# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2016

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

data_2013dcp023
_database_code_depnum_ccdc_archive 'CCDC 1432360'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 F18 P, C4 H12 N'
_chemical_formula_sum            'C10 H12 F18 N P'
_chemical_formula_weight         519.18

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'
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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_Int_Tables_number      62

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

_cell_length_a                   18.972(2)
_cell_length_b                   11.8654(13)
_cell_length_c                   7.9166(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1782.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5095
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      34.6

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9707
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6166
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2130
_reflns_number_gt                1961
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0738P)²+0.5772P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2130
_refine_ls_number_parameters     166
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.39226(9) 0.08720(16) 0.1229(2) 0.0186(4) Uani 1 1 d . . .
C2 C 0.36684(10) 0.02235(16) -0.0344(2) 0.0239(4) Uani 1 1 d . . .
C3 C 0.29741(11) 0.2500 0.2644(3) 0.0171(5) Uani 1 2 d S . .
C4 C 0.30055(13) 0.2500 0.4607(3) 0.0243(6) Uani 1 2 d S . .
C5 C 0.02739(14) 0.2500 0.8350(4) 0.0332(7) Uani 1 2 d SD . .
C6 C 0.08612(10) 0.14754(18) 1.0621(3) 0.0303(5) Uani 1 1 d . . .
H6A H 0.0428 0.1482 1.1296 0.045 Uiso 1 1 calc R . .
H6B H 0.1271 0.1470 1.1374 0.045 Uiso 1 1 calc R . .
H6C H 0.0869 0.0801 0.9907 0.045 Uiso 1 1 calc R . .
C7 C 0.15624(12) 0.2500 0.8538(3) 0.0194(5) Uani 1 2 d SD . .
N1 N 0.08845(9) 0.2500 0.9534(2) 0.0143(4) Uani 1 2 d S . .
F1 F 0.33055(7) 0.2500 -0.03512(17) 0.0176(3) Uani 1 2 d S . .
F2 F 0.45057(7) 0.2500 0.00248(18) 0.0215(3) Uani 1 2 d S . .
F3 F 0.43232(7) 0.2500 0.29533(17) 0.0173(3) Uani 1 2 d S . .
F4 F 0.46190(6) 0.06058(10) 0.13797(14) 0.0279(3) Uani 1 1 d . . .
F5 F 0.36106(6) 0.03380(10) 0.25658(13) 0.0273(3) Uani 1 1 d . . .
F6 F 0.38426(7) -0.08717(10) -0.01948(16) 0.0332(3) Uani 1 1 d . . .
F7 F 0.39811(6) 0.06013(10) -0.17474(14) 0.0291(3) Uani 1 1 d . . .
F8 F 0.29779(6) 0.02822(10) -0.05440(15) 0.0326(3) Uani 1 1 d . . .
F9 F 0.25695(5) 0.15923(9) 0.22261(14) 0.0249(3) Uani 1 1 d . . .
F10 F 0.33324(6) 0.15946(11) 0.52024(14) 0.0325(3) Uani 1 1 d . . .
F11 F 0.23502(9) 0.2500 0.5216(2) 0.0389(5) Uani 1 2 d S . .
P1 P 0.38278(3) 0.2500 0.12696(7) 0.01292(17) Uani 1 2 d S . .
H5A H -0.0142(7) 0.2500 0.902(3) 0.025(8) Uiso 1 2 d SD . .
H5B H 0.0351(7) 0.18258(4) 0.7728(7) 0.042(7) Uiso 1 1 d D . .
H7A H 0.1930(8) 0.2500 0.935(2) 0.013(6) Uiso 1 2 d SD . .
H7B H 0.1527(6) 0.18259(4) 0.7895(5) 0.032(6) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 F4 1.3637(19) . ?
C1 F5 1.368(2) . ?
C1 C2 1.541(2) . ?
C1 P1 1.9403(19) . ?
C2 F8 1.321(2) . ?
C2 F7 1.337(2) . ?
C2 F6 1.346(2) . ?
C3 F9 1.3634(17) . ?
C3 F9 1.3635(17) 7_565 ?
C3 C4 1.555(3) . ?
C3 P1 1.951(2) . ?
C4 F10 1.3269(19) 7_565 ?
C4 F10 1.3269(19) . ?
C4 F11 1.333(3) . ?
C5 N1 1.490(3) . ?
C5 H5A 0.9504(10) . ?
C5 H5B 0.9507(10) . ?
C6 N1 1.490(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 N1 1.508(3) . ?
C7 H7A 0.9504(10) . ?
C7 H7B 0.9506(10) . ?
N1 C6 1.490(2) 7_565 ?
F1 P1 1.6212(14) . ?
F2 P1 1.6201(14) . ?
F3 P1 1.6309(14) . ?
P1 C1 1.9403(19) 7_565 ?

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
F4 C1 F5 104.13(13) . . ?
F4 C1 C2 104.98(14) . . ?
F5 C1 C2 104.98(14) . . ?
F4 C1 P1 108.60(12) . . ?
F5 C1 P1 114.07(11) . . ?
C2 C1 P1 118.78(12) . . ?
F8 C2 F7 108.84(15) . . ?
F8 C2 F6 107.75(15) . . ?
F7 C2 F6 106.72(15) . . ?
F8 C2 C1 112.38(15) . . ?
F7 C2 C1 111.42(15) . . ?
F6 C2 C1 109.52(15) . . ?
F9 C3 F9 104.35(17) . 7_565 ?
F9 C3 C4 105.32(13) . . ?
F9 C3 C4 105.32(13) 7_565 . ?
F9 C3 P1 109.39(12) . . ?
F9 C3 P1 109.39(12) 7_565 . ?
C4 C3 P1 121.71(16) . . ?
F10 C4 F10 108.1(2) 7_565 . ?
F10 C4 F11 107.90(14) 7_565 . ?
F10 C4 F11 107.90(14) . . ?
F10 C4 C3 111.88(14) 7_565 . ?
F10 C4 C3 111.88(14) . . ?
F11 C4 C3 109.0(2) . . ?
N1 C5 H5A 107.2(15) . . ?
N1 C5 H5B 101.9(8) . . ?
H5A C5 H5B 114.59(16) . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 H7A 105.7(13) . . ?
N1 C7 H7B 102.6(7) . . ?
H7A C7 H7B 114.61(16) . . ?
C5 N1 C6 109.89(13) . . ?
C5 N1 C6 109.89(13) . 7_565 ?
C6 N1 C6 109.3(2) . 7_565 ?
C5 N1 C7 109.52(19) . . ?
C6 N1 C7 109.09(12) . . ?
C6 N1 C7 109.09(12) 7_565 . ?
F2 P1 F1 90.21(8) . . ?
F2 P1 F3 92.28(7) . . ?
F1 P1 F3 177.51(7) . . ?
F2 P1 C1 85.20(5) . . ?
F1 P1 C1 92.49(5) . . ?
F3 P1 C1 87.72(5) . . ?
F2 P1 C1 85.20(5) . 7_565 ?
F1 P1 C1 92.49(5) . 7_565 ?
F3 P1 C1 87.72(5) . 7_565 ?
C1 P1 C1 169.19(10) . 7_565 ?
F2 P1 C3 176.44(9) . . ?
F1 P1 C3 86.22(9) . . ?
F3 P1 C3 91.28(9) . . ?
C1 P1 C3 94.95(5) . . ?
C1 P1 C3 94.95(5) 7_565 . ?

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
F4 C1 C2 F8 172.12(15) . . . . ?
F5 C1 C2 F8 62.66(18) . . . . ?
P1 C1 C2 F8 -66.30(18) . . . . ?
F4 C1 C2 F7 -65.43(18) . . . . ?
F5 C1 C2 F7 -174.89(14) . . . . ?
P1 C1 C2 F7 56.15(19) . . . . ?
F4 C1 C2 F6 52.40(19) . . . . ?
F5 C1 C2 F6 -57.06(18) . . . . ?
P1 C1 C2 F6 173.98(11) . . . . ?
F9 C3 C4 F10 -174.24(15) . . . 7_565 ?
F9 C3 C4 F10 -64.3(2) 7_565 . . 7_565 ?
P1 C3 C4 F10 60.75(15) . . . 7_565 ?
F9 C3 C4 F10 64.3(2) . . . . ?
F9 C3 C4 F10 174.24(15) 7_565 . . . ?
P1 C3 C4 F10 -60.75(15) . . . . ?
F9 C3 C4 F11 -54.99(11) . . . . ?
F9 C3 C4 F11 54.99(11) 7_565 . . . ?
P1 C3 C4 F11 180.0 . . . . ?
F4 C1 P1 F2 43.15(11) . . . . ?
F5 C1 P1 F2 158.78(13) . . . . ?
C2 C1 P1 F2 -76.58(14) . . . . ?
F4 C1 P1 F1 133.16(11) . . . . ?
F5 C1 P1 F1 -111.22(12) . . . . ?
C2 C1 P1 F1 13.42(14) . . . . ?
F4 C1 P1 F3 -49.33(11) . . . . ?
F5 C1 P1 F3 66.30(12) . . . . ?
C2 C1 P1 F3 -169.06(14) . . . . ?
F4 C1 P1 C1 15.8(6) . . . 7_565 ?
F5 C1 P1 C1 131.4(5) . . . 7_565 ?
C2 C1 P1 C1 -103.9(5) . . . 7_565 ?
F4 C1 P1 C3 -140.42(12) . . . . ?
F5 C1 P1 C3 -24.79(13) . . . . ?
C2 C1 P1 C3 99.85(15) . . . . ?
F9 C3 P1 F2 56.87(12) . . . . ?
F9 C3 P1 F2 -56.87(12) 7_565 . . . ?
C4 C3 P1 F2 180.0 . . . . ?
F9 C3 P1 F1 56.87(12) . . . . ?
F9 C3 P1 F1 -56.87(12) 7_565 . . . ?
C4 C3 P1 F1 180.0 . . . . ?
F9 C3 P1 F3 -123.13(12) . . . . ?
F9 C3 P1 F3 123.13(12) 7_565 . . . ?
C4 C3 P1 F3 0.0 . . . . ?
F9 C3 P1 C1 -35.31(13) . . . . ?
F9 C3 P1 C1 -149.04(12) 7_565 . . . ?
C4 C3 P1 C1 87.82(5) . . . . ?
F9 C3 P1 C1 149.04(12) . . . 7_565 ?
F9 C3 P1 C1 35.31(13) 7_565 . . 7_565 ?
C4 C3 P1 C1 -87.82(5) . . . 7_565 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.076
####################################################################### 
# 
# 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_2013dcp026
_database_code_depnum_ccdc_archive 'CCDC 1432361'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 F18 P, C16 H36 N'
_chemical_formula_sum            'C22 H36 F18 N P'
_chemical_formula_weight         687.49

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'
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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61

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'
'-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                   17.591(3)
_cell_length_b                   17.971(3)
_cell_length_c                   18.534(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5859.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14752
_cell_measurement_theta_min      1.6
_cell_measurement_theta_max      34.8

