F1 F 0.48419(12) 0.20508(5) 0.94514(7) 0.0527(3) Uani 1 1 d . . .
F2 F 0.51814(12) 0.11027(6) 0.96540(8) 0.0635(4) Uani 1 1 d . . .
F3 F 0.31028(10) 0.14349(5) 0.91181(7) 0.0460(3) 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
Si C30 1.8491(13) . ?
Si C29 1.8496(15) . ?
Si C28 1.8519(15) . ?
Si C1 1.9330(12) . ?
N1 C1 1.3567(15) . ?
N1 C2 1.3841(15) . ?
N1 C4 1.4555(15) . ?
N2 C1 1.3570(15) . ?
N2 C3 1.3815(16) . ?
N2 C16 1.4531(15) . ?
C2 C3 1.3444(18) . ?
C4 C5 1.3989(17) . ?
C4 C9 1.4048(17) . ?
C5 C6 1.3982(17) . ?
C5 C10 1.5180(17) . ?
C6 C7 1.3844(18) . ?
C7 C8 1.3852(19) . ?
C8 C9 1.3945(17) . ?
C9 C13 1.5225(17) . ?
C10 C11 1.5335(18) . ?
C10 C12 1.5337(19) . ?
C13 C14 1.5300(19) . ?
C13 C15 1.5364(19) . ?
C16 C17 1.3962(18) . ?
C16 C21 1.4034(17) . ?
C17 C18 1.3997(18) . ?
C17 C22 1.5208(19) . ?
C18 C19 1.381(2) . ?
C19 C20 1.384(2) . ?
C20 C21 1.3991(19) . ?
C21 C25 1.520(2) . ?
C22 C24 1.532(2) . ?
C22 C23 1.532(2) . ?
C25 C27 1.532(2) . ?
C25 C26 1.534(2) . ?
S O3 1.4353(10) . ?
S O1 1.4405(11) . ?
S O2 1.4448(10) . ?
S C31 1.8107(16) . ?
C31 F2 1.3323(17) . ?
C31 F3 1.3335(17) . ?
C31 F1 1.343(2) . ?

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
C30 Si C29 109.53(7) . . ?
C30 Si C28 109.94(7) . . ?
C29 Si C28 112.42(8) . . ?
C30 Si C1 109.67(5) . . ?
C29 Si C1 104.77(6) . . ?
C28 Si C1 110.39(6) . . ?
C1 N1 C2 110.19(10) . . ?
C1 N1 C4 127.71(10) . . ?
C2 N1 C4 121.93(10) . . ?
C1 N2 C3 110.68(10) . . ?
C1 N2 C16 127.95(10) . . ?
C3 N2 C16 121.24(10) . . ?
N1 C1 N2 105.07(10) . . ?
N1 C1 Si 126.65(8) . . ?
N2 C1 Si 127.79(9) . . ?
C3 C2 N1 107.32(11) . . ?
C2 C3 N2 106.73(11) . . ?
C5 C4 C9 123.62(11) . . ?
C5 C4 N1 118.42(10) . . ?
C9 C4 N1 117.77(10) . . ?
C6 C5 C4 116.73(11) . . ?
C6 C5 C10 119.72(11) . . ?
C4 C5 C10 123.46(11) . . ?
C7 C6 C5 121.09(12) . . ?
C6 C7 C8 120.71(12) . . ?
C7 C8 C9 120.81(12) . . ?
C8 C9 C4 117.02(11) . . ?
C8 C9 C13 120.67(11) . . ?
C4 C9 C13 122.30(11) . . ?
C5 C10 C11 112.67(11) . . ?
C5 C10 C12 109.72(11) . . ?
C11 C10 C12 109.25(11) . . ?
C9 C13 C14 112.42(11) . . ?
C9 C13 C15 111.14(11) . . ?
C14 C13 C15 110.16(11) . . ?
C17 C16 C21 123.91(12) . . ?
C17 C16 N2 118.23(11) . . ?
C21 C16 N2 117.78(11) . . ?
C16 C17 C18 117.18(12) . . ?
C16 C17 C22 123.04(11) . . ?
C18 C17 C22 119.77(12) . . ?
C19 C18 C17 120.46(14) . . ?
C18 C19 C20 120.95(13) . . ?
C19 C20 C21 121.23(13) . . ?
C20 C21 C16 116.24(13) . . ?
C20 C21 C25 121.41(12) . . ?
C16 C21 C25 122.34(12) . . ?
C17 C22 C24 110.78(12) . . ?
C17 C22 C23 111.54(13) . . ?
C24 C22 C23 110.61(13) . . ?
C21 C25 C27 112.17(11) . . ?
C21 C25 C26 112.26(14) . . ?
C27 C25 C26 109.39(12) . . ?
O3 S O1 115.72(7) . . ?
O3 S O2 114.86(7) . . ?
O1 S O2 115.25(6) . . ?
O3 S C31 103.49(8) . . ?
O1 S C31 102.22(7) . . ?
O2 S C31 102.52(7) . . ?
F2 C31 F3 106.69(13) . . ?
F2 C31 F1 107.87(14) . . ?
F3 C31 F1 107.11(13) . . ?
F2 C31 S 111.99(11) . . ?
F3 C31 S 112.26(11) . . ?
F1 C31 S 110.65(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N2 -0.90(13) . . . . ?
C4 N1 C1 N2 174.49(10) . . . . ?
C2 N1 C1 Si 171.53(9) . . . . ?
C4 N1 C1 Si -13.08(17) . . . . ?
C3 N2 C1 N1 0.98(13) . . . . ?
C16 N2 C1 N1 -174.89(11) . . . . ?
C3 N2 C1 Si -171.33(9) . . . . ?
C16 N2 C1 Si 12.80(17) . . . . ?
C30 Si C1 N1 176.05(10) . . . . ?
C29 Si C1 N1 -66.47(12) . . . . ?
C28 Si C1 N1 54.78(12) . . . . ?
C30 Si C1 N2 -13.21(12) . . . . ?
C29 Si C1 N2 104.27(11) . . . . ?
C28 Si C1 N2 -134.48(11) . . . . ?
C1 N1 C2 C3 0.50(14) . . . . ?
C4 N1 C2 C3 -175.21(11) . . . . ?
N1 C2 C3 N2 0.12(14) . . . . ?
C1 N2 C3 C2 -0.70(14) . . . . ?
C16 N2 C3 C2 175.49(11) . . . . ?
C1 N1 C4 C5 104.67(14) . . . . ?
C2 N1 C4 C5 -80.42(14) . . . . ?
C1 N1 C4 C9 -80.19(15) . . . . ?
C2 N1 C4 C9 94.72(14) . . . . ?
C9 C4 C5 C6 -0.32(18) . . . . ?
N1 C4 C5 C6 174.51(11) . . . . ?
C9 C4 C5 C10 -176.86(11) . . . . ?
N1 C4 C5 C10 -2.03(17) . . . . ?
C4 C5 C6 C7 0.48(18) . . . . ?
C10 C5 C6 C7 177.16(12) . . . . ?
C5 C6 C7 C8 0.3(2) . . . . ?
C6 C7 C8 C9 -1.3(2) . . . . ?
C7 C8 C9 C4 1.45(18) . . . . ?
C7 C8 C9 C13 -177.32(12) . . . . ?
C5 C4 C9 C8 -0.63(18) . . . . ?
N1 C4 C9 C8 -175.49(11) . . . . ?
C5 C4 C9 C13 178.12(11) . . . . ?
N1 C4 C9 C13 3.26(17) . . . . ?
C6 C5 C10 C11 42.43(16) . . . . ?
C4 C5 C10 C11 -141.13(12) . . . . ?
C6 C5 C10 C12 -79.53(15) . . . . ?
C4 C5 C10 C12 96.91(14) . . . . ?
C8 C9 C13 C14 -29.85(17) . . . . ?
C4 C9 C13 C14 151.45(12) . . . . ?
C8 C9 C13 C15 94.16(14) . . . . ?
C4 C9 C13 C15 -84.54(15) . . . . ?
C1 N2 C16 C17 -102.63(14) . . . . ?
C3 N2 C16 C17 81.89(15) . . . . ?
C1 N2 C16 C21 80.45(15) . . . . ?
C3 N2 C16 C21 -95.03(14) . . . . ?
C21 C16 C17 C18 0.84(19) . . . . ?
N2 C16 C17 C18 -175.87(11) . . . . ?
C21 C16 C17 C22 -179.34(12) . . . . ?
N2 C16 C17 C22 3.95(18) . . . . ?
C16 C17 C18 C19 -0.2(2) . . . . ?
C22 C17 C18 C19 179.99(13) . . . . ?
C17 C18 C19 C20 -0.7(2) . . . . ?
C18 C19 C20 C21 1.0(2) . . . . ?
C19 C20 C21 C16 -0.3(2) . . . . ?
C19 C20 C21 C25 179.64(13) . . . . ?
C17 C16 C21 C20 -0.58(19) . . . . ?
N2 C16 C21 C20 176.14(11) . . . . ?
C17 C16 C21 C25 179.44(12) . . . . ?
N2 C16 C21 C25 -3.83(18) . . . . ?
C16 C17 C22 C24 -107.62(15) . . . . ?
C18 C17 C22 C24 72.20(17) . . . . ?
C16 C17 C22 C23 128.70(14) . . . . ?
C18 C17 C22 C23 -51.48(17) . . . . ?
C20 C21 C25 C27 -90.04(16) . . . . ?
C16 C21 C25 C27 89.93(15) . . . . ?
C20 C21 C25 C26 33.60(18) . . . . ?
C16 C21 C25 C26 -146.43(13) . . . . ?
O3 S C31 F2 62.02(14) . . . . ?
O1 S C31 F2 -177.41(12) . . . . ?
O2 S C31 F2 -57.73(13) . . . . ?
O3 S C31 F3 -57.98(13) . . . . ?
O1 S C31 F3 62.58(12) . . . . ?
O2 S C31 F3 -177.73(11) . . . . ?
O3 S C31 F1 -177.60(10) . . . . ?
O1 S C31 F1 -57.03(11) . . . . ?
O2 S C31 F1 62.66(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.042
_refine_instructions_details     
;
TITL eileen64 in P2(1)/n
CELL 1.54184   9.716539  22.408394  15.656612  90.0000 103.0178  90.0000
ZERR    4.00   0.00013   0.00020   0.00018   0.0000   0.0012   0.0000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    F    SI   S
UNIT  124  180  8  12  12  4  4
MERG   2
TEMP -173
 
FMAP   2
PLAN   10
 
ACTA 150
CONF
 
L.S.   4
 
WGHT    0.042900    1.526700
FVAR       3.65196
SI    6    0.828259    0.451620    0.733848    11.00000    0.01580    0.01644 =
         0.02072    0.00441    0.00167   -0.00158
N1    3    0.584896    0.371641    0.727541    11.00000    0.01561    0.01348 =
         0.01864    0.00059    0.00175   -0.00042
N2    3    0.776858    0.332147    0.801926    11.00000    0.01712    0.01370 =
         0.01835    0.00163    0.00216    0.00017
C1    1    0.724378    0.382735    0.759046    11.00000    0.01544    0.01506 =
         0.01577    0.00019    0.00172    0.00089
C2    1    0.552265    0.314399    0.749698    11.00000    0.02143    0.01415 =
         0.02481    0.00083    0.00456   -0.00429
AFIX  43
H2    2    0.461946    0.295985    0.734901    11.00000   -1.20000
AFIX   0
C3    1    0.672055    0.289686    0.796036    11.00000    0.02249    0.01457 =
         0.02426    0.00104    0.00429   -0.00319
AFIX  43
H3    2    0.682595    0.250586    0.820079    11.00000   -1.20000
AFIX   0
C4    1    0.476892    0.412911    0.682640    11.00000    0.01332    0.01458 =
         0.02105    0.00145    0.00207   -0.00029
C5    1    0.428196    0.407322    0.591853    11.00000    0.01566    0.01646 =
         0.02133   -0.00087    0.00276   -0.00193
C6    1    0.315853    0.444210    0.552202    11.00000    0.01892    0.02269 =
         0.02106    0.00168    0.00031    0.00112
AFIX  43
H6    2    0.279070    0.441626    0.490727    11.00000   -1.20000
AFIX   0
C7    1    0.257332    0.484438    0.601047    11.00000    0.01851    0.02235 =
         0.02856    0.00405    0.00300    0.00520
AFIX  43
H7    2    0.180725    0.508914    0.572762    11.00000   -1.20000
AFIX   0
C8    1    0.309277    0.489384    0.690717    11.00000    0.02092    0.01981 =
         0.02765   -0.00028    0.00818    0.00344
AFIX  43
H8    2    0.269186    0.517822    0.723027    11.00000   -1.20000
AFIX   0
C9    1    0.419695    0.453133    0.734143    11.00000    0.01726    0.01790 =
         0.02116   -0.00069    0.00511   -0.00161
C10   1    0.485380    0.361702    0.537069    11.00000    0.01861    0.02328 =
         0.02125   -0.00453    0.00035    0.00215
AFIX  13
H10   2    0.581209    0.348984    0.570233    11.00000   -1.20000
AFIX   0
C11   1    0.498904    0.386598    0.448094    11.00000    0.02582    0.03966 =
         0.02164   -0.00543    0.00485   -0.00078
AFIX 137
H11A  2    0.404527    0.393238    0.411002    11.00000   -1.50000
H11B  2    0.550239    0.357992    0.419518    11.00000   -1.50000
H11C  2    0.550590    0.424475    0.456899    11.00000   -1.50000
AFIX   0
C12   1    0.388957    0.306707    0.522282    11.00000    0.03278    0.02292 =
         0.03432   -0.00859    0.00304   -0.00114
AFIX 137
H12A  2    0.385578    0.288957    0.578980    11.00000   -1.50000
H12B  2    0.426119    0.277407    0.486802    11.00000   -1.50000
H12C  2    0.293562    0.318616    0.491616    11.00000   -1.50000
AFIX   0
C13   1    0.472260    0.456794    0.833244    11.00000    0.02111    0.02617 =
         0.02053   -0.00267    0.00497    0.00022
AFIX  13
H13   2    0.575641    0.447633    0.847300    11.00000   -1.20000
AFIX   0
C14   1    0.453568    0.519107    0.868952    11.00000    0.04379    0.03270 =
         0.02693   -0.00879    0.01038    0.00133
AFIX 137
H14A  2    0.491598    0.548979    0.834757    11.00000   -1.50000
H14B  2    0.504225    0.521436    0.930519    11.00000   -1.50000
H14C  2    0.352907    0.526818    0.864453    11.00000   -1.50000
AFIX   0
C15   1    0.399380    0.410003    0.879653    11.00000    0.02662    0.03644 =
         0.02273    0.00404    0.00672   -0.00021
AFIX 137
H15A  2    0.298450    0.419245    0.869856    11.00000   -1.50000
H15B  2    0.441744    0.410585    0.942682    11.00000   -1.50000
H15C  2    0.411460    0.370333    0.856024    11.00000   -1.50000
AFIX   0
C16   1    0.918910    0.321597    0.853547    11.00000    0.01724    0.01582 =
         0.01954    0.00521   -0.00060   -0.00015
C17   1    1.011397    0.288337    0.815890    11.00000    0.02087    0.02229 =
         0.02269    0.00718    0.00302    0.00332
C18   1    1.144418    0.275398    0.868832    11.00000    0.02033    0.03048 =
         0.03368    0.01145    0.00387    0.00493
AFIX  43
H18   2    1.210303    0.252770    0.845702    11.00000   -1.20000
AFIX   0
C19   1    1.180567    0.295296    0.954468    11.00000    0.02300    0.03303 =
         0.03494    0.01070   -0.00627   -0.00122
AFIX  43
H19   2    1.270848    0.285793    0.989822    11.00000   -1.20000
AFIX   0
C20   1    1.087169    0.328877    0.989511    11.00000    0.03444    0.02488 =
         0.02430    0.00328   -0.00731   -0.00543
AFIX  43
H20   2    1.115023    0.342569    1.048305    11.00000   -1.20000
AFIX   0
C21   1    0.952495    0.343038    0.939974    11.00000    0.02979    0.01545 =
         0.02042    0.00290    0.00063   -0.00170
C22   1    0.973343    0.266084    0.721735    11.00000    0.03129    0.03454 =
         0.02181    0.00492    0.00535    0.01512
AFIX  13
H22   2    0.882930    0.285701    0.691703    11.00000   -1.20000
AFIX   0
C23   1    1.086548    0.282923    0.671892    11.00000    0.05079    0.05727 =
         0.03380    0.01447    0.02209    0.02201
AFIX 137
H23A  2    1.102627    0.326109    0.675862    11.00000   -1.50000
H23B  2    1.054702    0.271391    0.610215    11.00000   -1.50000
H23C  2    1.174717    0.262039    0.697721    11.00000   -1.50000
AFIX   0
C24   1    0.949062    0.198490    0.718864    11.00000    0.05417    0.03707 =
         0.02807   -0.00546    0.00314    0.00904
AFIX 137
H24A  2    1.036773    0.178183    0.747267    11.00000   -1.50000
H24B  2    0.920075    0.185387    0.657724    11.00000   -1.50000
H24C  2    0.874807    0.188662    0.749766    11.00000   -1.50000
AFIX   0
C25   1    0.849276    0.379601    0.978361    11.00000    0.04459    0.02189 =
         0.02052    0.00031    0.00350    0.00677
AFIX  13
H25   2    0.786032    0.401376    0.928950    11.00000   -1.20000
AFIX   0
C26   1    0.924182    0.426389    1.044237    11.00000    0.07333    0.02967 =
         0.03849   -0.01117    0.02240   -0.01340
AFIX 137
H26A  2    0.970978    0.406558    1.098860    11.00000   -1.50000
H26B  2    0.854670    0.455011    1.056275    11.00000   -1.50000
H26C  2    0.994737    0.447479    1.019651    11.00000   -1.50000
AFIX   0
C27   1    0.755723    0.340321    1.022007    11.00000    0.03205    0.03203 =
         0.03759   -0.00729    0.00892    0.00171
AFIX 137
H27A  2    0.707809    0.310418    0.979997    11.00000   -1.50000
H27B  2    0.685181    0.365221    1.040930    11.00000   -1.50000
H27C  2    0.814344    0.320201    1.073007    11.00000   -1.50000
AFIX   0
C28   1    0.743008    0.521205    0.759538    11.00000    0.02478    0.01871 =
         0.05941    0.00471    0.01237   -0.00170
AFIX 137
H28A  2    0.745011    0.522452    0.822374    11.00000   -1.50000
H28B  2    0.644820    0.522265    0.726041    11.00000   -1.50000
H28C  2    0.794079    0.555723    0.743793    11.00000   -1.50000
AFIX   0
C29   1    0.827273    0.445090    0.615946    11.00000    0.03510    0.04584 =
         0.02358    0.00783    0.00332   -0.01332
AFIX 137
H29A  2    0.888042    0.476031    0.599810    11.00000   -1.50000
H29B  2    0.730609    0.450129    0.581226    11.00000   -1.50000
H29C  2    0.862645    0.405651    0.604331    11.00000   -1.50000
AFIX   0
C30   1    1.012166    0.448008    0.799004    11.00000    0.02021    0.02194 =
         0.02897    0.00613    0.00075   -0.00427
AFIX 137
H30A  2    1.058151    0.412161    0.782796    11.00000   -1.50000
H30B  2    1.011944    0.446459    0.861527    11.00000   -1.50000
H30C  2    1.063872    0.483491    0.787223    11.00000   -1.50000
AFIX   0
S     7    0.478053    0.144864    0.801853    11.00000    0.02581    0.01575 =
         0.03221   -0.00362    0.01111   -0.00413
O1    4    0.396648    0.193863    0.756942    11.00000    0.03744    0.03030 =
         0.03126    0.00678    0.00173   -0.00215
O2    4    0.629495    0.151818    0.817437    11.00000    0.02605    0.02168 =
         0.05705   -0.00278    0.02062   -0.00281
O3    4    0.426798    0.086325    0.774108    11.00000    0.04552    0.02323 =
         0.07483   -0.01973    0.02525   -0.01460
C31   1    0.446173    0.150951    0.911095    11.00000    0.02388    0.04171 =
         0.03292    0.00955    0.00733    0.00949
F1    5    0.484192    0.205081    0.945138    11.00000    0.05258    0.06721 =
         0.03686   -0.02143    0.00710    0.00151
F2    5    0.518138    0.110271    0.965404    11.00000    0.04386    0.09176 =
         0.05736    0.04752    0.01653    0.02849
F3    5    0.310280    0.143493    0.911808    11.00000    0.02927    0.05950 =
         0.05617    0.01977    0.02413    0.01300
 
HKLF    4
;
####################################################################### 
# 
# 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_eileen66
_database_code_depnum_ccdc_archive 'CCDC 1052443'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H35.50 Br0.50 F6 N3 O4 S2 Si'
_chemical_formula_weight         640.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.3958(2)
_cell_length_b                   10.8527(3)
_cell_length_c                   14.7369(3)
_cell_angle_alpha                92.433(2)
_cell_angle_beta                 92.837(2)
_cell_angle_gamma                109.133(2)
_cell_volume                     1415.23(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    87602
_cell_measurement_theta_min      4.2980
_cell_measurement_theta_max      75.5890

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.33645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            113557
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.32
_diffrn_reflns_theta_max         75.72
_reflns_number_total             5868
_reflns_number_gt                5800
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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. 

 One SO2CF3 group of the anion ist disordered and was refined on two
 positions. A molecule of bromobenzene is half occupied over an inversion
 centre.
;

_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)+(0.0444P)²+0.7441P] 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         5868
_refine_ls_number_parameters     424
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.040
_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
N1 N 0.91065(12) 0.20841(11) 0.80686(7) 0.0168(2) Uani 1 1 d . . .
N2 N 0.71257(12) 0.19552(11) 0.71760(7) 0.0170(2) Uani 1 1 d . . .
C1 C 0.86696(14) 0.23911(12) 0.72347(8) 0.0161(2) Uani 1 1 d . . .
C2 C 0.78364(15) 0.13292(13) 0.84847(9) 0.0198(3) Uani 1 1 d . . .
C3 C 0.66110(15) 0.12506(13) 0.79340(9) 0.0203(3) Uani 1 1 d . . .
C4 C 1.06018(15) 0.28063(13) 0.86121(9) 0.0191(3) Uani 1 1 d . . .
C5 C 1.02030(17) 0.35495(15) 0.94236(9) 0.0267(3) Uani 1 1 d . . .
H5A H 1.1128 0.4041 0.9793 0.040 Uiso 1 1 calc R . .
H5B H 0.9516 0.2924 0.9797 0.040 Uiso 1 1 calc R . .
H5C H 0.9712 0.4156 0.9196 0.040 Uiso 1 1 calc R . .
C6 C 1.13756(18) 0.18385(16) 0.89214(10) 0.0294(3) Uani 1 1 d . . .
H6A H 1.1376 0.1238 0.8406 0.044 Uiso 1 1 calc R . .
H6B H 1.0827 0.1340 0.9409 0.044 Uiso 1 1 calc R . .
H6C H 1.2418 0.2319 0.9148 0.044 Uiso 1 1 calc R . .
C7 C 1.16334(16) 0.38556(14) 0.80634(10) 0.0249(3) Uani 1 1 d . . .
H7A H 1.1986 0.3440 0.7559 0.037 Uiso 1 1 calc R . .
H7B H 1.2502 0.4399 0.8458 0.037 Uiso 1 1 calc R . .
H7C H 1.1075 0.4403 0.7821 0.037 Uiso 1 1 calc R . .
C8 C 0.78362(19) 0.05676(15) 0.93103(10) 0.0287(3) Uani 1 1 d . . .
H8A H 0.6822 0.0280 0.9536 0.043 Uiso 1 1 calc R . .
H8B H 0.8556 0.1122 0.9785 0.043 Uiso 1 1 calc R . .
H8C H 0.8130 -0.0197 0.9149 0.043 Uiso 1 1 calc R . .
C9 C 0.50180(17) 0.04315(16) 0.80771(11) 0.0305(3) Uani 1 1 d . . .
H9A H 0.5001 -0.0426 0.8269 0.046 Uiso 1 1 calc R . .
H9B H 0.4395 0.0320 0.7507 0.046 Uiso 1 1 calc R . .
H9C H 0.4617 0.0865 0.8549 0.046 Uiso 1 1 calc R . .
C10 C 0.61327(15) 0.24636(14) 0.65499(9) 0.0208(3) Uani 1 1 d . . .
C11 C 0.51039(17) 0.13615(16) 0.59009(10) 0.0287(3) Uani 1 1 d . . .
H11A H 0.5720 0.0970 0.5547 0.043 Uiso 1 1 calc R . .
H11B H 0.4505 0.1714 0.5487 0.043 Uiso 1 1 calc R . .
H11C H 0.4426 0.0694 0.6252 0.043 Uiso 1 1 calc R . .
C12 C 0.71017(16) 0.35866(14) 0.60264(10) 0.0241(3) Uani 1 1 d . . .
H12A H 0.7796 0.4253 0.6456 0.036 Uiso 1 1 calc R . .
H12B H 0.6449 0.3972 0.5685 0.036 Uiso 1 1 calc R . .
H12C H 0.7682 0.3255 0.5602 0.036 Uiso 1 1 calc R . .
C13 C 0.52320(17) 0.30716(16) 0.71628(11) 0.0302(3) Uani 1 1 d . . .
H13A H 0.4577 0.2395 0.7518 0.045 Uiso 1 1 calc R . .
H13B H 0.4613 0.3449 0.6785 0.045 Uiso 1 1 calc R . .
H13C H 0.5932 0.3758 0.7577 0.045 Uiso 1 1 calc R . .
C14 C 1.09696(17) 0.40533(14) 0.58083(10) 0.0268(3) Uani 1 1 d . . .
H14A H 1.1896 0.4416 0.6205 0.040 Uiso 1 1 calc R . .
H14B H 1.0364 0.4634 0.5851 0.040 Uiso 1 1 calc R . .
H14C H 1.1231 0.3975 0.5178 0.040 Uiso 1 1 calc R . .
C15 C 1.10498(16) 0.13805(14) 0.64607(9) 0.0225(3) Uani 1 1 d . . .
H15A H 1.1565 0.1238 0.5924 0.034 Uiso 1 1 calc R . .
H15B H 1.0408 0.0537 0.6654 0.034 Uiso 1 1 calc R . .
H15C H 1.1801 0.1827 0.6956 0.034 Uiso 1 1 calc R . .
C16 C 0.86323(16) 0.14069(14) 0.51891(9) 0.0237(3) Uani 1 1 d . . .
H16A H 0.9264 0.1198 0.4737 0.036 Uiso 1 1 calc R . .
H16B H 0.8039 0.1902 0.4911 0.036 Uiso 1 1 calc R . .
H16C H 0.7950 0.0595 0.5404 0.036 Uiso 1 1 calc R . .
Si Si 0.98614(4) 0.24073(3) 0.61721(2) 0.01693(9) Uani 1 1 d . . .
N3 N 0.82488(14) 0.69082(12) 0.69024(8) 0.0244(2) Uani 1 1 d . A .
S1 S 0.90616(4) 0.69325(3) 0.78651(2) 0.01950(8) Uani 1 1 d . . .
O1 O 0.88573(13) 0.78012(11) 0.85635(7) 0.0310(2) Uani 1 1 d . . .
O2 O 0.88948(12) 0.56167(10) 0.80731(7) 0.0281(2) Uani 1 1 d . . .
C17 C 1.10556(16) 0.76214(14) 0.76343(10) 0.0252(3) Uani 1 1 d . . .
F1 F 1.13757(10) 0.88282(9) 0.73613(7) 0.0379(2) Uani 1 1 d . . .
F2 F 1.14266(11) 0.69091(10) 0.69966(7) 0.0392(2) Uani 1 1 d . . .
F3 F 1.19117(11) 0.76658(11) 0.83907(7) 0.0431(3) Uani 1 1 d . . .
S2 S 0.74636(4) 0.79021(3) 0.65766(2) 0.02004(9) Uani 1 1 d D . .
O3 O 0.7885(9) 0.9113(7) 0.7100(6) 0.0294(12) Uani 0.503(14) 1 d PDU A 1
O4 O 0.7505(17) 0.7909(14) 0.5606(6) 0.0304(18) Uani 0.503(14) 1 d PDU A 1
C18 C 0.5460(7) 0.7095(8) 0.6740(6) 0.0323(15) Uani 0.503(14) 1 d PDU A 1
F4 F 0.4704(7) 0.7876(7) 0.6480(5) 0.0399(11) Uani 0.503(14) 1 d PDU A 1
F5 F 0.5265(5) 0.6911(9) 0.7620(5) 0.0567(18) Uani 0.503(14) 1 d PDU A 1
F6 F 0.4926(5) 0.5963(4) 0.6264(7) 0.0538(19) Uani 0.503(14) 1 d PDU A 1
O3' O 0.7470(11) 0.8931(8) 0.7215(6) 0.0385(16) Uani 0.497(14) 1 d PDU A 2
O4' O 0.7745(18) 0.8192(15) 0.5659(7) 0.033(2) Uani 0.497(14) 1 d PDU A 2
C18' C 0.5482(8) 0.6820(8) 0.6477(5) 0.0283(15) Uani 0.497(14) 1 d PDU A 2
F4' F 0.4584(7) 0.7508(7) 0.6253(4) 0.0379(10) Uani 0.497(14) 1 d PDU A 2
F5' F 0.5059(3) 0.6286(7) 0.7255(4) 0.0503(14) Uani 0.497(14) 1 d PDU A 2
F6' F 0.5249(6) 0.5874(3) 0.5837(4) 0.0383(10) Uani 0.497(14) 1 d PDU A 2
Br Br 0.57852(6) 0.31809(4) 1.00126(4) 0.02820(14) Uani 0.50 1 d P B -1
C91 C 0.5196(3) 0.46773(18) 0.99601(16) 0.0237(6) Uani 0.50 1 d PG B -1
C92 C 0.5832(2) 0.5622(2) 0.93549(14) 0.0234(8) Uani 0.50 1 d PG B -1
H92 H 0.6557 0.5508 0.8962 0.028 Uiso 0.50 1 calc PR B -1
C93 C 0.5408(3) 0.67325(18) 0.93247(14) 0.0279(6) Uani 0.50 1 d PG B -1
H93 H 0.5842 0.7378 0.8911 0.034 Uiso 0.50 1 calc PR B -1
C94 C 0.4347(3) 0.68986(19) 0.98997(17) 0.074(4) Uani 0.50 1 d PG B -1
H94 H 0.4057 0.7658 0.9879 0.089 Uiso 0.50 1 calc PR B -1
C95 C 0.3711(2) 0.5954(2) 1.05049(14) 0.0275(6) Uani 0.50 1 d PG B -1
H95 H 0.2986 0.6068 1.0898 0.033 Uiso 0.50 1 calc PR B -1
C96 C 0.4135(2) 0.48434(19) 1.05351(13) 0.0237(9) Uani 0.50 1 d PG B -1
H96 H 0.3701 0.4198 1.0949 0.028 Uiso 0.50 1 calc PR B -1


_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
N1 C1 1.3653(16) . ?
N1 C2 1.3949(17) . ?
N1 C4 1.5308(16) . ?
N2 C1 1.3674(16) . ?
N2 C3 1.3964(17) . ?
N2 C10 1.5237(16) . ?
C1 Si 1.9671(13) . ?
C2 C3 1.352(2) . ?
C2 C8 1.4996(19) . ?
C3 C9 1.5000(19) . ?
C4 C7 1.524(2) . ?
C4 C6 1.5324(18) . ?
C4 C5 1.5432(18) . ?
C10 C12 1.527(2) . ?
C10 C11 1.5274(18) . ?
C10 C13 1.5358(19) . ?
C14 Si 1.8655(15) . ?
C15 Si 1.8650(14) . ?
C16 Si 1.8681(14) . ?
N3 S2 1.5713(12) . ?
N3 S1 1.5726(12) . ?
S1 O1 1.4285(11) . ?
S1 O2 1.4329(11) . ?
S1 C17 1.8307(15) . ?
C17 F2 1.3226(18) . ?
C17 F1 1.3290(17) . ?
C17 F3 1.3316(17) . ?
S2 O4' 1.420(9) . ?
S2 O3 1.422(7) . ?
S2 O3' 1.428(7) . ?
S2 O4 1.433(8) . ?
S2 C18 1.831(6) . ?
S2 C18' 1.842(7) . ?
C18 F6 1.319(6) . ?
C18 F4 1.329(8) . ?
C18 F5 1.333(7) . ?
C18' F6' 1.320(6) . ?
C18' F5' 1.327(7) . ?
C18' F4' 1.336(8) . ?
Br C91 1.8829(14) . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C92 C93 1.3900 . ?
C93 C94 1.3900 . ?
C94 C95 1.3900 . ?
C95 C96 1.3900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 109.26(11) . . ?
C1 N1 C4 125.60(11) . . ?
C2 N1 C4 122.01(10) . . ?
C1 N2 C3 109.13(11) . . ?
C1 N2 C10 125.27(11) . . ?
C3 N2 C10 123.50(11) . . ?
N1 C1 N2 106.35(11) . . ?
N1 C1 Si 121.67(9) . . ?
N2 C1 Si 122.72(9) . . ?
C3 C2 N1 107.42(11) . . ?
C3 C2 C8 125.70(13) . . ?
N1 C2 C8 126.21(13) . . ?
C2 C3 N2 107.40(11) . . ?
C2 C3 C9 125.32(13) . . ?
N2 C3 C9 126.98(13) . . ?
C7 C4 N1 111.09(10) . . ?
C7 C4 C6 111.31(12) . . ?
N1 C4 C6 110.47(11) . . ?
C7 C4 C5 105.55(11) . . ?
N1 C4 C5 106.04(10) . . ?
C6 C4 C5 112.18(11) . . ?
N2 C10 C12 110.50(11) . . ?
N2 C10 C11 110.65(11) . . ?
C12 C10 C11 111.12(12) . . ?
N2 C10 C13 106.97(11) . . ?
C12 C10 C13 105.33(12) . . ?
C11 C10 C13 112.08(12) . . ?
C15 Si C14 113.36(7) . . ?
C15 Si C16 101.00(6) . . ?
C14 Si C16 109.96(7) . . ?
C15 Si C1 105.10(6) . . ?
C14 Si C1 115.93(6) . . ?
C16 Si C1 110.40(6) . . ?
S2 N3 S1 126.62(8) . . ?
O1 S1 O2 118.64(7) . . ?
O1 S1 N3 117.03(7) . . ?
O2 S1 N3 108.67(7) . . ?
O1 S1 C17 104.49(7) . . ?
O2 S1 C17 103.48(6) . . ?
N3 S1 C17 102.05(7) . . ?
F2 C17 F1 107.99(12) . . ?
F2 C17 F3 108.18(12) . . ?
F1 C17 F3 108.28(12) . . ?
F2 C17 S1 111.71(10) . . ?
F1 C17 S1 111.09(10) . . ?
F3 C17 S1 109.48(10) . . ?
O4' S2 O3 107.2(7) . . ?
O4' S2 O3' 118.8(7) . . ?
O3 S2 O3' 17.0(4) . . ?
O4' S2 O4 12.9(9) . . ?
O3 S2 O4 119.1(6) . . ?
O3' S2 O4 128.9(8) . . ?
O4' S2 N3 111.1(8) . . ?
O3 S2 N3 115.5(4) . . ?
O3' S2 N3 117.4(4) . . ?
O4 S2 N3 107.3(7) . . ?
O4' S2 C18 112.9(7) . . ?
O3 S2 C18 105.7(3) . . ?
O3' S2 C18 89.1(3) . . ?
O4 S2 C18 103.1(6) . . ?
N3 S2 C18 104.4(2) . . ?
O4' S2 C18' 102.3(6) . . ?
O3 S2 C18' 120.2(3) . . ?
O3' S2 C18' 104.0(3) . . ?
O4 S2 C18' 91.2(6) . . ?
N3 S2 C18' 99.6(2) . . ?
C18 S2 C18' 15.2(2) . . ?
F6 C18 F4 109.7(5) . . ?
F6 C18 F5 109.7(5) . . ?
F4 C18 F5 107.7(5) . . ?
F6 C18 S2 111.3(4) . . ?
F4 C18 S2 108.5(5) . . ?
F5 C18 S2 109.9(4) . . ?
F6' C18' F5' 108.5(5) . . ?
F6' C18' F4' 107.4(5) . . ?
F5' C18' F4' 107.8(5) . . ?
F6' C18' S2 111.7(4) . . ?
F5' C18' S2 111.7(4) . . ?
F4' C18' S2 109.6(5) . . ?
C92 C91 C96 120.0 . . ?
C92 C91 Br 120.12(13) . . ?
C96 C91 Br 119.87(13) . . ?
C93 C92 C91 120.0 . . ?
C94 C93 C92 120.0 . . ?
C95 C94 C93 120.0 . . ?
C94 C95 C96 120.0 . . ?
C95 C96 C91 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N2 6.59(13) . . . . ?
C4 N1 C1 N2 -153.55(11) . . . . ?
C2 N1 C1 Si -140.85(9) . . . . ?
C4 N1 C1 Si 59.01(15) . . . . ?
C3 N2 C1 N1 -6.49(14) . . . . ?
C10 N2 C1 N1 157.43(11) . . . . ?
C3 N2 C1 Si 140.52(10) . . . . ?
C10 N2 C1 Si -55.55(15) . . . . ?
C1 N1 C2 C3 -4.23(14) . . . . ?
C4 N1 C2 C3 156.76(11) . . . . ?
C1 N1 C2 C8 166.81(13) . . . . ?
C4 N1 C2 C8 -32.20(19) . . . . ?
N1 C2 C3 N2 0.15(14) . . . . ?
C8 C2 C3 N2 -170.95(12) . . . . ?
N1 C2 C3 C9 174.16(13) . . . . ?
C8 C2 C3 C9 3.1(2) . . . . ?
C1 N2 C3 C2 3.98(14) . . . . ?
C10 N2 C3 C2 -160.30(11) . . . . ?
C1 N2 C3 C9 -169.91(13) . . . . ?
C10 N2 C3 C9 25.8(2) . . . . ?
C1 N1 C4 C7 -5.35(17) . . . . ?
C2 N1 C4 C7 -163.13(11) . . . . ?
C1 N1 C4 C6 -129.38(13) . . . . ?
C2 N1 C4 C6 72.84(15) . . . . ?
C1 N1 C4 C5 108.85(14) . . . . ?
C2 N1 C4 C5 -48.93(15) . . . . ?
C1 N2 C10 C12 -2.97(16) . . . . ?
C3 N2 C10 C12 158.75(12) . . . . ?
C1 N2 C10 C11 120.53(13) . . . . ?
C3 N2 C10 C11 -77.75(15) . . . . ?
C1 N2 C10 C13 -117.12(13) . . . . ?
C3 N2 C10 C13 44.59(16) . . . . ?
N1 C1 Si C15 20.48(12) . . . . ?
N2 C1 Si C15 -121.65(11) . . . . ?
N1 C1 Si C14 -105.52(11) . . . . ?
N2 C1 Si C14 112.34(11) . . . . ?
N1 C1 Si C16 128.62(11) . . . . ?
N2 C1 Si C16 -13.52(13) . . . . ?
S2 N3 S1 O1 11.25(13) . . . . ?
S2 N3 S1 O2 149.02(9) . . . . ?
S2 N3 S1 C17 -102.09(11) . . . . ?
O1 S1 C17 F2 179.56(10) . . . . ?
O2 S1 C17 F2 54.73(11) . . . . ?
N3 S1 C17 F2 -58.08(11) . . . . ?
O1 S1 C17 F1 -59.78(12) . . . . ?
O2 S1 C17 F1 175.40(10) . . . . ?
N3 S1 C17 F1 62.58(12) . . . . ?
O1 S1 C17 F3 59.76(12) . . . . ?
O2 S1 C17 F3 -65.07(12) . . . . ?
N3 S1 C17 F3 -177.88(10) . . . . ?
S1 N3 S2 O4' 140.8(6) . . . . ?
S1 N3 S2 O3 18.4(3) . . . . ?
S1 N3 S2 O3' -0.5(5) . . . . ?
S1 N3 S2 O4 153.8(6) . . . . ?
S1 N3 S2 C18 -97.2(3) . . . . ?
S1 N3 S2 C18' -111.9(2) . . . . ?
O4' S2 C18 F6 61.5(9) . . . . ?
O3 S2 C18 F6 178.4(6) . . . . ?
O3' S2 C18 F6 -177.4(6) . . . . ?
O4 S2 C18 F6 52.7(8) . . . . ?
N3 S2 C18 F6 -59.3(5) . . . . ?
C18' S2 C18 F6 14.0(12) . . . . ?
O4' S2 C18 F4 -59.3(9) . . . . ?
O3 S2 C18 F4 57.6(6) . . . . ?
O3' S2 C18 F4 61.8(6) . . . . ?
O4 S2 C18 F4 -68.1(8) . . . . ?
N3 S2 C18 F4 179.9(4) . . . . ?
C18' S2 C18 F4 -106.8(17) . . . . ?
O4' S2 C18 F5 -176.8(8) . . . . ?
O3 S2 C18 F5 -59.9(6) . . . . ?
O3' S2 C18 F5 -55.7(6) . . . . ?
O4 S2 C18 F5 174.4(8) . . . . ?
N3 S2 C18 F5 62.4(4) . . . . ?
C18' S2 C18 F5 135.6(19) . . . . ?
O4' S2 C18' F6' 49.5(9) . . . . ?
O3 S2 C18' F6' 168.0(6) . . . . ?
O3' S2 C18' F6' 173.7(6) . . . . ?
O4 S2 C18' F6' 43.0(8) . . . . ?
N3 S2 C18' F6' -64.8(4) . . . . ?
C18 S2 C18' F6' -175(2) . . . . ?
O4' S2 C18' F5' 171.1(9) . . . . ?
O3 S2 C18' F5' -70.3(7) . . . . ?
O3' S2 C18' F5' -64.6(6) . . . . ?
O4 S2 C18' F5' 164.6(8) . . . . ?
N3 S2 C18' F5' 56.9(4) . . . . ?
C18 S2 C18' F5' -52.9(14) . . . . ?
O4' S2 C18' F4' -69.5(9) . . . . ?
O3 S2 C18' F4' 49.1(7) . . . . ?
O3' S2 C18' F4' 54.8(6) . . . . ?
O4 S2 C18' F4' -76.0(8) . . . . ?
N3 S2 C18' F4' 176.3(4) . . . . ?
C18 S2 C18' F4' 66.5(15) . . . . ?
C96 C91 C92 C93 0.0 . . . . ?
Br C91 C92 C93 -179.28(19) . . . . ?
C91 C92 C93 C94 0.0 . . . . ?
C92 C93 C94 C95 0.0 . . . . ?
C93 C94 C95 C96 0.0 . . . . ?
C94 C95 C96 C91 0.0 . . . . ?
C92 C91 C96 C95 0.0 . . . . ?
Br C91 C96 C95 179.29(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.052
_refine_instructions_details     
;
TITL eileen66 in P-1
CELL 1.54184   9.395844  10.852720  14.736860  92.4330  92.8372 109.1328
ZERR    2.00   0.000200   0.000300   0.000300   0.0020   0.0020   0.0020
LATT   1
SFAC  C    H    N    O    F    SI   S    Br
UNIT  42  71  6  8  12  2  4  1
MERG   2
FMAP   2
 
