# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Darren Johnson'
_publ_contact_author_address     
;
Department of Chemistry
University of Oregon
Eugene
OR
97403-1253
UNITED STATES OF AMERICA
;

_publ_contact_author_email       DWJ@UOREGON.EDU

_publ_section_title              
;
Anion-pi Interaction Augments Halide Binding in
Solution
;
loop_
_publ_author_name
'Darren Johnson'
'Orion B. Berryman'
'Fraser Hol'

# Attachment 'cifs_1_and_1BrNEt4.cif'

data_ob016
_database_code_depnum_ccdc_archive 'CCDC 261862'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H12 F5 N O2 S'
_chemical_formula_weight         413.36

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'

_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                   9.0547(11)
_cell_length_b                   10.2933(12)
_cell_length_c                   10.4106(13)
_cell_angle_alpha                97.125(2)
_cell_angle_beta                 112.783(2)
_cell_angle_gamma                101.426(2)
_cell_volume                     854.95(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    511
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.01

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             420
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6901
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3444
_reflns_number_gt                1840
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1142P)^2^+0.5391P] where P=(Fo^2^+2Fc^2^)/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         3444
_refine_ls_number_parameters     242
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.2413
_refine_ls_wR_factor_gt          0.2005
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.042
_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
S1 S 0.26048(17) 0.48432(15) 0.29985(15) 0.0302(4) Uani 1 1 d . . .
O1 O 0.4365(5) 0.5456(4) 0.3609(4) 0.0410(11) Uani 1 1 d . . .
O2 O 0.1515(5) 0.5649(4) 0.2381(4) 0.0361(10) Uani 1 1 d . . .
N1 N 0.2293(5) 0.4321(5) 0.4311(5) 0.0303(11) Uani 1 1 d . . .
H1N H 0.3363 0.4377 0.5158 0.036 Uiso 1 1 d R . .
F1 F 0.2766(4) 0.1100(4) 0.4559(4) 0.0474(10) Uani 1 1 d . . .
F2 F 0.5587(4) 0.0804(4) 0.6554(4) 0.0538(11) Uani 1 1 d . . .
F3 F 0.6719(4) 0.2079(4) 0.9330(4) 0.0570(11) Uani 1 1 d . . .
F4 F 0.5021(5) 0.3670(4) 1.0103(3) 0.0525(11) Uani 1 1 d . . .
F5 F 0.2236(4) 0.4026(4) 0.8116(4) 0.0442(9) Uani 1 1 d . . .
C1 C 0.1124(9) -0.0123(6) -0.1528(7) 0.0471(17) Uani 1 1 d . . .
H1A H -0.0079 -0.0513 -0.2074 0.071 Uiso 1 1 calc R . .
H1B H 0.1622 -0.0806 -0.1078 0.071 Uiso 1 1 calc R . .
H1C H 0.1616 0.0159 -0.2172 0.071 Uiso 1 1 calc R . .
C2 C 0.1450(8) 0.1092(6) -0.0392(6) 0.0349(14) Uani 1 1 d . . .
C3 C 0.2750(8) 0.1353(7) 0.0965(7) 0.0425(16) Uani 1 1 d . . .
H3 H 0.3415 0.0734 0.1175 0.051 Uiso 1 1 calc R . .
C4 C 0.3103(7) 0.2473(6) 0.2007(6) 0.0346(14) Uani 1 1 d . . .
H4 H 0.4003 0.2635 0.2920 0.042 Uiso 1 1 calc R . .
C5 C 0.2102(7) 0.3368(6) 0.1688(6) 0.0291(13) Uani 1 1 d . . .
C6 C 0.0784(7) 0.3128(6) 0.0364(6) 0.0289(13) Uani 1 1 d . . .
H6 H 0.0105 0.3738 0.0154 0.035 Uiso 1 1 calc R . .
C7 C 0.0477(7) 0.1989(6) -0.0646(6) 0.0343(14) Uani 1 1 d . . .
H7 H -0.0439 0.1814 -0.1551 0.041 Uiso 1 1 calc R . .
C8 C 0.0761(6) 0.3556(5) 0.4227(6) 0.0267(13) Uani 1 1 d . . .
C9 C -0.0751(7) 0.3649(6) 0.3242(6) 0.0323(14) Uani 1 1 d . . .
H9 H -0.0781 0.4204 0.2573 0.039 Uiso 1 1 calc R . .
C10 C -0.2216(7) 0.2929(6) 0.3239(6) 0.0360(15) Uani 1 1 d . . .
H10 H -0.3249 0.2992 0.2561 0.043 Uiso 1 1 calc R . .
C11 C -0.2202(7) 0.2130(6) 0.4191(6) 0.0380(15) Uani 1 1 d . . .
H11 H -0.3216 0.1651 0.4186 0.046 Uiso 1 1 calc R . .
C12 C -0.0708(7) 0.2024(6) 0.5160(6) 0.0364(15) Uani 1 1 d . . .
H12 H -0.0701 0.1461 0.5818 0.044 Uiso 1 1 calc R . .
C13 C 0.0793(7) 0.2720(6) 0.5197(6) 0.0299(13) Uani 1 1 d . . .
C14 C 0.2410(3) 0.2553(4) 0.6304(3) 0.0220(11) Uani 1 1 d GU . .
C15 C 0.3272(4) 0.1729(4) 0.5901(3) 0.0339(14) Uani 1 1 d GU . .
C16 C 0.4726(4) 0.1569(4) 0.6918(4) 0.0389(15) Uani 1 1 d GU . .