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9846
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35369
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6685
_reflns_number_gt                5395
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2σ(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)+(0.0260P)²+4.3898P] 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         6685
_refine_ls_number_parameters     549
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0745
_refine_ls_wR_factor_ref         0.1240
_refine_ls_wR_factor_gt          0.1165
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_restrained_S_all      1.184
_refine_ls_shift/su_max          0.017
_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
C1 C 0.87304(19) 0.11545(17) 0.64374(17) 0.0213(7) Uani 0.8207(17) 1 d P A 1
C2 C 0.7935(3) 0.0838(2) 0.6623(2) 0.0307(10) Uani 0.8207(17) 1 d P A 1
C3 C 0.96940(19) 0.11507(18) 0.76923(17) 0.0218(7) Uani 0.8207(17) 1 d P A 1
C4 C 1.0529(2) 0.0917(2) 0.7592(2) 0.0254(9) Uani 0.8207(17) 1 d P A 1
C5 C 0.8852(3) 0.2741(3) 0.6490(4) 0.0168(10) Uani 0.8207(17) 1 d P A 1
C6 C 0.8880(4) 0.3500(4) 0.6877(3) 0.0279(12) Uani 0.8207(17) 1 d P A 1
C7 C 1.04896(14) 0.12543(14) 0.45816(14) 0.0184(5) Uani 1 1 d . . .
H7A H 1.0437 0.1178 0.5108 0.022 Uiso 1 1 calc R . .
H7B H 1.0754 0.0813 0.4384 0.022 Uiso 1 1 calc R . .
C8 C 0.96926(14) 0.12848(15) 0.42532(14) 0.0212(6) Uani 1 1 d . . .
H8A H 0.9404 0.1705 0.4463 0.025 Uiso 1 1 calc R . .
H8B H 0.9728 0.1362 0.3725 0.025 Uiso 1 1 calc R . .
C9 C 0.92864(14) 0.05541(14) 0.44119(14) 0.0207(6) Uani 1 1 d . . .
H9A H 0.9300 0.0459 0.4938 0.025 Uiso 1 1 calc R . .
H9B H 0.9560 0.0143 0.4170 0.025 Uiso 1 1 calc R . .
C10 C 0.84623(16) 0.05590(16) 0.41581(16) 0.0280(7) Uani 1 1 d . . .
H10A H 0.8192 0.0974 0.4386 0.042 Uiso 1 1 calc R . .
H10B H 0.8218 0.0089 0.4292 0.042 Uiso 1 1 calc R . .
H10C H 0.8447 0.0618 0.3633 0.042 Uiso 1 1 calc R . .
C11 C 1.11017(14) 0.20864(13) 0.36601(13) 0.0168(5) Uani 1 1 d . . .
H11A H 1.1480 0.2491 0.3610 0.020 Uiso 1 1 calc R . .
H11B H 1.0614 0.2274 0.3465 0.020 Uiso 1 1 calc R . .
C12 C 1.13597(15) 0.14347(14) 0.31925(13) 0.0195(6) Uani 1 1 d . . .
H12A H 1.0955 0.1053 0.3172 0.023 Uiso 1 1 calc R . .
H12B H 1.1820 0.1204 0.3404 0.023 Uiso 1 1 calc R . .
C13 C 1.15339(16) 0.17190(14) 0.24311(13) 0.0204(6) Uani 1 1 d . . .
H13A H 1.1081 0.1979 0.2239 0.025 Uiso 1 1 calc R . .
H13B H 1.1955 0.2083 0.2456 0.025 Uiso 1 1 calc R . .
C14 C 1.17522(17) 0.10965(16) 0.19203(15) 0.0269(6) Uani 1 1 d . . .
H14A H 1.2199 0.0836 0.2109 0.040 Uiso 1 1 calc R . .
H14B H 1.1871 0.1305 0.1445 0.040 Uiso 1 1 calc R . .
H14C H 1.1328 0.0746 0.1877 0.040 Uiso 1 1 calc R . .
C15 C 1.06244(14) 0.26077(14) 0.48073(14) 0.0189(5) Uani 1 1 d . . .
H15A H 1.0135 0.2703 0.4561 0.023 Uiso 1 1 calc R . .
H15B H 1.0509 0.2487 0.5317 0.023 Uiso 1 1 calc R . .
C16 C 1.10908(15) 0.33208(14) 0.47913(14) 0.0211(6) Uani 1 1 d . . .
H16A H 1.1192 0.3465 0.4285 0.025 Uiso 1 1 calc R . .
H16B H 1.1585 0.3237 0.5033 0.025 Uiso 1 1 calc R . .
C17 C 1.06629(16) 0.39450(15) 0.51736(17) 0.0287(7) Uani 1 1 d . . .
H17A H 1.0159 0.4008 0.4944 0.034 Uiso 1 1 calc R . .
H17B H 1.0579 0.3803 0.5684 0.034 Uiso 1 1 calc R . .
C18 C 1.10876(18) 0.46824(15) 0.51480(17) 0.0338(7) Uani 1 1 d . . .
H18A H 1.1597 0.4617 0.5352 0.051 Uiso 1 1 calc R . .
H18B H 1.0809 0.5055 0.5429 0.051 Uiso 1 1 calc R . .
H18C H 1.1130 0.4849 0.4646 0.051 Uiso 1 1 calc R . .
C19 C 1.17681(14) 0.17719(14) 0.47975(14) 0.0192(6) Uani 1 1 d . . .
H19A H 1.1969 0.1306 0.4585 0.023 Uiso 1 1 calc R . .
H19B H 1.2119 0.2178 0.4658 0.023 Uiso 1 1 calc R . .
C20 C 1.17854(16) 0.16962(16) 0.56145(14) 0.0251(6) Uani 1 1 d . . .
H20A H 1.1454 0.1279 0.5765 0.030 Uiso 1 1 calc R . .
H20B H 1.1590 0.2158 0.5839 0.030 Uiso 1 1 calc R . .
C21 C 1.26000(17) 0.15524(17) 0.58724(16) 0.0312(7) Uani 1 1 d . . .
H21A H 1.2587 0.1401 0.6386 0.037 Uiso 1 1 calc R . .
H21B H 1.2817 0.1135 0.5592 0.037 Uiso 1 1 calc R . .
C22 C 1.31140(17) 0.22251(18) 0.57946(17) 0.0369(8) Uani 1 1 d . . .
H22A H 1.3155 0.2360 0.5284 0.055 Uiso 1 1 calc R . .
H22B H 1.3620 0.2106 0.5984 0.055 Uiso 1 1 calc R . .
H22C H 1.2899 0.2644 0.6066 0.055 Uiso 1 1 calc R . .
N1 N 1.09942(11) 0.19294(11) 0.44603(11) 0.0162(4) Uani 1 1 d . . .
F1 F 0.99622(11) 0.18114(12) 0.64816(10) 0.0225(4) Uani 0.8207(17) 1 d P A 1
F2 F 0.97273(11) 0.24958(12) 0.75106(10) 0.0237(5) Uani 0.8207(17) 1 d P A 1
F3 F 0.85267(11) 0.19421(10) 0.75780(9) 0.0220(4) Uani 0.8207(17) 1 d P A 1
F4 F 0.86537(12) 0.14369(11) 0.57549(10) 0.0283(5) Uani 0.8207(17) 1 d P A 1
F5 F 0.91853(11) 0.05388(10) 0.63552(11) 0.0285(5) Uani 0.8207(17) 1 d P A 1
F6 F 0.73999(11) 0.13599(12) 0.65920(14) 0.0373(6) Uani 0.8207(17) 1 d P A 1
F7 F 0.77505(16) 0.03179(13) 0.61216(15) 0.0498(7) Uani 0.8207(17) 1 d P A 1
F8 F 0.79010(13) 0.05151(12) 0.72585(13) 0.0402(6) Uani 0.8207(17) 1 d P A 1
F9 F 0.96766(12) 0.14386(12) 0.83818(10) 0.0307(5) Uani 0.8207(17) 1 d P A 1
F10 F 0.92896(12) 0.05084(11) 0.77304(11) 0.0323(5) Uani 0.8207(17) 1 d P A 1
F11 F 1.06280(12) 0.05223(12) 0.69884(12) 0.0357(6) Uani 0.8207(17) 1 d P A 1
F12 F 1.0992(3) 0.1500(3) 0.7573(2) 0.0345(10) Uani 0.8207(17) 1 d P A 1
F13 F 1.07481(18) 0.04839(15) 0.81444(15) 0.0391(7) Uani 0.8207(17) 1 d P A 1
F14 F 0.9174(2) 0.28081(15) 0.5849(2) 0.0259(6) Uani 0.8207(17) 1 d P A 1
F15 F 0.8076(2) 0.2615(2) 0.63772(17) 0.0208(7) Uani 0.8207(17) 1 d P A 1
F16 F 0.8489(5) 0.4000(4) 0.6490(4) 0.0477(15) Uani 0.8207(17) 1 d P A 1
F17 F 0.8554(4) 0.3481(4) 0.7527(4) 0.0470(15) Uani 0.8207(17) 1 d P A 1
F18 F 0.9589(5) 0.3744(5) 0.6928(4) 0.0567(15) Uani 0.8207(17) 1 d P A 1
P1 P 0.92554(9) 0.18846(9) 0.70407(7) 0.0153(3) Uani 0.8207(17) 1 d P A 1
C1A C 0.9966(10) 0.0954(9) 0.7016(9) 0.033(3) Uani 0.1793(17) 1 d PD A 2
C2A C 1.0363(9) 0.0886(9) 0.7753(8) 0.033(3) Uani 0.1793(17) 1 d PD A 2
C3A C 0.8387(9) 0.1313(9) 0.7040(9) 0.033(3) Uani 0.1793(17) 1 d PD A 2
C4A C 0.7929(8) 0.0866(8) 0.6477(8) 0.033(3) Uani 0.1793(17) 1 d PD A 2
C5A C 0.885(2) 0.2618(18) 0.655(3) 0.033(3) Uani 0.1793(17) 1 d PD A 2
C6A C 0.8915(18) 0.3444(18) 0.6760(17) 0.033(3) Uani 0.1793(17) 1 d PD A 2
F1A F 0.9300(5) 0.1519(5) 0.5979(4) 0.026(2) Uani 0.1793(17) 1 d P A 2
F2A F 1.0145(5) 0.2255(5) 0.6658(5) 0.030(2) Uani 0.1793(17) 1 d P A 2
F3A F 0.9381(6) 0.2104(5) 0.7643(5) 0.027(2) Uani 0.1793(17) 1 d P A 2
F4A F 0.9597(5) 0.0296(4) 0.6908(5) 0.030(2) Uani 0.1793(17) 1 d P A 2
F5A F 1.0554(5) 0.0933(5) 0.6533(6) 0.033(2) Uani 0.1793(17) 1 d P A 2
F6A F 0.9882(7) 0.0822(7) 0.8301(6) 0.059(4) Uani 0.1793(17) 1 d PD A 2
F7A F 1.0818(8) 0.0288(7) 0.7770(8) 0.045(3) Uani 0.1793(17) 1 d PD A 2
F8A F 1.0821(13) 0.1471(13) 0.7861(12) 0.059(7) Uani 0.1793(17) 1 d PD A 2
F9A F 0.8520(6) 0.0839(6) 0.7617(6) 0.044(3) Uani 0.1793(17) 1 d P A 2