TEMP -173
 
ACTA 150
CONF
 
OMIT 4 -4 3
 
PLAN   10
 
L.S.   10
 
WGHT    0.044400    0.744100
FVAR       6.87237   0.50320
N1    3    0.910651    0.208414    0.806862    11.00000    0.01752    0.01907 =
         0.01450   -0.00184   -0.00060    0.00758
N2    3    0.712572    0.195518    0.717602    11.00000    0.01557    0.02011 =
         0.01548   -0.00248    0.00003    0.00659
C1    1    0.866960    0.239115    0.723475    11.00000    0.01677    0.01656 =
         0.01538   -0.00169   -0.00012    0.00643
C2    1    0.783635    0.132920    0.848472    11.00000    0.02470    0.02025 =
         0.01600   -0.00046    0.00580    0.00921
C3    1    0.661100    0.125065    0.793405    11.00000    0.02041    0.02116 =
         0.01882   -0.00157    0.00582    0.00596
C4    1    1.060182    0.280633    0.861211    11.00000    0.01882    0.02247 =
         0.01676   -0.00498   -0.00652    0.00962
C5    1    1.020298    0.354950    0.942357    11.00000    0.03162    0.03083 =
         0.01922   -0.00764   -0.00612    0.01480
AFIX 137
H5A   2    1.112771    0.404064    0.979301    11.00000   -1.50000
H5B   2    0.951568    0.292400    0.979709    11.00000   -1.50000
H5C   2    0.971227    0.415579    0.919590    11.00000   -1.50000
AFIX   0
C6    1    1.137562    0.183847    0.892141    11.00000    0.03101    0.03475 =
         0.02778   -0.00199   -0.00734    0.01997
AFIX 137
H6A   2    1.137628    0.123778    0.840590    11.00000   -1.50000
H6B   2    1.082728    0.134012    0.940862    11.00000   -1.50000
H6C   2    1.241815    0.231854    0.914752    11.00000   -1.50000
AFIX   0
C7    1    1.163335    0.385561    0.806343    11.00000    0.01968    0.02507 =
         0.02766   -0.00524   -0.00355    0.00588
AFIX 137
H7A   2    1.198644    0.343988    0.755895    11.00000   -1.50000
H7B   2    1.250249    0.439876    0.845774    11.00000   -1.50000
H7C   2    1.107450    0.440297    0.782076    11.00000   -1.50000
AFIX   0
C8    1    0.783618    0.056763    0.931030    11.00000    0.03987    0.02900 =
         0.02070    0.00595    0.00750    0.01481
AFIX 137
H8A   2    0.682242    0.027969    0.953579    11.00000   -1.50000
H8B   2    0.855631    0.112236    0.978521    11.00000   -1.50000
H8C   2    0.812971   -0.019686    0.914943    11.00000   -1.50000
AFIX   0
C9    1    0.501798    0.043147    0.807708    11.00000    0.02197    0.03196 =
         0.03313   -0.00048    0.00889    0.00225
AFIX 137
H9A   2    0.500106   -0.042639    0.826930    11.00000   -1.50000
H9B   2    0.439465    0.032041    0.750673    11.00000   -1.50000
H9C   2    0.461745    0.086519    0.854867    11.00000   -1.50000
AFIX   0
C10   1    0.613270    0.246358    0.654991    11.00000    0.01798    0.02537 =
         0.02026   -0.00374   -0.00449    0.01044
C11   1    0.510390    0.136149    0.590094    11.00000    0.02316    0.03288 =
         0.02685   -0.00719   -0.00853    0.00728
AFIX 137
H11A  2    0.571990    0.096982    0.554680    11.00000   -1.50000
H11B  2    0.450543    0.171352    0.548730    11.00000   -1.50000
H11C  2    0.442630    0.069405    0.625235    11.00000   -1.50000
AFIX   0
C12   1    0.710172    0.358664    0.602636    11.00000    0.02657    0.02425 =
         0.02375   -0.00069   -0.00365    0.01251
AFIX 137
H12A  2    0.779636    0.425336    0.645561    11.00000   -1.50000
H12B  2    0.644870    0.397234    0.568503    11.00000   -1.50000
H12C  2    0.768200    0.325496    0.560244    11.00000   -1.50000
AFIX   0
C13   1    0.523197    0.307162    0.716281    11.00000    0.02416    0.03650 =
         0.03482   -0.00528    0.00084    0.01762
AFIX 137
H13A  2    0.457671    0.239503    0.751800    11.00000   -1.50000
H13B  2    0.461287    0.344934    0.678478    11.00000   -1.50000
H13C  2    0.593158    0.375850    0.757676    11.00000   -1.50000
AFIX   0
C14   1    1.096958    0.405331    0.580834    11.00000    0.02928    0.02374 =
         0.02673    0.00517    0.00699    0.00660
AFIX 137
H14A  2    1.189615    0.441587    0.620526    11.00000   -1.50000
H14B  2    1.036398    0.463417    0.585082    11.00000   -1.50000
H14C  2    1.123078    0.397459    0.517786    11.00000   -1.50000
AFIX   0
C15   1    1.104978    0.138048    0.646072    11.00000    0.02242    0.02420 =
         0.02301   -0.00018    0.00392    0.01041
AFIX 137
H15A  2    1.156503    0.123775    0.592410    11.00000   -1.50000
H15B  2    1.040759    0.053687    0.665394    11.00000   -1.50000
H15C  2    1.180119    0.182730    0.695578    11.00000   -1.50000
AFIX   0
C16   1    0.863232    0.140686    0.518914    11.00000    0.02867    0.02664 =
         0.01665   -0.00137    0.00145    0.01054
AFIX 137
H16A  2    0.926363    0.119837    0.473746    11.00000   -1.50000
H16B  2    0.803901    0.190210    0.491078    11.00000   -1.50000
H16C  2    0.794956    0.059530    0.540352    11.00000   -1.50000
AFIX   0
 
SI    6    0.986136    0.240726    0.617210    11.00000    0.01826    0.01779 =
         0.01518    0.00105    0.00315    0.00625
N3    3    0.824883    0.690817    0.690237    11.00000    0.02663    0.02457 =
         0.02437   -0.00447   -0.00589    0.01330
S1    7    0.906157    0.693254    0.786513    11.00000    0.01964    0.02118 =
         0.01854    0.00199    0.00151    0.00777
O1    4    0.885733    0.780123    0.856351    11.00000    0.04127    0.03748 =
         0.01976   -0.00185    0.00365    0.02090
O2    4    0.889479    0.561667    0.807313    11.00000    0.02780    0.02369 =
         0.03318    0.00962    0.00266    0.00779
C17   1    1.105562    0.762136    0.763429    11.00000    0.02170    0.02474 =
         0.02961    0.00590   -0.00084    0.00823
F1    5    1.137573    0.882819    0.736133    11.00000    0.02790    0.02602 =
         0.05699    0.01556    0.00192    0.00356
F2    5    1.142656    0.690911    0.699663    11.00000    0.03333    0.04326 =
         0.04758    0.00519    0.01689    0.01942
F3    5    1.191174    0.766580    0.839066    11.00000    0.02659    0.05401 =
         0.04454    0.01125   -0.01288    0.00875
SAME S2 O3' O4' C18' F4' F5' F6'
SADI S2 O3 S2 O4
SADI C18 F4 C18 F5 C18 F6
SADI F4 F5 F5 F6 F6 F4
SIMU 0.02 0.04 0.9 S2 > F6'
 
S2    7    0.746359    0.790211    0.657661    11.00000    0.01962    0.01961 =
         0.02189    0.00313    0.00154    0.00759
PART1 21
O3    4    0.788456    0.911314    0.710010    21.00000    0.03536    0.01861 =
         0.03589    0.00255    0.00199    0.01125
O4    4    0.750489    0.790869    0.560629    21.00000    0.03252    0.04362 =
         0.02097    0.00727    0.00330    0.01979
C18   1    0.546027    0.709470    0.674034    21.00000    0.01946    0.03713 =
         0.04304    0.01489    0.00655    0.01087
F4    5    0.470419    0.787580    0.648017    21.00000    0.02600    0.05365 =
         0.04956    0.01413    0.00522    0.02425
F5    5    0.526451    0.691062    0.762009    21.00000    0.03447    0.09234 =
         0.04909    0.04111    0.02147    0.02179
F6    5    0.492637    0.596303    0.626401    21.00000    0.03008    0.03241 =
         0.08833    0.00184   -0.01646   -0.00093
PART2 -21
O3'   4    0.746983    0.893134    0.721486   -21.00000    0.04710    0.02832 =
         0.04419   -0.01519   -0.01504    0.02287
O4'   4    0.774508    0.819217    0.565885   -21.00000    0.02957    0.03991 =
         0.03153    0.01916    0.01022    0.00976
C18'  1    0.548186    0.682002    0.647721   -21.00000    0.02649    0.04223 =
         0.02252    0.01098    0.00554    0.01837
F4'   5    0.458375    0.750806    0.625293   -21.00000    0.02651    0.05448 =
         0.03966    0.00165    0.00013    0.02330
F5'   5    0.505851    0.628578    0.725547   -21.00000    0.03478    0.07215 =
         0.03711    0.02767    0.01168    0.00420
F6'   5    0.524897    0.587389    0.583708   -21.00000    0.03589    0.03333 =
         0.04108   -0.00604   -0.01463    0.00884
PART0
 
SIMU C91 > C96 0.01 0.04 0.9
 
PART  -1
BR    8    0.578522    0.318093    1.001261    10.50000    0.02808    0.02888 =
         0.03073   -0.00315   -0.00072    0.01458
AFIX  66
C91   1    0.519615    0.467729    0.996008    10.50000    0.01875    0.03264 =
         0.01612   -0.00466   -0.00077    0.00455
C92   1    0.583217    0.562181    0.935490    10.50000    0.02035    0.02740 =
         0.01909   -0.00281    0.00386    0.00338
AFIX  43
H92   2    0.655707    0.550825    0.896191    10.50000   -1.20000
AFIX  65
C93   1    0.540756    0.673246    0.932472    10.50000    0.02918    0.02843 =
         0.02176    0.00112    0.00180    0.00360
AFIX  43
H93   2    0.584225    0.737800    0.891110    10.50000   -1.20000
AFIX  65
C94   1    0.434692    0.689862    0.989971    10.50000    0.06253    0.09564 =
         0.05015    0.00476   -0.01881    0.01083
AFIX  43
H94   2    0.405672    0.765770    0.987908    10.50000   -1.20000
AFIX  65
C95   1    0.371089    0.595411    1.050490    10.50000    0.02290    0.03993 =
         0.02107   -0.00243    0.00228    0.01268
AFIX  43
H95   2    0.298599    0.606767    1.089788    10.50000   -1.20000
AFIX  65
C96   1    0.413549    0.484345    1.053509    10.50000    0.02094    0.03066 =
         0.01881   -0.00046    0.00046    0.00795
AFIX  43
H96   2    0.370079    0.419792    1.094871    10.50000   -1.20000
PART   0
 
HKLF    4
;
####################################################################### 
# 
# 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_eileen24
_database_code_depnum_ccdc_archive 'CCDC 1052444'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H33 B2 F30 N5 Si'
_chemical_formula_weight         1347.54

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   10.5595(6)
_cell_length_b                   14.6325(8)
_cell_length_c                   18.5185(10)
_cell_angle_alpha                97.231(4)
_cell_angle_beta                 94.146(4)
_cell_angle_gamma                110.557(6)
_cell_volume                     2636.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17543
_cell_measurement_theta_min      2.2265
_cell_measurement_theta_max      29.1846

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1348
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9563
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_process_details   
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39)  
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69215
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.48
_reflns_number_total             11974
_reflns_number_gt                9492
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39)  
;
_computing_cell_refinement       
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39)  
;
_computing_data_reduction        
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) 
(compiled May 16 2011,17:55:39)  
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER XP'
_computing_publication_material  SHELXL-97

_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)+(0.0313P)²+1.4470P] 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         11974
_refine_ls_number_parameters     822
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
Si Si 0.25496(5) 0.98070(4) 0.30696(3) 0.02217(11) Uani 1 1 d . . .
B1 B 0.24847(19) 0.30400(13) 0.13983(9) 0.0148(3) Uani 1 1 d . . .
B2 B 0.08604(18) 0.35843(13) 0.37931(9) 0.0130(3) Uani 1 1 d . . .
N1 N 0.29453(14) 0.82853(10) 0.19931(7) 0.0188(3) Uani 1 1 d . . .
N2 N 0.48850(14) 0.93132(10) 0.26051(7) 0.0190(3) Uani 1 1 d . . .
N3 N 0.26089(13) 0.29060(10) 0.22716(7) 0.0148(3) Uani 1 1 d . . .
N4 N 0.18384(13) 0.29365(9) 0.26929(7) 0.0131(3) Uani 1 1 d . . .
N5 N 0.10385(13) 0.28519(10) 0.31092(7) 0.0157(3) Uani 1 1 d . . .
F1 F 0.00182(10) 0.15330(7) 0.16741(5) 0.0207(2) Uani 1 1 d . . .
F2 F -0.25110(10) 0.15226(8) 0.14844(6) 0.0287(2) Uani 1 1 d . . .
F3 F -0.30374(10) 0.29703(8) 0.08752(5) 0.0277(2) Uani 1 1 d . . .
F4 F -0.09441(10) 0.44547(8) 0.04760(6) 0.0288(2) Uani 1 1 d . . .
F5 F 0.16045(9) 0.45080(7) 0.06827(5) 0.0219(2) Uani 1 1 d . . .
F6 F 0.30723(10) 0.49057(7) 0.23513(5) 0.0240(2) Uani 1 1 d . . .
F7 F 0.52132(12) 0.65800(8) 0.24079(6) 0.0384(3) Uani 1 1 d . . .
F8 F 0.70652(12) 0.66944(9) 0.14381(7) 0.0448(3) Uani 1 1 d . . .
F9 F 0.66996(11) 0.50927(9) 0.04025(7) 0.0391(3) Uani 1 1 d . . .
F10 F 0.45688(11) 0.34288(8) 0.03304(5) 0.0278(2) Uani 1 1 d . . .
F11 F 0.08812(11) 0.16957(8) 0.00120(5) 0.0311(3) Uani 1 1 d . . .
F12 F 0.11104(11) 0.00175(8) -0.05493(6) 0.0355(3) Uani 1 1 d . . .
F13 F 0.30211(11) -0.06039(8) 0.00806(6) 0.0351(3) Uani 1 1 d . . .
F14 F 0.47525(10) 0.05521(7) 0.12723(6) 0.0287(2) Uani 1 1 d . . .
F15 F 0.46154(9) 0.22894(7) 0.18160(5) 0.0206(2) Uani 1 1 d . . .
F16 F 0.36190(9) 0.37087(7) 0.40308(5) 0.0195(2) Uani 1 1 d . . .
F17 F 0.58865(9) 0.53257(8) 0.42699(5) 0.0253(2) Uani 1 1 d . . .
F18 F 0.57251(10) 0.71520(8) 0.42779(6) 0.0331(3) Uani 1 1 d . . .
F19 F 0.32467(11) 0.73105(7) 0.40397(6) 0.0297(2) Uani 1 1 d . . .
F20 F 0.09843(9) 0.57262(7) 0.38196(5) 0.0202(2) Uani 1 1 d . . .
F21 F 0.02129(10) 0.43509(7) 0.25240(5) 0.0210(2) Uani 1 1 d . . .
F22 F -0.21140(11) 0.45843(8) 0.21023(5) 0.0280(2) Uani 1 1 d . . .
F23 F -0.42575(10) 0.40154(8) 0.28924(6) 0.0288(2) Uani 1 1 d . . .
F24 F -0.39981(10) 0.32076(8) 0.41276(6) 0.0270(2) Uani 1 1 d . . .
F25 F -0.17171(9) 0.29852(7) 0.45590(5) 0.0214(2) Uani 1 1 d . . .
F26 F 0.10982(10) 0.45647(7) 0.52423(5) 0.0204(2) Uani 1 1 d . . .
F27 F 0.14734(10) 0.39159(7) 0.65062(5) 0.0221(2) Uani 1 1 d . . .
F28 F 0.14639(10) 0.20616(7) 0.64907(5) 0.0246(2) Uani 1 1 d . . .
F29 F 0.11096(12) 0.08615(7) 0.51839(5) 0.0305(2) Uani 1 1 d . . .
F30 F 0.07290(11) 0.14676(7) 0.39261(5) 0.0270(2) Uani 1 1 d . . .
C1 C 0.35003(17) 0.89922(12) 0.26062(8) 0.0187(3) Uani 1 1 d . . .
C2 C 0.39811(18) 0.82504(13) 0.15789(9) 0.0221(4) Uani 1 1 d . . .
C3 C 0.51752(18) 0.88840(12) 0.19563(9) 0.0217(4) Uani 1 1 d . . .
C4 C 0.15271(18) 0.74751(13) 0.18676(9) 0.0235(4) Uani 1 1 d . . .
C5 C 0.0661(2) 0.75996(16) 0.12165(10) 0.0336(4) Uani 1 1 d . . .
H5A H -0.0222 0.7050 0.1126 0.050 Uiso 1 1 calc R . .
H5B H 0.1133 0.7602 0.0780 0.050 Uiso 1 1 calc R . .
H5C H 0.0517 0.8226 0.1326 0.050 Uiso 1 1 calc R . .
C6 C 0.08316(19) 0.74674(14) 0.25623(10) 0.0271(4) Uani 1 1 d . . .
H6A H 0.1419 0.7402 0.2972 0.041 Uiso 1 1 calc R . .
H6B H -0.0041 0.6908 0.2486 0.041 Uiso 1 1 calc R . .
H6C H 0.0670 0.8087 0.2676 0.041 Uiso 1 1 calc R . .
C7 C 0.1716(2) 0.64764(14) 0.17355(12) 0.0358(5) Uani 1 1 d . . .
H7A H 0.2388 0.6459 0.2122 0.054 Uiso 1 1 calc R . .
H7B H 0.2038 0.6391 0.1257 0.054 Uiso 1 1 calc R . .
H7C H 0.0843 0.5941 0.1743 0.054 Uiso 1 1 calc R . .
C8 C 0.3834(2) 0.76629(15) 0.08326(10) 0.0312(4) Uani 1 1 d . . .
H8A H 0.4470 0.8066 0.0535 0.047 Uiso 1 1 calc R . .
H8B H 0.2898 0.7471 0.0595 0.047 Uiso 1 1 calc R . .
H8C H 0.4037 0.7068 0.0881 0.047 Uiso 1 1 calc R . .
C9 C 0.6531(2) 0.91088(15) 0.16782(11) 0.0327(4) Uani 1 1 d . . .
H9A H 0.6903 0.8605 0.1779 0.049 Uiso 1 1 calc R . .
H9B H 0.7157 0.9761 0.1925 0.049 Uiso 1 1 calc R . .
H9C H 0.6420 0.9108 0.1148 0.049 Uiso 1 1 calc R . .
C10 C 0.59592(18) 0.98185(13) 0.32705(9) 0.0240(4) Uani 1 1 d . . .
C11 C 0.5284(2) 0.97926(14) 0.39737(9) 0.0283(4) Uani 1 1 d . . .
H11A H 0.4724 1.0203 0.3974 0.042 Uiso 1 1 calc R . .
H11B H 0.5989 1.0048 0.4399 0.042 Uiso 1 1 calc R . .
H11C H 0.4707 0.9110 0.3999 0.042 Uiso 1 1 calc R . .
C12 C 0.6858(2) 0.91968(15) 0.33373(11) 0.0346(5) Uani 1 1 d . . .
H12A H 0.6277 0.8499 0.3302 0.052 Uiso 1 1 calc R . .
H12B H 0.7435 0.9422 0.3812 0.052 Uiso 1 1 calc R . .
H12C H 0.7434 0.9273 0.2941 0.052 Uiso 1 1 calc R . .
C13 C 0.6818(2) 1.08730(13) 0.31856(11) 0.0320(4) Uani 1 1 d . . .
H13A H 0.7288 1.0859 0.2749 0.048 Uiso 1 1 calc R . .
H13B H 0.7492 1.1184 0.3621 0.048 Uiso 1 1 calc R . .
H13C H 0.6225 1.1253 0.3132 0.048 Uiso 1 1 calc R . .
C14 C 0.1912(2) 0.94248(14) 0.39404(10) 0.0293(4) Uani 1 1 d . . .
H14A H 0.2511 0.9891 0.4360 0.044 Uiso 1 1 calc R . .
H14B H 0.1905 0.8759 0.3970 0.044 Uiso 1 1 calc R . .
H14C H 0.0984 0.9424 0.3949 0.044 Uiso 1 1 calc R . .
C15 C 0.1160(2) 0.98184(15) 0.23874(11) 0.0341(5) Uani 1 1 d . . .
H15A H 0.0393 0.9185 0.2325 0.051 Uiso 1 1 calc R . .
H15B H 0.1506 0.9921 0.1915 0.051 Uiso 1 1 calc R . .
H15C H 0.0853 1.0356 0.2564 0.051 Uiso 1 1 calc R . .
C16 C 0.3674(2) 1.11408(13) 0.32332(11) 0.0326(4) Uani 1 1 d . . .
H16A H 0.3118 1.1550 0.3312 0.049 Uiso 1 1 calc R . .
H16B H 0.4155 1.1298 0.2805 0.049 Uiso 1 1 calc R . .
H16C H 0.4339 1.1276 0.3668 0.049 Uiso 1 1 calc R . .
C17 C 0.09513(16) 0.30404(11) 0.12119(8) 0.0146(3) Uani 1 1 d . . .
C18 C -0.01668(16) 0.22924(11) 0.13865(8) 0.0163(3) Uani 1 1 d . . .
C19 C -0.14865(17) 0.22586(12) 0.12858(8) 0.0197(3) Uani 1 1 d . . .
C20 C -0.17549(16) 0.29909(13) 0.09772(8) 0.0196(3) Uani 1 1 d . . .
C21 C -0.06935(17) 0.37393(13) 0.07778(8) 0.0188(3) Uani 1 1 d . . .
C22 C 0.06222(16) 0.37509(12) 0.08971(8) 0.0162(3) Uani 1 1 d . . .
C23 C 0.37420(16) 0.40620(12) 0.13639(8) 0.0163(3) Uani 1 1 d . . .
C24 C 0.39728(17) 0.49153(12) 0.18670(9) 0.0191(3) Uani 1 1 d . . .
C25 C 0.50590(19) 0.57862(13) 0.19025(10) 0.0252(4) Uani 1 1 d . . .
C26 C 0.59930(18) 0.58471(14) 0.14100(11) 0.0287(4) Uani 1 1 d . . .
C27 C 0.58084(18) 0.50395(14) 0.08914(10) 0.0258(4) Uani 1 1 d . . .
C28 C 0.47000(17) 0.41772(13) 0.08743(9) 0.0200(3) Uani 1 1 d . . .
C29 C 0.26731(16) 0.20503(12) 0.09830(8) 0.0151(3) Uani 1 1 d . . .
C30 C 0.18482(17) 0.14458(13) 0.03603(9) 0.0206(3) Uani 1 1 d . . .
C31 C 0.19522(18) 0.05682(13) 0.00517(9) 0.0235(4) Uani 1 1 d . . .
C32 C 0.29164(18) 0.02566(12) 0.03611(9) 0.0230(4) Uani 1 1 d . . .
C33 C 0.37981(17) 0.08455(12) 0.09652(9) 0.0197(3) Uani 1 1 d . . .
C34 C 0.36779(16) 0.17261(12) 0.12499(8) 0.0161(3) Uani 1 1 d . . .
C35 C 0.21791(15) 0.46221(11) 0.38971(8) 0.0137(3) Uani 1 1 d . . .
C36 C 0.34770(16) 0.45910(11) 0.40208(8) 0.0157(3) Uani 1 1 d . . .
C37 C 0.46653(16) 0.54151(13) 0.41440(8) 0.0191(3) Uani 1 1 d . . .
C38 C 0.45906(17) 0.63352(12) 0.41529(9) 0.0219(4) Uani 1 1 d . . .
C39 C 0.33321(17) 0.64117(12) 0.40340(9) 0.0201(3) Uani 1 1 d . . .
C40 C 0.21666(16) 0.55710(12) 0.39134(8) 0.0158(3) Uani 1 1 d . . .
C41 C -0.06176(16) 0.36550(11) 0.35592(8) 0.0149(3) Uani 1 1 d . . .
C42 C -0.08300(16) 0.40341(12) 0.29281(8) 0.0169(3) Uani 1 1 d . . .
C43 C -0.20239(18) 0.41519(12) 0.26958(9) 0.0201(3) Uani 1 1 d . . .
C44 C -0.31053(16) 0.38753(12) 0.30968(9) 0.0203(3) Uani 1 1 d . . .
C45 C -0.29635(16) 0.34805(12) 0.37206(9) 0.0191(3) Uani 1 1 d . . .
C46 C -0.17450(16) 0.33740(11) 0.39359(8) 0.0162(3) Uani 1 1 d . . .
C47 C 0.09273(15) 0.30666(11) 0.45192(8) 0.0132(3) Uani 1 1 d . . .
C48 C 0.10961(15) 0.36366(11) 0.52047(8) 0.0145(3) Uani 1 1 d . . .
C49 C 0.12685(16) 0.33201(11) 0.58619(8) 0.0153(3) Uani 1 1 d . . .
C50 C 0.12717(16) 0.23810(12) 0.58562(8) 0.0167(3) Uani 1 1 d . . .
C51 C 0.10917(17) 0.17778(12) 0.51962(9) 0.0184(3) Uani 1 1 d . . .
C52 C 0.09145(16) 0.21232(12) 0.45482(8) 0.0165(3) 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
Si C16 1.866(2) . ?
Si C14 1.8674(18) . ?
Si C15 1.872(2) . ?
Si C1 1.9680(17) . ?
B1 C23 1.626(2) . ?
B1 C17 1.631(2) . ?
B1 C29 1.635(2) . ?
B1 N3 1.655(2) . ?
B2 N5 1.619(2) . ?
B2 C41 1.631(2) . ?
B2 C47 1.633(2) . ?
B2 C35 1.639(2) . ?
N1 C1 1.373(2) . ?
N1 C2 1.392(2) . ?
N1 C4 1.528(2) . ?
N2 C1 1.370(2) . ?
N2 C3 1.389(2) . ?
N2 C10 1.527(2) . ?
N3 N4 1.1753(17) . ?
N4 N5 1.1695(17) . ?
F1 C18 1.3575(18) . ?
F2 C19 1.3434(19) . ?
F3 C20 1.3430(18) . ?
F4 C21 1.3411(18) . ?
F5 C22 1.3506(18) . ?
F6 C24 1.3512(18) . ?
F7 C25 1.350(2) . ?
F8 C26 1.346(2) . ?
F9 C27 1.3420(19) . ?
F10 C28 1.3522(19) . ?
F11 C30 1.3487(19) . ?
F12 C31 1.3440(19) . ?
F13 C32 1.3449(19) . ?
F14 C33 1.3439(19) . ?
F15 C34 1.3482(18) . ?
F16 C36 1.3532(18) . ?
F17 C37 1.3480(18) . ?
F18 C38 1.3424(19) . ?
F19 C39 1.3483(19) . ?
F20 C40 1.3483(18) . ?
F21 C42 1.3548(18) . ?
F22 C43 1.3489(19) . ?
F23 C44 1.3394(18) . ?
F24 C45 1.3452(18) . ?
F25 C46 1.3521(18) . ?
F26 C48 1.3502(17) . ?
F27 C49 1.3412(17) . ?
F28 C50 1.3456(17) . ?
F29 C51 1.3450(18) . ?
F30 C52 1.3575(17) . ?
C2 C3 1.351(3) . ?
C2 C8 1.500(2) . ?
C3 C9 1.497(2) . ?
C4 C6 1.526(2) . ?
C4 C5 1.528(2) . ?
C4 C7 1.535(2) . ?
C10 C13 1.525(2) . ?
C10 C11 1.527(2) . ?
C10 C12 1.537(3) . ?
C17 C22 1.385(2) . ?
C17 C18 1.390(2) . ?
C18 C19 1.375(2) . ?
C19 C20 1.378(2) . ?
C20 C21 1.375(2) . ?
C21 C22 1.385(2) . ?
C23 C28 1.388(2) . ?
C23 C24 1.395(2) . ?
C24 C25 1.373(2) . ?
C25 C26 1.379(3) . ?
C26 C27 1.372(3) . ?
C27 C28 1.382(2) . ?
C29 C30 1.388(2) . ?
C29 C34 1.390(2) . ?
C30 C31 1.382(2) . ?
C31 C32 1.371(3) . ?
C32 C33 1.380(2) . ?
C33 C34 1.381(2) . ?
C35 C40 1.390(2) . ?
C35 C36 1.391(2) . ?
C36 C37 1.381(2) . ?
C37 C38 1.374(2) . ?
C38 C39 1.377(2) . ?
C39 C40 1.380(2) . ?
C41 C46 1.386(2) . ?
C41 C42 1.392(2) . ?
C42 C43 1.377(2) . ?
C43 C44 1.376(2) . ?
C44 C45 1.376(2) . ?
C45 C46 1.386(2) . ?
C47 C52 1.384(2) . ?
C47 C48 1.391(2) . ?
C48 C49 1.378(2) . ?
C49 C50 1.374(2) . ?
C50 C51 1.373(2) . ?
C51 C52 1.385(2) . ?