C17 C 0.5319(4) 0.2233(4) 0.8339(3) 0.0395(15) Uani 1 1 d GU . .
C18 C 0.4457(4) 0.3057(4) 0.8742(3) 0.0365(15) Uani 1 1 d GU . .
C19 C 0.3002(4) 0.3217(4) 0.7725(4) 0.0352(14) Uani 1 1 d GU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0257(8) 0.0313(8) 0.0268(8) 0.0155(6) 0.0040(6) 0.0023(6)
O1 0.026(2) 0.046(3) 0.034(2) 0.020(2) 0.0011(18) -0.0096(19)
O2 0.040(2) 0.028(2) 0.030(2) 0.0110(17) 0.0033(18) 0.0075(19)
N1 0.025(2) 0.036(3) 0.022(2) 0.010(2) 0.0009(19) 0.005(2)
F1 0.052(2) 0.052(2) 0.036(2) 0.0051(17) 0.0149(18) 0.0187(19)
F2 0.053(2) 0.058(3) 0.059(3) 0.018(2) 0.023(2) 0.033(2)
F3 0.044(2) 0.066(3) 0.052(2) 0.023(2) 0.0039(19) 0.023(2)
F4 0.060(2) 0.055(2) 0.0265(19) 0.0065(17) 0.0033(17) 0.013(2)
F5 0.047(2) 0.050(2) 0.039(2) 0.0128(17) 0.0167(17) 0.0215(18)
C1 0.065(5) 0.039(4) 0.051(4) 0.014(3) 0.036(4) 0.016(3)
C2 0.038(3) 0.038(4) 0.037(3) 0.013(3) 0.023(3) 0.010(3)
C3 0.043(4) 0.050(4) 0.052(4) 0.031(4) 0.026(3) 0.025(3)
C4 0.026(3) 0.046(4) 0.032(3) 0.015(3) 0.009(3) 0.014(3)
C5 0.025(3) 0.034(3) 0.031(3) 0.015(3) 0.013(3) 0.009(3)
C6 0.023(3) 0.036(3) 0.028(3) 0.018(3) 0.007(2) 0.011(3)
C7 0.033(3) 0.045(4) 0.024(3) 0.012(3) 0.010(3) 0.010(3)
C8 0.023(3) 0.026(3) 0.026(3) 0.004(2) 0.007(2) 0.004(2)
C9 0.033(3) 0.033(3) 0.029(3) 0.008(3) 0.008(3) 0.015(3)
C10 0.027(3) 0.051(4) 0.030(3) 0.008(3) 0.009(3) 0.017(3)
C11 0.029(3) 0.042(4) 0.038(4) 0.003(3) 0.014(3) 0.005(3)
C12 0.035(4) 0.041(4) 0.035(3) 0.013(3) 0.017(3) 0.006(3)
C13 0.028(3) 0.036(3) 0.024(3) 0.011(3) 0.009(2) 0.007(3)
C14 0.0166(18) 0.0241(18) 0.0250(18) 0.0187(15) 0.0067(14) 0.0011(14)
C15 0.036(2) 0.031(2) 0.032(2) 0.0113(16) 0.0130(16) 0.0049(16)
C16 0.038(2) 0.040(2) 0.041(2) 0.0113(17) 0.0170(17) 0.0123(17)
C17 0.038(2) 0.039(2) 0.040(2) 0.0135(17) 0.0128(16) 0.0117(17)
C18 0.037(2) 0.037(2) 0.034(2) 0.0107(16) 0.0130(16) 0.0083(16)
C19 0.034(2) 0.033(2) 0.042(2) 0.0076(16) 0.0193(16) 0.0097(16)

_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 O2 1.428(4) . ?
S1 O1 1.435(4) . ?
S1 N1 1.630(5) . ?
S1 C5 1.762(6) . ?
N1 C8 1.417(7) . ?
F1 C15 1.320(4) . ?
F2 C16 1.331(4) . ?
F3 C17 1.343(4) . ?
F4 C18 1.325(4) . ?
F5 C19 1.306(4) . ?
C1 C2 1.505(8) . ?
C2 C7 1.379(8) . ?
C2 C3 1.395(9) . ?
C3 C4 1.372(8) . ?
C4 C5 1.398(8) . ?
C5 C6 1.382(7) . ?
C6 C7 1.377(8) . ?
C8 C9 1.387(7) . ?
C8 C13 1.401(7) . ?
C9 C10 1.384(8) . ?
C10 C11 1.361(8) . ?
C11 C12 1.375(8) . ?
C12 C13 1.389(8) . ?
C13 C14 1.531(6) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 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
O2 S1 O1 118.3(2) . . ?
O2 S1 N1 111.0(3) . . ?
O1 S1 N1 103.7(2) . . ?
O2 S1 C5 107.8(2) . . ?
O1 S1 C5 109.3(3) . . ?
N1 S1 C5 106.1(2) . . ?
C8 N1 S1 125.9(4) . . ?
C7 C2 C3 117.3(5) . . ?
C7 C2 C1 121.5(6) . . ?
C3 C2 C1 121.2(6) . . ?
C4 C3 C2 122.4(6) . . ?
C3 C4 C5 118.2(5) . . ?
C6 C5 C4 121.0(5) . . ?
C6 C5 S1 120.7(4) . . ?
C4 C5 S1 118.3(4) . . ?
C7 C6 C5 118.6(5) . . ?
C2 C7 C6 122.4(5) . . ?
C9 C8 C13 119.7(5) . . ?
C9 C8 N1 121.6(5) . . ?