F10A F 0.7902(6) 0.1836(5) 0.7323(6) 0.038(3) Uani 0.1793(17) 1 d P A 2
F11A F 0.8324(6) 0.0299(5) 0.6189(7) 0.045(3) Uani 0.1793(17) 1 d PD A 2
F12A F 0.7693(6) 0.1298(6) 0.5930(7) 0.057(4) Uani 0.1793(17) 1 d PD A 2
F13A F 0.7316(6) 0.0565(7) 0.6798(9) 0.074(5) Uani 0.1793(17) 1 d PD A 2
F14A F 0.9262(12) 0.3013(9) 0.5818(11) 0.0259(6) Uani 0.1793(17) 1 d P A 2
F15A F 0.8161(14) 0.2699(14) 0.6239(11) 0.0259(6) Uani 0.1793(17) 1 d PD A 2
F16A F 0.851(2) 0.3938(17) 0.6376(15) 0.0259(6) Uani 0.1793(17) 1 d PD A 2
F17A F 0.866(2) 0.3537(18) 0.7438(18) 0.0259(6) Uani 0.1793(17) 1 d PD A 2
F18A F 0.960(2) 0.377(2) 0.6815(15) 0.0259(6) Uani 0.1793(17) 1 d PD A 2
P1A P 0.9328(6) 0.1807(6) 0.6786(4) 0.038(2) Uani 0.1793(17) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 F4 1.370(4) . ?
C1 F5 1.374(3) . ?
C1 C2 1.549(6) . ?
C1 P1 1.956(4) . ?
C2 F8 1.315(5) . ?
C2 F6 1.331(5) . ?
C2 F7 1.356(5) . ?
C3 F10 1.358(4) . ?
C3 F9 1.379(4) . ?
C3 C4 1.539(5) . ?
C3 P1 1.948(4) . ?
C4 F12 1.327(5) . ?
C4 F11 1.336(4) . ?
C4 F13 1.343(4) . ?
C5 F14 1.324(9) . ?
C5 F15 1.399(5) . ?
C5 C6 1.541(5) . ?
C5 P1 1.979(5) . ?
C6 F18 1.327(5) . ?
C6 F17 1.335(5) . ?
C6 F16 1.338(5) . ?
C7 N1 1.520(3) . ?
C7 C8 1.529(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.524(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.524(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N1 1.522(3) . ?
C11 C12 1.526(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.532(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.515(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.522(3) . ?
C15 N1 1.524(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.525(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.522(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.521(4) . ?
C19 N1 1.524(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.533(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.517(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
F1 P1 1.624(2) . ?
F2 P1 1.629(3) . ?
F3 P1 1.626(2) . ?
C1A F4A 1.364(18) . ?
C1A F5A 1.368(19) . ?
C1A C2A 1.539(10) . ?
C1A P1A 1.95(2) . ?
C2A F6A 1.326(10) . ?
C2A F7A 1.340(10) . ?
C2A F8A 1.340(10) . ?
C3A F10A 1.374(18) . ?
C3A F9A 1.387(19) . ?
C3A C4A 1.544(10) . ?
C3A P1A 1.94(2) . ?
C4A F12A 1.341(10) . ?
C4A F11A 1.344(10) . ?
C4A F13A 1.345(10) . ?
C5A F15A 1.347(10) . ?
C5A C6A 1.540(10) . ?
C5A F14A 1.69(5) . ?
C5A P1A 1.74(3) . ?
C6A F16A 1.342(10) . ?
C6A F17A 1.344(10) . ?
C6A F18A 1.345(10) . ?
F1A P1A 1.584(11) . ?
F2A P1A 1.664(15) . ?
F3A P1A 1.678(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F4 C1 F5 104.7(2) . . ?
F4 C1 C2 104.6(3) . . ?
F5 C1 C2 104.7(3) . . ?
F4 C1 P1 109.0(2) . . ?
F5 C1 P1 109.2(2) . . ?
C2 C1 P1 123.1(3) . . ?
F8 C2 F6 108.5(4) . . ?
F8 C2 F7 107.4(3) . . ?
F6 C2 F7 106.7(3) . . ?
F8 C2 C1 113.7(3) . . ?
F6 C2 C1 111.7(3) . . ?
F7 C2 C1 108.5(4) . . ?
F10 C3 F9 105.0(3) . . ?
F10 C3 C4 105.9(3) . . ?
F9 C3 C4 103.6(3) . . ?
F10 C3 P1 113.6(2) . . ?
F9 C3 P1 108.2(2) . . ?
C4 C3 P1 119.2(2) . . ?
F12 C4 F11 108.5(4) . . ?
F12 C4 F13 107.6(4) . . ?
F11 C4 F13 107.1(3) . . ?
F12 C4 C3 111.9(4) . . ?
F11 C4 C3 111.7(3) . . ?
F13 C4 C3 109.9(3) . . ?
F14 C5 F15 107.4(4) . . ?
F14 C5 C6 108.9(4) . . ?
F15 C5 C6 104.2(5) . . ?
F14 C5 P1 112.3(4) . . ?
F15 C5 P1 107.5(3) . . ?
C6 C5 P1 116.0(5) . . ?
F18 C6 F17 110.3(6) . . ?
F18 C6 F16 107.5(8) . . ?
F17 C6 F16 106.3(6) . . ?
F18 C6 C5 110.9(6) . . ?
F17 C6 C5 112.5(7) . . ?
F16 C6 C5 109.2(5) . . ?
N1 C7 C8 116.6(2) . . ?
N1 C7 H7A 108.1 . . ?
C8 C7 H7A 108.1 . . ?
N1 C7 H7B 108.1 . . ?
C8 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C9 C8 C7 108.8(2) . . ?
C9 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
C9 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
C8 C9 C10 112.4(2) . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C12 116.6(2) . . ?
N1 C11 H11A 108.1 . . ?
C12 C11 H11A 108.1 . . ?
N1 C11 H11B 108.1 . . ?
C12 C11 H11B 108.1 . . ?
H11A C11 H11B 107.3 . . ?
C11 C12 C13 109.1(2) . . ?
C11 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C14 C13 C12 112.3(2) . . ?
C14 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N1 115.8(2) . . ?
C16 C15 H15A 108.3 . . ?
N1 C15 H15A 108.3 . . ?
C16 C15 H15B 108.3 . . ?
N1 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 C17 110.1(2) . . ?
C15 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C18 C17 C16 112.6(2) . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N1 116.3(2) . . ?
C20 C19 H19A 108.2 . . ?
N1 C19 H19A 108.2 . . ?
C20 C19 H19B 108.2 . . ?
N1 C19 H19B 108.2 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 C21 110.1(2) . . ?
C19 C20 H20A 109.6 . . ?
C21 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C21 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C22 C21 C20 113.2(2) . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C7 N1 C11 111.40(18) . . ?
C7 N1 C15 109.07(18) . . ?
C11 N1 C15 108.43(18) . . ?
C7 N1 C19 108.22(18) . . ?
C11 N1 C19 108.85(18) . . ?
C15 N1 C19 110.89(19) . . ?
F1 P1 F3 177.80(15) . . ?
F1 P1 F2 90.32(13) . . ?
F3 P1 F2 91.81(12) . . ?
F1 P1 C3 92.15(14) . . ?
F3 P1 C3 88.61(14) . . ?
F2 P1 C3 85.60(13) . . ?
F1 P1 C1 86.69(14) . . ?
F3 P1 C1 91.18(14) . . ?
F2 P1 C1 176.97(16) . . ?
C3 P1 C1 95.01(15) . . ?
F1 P1 C5 90.5(3) . . ?
F3 P1 C5 89.0(3) . . ?
F2 P1 C5 86.20(19) . . ?
C3 P1 C5 171.4(2) . . ?
C1 P1 C5 93.3(2) . . ?
F4A C1A F5A 103.9(12) . . ?
F4A C1A C2A 106.1(13) . . ?
F5A C1A C2A 103.6(12) . . ?
F4A C1A P1A 112.1(11) . . ?
F5A C1A P1A 108.2(11) . . ?
C2A C1A P1A 121.2(11) . . ?
F6A C2A F7A 107.0(14) . . ?
F6A C2A F8A 109.7(16) . . ?
F7A C2A F8A 105.5(17) . . ?
F6A C2A C1A 113.4(13) . . ?
F7A C2A C1A 110.9(14) . . ?
F8A C2A C1A 110.1(15) . . ?
F10A C3A F9A 103.3(12) . . ?
F10A C3A C4A 106.9(12) . . ?
F9A C3A C4A 106.8(12) . . ?
F10A C3A P1A 108.0(10) . . ?
F9A C3A P1A 108.9(11) . . ?
C4A C3A P1A 121.4(11) . . ?
F12A C4A F11A 107.4(12) . . ?
F12A C4A F13A 108.6(14) . . ?
F11A C4A F13A 106.5(12) . . ?
F12A C4A C3A 111.8(12) . . ?
F11A C4A C3A 113.1(12) . . ?
F13A C4A C3A 109.2(12) . . ?
F15A C5A C6A 94(2) . . ?
F15A C5A F14A 90(3) . . ?
C6A C5A F14A 76(2) . . ?
F15A C5A P1A 129(2) . . ?
C6A C5A P1A 135(2) . . ?
F14A C5A P1A 110(3) . . ?
F16A C6A F17A 104(3) . . ?
F16A C6A F18A 103(3) . . ?
F17A C6A F18A 100(3) . . ?
F16A C6A C5A 118(3) . . ?
F17A C6A C5A 109(4) . . ?
F18A C6A C5A 121(3) . . ?
F1A P1A F2A 92.9(6) . . ?
F1A P1A F3A 178.6(9) . . ?
F2A P1A F3A 86.2(7) . . ?
F1A P1A C5A 91.1(17) . . ?
F2A P1A C5A 88.7(14) . . ?
F3A P1A C5A 90.0(17) . . ?
F1A P1A C3A 93.0(7) . . ?
F2A P1A C3A 174.1(8) . . ?
F3A P1A C3A 87.9(7) . . ?
C5A P1A C3A 91.8(15) . . ?
F1A P1A C1A 88.1(7) . . ?
F2A P1A C1A 85.1(8) . . ?
F3A P1A C1A 90.7(7) . . ?
C5A P1A C1A 173.7(16) . . ?
C3A P1A C1A 94.5(8) . . ?