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
C16 Si C14 110.25(9) . . ?
C16 Si C15 100.62(9) . . ?
C14 Si C15 112.28(9) . . ?
C16 Si C1 110.37(8) . . ?
C14 Si C1 113.33(8) . . ?
C15 Si C1 109.28(8) . . ?
C23 B1 C17 116.56(13) . . ?
C23 B1 C29 113.82(13) . . ?
C17 B1 C29 112.70(13) . . ?
C23 B1 N3 104.20(12) . . ?
C17 B1 N3 104.99(12) . . ?
C29 B1 N3 102.68(12) . . ?
N5 B2 C41 103.77(12) . . ?
N5 B2 C47 106.53(12) . . ?
C41 B2 C47 114.24(13) . . ?
N5 B2 C35 107.38(12) . . ?
C41 B2 C35 116.01(13) . . ?
C47 B2 C35 108.19(12) . . ?
C1 N1 C2 108.92(14) . . ?
C1 N1 C4 126.48(13) . . ?
C2 N1 C4 122.76(13) . . ?
C1 N2 C3 109.19(14) . . ?
C1 N2 C10 126.14(13) . . ?
C3 N2 C10 122.70(14) . . ?
N4 N3 B1 127.58(13) . . ?
N5 N4 N3 172.23(15) . . ?
N4 N5 B2 134.01(14) . . ?
N2 C1 N1 106.23(13) . . ?
N2 C1 Si 123.74(12) . . ?
N1 C1 Si 123.78(12) . . ?
C3 C2 N1 107.66(14) . . ?
C3 C2 C8 124.81(16) . . ?
N1 C2 C8 127.47(16) . . ?
C2 C3 N2 107.60(15) . . ?
C2 C3 C9 124.43(16) . . ?
N2 C3 C9 127.85(16) . . ?
C6 C4 N1 110.61(13) . . ?
C6 C4 C5 111.34(15) . . ?
N1 C4 C5 110.77(14) . . ?
C6 C4 C7 105.24(15) . . ?
N1 C4 C7 107.43(14) . . ?
C5 C4 C7 111.26(15) . . ?
C13 C10 N2 110.96(14) . . ?
C13 C10 C11 111.62(15) . . ?
N2 C10 C11 110.32(14) . . ?
C13 C10 C12 110.66(16) . . ?
N2 C10 C12 107.54(14) . . ?
C11 C10 C12 105.54(15) . . ?
C22 C17 C18 113.99(14) . . ?
C22 C17 B1 125.87(14) . . ?
C18 C17 B1 120.12(13) . . ?
F1 C18 C19 116.18(14) . . ?
F1 C18 C17 119.57(14) . . ?
C19 C18 C17 124.25(15) . . ?
F2 C19 C18 120.80(15) . . ?
F2 C19 C20 119.87(15) . . ?
C18 C19 C20 119.33(15) . . ?
F3 C20 C21 120.76(15) . . ?
F3 C20 C19 120.15(15) . . ?
C21 C20 C19 119.09(14) . . ?
F4 C21 C20 119.56(14) . . ?
F4 C21 C22 120.76(15) . . ?
C20 C21 C22 119.68(15) . . ?
F5 C22 C21 115.97(14) . . ?
F5 C22 C17 120.39(14) . . ?
C21 C22 C17 123.64(15) . . ?
C28 C23 C24 113.60(15) . . ?
C28 C23 B1 125.39(14) . . ?
C24 C23 B1 120.97(14) . . ?
F6 C24 C25 116.65(15) . . ?
F6 C24 C23 118.97(14) . . ?
C25 C24 C23 124.37(15) . . ?
F7 C25 C24 120.81(16) . . ?
F7 C25 C26 119.97(16) . . ?
C24 C25 C26 119.22(16) . . ?
F8 C26 C27 120.76(17) . . ?
F8 C26 C25 119.99(17) . . ?
C27 C26 C25 119.25(17) . . ?
F9 C27 C26 119.88(17) . . ?
F9 C27 C28 120.45(17) . . ?
C26 C27 C28 119.67(16) . . ?
F10 C28 C27 115.84(14) . . ?
F10 C28 C23 120.30(15) . . ?
C27 C28 C23 123.84(16) . . ?
C30 C29 C34 113.98(14) . . ?
C30 C29 B1 124.50(14) . . ?
C34 C29 B1 121.48(13) . . ?
F11 C30 C31 115.50(14) . . ?
F11 C30 C29 120.84(14) . . ?
C31 C30 C29 123.66(15) . . ?
F12 C31 C32 119.83(15) . . ?
F12 C31 C30 120.31(16) . . ?
C32 C31 C30 119.86(15) . . ?
F13 C32 C31 121.06(15) . . ?
F13 C32 C33 119.91(16) . . ?
C31 C32 C33 119.03(15) . . ?
F14 C33 C32 119.71(14) . . ?
F14 C33 C34 120.90(15) . . ?
C32 C33 C34 119.39(15) . . ?
F15 C34 C33 116.31(14) . . ?
F15 C34 C29 119.78(13) . . ?
C33 C34 C29 123.91(15) . . ?
C40 C35 C36 113.98(14) . . ?
C40 C35 B2 127.36(13) . . ?
C36 C35 B2 118.58(13) . . ?
F16 C36 C37 116.33(14) . . ?
F16 C36 C35 119.45(14) . . ?
C37 C36 C35 124.22(15) . . ?
F17 C37 C38 120.01(15) . . ?
F17 C37 C36 120.73(15) . . ?
C38 C37 C36 119.24(15) . . ?
F18 C38 C37 120.76(15) . . ?
F18 C38 C39 120.12(15) . . ?
C37 C38 C39 119.12(15) . . ?
F19 C39 C38 119.63(15) . . ?
F19 C39 C40 120.40(15) . . ?
C38 C39 C40 119.97(15) . . ?
F20 C40 C39 115.41(14) . . ?
F20 C40 C35 121.12(14) . . ?
C39 C40 C35 123.47(15) . . ?
C46 C41 C42 113.70(14) . . ?
C46 C41 B2 126.37(14) . . ?
C42 C41 B2 119.93(14) . . ?
F21 C42 C43 116.78(14) . . ?
F21 C42 C41 118.79(14) . . ?
C43 C42 C41 124.37(15) . . ?
F22 C43 C44 119.87(14) . . ?
F22 C43 C42 120.49(15) . . ?
C44 C43 C42 119.55(15) . . ?
F23 C44 C43 120.32(15) . . ?
F23 C44 C45 120.91(15) . . ?
C43 C44 C45 118.75(14) . . ?
F24 C45 C44 120.27(14) . . ?
F24 C45 C46 119.78(15) . . ?
C44 C45 C46 119.94(15) . . ?
F25 C46 C45 114.88(14) . . ?
F25 C46 C41 121.44(14) . . ?
C45 C46 C41 123.67(15) . . ?
C52 C47 C48 113.90(14) . . ?
C52 C47 B2 127.88(13) . . ?
C48 C47 B2 118.11(13) . . ?
F26 C48 C49 116.68(13) . . ?
F26 C48 C47 119.00(13) . . ?
C49 C48 C47 124.32(14) . . ?
F27 C49 C50 119.20(13) . . ?
F27 C49 C48 121.61(14) . . ?
C50 C49 C48 119.16(14) . . ?
F28 C50 C51 120.50(14) . . ?
F28 C50 C49 120.25(14) . . ?
C51 C50 C49 119.25(14) . . ?
F29 C51 C50 119.75(14) . . ?
F29 C51 C52 120.50(14) . . ?
C50 C51 C52 119.74(14) . . ?
F30 C52 C47 121.15(14) . . ?
F30 C52 C51 115.24(13) . . ?
C47 C52 C51 123.61(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C23 B1 N3 N4 113.95(17) . . . . ?
C17 B1 N3 N4 -9.1(2) . . . . ?
C29 B1 N3 N4 -127.11(16) . . . . ?
B1 N3 N4 N5 110.9(11) . . . . ?
N3 N4 N5 B2 150.3(10) . . . . ?
C41 B2 N5 N4 119.81(18) . . . . ?
C47 B2 N5 N4 -119.28(18) . . . . ?
C35 B2 N5 N4 -3.6(2) . . . . ?
C3 N2 C1 N1 6.22(17) . . . . ?
C10 N2 C1 N1 -158.04(14) . . . . ?
C3 N2 C1 Si -146.76(12) . . . . ?
C10 N2 C1 Si 49.0(2) . . . . ?
C2 N1 C1 N2 -6.19(17) . . . . ?
C4 N1 C1 N2 158.57(14) . . . . ?
C2 N1 C1 Si 146.77(12) . . . . ?
C4 N1 C1 Si -48.5(2) . . . . ?
C16 Si C1 N2 17.66(16) . . . . ?
C14 Si C1 N2 -106.55(14) . . . . ?
C15 Si C1 N2 127.42(14) . . . . ?
C16 Si C1 N1 -130.68(14) . . . . ?
C14 Si C1 N1 105.11(14) . . . . ?
C15 Si C1 N1 -20.92(16) . . . . ?
C1 N1 C2 C3 3.88(18) . . . . ?
C4 N1 C2 C3 -161.57(14) . . . . ?
C1 N1 C2 C8 -173.48(17) . . . . ?
C4 N1 C2 C8 21.1(3) . . . . ?
N1 C2 C3 N2 0.02(18) . . . . ?
C8 C2 C3 N2 177.47(16) . . . . ?
N1 C2 C3 C9 -176.22(16) . . . . ?
C8 C2 C3 C9 1.2(3) . . . . ?
C1 N2 C3 C2 -3.93(18) . . . . ?
C10 N2 C3 C2 160.98(14) . . . . ?
C1 N2 C3 C9 172.15(17) . . . . ?
C10 N2 C3 C9 -22.9(3) . . . . ?
C1 N1 C4 C6 -6.7(2) . . . . ?
C2 N1 C4 C6 156.10(15) . . . . ?
C1 N1 C4 C5 117.25(17) . . . . ?
C2 N1 C4 C5 -79.95(19) . . . . ?
C1 N1 C4 C7 -121.05(17) . . . . ?
C2 N1 C4 C7 41.8(2) . . . . ?
C1 N2 C10 C13 -116.15(18) . . . . ?
C3 N2 C10 C13 81.57(19) . . . . ?
C1 N2 C10 C11 8.1(2) . . . . ?
C3 N2 C10 C11 -154.20(15) . . . . ?
C1 N2 C10 C12 122.70(17) . . . . ?
C3 N2 C10 C12 -39.6(2) . . . . ?
C23 B1 C17 C22 13.0(2) . . . . ?
C29 B1 C17 C22 -121.33(16) . . . . ?
N3 B1 C17 C22 127.68(15) . . . . ?
C23 B1 C17 C18 -165.45(13) . . . . ?
C29 B1 C17 C18 60.23(18) . . . . ?
N3 B1 C17 C18 -50.76(17) . . . . ?
C22 C17 C18 F1 177.66(13) . . . . ?
B1 C17 C18 F1 -3.7(2) . . . . ?
C22 C17 C18 C19 -2.2(2) . . . . ?
B1 C17 C18 C19 176.46(14) . . . . ?
F1 C18 C19 F2 1.8(2) . . . . ?
C17 C18 C19 F2 -178.39(14) . . . . ?
F1 C18 C19 C20 -178.22(13) . . . . ?
C17 C18 C19 C20 1.6(2) . . . . ?
F2 C19 C20 F3 0.0(2) . . . . ?
C18 C19 C20 F3 -179.95(13) . . . . ?
F2 C19 C20 C21 179.93(14) . . . . ?
C18 C19 C20 C21 -0.1(2) . . . . ?
F3 C20 C21 F4 -0.2(2) . . . . ?
C19 C20 C21 F4 179.89(14) . . . . ?
F3 C20 C21 C22 179.18(14) . . . . ?
C19 C20 C21 C22 -0.7(2) . . . . ?
F4 C21 C22 F5 -0.9(2) . . . . ?
C20 C21 C22 F5 179.69(14) . . . . ?
F4 C21 C22 C17 179.42(14) . . . . ?
C20 C21 C22 C17 0.0(2) . . . . ?
C18 C17 C22 F5 -178.32(13) . . . . ?
B1 C17 C22 F5 3.2(2) . . . . ?
C18 C17 C22 C21 1.3(2) . . . . ?
B1 C17 C22 C21 -177.19(14) . . . . ?
C17 B1 C23 C28 -115.73(17) . . . . ?
C29 B1 C23 C28 18.1(2) . . . . ?
N3 B1 C23 C28 129.13(15) . . . . ?
C17 B1 C23 C24 66.80(19) . . . . ?
C29 B1 C23 C24 -159.38(14) . . . . ?
N3 B1 C23 C24 -48.34(18) . . . . ?
C28 C23 C24 F6 177.14(14) . . . . ?
B1 C23 C24 F6 -5.1(2) . . . . ?
C28 C23 C24 C25 -2.0(2) . . . . ?
B1 C23 C24 C25 175.73(15) . . . . ?
F6 C24 C25 F7 1.0(2) . . . . ?
C23 C24 C25 F7 -179.80(15) . . . . ?
F6 C24 C25 C26 -178.43(15) . . . . ?
C23 C24 C25 C26 0.7(3) . . . . ?
F7 C25 C26 F8 0.7(3) . . . . ?
C24 C25 C26 F8 -179.87(16) . . . . ?
F7 C25 C26 C27 -178.82(16) . . . . ?
C24 C25 C26 C27 0.6(3) . . . . ?
F8 C26 C27 F9 -0.4(3) . . . . ?
C25 C26 C27 F9 179.11(16) . . . . ?
F8 C26 C27 C28 179.93(16) . . . . ?
C25 C26 C27 C28 -0.6(3) . . . . ?
F9 C27 C28 F10 -1.9(2) . . . . ?
C26 C27 C28 F10 177.79(15) . . . . ?
F9 C27 C28 C23 179.43(15) . . . . ?
C26 C27 C28 C23 -0.9(3) . . . . ?
C24 C23 C28 F10 -176.54(14) . . . . ?
B1 C23 C28 F10 5.8(2) . . . . ?
C24 C23 C28 C27 2.1(2) . . . . ?
B1 C23 C28 C27 -175.55(15) . . . . ?
C23 B1 C29 C30 -114.39(17) . . . . ?
C17 B1 C29 C30 21.2(2) . . . . ?
N3 B1 C29 C30 133.65(15) . . . . ?
C23 B1 C29 C34 67.70(18) . . . . ?
C17 B1 C29 C34 -156.70(14) . . . . ?
N3 B1 C29 C34 -44.27(18) . . . . ?
C34 C29 C30 F11 -175.94(14) . . . . ?
B1 C29 C30 F11 6.0(2) . . . . ?
C34 C29 C30 C31 3.6(2) . . . . ?
B1 C29 C30 C31 -174.48(16) . . . . ?
F11 C30 C31 F12 -0.9(2) . . . . ?
C29 C30 C31 F12 179.52(15) . . . . ?
F11 C30 C31 C32 179.22(15) . . . . ?
C29 C30 C31 C32 -0.3(3) . . . . ?
F12 C31 C32 F13 -1.2(3) . . . . ?
C30 C31 C32 F13 178.64(16) . . . . ?
F12 C31 C32 C33 178.12(15) . . . . ?
C30 C31 C32 C33 -2.0(3) . . . . ?
F13 C32 C33 F14 -0.4(2) . . . . ?
C31 C32 C33 F14 -179.69(15) . . . . ?
F13 C32 C33 C34 -179.79(15) . . . . ?
C31 C32 C33 C34 0.9(2) . . . . ?
F14 C33 C34 F15 3.9(2) . . . . ?
C32 C33 C34 F15 -176.67(14) . . . . ?
F14 C33 C34 C29 -176.65(14) . . . . ?
C32 C33 C34 C29 2.8(2) . . . . ?
C30 C29 C34 F15 174.59(14) . . . . ?
B1 C29 C34 F15 -7.3(2) . . . . ?
C30 C29 C34 C33 -4.8(2) . . . . ?
B1 C29 C34 C33 173.31(15) . . . . ?
N5 B2 C35 C40 125.60(15) . . . . ?
C41 B2 C35 C40 10.1(2) . . . . ?
C47 B2 C35 C40 -119.77(16) . . . . ?
N5 B2 C35 C36 -57.90(17) . . . . ?
C41 B2 C35 C36 -173.38(13) . . . . ?
C47 B2 C35 C36 56.73(17) . . . . ?
C40 C35 C36 F16 178.85(13) . . . . ?
B2 C35 C36 F16 1.9(2) . . . . ?
C40 C35 C36 C37 -0.5(2) . . . . ?
B2 C35 C36 C37 -177.49(14) . . . . ?
F16 C36 C37 F17 -0.3(2) . . . . ?
C35 C36 C37 F17 179.08(14) . . . . ?
F16 C36 C37 C38 -178.95(14) . . . . ?
C35 C36 C37 C38 0.5(2) . . . . ?
F17 C37 C38 F18 0.7(2) . . . . ?
C36 C37 C38 F18 179.37(14) . . . . ?
F17 C37 C38 C39 -179.03(14) . . . . ?
C36 C37 C38 C39 -0.4(2) . . . . ?
F18 C38 C39 F19 0.4(2) . . . . ?
C37 C38 C39 F19 -179.85(14) . . . . ?
F18 C38 C39 C40 -179.30(14) . . . . ?
C37 C38 C39 C40 0.5(2) . . . . ?
F19 C39 C40 F20 -1.1(2) . . . . ?
C38 C39 C40 F20 178.54(14) . . . . ?
F19 C39 C40 C35 179.72(14) . . . . ?
C38 C39 C40 C35 -0.6(2) . . . . ?
C36 C35 C40 F20 -178.49(13) . . . . ?
B2 C35 C40 F20 -1.9(2) . . . . ?
C36 C35 C40 C39 0.6(2) . . . . ?
B2 C35 C40 C39 177.24(14) . . . . ?
N5 B2 C41 C46 119.36(15) . . . . ?
C47 B2 C41 C46 3.8(2) . . . . ?
C35 B2 C41 C46 -123.13(16) . . . . ?
N5 B2 C41 C42 -61.12(17) . . . . ?
C47 B2 C41 C42 -176.69(13) . . . . ?
C35 B2 C41 C42 56.39(18) . . . . ?
C46 C41 C42 F21 178.71(13) . . . . ?
B2 C41 C42 F21 -0.9(2) . . . . ?
C46 C41 C42 C43 1.6(2) . . . . ?
B2 C41 C42 C43 -177.97(14) . . . . ?
F21 C42 C43 F22 -1.4(2) . . . . ?
C41 C42 C43 F22 175.73(14) . . . . ?
F21 C42 C43 C44 -177.84(14) . . . . ?
C41 C42 C43 C44 -0.7(2) . . . . ?
F22 C43 C44 F23 1.3(2) . . . . ?
C42 C43 C44 F23 177.75(14) . . . . ?
F22 C43 C44 C45 -176.82(14) . . . . ?
C42 C43 C44 C45 -0.4(2) . . . . ?
F23 C44 C45 F24 1.5(2) . . . . ?
C43 C44 C45 F24 179.62(14) . . . . ?
F23 C44 C45 C46 -177.74(14) . . . . ?
C43 C44 C45 C46 0.4(2) . . . . ?
F24 C45 C46 F25 0.3(2) . . . . ?
C44 C45 C46 F25 179.54(14) . . . . ?
F24 C45 C46 C41 -178.56(14) . . . . ?
C44 C45 C46 C41 0.7(2) . . . . ?
C42 C41 C46 F25 179.61(13) . . . . ?
B2 C41 C46 F25 -0.8(2) . . . . ?
C42 C41 C46 C45 -1.6(2) . . . . ?
B2 C41 C46 C45 177.95(14) . . . . ?
N5 B2 C47 C52 -9.6(2) . . . . ?
C41 B2 C47 C52 104.34(18) . . . . ?
C35 B2 C47 C52 -124.79(16) . . . . ?
N5 B2 C47 C48 166.32(13) . . . . ?
C41 B2 C47 C48 -79.73(17) . . . . ?
C35 B2 C47 C48 51.14(17) . . . . ?
C52 C47 C48 F26 -178.76(13) . . . . ?
B2 C47 C48 F26 4.8(2) . . . . ?
C52 C47 C48 C49 1.4(2) . . . . ?
B2 C47 C48 C49 -175.07(14) . . . . ?
F26 C48 C49 F27 -2.1(2) . . . . ?
C47 C48 C49 F27 177.68(14) . . . . ?
F26 C48 C49 C50 179.85(14) . . . . ?
C47 C48 C49 C50 -0.3(2) . . . . ?
F27 C49 C50 F28 0.7(2) . . . . ?
C48 C49 C50 F28 178.75(14) . . . . ?
F27 C49 C50 C51 -178.59(14) . . . . ?
C48 C49 C50 C51 -0.5(2) . . . . ?
F28 C50 C51 F29 -0.1(2) . . . . ?
C49 C50 C51 F29 179.19(15) . . . . ?
F28 C50 C51 C52 -179.08(14) . . . . ?
C49 C50 C51 C52 0.2(2) . . . . ?
C48 C47 C52 F30 178.56(14) . . . . ?
B2 C47 C52 F30 -5.4(2) . . . . ?
C48 C47 C52 C51 -1.8(2) . . . . ?
B2 C47 C52 C51 174.31(15) . . . . ?
F29 C51 C52 F30 1.8(2) . . . . ?
C50 C51 C52 F30 -179.27(14) . . . . ?
F29 C51 C52 C47 -177.94(15) . . . . ?
C50 C51 C52 C47 1.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.051
_refine_instructions_details     
;
TITL eileen24 in P-1
CELL  0.71073  10.5595  14.6325  18.5185   97.231   94.146  110.557
ZERR     2.00   0.0006   0.0008   0.0010    0.004    0.004    0.006
LATT   1
SFAC  C    H    B    N    F    SI
UNIT  104  66   4    10   60   2
SIZE  0.23 0.20 0.18
TEMP  -173
SHEL  999 0.77
ACTA
CONF
 
FMAP   2
PLAN   10
L.S.   8
 
MPLA 5 c1 n2 c2 c3 n2 Si C4 C10
 
WGHT    0.031300    1.447000
FVAR       4.42029
SI    6    0.254961    0.980705    0.306955    11.00000    0.03075    0.02102 =
         0.01923    0.00374    0.00753    0.01390
B1    3    0.248466    0.304002    0.139831    11.00000    0.01883    0.01897 =
         0.01024    0.00360    0.00318    0.01077
B2    3    0.086036    0.358428    0.379313    11.00000    0.01363    0.01467 =
         0.01181   -0.00041    0.00233    0.00714
N1    4    0.294532    0.828532    0.199313    11.00000    0.02410    0.01959 =
         0.01496    0.00304    0.00350    0.01049
N2    4    0.488499    0.931321    0.260507    11.00000    0.02341    0.01594 =
         0.01908    0.00429    0.00257    0.00853
N3    4    0.260891    0.290603    0.227159    11.00000    0.01600    0.01705 =
         0.01333    0.00208    0.00370    0.00839
N4    4    0.183837    0.293651    0.269294    11.00000    0.01504    0.01206 =
         0.01239    0.00140   -0.00177    0.00598
N5    4    0.103847    0.285189    0.310923    11.00000    0.01671    0.01683 =
         0.01414    0.00092    0.00345    0.00710
F1    5    0.001824    0.153304    0.167410    11.00000    0.02434    0.01489 =
         0.02086    0.00343    0.00135    0.00473
F2    5   -0.251102    0.152261    0.148442    11.00000    0.01768    0.03042 =
         0.03063    0.00712    0.00460   -0.00119
F3    5   -0.303743    0.297029    0.087525    11.00000    0.01483    0.04540 =
         0.02393    0.00332    0.00096    0.01348
F4    5   -0.094409    0.445468    0.047603    11.00000    0.02768    0.04026 =
         0.03011    0.01750    0.00575    0.02233
F5    5    0.160448    0.450800    0.068267    11.00000    0.01865    0.02541 =
         0.02575    0.01380    0.00695    0.00915
F6    5    0.307234    0.490571    0.235132    11.00000    0.02978    0.01906 =
         0.02286    0.00062    0.01088    0.00817
F7    5    0.521322    0.658003    0.240789    11.00000    0.04174    0.01925 =
         0.04255   -0.00344    0.00342    0.00020
F8    5    0.706522    0.669443    0.143807    11.00000    0.02491    0.03138 =
         0.07021    0.01669    0.01065   -0.00327
F9    5    0.669957    0.509268    0.040252    11.00000    0.02831    0.04730 =
         0.05383    0.02714    0.02745    0.01786
F10   5    0.456878    0.342880    0.033037    11.00000    0.03427    0.03068 =
         0.02501    0.00712    0.01650    0.01665
F11   5    0.088116    0.169569    0.001197    11.00000    0.03365    0.04638 =
         0.01793   -0.00633   -0.00722    0.02610
F12   5    0.111040    0.001752   -0.054933    11.00000    0.02977    0.04071 =
         0.02684   -0.01833   -0.00457    0.01138
F13   5    0.302113   -0.060387    0.008057    11.00000    0.03710    0.02045 =
         0.04576   -0.00943    0.00602    0.01298
F14   5    0.475248    0.055211    0.127232    11.00000    0.02636    0.02408 =
         0.04089    0.00433    0.00118    0.01643
F15   5    0.461541    0.228941    0.181599    11.00000    0.01789    0.02336 =
         0.01973   -0.00177   -0.00170    0.00913
F16   5    0.361898    0.370870    0.403084    11.00000    0.01652    0.01969 =
         0.02481    0.00329    0.00263    0.00980
F17   5    0.588652    0.532571    0.426985    11.00000    0.01093    0.03122 =
         0.03147    0.00372   -0.00061    0.00602
F18   5    0.572506    0.715200    0.427794    11.00000    0.01796    0.02373 =
         0.04817    0.00730    0.00065   -0.00383
F19   5    0.324672    0.731051    0.403974    11.00000    0.02808    0.01417 =
         0.04482    0.00741    0.00137    0.00513
F20   5    0.098429    0.572621    0.381957    11.00000    0.01553    0.01768 =
         0.02854    0.00291    0.00198    0.00797
F21   5    0.021294    0.435085    0.252398    11.00000    0.02259    0.02697 =
         0.01586    0.00604    0.00483    0.01082
F22   5   -0.211399    0.458429    0.210232    11.00000    0.03614    0.03506 =
         0.01861    0.00303   -0.00389    0.02195
F23   5   -0.425750    0.401544    0.289242    11.00000    0.01988    0.03651 =
         0.03142   -0.00610   -0.00849    0.01804
F24   5   -0.399807    0.320765    0.412765    11.00000    0.01327    0.03154 =
         0.03534    0.00215    0.00644    0.00767
F25   5   -0.171706    0.298517    0.455902    11.00000    0.01621    0.02741 =
         0.02240    0.00851    0.00584    0.00796
F26   5    0.109821    0.456468    0.524233    11.00000    0.03192    0.01352 =
         0.01815    0.00151    0.00793    0.01061
F27   5    0.147337    0.391591    0.650617    11.00000    0.03162    0.02016 =
         0.01307   -0.00250    0.00319    0.00922
F28   5    0.146393    0.206156    0.649070    11.00000    0.03576    0.02925 =
         0.01605    0.00736    0.00336    0.01936
F29   5    0.110963    0.086147    0.518394    11.00000    0.05669    0.02031 =
         0.02346    0.00482    0.00600    0.02447
F30   5    0.072898    0.146756    0.392615    11.00000    0.04926    0.01771 =
         0.01558   -0.00248    0.00244    0.01629
C1    1    0.350028    0.899219    0.260623    11.00000    0.02560    0.01673 =
         0.01609    0.00498    0.00247    0.00965
C2    1    0.398112    0.825044    0.157892    11.00000    0.03024    0.02308 =
         0.01904    0.00481    0.00639    0.01608
C3    1    0.517522    0.888402    0.195635    11.00000    0.02872    0.01928 =
         0.02225    0.00629    0.00793    0.01310
C4    1    0.152707    0.747515    0.186756    11.00000    0.02329    0.02220 =
         0.02268    0.00031    0.00105    0.00674
C5    1    0.066119    0.759961    0.121647    11.00000    0.02898    0.04598 =
         0.02265    0.00170   -0.00255    0.01211
AFIX 137
H5A   2   -0.022179    0.705049    0.112606    11.00000   -1.50000
H5B   2    0.113267    0.760190    0.077952    11.00000   -1.50000
H5C   2    0.051745    0.822623    0.132634    11.00000   -1.50000
AFIX   0
C6    1    0.083157    0.746737    0.256234    11.00000    0.02796    0.02657 =
         0.02509    0.00573    0.00475    0.00697
AFIX 137
H6A   2    0.141866    0.740213    0.297188    11.00000   -1.50000
H6B   2   -0.004060    0.690823    0.248560    11.00000   -1.50000
H6C   2    0.067006    0.808676    0.267568    11.00000   -1.50000
AFIX   0
C7    1    0.171601    0.647641    0.173551    11.00000    0.03987    0.02201 =
         0.04250   -0.00058    0.00837    0.00889
AFIX 137
H7A   2    0.238777    0.645946    0.212239    11.00000   -1.50000
H7B   2    0.203759    0.639120    0.125734    11.00000   -1.50000
H7C   2    0.084328    0.594105    0.174252    11.00000   -1.50000
AFIX   0
C8    1    0.383391    0.766291    0.083261    11.00000    0.03694    0.03469 =
         0.02410   -0.00158    0.00641    0.01745
AFIX 137
H8A   2    0.447027    0.806570    0.053478    11.00000   -1.50000
H8B   2    0.289827    0.747141    0.059462    11.00000   -1.50000
H8C   2    0.403699    0.706771    0.088077    11.00000   -1.50000
AFIX   0
C9    1    0.653084    0.910880    0.167816    11.00000    0.03007    0.03263 =
         0.03849    0.00627    0.01403    0.01296
AFIX 137
H9A   2    0.690308    0.860495    0.177891    11.00000   -1.50000
H9B   2    0.715730    0.976076    0.192544    11.00000   -1.50000
H9C   2    0.641951    0.910784    0.114805    11.00000   -1.50000
AFIX   0
C10   1    0.595919    0.981849    0.327047    11.00000    0.02617    0.01934 =
         0.02369    0.00332   -0.00370    0.00613
C11   1    0.528432    0.979255    0.397366    11.00000    0.03511    0.02292 =
         0.02114    0.00388   -0.00331    0.00472
AFIX 137
H11A  2    0.472426    1.020322    0.397390    11.00000   -1.50000
H11B  2    0.598879    1.004812    0.439940    11.00000   -1.50000
H11C  2    0.470690    0.910968    0.399889    11.00000   -1.50000
AFIX   0
C12   1    0.685776    0.919676    0.333731    11.00000    0.03647    0.03409 =
         0.03661    0.00733   -0.00418    0.01797
AFIX 137
H12A  2    0.627725    0.849902    0.330228    11.00000   -1.50000
H12B  2    0.743489    0.942190    0.381169    11.00000   -1.50000
H12C  2    0.743426    0.927280    0.294058    11.00000   -1.50000
AFIX   0
C13   1    0.681783    1.087301    0.318560    11.00000    0.03490    0.02077 =
         0.03444    0.00451    0.00217    0.00338
AFIX 137
H13A  2    0.728762    1.085914    0.274924    11.00000   -1.50000
H13B  2    0.749220    1.118399    0.362065    11.00000   -1.50000
H13C  2    0.622530    1.125337    0.313240    11.00000   -1.50000
AFIX   0
C14   1    0.191160    0.942482    0.394042    11.00000    0.03942    0.02598 =
         0.02261    0.00118    0.01093    0.01174
AFIX 137
H14A  2    0.251066    0.989082    0.435955    11.00000   -1.50000
H14B  2    0.190498    0.875911    0.396965    11.00000   -1.50000
H14C  2    0.098432    0.942393    0.394908    11.00000   -1.50000
AFIX   0
C15   1    0.115996    0.981840    0.238738    11.00000    0.04088    0.03719 =
         0.03451    0.00840    0.00752    0.02545
AFIX 137
H15A  2    0.039349    0.918487    0.232521    11.00000   -1.50000
H15B  2    0.150600    0.992052    0.191543    11.00000   -1.50000
H15C  2    0.085283    1.035575    0.256436    11.00000   -1.50000
AFIX   0
C16   1    0.367399    1.114082    0.323319    11.00000    0.04361    0.02128 =
         0.03815    0.00751    0.00926    0.01643
AFIX 137
H16A  2    0.311847    1.154969    0.331247    11.00000   -1.50000
H16B  2    0.415503    1.129753    0.280537    11.00000   -1.50000
H16C  2    0.433897    1.127570    0.366768    11.00000   -1.50000
AFIX   0
C17   1    0.095126    0.304043    0.121195    11.00000    0.01727    0.01761 =
         0.01011    0.00028    0.00239    0.00829
C18   1   -0.016684    0.229238    0.138646    11.00000    0.02079    0.01498 =
         0.01225    0.00026    0.00048    0.00626
C19   1   -0.148650    0.225860    0.128576    11.00000    0.01583    0.02232 =
         0.01500   -0.00033    0.00230    0.00067
C20   1   -0.175493    0.299086    0.097722    11.00000    0.01241    0.03209 =
         0.01451   -0.00137    0.00013    0.01024
C21   1   -0.069353    0.373927    0.077785    11.00000    0.02120    0.02669 =
         0.01378    0.00586    0.00276    0.01404
C22   1    0.062220    0.375095    0.089713    11.00000    0.01675    0.01947 =
         0.01230    0.00291    0.00351    0.00606
C23   1    0.374203    0.406200    0.136394    11.00000    0.01531    0.01930 =
         0.01625    0.00552    0.00058    0.00825
C24   1    0.397279    0.491533    0.186699    11.00000    0.01937    0.02184 =
         0.01810    0.00585    0.00394    0.00895
C25   1    0.505904    0.578616    0.190249    11.00000    0.02566    0.01961 =
         0.02813    0.00359   -0.00006    0.00628
C26   1    0.599303    0.584707    0.141004    11.00000    0.01595    0.02490 =
         0.04354    0.01490    0.00244    0.00246
C27   1    0.580835    0.503949    0.089143    11.00000    0.01777    0.03560 =
         0.03238    0.01848    0.01138    0.01381
C28   1    0.469997    0.417720    0.087427    11.00000    0.02092    0.02398 =
         0.02139    0.00870    0.00575    0.01340
C29   1    0.267308    0.205029    0.098295    11.00000    0.01649    0.01713 =
         0.01237    0.00248    0.00476    0.00638
C30   1    0.184818    0.144579    0.036030    11.00000    0.01904    0.02978 =
         0.01591    0.00107    0.00250    0.01323
C31   1    0.195220    0.056821    0.005166    11.00000    0.02028    0.02569 =
         0.01811   -0.00668    0.00151    0.00405
C32   1    0.291640    0.025662    0.036109    11.00000    0.02345    0.01656 =
         0.02785   -0.00298    0.00821    0.00731
C33   1    0.379807    0.084554    0.096519    11.00000    0.01772    0.01852 =
         0.02556    0.00468    0.00551    0.00889
C34   1    0.367793    0.172607    0.124994    11.00000    0.01521    0.01679 =
         0.01496    0.00112    0.00385    0.00433
C35   1    0.217912    0.462212    0.389705    11.00000    0.01293    0.01715 =
         0.01037    0.00201    0.00278    0.00461
C36   1    0.347700    0.459101    0.402075    11.00000    0.01759    0.01683 =
         0.01367    0.00255    0.00274    0.00739
C37   1    0.466527    0.541505    0.414403    11.00000    0.01309    0.02641 =
         0.01673    0.00347    0.00060    0.00601
C38   1    0.459059    0.633517    0.415285    11.00000    0.01495    0.01953 =
         0.02409    0.00369    0.00165   -0.00252
C39   1    0.333207    0.641168    0.403400    11.00000    0.02254    0.01515 =
         0.02174    0.00332    0.00345    0.00542
C40   1    0.216658    0.557103    0.391341    11.00000    0.01484    0.01899 =
         0.01407    0.00384    0.00313    0.00626
C41   1   -0.061758    0.365502    0.355916    11.00000    0.01540    0.01227 =
         0.01548   -0.00257   -0.00024    0.00514
C42   1   -0.082997    0.403408    0.292807    11.00000    0.01750    0.01661 =
         0.01531   -0.00203    0.00113    0.00635
C43   1   -0.202391    0.415193    0.269581    11.00000    0.02547    0.01822 =
         0.01654   -0.00261   -0.00547    0.01115
C44   1   -0.310526    0.387529    0.309681    11.00000    0.01464    0.01957 =
         0.02464   -0.00794   -0.00747    0.00952
C45   1   -0.296354    0.348051    0.372061    11.00000    0.01269    0.01741 =
         0.02344   -0.00498    0.00162    0.00394
C46   1   -0.174501    0.337402    0.393590    11.00000    0.01555    0.01451 =
         0.01662   -0.00059    0.00063    0.00457
C47   1    0.092727    0.306658    0.451921    11.00000    0.00903    0.01531 =
         0.01515    0.00144    0.00246    0.00437
C48   1    0.109613    0.363660    0.520467    11.00000    0.01209    0.01218 =
         0.01866    0.00128    0.00343    0.00389
C49   1    0.126849    0.332011    0.586186    11.00000    0.01354    0.01693 =
         0.01340   -0.00169    0.00285    0.00436
C50   1    0.127168    0.238099    0.585618    11.00000    0.01557    0.02238 =
         0.01440    0.00531    0.00284    0.00873
C51   1    0.109166    0.177780    0.519616    11.00000    0.02305    0.01376 =
         0.02142    0.00312    0.00442    0.01008
C52   1    0.091450    0.212321    0.454821    11.00000    0.01819    0.01703 =
         0.01353   -0.00325    0.00177    0.00742
HKLF    4
;
####################################################################### 
# 
# 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_eileen61
_database_code_depnum_ccdc_archive 'CCDC 1052445'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H33 F3 N2 O5 S Si'
_chemical_formula_weight         474.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

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

_cell_length_a                   10.6572(3)
_cell_length_b                   10.9091(3)
_cell_length_c                   20.6522(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2401.03(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23067
_cell_measurement_theta_min      4.2770
_cell_measurement_theta_max      76.6820

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    2.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.24052
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36236
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.28
_diffrn_reflns_theta_max         77.03
_reflns_number_total             5022
_reflns_number_gt                4932
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44)  
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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. 