C13 C8 N1 118.6(5) . . ?
C10 C9 C8 119.7(5) . . ?
C11 C10 C9 121.2(5) . . ?
C10 C11 C12 119.4(6) . . ?
C11 C12 C13 121.5(6) . . ?
C12 C13 C8 118.5(5) . . ?
C12 C13 C14 118.6(5) . . ?
C8 C13 C14 122.9(5) . . ?
C15 C14 C19 120.0 . . ?
C15 C14 C13 120.5(3) . . ?
C19 C14 C13 119.5(3) . . ?
F1 C15 C14 121.9(3) . . ?
F1 C15 C16 118.1(3) . . ?
C14 C15 C16 120.0 . . ?
F2 C16 C17 118.9(3) . . ?
F2 C16 C15 121.1(3) . . ?
C17 C16 C15 120.0 . . ?
F3 C17 C16 120.4(3) . . ?
F3 C17 C18 119.6(3) . . ?
C16 C17 C18 120.0 . . ?
F4 C18 C17 119.5(3) . . ?
F4 C18 C19 120.5(3) . . ?
C17 C18 C19 120.0 . . ?
F5 C19 C18 119.1(3) . . ?
F5 C19 C14 120.8(3) . . ?
C18 C19 C14 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.096

data_ob037
_database_code_depnum_ccdc_archive 'CCDC 286064'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H47 Br F5 N2 O2.50 S'
_chemical_formula_weight         742.72

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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                   10.863(4)
_cell_length_b                   16.807(6)
_cell_length_c                   21.000(7)
_cell_angle_alpha                74.118(6)
_cell_angle_beta                 83.011(6)
_cell_angle_gamma                89.974(6)
_cell_volume                     3658(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    899
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      17.26

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1548
_exptl_absorpt_coefficient_mu    1.240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15642
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_sigmaI/netI    0.1302
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.38
_diffrn_reflns_theta_max         19.78
_reflns_number_total             6598
_reflns_number_gt                4148
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

Hydrogen atoms were not added to the disordered solvent molecule.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         6598
_refine_ls_number_parameters     498
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0916
_refine_ls_wR_factor_ref         0.2477
_refine_ls_wR_factor_gt          0.2179
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
Br1 Br 0.42609(12) 0.97697(8) 0.14608(7) 0.0291(5) Uani 1 1 d . . .
Br2 Br 0.24820(12) 0.47489(8) 0.15022(7) 0.0306(5) Uani 1 1 d . . .
S2 S 0.6856(3) 1.00109(19) 0.28534(16) 0.0233(9) Uani 1 1 d . . .
S1 S 0.9165(3) 0.50043(19) 0.27735(17) 0.0251(9) Uani 1 1 d . . .
O1 O 0.8316(7) 0.4795(5) 0.3370(4) 0.027(2) Uani 1 1 d . . .
O2 O 0.9913(8) 0.5756(5) 0.2594(4) 0.035(2) Uani 1 1 d . . .
O3 O 0.7388(7) 0.9783(5) 0.3466(4) 0.029(2) Uani 1 1 d . . .
O4 O 0.6178(8) 1.0753(5) 0.2682(4) 0.033(2) Uani 1 1 d . . .
O5 O 0.6381(9) 0.0624(6) 0.0073(5) 0.065(3) Uani 1 1 d . . .
N1 N 1.0164(9) 0.4259(6) 0.2811(5) 0.025(3) Uani 1 1 d . . .
N2 N 0.3424(8) 0.2102(6) 0.2069(5) 0.020(3) Uani 1 1 d . . .
N3 N 0.6976(8) 0.2908(6) 0.7939(5) 0.019(3) Uani 1 1 d . . .
N4 N 0.5883(9) 0.9267(5) 0.2843(5) 0.025(3) Uani 1 1 d . . .
F1 F 1.1855(6) 0.3449(5) 0.3825(4) 0.047(2) Uani 1 1 d . . .
F2 F 1.2369(8) 0.4067(6) 0.4812(4) 0.079(3) Uani 1 1 d . . .
F3 F 1.0520(10) 0.4281(5) 0.5743(4) 0.078(3) Uani 1 1 d . . .
F4 F 0.8147(8) 0.3856(6) 0.5666(4) 0.072(3) Uani 1 1 d . . .
F5 F 0.7633(7) 0.3214(5) 0.4691(4) 0.050(2) Uani 1 1 d . . .
F6 F 0.7590(7) 0.8101(5) 0.4701(4) 0.046(2) Uani 1 1 d . . .
F7 F 0.6679(8) 0.8723(6) 0.5687(4) 0.068(3) Uani 1 1 d . . .
F8 F 0.4316(9) 0.9237(5) 0.5766(4) 0.072(3) Uani 1 1 d . . .
F9 F 0.2841(8) 0.9080(6) 0.4836(4) 0.072(3) Uani 1 1 d . . .
F10 F 0.3758(6) 0.8446(5) 0.3836(4) 0.047(2) Uani 1 1 d . . .
C1 C 0.9710(11) 0.3334(7) 0.4217(6) 0.021(3) Uiso 1 1 d . . .
C2 C 1.0906(13) 0.3551(8) 0.4265(7) 0.032(4) Uiso 1 1 d . . .
C3 C 1.1197(14) 0.3881(9) 0.4778(7) 0.042(4) Uiso 1 1 d . . .
C4 C 1.0265(13) 0.3974(9) 0.5228(7) 0.043(4) Uiso 1 1 d . . .