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
F4 C1 C2 F8 177.9(3) . . . . ?
F5 C1 C2 F8 68.0(4) . . . . ?
P1 C1 C2 F8 -57.2(4) . . . . ?
F4 C1 C2 F6 -59.0(4) . . . . ?
F5 C1 C2 F6 -168.8(3) . . . . ?
P1 C1 C2 F6 65.9(4) . . . . ?
F4 C1 C2 F7 58.4(4) . . . . ?
F5 C1 C2 F7 -51.4(4) . . . . ?
P1 C1 C2 F7 -176.7(2) . . . . ?
F10 C3 C4 F12 -177.7(3) . . . . ?
F9 C3 C4 F12 -67.5(4) . . . . ?
P1 C3 C4 F12 52.7(4) . . . . ?
F10 C3 C4 F11 60.4(4) . . . . ?
F9 C3 C4 F11 170.6(3) . . . . ?
P1 C3 C4 F11 -69.2(4) . . . . ?
F10 C3 C4 F13 -58.3(4) . . . . ?
F9 C3 C4 F13 52.0(4) . . . . ?
P1 C3 C4 F13 172.2(2) . . . . ?
F14 C5 C6 F18 -56.8(6) . . . . ?
F15 C5 C6 F18 -171.1(5) . . . . ?
P1 C5 C6 F18 71.0(7) . . . . ?
F14 C5 C6 F17 179.1(6) . . . . ?
F15 C5 C6 F17 64.8(7) . . . . ?
P1 C5 C6 F17 -53.1(7) . . . . ?
F14 C5 C6 F16 61.4(7) . . . . ?
F15 C5 C6 F16 -52.9(7) . . . . ?
P1 C5 C6 F16 -170.8(5) . . . . ?
N1 C7 C8 C9 178.3(2) . . . . ?
C7 C8 C9 C10 175.2(2) . . . . ?
N1 C11 C12 C13 -172.8(2) . . . . ?
C11 C12 C13 C14 -176.8(2) . . . . ?
N1 C15 C16 C17 -178.4(2) . . . . ?
C15 C16 C17 C18 -177.6(2) . . . . ?
N1 C19 C20 C21 -179.1(2) . . . . ?
C19 C20 C21 C22 70.4(3) . . . . ?
C8 C7 N1 C11 -57.8(3) . . . . ?
C8 C7 N1 C15 61.9(3) . . . . ?
C8 C7 N1 C19 -177.4(2) . . . . ?
C12 C11 N1 C7 -51.5(3) . . . . ?
C12 C11 N1 C15 -171.5(2) . . . . ?
C12 C11 N1 C19 67.8(3) . . . . ?
C16 C15 N1 C7 174.9(2) . . . . ?
C16 C15 N1 C11 -63.6(3) . . . . ?
C16 C15 N1 C19 55.9(3) . . . . ?
C20 C19 N1 C7 -66.1(3) . . . . ?
C20 C19 N1 C11 172.7(2) . . . . ?
C20 C19 N1 C15 53.5(3) . . . . ?
F10 C3 P1 F1 -112.5(2) . . . . ?
F9 C3 P1 F1 131.3(2) . . . . ?
C4 C3 P1 F1 13.5(3) . . . . ?
F10 C3 P1 F3 65.4(2) . . . . ?
F9 C3 P1 F3 -50.7(2) . . . . ?
C4 C3 P1 F3 -168.6(3) . . . . ?
F10 C3 P1 F2 157.3(2) . . . . ?
F9 C3 P1 F2 41.2(2) . . . . ?
C4 C3 P1 F2 -76.7(3) . . . . ?
F10 C3 P1 C1 -25.6(3) . . . . ?
F9 C3 P1 C1 -141.8(2) . . . . ?
C4 C3 P1 C1 100.3(3) . . . . ?
F4 C1 P1 F1 -60.5(2) . . . . ?
F5 C1 P1 F1 53.3(2) . . . . ?
C2 C1 P1 F1 176.6(3) . . . . ?
F4 C1 P1 F3 119.0(2) . . . . ?
F5 C1 P1 F3 -127.2(2) . . . . ?
C2 C1 P1 F3 -3.9(3) . . . . ?
F4 C1 P1 C3 -152.3(2) . . . . ?
F5 C1 P1 C3 -38.5(2) . . . . ?
C2 C1 P1 C3 84.8(3) . . . . ?
F4 C1 P1 C5 29.9(3) . . . . ?
F5 C1 P1 C5 143.7(3) . . . . ?
C2 C1 P1 C5 -93.0(4) . . . . ?
F14 C5 P1 F1 13.9(3) . . . . ?
F15 C5 P1 F1 131.8(5) . . . . ?
C6 C5 P1 F1 -112.2(5) . . . . ?
F14 C5 P1 F3 -164.0(3) . . . . ?
F15 C5 P1 F3 -46.1(5) . . . . ?
C6 C5 P1 F3 70.0(5) . . . . ?
F14 C5 P1 F2 104.2(3) . . . . ?
F15 C5 P1 F2 -138.0(5) . . . . ?
C6 C5 P1 F2 -21.9(5) . . . . ?
F14 C5 P1 C1 -72.8(3) . . . . ?
F15 C5 P1 C1 45.0(5) . . . . ?
C6 C5 P1 C1 161.1(5) . . . . ?
F4A C1A C2A F6A -64.7(17) . . . . ?
F5A C1A C2A F6A -173.9(13) . . . . ?
P1A C1A C2A F6A 64.6(18) . . . . ?
F4A C1A C2A F7A 55.6(17) . . . . ?
F5A C1A C2A F7A -53.5(17) . . . . ?
P1A C1A C2A F7A -175.1(12) . . . . ?
F4A C1A C2A F8A 171.9(15) . . . . ?
F5A C1A C2A F8A 62.8(18) . . . . ?
P1A C1A C2A F8A -58.7(19) . . . . ?
F10A C3A C4A F12A 62.8(16) . . . . ?
F9A C3A C4A F12A 172.8(12) . . . . ?
P1A C3A C4A F12A -61.6(16) . . . . ?
F10A C3A C4A F11A -175.8(12) . . . . ?
F9A C3A C4A F11A -65.8(16) . . . . ?
P1A C3A C4A F11A 59.8(17) . . . . ?
F10A C3A C4A F13A -57.4(15) . . . . ?
F9A C3A C4A F13A 52.7(16) . . . . ?
P1A C3A C4A F13A 178.2(11) . . . . ?
F15A C5A C6A F16A -24(4) . . . . ?
F14A C5A C6A F16A 65(3) . . . . ?
P1A C5A C6A F16A 170(4) . . . . ?
F15A C5A C6A F17A 94(4) . . . . ?
F14A C5A C6A F17A -177(3) . . . . ?
P1A C5A C6A F17A -72(6) . . . . ?
F15A C5A C6A F18A -151(3) . . . . ?
F14A C5A C6A F18A -62(3) . . . . ?
P1A C5A C6A F18A 43(7) . . . . ?
F15A C5A P1A F1A 58(5) . . . . ?
C6A C5A P1A F1A -140(5) . . . . ?
F14A C5A P1A F1A -49.3(18) . . . . ?
F15A C5A P1A F2A 151(5) . . . . ?
C6A C5A P1A F2A -47(5) . . . . ?
F14A C5A P1A F2A 43.6(17) . . . . ?
F15A C5A P1A F3A -123(5) . . . . ?
C6A C5A P1A F3A 39(5) . . . . ?
F14A C5A P1A F3A 129.8(17) . . . . ?
F15A C5A P1A C3A -35(5) . . . . ?
C6A C5A P1A C3A 127(5) . . . . ?
F14A C5A P1A C3A -142.4(17) . . . . ?
F10A C3A P1A F1A -125.4(11) . . . . ?
F9A C3A P1A F1A 123.1(11) . . . . ?
C4A C3A P1A F1A -1.5(14) . . . . ?
F10A C3A P1A F3A 55.8(11) . . . . ?
F9A C3A P1A F3A -55.8(11) . . . . ?
C4A C3A P1A F3A 179.6(13) . . . . ?
F10A C3A P1A C5A -34.2(19) . . . . ?
F9A C3A P1A C5A -145.7(19) . . . . ?
C4A C3A P1A C5A 90(2) . . . . ?
F10A C3A P1A C1A 146.3(11) . . . . ?
F9A C3A P1A C1A 34.7(11) . . . . ?
C4A C3A P1A C1A -89.9(13) . . . . ?
F4A C1A P1A F1A -62.7(11) . . . . ?
F5A C1A P1A F1A 51.4(11) . . . . ?
C2A C1A P1A F1A 170.7(13) . . . . ?
F4A C1A P1A F2A -155.7(11) . . . . ?
F5A C1A P1A F2A -41.7(11) . . . . ?
C2A C1A P1A F2A 77.6(13) . . . . ?
F4A C1A P1A F3A 118.1(11) . . . . ?
F5A C1A P1A F3A -127.8(11) . . . . ?
C2A C1A P1A F3A -8.5(14) . . . . ?
F4A C1A P1A C3A 30.2(12) . . . . ?
F5A C1A P1A C3A 144.2(11) . . . . ?
C2A C1A P1A C3A -96.4(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.056
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1432362'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 N, C2 F6 N O4 S2'
_chemical_formula_sum            'C18 H36 F6 N2 O4 S2'
_chemical_formula_weight         522.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.312(6)
_cell_length_b                   28.997(13)
_cell_length_c                   13.523(6)
_cell_angle_alpha                90
_cell_angle_beta                 94.059(9)
_cell_angle_gamma                90
_cell_volume                     5207(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10858
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      31.2