 The compound is not chiral but crystallises by chance in a Soehnke space
 group.
;

_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)+(0.0312P)²+0.5163P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.002(11)
_chemical_absolute_configuration .
_refine_ls_number_reflns         5022
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0598
_refine_ls_wR_factor_gt          0.0595
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
S1 S 0.68678(3) 0.49675(3) 0.003084(14) 0.01740(7) Uani 1 1 d . . .
Si Si 0.49215(3) 0.45904(3) 0.331671(17) 0.01685(8) Uani 1 1 d . . .
N1 N 0.19109(10) 0.39521(9) 0.15372(5) 0.0138(2) Uani 1 1 d . . .
N2 N 0.06779(10) 0.39799(10) 0.23977(5) 0.0142(2) Uani 1 1 d . . .
O1 O 0.36766(8) 0.40845(9) 0.28417(4) 0.01544(18) Uani 1 1 d . . .
O2 O 0.28602(9) 0.59270(9) 0.25921(5) 0.01900(19) Uani 1 1 d . . .
O3 O 0.75998(10) 0.49263(10) -0.05554(5) 0.0268(2) Uani 1 1 d . . .
O4 O 0.69969(10) 0.39182(9) 0.04485(5) 0.0244(2) Uani 1 1 d . . .
O5 O 0.56065(10) 0.54023(12) -0.00502(5) 0.0335(2) Uani 1 1 d . . .
F1 F 0.88327(10) 0.59318(11) 0.06025(6) 0.0497(3) Uani 1 1 d . . .
F2 F 0.75648(14) 0.72567(9) 0.01959(6) 0.0538(3) Uani 1 1 d . . .
F3 F 0.70821(12) 0.63216(10) 0.10773(5) 0.0459(3) Uani 1 1 d . . .
C1 C 0.18558(12) 0.41784(11) 0.21795(6) 0.0138(2) Uani 1 1 d . . .
C2 C 0.07028(12) 0.36120(12) 0.13382(6) 0.0158(2) Uani 1 1 d . . .
C3 C -0.00582(12) 0.36432(11) 0.18643(6) 0.0160(2) Uani 1 1 d . . .
C4 C 0.29996(12) 0.42292(11) 0.10732(6) 0.0160(2) Uani 1 1 d . . .
C5 C 0.42422(12) 0.43708(13) 0.14346(6) 0.0202(3) Uani 1 1 d . . .
H5A H 0.4928 0.4452 0.1121 0.030 Uiso 1 1 calc R . .
H5B H 0.4386 0.3647 0.1706 0.030 Uiso 1 1 calc R . .
H5C H 0.4209 0.5104 0.1708 0.030 Uiso 1 1 calc R . .
C6 C 0.26810(13) 0.54293(13) 0.07319(7) 0.0214(3) Uani 1 1 d . . .
H6A H 0.3346 0.5631 0.0422 0.032 Uiso 1 1 calc R . .
H6B H 0.2610 0.6087 0.1053 0.032 Uiso 1 1 calc R . .
H6C H 0.1882 0.5341 0.0501 0.032 Uiso 1 1 calc R . .
C7 C 0.31685(15) 0.31597(14) 0.06023(7) 0.0243(3) Uani 1 1 d . . .
H7A H 0.2467 0.3145 0.0296 0.036 Uiso 1 1 calc R . .
H7B H 0.3189 0.2388 0.0845 0.036 Uiso 1 1 calc R . .
H7C H 0.3958 0.3261 0.0365 0.036 Uiso 1 1 calc R . .
C8 C 0.03169(13) 0.32264(14) 0.06725(6) 0.0220(3) Uani 1 1 d . . .
H8A H 0.0646 0.2405 0.0582 0.033 Uiso 1 1 calc R . .
H8B H 0.0653 0.3807 0.0355 0.033 Uiso 1 1 calc R . .
H8C H -0.0601 0.3214 0.0644 0.033 Uiso 1 1 calc R . .
C9 C -0.14406(12) 0.33881(14) 0.18623(7) 0.0220(3) Uani 1 1 d . . .
H9A H -0.1787 0.3580 0.1435 0.033 Uiso 1 1 calc R . .
H9B H -0.1853 0.3897 0.2190 0.033 Uiso 1 1 calc R . .
H9C H -0.1585 0.2521 0.1960 0.033 Uiso 1 1 calc R . .
C10 C 0.01786(12) 0.41197(13) 0.30895(6) 0.0176(3) Uani 1 1 d . . .
C11 C 0.12333(13) 0.42622(15) 0.35840(6) 0.0235(3) Uani 1 1 d . . .
H11A H 0.0882 0.4236 0.4022 0.035 Uiso 1 1 calc R . .
H11B H 0.1657 0.5049 0.3516 0.035 Uiso 1 1 calc R . .
H11C H 0.1838 0.3593 0.3531 0.035 Uiso 1 1 calc R . .
C12 C -0.06238(15) 0.52803(15) 0.31032(7) 0.0284(3) Uani 1 1 d . . .
H12A H -0.1280 0.5223 0.2772 0.043 Uiso 1 1 calc R . .
H12B H -0.0094 0.5995 0.3016 0.043 Uiso 1 1 calc R . .
H12C H -0.1013 0.5367 0.3531 0.043 Uiso 1 1 calc R . .
C13 C -0.05351(15) 0.29560(15) 0.32755(7) 0.0282(3) Uani 1 1 d . . .
H13A H -0.1281 0.2875 0.3001 0.042 Uiso 1 1 calc R . .
H13B H -0.0791 0.3006 0.3731 0.042 Uiso 1 1 calc R . .
H13C H 0.0009 0.2241 0.3214 0.042 Uiso 1 1 calc R . .
C14 C 0.28684(11) 0.48206(11) 0.25649(6) 0.0138(2) Uani 1 1 d . . .
C15 C 0.58756(13) 0.56835(14) 0.28400(8) 0.0251(3) Uani 1 1 d . . .
H15A H 0.6162 0.5286 0.2441 0.038 Uiso 1 1 calc R . .
H15B H 0.6604 0.5941 0.3096 0.038 Uiso 1 1 calc R . .
H15C H 0.5366 0.6402 0.2731 0.038 Uiso 1 1 calc R . .
C16 C 0.57428(15) 0.31394(14) 0.34846(8) 0.0286(3) Uani 1 1 d . . .
H16A H 0.5175 0.2578 0.3711 0.043 Uiso 1 1 calc R . .
H16B H 0.6478 0.3301 0.3756 0.043 Uiso 1 1 calc R . .
H16C H 0.6012 0.2767 0.3076 0.043 Uiso 1 1 calc R . .
C17 C 0.42728(14) 0.53104(16) 0.40536(7) 0.0286(3) Uani 1 1 d . . .
H17A H 0.3816 0.6057 0.3935 0.043 Uiso 1 1 calc R . .
H17B H 0.4959 0.5519 0.4350 0.043 Uiso 1 1 calc R . .
H17C H 0.3699 0.4737 0.4267 0.043 Uiso 1 1 calc R . .
C18 C 0.76242(16) 0.61853(14) 0.04975(8) 0.0296(3) 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
S1 O5 1.4352(11) . ?
S1 O4 1.4398(10) . ?
S1 O3 1.4410(10) . ?
S1 C18 1.8285(16) . ?
Si O1 1.7399(10) . ?
Si C16 1.8417(16) . ?
Si C17 1.8469(15) . ?
Si C15 1.8507(15) . ?
N1 C1 1.3506(16) . ?
N1 C2 1.4014(16) . ?
N1 C4 1.5349(16) . ?
N2 C1 1.3513(17) . ?
N2 C3 1.4014(16) . ?
N2 C10 1.5321(16) . ?
O1 C14 1.3090(15) . ?
O2 C14 1.2083(16) . ?
F1 C18 1.335(2) . ?
F2 C18 1.3259(19) . ?
F3 C18 1.3378(19) . ?
C1 C14 1.5129(17) . ?
C2 C3 1.3562(18) . ?
C2 C8 1.4955(18) . ?
C3 C9 1.4993(18) . ?
C4 C6 1.5252(18) . ?
C4 C5 1.5279(18) . ?
C4 C7 1.5296(18) . ?
C10 C11 1.5266(18) . ?
C10 C12 1.528(2) . ?
C10 C13 1.529(2) . ?

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
O5 S1 O4 114.96(7) . . ?
O5 S1 O3 114.79(6) . . ?
O4 S1 O3 115.27(6) . . ?
O5 S1 C18 103.55(8) . . ?
O4 S1 C18 102.70(7) . . ?
O3 S1 C18 103.11(7) . . ?
O1 Si C16 101.30(6) . . ?
O1 Si C17 108.30(6) . . ?
C16 Si C17 112.85(8) . . ?
O1 Si C15 108.87(6) . . ?
C16 Si C15 113.13(7) . . ?
C17 Si C15 111.72(8) . . ?
C1 N1 C2 107.25(11) . . ?
C1 N1 C4 127.59(11) . . ?
C2 N1 C4 124.30(10) . . ?
C1 N2 C3 107.45(10) . . ?
C1 N2 C10 128.15(10) . . ?
C3 N2 C10 124.38(10) . . ?
C14 O1 Si 123.60(8) . . ?
N1 C1 N2 109.79(11) . . ?
N1 C1 C14 124.78(11) . . ?
N2 C1 C14 124.15(11) . . ?
C3 C2 N1 107.93(11) . . ?
C3 C2 C8 125.39(12) . . ?
N1 C2 C8 126.64(12) . . ?
C2 C3 N2 107.55(11) . . ?
C2 C3 C9 125.50(12) . . ?
N2 C3 C9 126.93(12) . . ?
C6 C4 C5 109.39(11) . . ?
C6 C4 C7 112.78(11) . . ?
C5 C4 C7 106.60(11) . . ?
C6 C4 N1 106.82(10) . . ?
C5 C4 N1 111.72(10) . . ?
C7 C4 N1 109.61(10) . . ?
C11 C10 C12 108.37(12) . . ?
C11 C10 C13 106.42(11) . . ?
C12 C10 C13 113.89(12) . . ?
C11 C10 N2 112.22(10) . . ?
C12 C10 N2 107.10(10) . . ?
C13 C10 N2 108.93(11) . . ?
O2 C14 O1 126.67(12) . . ?
O2 C14 C1 118.81(11) . . ?
O1 C14 C1 114.52(11) . . ?
F2 C18 F1 107.76(14) . . ?
F2 C18 F3 107.57(13) . . ?
F1 C18 F3 107.11(14) . . ?
F2 C18 S1 111.83(11) . . ?
F1 C18 S1 111.13(11) . . ?
F3 C18 S1 111.22(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 Si O1 C14 -175.07(10) . . . . ?
C17 Si O1 C14 66.04(11) . . . . ?
C15 Si O1 C14 -55.62(11) . . . . ?
C2 N1 C1 N2 0.94(14) . . . . ?
C4 N1 C1 N2 170.57(11) . . . . ?
C2 N1 C1 C14 -166.58(11) . . . . ?
C4 N1 C1 C14 3.05(19) . . . . ?
C3 N2 C1 N1 -1.66(14) . . . . ?
C10 N2 C1 N1 -179.97(11) . . . . ?
C3 N2 C1 C14 165.96(11) . . . . ?
C10 N2 C1 C14 -12.4(2) . . . . ?
C1 N1 C2 C3 0.17(14) . . . . ?
C4 N1 C2 C3 -169.88(11) . . . . ?
C1 N1 C2 C8 -177.34(13) . . . . ?
C4 N1 C2 C8 12.6(2) . . . . ?
N1 C2 C3 N2 -1.16(14) . . . . ?
C8 C2 C3 N2 176.38(13) . . . . ?
N1 C2 C3 C9 177.60(12) . . . . ?
C8 C2 C3 C9 -4.9(2) . . . . ?
C1 N2 C3 C2 1.73(14) . . . . ?
C10 N2 C3 C2 -179.87(11) . . . . ?
C1 N2 C3 C9 -177.00(13) . . . . ?
C10 N2 C3 C9 1.4(2) . . . . ?
C1 N1 C4 C6 -98.40(14) . . . . ?
C2 N1 C4 C6 69.59(14) . . . . ?
C1 N1 C4 C5 21.18(17) . . . . ?
C2 N1 C4 C5 -170.83(11) . . . . ?
C1 N1 C4 C7 139.12(13) . . . . ?
C2 N1 C4 C7 -52.90(16) . . . . ?
C1 N2 C10 C11 -12.47(18) . . . . ?
C3 N2 C10 C11 169.48(12) . . . . ?
C1 N2 C10 C12 106.35(14) . . . . ?
C3 N2 C10 C12 -71.70(15) . . . . ?
C1 N2 C10 C13 -130.05(14) . . . . ?
C3 N2 C10 C13 51.90(16) . . . . ?
Si O1 C14 O2 0.26(18) . . . . ?
Si O1 C14 C1 -179.46(8) . . . . ?
N1 C1 C14 O2 86.31(16) . . . . ?
N2 C1 C14 O2 -79.46(16) . . . . ?
N1 C1 C14 O1 -93.95(14) . . . . ?
N2 C1 C14 O1 100.28(14) . . . . ?
O5 S1 C18 F2 -58.02(14) . . . . ?
O4 S1 C18 F2 -177.97(12) . . . . ?
O3 S1 C18 F2 61.91(14) . . . . ?
O5 S1 C18 F1 -178.49(11) . . . . ?
O4 S1 C18 F1 61.55(13) . . . . ?
O3 S1 C18 F1 -58.56(13) . . . . ?
O5 S1 C18 F3 62.27(13) . . . . ?
O4 S1 C18 F3 -57.68(13) . . . . ?
O3 S1 C18 F3 -177.80(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.038
_refine_instructions_details     
;
TITL eileen61 in P2(1)2(1)2(1)
CELL 1.54184  10.657198  10.909093  20.652223  90.0000  90.0000  90.0000
ZERR    4.00   0.000300   0.000300   0.000600   0.0000   0.0000   0.0000
LATT  -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  - X, 1/2 + Y, 1/2 - Z
SYMM  1/2 + X, 1/2 - Y, - Z
SFAC  C    H    N    O    F    SI   S
UNIT  72  132  8  20  12  4  4
MERG   2
FMAP   2
TEMP -173
 
OMIT 0 7 10
 
ACTA 150
CONF
 
PLAN   10
L.S.   10
WGHT    0.031200    0.516300
FVAR       4.20515
S1    7    0.686785    0.496746    0.003084    11.00000    0.01507    0.02213 =
         0.01500   -0.00014    0.00007   -0.00119
SI    6    0.492153    0.459041    0.331671    11.00000    0.01299    0.02147 =
         0.01610   -0.00412   -0.00281    0.00213
N1    3    0.191088    0.395206    0.153722    11.00000    0.01310    0.01606 =
         0.01219   -0.00047    0.00037   -0.00129
N2    3    0.067788    0.397987    0.239772    11.00000    0.01180    0.01879 =
         0.01198    0.00085   -0.00052   -0.00087
O1    4    0.367658    0.408452    0.284173    11.00000    0.01255    0.01902 =
         0.01474   -0.00038   -0.00168    0.00158
O2    4    0.286020    0.592705    0.259211    11.00000    0.01718    0.01814 =
         0.02167   -0.00252    0.00122    0.00132
O3    4    0.759977    0.492630   -0.055542    11.00000    0.02730    0.03245 =
         0.02051   -0.00222    0.00696   -0.00400
O4    4    0.699688    0.391824    0.044850    11.00000    0.03080    0.02187 =
         0.02062    0.00241   -0.00143   -0.00109
O5    4    0.560652    0.540227   -0.005021    11.00000    0.01897    0.05250 =
         0.02898    0.00667   -0.00223    0.00701
F1    5    0.883265    0.593178    0.060254    11.00000    0.03328    0.05295 =
         0.06278   -0.01320   -0.01457   -0.01407
F2    5    0.756481    0.725675    0.019588    11.00000    0.08928    0.02178 =
         0.05024    0.00391   -0.00073   -0.01062
F3    5    0.708207    0.632156    0.107726    11.00000    0.07015    0.03962 =
         0.02802   -0.01526    0.00619   -0.00403
C1    1    0.185584    0.417840    0.217952    11.00000    0.01156    0.01585 =
         0.01407    0.00123   -0.00031    0.00160
C2    1    0.070283    0.361198    0.133822    11.00000    0.01545    0.01662 =
         0.01539    0.00088   -0.00312   -0.00172
C3    1   -0.005818    0.364324    0.186427    11.00000    0.01430    0.01785 =
         0.01594    0.00194   -0.00264   -0.00150
C4    1    0.299958    0.422922    0.107318    11.00000    0.01556    0.01937 =
         0.01300   -0.00057    0.00433   -0.00173
C5    1    0.424218    0.437079    0.143457    11.00000    0.01403    0.03069 =
         0.01598   -0.00021    0.00311   -0.00016
AFIX 137
H5A   2    0.492808    0.445230    0.112145    11.00000   -1.50000
H5B   2    0.438613    0.364706    0.170569    11.00000   -1.50000
H5C   2    0.420931    0.510382    0.170835    11.00000   -1.50000
AFIX   0
C6    1    0.268097    0.542934    0.073190    11.00000    0.02246    0.02231 =
         0.01955    0.00353    0.00097   -0.00216
AFIX 137
H6A   2    0.334626    0.563102    0.042212    11.00000   -1.50000
H6B   2    0.260963    0.608725    0.105291    11.00000   -1.50000
H6C   2    0.188231    0.534089    0.050139    11.00000   -1.50000
AFIX   0
C7    1    0.316852    0.315969    0.060227    11.00000    0.02398    0.02699 =
         0.02189   -0.00729    0.00690   -0.00287
AFIX 137
H7A   2    0.246704    0.314542    0.029553    11.00000   -1.50000
H7B   2    0.318875    0.238767    0.084467    11.00000   -1.50000
H7C   2    0.395800    0.326074    0.036488    11.00000   -1.50000
AFIX   0
C8    1    0.031686    0.322637    0.067246    11.00000    0.02176    0.03030 =
         0.01402   -0.00290   -0.00370   -0.00397
AFIX 137
H8A   2    0.064579    0.240499    0.058238    11.00000   -1.50000
H8B   2    0.065284    0.380719    0.035468    11.00000   -1.50000
H8C   2   -0.060098    0.321425    0.064407    11.00000   -1.50000
AFIX   0
C9    1   -0.144062    0.338815    0.186227    11.00000    0.01453    0.03054 =
         0.02082    0.00325   -0.00247   -0.00530
AFIX 137
H9A   2   -0.178733    0.357997    0.143461    11.00000   -1.50000
H9B   2   -0.185273    0.389703    0.219044    11.00000   -1.50000
H9C   2   -0.158537    0.252071    0.196047    11.00000   -1.50000
AFIX   0
C10   1    0.017860    0.411967    0.308949    11.00000    0.01390    0.02705 =
         0.01178    0.00117    0.00316   -0.00170
C11   1    0.123328    0.426220    0.358400    11.00000    0.01795    0.03962 =
         0.01282   -0.00008    0.00129   -0.00221
AFIX 137
H11A  2    0.088168    0.423583    0.402225    11.00000   -1.50000
H11B  2    0.165705    0.504914    0.351648    11.00000   -1.50000
H11C  2    0.183815    0.359312    0.353072    11.00000   -1.50000
AFIX   0
C12   1   -0.062383    0.528033    0.310319    11.00000    0.02540    0.03714 =
         0.02278   -0.00271    0.00422    0.00976
AFIX 137
H12A  2   -0.127983    0.522292    0.277205    11.00000   -1.50000
H12B  2   -0.009359    0.599529    0.301556    11.00000   -1.50000
H12C  2   -0.101265    0.536711    0.353076    11.00000   -1.50000
AFIX   0
C13   1   -0.053506    0.295597    0.327551    11.00000    0.02953    0.03619 =
         0.01898    0.00520    0.00249   -0.01284
AFIX 137
H13A  2   -0.128096    0.287480    0.300132    11.00000   -1.50000
H13B  2   -0.079099    0.300580    0.373053    11.00000   -1.50000
H13C  2    0.000932    0.224143    0.321392    11.00000   -1.50000
AFIX   0
C14   1    0.286838    0.482063    0.256494    11.00000    0.01105    0.01914 =
         0.01112   -0.00062    0.00242    0.00080
C15   1    0.587561    0.568346    0.283995    11.00000    0.01626    0.03013 =
         0.02888   -0.00273   -0.00262   -0.00368
AFIX 137
H15A  2    0.616160    0.528603    0.244080    11.00000   -1.50000
H15B  2    0.660426    0.594077    0.309553    11.00000   -1.50000
H15C  2    0.536618    0.640238    0.273107    11.00000   -1.50000
AFIX   0
C16   1    0.574280    0.313945    0.348457    11.00000    0.02448    0.02746 =
         0.03373   -0.00368   -0.01313    0.00477
AFIX 137
H16A  2    0.517467    0.257806    0.371104    11.00000   -1.50000
H16B  2    0.647835    0.330103    0.375626    11.00000   -1.50000
H16C  2    0.601239    0.276716    0.307573    11.00000   -1.50000
AFIX   0
C17   1    0.427278    0.531039    0.405361    11.00000    0.02096    0.04408 =
         0.02089   -0.01129   -0.00387    0.00151
AFIX 137
H17A  2    0.381612    0.605707    0.393496    11.00000   -1.50000
H17B  2    0.495911    0.551925    0.434953    11.00000   -1.50000
H17C  2    0.369886    0.473689    0.426737    11.00000   -1.50000
AFIX   0
C18   1    0.762423    0.618533    0.049745    11.00000    0.03790    0.02363 =
         0.02723   -0.00209   -0.00036   -0.00268
HKLF    4
;
####################################################################### 
# 
# 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_eileen63
_database_code_depnum_ccdc_archive 'CCDC 1052446'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H42 F3 N3 O4 S Si'
_chemical_formula_weight         529.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   18.8522(4)
_cell_length_b                   20.4483(3)
_cell_length_c                   15.2041(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.952(2)
_cell_angle_gamma                90.00
_cell_volume                     5473.57(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    44360
_cell_measurement_theta_min      3.7560
_cell_measurement_theta_max      76.8780

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2272
_exptl_absorpt_coefficient_mu    1.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Difraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            103018
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         77.07
_reflns_number_total             11498
_reflns_number_gt                10409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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. 

 One molecule of triflate is disordered and was refined on two positions.
;

_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)+(0.0487P)²+3.0850P] 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         11498
_refine_ls_number_parameters     674
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.024
_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
Si Si 0.22548(2) 0.378697(18) 0.39160(3) 0.01747(9) Uani 1 1 d . . .
O1 O 0.28002(5) 0.30975(5) 0.42404(6) 0.01507(19) Uani 1 1 d . . .
N1 N 0.42733(6) 0.21521(6) 0.45524(8) 0.0145(2) Uani 1 1 d . . .
N2 N 0.32211(6) 0.15675(5) 0.40194(8) 0.0144(2) Uani 1 1 d . . .
N3 N 0.29631(7) 0.30071(6) 0.28380(8) 0.0157(2) Uani 1 1 d . . .
C1 C 0.35099(7) 0.21795(6) 0.40981(9) 0.0136(2) Uani 1 1 d . . .
C2 C 0.44740(8) 0.14949(7) 0.47337(10) 0.0176(3) Uani 1 1 d . . .
C3 C 0.38255(8) 0.11354(7) 0.44054(10) 0.0179(3) Uani 1 1 d . . .
C4 C 0.48453(8) 0.27099(7) 0.48791(10) 0.0183(3) Uani 1 1 d . . .
C5 C 0.53967(9) 0.26634(9) 0.43460(12) 0.0284(3) Uani 1 1 d . . .
H5A H 0.5599 0.2218 0.4397 0.043 Uiso 1 1 calc R . .
H5B H 0.5816 0.2972 0.4619 0.043 Uiso 1 1 calc R . .
H5C H 0.5128 0.2771 0.3681 0.043 Uiso 1 1 calc R . .
C6 C 0.52410(9) 0.26480(8) 0.59514(10) 0.0245(3) Uani 1 1 d . . .
H6A H 0.4860 0.2663 0.6252 0.037 Uiso 1 1 calc R . .
H6B H 0.5600 0.3010 0.6186 0.037 Uiso 1 1 calc R . .
H6C H 0.5515 0.2232 0.6101 0.037 Uiso 1 1 calc R . .
C7 C 0.44788(9) 0.33858(7) 0.47019(12) 0.0272(3) Uani 1 1 d . . .
H7A H 0.4221 0.3452 0.4023 0.041 Uiso 1 1 calc R . .
H7B H 0.4871 0.3721 0.4951 0.041 Uiso 1 1 calc R . .
H7C H 0.4109 0.3419 0.5017 0.041 Uiso 1 1 calc R . .
C8 C 0.52481(9) 0.11993(8) 0.51905(11) 0.0247(3) Uani 1 1 d . . .
H8A H 0.5287 0.1003 0.5794 0.037 Uiso 1 1 calc R . .
H8B H 0.5635 0.1540 0.5297 0.037 Uiso 1 1 calc R . .
H8C H 0.5327 0.0861 0.4778 0.037 Uiso 1 1 calc R . .
C9 C 0.38083(10) 0.04047(7) 0.44748(12) 0.0263(3) Uani 1 1 d . . .
H9A H 0.4208 0.0216 0.4281 0.039 Uiso 1 1 calc R . .
H9B H 0.3312 0.0242 0.4062 0.039 Uiso 1 1 calc R . .
H9C H 0.3894 0.0279 0.5127 0.039 Uiso 1 1 calc R . .
C10 C 0.23930(8) 0.13420(7) 0.36153(10) 0.0165(3) Uani 1 1 d . . .
C11 C 0.22263(9) 0.09628(8) 0.43908(11) 0.0260(3) Uani 1 1 d . . .
H11A H 0.2352 0.1236 0.4956 0.039 Uiso 1 1 calc R . .
H11B H 0.2534 0.0563 0.4541 0.039 Uiso 1 1 calc R . .
H11C H 0.1686 0.0847 0.4171 0.039 Uiso 1 1 calc R . .
C12 C 0.22807(9) 0.09222(8) 0.27422(11) 0.0254(3) Uani 1 1 d . . .
H12A H 0.1813 0.0666 0.2594 0.038 Uiso 1 1 calc R . .
H12B H 0.2714 0.0626 0.2866 0.038 Uiso 1 1 calc R . .
H12C H 0.2243 0.1206 0.2208 0.038 Uiso 1 1 calc R . .
C13 C 0.18329(8) 0.19068(7) 0.33340(11) 0.0205(3) Uani 1 1 d . . .
H13A H 0.1900 0.2183 0.3885 0.031 Uiso 1 1 calc R . .
H13B H 0.1313 0.1735 0.3092 0.031 Uiso 1 1 calc R . .
H13C H 0.1924 0.2167 0.2844 0.031 Uiso 1 1 calc R . .
C14 C 0.30766(7) 0.27829(6) 0.36457(9) 0.0142(3) Uani 1 1 d . . .
C15 C 0.31843(8) 0.27613(7) 0.20499(9) 0.0143(3) Uani 1 1 d . . .
C16 C 0.36311(9) 0.21161(8) 0.22021(10) 0.0231(3) Uani 1 1 d . . .
H16A H 0.4119 0.2169 0.2720 0.035 Uiso 1 1 calc R . .
H16B H 0.3721 0.2000 0.1625 0.035 Uiso 1 1 calc R . .
H16C H 0.3338 0.1768 0.2358 0.035 Uiso 1 1 calc R . .
C17 C 0.36289(9) 0.33113(8) 0.18149(11) 0.0258(3) Uani 1 1 d . . .
H17A H 0.3342 0.3720 0.1736 0.039 Uiso 1 1 calc R . .
H17B H 0.3711 0.3208 0.1229 0.039 Uiso 1 1 calc R . .
H17C H 0.4121 0.3361 0.2328 0.039 Uiso 1 1 calc R . .
C18 C 0.24158(9) 0.26701(8) 0.12310(10) 0.0240(3) Uani 1 1 d . . .
H18A H 0.2126 0.2322 0.1390 0.036 Uiso 1 1 calc R . .
H18B H 0.2508 0.2552 0.0657 0.036 Uiso 1 1 calc R . .
H18C H 0.2127 0.3079 0.1127 0.036 Uiso 1 1 calc R . .
C19 C 0.27706(10) 0.44566(8) 0.35936(12) 0.0295(4) Uani 1 1 d . . .
H19A H 0.3260 0.4526 0.4104 0.044 Uiso 1 1 calc R . .
H19B H 0.2469 0.4859 0.3491 0.044 Uiso 1 1 calc R . .
H19C H 0.2858 0.4341 0.3015 0.044 Uiso 1 1 calc R . .
C20 C 0.20988(9) 0.39920(7) 0.50180(10) 0.0230(3) Uani 1 1 d . . .
H20A H 0.1823 0.3634 0.5183 0.034 Uiso 1 1 calc R . .
H20B H 0.1800 0.4395 0.4928 0.034 Uiso 1 1 calc R . .
H20C H 0.2590 0.4055 0.5527 0.034 Uiso 1 1 calc R . .
C21 C 0.13546(9) 0.35939(8) 0.29441(11) 0.0269(3) Uani 1 1 d . . .
H21A H 0.1466 0.3424 0.2405 0.040 Uiso 1 1 calc R . .
H21B H 0.1047 0.3992 0.2757 0.040 Uiso 1 1 calc R . .
H21C H 0.1074 0.3264 0.3156 0.040 Uiso 1 1 calc R . .
S S 0.47557(11) 0.45396(10) 0.74769(13) 0.0262(4) Uani 0.871(3) 1 d PDU A 1
O2 O 0.50951(11) 0.39235(9) 0.7393(2) 0.0369(5) Uani 0.871(3) 1 d PDU A 1
O3 O 0.51340(14) 0.48951(9) 0.83257(11) 0.0481(5) Uani 0.871(3) 1 d PDU A 1
O4 O 0.39352(8) 0.45406(8) 0.71787(16) 0.0377(4) Uani 0.871(3) 1 d PDU A 1
C22 C 0.49234(16) 0.50393(11) 0.65769(19) 0.0303(5) Uani 0.871(3) 1 d PDU A 1
F1 F 0.45616(13) 0.48075(9) 0.57191(10) 0.0750(7) Uani 0.871(3) 1 d PD A 1
F2 F 0.56560(9) 0.50758(9) 0.67121(17) 0.0765(9) Uani 0.871(3) 1 d PD A 1
F3 F 0.46902(17) 0.56524(12) 0.6575(2) 0.0388(7) Uani 0.871(3) 1 d PDU A 1
S" S 0.4682(6) 0.4530(5) 0.7449(7) 0.0096(19) Uiso 0.129(3) 1 d PDU A 2
O2" O 0.5132(8) 0.3951(6) 0.7712(8) 0.021(3) Uiso 0.129(3) 1 d PDU A 2
O3" O 0.4744(9) 0.4901(6) 0.8251(8) 0.046(3) Uiso 0.129(3) 1 d PDU A 2
O4" O 0.3954(6) 0.4462(6) 0.6741(9) 0.041(3) Uiso 0.129(3) 1 d PDU A 2
C22" C 0.5167(7) 0.5042(6) 0.6863(8) 0.027(4) Uiso 0.129(3) 1 d PDU A 2
F1" F 0.5240(6) 0.4731(5) 0.6130(6) 0.043(3) Uiso 0.129(3) 1 d PD A 2
F2" F 0.5863(5) 0.5178(4) 0.7439(7) 0.038(2) Uiso 0.129(3) 1 d PD A 2
F3" F 0.4773(14) 0.5583(11) 0.653(2) 0.057(8) Uiso 0.129(3) 1 d PDU A 2
Si' Si 0.74455(2) 0.114520(19) 0.87869(3) 0.01979(9) Uani 1 1 d . . .
O1' O 0.78812(5) 0.18843(5) 0.91322(6) 0.01561(19) Uani 1 1 d . . .
N1' N 0.81113(6) 0.34552(5) 0.89446(8) 0.0145(2) Uani 1 1 d . . .
N2' N 0.92255(6) 0.29605(6) 0.94806(8) 0.0149(2) Uani 1 1 d . . .
N3' N 0.80078(6) 0.20450(6) 0.77231(8) 0.0153(2) Uani 1 1 d . . .
C1' C 0.84726(7) 0.28747(6) 0.90019(9) 0.0135(2) Uani 1 1 d . . .
C2' C 0.86597(8) 0.39275(7) 0.93714(10) 0.0177(3) Uani 1 1 d . . .
C3' C 0.93446(8) 0.36228(7) 0.97137(10) 0.0178(3) Uani 1 1 d . . .
C4' C 0.72591(8) 0.36073(7) 0.85200(10) 0.0168(3) Uani 1 1 d . . .
C5' C 0.71106(9) 0.40238(8) 0.76369(11) 0.0257(3) Uani 1 1 d . . .
H5'1 H 0.7225 0.3768 0.7159 0.039 Uiso 1 1 calc R . .
H5'2 H 0.7435 0.4413 0.7796 0.039 Uiso 1 1 calc R . .
H5'3 H 0.6576 0.4158 0.7389 0.039 Uiso 1 1 calc R . .
C6' C 0.70300(9) 0.39610(8) 0.92698(11) 0.0243(3) Uani 1 1 d . . .
H6'1 H 0.6486 0.4062 0.9012 0.036 Uiso 1 1 calc R . .
H6'2 H 0.7321 0.4368 0.9453 0.036 Uiso 1 1 calc R . .
H6'3 H 0.7137 0.3679 0.9823 0.036 Uiso 1 1 calc R . .
C7' C 0.67687(8) 0.29954(7) 0.82539(10) 0.0195(3) Uani 1 1 d . . .
H7'1 H 0.6231 0.3120 0.8024 0.029 Uiso 1 1 calc R . .
H7'2 H 0.6879 0.2714 0.8808 0.029 Uiso 1 1 calc R . .
H7'3 H 0.6880 0.2759 0.7758 0.029 Uiso 1 1 calc R . .
C8' C 0.85578(9) 0.46503(7) 0.94393(12) 0.0253(3) Uani 1 1 d . . .
H8'1 H 0.8616 0.4765 1.0088 0.038 Uiso 1 1 calc R . .
H8'2 H 0.8050 0.4777 0.9013 0.038 Uiso 1 1 calc R . .
H8'3 H 0.8941 0.4882 0.9261 0.038 Uiso 1 1 calc R . .
C9' C 1.00753(9) 0.39655(8) 1.02358(11) 0.0256(3) Uani 1 1 d . . .
H9'1 H 1.0289 0.4143 0.9785 0.038 Uiso 1 1 calc R . .
H9'2 H 1.0435 0.3655 1.0656 0.038 Uiso 1 1 calc R . .
H9'3 H 0.9981 0.4323 1.0608 0.038 Uiso 1 1 calc R . .
C10' C 0.98637(8) 0.24511(7) 0.97888(10) 0.0179(3) Uani 1 1 d . . .
C11' C 1.04900(9) 0.26663(9) 0.94311(12) 0.0279(3) Uani 1 1 d . . .
H11D H 1.0887 0.2331 0.9587 0.042 Uiso 1 1 calc R . .
H11E H 1.0709 0.3080 0.9731 0.042 Uiso 1 1 calc R . .
H11F H 1.0275 0.2725 0.8747 0.042 Uiso 1 1 calc R . .
C12' C 1.01412(9) 0.23996(9) 1.08644(11) 0.0272(3) Uani 1 1 d . . .
H12D H 0.9734 0.2223 1.1053 0.041 Uiso 1 1 calc R . .
H12E H 1.0285 0.2835 1.1142 0.041 Uiso 1 1 calc R . .
H12F H 1.0583 0.2109 1.1086 0.041 Uiso 1 1 calc R . .
C13' C 0.96083(9) 0.17721(8) 0.93930(12) 0.0292(4) Uani 1 1 d . . .
H13D H 0.9421 0.1789 0.8703 0.044 Uiso 1 1 calc R . .
H13E H 0.9201 0.1621 0.9602 0.044 Uiso 1 1 calc R . .
H13F H 1.0038 0.1469 0.9619 0.044 Uiso 1 1 calc R . .
C14' C 0.81103(7) 0.22495(6) 0.85368(9) 0.0142(3) Uani 1 1 d . . .
C15' C 0.81868(7) 0.23359(6) 0.69302(9) 0.0131(2) Uani 1 1 d . . .
C16' C 0.86501(9) 0.29727(8) 0.71260(10) 0.0222(3) Uani 1 1 d . . .
H16D H 0.8386 0.3307 0.7356 0.033 Uiso 1 1 calc R . .
H16E H 0.8707 0.3126 0.6544 0.033 Uiso 1 1 calc R . .
H16F H 0.9153 0.2892 0.7603 0.033 Uiso 1 1 calc R . .
C17' C 0.74102(9) 0.24540(8) 0.61470(10) 0.0234(3) Uani 1 1 d . . .
H17D H 0.7109 0.2051 0.6036 0.035 Uiso 1 1 calc R . .
H17E H 0.7486 0.2582 0.5566 0.035 Uiso 1 1 calc R . .
H17F H 0.7141 0.2803 0.6340 0.035 Uiso 1 1 calc R . .
C18' C 0.86086(10) 0.17998(8) 0.66102(11) 0.0263(3) Uani 1 1 d . . .
H18D H 0.9113 0.1736 0.7092 0.040 Uiso 1 1 calc R . .
H18E H 0.8661 0.1930 0.6016 0.040 Uiso 1 1 calc R . .
H18F H 0.8321 0.1390 0.6518 0.040 Uiso 1 1 calc R . .
C19' C 0.72211(9) 0.09056(8) 0.98306(11) 0.0246(3) Uani 1 1 d . . .
H19D H 0.7691 0.0887 1.0384 0.037 Uiso 1 1 calc R . .
H19E H 0.6978 0.0474 0.9724 0.037 Uiso 1 1 calc R . .
H19F H 0.6876 0.1228 0.9937 0.037 Uiso 1 1 calc R . .
C20' C 0.81097(11) 0.05542(8) 0.85850(12) 0.0306(4) Uani 1 1 d . . .
H20D H 0.8219 0.0684 0.8026 0.046 Uiso 1 1 calc R . .
H20E H 0.7880 0.0118 0.8487 0.046 Uiso 1 1 calc R . .
H20F H 0.8583 0.0547 0.9134 0.046 Uiso 1 1 calc R . .
C21' C 0.65690(10) 0.12377(9) 0.77406(12) 0.0342(4) Uani 1 1 d . . .
H21D H 0.6232 0.1555 0.7877 0.051 Uiso 1 1 calc R . .
H21E H 0.6310 0.0814 0.7583 0.051 Uiso 1 1 calc R . .
H21F H 0.6699 0.1393 0.7208 0.051 Uiso 1 1 calc R . .
C22' C -0.01579(9) 0.46836(9) 0.64883(12) 0.0279(3) Uani 1 1 d . . .
S' S 0.00113(3) 0.46196(2) 0.77417(3) 0.02960(10) Uani 1 1 d . . .
O2' O 0.06360(10) 0.50642(8) 0.81561(10) 0.0557(4) Uani 1 1 d . . .
O3' O -0.06996(10) 0.48159(8) 0.78000(11) 0.0551(4) Uani 1 1 d . . .
O4' O 0.02019(7) 0.39431(6) 0.79432(10) 0.0371(3) Uani 1 1 d . . .
F1' F 0.04323(6) 0.44687(6) 0.62836(8) 0.0433(3) Uani 1 1 d . . .
F2' F -0.02959(7) 0.52949(6) 0.61808(9) 0.0505(3) Uani 1 1 d . . .
F3' F -0.07565(7) 0.43208(7) 0.59869(8) 0.0532(3) 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
Si O1 1.7103(10) . ?
Si C19 1.8444(17) . ?
Si C20 1.8498(15) . ?
Si C21 1.8509(17) . ?
O1 C14 1.3564(16) . ?
N1 C1 1.3565(17) . ?
N1 C2 1.3965(18) . ?
N1 C4 1.5257(17) . ?
N2 C1 1.3528(17) . ?
N2 C3 1.3947(17) . ?
N2 C10 1.5301(17) . ?
N3 C14 1.2555(18) . ?
N3 C15 1.4897(16) . ?
C1 C14 1.5038(18) . ?
C2 C3 1.359(2) . ?
C2 C8 1.5009(19) . ?
C3 C9 1.4990(19) . ?
C4 C7 1.525(2) . ?
C4 C5 1.533(2) . ?
C4 C6 1.537(2) . ?
C10 C13 1.5196(19) . ?
C10 C12 1.5306(19) . ?
C10 C11 1.535(2) . ?
C15 C17 1.520(2) . ?
C15 C16 1.5375(19) . ?
C15 C18 1.5471(19) . ?
S O3 1.430(2) . ?
S O2 1.439(2) . ?
S O4 1.448(2) . ?
S C22 1.824(3) . ?
C22 F2 1.324(3) . ?
C22 F1 1.325(3) . ?
C22 F3 1.328(3) . ?
S" O3" 1.405(11) . ?
S" O4" 1.417(11) . ?
S" O2" 1.428(12) . ?
S" C22" 1.818(13) . ?
C22" F2" 1.322(12) . ?
C22" F3" 1.328(13) . ?
C22" F1" 1.332(12) . ?
Si' O1' 1.7106(10) . ?
Si' C20' 1.8432(18) . ?
Si' C21' 1.8484(17) . ?
Si' C19' 1.8486(16) . ?
O1' C14' 1.3577(16) . ?
N1' C1' 1.3556(17) . ?
N1' C2' 1.3938(17) . ?
N1' C4' 1.5338(17) . ?
N2' C1' 1.3552(17) . ?
N2' C3' 1.3975(18) . ?
N2' C10' 1.5325(17) . ?
N3' C14' 1.2537(18) . ?
N3' C15' 1.4873(16) . ?
C1' C14' 1.5019(18) . ?
C2' C3' 1.359(2) . ?
C2' C8' 1.4988(19) . ?
C3' C9' 1.4956(19) . ?
C4' C7' 1.5221(19) . ?
C4' C5' 1.5289(19) . ?
C4' C6' 1.5367(19) . ?
C10' C13' 1.521(2) . ?
C10' C11' 1.531(2) . ?
C10' C12' 1.5321(19) . ?
C15' C18' 1.532(2) . ?
C15' C16' 1.5365(19) . ?
C15' C17' 1.5405(19) . ?
C22' F2' 1.327(2) . ?
C22' F1' 1.332(2) . ?
C22' F3' 1.338(2) . ?
C22' S' 1.8210(17) . ?
S' O3' 1.4318(15) . ?
S' O4' 1.4346(12) . ?
S' O2' 1.4420(16) . ?