C5 C 0.9076(14) 0.3766(9) 0.5209(7) 0.042(4) Uiso 1 1 d . . .
C6 C 0.8818(12) 0.3426(7) 0.4699(6) 0.024(3) Uiso 1 1 d . . .
C7 C 0.9441(11) 0.2974(7) 0.3667(6) 0.023(3) Uiso 1 1 d . . .
C8 C 0.8915(11) 0.2160(7) 0.3837(6) 0.026(3) Uiso 1 1 d . . .
H8 H 0.8766 0.1849 0.4292 0.031 Uiso 1 1 calc R . .
C9 C 0.8616(11) 0.1816(8) 0.3345(6) 0.029(3) Uiso 1 1 d . . .
H9 H 0.8265 0.1270 0.3461 0.035 Uiso 1 1 calc R . .
C10 C 0.8830(12) 0.2267(8) 0.2691(7) 0.034(4) Uiso 1 1 d . . .
H10 H 0.8620 0.2029 0.2356 0.041 Uiso 1 1 calc R . .
C11 C 0.9336(12) 0.3048(8) 0.2510(7) 0.034(4) Uiso 1 1 d . . .
H11 H 0.9479 0.3351 0.2053 0.041 Uiso 1 1 calc R . .
C12 C 0.9646(11) 0.3404(7) 0.3002(6) 0.023(3) Uiso 1 1 d . . .
C13 C 0.8316(10) 0.5008(7) 0.2107(6) 0.018(3) Uiso 1 1 d . . .
C14 C 0.8934(12) 0.5113(7) 0.1481(6) 0.028(3) Uiso 1 1 d . . .
H14 H 0.9811 0.5188 0.1399 0.034 Uiso 1 1 calc R . .
C15 C 0.8242(13) 0.5107(8) 0.0969(7) 0.043(4) Uiso 1 1 d . . .
H15 H 0.8660 0.5157 0.0534 0.052 Uiso 1 1 calc R . .
C16 C 0.6957(12) 0.5030(8) 0.1074(7) 0.033(4) Uiso 1 1 d . . .
C17 C 0.6355(12) 0.4929(8) 0.1696(6) 0.032(4) Uiso 1 1 d . . .
H17 H 0.5476 0.4868 0.1777 0.038 Uiso 1 1 calc R . .
C18 C 0.7047(11) 0.4917(7) 0.2217(6) 0.022(3) Uiso 1 1 d . . .
H18 H 0.6631 0.4845 0.2655 0.026 Uiso 1 1 calc R . .
C19 C 0.6206(13) 0.5105(9) 0.0473(7) 0.046(4) Uiso 1 1 d . . .
H19A H 0.5350 0.4900 0.0641 0.069 Uiso 1 1 calc R . .
H19B H 0.6591 0.4776 0.0188 0.069 Uiso 1 1 calc R . .
H19C H 0.6203 0.5686 0.0214 0.069 Uiso 1 1 calc R . .
C20 C 0.5724(11) 0.8271(7) 0.4215(6) 0.019(3) Uiso 1 1 d . . .
C21 C 0.4526(13) 0.8522(8) 0.4271(7) 0.033(4) Uiso 1 1 d . . .
C22 C 0.4016(14) 0.8836(9) 0.4799(7) 0.044(4) Uiso 1 1 d . . .
C23 C 0.4755(13) 0.8910(8) 0.5264(7) 0.040(4) Uiso 1 1 d . . .
C24 C 0.5946(13) 0.8662(8) 0.5220(7) 0.041(4) Uiso 1 1 d . . .
C25 C 0.6430(13) 0.8329(8) 0.4714(6) 0.030(4) Uiso 1 1 d . . .
C26 C 0.6249(10) 0.7960(7) 0.3655(6) 0.018(3) Uiso 1 1 d . . .
C27 C 0.6687(11) 0.7137(7) 0.3799(6) 0.026(3) Uiso 1 1 d . . .
H27 H 0.6612 0.6799 0.4247 0.032 Uiso 1 1 calc R . .
C28 C 0.7211(12) 0.6839(9) 0.3292(7) 0.039(4) Uiso 1 1 d . . .
H28 H 0.7513 0.6294 0.3392 0.047 Uiso 1 1 calc R . .
C29 C 0.7315(11) 0.7315(8) 0.2634(7) 0.030(4) Uiso 1 1 d . . .
H29 H 0.7687 0.7099 0.2286 0.036 Uiso 1 1 calc R . .
C30 C 0.6870(11) 0.8105(7) 0.2490(6) 0.027(3) Uiso 1 1 d . . .
H30 H 0.6941 0.8438 0.2040 0.032 Uiso 1 1 calc R . .
C31 C 0.6322(11) 0.8414(7) 0.3000(6) 0.021(3) Uiso 1 1 d . . .
C32 C 0.8063(11) 1.0076(7) 0.2197(6) 0.024(3) Uiso 1 1 d . . .
C33 C 0.9275(11) 0.9911(7) 0.2357(6) 0.024(3) Uiso 1 1 d . . .
H33 H 0.9445 0.9762 0.2807 0.029 Uiso 1 1 calc R . .
C34 C 1.0224(12) 0.9975(7) 0.1824(6) 0.030(3) Uiso 1 1 d . . .
H34 H 1.1060 0.9903 0.1913 0.036 Uiso 1 1 calc R . .
C35 C 0.9968(12) 1.0136(8) 0.1192(6) 0.030(4) Uiso 1 1 d . . .
C36 C 0.8732(12) 1.0304(8) 0.1040(7) 0.033(4) Uiso 1 1 d . . .