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             2208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.272
_shelx_estimated_absorpt_T_min   0.981
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r11 (Rigaku, 2011)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            21991
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.958
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_point_group_measured_fraction_full 0.836
_reflns_number_total             17489
_reflns_number_gt                12466
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.632
_reflns_Friedel_fraction_max     0.649
_reflns_Friedel_fraction_full    0.674

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

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

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0587P)²+7.6416P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3195 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.11(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         17489
_refine_ls_number_parameters     1212
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0947
_refine_ls_wR_factor_ref         0.2122
_refine_ls_wR_factor_gt          0.1823
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3939(9) 0.2638(4) 0.1866(9) 0.055(3) Uani 1 1 d . . . . .
C2 C 0.0835(10) 0.2709(4) 0.3836(9) 0.048(3) Uani 1 1 d . . . . .
C3 C 0.2862(11) 0.5149(6) 0.9108(9) 0.070(4) Uani 1 1 d . . . . .
C4 C 0.1017(10) 0.5125(4) 0.5683(8) 0.050(3) Uani 1 1 d . . . . .
C5 C 0.3374(10) 0.0552(4) 0.9331(9) 0.055(3) Uani 1 1 d . . . . .
C6 C 0.2810(9) 0.0234(4) 0.5612(8) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.5433(10) 0.2780(5) 0.8939(14) 0.077(5) Uani 1 1 d . . . . .
C8A C 0.8903(19) 0.2760(10) 0.792(2) 0.052(6) Uani 0.577(9) 1 d . . P A 1
C8B C 0.892(3) 0.2838(14) 0.736(3) 0.052(6) Uani 0.423(9) 1 d . . P A 2
C9 C 0.6357(10) -0.1418(5) 0.4431(10) 0.061(3) Uani 1 1 d . . . . .
H9A H 0.6486 -0.1671 0.4914 0.073 Uiso 1 1 calc R U . . .
H9B H 0.5902 -0.1538 0.3880 0.073 Uiso 1 1 calc R U . . .
C10 C 0.7324(10) -0.1282(5) 0.4033(12) 0.078(5) Uani 1 1 d . . . . .
H10A H 0.7863 -0.1267 0.4576 0.093 Uiso 1 1 calc R U . . .
H10B H 0.7260 -0.0973 0.3720 0.093 Uiso 1 1 calc R U . . .
C11 C 0.7602(11) -0.1665(5) 0.3216(11) 0.068(4) Uani 1 1 d . . . . .
H11A H 0.7552 -0.1979 0.3499 0.082 Uiso 1 1 calc R U . . .
H11B H 0.7123 -0.1643 0.2624 0.082 Uiso 1 1 calc R U . . .
C12 C 0.8647(14) -0.1580(8) 0.2933(13) 0.124(7) Uani 1 1 d . U . . .
H12A H 0.8706 -0.1260 0.2712 0.186 Uiso 1 1 calc R U . . .
H12B H 0.8798 -0.1789 0.2394 0.186 Uiso 1 1 calc R U . . .
H12C H 0.9123 -0.1635 0.3507 0.186 Uiso 1 1 calc R U . . .
C13A C 0.4766(12) -0.1173(10) 0.5191(19) 0.068(6) Uani 0.577(9) 1 d D U P A 1
H13A H 0.4385 -0.0897 0.5380 0.082 Uiso 0.577(9) 1 calc R U P A 1
H13B H 0.4407 -0.1310 0.4596 0.082 Uiso 0.577(9) 1 calc R U P A 1
C14A C 0.4792(16) -0.1524(9) 0.6040(19) 0.085(9) Uani 0.577(9) 1 d D . P A 1
H14A H 0.5083 -0.1382 0.6662 0.103 Uiso 0.577(9) 1 calc R U P A 1
H14B H 0.5207 -0.1794 0.5883 0.103 Uiso 0.577(9) 1 calc R U P A 1
C15A C 0.3693(15) -0.1670(9) 0.6148(18) 0.063(7) Uani 0.577(9) 1 d D . P A 1
H15A H 0.3686 -0.1870 0.6742 0.076 Uiso 0.577(9) 1 calc R U P A 1
H15B H 0.3305 -0.1389 0.6288 0.076 Uiso 0.577(9) 1 calc R U P A 1
C16A C 0.313(2) -0.1921(9) 0.5299(18) 0.063(3) Uani 0.577(9) 1 d . . P A 1
H16A H 0.3023 -0.1713 0.4731 0.095 Uiso 0.577(9) 1 calc R U P A 1
H16B H 0.2472 -0.2024 0.5506 0.095 Uiso 0.577(9) 1 calc R U P A 1
H16C H 0.3518 -0.2189 0.5110 0.095 Uiso 0.577(9) 1 calc R U P A 1
C17A C 0.651(3) -0.0790(13) 0.578(3) 0.063(3) Uani 0.45(2) 1 d . . P A 1
H17A H 0.6741 -0.1042 0.6242 0.076 Uiso 0.45(2) 1 calc R U P A 1
H17B H 0.7122 -0.0683 0.5469 0.076 Uiso 0.45(2) 1 calc R U P A 1
C18A C 0.622(3) -0.0404(13) 0.642(3) 0.063(3) Uani 0.45(2) 1 d . . P A 1
H18A H 0.5929 -0.0159 0.5978 0.076 Uiso 0.45(2) 1 calc R U P A 1
H18B H 0.5659 -0.0518 0.6808 0.076 Uiso 0.45(2) 1 calc R U P A 1
C19A C 0.748(3) -0.0498(11) 0.782(3) 0.063(3) Uani 0.45(2) 1 d . . P A 1
H19A H 0.7154 -0.0498 0.8445 0.095 Uiso 0.45(2) 1 calc R U P A 1
H19B H 0.8174 -0.0388 0.7932 0.095 Uiso 0.45(2) 1 calc R U P A 1
H19C H 0.7482 -0.0812 0.7550 0.095 Uiso 0.45(2) 1 calc R U P A 1
C20A C 0.692(3) -0.0191(13) 0.710(3) 0.063(3) Uani 0.45(2) 1 d . . P A 1
H20A H 0.6563 0.0042 0.7482 0.076 Uiso 0.45(2) 1 calc R U P A 1
H20B H 0.7416 -0.0024 0.6723 0.076 Uiso 0.45(2) 1 calc R U P A 1
C13B C 0.499(2) -0.1248(15) 0.552(2) 0.068(6) Uani 0.423(9) 1 d D U P A 2
H13C H 0.5314 -0.1497 0.5939 0.082 Uiso 0.423(9) 1 calc R U P A 2
H13D H 0.4760 -0.1012 0.5983 0.082 Uiso 0.423(9) 1 calc R U P A 2
C14B C 0.406(2) -0.1453(11) 0.496(2) 0.074(11) Uani 0.423(9) 1 d D . P A 2
H14C H 0.4287 -0.1663 0.4442 0.088 Uiso 0.423(9) 1 calc R U P A 2
H14D H 0.3679 -0.1199 0.4621 0.088 Uiso 0.423(9) 1 calc R U P A 2
C15B C 0.334(3) -0.1721(13) 0.559(2) 0.063(3) Uani 0.423(9) 1 d D . P A 2
H15C H 0.3716 -0.1970 0.5964 0.076 Uiso 0.423(9) 1 calc R U P A 2
H15D H 0.3056 -0.1512 0.6078 0.076 Uiso 0.423(9) 1 calc R U P A 2
C16B C 0.253(3) -0.1921(11) 0.492(2) 0.063(3) Uani 0.423(9) 1 d . . P A 2
H16D H 0.2105 -0.1672 0.4626 0.095 Uiso 0.423(9) 1 calc R U P A 2
H16E H 0.2115 -0.2129 0.5291 0.095 Uiso 0.423(9) 1 calc R U P A 2
H16F H 0.2825 -0.2094 0.4387 0.095 Uiso 0.423(9) 1 calc R U P A 2
C17B C 0.656(2) -0.0948(9) 0.5853(19) 0.063(3) Uani 0.55(2) 1 d D . P A 2
H17C H 0.6585 -0.1232 0.6258 0.076 Uiso 0.55(2) 1 calc R U P A 2
H17D H 0.7246 -0.0898 0.5626 0.076 Uiso 0.55(2) 1 calc R U P A 2
C18B C 0.634(3) -0.0588(10) 0.644(2) 0.063(3) Uani 0.55(2) 1 d . . P A 2
H18C H 0.5708 -0.0658 0.6759 0.076 Uiso 0.55(2) 1 calc R U P A 2
H18D H 0.6212 -0.0310 0.6021 0.076 Uiso 0.55(2) 1 calc R U P A 2
C19B C 0.718(2) -0.0480(9) 0.7252(15) 0.053(7) Uani 0.55(2) 1 d . . P A 2
H19D H 0.7300 -0.0755 0.7677 0.063 Uiso 0.55(2) 1 calc R U P A 2
H19E H 0.7812 -0.0412 0.6934 0.063 Uiso 0.55(2) 1 calc R U P A 2
C20B C 0.6924(19) -0.0070(8) 0.790(2) 0.073(9) Uani 0.55(2) 1 d . . P A 2
H20C H 0.6959 0.0215 0.7516 0.109 Uiso 0.55(2) 1 calc R U P A 2
H20D H 0.7406 -0.0055 0.8480 0.109 Uiso 0.55(2) 1 calc R U P A 2
H20E H 0.6242 -0.0109 0.8116 0.109 Uiso 0.55(2) 1 calc R U P A 2
C21 C 0.5537(11) -0.0631(5) 0.4264(10) 0.069(4) Uani 1 1 d . . . . .
H21A H 0.6143 -0.0439 0.4195 0.082 Uiso 1 1 calc R U . . .
H21B H 0.5042 -0.0439 0.4590 0.082 Uiso 1 1 calc R U . . .
C22 C 0.5099(9) -0.0751(5) 0.3245(9) 0.059(3) Uani 1 1 d . . . . .
H22A H 0.4543 -0.0975 0.3292 0.070 Uiso 1 1 calc R U . . .
H22B H 0.5622 -0.0896 0.2862 0.070 Uiso 1 1 calc R U . . .
C23 C 0.4700(12) -0.0315(5) 0.2710(10) 0.069(4) Uani 1 1 d . . . . .
H23A H 0.5239 -0.0079 0.2732 0.083 Uiso 1 1 calc R U . . .
H23B H 0.4132 -0.0189 0.3060 0.083 Uiso 1 1 calc R U . . .
C24 C 0.4340(10) -0.0412(5) 0.1616(10) 0.068(4) Uani 1 1 d . . . . .
H24A H 0.4919 -0.0494 0.1244 0.102 Uiso 1 1 calc R U . . .
H24B H 0.4015 -0.0136 0.1325 0.102 Uiso 1 1 calc R U . . .
H24C H 0.3857 -0.0668 0.1588 0.102 Uiso 1 1 calc R U . . .
C25 C -0.1108(7) 0.4380(3) -0.0113(7) 0.0265(19) Uani 1 1 d . . . . .
H25A H -0.1665 0.4597 -0.0003 0.032 Uiso 1 1 calc R U . . .
H25B H -0.0472 0.4557 -0.0032 0.032 Uiso 1 1 calc R U . . .
C26 C -0.1237(8) 0.4209(4) -0.1175(7) 0.038(2) Uani 1 1 d . . . . .
H26A H -0.0626 0.4038 -0.1336 0.046 Uiso 1 1 calc R U . . .
H26B H -0.1816 0.3995 -0.1245 0.046 Uiso 1 1 calc R U . . .
C27 C -0.1412(8) 0.4604(4) -0.1890(7) 0.041(3) Uani 1 1 d . . . . .
H27A H -0.0828 0.4816 -0.1825 0.050 Uiso 1 1 calc R U . . .
H27B H -0.2016 0.4778 -0.1719 0.050 Uiso 1 1 calc R U . . .
C28 C -0.1562(11) 0.4438(5) -0.2957(9) 0.064(4) Uani 1 1 d . . . . .
H28A H -0.0980 0.4253 -0.3119 0.097 Uiso 1 1 calc R U . . .
H28B H -0.1627 0.4705 -0.3402 0.097 Uiso 1 1 calc R U . . .
H28C H -0.2174 0.4250 -0.3038 0.097 Uiso 1 1 calc R U . . .
C29 C -0.2098(7) 0.3773(3) 0.0699(7) 0.031(2) Uani 1 1 d . . . . .
H29A H -0.2057 0.3542 0.1240 0.038 Uiso 1 1 calc R U . . .
H29B H -0.2216 0.3603 0.0067 0.038 Uiso 1 1 calc R U . . .
C30 C -0.3007(7) 0.4080(3) 0.0830(7) 0.034(2) Uani 1 1 d . . . . .
H30A H -0.2840 0.4301 0.1374 0.041 Uiso 1 1 calc R U . . .
H30B H -0.3160 0.4259 0.0214 0.041 Uiso 1 1 calc R U . . .
C31 C -0.3925(8) 0.3808(4) 0.1061(10) 0.048(3) Uani 1 1 d . . . . .
H31A H -0.4068 0.3577 0.0529 0.058 Uiso 1 1 calc R U . . .
H31B H -0.3774 0.3637 0.1688 0.058 Uiso 1 1 calc R U . . .
C32 C -0.4851(7) 0.4094(4) 0.1158(9) 0.048(3) Uani 1 1 d . . . . .
H32A H -0.4717 0.4325 0.1678 0.072 Uiso 1 1 calc R U . . .
H32B H -0.5406 0.3894 0.1332 0.072 Uiso 1 1 calc R U . . .
H32C H -0.5035 0.4248 0.0526 0.072 Uiso 1 1 calc R U . . .
C33 C -0.0306(7) 0.3647(3) 0.0502(7) 0.030(2) Uani 1 1 d . . . . .
H33A H -0.0310 0.3415 0.1038 0.036 Uiso 1 1 calc R U . . .
H33B H -0.0519 0.3490 -0.0127 0.036 Uiso 1 1 calc R U . . .
C34 C 0.0767(7) 0.3814(4) 0.0439(8) 0.037(2) Uani 1 1 d . . . . .
H34A H 0.1057 0.3895 0.1111 0.044 Uiso 1 1 calc R U . . .
H34B H 0.0766 0.4096 0.0024 0.044 Uiso 1 1 calc R U . . .
C35 C 0.1426(8) 0.3444(4) -0.0009(8) 0.039(2) Uani 1 1 d . . . . .
H35A H 0.1432 0.3165 0.0414 0.047 Uiso 1 1 calc R U . . .
H35B H 0.1121 0.3358 -0.0672 0.047 Uiso 1 1 calc R U . . .
C36 C 0.2489(9) 0.3597(4) -0.0107(10) 0.059(4) Uani 1 1 d . . . . .
H36A H 0.2493 0.3859 -0.0563 0.089 Uiso 1 1 calc R U . . .
H36B H 0.2877 0.3342 -0.0366 0.089 Uiso 1 1 calc R U . . .
H36C H 0.2793 0.3689 0.0544 0.089 Uiso 1 1 calc R U . . .
C37 C -0.0822(7) 0.4257(3) 0.1678(6) 0.028(2) Uani 1 1 d . . . . .
H37A H -0.0112 0.4359 0.1688 0.034 Uiso 1 1 calc R U . . .