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
O1 Si C19 111.64(7) . . ?
O1 Si C20 101.51(6) . . ?
C19 Si C20 110.01(7) . . ?
O1 Si C21 109.84(6) . . ?
C19 Si C21 111.48(8) . . ?
C20 Si C21 111.97(7) . . ?
C14 O1 Si 122.23(8) . . ?
C1 N1 C2 107.67(11) . . ?
C1 N1 C4 129.24(11) . . ?
C2 N1 C4 123.02(11) . . ?
C1 N2 C3 107.84(11) . . ?
C1 N2 C10 129.41(11) . . ?
C3 N2 C10 122.73(11) . . ?
C14 N3 C15 131.66(12) . . ?
N2 C1 N1 109.09(11) . . ?
N2 C1 C14 125.66(12) . . ?
N1 C1 C14 124.79(12) . . ?
C3 C2 N1 107.66(12) . . ?
C3 C2 C8 123.37(13) . . ?
N1 C2 C8 128.97(13) . . ?
C2 C3 N2 107.69(12) . . ?
C2 C3 C9 123.54(13) . . ?
N2 C3 C9 128.76(13) . . ?
C7 C4 N1 113.39(11) . . ?
C7 C4 C5 108.23(13) . . ?
N1 C4 C5 108.39(12) . . ?
C7 C4 C6 106.22(12) . . ?
N1 C4 C6 107.60(11) . . ?
C5 C4 C6 113.10(12) . . ?
C13 C10 N2 112.99(11) . . ?
C13 C10 C12 108.39(12) . . ?
N2 C10 C12 108.79(11) . . ?
C13 C10 C11 106.71(12) . . ?
N2 C10 C11 107.67(11) . . ?
C12 C10 C11 112.34(12) . . ?
N3 C14 O1 120.47(12) . . ?
N3 C14 C1 128.44(12) . . ?
O1 C14 C1 111.08(11) . . ?
N3 C15 C17 106.02(11) . . ?
N3 C15 C16 117.67(11) . . ?
C17 C15 C16 110.60(12) . . ?
N3 C15 C18 103.72(11) . . ?
C17 C15 C18 109.66(12) . . ?
C16 C15 C18 108.82(12) . . ?
O3 S O2 115.53(18) . . ?
O3 S O4 114.46(18) . . ?
O2 S O4 115.62(17) . . ?
O3 S C22 103.18(16) . . ?
O2 S C22 102.84(16) . . ?
O4 S C22 102.52(16) . . ?
F2 C22 F1 108.3(2) . . ?
F2 C22 F3 105.9(2) . . ?
F1 C22 F3 106.4(2) . . ?
F2 C22 S 111.48(19) . . ?
F1 C22 S 111.84(18) . . ?
F3 C22 S 112.62(19) . . ?
O3" S" O4" 118.0(11) . . ?
O3" S" O2" 110.4(10) . . ?
O4" S" O2" 116.6(10) . . ?
O3" S" C22" 102.4(9) . . ?
O4" S" C22" 101.8(8) . . ?
O2" S" C22" 105.2(9) . . ?
F2" C22" F3" 111.2(15) . . ?
F2" C22" F1" 106.2(11) . . ?
F3" C22" F1" 107.2(15) . . ?
F2" C22" S" 110.6(9) . . ?
F3" C22" S" 110.6(14) . . ?
F1" C22" S" 110.9(9) . . ?
O1' Si' C20' 110.50(7) . . ?
O1' Si' C21' 110.92(7) . . ?
C20' Si' C21' 112.03(9) . . ?
O1' Si' C19' 101.71(6) . . ?
C20' Si' C19' 110.30(8) . . ?
C21' Si' C19' 110.94(8) . . ?
C14' O1' Si' 120.91(8) . . ?
C1' N1' C2' 107.74(11) . . ?
C1' N1' C4' 129.14(11) . . ?
C2' N1' C4' 123.11(11) . . ?
C1' N2' C3' 107.70(11) . . ?
C1' N2' C10' 129.29(11) . . ?
C3' N2' C10' 122.94(11) . . ?
C14' N3' C15' 131.82(12) . . ?
N2' C1' N1' 109.08(11) . . ?
N2' C1' C14' 125.14(12) . . ?
N1' C1' C14' 125.56(12) . . ?
C3' C2' N1' 107.80(12) . . ?
C3' C2' C8' 123.61(13) . . ?
N1' C2' C8' 128.57(13) . . ?
C2' C3' N2' 107.62(12) . . ?
C2' C3' C9' 123.86(13) . . ?
N2' C3' C9' 128.51(13) . . ?
C7' C4' C5' 108.75(12) . . ?
C7' C4' N1' 112.97(11) . . ?
C5' C4' N1' 108.54(11) . . ?
C7' C4' C6' 106.20(12) . . ?
C5' C4' C6' 112.19(12) . . ?
N1' C4' C6' 108.24(11) . . ?
C13' C10' C11' 107.28(13) . . ?
C13' C10' C12' 107.36(13) . . ?
C11' C10' C12' 112.74(12) . . ?
C13' C10' N2' 113.37(11) . . ?
C11' C10' N2' 108.48(11) . . ?
C12' C10' N2' 107.71(11) . . ?
N3' C14' O1' 120.06(12) . . ?
N3' C14' C1' 129.22(12) . . ?
O1' C14' C1' 110.72(11) . . ?
N3' C15' C18' 105.37(11) . . ?
N3' C15' C16' 117.39(11) . . ?
C18' C15' C16' 110.14(12) . . ?
N3' C15' C17' 105.12(10) . . ?
C18' C15' C17' 108.93(11) . . ?
C16' C15' C17' 109.52(11) . . ?
F2' C22' F1' 107.65(14) . . ?
F2' C22' F3' 107.60(14) . . ?
F1' C22' F3' 106.78(14) . . ?
F2' C22' S' 112.04(12) . . ?
F1' C22' S' 111.85(11) . . ?
F3' C22' S' 110.67(12) . . ?
O3' S' O4' 115.18(9) . . ?
O3' S' O2' 115.63(11) . . ?
O4' S' O2' 114.30(9) . . ?
O3' S' C22' 103.12(8) . . ?
O4' S' C22' 103.27(8) . . ?
O2' S' C22' 102.83(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C19 Si O1 C14 -60.56(12) . . . . ?
C20 Si O1 C14 -177.71(10) . . . . ?
C21 Si O1 C14 63.64(12) . . . . ?
C3 N2 C1 N1 -2.28(15) . . . . ?
C10 N2 C1 N1 176.33(12) . . . . ?
C3 N2 C1 C14 170.22(12) . . . . ?
C10 N2 C1 C14 -11.2(2) . . . . ?
C2 N1 C1 N2 2.29(15) . . . . ?
C4 N1 C1 N2 -174.69(12) . . . . ?
C2 N1 C1 C14 -170.29(12) . . . . ?
C4 N1 C1 C14 12.7(2) . . . . ?
C1 N1 C2 C3 -1.41(15) . . . . ?
C4 N1 C2 C3 175.81(12) . . . . ?
C1 N1 C2 C8 177.83(14) . . . . ?
C4 N1 C2 C8 -5.0(2) . . . . ?
N1 C2 C3 N2 0.02(15) . . . . ?
C8 C2 C3 N2 -179.26(13) . . . . ?
N1 C2 C3 C9 -179.77(13) . . . . ?
C8 C2 C3 C9 0.9(2) . . . . ?
C1 N2 C3 C2 1.37(15) . . . . ?
C10 N2 C3 C2 -177.35(12) . . . . ?
C1 N2 C3 C9 -178.85(14) . . . . ?
C10 N2 C3 C9 2.4(2) . . . . ?
C1 N1 C4 C7 3.5(2) . . . . ?
C2 N1 C4 C7 -173.07(13) . . . . ?
C1 N1 C4 C5 -116.71(15) . . . . ?
C2 N1 C4 C5 66.72(16) . . . . ?
C1 N1 C4 C6 120.66(15) . . . . ?
C2 N1 C4 C6 -55.91(16) . . . . ?
C1 N2 C10 C13 -4.70(19) . . . . ?
C3 N2 C10 C13 173.72(12) . . . . ?
C1 N2 C10 C12 115.72(15) . . . . ?
C3 N2 C10 C12 -65.86(16) . . . . ?
C1 N2 C10 C11 -122.28(14) . . . . ?
C3 N2 C10 C11 56.14(16) . . . . ?
C15 N3 C14 O1 -178.75(12) . . . . ?
C15 N3 C14 C1 2.0(2) . . . . ?
Si O1 C14 N3 2.86(17) . . . . ?
Si O1 C14 C1 -177.79(8) . . . . ?
N2 C1 C14 N3 -86.97(19) . . . . ?
N1 C1 C14 N3 84.38(19) . . . . ?
N2 C1 C14 O1 93.75(15) . . . . ?
N1 C1 C14 O1 -94.90(15) . . . . ?
C14 N3 C15 C17 -123.99(16) . . . . ?
C14 N3 C15 C16 0.3(2) . . . . ?
C14 N3 C15 C18 120.53(16) . . . . ?
O3 S C22 F2 63.2(2) . . . . ?
O2 S C22 F2 -57.3(2) . . . . ?
O4 S C22 F2 -177.6(2) . . . . ?
O3 S C22 F1 -175.35(19) . . . . ?
O2 S C22 F1 64.2(2) . . . . ?
O4 S C22 F1 -56.2(2) . . . . ?
O3 S C22 F3 -55.6(3) . . . . ?
O2 S C22 F3 -176.1(2) . . . . ?
O4 S C22 F3 63.6(3) . . . . ?
O3" S" C22" F2" 55.5(12) . . . . ?
O4" S" C22" F2" 177.9(10) . . . . ?
O2" S" C22" F2" -60.0(12) . . . . ?
O3" S" C22" F3" -68.2(17) . . . . ?
O4" S" C22" F3" 54.2(17) . . . . ?
O2" S" C22" F3" 176.3(16) . . . . ?
O3" S" C22" F1" 173.0(11) . . . . ?
O4" S" C22" F1" -64.6(12) . . . . ?
O2" S" C22" F1" 57.5(12) . . . . ?
C20' Si' O1' C14' 65.95(11) . . . . ?
C21' Si' O1' C14' -58.91(12) . . . . ?
C19' Si' O1' C14' -176.94(10) . . . . ?
C3' N2' C1' N1' -1.43(15) . . . . ?
C10' N2' C1' N1' 175.44(12) . . . . ?
C3' N2' C1' C14' 173.55(12) . . . . ?
C10' N2' C1' C14' -9.6(2) . . . . ?
C2' N1' C1' N2' 2.27(15) . . . . ?
C4' N1' C1' N2' -176.59(12) . . . . ?
C2' N1' C1' C14' -172.69(12) . . . . ?
C4' N1' C1' C14' 8.5(2) . . . . ?
C1' N1' C2' C3' -2.24(15) . . . . ?
C4' N1' C2' C3' 176.70(12) . . . . ?
C1' N1' C2' C8' 175.90(14) . . . . ?
C4' N1' C2' C8' -5.2(2) . . . . ?
N1' C2' C3' N2' 1.35(15) . . . . ?
C8' C2' C3' N2' -176.89(13) . . . . ?
N1' C2' C3' C9' -179.00(13) . . . . ?
C8' C2' C3' C9' 2.8(2) . . . . ?
C1' N2' C3' C2' 0.02(15) . . . . ?
C10' N2' C3' C2' -177.10(12) . . . . ?
C1' N2' C3' C9' -179.61(14) . . . . ?
C10' N2' C3' C9' 3.3(2) . . . . ?
C1' N1' C4' C7' 8.87(19) . . . . ?
C2' N1' C4' C7' -169.83(12) . . . . ?
C1' N1' C4' C5' -111.82(15) . . . . ?
C2' N1' C4' C5' 69.48(16) . . . . ?
C1' N1' C4' C6' 126.17(14) . . . . ?
C2' N1' C4' C6' -52.53(16) . . . . ?
C1' N2' C10' C13' 7.6(2) . . . . ?
C3' N2' C10' C13' -175.91(13) . . . . ?
C1' N2' C10' C11' 126.69(15) . . . . ?
C3' N2' C10' C11' -56.86(16) . . . . ?
C1' N2' C10' C12' -110.99(15) . . . . ?
C3' N2' C10' C12' 65.46(16) . . . . ?
C15' N3' C14' O1' 179.14(12) . . . . ?
C15' N3' C14' C1' -1.1(2) . . . . ?
Si' O1' C14' N3' -0.40(17) . . . . ?
Si' O1' C14' C1' 179.80(8) . . . . ?
N2' C1' C14' N3' -87.42(19) . . . . ?
N1' C1' C14' N3' 86.75(19) . . . . ?
N2' C1' C14' O1' 92.35(15) . . . . ?
N1' C1' C14' O1' -93.48(15) . . . . ?
C14' N3' C15' C18' 129.89(15) . . . . ?
C14' N3' C15' C16' 6.9(2) . . . . ?
C14' N3' C15' C17' -115.10(16) . . . . ?
F2' C22' S' O3' 63.89(15) . . . . ?
F1' C22' S' O3' -175.13(13) . . . . ?
F3' C22' S' O3' -56.20(15) . . . . ?
F2' C22' S' O4' -175.85(12) . . . . ?
F1' C22' S' O4' -54.87(14) . . . . ?
F3' C22' S' O4' 64.06(14) . . . . ?
F2' C22' S' O2' -56.68(14) . . . . ?
F1' C22' S' O2' 64.30(15) . . . . ?
F3' C22' S' O2' -176.77(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.049
_refine_instructions_details     
;
TITL eileen63 in P2(1)/c
CELL 1.54184  18.852181  20.448292  15.204133  90.0000 110.9523  90.0000
ZERR    8.00   0.000400   0.000300   0.000300   0.0000   0.0020   0.0000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    F    SI   S
UNIT  176  336  24  32  24  8  8
MERG   2
FMAP   2
 
ACTA 150
CONF
 
TEMP -173
 
PLAN   10
L.S.   30
WGHT    0.048700    3.085000
FVAR       1.84370   0.87148
SI    6    0.225477    0.378697    0.391602    11.00000    0.01998    0.01541 =
         0.01772    0.00045    0.00758    0.00299
O1    4    0.280018    0.309754    0.424042    11.00000    0.01612    0.01511 =
         0.01491   -0.00031    0.00669    0.00145
N1    3    0.427325    0.215208    0.455236    11.00000    0.01151    0.01622 =
         0.01515   -0.00019    0.00398    0.00041
N2    3    0.322113    0.156751    0.401943    11.00000    0.01383    0.01364 =
         0.01524   -0.00010    0.00444    0.00045
N3    3    0.296309    0.300712    0.283796    11.00000    0.01621    0.01663 =
         0.01562    0.00023    0.00752    0.00150
C1    1    0.350995    0.217946    0.409812    11.00000    0.01234    0.01612 =
         0.01259   -0.00027    0.00465    0.00065
C2    1    0.447399    0.149494    0.473371    11.00000    0.01676    0.01833 =
         0.01698    0.00045    0.00504    0.00456
C3    1    0.382550    0.113538    0.440537    11.00000    0.01993    0.01470 =
         0.01799    0.00080    0.00539    0.00400
C4    1    0.484533    0.270990    0.487908    11.00000    0.01252    0.02087 =
         0.02019   -0.00199    0.00410   -0.00388
C5    1    0.539672    0.266339    0.434596    11.00000    0.01912    0.03990 =
         0.02874   -0.00277    0.01154   -0.00677
AFIX 137
H5A   2    0.559850    0.221764    0.439698    11.00000   -1.50000
H5B   2    0.581616    0.297176    0.461884    11.00000   -1.50000
H5C   2    0.512804    0.277101    0.368120    11.00000   -1.50000
AFIX   0
C6    1    0.524102    0.264798    0.595141    11.00000    0.01930    0.03006 =
         0.02057   -0.00470    0.00266   -0.00328
AFIX 137
H6A   2    0.485993    0.266292    0.625183    11.00000   -1.50000
H6B   2    0.560001    0.300999    0.618552    11.00000   -1.50000
H6C   2    0.551549    0.223155    0.610084    11.00000   -1.50000
AFIX   0
C7    1    0.447883    0.338577    0.470192    11.00000    0.01945    0.01897 =
         0.03636   -0.00096    0.00178   -0.00454
AFIX 137
H7A   2    0.422064    0.345155    0.402331    11.00000   -1.50000
H7B   2    0.487148    0.372084    0.495122    11.00000   -1.50000
H7C   2    0.410890    0.341914    0.501744    11.00000   -1.50000
AFIX   0
C8    1    0.524810    0.119931    0.519046    11.00000    0.01831    0.02518 =
         0.02618    0.00047    0.00250    0.00808
AFIX 137
H8A   2    0.528736    0.100339    0.579435    11.00000   -1.50000
H8B   2    0.563520    0.154031    0.529727    11.00000   -1.50000
H8C   2    0.532719    0.086119    0.477799    11.00000   -1.50000
AFIX   0
C9    1    0.380829    0.040472    0.447478    11.00000    0.02832    0.01581 =
         0.03226    0.00263    0.00791    0.00410
AFIX 137
H9A   2    0.420756    0.021588    0.428140    11.00000   -1.50000
H9B   2    0.331206    0.024185    0.406161    11.00000   -1.50000
H9C   2    0.389399    0.027873    0.512670    11.00000   -1.50000
AFIX   0
C10   1    0.239303    0.134200    0.361530    11.00000    0.01377    0.01798 =
         0.01764   -0.00230    0.00531   -0.00383
C11   1    0.222632    0.096282    0.439078    11.00000    0.02506    0.02723 =
         0.02578    0.00322    0.00920   -0.00783
AFIX 137
H11A  2    0.235237    0.123602    0.495575    11.00000   -1.50000
H11B  2    0.253367    0.056338    0.454072    11.00000   -1.50000
H11C  2    0.168647    0.084695    0.417109    11.00000   -1.50000
AFIX   0
C12   1    0.228071    0.092223    0.274219    11.00000    0.02051    0.02910 =
         0.02556   -0.01138    0.00698   -0.00407
AFIX 137
H12A  2    0.181320    0.066586    0.259414    11.00000   -1.50000
H12B  2    0.271425    0.062602    0.286557    11.00000   -1.50000
H12C  2    0.224277    0.120604    0.220785    11.00000   -1.50000
AFIX   0
C13   1    0.183288    0.190683    0.333405    11.00000    0.01244    0.02153 =
         0.02747   -0.00028    0.00691   -0.00117
AFIX 137
H13A  2    0.189984    0.218300    0.388479    11.00000   -1.50000
H13B  2    0.131344    0.173478    0.309239    11.00000   -1.50000
H13C  2    0.192412    0.216699    0.284358    11.00000   -1.50000
AFIX   0
C14   1    0.307660    0.278292    0.364575    11.00000    0.01100    0.01493 =
         0.01678   -0.00109    0.00494    0.00009
C15   1    0.318426    0.276126    0.204995    11.00000    0.01618    0.01816 =
         0.00939   -0.00033    0.00567    0.00320
C16   1    0.363108    0.211614    0.220214    11.00000    0.02682    0.02571 =
         0.01988   -0.00058    0.01203    0.00433
AFIX 137
H16A  2    0.411908    0.216861    0.272046    11.00000   -1.50000
H16B  2    0.372085    0.200030    0.162519    11.00000   -1.50000
H16C  2    0.333813    0.176830    0.235779    11.00000   -1.50000
AFIX   0
C17   1    0.362894    0.331134    0.181486    11.00000    0.02769    0.03012 =
         0.02250    0.00244    0.01259    0.00034
AFIX 137
H17A  2    0.334185    0.372034    0.173615    11.00000   -1.50000
H17B  2    0.371106    0.320773    0.122918    11.00000   -1.50000
H17C  2    0.412063    0.336062    0.232766    11.00000   -1.50000
AFIX   0
C18   1    0.241584    0.267009    0.123101    11.00000    0.02400    0.03182 =
         0.01608   -0.00215    0.00691    0.00098
AFIX 137
H18A  2    0.212577    0.232156    0.139035    11.00000   -1.50000
H18B  2    0.250821    0.255171    0.065661    11.00000   -1.50000
H18C  2    0.212679    0.307927    0.112733    11.00000   -1.50000
AFIX   0
C19   1    0.277060    0.445662    0.359365    11.00000    0.04079    0.01869 =
         0.03565   -0.00044    0.02174    0.00006
AFIX 137
H19A  2    0.325974    0.452589    0.410374    11.00000   -1.50000
H19B  2    0.246861    0.485854    0.349119    11.00000   -1.50000
H19C  2    0.285752    0.434124    0.301474    11.00000   -1.50000
AFIX   0
C20   1    0.209877    0.399200    0.501801    11.00000    0.02638    0.02105 =
         0.02301   -0.00135    0.01067    0.00471
AFIX 137
H20A  2    0.182347    0.363440    0.518322    11.00000   -1.50000
H20B  2    0.180016    0.439524    0.492779    11.00000   -1.50000
H20C  2    0.259004    0.405499    0.552683    11.00000   -1.50000
AFIX   0
C21   1    0.135458    0.359392    0.294412    11.00000    0.02651    0.02670 =
         0.02529    0.00059    0.00650    0.00958
AFIX 137
H21A  2    0.146636    0.342400    0.240505    11.00000   -1.50000
H21B  2    0.104691    0.399153    0.275701    11.00000   -1.50000
H21C  2    0.107386    0.326402    0.315570    11.00000   -1.50000
AFIX   0
 
SAME S" > F3"
SADI S O2 S O3 S O4
SADI O2 O3 O3 O4 O4 O2
SADI C22 F1 C22 F2 C22 F3
SADI F1 F2 F2 F3 F3 F1
SIMU 0.02 0.04 0.9 S > F3"
 
PART1 21
S     7    0.475571    0.453961    0.747689    21.00000    0.02058    0.02399 =
         0.03516    0.00383    0.01144    0.00050
O2    4    0.509505    0.392353    0.739303    21.00000    0.03093    0.02262 =
         0.06003    0.00553    0.01990    0.00746
O3    4    0.513401    0.489509    0.832569    21.00000    0.06085    0.04919 =
         0.02512   -0.00330    0.00405   -0.01014
O4    4    0.393519    0.454055    0.717875    21.00000    0.02039    0.03044 =
         0.06598    0.00672    0.02005    0.00101
C22   1    0.492336    0.503929    0.657691    21.00000    0.02833    0.03316 =
         0.03475    0.00609    0.01770    0.01114
F1    5    0.456164    0.480747    0.571910    21.00000    0.12974    0.06748 =
         0.02925   -0.00403    0.03008    0.01396
F2    5    0.565603    0.507580    0.671212    21.00000    0.04125    0.07878 =
         0.13439    0.06628    0.06176    0.03147
F3    5    0.469021    0.565238    0.657496    21.00000    0.03906    0.02750 =
         0.05817    0.01741    0.02753    0.00909
PART2 -21
S"    7    0.468218    0.453011    0.744908   -21.00000    0.00962
O2"   4    0.513156    0.395065    0.771174   -21.00000    0.02095
O3"   4    0.474361    0.490143    0.825082   -21.00000    0.04556
O4"   4    0.395368    0.446225    0.674083   -21.00000    0.04054
C22"  1    0.516688    0.504151    0.686285   -21.00000    0.02744
F1"   5    0.524044    0.473052    0.613025   -21.00000    0.04318
F2"   5    0.586337    0.517816    0.743899   -21.00000    0.03847
F3"   5    0.477256    0.558345    0.653489   -21.00000    0.05742
PART0
 
SI'   6    0.744548    0.114520    0.878694    11.00000    0.02283    0.01679 =
         0.01783    0.00073    0.00493   -0.00529
O1'   4    0.788116    0.188435    0.913223    11.00000    0.01679    0.01559 =
         0.01525    0.00092    0.00670   -0.00203
N1'   3    0.811128    0.345516    0.894463    11.00000    0.01420    0.01440 =
         0.01565   -0.00064    0.00627   -0.00080
N2'   3    0.922554    0.296051    0.948061    11.00000    0.01206    0.01729 =
         0.01545   -0.00140    0.00521   -0.00189
N3'   3    0.800778    0.204497    0.772312    11.00000    0.01413    0.01700 =
         0.01520   -0.00006    0.00560   -0.00141
C1'   1    0.847260    0.287475    0.900192    11.00000    0.01210    0.01531 =
         0.01359   -0.00062    0.00534   -0.00114
C2'   1    0.865967    0.392746    0.937140    11.00000    0.02061    0.01585 =
         0.01945   -0.00387    0.01066   -0.00499
C3'   1    0.934460    0.362277    0.971372    11.00000    0.01776    0.01862 =
         0.01894   -0.00415    0.00879   -0.00574
C4'   1    0.725914    0.360732    0.851997    11.00000    0.01379    0.01796 =
         0.01901    0.00225    0.00638    0.00365
C5'   1    0.711065    0.402379    0.763689    11.00000    0.02635    0.02722 =
         0.02331    0.00945    0.00858    0.00528
AFIX 137
H5'1  2    0.722508    0.376761    0.715924    11.00000   -1.50000
H5'2  2    0.743538    0.441288    0.779604    11.00000   -1.50000
H5'3  2    0.657630    0.415784    0.738934    11.00000   -1.50000
AFIX   0
C6'   1    0.703005    0.396096    0.926984    11.00000    0.02191    0.02717 =
         0.02610   -0.00218    0.01146    0.00514
AFIX 137
H6'1  2    0.648615    0.406212    0.901151    11.00000   -1.50000
H6'2  2    0.732071    0.436769    0.945305    11.00000   -1.50000
H6'3  2    0.713719    0.367860    0.982317    11.00000   -1.50000
AFIX   0
C7'   1    0.676871    0.299536    0.825385    11.00000    0.01284    0.02269 =
         0.02206    0.00057    0.00496    0.00074
AFIX 137
H7'1  2    0.623126    0.311996    0.802398    11.00000   -1.50000
H7'2  2    0.687865    0.271351    0.880812    11.00000   -1.50000
H7'3  2    0.688047    0.275862    0.775812    11.00000   -1.50000
AFIX   0
C8'   1    0.855784    0.465030    0.943930    11.00000    0.02795    0.01667 =
         0.03567   -0.00544    0.01662   -0.00315
AFIX 137
H8'1  2    0.861625    0.476459    1.008750    11.00000   -1.50000
H8'2  2    0.804954    0.477655    0.901343    11.00000   -1.50000
H8'3  2    0.894114    0.488241    0.926137    11.00000   -1.50000
AFIX   0
C9'   1    1.007528    0.396554    1.023581    11.00000    0.02011    0.02607 =
         0.02933   -0.00754    0.00709   -0.00982
AFIX 137
H9'1  2    1.028922    0.414262    0.978535    11.00000   -1.50000
H9'2  2    1.043471    0.365514    1.065589    11.00000   -1.50000
H9'3  2    0.998070    0.432346    1.060830    11.00000   -1.50000
AFIX   0
C10'  1    0.986366    0.245114    0.978875    11.00000    0.01167    0.02186 =
         0.01896    0.00100    0.00417    0.00189
C11'  1    1.049001    0.266631    0.943109    11.00000    0.01999    0.03540 =
         0.03342    0.00873    0.01572    0.00671
AFIX 137
H11D  2    1.088748    0.233113    0.958694    11.00000   -1.50000
H11E  2    1.070896    0.308038    0.973080    11.00000   -1.50000
H11F  2    1.027462    0.272520    0.874654    11.00000   -1.50000
AFIX   0
C12'  1    1.014124    0.239960    1.086437    11.00000    0.02047    0.04083 =
         0.01855    0.00325    0.00465    0.00532
AFIX 137
H12D  2    0.973379    0.222276    1.105290    11.00000   -1.50000
H12E  2    1.028458    0.283454    1.114178    11.00000   -1.50000
H12F  2    1.058288    0.210854    1.108644    11.00000   -1.50000
AFIX   0
C13'  1    0.960829    0.177206    0.939303    11.00000    0.01924    0.02216 =
         0.03832   -0.00267    0.00059    0.00511
AFIX 137
H13D  2    0.942101    0.178873    0.870342    11.00000   -1.50000
H13E  2    0.920091    0.162102    0.960185    11.00000   -1.50000
H13F  2    1.003846    0.146902    0.961893    11.00000   -1.50000
AFIX   0
C14'  1    0.811035    0.224950    0.853684    11.00000    0.01064    0.01463 =
         0.01701    0.00052    0.00452   -0.00012
C15'  1    0.818683    0.233594    0.693025    11.00000    0.01305    0.01738 =
         0.00970    0.00040    0.00517   -0.00130
C16'  1    0.865006    0.297274    0.712598    11.00000    0.02349    0.02596 =
         0.01936    0.00175    0.01029   -0.00358
AFIX 137
H16D  2    0.838601    0.330654    0.735595    11.00000   -1.50000
H16E  2    0.870664    0.312564    0.654372    11.00000   -1.50000
H16F  2    0.915297    0.289219    0.760312    11.00000   -1.50000
AFIX   0
C17'  1    0.741016    0.245399    0.614700    11.00000    0.02173    0.03180 =
         0.01614    0.00211    0.00630   -0.00161
AFIX 137
H17D  2    0.710883    0.205139    0.603648    11.00000   -1.50000
H17E  2    0.748648    0.258233    0.556614    11.00000   -1.50000
H17F  2    0.714109    0.280336    0.634013    11.00000   -1.50000
AFIX   0
C18'  1    0.860857    0.179983    0.661023    11.00000    0.02969    0.03124 =
         0.02216   -0.00164    0.01425    0.00180
AFIX 137
H18D  2    0.911350    0.173637    0.709164    11.00000   -1.50000
H18E  2    0.866091    0.192989    0.601604    11.00000   -1.50000
H18F  2    0.832105    0.139030    0.651832    11.00000   -1.50000
AFIX   0
C19'  1    0.722106    0.090557    0.983060    11.00000    0.02535    0.02174 =
         0.02763    0.00499    0.01050   -0.00330
AFIX 137
H19D  2    0.769067    0.088728    1.038401    11.00000   -1.50000
H19E  2    0.697790    0.047446    0.972383    11.00000   -1.50000
H19F  2    0.687564    0.122794    0.993726    11.00000   -1.50000
AFIX   0
C20'  1    0.810968    0.055423    0.858498    11.00000    0.04649    0.01901 =
         0.02861   -0.00207    0.01639   -0.00277
AFIX 137
H20D  2    0.821933    0.068399    0.802623    11.00000   -1.50000
H20E  2    0.788018    0.011761    0.848695    11.00000   -1.50000
H20F  2    0.858268    0.054689    0.913437    11.00000   -1.50000
AFIX   0
C21'  1    0.656900    0.123766    0.774065    11.00000    0.03101    0.03532 =
         0.02893    0.00729    0.00189   -0.01629
AFIX 137
H21D  2    0.623234    0.155502    0.787651    11.00000   -1.50000
H21E  2    0.631050    0.081442    0.758317    11.00000   -1.50000
H21F  2    0.669949    0.139256    0.720755    11.00000   -1.50000
AFIX   0
C22'  1   -0.015791    0.468361    0.648826    11.00000    0.02118    0.03479 =
         0.02673    0.00176    0.00751    0.00222
S'    7    0.001133    0.461962    0.774169    11.00000    0.03750    0.02776 =
         0.02403    0.00442    0.01162    0.01161
O2'   4    0.063600    0.506417    0.815611    11.00000    0.07032    0.04323 =
         0.03544   -0.01198   -0.00320   -0.01062
O3'   4   -0.069959    0.481588    0.780000    11.00000    0.06559    0.06231 =
         0.05447    0.02374    0.04212    0.04054
O4'   4    0.020190    0.394306    0.794321    11.00000    0.03428    0.03043 =
         0.04818    0.01583    0.01655    0.01263
F1'   5    0.043232    0.446872    0.628365    11.00000    0.03273    0.06460 =
         0.03836   -0.00189    0.01983    0.00530
F2'   5   -0.029593    0.529492    0.618077    11.00000    0.05753    0.04941 =
         0.04591    0.02679    0.02021    0.01517
F3'   5   -0.075647    0.432084    0.598688    11.00000    0.03262    0.07959 =
         0.03667   -0.01045   -0.00074   -0.01649
 
HKLF    4
;
####################################################################### 
# 
# 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_msv05
_database_code_depnum_ccdc_archive 'CCDC 1052447'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H43 F3 N2 O3 S Si'
_chemical_formula_weight         632.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   9.0006(2)
_cell_length_b                   13.4769(2)
_cell_length_c                   14.1223(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.137(2)
_cell_angle_gamma                90.00
_cell_volume                     1691.29(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30981
_cell_measurement_theta_min      4.5550
_cell_measurement_theta_max      75.5130

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.04728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38932
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.56
_diffrn_reflns_theta_max         75.67
_reflns_number_total             6988
_reflns_number_gt                6891
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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. 