H36 H 0.8555 1.0437 0.0592 0.040 Uiso 1 1 calc R . .
C37 C 0.7801(12) 1.0270(7) 0.1556(6) 0.026(3) Uiso 1 1 d . . .
H37 H 0.6974 1.0383 0.1464 0.031 Uiso 1 1 calc R . .
C38 C 1.1018(12) 1.0190(8) 0.0615(7) 0.042(4) Uiso 1 1 d . . .
H38A H 1.1808 1.0325 0.0748 0.063 Uiso 1 1 calc R . .
H38B H 1.0842 1.0622 0.0220 0.063 Uiso 1 1 calc R . .
H38C H 1.1071 0.9657 0.0509 0.063 Uiso 1 1 calc R . .
C46 C 0.5719(11) 0.2580(7) 0.8338(6) 0.022(3) Uiso 1 1 d . . .
H46A H 0.5118 0.2588 0.8018 0.026 Uiso 1 1 calc R . .
H46B H 0.5805 0.1995 0.8587 0.026 Uiso 1 1 calc R . .
C45 C 0.5175(11) 0.3040(8) 0.8828(6) 0.032(4) Uiso 1 1 d . . .
H45A H 0.5694 0.2963 0.9195 0.039 Uiso 1 1 calc R . .
H45B H 0.5175 0.3639 0.8599 0.039 Uiso 1 1 calc R . .
C44 C 0.3865(12) 0.2728(8) 0.9111(7) 0.034(4) Uiso 1 1 d . . .
H44A H 0.3528 0.3057 0.9414 0.041 Uiso 1 1 calc R . .
H44B H 0.3353 0.2830 0.8740 0.041 Uiso 1 1 calc R . .
C50 C 0.7902(11) 0.2967(7) 0.8425(6) 0.028(3) Uiso 1 1 d . . .
H50A H 0.8714 0.3169 0.8160 0.034 Uiso 1 1 calc R . .
H50B H 0.7613 0.3389 0.8653 0.034 Uiso 1 1 calc R . .
C49 C 0.8102(12) 0.2185(8) 0.8949(6) 0.034(4) Uiso 1 1 d . . .
H49A H 0.7316 0.1999 0.9246 0.040 Uiso 1 1 calc R . .
H49B H 0.8353 0.1745 0.8733 0.040 Uiso 1 1 calc R . .
C48 C 0.9088(11) 0.2321(8) 0.9354(7) 0.035(4) Uiso 1 1 d . . .
H48A H 0.9067 0.1840 0.9752 0.042 Uiso 1 1 calc R . .
H48B H 0.8886 0.2815 0.9512 0.042 Uiso 1 1 calc R . .
C47 C 1.0401(13) 0.2442(10) 0.8985(8) 0.058(5) Uiso 1 1 d . . .
H47A H 1.0440 0.2924 0.8594 0.087 Uiso 1 1 calc R . .
H47B H 1.0627 0.1948 0.8841 0.087 Uiso 1 1 calc R . .
H47C H 1.0982 0.2532 0.9283 0.087 Uiso 1 1 calc R . .
C54 C 0.7408(11) 0.2298(7) 0.7553(6) 0.024(3) Uiso 1 1 d . . .
H54A H 0.7366 0.1738 0.7869 0.029 Uiso 1 1 calc R . .
H54B H 0.6820 0.2297 0.7228 0.029 Uiso 1 1 calc R . .
C53 C 0.8695(11) 0.2462(7) 0.7183(6) 0.023(3) Uiso 1 1 d . . .
H53A H 0.9309 0.2368 0.7506 0.028 Uiso 1 1 calc R . .
H53B H 0.8791 0.3046 0.6911 0.028 Uiso 1 1 calc R . .
C52 C 0.8934(11) 0.1890(8) 0.6733(6) 0.029(3) Uiso 1 1 d . . .
H52A H 0.8725 0.1313 0.7002 0.035 Uiso 1 1 calc R . .
H52B H 0.8373 0.2031 0.6383 0.035 Uiso 1 1 calc R . .
C51 C 1.0253(12) 0.1936(8) 0.6402(7) 0.039(4) Uiso 1 1 d . . .
H51A H 1.0805 0.1718 0.6740 0.059 Uiso 1 1 calc R . .
H51B H 1.0496 0.2514 0.6169 0.059 Uiso 1 1 calc R . .
H51C H 1.0317 0.1607 0.6080 0.059 Uiso 1 1 calc R . .
C42 C 0.6886(11) 0.3759(7) 0.7491(6) 0.025(3) Uiso 1 1 d . . .
H42A H 0.7716 0.3938 0.7240 0.030 Uiso 1 1 calc R . .
H42B H 0.6675 0.4136 0.7774 0.030 Uiso 1 1 calc R . .
C41 C 0.5946(11) 0.3872(7) 0.6988(6) 0.029(3) Uiso 1 1 d . . .
H41A H 0.6093 0.3466 0.6725 0.034 Uiso 1 1 calc R . .
H41B H 0.5095 0.3768 0.7229 0.034 Uiso 1 1 calc R . .
C40 C 0.6066(12) 0.4740(8) 0.6524(6) 0.033(4) Uiso 1 1 d . . .
H40A H 0.6933 0.4853 0.6306 0.040 Uiso 1 1 calc R . .
H40B H 0.5871 0.5142 0.6787 0.040 Uiso 1 1 calc R . .
C39 C 0.5193(12) 0.4857(8) 0.5988(7) 0.040(4) Uiso 1 1 d . . .