H37B H -0.1244 0.4538 0.1700 0.034 Uiso 1 1 calc R U . . .
C38 C -0.0954(8) 0.3979(3) 0.2613(7) 0.034(2) Uani 1 1 d . . . . .
H38A H -0.0639 0.3672 0.2553 0.041 Uiso 1 1 calc R U . . .
H38B H -0.1680 0.3933 0.2694 0.041 Uiso 1 1 calc R U . . .
C39 C -0.0472(8) 0.4226(4) 0.3523(7) 0.041(3) Uani 1 1 d . . . . .
H39A H 0.0269 0.4224 0.3495 0.049 Uiso 1 1 calc R U . . .
H39B H -0.0697 0.4552 0.3515 0.049 Uiso 1 1 calc R U . . .
C40 C -0.0741(10) 0.4004(4) 0.4466(8) 0.055(3) Uani 1 1 d . . . . .
H40A H -0.1470 0.4023 0.4516 0.082 Uiso 1 1 calc R U . . .
H40B H -0.0395 0.4164 0.5031 0.082 Uiso 1 1 calc R U . . .
H40C H -0.0533 0.3680 0.4470 0.082 Uiso 1 1 calc R U . . .
C41 C 0.0161(8) 0.0989(3) 1.0305(7) 0.032(2) Uani 1 1 d . . . . .
H41A H 0.0882 0.0906 1.0303 0.038 Uiso 1 1 calc R U . . .
H41B H -0.0169 0.0749 1.0690 0.038 Uiso 1 1 calc R U . . .
C42 C -0.0296(7) 0.0972(3) 0.9241(7) 0.032(2) Uani 1 1 d . . . . .
H42A H -0.1003 0.1080 0.9218 0.039 Uiso 1 1 calc R U . . .
H42B H 0.0083 0.1181 0.8823 0.039 Uiso 1 1 calc R U . . .
C43 C -0.0264(8) 0.0485(3) 0.8834(7) 0.036(2) Uani 1 1 d . . . . .
H43A H -0.0720 0.0287 0.9194 0.044 Uiso 1 1 calc R U . . .
H43B H 0.0428 0.0362 0.8950 0.044 Uiso 1 1 calc R U . . .
C44 C -0.0578(8) 0.0468(4) 0.7723(7) 0.040(2) Uani 1 1 d . . . . .
H44A H -0.1247 0.0606 0.7601 0.061 Uiso 1 1 calc R U . . .
H44B H -0.0597 0.0146 0.7500 0.061 Uiso 1 1 calc R U . . .
H44C H -0.0090 0.0640 0.7358 0.061 Uiso 1 1 calc R U . . .
C45 C -0.0997(7) 0.1522(3) 1.1104(8) 0.038(2) Uani 1 1 d . . . . .
H45A H -0.1429 0.1521 1.0477 0.046 Uiso 1 1 calc R U . . .
H45B H -0.1199 0.1255 1.1502 0.046 Uiso 1 1 calc R U . . .
C46 C -0.1218(9) 0.1957(4) 1.1663(9) 0.049(3) Uani 1 1 d . . . . .
H46A H -0.1092 0.2230 1.1250 0.058 Uiso 1 1 calc R U . . .
H46B H -0.0768 0.1976 1.2278 0.058 Uiso 1 1 calc R U . . .
C47 C -0.2314(9) 0.1954(4) 1.1923(10) 0.057(3) Uani 1 1 d . . . . .
H47A H -0.2752 0.1921 1.1303 0.068 Uiso 1 1 calc R U . . .
H47B H -0.2426 0.1681 1.2341 0.068 Uiso 1 1 calc R U . . .
C48 C -0.2629(10) 0.2380(5) 1.2462(11) 0.070(4) Uani 1 1 d . . . . .
H48A H -0.2202 0.2416 1.3078 0.105 Uiso 1 1 calc R U . . .
H48B H -0.3334 0.2351 1.2617 0.105 Uiso 1 1 calc R U . . .
H48C H -0.2555 0.2651 1.2040 0.105 Uiso 1 1 calc R U . . .
C49 C 0.0816(8) 0.1452(4) 1.1774(7) 0.035(2) Uani 1 1 d . . . . .
H49A H 0.1495 0.1372 1.1571 0.042 Uiso 1 1 calc R U . . .
H49B H 0.0850 0.1769 1.2048 0.042 Uiso 1 1 calc R U . . .
C50 C 0.0553(7) 0.1123(4) 1.2591(7) 0.038(2) Uani 1 1 d . . . . .
H50A H -0.0056 0.1235 1.2895 0.046 Uiso 1 1 calc R U . . .
H50B H 0.0401 0.0814 1.2304 0.046 Uiso 1 1 calc R U . . .
C51 C 0.1409(8) 0.1083(4) 1.3379(7) 0.039(2) Uani 1 1 d . . . . .
H51A H 0.1168 0.0913 1.3950 0.047 Uiso 1 1 calc R U . . .
H51B H 0.1600 0.1397 1.3611 0.047 Uiso 1 1 calc R U . . .
C52 C 0.2344(9) 0.0843(5) 1.3048(10) 0.064(4) Uani 1 1 d . . . . .
H52A H 0.2196 0.0516 1.2928 0.096 Uiso 1 1 calc R U . . .
H52B H 0.2892 0.0873 1.3567 0.096 Uiso 1 1 calc R U . . .
H52C H 0.2545 0.0986 1.2436 0.096 Uiso 1 1 calc R U . . .
C53 C 0.0428(8) 0.1846(4) 1.0185(8) 0.042(3) Uani 1 1 d . . . . .
H53A H -0.0031 0.1853 0.9576 0.050 Uiso 1 1 calc R U . . .
H53B H 0.0346 0.2141 1.0536 0.050 Uiso 1 1 calc R U . . .
C54 C 0.1490(8) 0.1821(4) 0.9880(8) 0.042(3) Uani 1 1 d . . . . .
H54A H 0.1632 0.1504 0.9654 0.050 Uiso 1 1 calc R U . . .
H54B H 0.1963 0.1891 1.0459 0.050 Uiso 1 1 calc R U . . .
C55 C 0.1658(10) 0.2160(4) 0.9051(8) 0.055(3) Uani 1 1 d . . . . .
H55A H 0.1450 0.2472 0.9255 0.066 Uiso 1 1 calc R U . . .
H55B H 0.1227 0.2072 0.8454 0.066 Uiso 1 1 calc R U . . .
C56 C 0.2756(11) 0.2176(5) 0.8789(9) 0.069(4) Uani 1 1 d . . . . .
H56A H 0.3194 0.2228 0.9393 0.104 Uiso 1 1 calc R U . . .
H56B H 0.2845 0.2427 0.8319 0.104 Uiso 1 1 calc R U . . .
H56C H 0.2934 0.1882 0.8489 0.104 Uiso 1 1 calc R U . . .
C57 C 0.6916(9) 0.1726(4) 0.5691(7) 0.050(3) Uani 1 1 d . . . . .
H57A H 0.6912 0.1882 0.5040 0.060 Uiso 1 1 calc R U . . .
H57B H 0.6980 0.1968 0.6208 0.060 Uiso 1 1 calc R U . . .
C58 C 0.7830(8) 0.1426(5) 0.5805(9) 0.056(3) Uani 1 1 d . . . . .
H58A H 0.7700 0.1128 0.5459 0.067 Uiso 1 1 calc R U . . .
H58B H 0.8006 0.1361 0.6515 0.067 Uiso 1 1 calc R U . . .
C59 C 0.8729(10) 0.1691(5) 0.5337(13) 0.077(5) Uani 1 1 d . . . . .
H59A H 0.8613 0.1695 0.4606 0.092 Uiso 1 1 calc R U . . .
H59B H 0.8748 0.2015 0.5572 0.092 Uiso 1 1 calc R U . . .
C60 C 0.9686(14) 0.1470(7) 0.5613(14) 0.111(7) Uani 1 1 d . . . . .
H60A H 0.9874 0.1527 0.6316 0.167 Uiso 1 1 calc R U . . .
H60B H 1.0206 0.1596 0.5211 0.167 Uiso 1 1 calc R U . . .
H60C H 0.9625 0.1137 0.5498 0.167 Uiso 1 1 calc R U . . .
C61 C 0.5668(8) 0.1160(4) 0.4884(7) 0.036(2) Uani 1 1 d . . . . .
H61A H 0.6207 0.0925 0.4898 0.044 Uiso 1 1 calc R U . . .
H61B H 0.5029 0.0997 0.4984 0.044 Uiso 1 1 calc R U . . .
C62 C 0.5580(9) 0.1374(4) 0.3857(7) 0.048(3) Uani 1 1 d . . . . .
H62A H 0.6241 0.1500 0.3702 0.058 Uiso 1 1 calc R U . . .
H62B H 0.5092 0.1632 0.3845 0.058 Uiso 1 1 calc R U . . .
C63 C 0.5234(9) 0.1019(4) 0.3076(8) 0.047(3) Uani 1 1 d . . . . .
H63A H 0.5759 0.0779 0.3056 0.056 Uiso 1 1 calc R U . . .
H63B H 0.4616 0.0869 0.3286 0.056 Uiso 1 1 calc R U . . .
C64 C 0.5016(11) 0.1205(5) 0.2034(8) 0.065(4) Uani 1 1 d . . . . .
H64A H 0.4448 0.1421 0.2026 0.098 Uiso 1 1 calc R U . . .
H64B H 0.4847 0.0949 0.1580 0.098 Uiso 1 1 calc R U . . .
H64C H 0.5612 0.1366 0.1823 0.098 Uiso 1 1 calc R U . . .
C65 C 0.5898(8) 0.1181(3) 0.6685(7) 0.034(2) Uani 1 1 d . . . . .
H65A H 0.6482 0.0969 0.6688 0.041 Uiso 1 1 calc R U . . .
H65B H 0.5280 0.0990 0.6647 0.041 Uiso 1 1 calc R U . . .
C66 C 0.5955(9) 0.1449(4) 0.7660(7) 0.042(3) Uani 1 1 d . . . . .
H66A H 0.5302 0.1603 0.7742 0.050 Uiso 1 1 calc R U . . .
H66B H 0.6480 0.1691 0.7645 0.050 Uiso 1 1 calc R U . . .
C67 C 0.6208(10) 0.1123(5) 0.8543(8) 0.056(3) Uani 1 1 d . . . . .
H67A H 0.5740 0.0857 0.8499 0.067 Uiso 1 1 calc R U . . .
H67B H 0.6901 0.1003 0.8507 0.067 Uiso 1 1 calc R U . . .
C68 C 0.6126(12) 0.1365(5) 0.9527(9) 0.076(4) Uani 1 1 d . . . . .
H68A H 0.6556 0.1640 0.9556 0.114 Uiso 1 1 calc R U . . .
H68B H 0.6345 0.1156 1.0069 0.114 Uiso 1 1 calc R U . . .
H68C H 0.5426 0.1456 0.9594 0.114 Uiso 1 1 calc R U . . .
C69 C 0.5099(8) 0.1854(4) 0.5786(8) 0.041(3) Uani 1 1 d . . . . .
H69A H 0.5256 0.2044 0.6386 0.049 Uiso 1 1 calc R U . . .
H69B H 0.5163 0.2057 0.5205 0.049 Uiso 1 1 calc R U . . .
C70 C 0.4031(9) 0.1707(4) 0.5786(8) 0.043(3) Uani 1 1 d . . . . .
H70A H 0.3979 0.1456 0.6276 0.052 Uiso 1 1 calc R U . . .
H70B H 0.3815 0.1581 0.5124 0.052 Uiso 1 1 calc R U . . .
C71 C 0.3326(9) 0.2093(4) 0.6028(9) 0.054(3) Uani 1 1 d . . . . .
H71A H 0.3332 0.2331 0.5505 0.065 Uiso 1 1 calc R U . . .
H71B H 0.3575 0.2237 0.6663 0.065 Uiso 1 1 calc R U . . .
C72 C 0.2243(10) 0.1930(5) 0.6113(8) 0.058(3) Uani 1 1 d . . . . .
H72A H 0.2007 0.1768 0.5504 0.086 Uiso 1 1 calc R U . . .
H72B H 0.1810 0.2197 0.6210 0.086 Uiso 1 1 calc R U . . .
H72C H 0.2219 0.1720 0.6679 0.086 Uiso 1 1 calc R U . . .
N1 N 0.2686(7) 0.2883(3) 0.3247(7) 0.050(2) Uani 1 1 d . . . . .
N2 N 0.1573(9) 0.5311(4) 0.7623(9) 0.072(3) Uani 1 1 d . . . . .
N3 N 0.2658(6) 0.0224(3) 0.7598(6) 0.038(2) Uani 1 1 d . . . . .
N4 N 0.6996(6) 0.2578(3) 0.7849(8) 0.051(3) Uani 1 1 d . . . . .
N5 N 0.5828(7) -0.1025(4) 0.4937(7) 0.051(2) Uani 1 1 d D . . . .
N6 N -0.1087(6) 0.4013(3) 0.0693(6) 0.0286(17) Uani 1 1 d . . . . .
N7 N 0.0085(6) 0.1451(3) 1.0856(6) 0.0357(19) Uani 1 1 d . . . . .
N8 N 0.5890(6) 0.1484(3) 0.5760(5) 0.0335(19) Uani 1 1 d . . . . .
O1 O 0.2856(7) 0.2034(3) 0.2723(8) 0.066(3) Uani 1 1 d . . . . .
O2 O 0.4202(7) 0.2441(4) 0.3706(7) 0.089(4) Uani 1 1 d . . . . .
O3 O 0.1335(7) 0.3424(3) 0.2846(6) 0.058(2) Uani 1 1 d . . . . .
O4 O 0.1199(6) 0.2672(3) 0.1997(6) 0.0481(19) Uani 1 1 d . . . . .
O5 O 0.2448(8) 0.4541(4) 0.7837(8) 0.083(2) Uani 1 1 d . . . . .
O6 O 0.1117(8) 0.4746(4) 0.8850(8) 0.083(2) Uani 1 1 d . . . . .
O7 O 0.2887(7) 0.5221(4) 0.6271(10) 0.092(4) Uani 1 1 d . . . . .
O8 O 0.1824(7) 0.5875(3) 0.6392(7) 0.063(2) Uani 1 1 d . . . . .
O9 O 0.3615(5) 0.1006(3) 0.7741(5) 0.0434(18) Uani 1 1 d . . . . .
O10 O 0.1890(6) 0.0918(3) 0.8292(6) 0.053(2) Uani 1 1 d . . . . .
O11 O 0.3195(7) -0.0462(3) 0.6750(6) 0.056(2) Uani 1 1 d . . . . .
O12 O 0.4387(6) 0.0176(3) 0.6848(7) 0.058(2) Uani 1 1 d . . . . .
O13 O 0.5598(7) 0.3033(4) 0.7102(7) 0.079(3) Uani 1 1 d . . . . .
O14 O 0.6707(6) 0.3414(2) 0.8444(7) 0.057(2) Uani 1 1 d . . . . .
O15A O 0.8263(16) 0.2014(8) 0.8637(14) 0.048(5) Uani 0.577(9) 1 d . . P A 1
O16A O 0.8064(14) 0.2742(7) 0.9533(15) 0.042(4) Uani 0.577(9) 1 d . . P A 1
O15B O 0.839(2) 0.2055(11) 0.8153(18) 0.049(7) Uani 0.423(9) 1 d . . P A 2
O16B O 0.840(2) 0.2771(11) 0.918(2) 0.055(8) Uani 0.423(9) 1 d . . P A 2
F1 F 0.3252(5) 0.2704(3) 0.1112(5) 0.064(2) Uani 1 1 d . . . . .
F2 F 0.4432(6) 0.3031(3) 0.1983(6) 0.087(3) Uani 1 1 d . . . . .
F3 F 0.4599(6) 0.2337(3) 0.1583(7) 0.091(3) Uani 1 1 d . . . . .
F4 F 0.1107(6) 0.2906(3) 0.4708(5) 0.072(2) Uani 1 1 d . . . . .
F5 F 0.0976(6) 0.2257(2) 0.3944(6) 0.067(2) Uani 1 1 d . . . . .
F6 F -0.0146(5) 0.2781(2) 0.3655(5) 0.0607(19) Uani 1 1 d . . . . .
F7 F 0.3227(7) 0.4864(3) 0.9796(7) 0.101(3) Uani 1 1 d . . . . .
F8 F 0.3572(6) 0.5355(3) 0.8694(6) 0.073(2) Uani 1 1 d . . . . .
F9 F 0.2420(6) 0.5485(3) 0.9688(6) 0.085(3) Uani 1 1 d . . . . .
F10 F 0.1070(7) 0.4678(3) 0.5752(9) 0.112(4) Uani 1 1 d . . . . .
F11 F 0.1262(9) 0.5220(4) 0.4741(7) 0.126(4) Uani 1 1 d . . . . .
F12 F 0.0122(5) 0.5248(3) 0.5842(8) 0.097(3) Uani 1 1 d . . . . .