 The compound crystallises per chance in a Soehnke space group.
;

_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)+(0.0474P)²+0.3057P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(10)
_chemical_absolute_configuration .
_refine_ls_number_reflns         6988
_refine_ls_number_parameters     399
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0768
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
Si Si 0.38323(4) 0.50469(3) 0.47961(2) 0.02209(9) Uani 1 1 d . . .
N1 N 0.45573(12) 0.65310(9) 0.16535(8) 0.0191(2) Uani 1 1 d . . .
N2 N 0.63408(12) 0.53978(9) 0.17503(8) 0.0196(2) Uani 1 1 d . . .
C1 C 0.50013(14) 0.56331(9) 0.20233(9) 0.0177(2) Uani 1 1 d . . .
C2 C 0.56588(16) 0.68740(12) 0.11392(11) 0.0260(3) Uani 1 1 d . . .
C3 C 0.67686(16) 0.61892(12) 0.12186(10) 0.0243(3) Uani 1 1 d . . .
C4 C 0.31301(15) 0.71307(10) 0.17271(10) 0.0215(3) Uani 1 1 d . . .
C5 C 0.21706(17) 0.67070(12) 0.24292(11) 0.0284(3) Uani 1 1 d . . .
H5A H 0.2743 0.6724 0.3080 0.043 Uiso 1 1 calc R . .
H5B H 0.1898 0.6020 0.2253 0.043 Uiso 1 1 calc R . .
H5C H 0.1255 0.7105 0.2406 0.043 Uiso 1 1 calc R . .
C6 C 0.3615(2) 0.81659(13) 0.20895(17) 0.0444(5) Uani 1 1 d . . .
H6A H 0.4020 0.8529 0.1586 0.067 Uiso 1 1 calc R . .
H6B H 0.4390 0.8110 0.2658 0.067 Uiso 1 1 calc R . .
H6C H 0.2744 0.8523 0.2257 0.067 Uiso 1 1 calc R . .
C7 C 0.21605(17) 0.71424(12) 0.07323(11) 0.0273(3) Uani 1 1 d . . .
H7A H 0.1370 0.7645 0.0717 0.041 Uiso 1 1 calc R . .
H7B H 0.1700 0.6489 0.0595 0.041 Uiso 1 1 calc R . .
H7C H 0.2792 0.7301 0.0248 0.041 Uiso 1 1 calc R . .
C8 C 0.5675(2) 0.78051(15) 0.05654(16) 0.0448(5) Uani 1 1 d . . .
H8A H 0.6296 0.8305 0.0946 0.067 Uiso 1 1 calc R . .
H8B H 0.4645 0.8056 0.0394 0.067 Uiso 1 1 calc R . .
H8C H 0.6094 0.7665 -0.0020 0.067 Uiso 1 1 calc R . .
C9 C 0.81938(18) 0.63228(15) 0.08087(12) 0.0343(3) Uani 1 1 d . . .
H9A H 0.8044 0.6083 0.0145 0.051 Uiso 1 1 calc R . .
H9B H 0.9006 0.5945 0.1192 0.051 Uiso 1 1 calc R . .
H9C H 0.8463 0.7028 0.0821 0.051 Uiso 1 1 calc R . .
C10 C 0.72939(16) 0.44666(10) 0.19510(11) 0.0248(3) Uani 1 1 d . . .
C11 C 0.64634(19) 0.36192(12) 0.23500(15) 0.0367(4) Uani 1 1 d . . .
H11A H 0.5548 0.3463 0.1900 0.055 Uiso 1 1 calc R . .
H11B H 0.6193 0.3816 0.2969 0.055 Uiso 1 1 calc R . .
H11C H 0.7115 0.3033 0.2438 0.055 Uiso 1 1 calc R . .
C12 C 0.86977(16) 0.47167(12) 0.26691(11) 0.0275(3) Uani 1 1 d . . .
H12A H 0.9408 0.4161 0.2710 0.041 Uiso 1 1 calc R . .
H12B H 0.8414 0.4835 0.3301 0.041 Uiso 1 1 calc R . .
H12C H 0.9172 0.5314 0.2457 0.041 Uiso 1 1 calc R . .
C13 C 0.7688(2) 0.41156(14) 0.09872(13) 0.0376(4) Uani 1 1 d . . .
H13A H 0.6790 0.4153 0.0495 0.056 Uiso 1 1 calc R . .
H13B H 0.8046 0.3428 0.1048 0.056 Uiso 1 1 calc R . .
H13C H 0.8478 0.4541 0.0804 0.056 Uiso 1 1 calc R . .
C14 C 0.42479(14) 0.50666(10) 0.27241(9) 0.0183(2) Uani 1 1 d . . .
C15 C 0.46898(15) 0.53215(10) 0.36619(10) 0.0201(3) Uani 1 1 d . . .
C16 C 0.59440(16) 0.59808(10) 0.38712(9) 0.0213(3) Uani 1 1 d . . .
C17 C 0.70598(16) 0.64789(11) 0.40985(10) 0.0227(3) Uani 1 1 d . . .
C18 C 0.31663(15) 0.42892(10) 0.23282(9) 0.0200(2) Uani 1 1 d . . .
C19 C 0.29301(17) 0.34407(11) 0.28620(10) 0.0247(3) Uani 1 1 d . . .
H19 H 0.3395 0.3394 0.3513 0.030 Uiso 1 1 calc R . .
C20 C 0.20276(18) 0.26699(11) 0.24523(11) 0.0278(3) Uani 1 1 d . . .
H20 H 0.1886 0.2100 0.2823 0.033 Uiso 1 1 calc R . .
C21 C 0.13276(16) 0.27267(11) 0.15006(11) 0.0258(3) Uani 1 1 d . . .
H21 H 0.0708 0.2199 0.1222 0.031 Uiso 1 1 calc R . .
C22 C 0.15436(16) 0.35618(11) 0.09618(10) 0.0237(3) Uani 1 1 d . . .
H22 H 0.1061 0.3609 0.0314 0.028 Uiso 1 1 calc R . .
C23 C 0.24646(15) 0.43289(10) 0.13681(9) 0.0203(2) Uani 1 1 d . . .
H23 H 0.2621 0.4890 0.0989 0.024 Uiso 1 1 calc R . .
C24 C 0.84194(16) 0.70230(10) 0.43974(10) 0.0229(3) Uani 1 1 d . . .
C25 C 0.92345(17) 0.68508(12) 0.53136(11) 0.0266(3) Uani 1 1 d . . .
H25 H 0.8882 0.6381 0.5728 0.032 Uiso 1 1 calc R . .
C26 C 1.05591(18) 0.73692(13) 0.56144(12) 0.0325(3) Uani 1 1 d . . .
H26 H 1.1111 0.7254 0.6236 0.039 Uiso 1 1 calc R . .
C27 C 1.10785(18) 0.80519(13) 0.50151(13) 0.0340(4) Uani 1 1 d . . .
H27 H 1.1983 0.8406 0.5228 0.041 Uiso 1 1 calc R . .
C28 C 1.02833(18) 0.82245(12) 0.40996(13) 0.0315(3) Uani 1 1 d . . .
H28 H 1.0645 0.8695 0.3690 0.038 Uiso 1 1 calc R . .
C29 C 0.89595(17) 0.77060(11) 0.37883(11) 0.0269(3) Uani 1 1 d . . .
H29 H 0.8422 0.7816 0.3162 0.032 Uiso 1 1 calc R . .
C30 C 0.17522(17) 0.49263(13) 0.45244(11) 0.0309(3) Uani 1 1 d . . .
H30A H 0.1341 0.4885 0.5125 0.046 Uiso 1 1 calc R . .
H30B H 0.1489 0.4324 0.4146 0.046 Uiso 1 1 calc R . .
H30C H 0.1329 0.5507 0.4159 0.046 Uiso 1 1 calc R . .
C31 C 0.4734(2) 0.39371(13) 0.54316(12) 0.0352(4) Uani 1 1 d . . .
H31A H 0.4277 0.3807 0.6005 0.053 Uiso 1 1 calc R . .
H31B H 0.5814 0.4060 0.5621 0.053 Uiso 1 1 calc R . .
H31C H 0.4586 0.3361 0.5004 0.053 Uiso 1 1 calc R . .
C32 C 0.42986(19) 0.61495(13) 0.55904(11) 0.0320(3) Uani 1 1 d . . .
H32A H 0.3956 0.6755 0.5237 0.048 Uiso 1 1 calc R . .
H32B H 0.5390 0.6182 0.5797 0.048 Uiso 1 1 calc R . .
H32C H 0.3794 0.6090 0.6154 0.048 Uiso 1 1 calc R . .
S S 0.96763(5) -0.01496(3) 0.16465(3) 0.03157(9) Uani 1 1 d . . .
O1 O 0.99646(17) 0.02967(10) 0.07688(10) 0.0438(3) Uani 1 1 d . . .
O2 O 1.0617(2) 0.01876(11) 0.25048(10) 0.0548(4) Uani 1 1 d . . .
O3 O 0.94005(15) -0.12002(8) 0.15975(9) 0.0347(3) Uani 1 1 d . . .
C33 C 0.7841(3) 0.03584(14) 0.17624(16) 0.0461(5) Uani 1 1 d . . .
F1 F 0.7903(2) 0.13426(10) 0.18827(12) 0.0725(4) Uani 1 1 d . . .
F2 F 0.7294(2) -0.00290(13) 0.24956(12) 0.0761(5) Uani 1 1 d . . .
F3 F 0.68189(15) 0.01821(10) 0.09677(11) 0.0597(3) 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
Si C30 1.8576(16) . ?
Si C31 1.8627(17) . ?
Si C32 1.8690(16) . ?
Si C15 1.9211(14) . ?
N1 C1 1.3529(18) . ?
N1 C2 1.3974(18) . ?
N1 C4 1.5351(17) . ?
N2 C1 1.3602(18) . ?
N2 C3 1.3934(18) . ?
N2 C10 1.5212(17) . ?
C1 C14 1.4951(17) . ?
C2 C3 1.351(2) . ?
C2 C8 1.495(2) . ?
C3 C9 1.500(2) . ?
C4 C5 1.525(2) . ?
C4 C6 1.526(2) . ?
C4 C7 1.5318(19) . ?
C10 C11 1.521(2) . ?
C10 C12 1.5269(19) . ?
C10 C13 1.535(2) . ?
C14 C15 1.3649(18) . ?
C14 C18 1.4783(18) . ?
C15 C16 1.4301(19) . ?
C16 C17 1.208(2) . ?
C17 C24 1.4316(19) . ?
C18 C23 1.4029(18) . ?
C18 C19 1.4042(19) . ?
C19 C20 1.387(2) . ?
C20 C21 1.393(2) . ?
C21 C22 1.389(2) . ?
C22 C23 1.3907(19) . ?
C24 C29 1.399(2) . ?
C24 C25 1.402(2) . ?
C25 C26 1.389(2) . ?
C26 C27 1.381(3) . ?
C27 C28 1.394(3) . ?
C28 C29 1.391(2) . ?
S O3 1.4374(12) . ?
S O2 1.4376(14) . ?
S O1 1.4380(13) . ?
S C33 1.819(2) . ?
C33 F2 1.323(2) . ?
C33 F1 1.337(2) . ?
C33 F3 1.354(3) . ?

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
C30 Si C31 112.14(8) . . ?
C30 Si C32 108.45(8) . . ?
C31 Si C32 108.06(8) . . ?
C30 Si C15 111.71(6) . . ?
C31 Si C15 110.76(7) . . ?
C32 Si C15 105.40(7) . . ?
C1 N1 C2 107.82(11) . . ?
C1 N1 C4 130.07(11) . . ?
C2 N1 C4 122.10(11) . . ?
C1 N2 C3 107.91(11) . . ?
C1 N2 C10 129.68(12) . . ?
C3 N2 C10 122.41(11) . . ?
N1 C1 N2 108.66(11) . . ?
N1 C1 C14 125.10(12) . . ?
N2 C1 C14 125.74(12) . . ?
C3 C2 N1 107.88(12) . . ?
C3 C2 C8 123.19(14) . . ?
N1 C2 C8 128.91(14) . . ?
C2 C3 N2 107.67(12) . . ?
C2 C3 C9 123.52(14) . . ?
N2 C3 C9 128.79(14) . . ?
C5 C4 C6 106.59(14) . . ?
C5 C4 C7 107.53(12) . . ?
C6 C4 C7 112.90(13) . . ?
C5 C4 N1 114.40(11) . . ?
C6 C4 N1 107.85(12) . . ?
C7 C4 N1 107.72(11) . . ?
N2 C10 C11 113.11(12) . . ?
N2 C10 C12 108.93(11) . . ?
C11 C10 C12 108.86(13) . . ?
N2 C10 C13 106.97(12) . . ?
C11 C10 C13 107.05(14) . . ?
C12 C10 C13 111.95(13) . . ?
C15 C14 C18 128.19(12) . . ?
C15 C14 C1 114.89(11) . . ?
C18 C14 C1 116.89(11) . . ?
C14 C15 C16 117.11(12) . . ?
C14 C15 Si 131.82(10) . . ?
C16 C15 Si 110.84(10) . . ?
C17 C16 C15 174.63(15) . . ?
C16 C17 C24 176.83(16) . . ?
C23 C18 C19 117.82(12) . . ?
C23 C18 C14 120.46(12) . . ?
C19 C18 C14 121.39(12) . . ?
C20 C19 C18 120.96(13) . . ?
C19 C20 C21 120.43(14) . . ?
C22 C21 C20 119.45(13) . . ?
C21 C22 C23 120.15(13) . . ?
C22 C23 C18 121.18(13) . . ?
C29 C24 C25 119.64(14) . . ?
C29 C24 C17 121.34(13) . . ?
C25 C24 C17 119.01(14) . . ?
C26 C25 C24 119.80(15) . . ?
C27 C26 C25 120.36(15) . . ?
C26 C27 C28 120.37(15) . . ?
C29 C28 C27 119.81(15) . . ?
C28 C29 C24 120.01(14) . . ?
O3 S O2 115.22(8) . . ?
O3 S O1 115.09(8) . . ?
O2 S O1 115.58(9) . . ?
O3 S C33 102.87(9) . . ?
O2 S C33 103.12(10) . . ?
O1 S C33 102.17(9) . . ?
F2 C33 F1 107.78(17) . . ?
F2 C33 F3 106.90(19) . . ?
F1 C33 F3 106.77(18) . . ?
F2 C33 S 112.23(15) . . ?
F1 C33 S 111.37(16) . . ?
F3 C33 S 111.50(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 N2 -0.52(15) . . . . ?
C4 N1 C1 N2 178.89(12) . . . . ?
C2 N1 C1 C14 171.73(12) . . . . ?
C4 N1 C1 C14 -8.9(2) . . . . ?
C3 N2 C1 N1 1.93(14) . . . . ?
C10 N2 C1 N1 -178.24(12) . . . . ?
C3 N2 C1 C14 -170.26(12) . . . . ?
C10 N2 C1 C14 9.6(2) . . . . ?
C1 N1 C2 C3 -1.13(16) . . . . ?
C4 N1 C2 C3 179.41(12) . . . . ?
C1 N1 C2 C8 177.33(17) . . . . ?
C4 N1 C2 C8 -2.1(2) . . . . ?
N1 C2 C3 N2 2.29(16) . . . . ?
C8 C2 C3 N2 -176.28(15) . . . . ?
N1 C2 C3 C9 -176.29(14) . . . . ?
C8 C2 C3 C9 5.1(3) . . . . ?
C1 N2 C3 C2 -2.62(16) . . . . ?
C10 N2 C3 C2 177.53(12) . . . . ?
C1 N2 C3 C9 175.86(15) . . . . ?
C10 N2 C3 C9 -4.0(2) . . . . ?
C1 N1 C4 C5 8.8(2) . . . . ?
C2 N1 C4 C5 -171.89(13) . . . . ?
C1 N1 C4 C6 127.16(16) . . . . ?
C2 N1 C4 C6 -53.51(18) . . . . ?
C1 N1 C4 C7 -110.70(15) . . . . ?
C2 N1 C4 C7 68.63(16) . . . . ?
C1 N2 C10 C11 12.7(2) . . . . ?
C3 N2 C10 C11 -167.44(14) . . . . ?
C1 N2 C10 C12 -108.45(15) . . . . ?
C3 N2 C10 C12 71.37(16) . . . . ?
C1 N2 C10 C13 130.36(15) . . . . ?
C3 N2 C10 C13 -49.82(17) . . . . ?
N1 C1 C14 C15 -84.60(16) . . . . ?
N2 C1 C14 C15 86.34(16) . . . . ?
N1 C1 C14 C18 97.20(15) . . . . ?
N2 C1 C14 C18 -91.86(15) . . . . ?
C18 C14 C15 C16 169.37(13) . . . . ?
C1 C14 C15 C16 -8.59(18) . . . . ?
C18 C14 C15 Si -16.7(2) . . . . ?
C1 C14 C15 Si 165.37(10) . . . . ?
C30 Si C15 C14 -30.29(16) . . . . ?
C31 Si C15 C14 95.49(15) . . . . ?
C32 Si C15 C14 -147.87(14) . . . . ?
C30 Si C15 C16 143.95(10) . . . . ?
C31 Si C15 C16 -90.26(11) . . . . ?
C32 Si C15 C16 26.38(12) . . . . ?
C14 C15 C16 C17 -123.3(16) . . . . ?
Si C15 C16 C17 61.5(16) . . . . ?
C15 C16 C17 C24 6(4) . . . . ?
C15 C14 C18 C23 158.86(14) . . . . ?
C1 C14 C18 C23 -23.22(18) . . . . ?
C15 C14 C18 C19 -28.0(2) . . . . ?
C1 C14 C18 C19 149.92(13) . . . . ?
C23 C18 C19 C20 -0.2(2) . . . . ?
C14 C18 C19 C20 -173.54(14) . . . . ?
C18 C19 C20 C21 -0.4(2) . . . . ?
C19 C20 C21 C22 0.2(2) . . . . ?
C20 C21 C22 C23 0.7(2) . . . . ?
C21 C22 C23 C18 -1.4(2) . . . . ?
C19 C18 C23 C22 1.1(2) . . . . ?
C14 C18 C23 C22 174.49(13) . . . . ?
C16 C17 C24 C29 144(3) . . . . ?
C16 C17 C24 C25 -35(3) . . . . ?
C29 C24 C25 C26 0.9(2) . . . . ?
C17 C24 C25 C26 179.76(14) . . . . ?
C24 C25 C26 C27 -0.1(2) . . . . ?
C25 C26 C27 C28 -0.3(3) . . . . ?
C26 C27 C28 C29 0.0(2) . . . . ?
C27 C28 C29 C24 0.8(2) . . . . ?
C25 C24 C29 C28 -1.3(2) . . . . ?
C17 C24 C29 C28 179.91(14) . . . . ?
O3 S C33 F2 54.94(17) . . . . ?
O2 S C33 F2 -65.20(17) . . . . ?
O1 S C33 F2 174.55(16) . . . . ?
O3 S C33 F1 175.88(15) . . . . ?
O2 S C33 F1 55.75(18) . . . . ?
O1 S C33 F1 -64.51(17) . . . . ?
O3 S C33 F3 -64.97(15) . . . . ?
O2 S C33 F3 174.90(14) . . . . ?
O1 S C33 F3 54.64(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.037
_refine_instructions_details     
;
TITL MSV05 in P2(1)
CELL 1.54184   9.000584  13.476861  14.122296  90.0000  99.1372  90.0000
ZERR    2.00   0.000200   0.000200   0.000200   0.0000   0.0020   0.0000
LATT  -1
SYMM  - X, 1/2 + Y, - Z
SFAC  C    H    N    O    F    SI   S
UNIT  66   86   4    6    6    2    2
MERG   2
FMAP   2
 
ACTA 150
CONF
 
OMIT    -6  -3  16
 
TEMP -173
 
PLAN   10
L.S.   4
 
WGHT    0.047400    0.305700
FVAR       5.74649
SI    6    0.383229    0.504688    0.479605    11.00000    0.02290    0.02470 =
         0.01902    0.00173    0.00436   -0.00280
N1    3    0.455734    0.653104    0.165353    11.00000    0.01503    0.01951 =
         0.02297    0.00279    0.00343   -0.00073
N2    3    0.634076    0.539784    0.175034    11.00000    0.01672    0.02179 =
         0.02075   -0.00118    0.00417    0.00050
C1    1    0.500135    0.563313    0.202331    11.00000    0.01633    0.01877 =
         0.01796   -0.00128    0.00259   -0.00186
C2    1    0.565883    0.687400    0.113921    11.00000    0.01912    0.02903 =
         0.03005    0.00973    0.00466   -0.00289
C3    1    0.676856    0.618919    0.121855    11.00000    0.01896    0.02972 =
         0.02471    0.00271    0.00506   -0.00373
C4    1    0.313007    0.713069    0.172713    11.00000    0.01747    0.01809 =
         0.02849   -0.00015    0.00194    0.00291
C5    1    0.217063    0.670702    0.242917    11.00000    0.02571    0.03343 =
         0.02786    0.00324    0.00960    0.01107
AFIX 137
H5A   2    0.274330    0.672352    0.307996    11.00000   -1.50000
H5B   2    0.189752    0.601999    0.225264    11.00000   -1.50000
H5C   2    0.125462    0.710535    0.240596    11.00000   -1.50000
AFIX   0
C6    1    0.361451    0.816592    0.208948    11.00000    0.03363    0.02431 =
         0.07163   -0.01455   -0.00310    0.00037
AFIX 137
H6A   2    0.402042    0.852924    0.158641    11.00000   -1.50000
H6B   2    0.439040    0.811018    0.265827    11.00000   -1.50000
H6C   2    0.274388    0.852331    0.225652    11.00000   -1.50000
AFIX   0
C7    1    0.216045    0.714237    0.073226    11.00000    0.02182    0.03301 =
         0.02661    0.00602    0.00270    0.00499
AFIX 137
H7A   2    0.136953    0.764455    0.071700    11.00000   -1.50000
H7B   2    0.169955    0.648855    0.059539    11.00000   -1.50000
H7C   2    0.279195    0.730148    0.024790    11.00000   -1.50000
AFIX   0
C8    1    0.567492    0.780506    0.056541    11.00000    0.02717    0.04467 =
         0.06358    0.03252    0.01034   -0.00076
AFIX 137
H8A   2    0.629606    0.830502    0.094631    11.00000   -1.50000
H8B   2    0.464531    0.805580    0.039373    11.00000   -1.50000
H8C   2    0.609393    0.766467   -0.001995    11.00000   -1.50000
AFIX   0
C9    1    0.819384    0.632280    0.080866    11.00000    0.02302    0.04444 =
         0.03762    0.00870    0.01171    0.00021
AFIX 137
H9A   2    0.804428    0.608284    0.014525    11.00000   -1.50000
H9B   2    0.900590    0.594501    0.119162    11.00000   -1.50000
H9C   2    0.846273    0.702786    0.082126    11.00000   -1.50000
AFIX   0
C10   1    0.729394    0.446663    0.195104    11.00000    0.01733    0.02271 =
         0.03363   -0.00552    0.00152    0.00407
C11   1    0.646338    0.361924    0.234997    11.00000    0.02536    0.01992 =
         0.06492    0.00139    0.00745    0.00466
AFIX 137
H11A  2    0.554794    0.346299    0.190025    11.00000   -1.50000
H11B  2    0.619263    0.381603    0.296853    11.00000   -1.50000
H11C  2    0.711452    0.303282    0.243814    11.00000   -1.50000
AFIX   0
C12   1    0.869765    0.471672    0.266911    11.00000    0.02012    0.02892 =
         0.03192   -0.00326   -0.00106    0.00438
AFIX 137
H12A  2    0.940774    0.416132    0.270959    11.00000   -1.50000
H12B  2    0.841400    0.483539    0.330136    11.00000   -1.50000
H12C  2    0.917218    0.531399    0.245727    11.00000   -1.50000
AFIX   0
C13   1    0.768765    0.411555    0.098717    11.00000    0.02892    0.04282 =
         0.03924   -0.01897   -0.00003    0.00907
AFIX 137
H13A  2    0.679020    0.415286    0.049462    11.00000   -1.50000
H13B  2    0.804637    0.342839    0.104763    11.00000   -1.50000
H13C  2    0.847778    0.454123    0.080381    11.00000   -1.50000
AFIX   0
C14   1    0.424794    0.506661    0.272408    11.00000    0.01718    0.01702 =
         0.02107    0.00165    0.00422    0.00022
C15   1    0.468983    0.532147    0.366190    11.00000    0.01959    0.01913 =
         0.02155    0.00185    0.00302    0.00007
C16   1    0.594400    0.598081    0.387119    11.00000    0.02274    0.02289 =
         0.01848    0.00027    0.00435    0.00014
C17   1    0.705978    0.647888    0.409849    11.00000    0.02254    0.02415 =
         0.02211   -0.00323    0.00545   -0.00170
C18   1    0.316625    0.428919    0.232816    11.00000    0.01813    0.02004 =
         0.02270   -0.00016    0.00551   -0.00117
C19   1    0.293013    0.344074    0.286199    11.00000    0.02887    0.02240 =
         0.02288    0.00153    0.00424   -0.00249
AFIX  43
H19   2    0.339519    0.339393    0.351311    11.00000   -1.20000
AFIX   0
C20   1    0.202762    0.266991    0.245233    11.00000    0.03200    0.02288 =
         0.03027    0.00084    0.01019   -0.00658
AFIX  43
H20   2    0.188606    0.209965    0.282327    11.00000   -1.20000
AFIX   0
C21   1    0.132763    0.272667    0.150063    11.00000    0.02378    0.02337 =
         0.03173   -0.00819    0.00890   -0.00578
AFIX  43
H21   2    0.070771    0.219871    0.122224    11.00000   -1.20000
AFIX   0
C22   1    0.154356    0.356184    0.096182    11.00000    0.02013    0.02630 =
         0.02521   -0.00517    0.00514   -0.00136
AFIX  43
H22   2    0.106095    0.360898    0.031442    11.00000   -1.20000
AFIX   0
C23   1    0.246458    0.432891    0.136811    11.00000    0.01943    0.02013 =
         0.02188   -0.00123    0.00522    0.00012
AFIX  43
H23   2    0.262138    0.488985    0.098872    11.00000   -1.20000
AFIX   0
C24   1    0.841945    0.702298    0.439740    11.00000    0.01949    0.02240 =
         0.02734   -0.00756    0.00575   -0.00113
C25   1    0.923447    0.685083    0.531358    11.00000    0.02423    0.02789 =
         0.02803   -0.00543    0.00482   -0.00175
AFIX  43
H25   2    0.888190    0.638095    0.572761    11.00000   -1.20000
AFIX   0
C26   1    1.055909    0.736924    0.561436    11.00000    0.02375    0.03828 =
         0.03389   -0.01048   -0.00060   -0.00076
AFIX  43
H26   2    1.111075    0.725356    0.623573    11.00000   -1.20000
AFIX   0
C27   1    1.107851    0.805189    0.501507    11.00000    0.02111    0.03609 =
         0.04549   -0.01585    0.00763   -0.00606
AFIX  43
H27   2    1.198273    0.840587    0.522774    11.00000   -1.20000
AFIX   0
C28   1    1.028333    0.822453    0.409964    11.00000    0.02930    0.02847 =
         0.03999   -0.00809    0.01569   -0.00699
AFIX  43
H28   2    1.064451    0.869493    0.368971    11.00000   -1.20000
AFIX   0
C29   1    0.895953    0.770596    0.378828    11.00000    0.02609    0.02747 =
         0.02822   -0.00517    0.00772   -0.00171
AFIX  43
H29   2    0.842223    0.781571    0.316185    11.00000   -1.20000
AFIX   0
C30   1    0.175223    0.492627    0.452442    11.00000    0.02602    0.03781 =
         0.03001   -0.00138    0.00761   -0.00420
AFIX 137
H30A  2    0.134070    0.488452    0.512534    11.00000   -1.50000
H30B  2    0.148924    0.432414    0.414568    11.00000   -1.50000
H30C  2    0.132937    0.550651    0.415892    11.00000   -1.50000
AFIX   0
C31   1    0.473394    0.393713    0.543163    11.00000    0.04054    0.03683 =
         0.02799    0.00931    0.00472    0.00257
AFIX 137
H31A  2    0.427684    0.380730    0.600461    11.00000   -1.50000
H31B  2    0.581360    0.405957    0.562062    11.00000   -1.50000
H31C  2    0.458576    0.336067    0.500404    11.00000   -1.50000
AFIX   0
C32   1    0.429858    0.614953    0.559039    11.00000    0.03547    0.03655 =
         0.02579   -0.00587    0.01063   -0.00738
AFIX 137
H32A  2    0.395612    0.675462    0.523686    11.00000   -1.50000
H32B  2    0.538964    0.618231    0.579689    11.00000   -1.50000
H32C  2    0.379446    0.608982    0.615393    11.00000   -1.50000
AFIX   0
S     7    0.967633   -0.014956    0.164653    11.00000    0.04185    0.02443 =
         0.03000   -0.00078    0.01046   -0.00423
O1    4    0.996461    0.029672    0.076876    11.00000    0.05844    0.03731 =
         0.03986    0.00383    0.02104   -0.00695
O2    4    1.061726    0.018762    0.250479    11.00000    0.07327    0.04367 =
         0.04341   -0.00315   -0.00335   -0.01680
O3    4    0.940045   -0.120024    0.159754    11.00000    0.04426    0.02284 =
         0.03802   -0.00116    0.00991    0.00055
C33   1    0.784124    0.035843    0.176240    11.00000    0.06134    0.02860 =
         0.05369   -0.00517    0.02514    0.00670
F1    5    0.790339    0.134259    0.188267    11.00000    0.10513    0.02852 =
         0.09009   -0.01397    0.03455    0.01371
F2    5    0.729375   -0.002903    0.249555    11.00000    0.09798    0.06653 =
         0.08068    0.00550    0.06621    0.01275
F3    5    0.681890    0.018211    0.096774    11.00000    0.04886    0.04709 =
         0.08267    0.00081    0.00893    0.00869
 
HKLF    4
;
####################################################################### 
# 
# 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_eileen62
_database_code_depnum_ccdc_archive 'CCDC 1052448'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35.50 H43 Au F3 N2 O3 P S'
_chemical_formula_weight         862.72

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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   9.2711(5)
_cell_length_b                   16.7779(8)
_cell_length_c                   22.7298(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.201(4)
_cell_angle_gamma                90.00
_cell_volume                     3514.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8282
_cell_measurement_theta_min      2.4240
_cell_measurement_theta_max      24.4730

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1724
_exptl_absorpt_coefficient_mu    4.344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            93410
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         30.90
_reflns_number_total             10522
_reflns_number_gt                8019
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

# 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 0.000 149 55 ' '
2 0.500 0.500 0.500 149 55 ' '
_platon_squeeze_details          
;
A badly resolved rigion of residual electron density around the inversion 
centre 0.5, 0.5, 0.5 was tentatively identified as half a disordered 
molecule of toluene but could not be refined satisfactorily. For this 
reason the program SQEEZE (part of the PLATON suite, A. Spek, University 
of Utrecht, Metherlands, 2009) was used to remove mathematically the 
effects of the solvent. Derived parameters such as the formular weight 
correspond two molecules of toluene per cell.
;