H39A H 0.4332 0.4760 0.6202 0.061 Uiso 1 1 calc R . .
H39B H 0.5389 0.4464 0.5724 0.061 Uiso 1 1 calc R . .
H39C H 0.5299 0.5424 0.5695 0.061 Uiso 1 1 calc R . .
C58 C 0.2338(10) 0.2449(7) 0.1688(6) 0.018(3) Uiso 1 1 d . . .
H58A H 0.1604 0.2456 0.2016 0.022 Uiso 1 1 calc R . .
H58B H 0.2553 0.3030 0.1430 0.022 Uiso 1 1 calc R . .
C57 C 0.1982(11) 0.1974(8) 0.1212(6) 0.030(3) Uiso 1 1 d . . .
H57A H 0.1837 0.1380 0.1453 0.036 Uiso 1 1 calc R . .
H57B H 0.2669 0.2022 0.0846 0.036 Uiso 1 1 calc R . .
C56 C 0.0805(12) 0.2323(8) 0.0923(7) 0.034(4) Uiso 1 1 d . . .
H56A H 0.0571 0.1990 0.0630 0.041 Uiso 1 1 calc R . .
H56B H 0.0125 0.2253 0.1295 0.041 Uiso 1 1 calc R . .
C62 C 0.3135(10) 0.1256(7) 0.2524(6) 0.021(3) Uiso 1 1 d . . .
H62A H 0.3845 0.1089 0.2780 0.026 Uiso 1 1 calc R . .
H62B H 0.3074 0.0870 0.2247 0.026 Uiso 1 1 calc R . .
C61 C 0.1963(11) 0.1141(7) 0.3018(6) 0.026(3) Uiso 1 1 d . . .
H61A H 0.1976 0.1551 0.3278 0.031 Uiso 1 1 calc R . .
H61B H 0.1231 0.1241 0.2772 0.031 Uiso 1 1 calc R . .
C59 C 0.0765(12) 0.0141(9) 0.4034(7) 0.047(4) Uiso 1 1 d . . .
H59A H 0.0861 0.0512 0.4313 0.070 Uiso 1 1 calc R . .
H59B H 0.0733 -0.0435 0.4309 0.070 Uiso 1 1 calc R . .
H59C H -0.0005 0.0258 0.3832 0.070 Uiso 1 1 calc R . .
C70 C 0.3664(11) 0.2707(7) 0.2460(6) 0.023(3) Uiso 1 1 d . . .
H70A H 0.2932 0.2687 0.2795 0.028 Uiso 1 1 calc R . .
H70B H 0.3730 0.3272 0.2149 0.028 Uiso 1 1 calc R . .
C69 C 0.4828(11) 0.2575(7) 0.2823(6) 0.026(3) Uiso 1 1 d . . .
H69A H 0.4818 0.2000 0.3113 0.031 Uiso 1 1 calc R . .
H69B H 0.5583 0.2666 0.2494 0.031 Uiso 1 1 calc R . .
C68 C 0.4839(11) 0.3177(8) 0.3240(6) 0.028(3) Uiso 1 1 d . . .
H68A H 0.4106 0.3060 0.3586 0.033 Uiso 1 1 calc R . .
H68B H 0.4782 0.3747 0.2953 0.033 Uiso 1 1 calc R . .
C67 C 0.6021(12) 0.3115(8) 0.3578(7) 0.039(4) Uiso 1 1 d . . .
H67A H 0.6076 0.2552 0.3865 0.059 Uiso 1 1 calc R . .
H67B H 0.5998 0.3508 0.3848 0.059 Uiso 1 1 calc R . .
H67C H 0.6747 0.3247 0.3236 0.059 Uiso 1 1 calc R . .
C66 C 0.4544(11) 0.2038(7) 0.1592(6) 0.024(3) Uiso 1 1 d . . .
H66A H 0.4353 0.1617 0.1364 0.029 Uiso 1 1 calc R . .
H66B H 0.5233 0.1832 0.1854 0.029 Uiso 1 1 calc R . .
C65 C 0.4996(11) 0.2841(7) 0.1057(6) 0.030(4) Uiso 1 1 d . . .
H65A H 0.4366 0.3012 0.0747 0.036 Uiso 1 1 calc R . .
H65B H 0.5105 0.3287 0.1272 0.036 Uiso 1 1 calc R . .
C64 C 0.6216(11) 0.2718(8) 0.0667(6) 0.031(4) Uiso 1 1 d . . .
H64A H 0.6396 0.3204 0.0273 0.037 Uiso 1 1 calc R . .
H64B H 0.6123 0.2226 0.0502 0.037 Uiso 1 1 calc R . .
C60 C 0.1857(12) 0.0275(8) 0.3489(6) 0.032(4) Uiso 1 1 d . . .
H60A H 0.2631 0.0162 0.3699 0.038 Uiso 1 1 calc R . .
H60B H 0.1779 -0.0127 0.3228 0.038 Uiso 1 1 calc R . .
C55 C 0.0908(12) 0.3199(8) 0.0538(6) 0.035(4) Uiso 1 1 d . . .
H55A H 0.1070 0.3541 0.0831 0.052 Uiso 1 1 calc R . .
H55B H 0.0131 0.3360 0.0353 0.052 Uiso 1 1 calc R . .
H55C H 0.1592 0.3280 0.0174 0.052 Uiso 1 1 calc R . .
C63 C 0.7319(13) 0.2604(9) 0.1064(7) 0.050(4) Uiso 1 1 d . . .
H63A H 0.7450 0.3100 0.1210 0.075 Uiso 1 1 calc R . .