F13 F 0.3552(6) 0.0932(2) 0.9898(5) 0.069(2) Uani 1 1 d . . . . .
F14 F 0.2705(6) 0.0300(2) 0.9832(5) 0.063(2) Uani 1 1 d . . . . .
F15 F 0.4216(5) 0.0313(2) 0.9330(5) 0.0594(19) Uani 1 1 d . . . . .
F16 F 0.1868(5) 0.0114(2) 0.5440(5) 0.060(2) Uani 1 1 d . . . . .
F17 F 0.2848(5) 0.0698(2) 0.5591(5) 0.0536(17) Uani 1 1 d . . . . .
F18 F 0.3324(6) 0.0077(3) 0.4885(5) 0.070(2) Uani 1 1 d . . . . .
F19 F 0.4988(7) 0.2393(3) 0.8600(8) 0.100(3) Uani 1 1 d . . . . .
F20 F 0.5961(7) 0.2688(3) 0.9771(7) 0.092(3) Uani 1 1 d . . . . .
F21 F 0.4743(6) 0.3093(3) 0.9092(8) 0.097(3) Uani 1 1 d . . . . .
F22A F 0.9801(10) 0.2747(5) 0.8463(15) 0.087(3) Uani 0.577(9) 1 d . . P A 1
F23A F 0.8838(13) 0.3212(10) 0.759(3) 0.087(3) Uani 0.577(9) 1 d . . P A 1
F24A F 0.9060(11) 0.2546(6) 0.7040(15) 0.087(3) Uani 0.577(9) 1 d . . P A 1
F22B F 0.9884(13) 0.2721(7) 0.761(2) 0.087(3) Uani 0.423(9) 1 d . . P A 2
F23B F 0.8598(18) 0.3239(14) 0.753(4) 0.087(3) Uani 0.423(9) 1 d . . P A 2
F24B F 0.8691(15) 0.2675(8) 0.651(2) 0.087(3) Uani 0.423(9) 1 d . . P A 2
S1 S 0.3353(2) 0.24592(11) 0.2988(2) 0.0499(7) Uani 1 1 d . . . . .
S2 S 0.1541(2) 0.29419(10) 0.2837(2) 0.0439(7) Uani 1 1 d . . . . .
S3 S 0.1865(2) 0.49114(11) 0.8271(2) 0.0494(7) Uani 1 1 d . . . . .
S4 S 0.1978(2) 0.53968(11) 0.6505(2) 0.0489(8) Uani 1 1 d . . . . .
S5 S 0.2844(2) 0.07123(9) 0.81152(19) 0.0375(6) Uani 1 1 d . . . . .
S6 S 0.3367(2) 0.00211(9) 0.6807(2) 0.0397(6) Uani 1 1 d . . . . .
S7 S 0.6263(2) 0.29975(11) 0.7997(3) 0.0550(8) Uani 1 1 d . . . . .
S8A S 0.7973(7) 0.2491(3) 0.8624(7) 0.0386(18) Uani 0.577(9) 1 d . . P A 1
S8B S 0.8143(10) 0.2547(5) 0.8237(10) 0.047(3) Uani 0.423(9) 1 d . . P 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
C1 F3 1.313(14) . ?
C1 F2 1.321(14) . ?
C1 F1 1.335(13) . ?
C1 S1 1.829(13) . ?
C2 F5 1.328(12) . ?
C2 F6 1.329(13) . ?
C2 F4 1.337(13) . ?
C2 S2 1.828(13) . ?
C3 F8 1.281(15) . ?
C3 F7 1.311(16) . ?
C3 F9 1.407(16) . ?
C3 S3 1.817(15) . ?
C4 F12 1.276(14) . ?
C4 F10 1.301(14) . ?
C4 F11 1.365(15) . ?
C4 S4 1.814(12) . ?
C5 F15 1.318(15) . ?
C5 F13 1.352(13) . ?
C5 F14 1.369(13) . ?
C5 S5 1.804(12) . ?
C6 F16 1.306(13) . ?
C6 F18 1.318(13) . ?
C6 F17 1.348(12) . ?
C6 S6 1.836(11) . ?
C7 F20 1.311(18) . ?
C7 F21 1.317(15) . ?
C7 F19 1.335(15) . ?
C7 S7 1.854(17) . ?
C8A F22A 1.36(3) . ?
C8A F24A 1.37(3) . ?
C8A F23A 1.38(4) . ?
C8A S8A 1.79(3) . ?
C8B F24B 1.26(4) . ?
C8B F23B 1.27(6) . ?
C8B F22B 1.34(4) . ?
C8B S8B 1.84(4) . ?
C9 C10 1.484(17) . ?
C9 N5 1.527(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.63(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.49(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13A C14A 1.531(13) . ?
C13A N5 1.539(12) . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C14A C15A 1.542(12) . ?
C14A H14A 0.9900 . ?
C14A H14B 0.9900 . ?
C15A C16A 1.51(3) . ?
C15A H15A 0.9900 . ?
C15A H15B 0.9900 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C17A C18A 1.49(5) . ?
C17A N5 1.57(3) . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A C20A 1.41(5) . ?
C18A H18A 0.9900 . ?
C18A H18B 0.9900 . ?
C19A C20A 1.47(5) . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C13B C14B 1.531(13) . ?
C13B N5 1.551(13) . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C14B C15B 1.538(13) . ?
C14B H14C 0.9900 . ?
C14B H14D 0.9900 . ?
C15B C16B 1.49(4) . ?
C15B H15C 0.9900 . ?
C15B H15D 0.9900 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17B C18B 1.36(4) . ?
C17B N5 1.540(13) . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B C19B 1.55(4) . ?
C18B H18C 0.9900 . ?
C18B H18D 0.9900 . ?
C19B C20B 1.53(4) . ?
C19B H19D 0.9900 . ?
C19B H19E 0.9900 . ?
C20B H20C 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C21 N5 1.494(16) . ?
C21 C22 1.499(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.533(18) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.548(17) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.518(13) . ?
C25 N6 1.523(11) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.506(14) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.520(15) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 N6 1.515(11) . ?
C29 C30 1.523(13) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.506(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.499(14) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.517(13) . ?
C33 N6 1.519(11) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.537(13) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.498(15) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.521(12) . ?
C37 N6 1.527(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.525(14) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.495(14) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.524(12) . ?
C41 N7 1.539(12) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.516(12) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.531(13) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.510(14) . ?
C45 N7 1.517(12) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.526(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.510(15) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.520(13) . ?
C49 N7 1.522(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.508(13) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.520(15) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.502(14) . ?
C53 N7 1.549(13) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.520(14) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.529(18) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.495(17) . ?
C57 N8 1.545(13) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.591(17) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.45(2) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.517(14) . ?
C61 N8 1.525(11) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.521(14) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.517(16) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 N8 1.527(11) . ?
C65 C66 1.528(13) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.541(14) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 C68 1.516(17) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C70 1.485(15) . ?
C69 N8 1.506(13) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C70 C71 1.512(15) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.528(17) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N1 S1 1.571(10) . ?
N1 S2 1.595(10) . ?
N2 S3 1.488(11) . ?
N2 S4 1.659(12) . ?
N3 S6 1.589(9) . ?
N3 S5 1.591(8) . ?
N4 S7 1.581(9) . ?
N4 S8B 1.582(17) . ?
N4 S8A 1.632(13) . ?
O1 S1 1.431(9) . ?
O2 S1 1.437(9) . ?
O3 S2 1.424(8) . ?
O4 S2 1.427(8) . ?
O5 S3 1.472(11) . ?
O6 S3 1.395(11) . ?
O7 S4 1.372(10) . ?
O8 S4 1.410(9) . ?
O9 S5 1.451(7) . ?
O10 S5 1.438(8) . ?
O11 S6 1.421(8) . ?
O12 S6 1.427(8) . ?
O13 S7 1.451(9) . ?
O14 S7 1.458(8) . ?
O15A S8A 1.44(2) . ?
O16A S8A 1.43(2) . ?
O15B S8B 1.47(3) . ?
O16B S8B 1.45(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
F3 C1 F2 105.7(11) . . ?
F3 C1 F1 108.1(11) . . ?
F2 C1 F1 105.9(10) . . ?
F3 C1 S1 112.8(8) . . ?
F2 C1 S1 112.5(10) . . ?
F1 C1 S1 111.5(9) . . ?
F5 C2 F6 107.7(10) . . ?
F5 C2 F4 107.2(10) . . ?
F6 C2 F4 107.2(9) . . ?
F5 C2 S2 111.7(8) . . ?
F6 C2 S2 110.8(8) . . ?
F4 C2 S2 111.9(9) . . ?
F8 C3 F7 111.0(12) . . ?
F8 C3 F9 105.6(13) . . ?
F7 C3 F9 100.9(10) . . ?
F8 C3 S3 115.7(9) . . ?
F7 C3 S3 114.9(12) . . ?
F9 C3 S3 107.1(9) . . ?
F12 C4 F10 108.3(12) . . ?
F12 C4 F11 112.9(11) . . ?
F10 C4 F11 104.6(11) . . ?
F12 C4 S4 113.6(8) . . ?
F10 C4 S4 110.9(9) . . ?
F11 C4 S4 106.3(9) . . ?
F15 C5 F13 108.4(10) . . ?
F15 C5 F14 107.6(10) . . ?
F13 C5 F14 104.4(10) . . ?
F15 C5 S5 114.3(9) . . ?
F13 C5 S5 110.3(9) . . ?
F14 C5 S5 111.2(9) . . ?
F16 C6 F18 108.6(9) . . ?
F16 C6 F17 107.4(10) . . ?
F18 C6 F17 107.8(10) . . ?
F16 C6 S6 113.0(8) . . ?
F18 C6 S6 110.0(8) . . ?
F17 C6 S6 109.9(7) . . ?
F20 C7 F21 110.1(14) . . ?
F20 C7 F19 108.7(15) . . ?
F21 C7 F19 109.5(11) . . ?
F20 C7 S7 110.5(10) . . ?
F21 C7 S7 109.3(12) . . ?
F19 C7 S7 108.7(11) . . ?
F22A C8A F24A 105.8(19) . . ?
F22A C8A F23A 103(2) . . ?
F24A C8A F23A 99(2) . . ?
F22A C8A S8A 108.5(18) . . ?
F24A C8A S8A 114.6(19) . . ?
F23A C8A S8A 123.5(19) . . ?
F24B C8B F23B 116(4) . . ?
F24B C8B F22B 108(3) . . ?
F23B C8B F22B 121(4) . . ?
F24B C8B S8B 108(3) . . ?
F23B C8B S8B 95(3) . . ?
F22B C8B S8B 107(3) . . ?
C10 C9 N5 113.8(11) . . ?
C10 C9 H9A 108.8 . . ?
N5 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
N5 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 C11 107.9(12) . . ?
C9 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C12 C11 C10 108.8(14) . . ?
C12 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14A C13A N5 112.3(14) . . ?
C14A C13A H13A 109.1 . . ?
N5 C13A H13A 109.1 . . ?
C14A C13A H13B 109.1 . . ?
N5 C13A H13B 109.1 . . ?
H13A C13A H13B 107.9 . . ?
C13A C14A C15A 106.4(16) . . ?
C13A C14A H14A 110.4 . . ?
C15A C14A H14A 110.4 . . ?
C13A C14A H14B 110.4 . . ?
C15A C14A H14B 110.4 . . ?
H14A C14A H14B 108.6 . . ?
C16A C15A C14A 119(2) . . ?
C16A C15A H15A 107.6 . . ?
C14A C15A H15A 107.6 . . ?
C16A C15A H15B 107.6 . . ?
C14A C15A H15B 107.6 . . ?
H15A C15A H15B 107.0 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C18A C17A N5 126(3) . . ?
C18A C17A H17A 105.9 . . ?
N5 C17A H17A 105.9 . . ?
C18A C17A H17B 105.9 . . ?
N5 C17A H17B 105.9 . . ?
H17A C17A H17B 106.2 . . ?
C20A C18A C17A 121(3) . . ?
C20A C18A H18A 107.1 . . ?
C17A C18A H18A 107.1 . . ?
C20A C18A H18B 107.1 . . ?
C17A C18A H18B 107.1 . . ?
H18A C18A H18B 106.8 . . ?
C20A C19A H19A 109.5 . . ?