_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)+(0.0191P)²+0.3978P] 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         10522
_refine_ls_number_parameters     396
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0671
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_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
Au Au 0.917743(17) 0.521774(9) 0.810612(6) 0.01291(4) Uani 1 1 d . . .
P P 0.85172(11) 0.60973(6) 0.73622(4) 0.0124(2) Uani 1 1 d . . .
N1 N 0.8811(4) 0.4281(2) 0.92321(14) 0.0162(7) Uani 1 1 d . . .
N2 N 1.0667(3) 0.38327(19) 0.88227(13) 0.0135(7) Uani 1 1 d . . .
C1 C 0.9645(4) 0.4419(2) 0.87900(15) 0.0121(8) Uani 1 1 d . . .
C2 C 0.9246(5) 0.3567(3) 0.95136(19) 0.0233(10) Uani 1 1 d . . .
C3 C 1.0413(5) 0.3298(2) 0.92679(18) 0.0189(9) Uani 1 1 d . . .
C4 C 0.7605(5) 0.4843(3) 0.93816(17) 0.0194(9) Uani 1 1 d . . .
C5 C 0.8075(6) 0.5706(3) 0.9317(2) 0.0387(13) Uani 1 1 d . . .
H5A H 0.7351 0.6062 0.9461 0.058 Uiso 1 1 calc R . .
H5B H 0.8159 0.5821 0.8899 0.058 Uiso 1 1 calc R . .
H5C H 0.9016 0.5791 0.9549 0.058 Uiso 1 1 calc R . .
C6 C 0.6256(5) 0.4657(4) 0.8969(2) 0.0527(18) Uani 1 1 d . . .
H6A H 0.5952 0.4108 0.9033 0.079 Uiso 1 1 calc R . .
H6B H 0.6466 0.4720 0.8558 0.079 Uiso 1 1 calc R . .
H6C H 0.5477 0.5024 0.9048 0.079 Uiso 1 1 calc R . .
C7 C 0.7313(6) 0.4763(3) 1.00280(19) 0.0352(12) Uani 1 1 d . . .
H7A H 0.6838 0.4252 1.0085 0.053 Uiso 1 1 calc R . .
H7B H 0.6680 0.5199 1.0129 0.053 Uiso 1 1 calc R . .
H7C H 0.8232 0.4789 1.0284 0.053 Uiso 1 1 calc R . .
C8 C 0.8462(6) 0.3141(3) 0.9971(2) 0.0471(16) Uani 1 1 d . . .
H8A H 0.8784 0.2585 1.0002 0.071 Uiso 1 1 calc R . .
H8B H 0.7414 0.3158 0.9853 0.071 Uiso 1 1 calc R . .
H8C H 0.8680 0.3403 1.0356 0.071 Uiso 1 1 calc R . .
C9 C 1.1263(5) 0.2569(3) 0.9462(2) 0.0319(12) Uani 1 1 d . . .
H9A H 1.0822 0.2311 0.9786 0.048 Uiso 1 1 calc R . .
H9B H 1.2264 0.2721 0.9599 0.048 Uiso 1 1 calc R . .
H9C H 1.1260 0.2199 0.9129 0.048 Uiso 1 1 calc R . .
C10 C 1.1775(4) 0.3774(2) 0.83767(17) 0.0151(8) Uani 1 1 d . . .
C11 C 1.2446(5) 0.4586(2) 0.82798(18) 0.0205(10) Uani 1 1 d . . .
H11A H 1.1718 0.4934 0.8066 0.031 Uiso 1 1 calc R . .
H11B H 1.3269 0.4522 0.8048 0.031 Uiso 1 1 calc R . .
H11C H 1.2782 0.4826 0.8664 0.031 Uiso 1 1 calc R . .
C12 C 1.1001(5) 0.3435(3) 0.78044(18) 0.0256(10) Uani 1 1 d . . .
H12A H 1.0641 0.2899 0.7879 0.038 Uiso 1 1 calc R . .
H12B H 1.1682 0.3406 0.7504 0.038 Uiso 1 1 calc R . .
H12C H 1.0185 0.3780 0.7663 0.038 Uiso 1 1 calc R . .
C13 C 1.3039(5) 0.3224(3) 0.8597(2) 0.0277(11) Uani 1 1 d . . .
H13A H 1.3425 0.3380 0.8999 0.042 Uiso 1 1 calc R . .
H13B H 1.3805 0.3268 0.8334 0.042 Uiso 1 1 calc R . .
H13C H 1.2695 0.2672 0.8600 0.042 Uiso 1 1 calc R . .
C14 C 0.6565(4) 0.6079(2) 0.71600(16) 0.0126(8) Uani 1 1 d . . .
C15 C 0.5962(4) 0.5887(2) 0.65918(17) 0.0172(9) Uani 1 1 d . . .
H15 H 0.6570 0.5795 0.6288 0.021 Uiso 1 1 calc R . .
C16 C 0.4472(5) 0.5831(3) 0.64710(18) 0.0207(10) Uani 1 1 d . . .
H16 H 0.4058 0.5693 0.6084 0.025 Uiso 1 1 calc R . .
C17 C 0.3580(5) 0.5975(2) 0.69074(18) 0.0195(9) Uani 1 1 d . . .
H17 H 0.2557 0.5939 0.6819 0.023 Uiso 1 1 calc R . .
C18 C 0.4171(4) 0.6171(2) 0.74726(18) 0.0180(9) Uani 1 1 d . . .
H18 H 0.3554 0.6276 0.7771 0.022 Uiso 1 1 calc R . .
C19 C 0.5658(4) 0.6215(2) 0.76043(17) 0.0158(9) Uani 1 1 d . . .
H19 H 0.6065 0.6337 0.7995 0.019 Uiso 1 1 calc R . .
C20 C 0.8986(4) 0.7111(2) 0.75812(16) 0.0141(8) Uani 1 1 d . . .
C21 C 0.8149(5) 0.7761(2) 0.73835(17) 0.0186(9) Uani 1 1 d . . .
H21 H 0.7276 0.7680 0.7131 0.022 Uiso 1 1 calc R . .
C22 C 0.8570(5) 0.8526(3) 0.75497(19) 0.0239(10) Uani 1 1 d . . .
H22 H 0.7989 0.8967 0.7409 0.029 Uiso 1 1 calc R . .
C23 C 0.9832(5) 0.8651(3) 0.7919(2) 0.0289(11) Uani 1 1 d . . .
H23 H 1.0119 0.9177 0.8034 0.035 Uiso 1 1 calc R . .
C24 C 1.0679(5) 0.8005(3) 0.81229(19) 0.0265(11) Uani 1 1 d . . .
H24 H 1.1552 0.8089 0.8375 0.032 Uiso 1 1 calc R . .
C25 C 1.0257(5) 0.7243(3) 0.79599(17) 0.0187(9) Uani 1 1 d . . .
H25 H 1.0833 0.6803 0.8106 0.022 Uiso 1 1 calc R . .
C26 C 0.9336(4) 0.5926(2) 0.66827(16) 0.0125(8) Uani 1 1 d . . .
C27 C 0.9490(4) 0.6546(3) 0.62858(16) 0.0183(9) Uani 1 1 d . . .
H27 H 0.9162 0.7067 0.6368 0.022 Uiso 1 1 calc R . .
C28 C 1.0119(5) 0.6402(3) 0.57723(18) 0.0260(11) Uani 1 1 d . . .
H28 H 1.0219 0.6825 0.5502 0.031 Uiso 1 1 calc R . .
C29 C 1.0601(5) 0.5652(3) 0.56500(17) 0.0227(10) Uani 1 1 d . . .
H29 H 1.1040 0.5562 0.5297 0.027 Uiso 1 1 calc R . .
C30 C 1.0452(5) 0.5027(3) 0.60366(18) 0.0218(10) Uani 1 1 d . . .
H30 H 1.0782 0.4508 0.5950 0.026 Uiso 1 1 calc R . .
C31 C 0.9813(4) 0.5169(2) 0.65529(17) 0.0158(8) Uani 1 1 d . . .
H31 H 0.9703 0.4743 0.6819 0.019 Uiso 1 1 calc R . .
S S 0.46464(12) 0.72732(7) 0.92386(4) 0.0206(2) Uani 1 1 d . . .
O1 O 0.5283(3) 0.70003(18) 0.98106(12) 0.0260(7) Uani 1 1 d . . .
O2 O 0.4322(4) 0.6657(2) 0.88111(13) 0.0413(10) Uani 1 1 d . . .
O3 O 0.3565(4) 0.7887(2) 0.92574(14) 0.0378(9) Uani 1 1 d . . .
C32 C 0.6124(5) 0.7826(3) 0.89576(19) 0.0227(10) Uani 1 1 d . . .
F1 F 0.7276(3) 0.73761(16) 0.88911(12) 0.0360(7) Uani 1 1 d . . .
F2 F 0.6569(3) 0.84175(16) 0.93264(12) 0.0398(7) Uani 1 1 d . . .
F3 F 0.5698(3) 0.81574(17) 0.84334(11) 0.0373(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
Au C1 2.063(4) . ?
Au P 2.2777(10) . ?
P C20 1.812(4) . ?
P C26 1.816(4) . ?
P C14 1.818(4) . ?
N1 C1 1.353(5) . ?
N1 C2 1.397(5) . ?
N1 C4 1.529(5) . ?
N2 C1 1.362(5) . ?
N2 C3 1.391(5) . ?
N2 C10 1.522(5) . ?
C2 C3 1.347(6) . ?
C2 C8 1.511(6) . ?
C3 C9 1.495(6) . ?
C4 C6 1.513(6) . ?
C4 C5 1.524(6) . ?
C4 C7 1.529(5) . ?
C10 C11 1.524(5) . ?
C10 C12 1.526(6) . ?
C10 C13 1.533(5) . ?
C14 C15 1.389(5) . ?
C14 C19 1.401(5) . ?
C15 C16 1.383(6) . ?
C16 C17 1.379(5) . ?
C17 C18 1.381(5) . ?
C18 C19 1.381(5) . ?
C20 C21 1.385(5) . ?
C20 C25 1.399(5) . ?
C21 C22 1.382(6) . ?
C22 C23 1.381(6) . ?
C23 C24 1.389(6) . ?
C24 C25 1.377(6) . ?
C26 C31 1.388(5) . ?
C26 C27 1.394(5) . ?
C27 C28 1.381(5) . ?
C28 C29 1.373(6) . ?
C29 C30 1.385(6) . ?
C30 C31 1.391(5) . ?
S O2 1.429(3) . ?
S O3 1.441(3) . ?
S O1 1.443(3) . ?
S C32 1.825(5) . ?
C32 F1 1.330(5) . ?
C32 F3 1.336(5) . ?
C32 F2 1.336(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au P 176.52(11) . . ?
C20 P C26 105.79(18) . . ?
C20 P C14 106.75(18) . . ?
C26 P C14 106.17(18) . . ?
C20 P Au 111.52(13) . . ?
C26 P Au 115.17(13) . . ?
C14 P Au 110.91(13) . . ?
C1 N1 C2 109.1(3) . . ?
C1 N1 C4 123.4(3) . . ?
C2 N1 C4 127.6(3) . . ?
C1 N2 C3 109.5(3) . . ?
C1 N2 C10 121.7(3) . . ?
C3 N2 C10 128.5(3) . . ?
N1 C1 N2 106.6(3) . . ?
N1 C1 Au 125.5(3) . . ?
N2 C1 Au 126.8(3) . . ?
C3 C2 N1 107.6(4) . . ?
C3 C2 C8 126.5(4) . . ?
N1 C2 C8 125.7(4) . . ?
C2 C3 N2 107.0(4) . . ?
C2 C3 C9 124.9(4) . . ?
N2 C3 C9 128.1(4) . . ?
C6 C4 C5 111.2(4) . . ?
C6 C4 N1 108.1(3) . . ?
C5 C4 N1 110.0(3) . . ?
C6 C4 C7 110.9(4) . . ?
C5 C4 C7 105.0(4) . . ?
N1 C4 C7 111.7(3) . . ?
N2 C10 C11 110.7(3) . . ?
N2 C10 C12 107.7(3) . . ?
C11 C10 C12 111.8(3) . . ?
N2 C10 C13 111.6(3) . . ?
C11 C10 C13 106.0(3) . . ?
C12 C10 C13 109.0(3) . . ?
C15 C14 C19 119.7(4) . . ?
C15 C14 P 121.9(3) . . ?
C19 C14 P 118.3(3) . . ?
C16 C15 C14 119.6(4) . . ?
C17 C16 C15 120.6(4) . . ?
C16 C17 C18 120.2(4) . . ?
C19 C18 C17 120.1(4) . . ?
C18 C19 C14 119.9(4) . . ?
C21 C20 C25 118.7(4) . . ?
C21 C20 P 122.7(3) . . ?
C25 C20 P 118.6(3) . . ?
C22 C21 C20 120.7(4) . . ?
C23 C22 C21 120.3(4) . . ?
C22 C23 C24 119.7(4) . . ?
C25 C24 C23 120.1(4) . . ?
C24 C25 C20 120.6(4) . . ?
C31 C26 C27 119.2(4) . . ?
C31 C26 P 119.9(3) . . ?
C27 C26 P 120.9(3) . . ?
C28 C27 C26 119.9(4) . . ?
C29 C28 C27 120.5(4) . . ?
C28 C29 C30 120.6(4) . . ?
C29 C30 C31 119.1(4) . . ?
C26 C31 C30 120.7(4) . . ?
O2 S O3 116.2(2) . . ?
O2 S O1 114.8(2) . . ?
O3 S O1 114.71(19) . . ?
O2 S C32 103.9(2) . . ?
O3 S C32 101.4(2) . . ?
O1 S C32 103.1(2) . . ?
F1 C32 F3 107.4(3) . . ?
F1 C32 F2 107.2(4) . . ?
F3 C32 F2 106.9(4) . . ?
F1 C32 S 113.2(3) . . ?
F3 C32 S 111.3(3) . . ?
F2 C32 S 110.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Au P C20 102.4(18) . . . . ?
C1 Au P C26 -137.1(18) . . . . ?
C1 Au P C14 -16.5(18) . . . . ?
C2 N1 C1 N2 -4.7(4) . . . . ?
C4 N1 C1 N2 174.9(3) . . . . ?
C2 N1 C1 Au 163.9(3) . . . . ?
C4 N1 C1 Au -16.5(5) . . . . ?
C3 N2 C1 N1 3.5(4) . . . . ?
C10 N2 C1 N1 177.6(3) . . . . ?
C3 N2 C1 Au -164.9(3) . . . . ?
C10 N2 C1 Au 9.2(5) . . . . ?
P Au C1 N1 -20(2) . . . . ?
P Au C1 N2 145.9(16) . . . . ?
C1 N1 C2 C3 4.1(5) . . . . ?
C4 N1 C2 C3 -175.4(4) . . . . ?
C1 N1 C2 C8 -170.9(4) . . . . ?
C4 N1 C2 C8 9.6(7) . . . . ?
N1 C2 C3 N2 -1.9(5) . . . . ?
C8 C2 C3 N2 173.1(5) . . . . ?
N1 C2 C3 C9 176.8(4) . . . . ?
C8 C2 C3 C9 -8.3(8) . . . . ?
C1 N2 C3 C2 -1.0(5) . . . . ?
C10 N2 C3 C2 -174.6(4) . . . . ?
C1 N2 C3 C9 -179.6(4) . . . . ?
C10 N2 C3 C9 6.9(7) . . . . ?
C1 N1 C4 C6 83.1(5) . . . . ?
C2 N1 C4 C6 -97.4(5) . . . . ?
C1 N1 C4 C5 -38.4(5) . . . . ?
C2 N1 C4 C5 141.0(4) . . . . ?
C1 N1 C4 C7 -154.6(4) . . . . ?
C2 N1 C4 C7 24.9(6) . . . . ?
C1 N2 C10 C11 46.6(5) . . . . ?
C3 N2 C10 C11 -140.6(4) . . . . ?
C1 N2 C10 C12 -76.0(4) . . . . ?
C3 N2 C10 C12 96.9(5) . . . . ?
C1 N2 C10 C13 164.4(4) . . . . ?
C3 N2 C10 C13 -22.7(6) . . . . ?
C20 P C14 C15 118.0(3) . . . . ?
C26 P C14 C15 5.5(4) . . . . ?
Au P C14 C15 -120.3(3) . . . . ?
C20 P C14 C19 -66.0(3) . . . . ?
C26 P C14 C19 -178.6(3) . . . . ?
Au P C14 C19 55.6(3) . . . . ?
C19 C14 C15 C16 -0.1(6) . . . . ?
P C14 C15 C16 175.8(3) . . . . ?
C14 C15 C16 C17 0.9(6) . . . . ?
C15 C16 C17 C18 -0.4(7) . . . . ?
C16 C17 C18 C19 -0.8(6) . . . . ?
C17 C18 C19 C14 1.6(6) . . . . ?
C15 C14 C19 C18 -1.1(6) . . . . ?
P C14 C19 C18 -177.2(3) . . . . ?
C26 P C20 C21 88.1(4) . . . . ?
C14 P C20 C21 -24.7(4) . . . . ?
Au P C20 C21 -146.0(3) . . . . ?
C26 P C20 C25 -91.1(3) . . . . ?
C14 P C20 C25 156.1(3) . . . . ?
Au P C20 C25 34.8(3) . . . . ?
C25 C20 C21 C22 1.0(6) . . . . ?
P C20 C21 C22 -178.2(3) . . . . ?
C20 C21 C22 C23 -0.4(6) . . . . ?
C21 C22 C23 C24 0.1(7) . . . . ?
C22 C23 C24 C25 -0.4(7) . . . . ?
C23 C24 C25 C20 1.0(6) . . . . ?
C21 C20 C25 C24 -1.3(6) . . . . ?
P C20 C25 C24 178.0(3) . . . . ?
C20 P C26 C31 148.3(3) . . . . ?
C14 P C26 C31 -98.5(3) . . . . ?
Au P C26 C31 24.6(4) . . . . ?
C20 P C26 C27 -32.0(4) . . . . ?
C14 P C26 C27 81.2(4) . . . . ?
Au P C26 C27 -155.6(3) . . . . ?
C31 C26 C27 C28 -0.4(6) . . . . ?
P C26 C27 C28 179.9(3) . . . . ?
C26 C27 C28 C29 -0.2(7) . . . . ?
C27 C28 C29 C30 0.6(7) . . . . ?
C28 C29 C30 C31 -0.3(6) . . . . ?
C27 C26 C31 C30 0.7(6) . . . . ?
P C26 C31 C30 -179.6(3) . . . . ?
C29 C30 C31 C26 -0.3(6) . . . . ?
O2 S C32 F1 -58.2(4) . . . . ?
O3 S C32 F1 -179.1(3) . . . . ?
O1 S C32 F1 61.8(3) . . . . ?
O2 S C32 F3 62.9(4) . . . . ?
O3 S C32 F3 -58.1(3) . . . . ?
O1 S C32 F3 -177.1(3) . . . . ?
O2 S C32 F2 -178.5(3) . . . . ?
O3 S C32 F2 60.6(3) . . . . ?
O1 S C32 F2 -58.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.195
_refine_instructions_details     
;
CELL 0.71073   9.271150  16.777888  22.729799  90.0000  96.2013  90.0000
ZERR    4.00   0.000500   0.000800   0.001000   0.0000   0.0040   0.0000
LATT   1
SYMM  1/2 - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    F    P    S    AU
UNIT  142  172  8  12  12  4  4  4
MERG   2
FMAP   2
 
ACTA 60
CONF
 
OMIT -1 2 8
 
TEMP -173
 
PLAN   10
L.S.   4
WGHT    0.019100    0.397800
FVAR      19.60560
AU    8    0.917743    0.521774    0.810612    11.00000    0.01251    0.01453 =
         0.01166    0.00116    0.00114    0.00161
P     6    0.851717    0.609728    0.736221    11.00000    0.01227    0.01444 =
         0.01057    0.00107    0.00220    0.00033
N1    3    0.881067    0.428069    0.923212    11.00000    0.01336    0.01891 =
         0.01623   -0.00144    0.00178    0.00105
N2    3    1.066681    0.383267    0.882272    11.00000    0.01093    0.01466 =
         0.01512    0.00159    0.00256    0.00069
C1    1    0.964533    0.441864    0.878996    11.00000    0.01293    0.01628 =
         0.00678   -0.00138    0.00024   -0.00273
C2    1    0.924629    0.356674    0.951356    11.00000    0.02043    0.02413 =
         0.02567    0.00934    0.00438    0.00205
C3    1    1.041272    0.329793    0.926792    11.00000    0.01766    0.01685 =
         0.02203    0.00657    0.00175   -0.00002
C4    1    0.760549    0.484318    0.938159    11.00000    0.01651    0.02519 =
         0.01722   -0.00329    0.00567    0.00262
C5    1    0.807477    0.570626    0.931680    11.00000    0.05607    0.02968 =
         0.03443    0.00400    0.02376    0.01798
AFIX 137
H5A   2    0.735110    0.606182    0.946069    11.00000   -1.50000
H5B   2    0.815927    0.582067    0.889911    11.00000   -1.50000
H5C   2    0.901575    0.579138    0.954892    11.00000   -1.50000
AFIX   0
C6    1    0.625641    0.465749    0.896886    11.00000    0.01711    0.08281 =
         0.05608   -0.03185   -0.00593    0.01288
AFIX 137
H6A   2    0.595211    0.410783    0.903321    11.00000   -1.50000
H6B   2    0.646578    0.472032    0.855792    11.00000   -1.50000
H6C   2    0.547731    0.502403    0.904803    11.00000   -1.50000
AFIX   0
C7    1    0.731256    0.476335    1.002800    11.00000    0.04656    0.03728 =
         0.02539    0.00479    0.02079    0.00659
AFIX 137
H7A   2    0.683794    0.425151    1.008524    11.00000   -1.50000
H7B   2    0.667953    0.519885    1.012918    11.00000   -1.50000
H7C   2    0.823241    0.478851    1.028398    11.00000   -1.50000
AFIX   0
C8    1    0.846228    0.314078    0.997118    11.00000    0.04581    0.03895 =
         0.06230    0.02809    0.03213    0.01119
AFIX 137
H8A   2    0.878415    0.258451    1.000152    11.00000   -1.50000
H8B   2    0.741443    0.315841    0.985303    11.00000   -1.50000
H8C   2    0.867992    0.340322    1.035571    11.00000   -1.50000
AFIX   0
C9    1    1.126305    0.256934    0.946211    11.00000    0.03645    0.02051 =
         0.04137    0.01451    0.01570    0.00704
AFIX 137
H9A   2    1.082206    0.231129    0.978565    11.00000   -1.50000
H9B   2    1.226417    0.272051    0.959919    11.00000   -1.50000
H9C   2    1.126028    0.219868    0.912878    11.00000   -1.50000
AFIX   0
C10   1    1.177466    0.377377    0.837669    11.00000    0.01326    0.01648 =
         0.01594    0.00038    0.00342    0.00378
C11   1    1.244567    0.458635    0.827983    11.00000    0.01418    0.02389 =
         0.02447    0.00397    0.00749    0.00014
AFIX 137
H11A  2    1.171756    0.493362    0.806605    11.00000   -1.50000
H11B  2    1.326926    0.452212    0.804758    11.00000   -1.50000
H11C  2    1.278158    0.482569    0.866358    11.00000   -1.50000
AFIX   0
C12   1    1.100149    0.343452    0.780444    11.00000    0.02443    0.02872 =
         0.02415   -0.00900    0.00499    0.00574
AFIX 137
H12A  2    1.064060    0.289879    0.787852    11.00000   -1.50000
H12B  2    1.168242    0.340649    0.750395    11.00000   -1.50000
H12C  2    1.018486    0.378040    0.766331    11.00000   -1.50000
AFIX   0
C13   1    1.303894    0.322377    0.859717    11.00000    0.01888    0.03020 =
         0.03498    0.00821    0.00731    0.00707
AFIX 137
H13A  2    1.342474    0.337964    0.899911    11.00000   -1.50000
H13B  2    1.380514    0.326849    0.833383    11.00000   -1.50000
H13C  2    1.269522    0.267154    0.859954    11.00000   -1.50000
AFIX   0
C14   1    0.656549    0.607882    0.716005    11.00000    0.01295    0.01058 =
         0.01341    0.00100   -0.00249    0.00228
C15   1    0.596217    0.588695    0.659175    11.00000    0.01490    0.02240 =
         0.01496   -0.00165    0.00444    0.00311
AFIX  43
H15   2    0.656984    0.579455    0.628790    11.00000   -1.20000
AFIX   0
C16   1    0.447156    0.583124    0.647097    11.00000    0.01938    0.02402 =
         0.01714   -0.00362   -0.00499    0.00319
AFIX  43
H16   2    0.405768    0.569278    0.608385    11.00000   -1.20000
AFIX   0
C17   1    0.358021    0.597486    0.690738    11.00000    0.01224    0.01937 =
         0.02589   -0.00257   -0.00280   -0.00166
AFIX  43
H17   2    0.255717    0.593869    0.681896    11.00000   -1.20000
AFIX   0
C18   1    0.417128    0.617115    0.747263    11.00000    0.01343    0.01990 =
         0.02186    0.00221    0.00771    0.00069
AFIX  43
H18   2    0.355420    0.627621    0.777111    11.00000   -1.20000
AFIX   0
C19   1    0.565819    0.621482    0.760431    11.00000    0.01470    0.01818 =
         0.01485   -0.00048    0.00287    0.00040
AFIX  43
H19   2    0.606539    0.633688    0.799548    11.00000   -1.20000
AFIX   0
C20   1    0.898642    0.711087    0.758119    11.00000    0.01758    0.01528 =
         0.00977   -0.00175    0.00314   -0.00356
C21   1    0.814861    0.776070    0.738346    11.00000    0.01871    0.02014 =
         0.01790   -0.00333    0.00648   -0.00011
AFIX  43
H21   2    0.727551    0.767981    0.713104    11.00000   -1.20000
AFIX   0
C22   1    0.856995    0.852577    0.754968    11.00000    0.02722    0.01783 =
         0.02808    0.00005    0.00977    0.00157
AFIX  43
H22   2    0.798909    0.896678    0.740902    11.00000   -1.20000
AFIX   0
C23   1    0.983179    0.865144    0.791935    11.00000    0.03550    0.02142 =
         0.03125   -0.00741    0.01098   -0.00782
AFIX  43
H23   2    1.011886    0.917746    0.803387    11.00000   -1.20000
AFIX   0
C24   1    1.067905    0.800522    0.812289    11.00000    0.02057    0.03169 =
         0.02698   -0.00732    0.00160   -0.00917
AFIX  43
H24   2    1.155154    0.808931    0.837503    11.00000   -1.20000
AFIX   0
C25   1    1.025671    0.724284    0.795987    11.00000    0.01772    0.02401 =
         0.01469   -0.00046    0.00264    0.00030
AFIX  43
H25   2    1.083269    0.680257    0.810575    11.00000   -1.20000
AFIX   0
C26   1    0.933615    0.592606    0.668273    11.00000    0.01389    0.01305 =
         0.01095    0.00170    0.00251   -0.00292
C27   1    0.948975    0.654612    0.628581    11.00000    0.02279    0.01871 =
         0.01384    0.00046    0.00442   -0.00267
AFIX  43
H27   2    0.916228    0.706666    0.636840    11.00000   -1.20000
AFIX   0
C28   1    1.011890    0.640211    0.577233    11.00000    0.02896    0.03300 =
         0.01629    0.00212    0.00353   -0.00961
AFIX  43
H28   2    1.021906    0.682494    0.550174    11.00000   -1.20000
AFIX   0
C29   1    1.060071    0.565246    0.564996    11.00000    0.02073    0.03308 =
         0.01530   -0.00742    0.00657   -0.01137
AFIX  43
H29   2    1.103984    0.556201    0.529713    11.00000   -1.20000
AFIX   0
C30   1    1.045191    0.502703    0.603659    11.00000    0.01838    0.02458 =
         0.02357   -0.00731    0.00704   -0.00240
AFIX  43
H30   2    1.078162    0.450825    0.595027    11.00000   -1.20000
AFIX   0
C31   1    0.981327    0.516880    0.655288    11.00000    0.01612    0.01569 =
         0.01599   -0.00029    0.00361   -0.00249
AFIX  43
H31   2    0.970254    0.474260    0.681947    11.00000   -1.20000
AFIX   0
S     7    0.464640    0.727318    0.923864    11.00000    0.02289    0.02421 =
         0.01574   -0.00037    0.00686    0.00186
O1    4    0.528277    0.700034    0.981064    11.00000    0.03185    0.02723 =
         0.01915    0.00512    0.00416    0.00196
O2    4    0.432158    0.665685    0.881115    11.00000    0.05611    0.04431 =
         0.02539   -0.01360    0.01283   -0.02283
O3    4    0.356493    0.788686    0.925743    11.00000    0.02831    0.04835 =
         0.03931    0.01572    0.01537    0.01745
C32   1    0.612365    0.782551    0.895761    11.00000    0.02462    0.02091 =
         0.02339    0.00368    0.00600    0.00369
F1    5    0.727608    0.737609    0.889114    11.00000    0.02936    0.03156 =
         0.05114    0.01244    0.02239    0.00937
F2    5    0.656914    0.841750    0.932641    11.00000    0.04994    0.02526 =
         0.04352   -0.00330    0.00210   -0.00967
F3    5    0.569791    0.815741    0.843336    11.00000    0.04307    0.04249 =
         0.02785    0.01931    0.01101    0.00673
 
HKLF    4
;
####################################################################### 
# 
# 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_msv03
_database_code_depnum_ccdc_archive 'CCDC 1052449'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H39 Au F6 N3 O4 P S2'
_chemical_formula_weight         947.73

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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   13.3594(4)
_cell_length_b                   14.4701(5)
_cell_length_c                   18.7666(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.246(3)
_cell_angle_gamma                90.00
_cell_volume                     3627.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11219
_cell_measurement_theta_min      2.3290
_cell_measurement_theta_max      23.4960

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    4.286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            122840
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         30.99
_reflns_number_total             10993
_reflns_number_gt                8155
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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)+(0.0170P)²+4.0713P] 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         10993
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0610
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.003
_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
Au Au 0.277916(10) 0.614573(10) 0.426251(7) 0.01245(4) Uani 1 1 d . . .
P P 0.16764(7) 0.53784(6) 0.35473(5) 0.01186(19) Uani 1 1 d . . .
N1 N 0.4813(2) 0.6669(2) 0.48877(15) 0.0123(6) Uani 1 1 d . . .
N2 N 0.3632(2) 0.6914(2) 0.56582(15) 0.0127(6) Uani 1 1 d . . .
C1 C 0.3806(2) 0.6721(2) 0.49607(18) 0.0121(7) Uani 1 1 d . . .
C2 C 0.5269(3) 0.6750(2) 0.55585(19) 0.0137(7) Uani 1 1 d . . .
C3 C 0.4534(3) 0.6901(2) 0.60359(19) 0.0140(7) Uani 1 1 d . . .
C4 C 0.5325(3) 0.6528(3) 0.41771(19) 0.0154(7) Uani 1 1 d . . .
C5 C 0.5395(3) 0.5489(3) 0.4041(2) 0.0240(9) Uani 1 1 d . . .
H5A H 0.5821 0.5204 0.4406 0.036 Uiso 1 1 calc R . .
H5B H 0.5685 0.5381 0.3570 0.036 Uiso 1 1 calc R . .
H5C H 0.4724 0.5217 0.4061 0.036 Uiso 1 1 calc R . .
C6 C 0.4744(3) 0.7015(3) 0.3585(2) 0.0220(9) Uani 1 1 d . . .
H6A H 0.4097 0.6708 0.3516 0.033 Uiso 1 1 calc R . .
H6B H 0.5128 0.6987 0.3142 0.033 Uiso 1 1 calc R . .
H6C H 0.4635 0.7662 0.3718 0.033 Uiso 1 1 calc R . .
C7 C 0.6376(3) 0.6953(3) 0.4177(2) 0.0282(10) Uani 1 1 d . . .
H7A H 0.6347 0.7579 0.4375 0.042 Uiso 1 1 calc R . .
H7B H 0.6627 0.6980 0.3687 0.042 Uiso 1 1 calc R . .
H7C H 0.6825 0.6572 0.4468 0.042 Uiso 1 1 calc R . .
C8 C 0.6351(3) 0.6610(3) 0.5727(2) 0.0218(9) Uani 1 1 d . . .
H8A H 0.6442 0.6571 0.6244 0.033 Uiso 1 1 calc R . .
H8B H 0.6739 0.7132 0.5541 0.033 Uiso 1 1 calc R . .
H8C H 0.6583 0.6036 0.5505 0.033 Uiso 1 1 calc R . .
C9 C 0.4654(3) 0.6967(3) 0.68271(19) 0.0207(8) Uani 1 1 d . . .
H9A H 0.5339 0.6797 0.6961 0.031 Uiso 1 1 calc R . .
H9B H 0.4181 0.6546 0.7058 0.031 Uiso 1 1 calc R . .
H9C H 0.4519 0.7602 0.6981 0.031 Uiso 1 1 calc R . .
C10 C 0.2599(3) 0.7118(3) 0.5944(2) 0.0156(8) Uani 1 1 d . . .
C11 C 0.2642(3) 0.7748(3) 0.6602(2) 0.0292(10) Uani 1 1 d . . .
H11A H 0.2886 0.7394 0.7013 0.044 Uiso 1 1 calc R . .
H11B H 0.1971 0.7986 0.6703 0.044 Uiso 1 1 calc R . .
H11C H 0.3097 0.8266 0.6510 0.044 Uiso 1 1 calc R . .
C12 C 0.2096(3) 0.6209(3) 0.6141(3) 0.0383(12) Uani 1 1 d . . .
H12A H 0.2018 0.5827 0.5714 0.057 Uiso 1 1 calc R . .
H12B H 0.1437 0.6335 0.6347 0.057 Uiso 1 1 calc R . .
H12C H 0.2511 0.5880 0.6491 0.057 Uiso 1 1 calc R . .
C13 C 0.1996(3) 0.7648(3) 0.5385(2) 0.0329(11) Uani 1 1 d . . .
H13A H 0.2381 0.8186 0.5225 0.049 Uiso 1 1 calc R . .
H13B H 0.1363 0.7856 0.5593 0.049 Uiso 1 1 calc R . .
H13C H 0.1857 0.7244 0.4977 0.049 Uiso 1 1 calc R . .
C14 C 0.1308(2) 0.4263(2) 0.39163(18) 0.0118(7) Uani 1 1 d . . .
C15 C 0.1022(3) 0.4219(3) 0.46276(19) 0.0176(8) Uani 1 1 d . . .
H15 H 0.0998 0.4766 0.4906 0.021 Uiso 1 1 calc R . .
C16 C 0.0774(3) 0.3377(3) 0.4930(2) 0.0208(8) Uani 1 1 d . . .
H16 H 0.0573 0.3348 0.5414 0.025 Uiso 1 1 calc R . .
C17 C 0.0817(3) 0.2577(3) 0.4527(2) 0.0192(8) Uani 1 1 d . . .
H17 H 0.0654 0.1999 0.4737 0.023 Uiso 1 1 calc R . .
C18 C 0.1096(3) 0.2616(3) 0.3821(2) 0.0179(8) Uani 1 1 d . . .
H18 H 0.1125 0.2066 0.3545 0.021 Uiso 1 1 calc R . .
C19 C 0.1335(3) 0.3457(3) 0.35123(19) 0.0168(8) Uani 1 1 d . . .
H19 H 0.1518 0.3483 0.3024 0.020 Uiso 1 1 calc R . .
C20 C 0.0531(3) 0.6015(2) 0.33896(18) 0.0128(7) Uani 1 1 d . . .
C21 C -0.0394(3) 0.5563(3) 0.33395(19) 0.0154(8) Uani 1 1 d . . .
H21 H -0.0432 0.4913 0.3402 0.018 Uiso 1 1 calc R . .
C22 C -0.1249(3) 0.6066(3) 0.3199(2) 0.0186(8) Uani 1 1 d . . .
H22 H -0.1878 0.5760 0.3176 0.022 Uiso 1 1 calc R . .
C23 C -0.1202(3) 0.7007(3) 0.3093(2) 0.0189(8) Uani 1 1 d . . .
H23 H -0.1795 0.7346 0.2991 0.023 Uiso 1 1 calc R . .
C24 C -0.0288(3) 0.7459(3) 0.3136(2) 0.0177(8) Uani 1 1 d . . .
H24 H -0.0254 0.8108 0.3065 0.021 Uiso 1 1 calc R . .
C25 C 0.0576(3) 0.6965(3) 0.32827(19) 0.0160(8) Uani 1 1 d . . .
H25 H 0.1202 0.7275 0.3310 0.019 Uiso 1 1 calc R . .
C26 C 0.2155(3) 0.5093(2) 0.26699(19) 0.0135(7) Uani 1 1 d . . .
C27 C 0.3176(3) 0.4924(3) 0.2587(2) 0.0198(8) Uani 1 1 d . . .
H27 H 0.3619 0.5017 0.2978 0.024 Uiso 1 1 calc R . .
C28 C 0.3547(3) 0.4622(3) 0.1941(2) 0.0219(9) Uani 1 1 d . . .
H28 H 0.4241 0.4502 0.1888 0.026 Uiso 1 1 calc R . .
C29 C 0.2900(3) 0.4497(3) 0.1370(2) 0.0234(9) Uani 1 1 d . . .
H29 H 0.3153 0.4292 0.0925 0.028 Uiso 1 1 calc R . .
C30 C 0.1889(3) 0.4668(3) 0.1448(2) 0.0223(9) Uani 1 1 d . . .
H30 H 0.1449 0.4582 0.1055 0.027 Uiso 1 1 calc R . .
C31 C 0.1516(3) 0.4963(3) 0.2093(2) 0.0188(8) Uani 1 1 d . . .
H31 H 0.0820 0.5078 0.2143 0.023 Uiso 1 1 calc R . .
C32 C 0.4081(3) 1.0590(3) 0.4066(2) 0.0243(9) Uani 1 1 d . . .
C33 C 0.1084(3) 0.9640(3) 0.4219(2) 0.0230(9) Uani 1 1 d . . .
S1 S 0.34354(7) 1.06288(7) 0.32005(5) 0.0201(2) Uani 1 1 d . . .
S2 S 0.18459(7) 0.94163(7) 0.34345(5) 0.0182(2) Uani 1 1 d . . .
N3 N 0.2317(2) 1.0409(2) 0.33717(17) 0.0201(7) Uani 1 1 d . . .
O1 O 0.3506(2) 1.1578(2) 0.29947(15) 0.0296(7) Uani 1 1 d . . .
O2 O 0.3935(2) 0.9947(2) 0.27805(15) 0.0312(7) Uani 1 1 d . . .
O3 O 0.1127(2) 0.9249(2) 0.28863(14) 0.0287(7) Uani 1 1 d . . .
O4 O 0.2501(2) 0.86816(19) 0.36299(17) 0.0320(7) Uani 1 1 d . . .
F1 F 0.36095(19) 1.11101(18) 0.45452(13) 0.0359(6) Uani 1 1 d . . .
F2 F 0.50064(18) 1.09127(18) 0.40006(14) 0.0363(6) Uani 1 1 d . . .
F3 F 0.4126(2) 0.97400(17) 0.43204(14) 0.0436(7) Uani 1 1 d . . .
F4 F 0.1635(2) 0.98650(19) 0.47771(12) 0.0387(7) Uani 1 1 d . . .
F5 F 0.04250(18) 1.03155(17) 0.41041(14) 0.0337(6) Uani 1 1 d . . .
F6 F 0.05627(18) 0.88775(17) 0.43834(12) 0.0307(6) 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
Au C1 2.068(3) . ?
Au P 2.2777(9) . ?
P C20 1.809(4) . ?
P C26 1.816(4) . ?
P C14 1.824(4) . ?
N1 C1 1.355(4) . ?
N1 C2 1.401(4) . ?
N1 C4 1.515(4) . ?
N2 C1 1.360(4) . ?
N2 C3 1.396(4) . ?
N2 C10 1.511(4) . ?
C2 C3 1.349(5) . ?
C2 C8 1.493(5) . ?
C3 C9 1.496(5) . ?
C4 C6 1.525(5) . ?
C4 C5 1.527(5) . ?
C4 C7 1.533(5) . ?
C10 C12 1.523(5) . ?
C10 C13 1.528(6) . ?
C10 C11 1.536(5) . ?
C14 C15 1.391(5) . ?
C14 C19 1.392(5) . ?
C15 C16 1.385(5) . ?
C16 C17 1.384(5) . ?
C17 C18 1.380(5) . ?
C18 C19 1.385(5) . ?
C20 C25 1.391(5) . ?
C20 C21 1.401(5) . ?
C21 C22 1.379(5) . ?
C22 C23 1.377(5) . ?
C23 C24 1.388(5) . ?
C24 C25 1.384(5) . ?
C26 C31 1.388(5) . ?
C26 C27 1.394(5) . ?
C27 C28 1.383(5) . ?
C28 C29 1.384(6) . ?
C29 C30 1.382(5) . ?
C30 C31 1.380(5) . ?
C32 F3 1.320(5) . ?
C32 F2 1.328(5) . ?
C32 F1 1.333(5) . ?
C32 S1 1.836(4) . ?
C33 F4 1.319(5) . ?
C33 F5 1.332(5) . ?
C33 F6 1.341(4) . ?
C33 S2 1.823(4) . ?
S1 O2 1.430(3) . ?
S1 O1 1.430(3) . ?
S1 N3 1.563(3) . ?
S2 O4 1.424(3) . ?
S2 O3 1.425(3) . ?
S2 N3 1.573(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Au P 174.43(10) . . ?
C20 P C26 105.56(16) . . ?
C20 P C14 106.40(16) . . ?
C26 P C14 103.87(16) . . ?
C20 P Au 113.13(12) . . ?
C26 P Au 114.56(12) . . ?
C14 P Au 112.48(11) . . ?
C1 N1 C2 109.4(3) . . ?
C1 N1 C4 123.3(3) . . ?
C2 N1 C4 127.4(3) . . ?
C1 N2 C3 109.5(3) . . ?
C1 N2 C10 122.9(3) . . ?
C3 N2 C10 127.6(3) . . ?
N1 C1 N2 106.5(3) . . ?
N1 C1 Au 124.7(2) . . ?
N2 C1 Au 125.2(2) . . ?
C3 C2 N1 107.2(3) . . ?
C3 C2 C8 126.0(3) . . ?
N1 C2 C8 126.5(3) . . ?
C2 C3 N2 107.1(3) . . ?
C2 C3 C9 126.5(3) . . ?
N2 C3 C9 126.2(3) . . ?
N1 C4 C6 110.4(3) . . ?
N1 C4 C5 107.9(3) . . ?
C6 C4 C5 111.4(3) . . ?
N1 C4 C7 111.3(3) . . ?
C6 C4 C7 106.1(3) . . ?
C5 C4 C7 109.8(3) . . ?
N2 C10 C12 108.8(3) . . ?
N2 C10 C13 109.5(3) . . ?
C12 C10 C13 111.7(4) . . ?
N2 C10 C11 111.7(3) . . ?
C12 C10 C11 109.4(3) . . ?
C13 C10 C11 105.8(3) . . ?
C15 C14 C19 119.4(3) . . ?
C15 C14 P 118.7(3) . . ?
C19 C14 P 121.8(3) . . ?
C16 C15 C14 120.0(4) . . ?
C17 C16 C15 120.1(4) . . ?
C18 C17 C16 120.1(4) . . ?
C17 C18 C19 120.1(4) . . ?
C18 C19 C14 120.1(3) . . ?
C25 C20 C21 119.4(3) . . ?
C25 C20 P 119.3(3) . . ?
C21 C20 P 121.3(3) . . ?
C22 C21 C20 119.8(3) . . ?
C23 C22 C21 120.8(3) . . ?
C22 C23 C24 119.9(4) . . ?
C25 C24 C23 120.1(3) . . ?
C24 C25 C20 120.1(3) . . ?
C31 C26 C27 119.2(3) . . ?
C31 C26 P 121.3(3) . . ?
C27 C26 P 119.3(3) . . ?
C28 C27 C26 120.5(4) . . ?
C27 C28 C29 119.7(4) . . ?
C30 C29 C28 120.1(4) . . ?
C31 C30 C29 120.3(4) . . ?
C30 C31 C26 120.2(4) . . ?
F3 C32 F2 108.6(3) . . ?
F3 C32 F1 107.7(3) . . ?
F2 C32 F1 107.8(3) . . ?
F3 C32 S1 111.7(3) . . ?
F2 C32 S1 109.9(3) . . ?
F1 C32 S1 111.0(3) . . ?
F4 C33 F5 108.3(3) . . ?
F4 C33 F6 108.0(3) . . ?
F5 C33 F6 107.3(3) . . ?
F4 C33 S2 111.9(3) . . ?
F5 C33 S2 111.7(3) . . ?
F6 C33 S2 109.3(3) . . ?
O2 S1 O1 118.86(18) . . ?
O2 S1 N3 114.96(18) . . ?
O1 S1 N3 108.35(18) . . ?
O2 S1 C32 104.34(19) . . ?
O1 S1 C32 103.73(18) . . ?
N3 S1 C32 104.93(19) . . ?
O4 S2 O3 118.06(19) . . ?
O4 S2 N3 117.11(17) . . ?
O3 S2 N3 111.70(18) . . ?
O4 S2 C33 105.64(19) . . ?
O3 S2 C33 103.67(18) . . ?
N3 S2 C33 97.07(18) . . ?
S1 N3 S2 125.8(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Au P C20 137.9(10) . . . . ?
C1 Au P C26 -101.0(10) . . . . ?
C1 Au P C14 17.3(10) . . . . ?
C2 N1 C1 N2 5.2(4) . . . . ?
C4 N1 C1 N2 -175.8(3) . . . . ?
C2 N1 C1 Au -154.3(2) . . . . ?
C4 N1 C1 Au 24.8(5) . . . . ?
C3 N2 C1 N1 -5.2(4) . . . . ?
C10 N2 C1 N1 174.0(3) . . . . ?
C3 N2 C1 Au 154.1(2) . . . . ?
C10 N2 C1 Au -26.7(5) . . . . ?
P Au C1 N1 79.9(11) . . . . ?
P Au C1 N2 -75.7(11) . . . . ?
C1 N1 C2 C3 -3.2(4) . . . . ?
C4 N1 C2 C3 177.8(3) . . . . ?
C1 N1 C2 C8 171.7(3) . . . . ?
C4 N1 C2 C8 -7.3(6) . . . . ?
N1 C2 C3 N2 -0.1(4) . . . . ?
C8 C2 C3 N2 -175.0(3) . . . . ?
N1 C2 C3 C9 175.4(3) . . . . ?
C8 C2 C3 C9 0.6(6) . . . . ?
C1 N2 C3 C2 3.3(4) . . . . ?
C10 N2 C3 C2 -175.8(3) . . . . ?
C1 N2 C3 C9 -172.2(3) . . . . ?
C10 N2 C3 C9 8.6(6) . . . . ?
C1 N1 C4 C6 34.5(5) . . . . ?
C2 N1 C4 C6 -146.6(3) . . . . ?
C1 N1 C4 C5 -87.4(4) . . . . ?
C2 N1 C4 C5 91.4(4) . . . . ?
C1 N1 C4 C7 152.1(3) . . . . ?
C2 N1 C4 C7 -29.1(5) . . . . ?
C1 N2 C10 C12 87.1(4) . . . . ?
C3 N2 C10 C12 -93.8(4) . . . . ?
C1 N2 C10 C13 -35.2(5) . . . . ?
C3 N2 C10 C13 143.9(4) . . . . ?
C1 N2 C10 C11 -152.0(3) . . . . ?
C3 N2 C10 C11 27.1(5) . . . . ?
C20 P C14 C15 -76.9(3) . . . . ?
C26 P C14 C15 171.9(3) . . . . ?
Au P C14 C15 47.5(3) . . . . ?
C20 P C14 C19 105.1(3) . . . . ?
C26 P C14 C19 -6.0(3) . . . . ?
Au P C14 C19 -130.5(3) . . . . ?
C19 C14 C15 C16 0.3(5) . . . . ?
P C14 C15 C16 -177.7(3) . . . . ?
C14 C15 C16 C17 0.6(6) . . . . ?
C15 C16 C17 C18 -0.8(6) . . . . ?
C16 C17 C18 C19 0.0(6) . . . . ?
C17 C18 C19 C14 0.9(6) . . . . ?
C15 C14 C19 C18 -1.1(5) . . . . ?
P C14 C19 C18 176.8(3) . . . . ?
C26 P C20 C25 -86.4(3) . . . . ?
C14 P C20 C25 163.7(3) . . . . ?
Au P C20 C25 39.7(3) . . . . ?
C26 P C20 C21 90.5(3) . . . . ?
C14 P C20 C21 -19.4(3) . . . . ?
Au P C20 C21 -143.4(3) . . . . ?
C25 C20 C21 C22 -1.3(5) . . . . ?
P C20 C21 C22 -178.2(3) . . . . ?
C20 C21 C22 C23 1.4(6) . . . . ?
C21 C22 C23 C24 -0.8(6) . . . . ?
C22 C23 C24 C25 0.2(6) . . . . ?
C23 C24 C25 C20 -0.2(6) . . . . ?
C21 C20 C25 C24 0.7(5) . . . . ?
P C20 C25 C24 177.7(3) . . . . ?
C20 P C26 C31 -29.7(3) . . . . ?
C14 P C26 C31 82.1(3) . . . . ?
Au P C26 C31 -154.8(3) . . . . ?
C20 P C26 C27 155.8(3) . . . . ?
C14 P C26 C27 -92.4(3) . . . . ?
Au P C26 C27 30.7(3) . . . . ?
C31 C26 C27 C28 -0.6(6) . . . . ?
P C26 C27 C28 174.0(3) . . . . ?
C26 C27 C28 C29 0.7(6) . . . . ?
C27 C28 C29 C30 -0.3(6) . . . . ?
C28 C29 C30 C31 -0.1(6) . . . . ?
C29 C30 C31 C26 0.2(6) . . . . ?
C27 C26 C31 C30 0.2(6) . . . . ?
P C26 C31 C30 -174.3(3) . . . . ?
F3 C32 S1 O2 -51.9(3) . . . . ?
F2 C32 S1 O2 68.8(3) . . . . ?
F1 C32 S1 O2 -172.0(3) . . . . ?
F3 C32 S1 O1 -177.0(3) . . . . ?
F2 C32 S1 O1 -56.3(3) . . . . ?
F1 C32 S1 O1 62.9(3) . . . . ?
F3 C32 S1 N3 69.4(3) . . . . ?
F2 C32 S1 N3 -170.0(3) . . . . ?
F1 C32 S1 N3 -50.8(3) . . . . ?
F4 C33 S2 O4 58.9(3) . . . . ?
F5 C33 S2 O4 -179.4(3) . . . . ?
F6 C33 S2 O4 -60.8(3) . . . . ?
F4 C33 S2 O3 -176.3(3) . . . . ?
F5 C33 S2 O3 -54.6(3) . . . . ?
F6 C33 S2 O3 64.0(3) . . . . ?
F4 C33 S2 N3 -61.9(3) . . . . ?
F5 C33 S2 N3 59.8(3) . . . . ?
F6 C33 S2 N3 178.5(3) . . . . ?
O2 S1 N3 S2 28.3(3) . . . . ?
O1 S1 N3 S2 164.0(2) . . . . ?
C32 S1 N3 S2 -85.7(3) . . . . ?
O4 S2 N3 S1 26.1(3) . . . . ?
O3 S2 N3 S1 -114.5(3) . . . . ?
C33 S2 N3 S1 137.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         2.808
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.196
_refine_instructions_details     
;
TITL MSV03 in P2(1)/c
CELL 0.71073  13.359364  14.470148  18.766588  90.0000  90.2456  90.0000
ZERR    4.00   0.000400   0.000500   0.000600   0.0000   0.0030   0.0000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    N    O    F    P    S    AU
UNIT  132  156  12   16   24   4    8    4
MERG   2
FMAP   2
 