H63B H 0.8064 0.2514 0.0782 0.075 Uiso 1 1 calc R . .
H63C H 0.7153 0.2123 0.1456 0.075 Uiso 1 1 calc R . .
C43 C 0.3731(12) 0.1834(8) 0.9484(7) 0.038(4) Uiso 1 1 d . . .
H43A H 0.4313 0.1708 0.9817 0.057 Uiso 1 1 calc R . .
H43B H 0.3911 0.1497 0.9172 0.057 Uiso 1 1 calc R . .
H43C H 0.2880 0.1708 0.9709 0.057 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0326(9) 0.0224(8) 0.0338(9) -0.0097(7) -0.0054(7) 0.0000(6)
Br2 0.0341(9) 0.0218(8) 0.0378(10) -0.0125(7) -0.0018(7) 0.0011(6)
S2 0.026(2) 0.019(2) 0.025(2) -0.0066(17) -0.0050(17) 0.0023(17)
S1 0.025(2) 0.020(2) 0.029(2) -0.0057(17) -0.0024(19) 0.0023(18)
O1 0.019(5) 0.029(5) 0.032(6) -0.007(5) -0.001(5) 0.005(4)
O2 0.038(6) 0.017(5) 0.044(6) -0.001(5) 0.002(5) -0.013(5)
O3 0.033(6) 0.027(5) 0.029(6) -0.010(4) -0.011(5) -0.006(4)
O4 0.043(6) 0.018(5) 0.036(6) -0.007(4) -0.001(5) 0.007(5)
O5 0.041(7) 0.073(8) 0.078(8) -0.015(7) -0.007(6) -0.001(6)
N1 0.029(7) 0.016(6) 0.030(7) -0.005(5) -0.011(5) 0.007(5)
N2 0.018(6) 0.020(6) 0.026(6) -0.013(5) 0.002(5) 0.002(5)
N3 0.014(6) 0.021(6) 0.025(6) -0.011(5) 0.000(5) -0.004(5)
N4 0.033(7) 0.006(6) 0.034(7) -0.003(5) -0.004(5) -0.005(5)
F1 0.023(5) 0.069(6) 0.039(5) 0.003(4) -0.009(4) 0.005(4)
F2 0.076(7) 0.087(7) 0.056(6) 0.027(5) -0.044(5) -0.060(6)
F3 0.160(10) 0.044(6) 0.041(6) -0.012(5) -0.050(6) -0.001(6)
F4 0.085(7) 0.095(7) 0.045(6) -0.037(5) -0.013(5) 0.041(6)
F5 0.026(5) 0.088(6) 0.037(5) -0.019(5) -0.002(4) 0.015(4)
F6 0.030(5) 0.072(6) 0.037(5) -0.014(4) -0.009(4) -0.002(4)
F7 0.081(7) 0.093(7) 0.035(5) -0.029(5) 0.003(5) -0.036(5)
F8 0.118(8) 0.055(6) 0.039(6) -0.022(5) 0.030(5) 0.013(5)
F9 0.056(6) 0.084(7) 0.053(6) 0.013(5) 0.016(5) 0.041(5)
F10 0.026(5) 0.066(6) 0.040(5) -0.001(4) -0.005(4) -0.003(4)

_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
S2 O4 1.430(8) . ?
S2 O3 1.431(8) . ?
S2 N4 1.645(10) . ?
S2 C32 1.764(13) . ?
S1 O1 1.422(8) . ?
S1 O2 1.436(8) . ?
S1 N1 1.649(10) . ?
S1 C13 1.766(12) . ?
N1 C12 1.473(15) . ?
N2 C62 1.489(14) . ?
N2 C66 1.502(14) . ?
N2 C70 1.512(14) . ?
N2 C58 1.532(14) . ?
N3 C42 1.491(14) . ?
N3 C54 1.513(14) . ?
N3 C46 1.530(14) . ?
N3 C50 1.539(15) . ?
N4 C31 1.473(15) . ?
F1 C2 1.342(14) . ?
F2 C3 1.326(16) . ?
F3 C4 1.375(16) . ?
F4 C5 1.344(16) . ?
F5 C6 1.339(14) . ?
F6 C25 1.316(14) . ?
F7 C24 1.361(16) . ?
F8 C23 1.354(15) . ?
F9 C22 1.340(15) . ?
F10 C21 1.340(15) . ?
C1 C6 1.353(16) . ?
C1 C2 1.372(16) . ?
C1 C7 1.501(16) . ?
C2 C3 1.407(18) . ?
C3 C4 1.338(18) . ?
C4 C5 1.347(18) . ?
C5 C6 1.400(18) . ?
C7 C12 1.377(16) . ?
C7 C8 1.417(16) . ?
C8 C9 1.384(16) . ?
C9 C10 1.365(16) . ?
C10 C11 1.360(17) . ?
C11 C12 1.401(17) . ?
C13 C14 1.367(16) . ?
C13 C18 1.372(15) . ?
C14 C15 1.386(17) . ?
C15 C16 1.387(17) . ?
C16 C17 1.354(17) . ?
C16 C19 1.562(18) . ?
C17 C18 1.396(16) . ?
C20 C21 1.369(16) . ?
C20 C25 1.396(17) . ?
C20 C26 1.467(16) . ?
C21 C22 1.410(18) . ?
C22 C23 1.368(18) . ?
C23 C24 1.360(18) . ?
C24 C25 1.381(18) . ?
C26 C31 1.372(15) . ?
C26 C27 1.426(16) . ?