C20A C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
C20A C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C18A C20A C19A 116(3) . . ?
C18A C20A H20A 108.2 . . ?
C19A C20A H20A 108.2 . . ?
C18A C20A H20B 108.2 . . ?
C19A C20A H20B 108.2 . . ?
H20A C20A H20B 107.3 . . ?
C14B C13B N5 119.3(19) . . ?
C14B C13B H13C 107.5 . . ?
N5 C13B H13C 107.5 . . ?
C14B C13B H13D 107.5 . . ?
N5 C13B H13D 107.5 . . ?
H13C C13B H13D 107.0 . . ?
C13B C14B C15B 116(2) . . ?
C13B C14B H14C 108.4 . . ?
C15B C14B H14C 108.4 . . ?
C13B C14B H14D 108.4 . . ?
C15B C14B H14D 108.4 . . ?
H14C C14B H14D 107.5 . . ?
C16B C15B C14B 108(3) . . ?
C16B C15B H15C 110.1 . . ?
C14B C15B H15C 110.1 . . ?
C16B C15B H15D 110.1 . . ?
C14B C15B H15D 110.1 . . ?
H15C C15B H15D 108.4 . . ?
C15B C16B H16D 109.5 . . ?
C15B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C18B C17B N5 115(2) . . ?
C18B C17B H17C 108.5 . . ?
N5 C17B H17C 108.5 . . ?
C18B C17B H17D 108.5 . . ?
N5 C17B H17D 108.5 . . ?
H17C C17B H17D 107.5 . . ?
C17B C18B C19B 113(2) . . ?
C17B C18B H18C 109.0 . . ?
C19B C18B H18C 109.0 . . ?
C17B C18B H18D 109.0 . . ?
C19B C18B H18D 109.0 . . ?
H18C C18B H18D 107.8 . . ?
C20B C19B C18B 112(3) . . ?
C20B C19B H19D 109.1 . . ?
C18B C19B H19D 109.1 . . ?
C20B C19B H19E 109.1 . . ?
C18B C19B H19E 109.1 . . ?
H19D C19B H19E 107.8 . . ?
C19B C20B H20C 109.5 . . ?
C19B C20B H20D 109.5 . . ?
H20C C20B H20D 109.5 . . ?
C19B C20B H20E 109.5 . . ?
H20C C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
N5 C21 C22 116.7(11) . . ?
N5 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
N5 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C21 C22 C23 110.0(11) . . ?
C21 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C22 C23 C24 112.0(11) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N6 116.4(7) . . ?
C26 C25 H25A 108.2 . . ?
N6 C25 H25A 108.2 . . ?
C26 C25 H25B 108.2 . . ?
N6 C25 H25B 108.2 . . ?
H25A C25 H25B 107.3 . . ?
C27 C26 C25 111.2(9) . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C26 C27 C28 111.9(9) . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27B 109.2 . . ?
C28 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N6 C29 C30 116.5(8) . . ?
N6 C29 H29A 108.2 . . ?
C30 C29 H29A 108.2 . . ?
N6 C29 H29B 108.2 . . ?
C30 C29 H29B 108.2 . . ?
H29A C29 H29B 107.3 . . ?
C31 C30 C29 112.4(8) . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C32 C31 C30 114.4(10) . . ?
C32 C31 H31A 108.7 . . ?
C30 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 107.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N6 116.5(8) . . ?
C34 C33 H33A 108.2 . . ?
N6 C33 H33A 108.2 . . ?
C34 C33 H33B 108.2 . . ?
N6 C33 H33B 108.2 . . ?
H33A C33 H33B 107.3 . . ?
C33 C34 C35 111.5(8) . . ?
C33 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 113.4(9) . . ?
C36 C35 H35A 108.9 . . ?
C34 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C34 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N6 116.5(8) . . ?
C38 C37 H37A 108.2 . . ?
N6 C37 H37A 108.2 . . ?
C38 C37 H37B 108.2 . . ?
N6 C37 H37B 108.2 . . ?
H37A C37 H37B 107.3 . . ?
C37 C38 C39 110.8(8) . . ?
C37 C38 H38A 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 C38 111.9(9) . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39B 109.2 . . ?
C38 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N7 116.7(7) . . ?
C42 C41 H41A 108.1 . . ?
N7 C41 H41A 108.1 . . ?
C42 C41 H41B 108.1 . . ?
N7 C41 H41B 108.1 . . ?
H41A C41 H41B 107.3 . . ?
C43 C42 C41 110.7(8) . . ?
C43 C42 H42A 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 108.1 . . ?
C42 C43 C44 111.9(8) . . ?
C42 C43 H43A 109.2 . . ?
C44 C43 H43A 109.2 . . ?
C42 C43 H43B 109.2 . . ?
C44 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 N7 116.5(9) . . ?
C46 C45 H45A 108.2 . . ?
N7 C45 H45A 108.2 . . ?
C46 C45 H45B 108.2 . . ?
N7 C45 H45B 108.2 . . ?
H45A C45 H45B 107.3 . . ?
C45 C46 C47 109.4(9) . . ?
C45 C46 H46A 109.8 . . ?
C47 C46 H46A 109.8 . . ?
C45 C46 H46B 109.8 . . ?
C47 C46 H46B 109.8 . . ?
H46A C46 H46B 108.2 . . ?
C48 C47 C46 114.1(10) . . ?
C48 C47 H47A 108.7 . . ?
C46 C47 H47A 108.7 . . ?
C48 C47 H47B 108.7 . . ?
C46 C47 H47B 108.7 . . ?
H47A C47 H47B 107.6 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N7 115.2(8) . . ?
C50 C49 H49A 108.5 . . ?
N7 C49 H49A 108.5 . . ?
C50 C49 H49B 108.5 . . ?
N7 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
C51 C50 C49 111.1(8) . . ?
C51 C50 H50A 109.4 . . ?
C49 C50 H50A 109.4 . . ?
C51 C50 H50B 109.4 . . ?
C49 C50 H50B 109.4 . . ?
H50A C50 H50B 108.0 . . ?
C50 C51 C52 114.9(9) . . ?
C50 C51 H51A 108.5 . . ?
C52 C51 H51A 108.5 . . ?
C50 C51 H51B 108.6 . . ?
C52 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N7 116.6(8) . . ?
C54 C53 H53A 108.1 . . ?
N7 C53 H53A 108.1 . . ?
C54 C53 H53B 108.1 . . ?
N7 C53 H53B 108.1 . . ?
H53A C53 H53B 107.3 . . ?
C53 C54 C55 111.2(10) . . ?
C53 C54 H54A 109.4 . . ?
C55 C54 H54A 109.4 . . ?
C53 C54 H54B 109.4 . . ?
C55 C54 H54B 109.4 . . ?
H54A C54 H54B 108.0 . . ?
C54 C55 C56 112.5(11) . . ?
C54 C55 H55A 109.1 . . ?
C56 C55 H55A 109.1 . . ?
C54 C55 H55B 109.1 . . ?
C56 C55 H55B 109.1 . . ?
H55A C55 H55B 107.8 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 N8 116.5(10) . . ?
C58 C57 H57A 108.2 . . ?
N8 C57 H57A 108.2 . . ?
C58 C57 H57B 108.2 . . ?
N8 C57 H57B 108.2 . . ?
H57A C57 H57B 107.3 . . ?
C57 C58 C59 107.8(11) . . ?
C57 C58 H58A 110.1 . . ?
C59 C58 H58A 110.1 . . ?
C57 C58 H58B 110.1 . . ?
C59 C58 H58B 110.1 . . ?
H58A C58 H58B 108.5 . . ?
C60 C59 C58 110.7(14) . . ?
C60 C59 H59A 109.5 . . ?
C58 C59 H59A 109.5 . . ?
C60 C59 H59B 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 108.1 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C62 C61 N8 117.3(8) . . ?
C62 C61 H61A 108.0 . . ?
N8 C61 H61A 108.0 . . ?
C62 C61 H61B 108.0 . . ?
N8 C61 H61B 108.0 . . ?
H61A C61 H61B 107.2 . . ?
C61 C62 C63 111.1(10) . . ?
C61 C62 H62A 109.4 . . ?
C63 C62 H62A 109.4 . . ?
C61 C62 H62B 109.4 . . ?
C63 C62 H62B 109.4 . . ?
H62A C62 H62B 108.0 . . ?
C64 C63 C62 115.7(10) . . ?
C64 C63 H63A 108.4 . . ?
C62 C63 H63A 108.4 . . ?
C64 C63 H63B 108.4 . . ?
C62 C63 H63B 108.4 . . ?
H63A C63 H63B 107.4 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N8 C65 C66 114.3(8) . . ?
N8 C65 H65A 108.7 . . ?
C66 C65 H65A 108.7 . . ?
N8 C65 H65B 108.7 . . ?
C66 C65 H65B 108.7 . . ?
H65A C65 H65B 107.6 . . ?
C65 C66 C67 110.5(9) . . ?
C65 C66 H66A 109.5 . . ?
C67 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C67 C66 H66B 109.5 . . ?
H66A C66 H66B 108.1 . . ?
C68 C67 C66 111.8(11) . . ?
C68 C67 H67A 109.3 . . ?
C66 C67 H67A 109.3 . . ?
C68 C67 H67B 109.3 . . ?
C66 C67 H67B 109.3 . . ?
H67A C67 H67B 107.9 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C70 C69 N8 117.7(8) . . ?
C70 C69 H69A 107.9 . . ?
N8 C69 H69A 107.9 . . ?
C70 C69 H69B 107.9 . . ?
N8 C69 H69B 107.9 . . ?
H69A C69 H69B 107.2 . . ?
C69 C70 C71 113.3(10) . . ?
C69 C70 H70A 108.9 . . ?
C71 C70 H70A 108.9 . . ?
C69 C70 H70B 108.9 . . ?
C71 C70 H70B 108.9 . . ?
H70A C70 H70B 107.7 . . ?
C70 C71 C72 113.0(10) . . ?
C70 C71 H71A 109.0 . . ?
C72 C71 H71A 109.0 . . ?
C70 C71 H71B 109.0 . . ?
C72 C71 H71B 109.0 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
S1 N1 S2 123.2(6) . . ?
S3 N2 S4 124.4(8) . . ?
S6 N3 S5 123.0(5) . . ?
S7 N4 S8B 126.3(7) . . ?
S7 N4 S8A 120.6(6) . . ?
C21 N5 C9 113.9(10) . . ?
C21 N5 C13A 98.5(12) . . ?
C9 N5 C13A 110.7(15) . . ?
C21 N5 C17B 120.0(13) . . ?
C9 N5 C17B 100.5(15) . . ?
C21 N5 C13B 117.9(18) . . ?
C9 N5 C13B 106.7(19) . . ?
C17B N5 C13B 94.9(18) . . ?
C21 N5 C17A 103.0(16) . . ?
C9 N5 C17A 112.8(19) . . ?
C13A N5 C17A 117(2) . . ?
C29 N6 C33 107.4(7) . . ?
C29 N6 C25 110.7(7) . . ?
C33 N6 C25 110.1(7) . . ?
C29 N6 C37 111.0(7) . . ?
C33 N6 C37 110.7(7) . . ?
C25 N6 C37 106.9(7) . . ?
C45 N7 C49 112.4(8) . . ?
C45 N7 C41 108.8(8) . . ?
C49 N7 C41 109.6(7) . . ?
C45 N7 C53 110.7(7) . . ?
C49 N7 C53 106.2(8) . . ?
C41 N7 C53 109.1(7) . . ?
C69 N8 C61 111.1(8) . . ?
C69 N8 C65 110.9(7) . . ?
C61 N8 C65 105.8(7) . . ?
C69 N8 C57 107.4(8) . . ?
C61 N8 C57 110.9(7) . . ?
C65 N8 C57 110.8(8) . . ?
O1 S1 O2 117.7(6) . . ?
O1 S1 N1 118.1(5) . . ?
O2 S1 N1 107.8(6) . . ?
O1 S1 C1 104.6(6) . . ?
O2 S1 C1 102.1(6) . . ?
N1 S1 C1 104.2(6) . . ?
O3 S2 O4 119.6(5) . . ?
O3 S2 N1 106.3(5) . . ?
O4 S2 N1 117.5(5) . . ?
O3 S2 C2 104.4(5) . . ?
O4 S2 C2 103.5(5) . . ?
N1 S2 C2 103.4(6) . . ?
O6 S3 O5 112.9(7) . . ?
O6 S3 N2 115.5(7) . . ?
O5 S3 N2 117.2(7) . . ?
O6 S3 C3 107.4(6) . . ?
O5 S3 C3 98.2(7) . . ?
N2 S3 C3 102.8(7) . . ?
O7 S4 O8 117.7(6) . . ?
O7 S4 N2 120.2(7) . . ?
O8 S4 N2 101.1(6) . . ?
O7 S4 C4 107.0(7) . . ?
O8 S4 C4 105.7(6) . . ?
N2 S4 C4 103.5(6) . . ?
O10 S5 O9 117.9(5) . . ?
O10 S5 N3 109.4(5) . . ?
O9 S5 N3 117.4(5) . . ?
O10 S5 C5 104.4(6) . . ?
O9 S5 C5 103.2(5) . . ?
N3 S5 C5 102.1(5) . . ?
O11 S6 O12 117.5(5) . . ?
O11 S6 N3 107.5(5) . . ?
O12 S6 N3 117.7(5) . . ?
O11 S6 C6 103.3(5) . . ?
O12 S6 C6 104.7(5) . . ?
N3 S6 C6 104.2(5) . . ?
O13 S7 O14 119.5(6) . . ?
O13 S7 N4 107.1(5) . . ?
O14 S7 N4 117.0(4) . . ?
O13 S7 C7 103.9(7) . . ?
O14 S7 C7 103.9(6) . . ?
N4 S7 C7 103.2(7) . . ?
O16A S8A O15A 118.4(13) . . ?
O16A S8A N4 119.3(11) . . ?
O15A S8A N4 111.0(11) . . ?
O16A S8A C8A 102.4(13) . . ?
O15A S8A C8A 103.3(13) . . ?
N4 S8A C8A 98.1(10) . . ?
O16B S8B O15B 117.5(19) . . ?
O16B S8B N4 115.6(14) . . ?
O15B S8B N4 104.5(15) . . ?
O16B S8B C8B 104.4(19) . . ?
O15B S8B C8B 104.7(18) . . ?
N4 S8B C8B 109.6(14) . . ?

_refine_diff_density_max         0.984
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.075

_shelxl_version_number           2013-4