TEMP -173
 
ACTA 61
CONF
 
PLAN   10
 
L.S.   4
 
WGHT    0.017000    4.071300
FVAR       0.83965
AU    8    0.277916    0.614573    0.426251    11.00000    0.01234    0.01338 =
         0.01159   -0.00093   -0.00209   -0.00158
P     6    0.167639    0.537844    0.354726    11.00000    0.01222    0.01286 =
         0.01047   -0.00046   -0.00102   -0.00116
N1    3    0.481337    0.666907    0.488765    11.00000    0.01260    0.01232 =
         0.01193   -0.00054    0.00151   -0.00070
N2    3    0.363154    0.691376    0.565822    11.00000    0.01261    0.01275 =
         0.01268   -0.00002    0.00085   -0.00242
C1    1    0.380633    0.672112    0.496071    11.00000    0.01294    0.01128 =
         0.01199    0.00210   -0.00074    0.00060
C2    1    0.526856    0.675045    0.555848    11.00000    0.01659    0.01061 =
         0.01396    0.00130   -0.00536   -0.00234
C3    1    0.453427    0.690143    0.603590    11.00000    0.01933    0.01103 =
         0.01177    0.00110   -0.00258   -0.00344
C4    1    0.532497    0.652768    0.417713    11.00000    0.01472    0.01576 =
         0.01574   -0.00205    0.00333   -0.00133
C5    1    0.539524    0.548944    0.404130    11.00000    0.02893    0.02231 =
         0.02088    0.00061    0.00506    0.00557
AFIX 137
H5A   2    0.582145    0.520443    0.440640    11.00000   -1.50000
H5B   2    0.568490    0.538085    0.356977    11.00000   -1.50000
H5C   2    0.472448    0.521663    0.406054    11.00000   -1.50000
AFIX   0
C6    1    0.474414    0.701489    0.358525    11.00000    0.02075    0.02953 =
         0.01582    0.00601    0.00561    0.00434
AFIX 137
H6A   2    0.409682    0.670845    0.351603    11.00000   -1.50000
H6B   2    0.512775    0.698725    0.314182    11.00000   -1.50000
H6C   2    0.463460    0.766209    0.371755    11.00000   -1.50000
AFIX   0
C7    1    0.637556    0.695305    0.417695    11.00000    0.01735    0.04084 =
         0.02659    0.00163    0.00504   -0.00789
AFIX 137
H7A   2    0.634654    0.757889    0.437536    11.00000   -1.50000
H7B   2    0.662655    0.698020    0.368747    11.00000   -1.50000
H7C   2    0.682540    0.657205    0.446790    11.00000   -1.50000
AFIX   0
C8    1    0.635090    0.661034    0.572677    11.00000    0.01649    0.02371 =
         0.02515   -0.00017   -0.00488    0.00073
AFIX 137
H8A   2    0.644171    0.657095    0.624435    11.00000   -1.50000
H8B   2    0.673864    0.713185    0.554135    11.00000   -1.50000
H8C   2    0.658301    0.603624    0.550512    11.00000   -1.50000
AFIX   0
C9    1    0.465363    0.696718    0.682708    11.00000    0.02232    0.02650 =
         0.01338    0.00063   -0.00470   -0.00583
AFIX 137
H9A   2    0.533921    0.679685    0.696058    11.00000   -1.50000
H9B   2    0.418124    0.654571    0.705803    11.00000   -1.50000
H9C   2    0.451865    0.760205    0.698103    11.00000   -1.50000
AFIX   0
C10   1    0.259933    0.711757    0.594410    11.00000    0.01292    0.01576 =
         0.01823   -0.00266    0.00593   -0.00286
C11   1    0.264219    0.774801    0.660215    11.00000    0.02666    0.03466 =
         0.02620   -0.01224    0.00108    0.00620
AFIX 137
H11A  2    0.288647    0.739435    0.701289    11.00000   -1.50000
H11B  2    0.197088    0.798611    0.670319    11.00000   -1.50000
H11C  2    0.309654    0.826575    0.651016    11.00000   -1.50000
AFIX   0
C12   1    0.209620    0.620877    0.614150    11.00000    0.03569    0.02876 =
         0.05070   -0.00887    0.02591   -0.01400
AFIX 137
H12A  2    0.201762    0.582690    0.571362    11.00000   -1.50000
H12B  2    0.143675    0.633470    0.634660    11.00000   -1.50000
H12C  2    0.251056    0.588004    0.649126    11.00000   -1.50000
AFIX   0
C13   1    0.199608    0.764849    0.538464    11.00000    0.01909    0.05124 =
         0.02824   -0.00819    0.00225    0.01685
AFIX 137
H13A  2    0.238078    0.818616    0.522511    11.00000   -1.50000
H13B  2    0.136316    0.785575    0.559284    11.00000   -1.50000
H13C  2    0.185740    0.724406    0.497714    11.00000   -1.50000
AFIX   0
C14   1    0.130755    0.426348    0.391630    11.00000    0.01260    0.01065 =
         0.01219    0.00122   -0.00312   -0.00033
C15   1    0.102244    0.421888    0.462764    11.00000    0.02037    0.01889 =
         0.01360   -0.00387    0.00161    0.00054
AFIX  43
H15   2    0.099842    0.476640    0.490639    11.00000   -1.20000
AFIX   0
C16   1    0.077362    0.337675    0.492965    11.00000    0.02421    0.02177 =
         0.01660    0.00260    0.00485   -0.00104
AFIX  43
H16   2    0.057289    0.334835    0.541417    11.00000   -1.20000
AFIX   0
C17   1    0.081679    0.257660    0.452705    11.00000    0.01878    0.01730 =
         0.02144    0.00454   -0.00017   -0.00180
AFIX  43
H17   2    0.065364    0.199899    0.473729    11.00000   -1.20000
AFIX   0
C18   1    0.109648    0.261639    0.382065    11.00000    0.01928    0.01585 =
         0.01847   -0.00357    0.00296   -0.00013
AFIX  43
H18   2    0.112547    0.206608    0.354546    11.00000   -1.20000
AFIX   0
C19   1    0.133491    0.345694    0.351225    11.00000    0.02141    0.01686 =
         0.01227   -0.00062    0.00104    0.00226
AFIX  43
H19   2    0.151754    0.348336    0.302399    11.00000   -1.20000
AFIX   0
C20   1    0.053066    0.601470    0.338963    11.00000    0.01419    0.01493 =
         0.00912    0.00020   -0.00122    0.00002
C21   1   -0.039430    0.556308    0.333947    11.00000    0.01800    0.01159 =
         0.01648    0.00020   -0.00015   -0.00049
AFIX  43
H21   2   -0.043244    0.491251    0.340167    11.00000   -1.20000
AFIX   0
C22   1   -0.124920    0.606619    0.319948    11.00000    0.01337    0.02204 =
         0.02034    0.00102   -0.00182   -0.00474
AFIX  43
H22   2   -0.187780    0.576048    0.317607    11.00000   -1.20000
AFIX   0
C23   1   -0.120231    0.700676    0.309322    11.00000    0.01637    0.02291 =
         0.01739    0.00388    0.00030    0.00195
AFIX  43
H23   2   -0.179479    0.734556    0.299080    11.00000   -1.20000
AFIX   0
C24   1   -0.028752    0.745893    0.313605    11.00000    0.01877    0.01422 =
         0.01997    0.00560   -0.00114   -0.00098
AFIX  43
H24   2   -0.025440    0.810815    0.306463    11.00000   -1.20000
AFIX   0
C25   1    0.057649    0.696488    0.328270    11.00000    0.01681    0.01435 =
         0.01687    0.00351   -0.00123   -0.00443
AFIX  43
H25   2    0.120196    0.727545    0.331037    11.00000   -1.20000
AFIX   0
C26   1    0.215512    0.509311    0.266989    11.00000    0.01485    0.01234 =
         0.01342    0.00203    0.00253   -0.00306
C27   1    0.317554    0.492413    0.258722    11.00000    0.01898    0.02380 =
         0.01673    0.00195   -0.00108   -0.00001
AFIX  43
H27   2    0.361920    0.501689    0.297767    11.00000   -1.20000
AFIX   0
C28   1    0.354651    0.462237    0.194067    11.00000    0.01855    0.02321 =
         0.02410    0.00139    0.00642    0.00194
AFIX  43
H28   2    0.424137    0.450198    0.188835    11.00000   -1.20000
AFIX   0
C29   1    0.290048    0.449672    0.137048    11.00000    0.03084    0.02220 =
         0.01732   -0.00457    0.00703    0.00321
AFIX  43
H29   2    0.315278    0.429236    0.092496    11.00000   -1.20000
AFIX   0
C30   1    0.188913    0.466791    0.144783    11.00000    0.02846    0.02399 =
         0.01441   -0.00291   -0.00226   -0.00486
AFIX  43
H30   2    0.144862    0.458174    0.105468    11.00000   -1.20000
AFIX   0
C31   1    0.151604    0.496339    0.209329    11.00000    0.01679    0.02371 =
         0.01596    0.00166    0.00166   -0.00133
AFIX  43
H31   2    0.081976    0.507840    0.214328    11.00000   -1.20000
AFIX   0
C32   1    0.408059    1.058964    0.406600    11.00000    0.02935    0.01975 =
         0.02377   -0.00347   -0.00023   -0.00215
C33   1    0.108363    0.964033    0.421925    11.00000    0.02244    0.02462 =
         0.02211    0.00090    0.00438   -0.00528
S1    7    0.343540    1.062876    0.320048    11.00000    0.01924    0.02335 =
         0.01775   -0.00147    0.00239   -0.00579
S2    7    0.184589    0.941625    0.343454    11.00000    0.02130    0.01456 =
         0.01863    0.00024    0.00305   -0.00297
N3    3    0.231658    1.040902    0.337166    11.00000    0.01583    0.01785 =
         0.02662    0.00036    0.00377   -0.00483
O1    4    0.350566    1.157821    0.299469    11.00000    0.03148    0.02492 =
         0.03248    0.00887    0.00164   -0.01153
O2    4    0.393513    0.994668    0.278046    11.00000    0.02496    0.04075 =
         0.02811   -0.01514    0.00931   -0.00587
O3    4    0.112690    0.924852    0.288631    11.00000    0.03998    0.02848 =
         0.01774    0.00376   -0.00437   -0.01728
O4    4    0.250110    0.868161    0.362993    11.00000    0.02481    0.01735 =
         0.05389    0.00302    0.00259    0.00148
F1    5    0.360949    1.111008    0.454517    11.00000    0.04601    0.03961 =
         0.02220   -0.01034    0.00475   -0.00439
F2    5    0.500638    1.091273    0.400058    11.00000    0.02507    0.03922 =
         0.04464   -0.00825   -0.00866   -0.00570
F3    5    0.412619    0.973996    0.432040    11.00000    0.06207    0.02319 =
         0.04519    0.00764   -0.02617   -0.00546
F4    5    0.163549    0.986497    0.477711    11.00000    0.05180    0.04767 =
         0.01666   -0.00579   -0.00401   -0.01546
F5    5    0.042505    1.031552    0.410410    11.00000    0.02729    0.02529 =
         0.04853   -0.00190    0.01303    0.00317
F6    5    0.056274    0.887746    0.438337    11.00000    0.03784    0.02940 =
         0.02486    0.00677    0.00867   -0.01258
HKLF    4
;
####################################################################### 
# 
# 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_msv13
_database_code_depnum_ccdc_archive 'CCDC 1052450'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H35 F3 N2 O3 S'
_chemical_formula_weight         560.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.7510(5)
_cell_length_b                   11.0657(6)
_cell_length_c                   15.6228(8)
_cell_angle_alpha                73.544(5)
_cell_angle_beta                 79.645(5)
_cell_angle_gamma                83.429(4)
_cell_volume                     1424.00(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    20644
_cell_measurement_theta_min      4.1560
_cell_measurement_theta_max      75.4670

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.34284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28723
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.18
_diffrn_reflns_theta_max         75.66
_reflns_number_total             5870
_reflns_number_gt                5528
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) 
(compiled Feb  1 2013,16:14:44) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  SHELXL-97

_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. 

 The triflate anion is disordered and was refined on two positions.
;

_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)+(0.0614P)²+0.9836P] 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         5870
_refine_ls_number_parameters     393
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1344
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.023
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.47644(15) 0.12766(12) 0.71240(9) 0.0239(3) Uani 1 1 d . . .
N2 N 0.26383(14) 0.18383(11) 0.79501(8) 0.0210(3) Uani 1 1 d . . .
C1 C 0.35236(17) 0.21293(14) 0.71250(10) 0.0206(3) Uani 1 1 d . . .
C2 C 0.46674(19) 0.04368(15) 0.79825(12) 0.0283(3) Uani 1 1 d . . .
C3 C 0.33654(19) 0.07879(15) 0.84904(11) 0.0274(3) Uani 1 1 d . . .
C4 C 0.61295(19) 0.12038(19) 0.63753(13) 0.0353(4) Uani 1 1 d . . .
C5 C 0.5960(2) 0.2143(3) 0.54694(13) 0.0525(6) Uani 1 1 d . . .
H5A H 0.5003 0.2011 0.5274 0.079 Uiso 1 1 calc R . .
H5B H 0.6858 0.2018 0.5020 0.079 Uiso 1 1 calc R . .
H5C H 0.5910 0.3005 0.5530 0.079 Uiso 1 1 calc R . .
C6 C 0.7573(2) 0.1501(3) 0.66874(16) 0.0540(6) Uani 1 1 d . . .
H6A H 0.8498 0.1394 0.6251 0.081 Uiso 1 1 calc R . .
H6B H 0.7689 0.0924 0.7281 0.081 Uiso 1 1 calc R . .
H6C H 0.7454 0.2374 0.6730 0.081 Uiso 1 1 calc R . .
C7 C 0.6263(3) -0.0123(3) 0.6248(2) 0.0647(7) Uani 1 1 d . . .
H7A H 0.5237 -0.0346 0.6197 0.097 Uiso 1 1 calc R . .
H7B H 0.6646 -0.0727 0.6769 0.097 Uiso 1 1 calc R . .
H7C H 0.6990 -0.0148 0.5697 0.097 Uiso 1 1 calc R . .
C8 C 0.5730(2) -0.07096(18) 0.82994(16) 0.0451(5) Uani 1 1 d . . .
H8A H 0.5689 -0.0898 0.8955 0.068 Uiso 1 1 calc R . .
H8B H 0.6799 -0.0547 0.7999 0.068 Uiso 1 1 calc R . .
H8C H 0.5396 -0.1432 0.8151 0.068 Uiso 1 1 calc R . .
C9 C 0.2789(2) 0.0084(2) 0.94418(13) 0.0429(5) Uani 1 1 d . . .
H9A H 0.2044 -0.0514 0.9442 0.064 Uiso 1 1 calc R . .
H9B H 0.2276 0.0682 0.9778 0.064 Uiso 1 1 calc R . .
H9C H 0.3669 -0.0379 0.9729 0.064 Uiso 1 1 calc R . .
C10 C 0.11200(18) 0.25028(15) 0.82927(10) 0.0241(3) Uani 1 1 d . . .
C11 C 0.03937(19) 0.34624(16) 0.75383(12) 0.0312(4) Uani 1 1 d . . .
H11A H 0.1083 0.4152 0.7257 0.047 Uiso 1 1 calc R . .
H11B H -0.0617 0.3802 0.7790 0.047 Uiso 1 1 calc R . .
H11C H 0.0248 0.3049 0.7083 0.047 Uiso 1 1 calc R . .
C12 C 0.1491(2) 0.31768(19) 0.89499(13) 0.0377(4) Uani 1 1 d . . .
H12A H 0.2266 0.3791 0.8636 0.056 Uiso 1 1 calc R . .
H12B H 0.1906 0.2557 0.9453 0.056 Uiso 1 1 calc R . .
H12C H 0.0539 0.3615 0.9183 0.056 Uiso 1 1 calc R . .
C13 C -0.0079(2) 0.15157(17) 0.87329(13) 0.0359(4) Uani 1 1 d . . .
H13A H -0.1114 0.1943 0.8832 0.054 Uiso 1 1 calc R . .
H13B H 0.0196 0.0999 0.9313 0.054 Uiso 1 1 calc R . .
H13C H -0.0087 0.0973 0.8335 0.054 Uiso 1 1 calc R . .
C14 C 0.32975(17) 0.32916(15) 0.63797(10) 0.0233(3) Uani 1 1 d . . .
C15 C 0.3914(2) 0.43376(16) 0.64126(11) 0.0289(3) Uani 1 1 d . . .
H15 H 0.3797 0.5084 0.5939 0.035 Uiso 1 1 calc R . .
C16 C 0.47219(19) 0.43978(15) 0.71051(11) 0.0286(3) Uani 1 1 d . . .
C17 C 0.53754(19) 0.45060(15) 0.76915(11) 0.0275(3) Uani 1 1 d . . .
C18 C 0.24578(18) 0.32492(17) 0.56491(10) 0.0273(3) Uani 1 1 d . . .
C19 C 0.2279(2) 0.4314(2) 0.49218(13) 0.0420(5) Uani 1 1 d . . .
H19 H 0.2657 0.5090 0.4911 0.050 Uiso 1 1 calc R . .
C20 C 0.1558(3) 0.4246(3) 0.42185(14) 0.0528(6) Uani 1 1 d . . .
H20 H 0.1457 0.4971 0.3726 0.063 Uiso 1 1 calc R . .
C21 C 0.0991(2) 0.3138(2) 0.42286(13) 0.0469(5) Uani 1 1 d . . .
H21 H 0.0503 0.3096 0.3742 0.056 Uiso 1 1 calc R . .
C22 C 0.1127(2) 0.2085(2) 0.49438(14) 0.0406(4) Uani 1 1 d . . .
H22 H 0.0719 0.1321 0.4952 0.049 Uiso 1 1 calc R . .
C23 C 0.1860(2) 0.21322(18) 0.56564(12) 0.0327(4) Uani 1 1 d . . .
H23 H 0.1951 0.1402 0.6147 0.039 Uiso 1 1 calc R . .
C24 C 0.61236(18) 0.46094(15) 0.84064(11) 0.0253(3) Uani 1 1 d . . .
C25 C 0.69333(19) 0.56714(16) 0.83130(12) 0.0285(3) Uani 1 1 d . . .
H25 H 0.6978 0.6340 0.7773 0.034 Uiso 1 1 calc R . .
C26 C 0.7670(2) 0.57454(17) 0.90110(12) 0.0328(4) Uani 1 1 d . . .
H26 H 0.8226 0.6463 0.8948 0.039 Uiso 1 1 calc R . .
C27 C 0.7595(2) 0.47728(18) 0.97998(13) 0.0357(4) Uani 1 1 d . . .
H27 H 0.8101 0.4826 1.0276 0.043 Uiso 1 1 calc R . .
C28 C 0.6784(2) 0.37197(18) 0.99011(12) 0.0356(4) Uani 1 1 d . . .
H28 H 0.6733 0.3059 1.0446 0.043 Uiso 1 1 calc R . .
C29 C 0.6054(2) 0.36352(16) 0.92082(12) 0.0301(4) Uani 1 1 d . . .
H29 H 0.5504 0.2914 0.9276 0.036 Uiso 1 1 calc R . .
S S 0.07081(7) 0.85262(5) 0.78022(4) 0.02915(18) Uani 0.6910(14) 1 d PD A 1
O1 O -0.0600(4) 0.8422(4) 0.7369(3) 0.0586(10) Uani 0.6910(14) 1 d PDU A 1
O2 O 0.1535(6) 0.9632(3) 0.7377(3) 0.0444(10) Uani 0.6910(14) 1 d PDU A 1
O3 O 0.0420(3) 0.8174(2) 0.87645(13) 0.0457(5) Uani 0.6910(14) 1 d PD A 1
C30 C 0.2071(4) 0.7281(3) 0.7524(2) 0.0284(7) Uani 0.6910(14) 1 d PDU A 1
F1 F 0.2454(2) 0.74320(19) 0.66395(12) 0.0493(5) Uani 0.6910(14) 1 d PD A 1
F2 F 0.3407(2) 0.7238(2) 0.78375(14) 0.0574(5) Uani 0.6910(14) 1 d PD A 1
F3 F 0.1522(3) 0.61593(16) 0.78749(16) 0.0651(6) Uani 0.6910(14) 1 d PD A 1
S' S 0.09326(15) 0.87315(12) 0.70720(9) 0.0267(4) Uiso 0.3090(14) 1 d PD A 2
O1' O 0.1033(5) 0.9089(4) 0.6108(3) 0.0364(9) Uiso 0.3090(14) 1 d PD A 2
O2' O 0.166(2) 0.9540(14) 0.7462(12) 0.089(6) Uiso 0.3090(14) 1 d PDU A 2
O3' O -0.0516(9) 0.8249(7) 0.7588(5) 0.0357(17) Uiso 0.3090(14) 1 d PDU A 2
C30' C 0.2300(8) 0.7347(6) 0.7246(6) 0.026(2) Uiso 0.3090(14) 1 d PDU A 2
F1' F 0.1903(5) 0.6437(4) 0.6964(3) 0.0474(10) Uiso 0.3090(14) 1 d PD A 2
F2' F 0.3733(5) 0.7608(4) 0.6876(3) 0.0531(10) Uiso 0.3090(14) 1 d PD A 2
F3' F 0.2375(6) 0.6812(4) 0.8138(3) 0.0538(11) Uiso 0.3090(14) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.3547(19) . ?
N1 C2 1.393(2) . ?
N1 C4 1.527(2) . ?
N2 C1 1.3522(19) . ?
N2 C3 1.3915(19) . ?
N2 C10 1.5285(19) . ?
C1 C14 1.492(2) . ?
C2 C3 1.352(2) . ?
C2 C8 1.503(2) . ?
C3 C9 1.495(2) . ?
C4 C5 1.520(3) . ?
C4 C7 1.525(3) . ?
C4 C6 1.532(3) . ?
C10 C12 1.525(2) . ?
C10 C11 1.525(2) . ?
C10 C13 1.531(2) . ?
C14 C15 1.349(2) . ?
C14 C18 1.478(2) . ?
C15 C16 1.415(2) . ?
C16 C17 1.203(2) . ?
C17 C24 1.429(2) . ?
C18 C23 1.393(2) . ?
C18 C19 1.402(3) . ?
C19 C20 1.385(3) . ?
C20 C21 1.369(3) . ?
C21 C22 1.378(3) . ?
C22 C23 1.397(3) . ?
C24 C29 1.399(2) . ?
C24 C25 1.400(2) . ?
C25 C26 1.388(2) . ?
C26 C27 1.384(3) . ?
C27 C28 1.389(3) . ?
C28 C29 1.382(3) . ?
S O3 1.425(2) . ?
S O2 1.425(3) . ?
S O1 1.462(3) . ?
S C30 1.813(3) . ?
C30 F3 1.315(4) . ?
C30 F1 1.329(4) . ?
C30 F2 1.337(3) . ?
S' O1' 1.434(4) . ?
S' O3' 1.444(7) . ?
S' O2' 1.466(11) . ?
S' C30' 1.820(7) . ?
C30' F1' 1.310(8) . ?
C30' F2' 1.310(8) . ?
C30' F3' 1.362(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 107.90(13) . . ?
C1 N1 C4 129.66(14) . . ?
C2 N1 C4 122.36(13) . . ?
C1 N2 C3 107.87(13) . . ?
C1 N2 C10 129.10(12) . . ?
C3 N2 C10 123.01(12) . . ?
N2 C1 N1 108.73(13) . . ?
N2 C1 C14 125.68(13) . . ?
N1 C1 C14 125.10(13) . . ?
C3 C2 N1 107.60(14) . . ?
C3 C2 C8 124.56(16) . . ?
N1 C2 C8 127.75(16) . . ?
C2 C3 N2 107.88(14) . . ?
C2 C3 C9 124.43(15) . . ?
N2 C3 C9 127.54(15) . . ?
C5 C4 C7 108.00(19) . . ?
C5 C4 N1 114.25(14) . . ?
C7 C4 N1 107.81(16) . . ?
C5 C4 C6 107.85(18) . . ?
C7 C4 C6 112.55(19) . . ?
N1 C4 C6 106.49(15) . . ?
C12 C10 C11 109.21(14) . . ?
C12 C10 N2 107.31(13) . . ?
C11 C10 N2 113.12(12) . . ?
C12 C10 C13 112.81(14) . . ?
C11 C10 C13 105.81(14) . . ?
N2 C10 C13 108.67(12) . . ?
C15 C14 C18 123.54(14) . . ?
C15 C14 C1 116.50(14) . . ?
C18 C14 C1 119.95(14) . . ?
C14 C15 C16 124.42(15) . . ?
C17 C16 C15 176.86(18) . . ?
C16 C17 C24 178.37(18) . . ?
C23 C18 C19 118.36(16) . . ?
C23 C18 C14 120.40(15) . . ?
C19 C18 C14 121.22(16) . . ?
C20 C19 C18 120.7(2) . . ?
C21 C20 C19 120.4(2) . . ?
C20 C21 C22 120.03(18) . . ?
C21 C22 C23 120.46(19) . . ?
C18 C23 C22 120.06(18) . . ?
C29 C24 C25 119.54(15) . . ?
C29 C24 C17 119.65(15) . . ?
C25 C24 C17 120.81(15) . . ?
C26 C25 C24 119.90(16) . . ?
C27 C26 C25 119.93(16) . . ?
C26 C27 C28 120.57(17) . . ?
C29 C28 C27 119.89(17) . . ?
C28 C29 C24 120.17(16) . . ?
O3 S O2 116.4(2) . . ?
O3 S O1 115.12(19) . . ?
O2 S O1 114.2(3) . . ?
O3 S C30 104.05(14) . . ?
O2 S C30 102.8(2) . . ?
O1 S C30 101.44(18) . . ?
F3 C30 F1 107.2(2) . . ?
F3 C30 F2 106.7(2) . . ?
F1 C30 F2 106.1(3) . . ?
F3 C30 S 112.2(2) . . ?
F1 C30 S 112.84(19) . . ?
F2 C30 S 111.4(2) . . ?
O1' S' O3' 116.6(3) . . ?
O1' S' O2' 116.8(7) . . ?
O3' S' O2' 114.9(8) . . ?
O1' S' C30' 101.2(3) . . ?
O3' S' C30' 103.4(4) . . ?
O2' S' C30' 100.2(8) . . ?
F1' C30' F2' 109.1(6) . . ?
F1' C30' F3' 104.3(5) . . ?
F2' C30' F3' 104.9(6) . . ?
F1' C30' S' 113.0(5) . . ?
F2' C30' S' 113.0(5) . . ?
F3' C30' S' 111.9(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 1.42(17) . . . . ?
C10 N2 C1 N1 -179.74(13) . . . . ?
C3 N2 C1 C14 -170.85(14) . . . . ?
C10 N2 C1 C14 8.0(2) . . . . ?
C2 N1 C1 N2 -1.08(17) . . . . ?
C4 N1 C1 N2 -177.97(15) . . . . ?
C2 N1 C1 C14 171.25(14) . . . . ?
C4 N1 C1 C14 -5.6(2) . . . . ?
C1 N1 C2 C3 0.31(18) . . . . ?
C4 N1 C2 C3 177.47(15) . . . . ?
C1 N1 C2 C8 176.72(17) . . . . ?
C4 N1 C2 C8 -6.1(3) . . . . ?
N1 C2 C3 N2 0.56(19) . . . . ?
C8 C2 C3 N2 -176.00(16) . . . . ?
N1 C2 C3 C9 176.33(17) . . . . ?
C8 C2 C3 C9 -0.2(3) . . . . ?
C1 N2 C3 C2 -1.23(18) . . . . ?
C10 N2 C3 C2 179.85(14) . . . . ?
C1 N2 C3 C9 -176.83(18) . . . . ?
C10 N2 C3 C9 4.2(3) . . . . ?
C1 N1 C4 C5 -7.8(3) . . . . ?
C2 N1 C4 C5 175.74(17) . . . . ?
C1 N1 C4 C7 -127.8(2) . . . . ?
C2 N1 C4 C7 55.7(2) . . . . ?
C1 N1 C4 C6 111.2(2) . . . . ?
C2 N1 C4 C6 -65.3(2) . . . . ?
C1 N2 C10 C12 -108.23(18) . . . . ?
C3 N2 C10 C12 70.45(18) . . . . ?
C1 N2 C10 C11 12.3(2) . . . . ?
C3 N2 C10 C11 -169.03(14) . . . . ?
C1 N2 C10 C13 129.49(16) . . . . ?
C3 N2 C10 C13 -51.83(19) . . . . ?
N2 C1 C14 C15 82.9(2) . . . . ?
N1 C1 C14 C15 -88.15(19) . . . . ?
N2 C1 C14 C18 -98.10(18) . . . . ?
N1 C1 C14 C18 90.85(18) . . . . ?
C18 C14 C15 C16 -179.96(15) . . . . ?
C1 C14 C15 C16 -1.0(2) . . . . ?
C14 C15 C16 C17 -142(3) . . . . ?
C15 C16 C17 C24 108(7) . . . . ?
C15 C14 C18 C23 179.61(16) . . . . ?
C1 C14 C18 C23 0.7(2) . . . . ?
C15 C14 C18 C19 1.4(3) . . . . ?
C1 C14 C18 C19 -177.53(16) . . . . ?
C23 C18 C19 C20 -1.5(3) . . . . ?
C14 C18 C19 C20 176.76(18) . . . . ?
C18 C19 C20 C21 0.8(3) . . . . ?
C19 C20 C21 C22 0.4(3) . . . . ?
C20 C21 C22 C23 -0.8(3) . . . . ?
C19 C18 C23 C22 1.0(3) . . . . ?
C14 C18 C23 C22 -177.23(15) . . . . ?
C21 C22 C23 C18 0.1(3) . . . . ?
C16 C17 C24 C29 22(7) . . . . ?
C16 C17 C24 C25 -158(6) . . . . ?
C29 C24 C25 C26 0.5(2) . . . . ?
C17 C24 C25 C26 -179.12(15) . . . . ?
C24 C25 C26 C27 -0.4(3) . . . . ?
C25 C26 C27 C28 -0.1(3) . . . . ?
C26 C27 C28 C29 0.4(3) . . . . ?
C27 C28 C29 C24 -0.3(3) . . . . ?
C25 C24 C29 C28 -0.2(2) . . . . ?
C17 C24 C29 C28 179.45(16) . . . . ?
O3 S C30 F3 57.2(2) . . . . ?
O2 S C30 F3 179.0(3) . . . . ?
O1 S C30 F3 -62.6(3) . . . . ?
O3 S C30 F1 178.4(2) . . . . ?
O2 S C30 F1 -59.7(3) . . . . ?
O1 S C30 F1 58.6(3) . . . . ?
O3 S C30 F2 -62.4(3) . . . . ?
O2 S C30 F2 59.5(3) . . . . ?
O1 S C30 F2 177.8(3) . . . . ?
O1' S' C30' F1' -61.2(6) . . . . ?
O3' S' C30' F1' 59.9(7) . . . . ?
O2' S' C30' F1' 178.7(9) . . . . ?
O1' S' C30' F2' 63.4(6) . . . . ?
O3' S' C30' F2' -175.5(6) . . . . ?
O2' S' C30' F2' -56.7(9) . . . . ?
O1' S' C30' F3' -178.5(4) . . . . ?
O3' S' C30' F3' -57.5(6) . . . . ?
O2' S' C30' F3' 61.4(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        75.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.049

#=============================================================================
#  end of cif data for "MSV13" (compound [(1b)C4Ph2H]OTf)
#=============================================================================

#=============================================================================
#  end of combined cif data
#=============================================================================