C27 C28 1.362(17) . ?
C28 C29 1.385(17) . ?
C29 C30 1.380(16) . ?
C30 C31 1.385(16) . ?
C32 C37 1.361(16) . ?
C32 C33 1.407(16) . ?
C33 C34 1.408(16) . ?
C34 C35 1.344(17) . ?
C35 C36 1.427(17) . ?
C35 C38 1.544(17) . ?
C36 C37 1.378(16) . ?
C46 C45 1.514(16) . ?
C45 C44 1.509(17) . ?
C44 C43 1.491(17) . ?
C50 C49 1.500(16) . ?
C49 C48 1.499(17) . ?
C48 C47 1.524(18) . ?
C54 C53 1.502(16) . ?
C53 C52 1.525(16) . ?
C52 C51 1.507(17) . ?
C42 C41 1.532(16) . ?
C41 C40 1.512(16) . ?
C40 C39 1.530(17) . ?
C58 C57 1.523(16) . ?
C57 C56 1.530(17) . ?
C56 C55 1.470(16) . ?
C62 C61 1.517(16) . ?
C61 C60 1.515(16) . ?
C59 C60 1.515(17) . ?
C70 C69 1.540(16) . ?
C69 C68 1.509(16) . ?
C68 C67 1.531(17) . ?
C66 C65 1.538(16) . ?
C65 C64 1.515(16) . ?
C64 C63 1.524(17) . ?

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
O4 S2 O3 120.2(5) . . ?
O4 S2 N4 105.0(5) . . ?
O3 S2 N4 109.0(5) . . ?
O4 S2 C32 107.2(6) . . ?
O3 S2 C32 107.7(5) . . ?
N4 S2 C32 107.0(5) . . ?
O1 S1 O2 120.3(5) . . ?
O1 S1 N1 108.5(5) . . ?
O2 S1 N1 105.1(5) . . ?
O1 S1 C13 107.4(5) . . ?
O2 S1 C13 108.2(5) . . ?
N1 S1 C13 106.6(5) . . ?
C12 N1 S1 116.9(8) . . ?
C62 N2 C66 106.8(8) . . ?
C62 N2 C70 110.8(9) . . ?
C66 N2 C70 111.4(9) . . ?
C62 N2 C58 112.3(9) . . ?
C66 N2 C58 110.6(9) . . ?
C70 N2 C58 105.2(8) . . ?
C42 N3 C54 112.0(9) . . ?
C42 N3 C46 111.2(9) . . ?
C54 N3 C46 107.2(8) . . ?
C42 N3 C50 107.0(8) . . ?
C54 N3 C50 110.3(9) . . ?
C46 N3 C50 109.1(9) . . ?
C31 N4 S2 117.9(8) . . ?
C6 C1 C2 117.2(12) . . ?
C6 C1 C7 122.6(11) . . ?
C2 C1 C7 120.1(11) . . ?
F1 C2 C1 121.2(12) . . ?
F1 C2 C3 116.9(12) . . ?
C1 C2 C3 121.8(13) . . ?
F2 C3 C4 122.5(14) . . ?
F2 C3 C2 119.7(13) . . ?
C4 C3 C2 117.8(14) . . ?
C3 C4 C5 122.9(15) . . ?
C3 C4 F3 119.3(13) . . ?
C5 C4 F3 117.8(14) . . ?
F4 C5 C4 122.4(14) . . ?
F4 C5 C6 119.6(12) . . ?
C4 C5 C6 118.0(14) . . ?
F5 C6 C1 120.5(11) . . ?
F5 C6 C5 117.2(11) . . ?
C1 C6 C5 122.3(12) . . ?
C12 C7 C8 118.0(11) . . ?
C12 C7 C1 123.2(11) . . ?
C8 C7 C1 118.8(11) . . ?
C9 C8 C7 120.6(12) . . ?
C10 C9 C8 119.6(12) . . ?
C11 C10 C9 121.5(13) . . ?
C10 C11 C12 119.6(13) . . ?
C7 C12 C11 120.8(11) . . ?
C7 C12 N1 119.3(11) . . ?
C11 C12 N1 119.9(11) . . ?
C14 C13 C18 120.5(11) . . ?
C14 C13 S1 119.4(9) . . ?
C18 C13 S1 120.1(9) . . ?
C13 C14 C15 118.1(12) . . ?
C14 C15 C16 121.8(13) . . ?
C17 C16 C15 119.6(13) . . ?
C17 C16 C19 120.1(12) . . ?
C15 C16 C19 120.2(12) . . ?
C16 C17 C18 119.0(12) . . ?
C13 C18 C17 121.1(12) . . ?
C21 C20 C25 116.9(11) . . ?
C21 C20 C26 121.8(11) . . ?
C25 C20 C26 121.2(11) . . ?
F10 C21 C20 121.1(12) . . ?
F10 C21 C22 116.4(12) . . ?
C20 C21 C22 122.4(13) . . ?
F9 C22 C23 120.5(13) . . ?
F9 C22 C21 120.8(13) . . ?
C23 C22 C21 118.7(14) . . ?
F8 C23 C24 119.5(13) . . ?
F8 C23 C22 120.7(13) . . ?
C24 C23 C22 119.8(14) . . ?
C23 C24 F7 120.0(13) . . ?
C23 C24 C25 121.3(14) . . ?
F7 C24 C25 118.7(13) . . ?
F6 C25 C24 118.1(12) . . ?
F6 C25 C20 121.1(11) . . ?
C24 C25 C20 120.7(13) . . ?
C31 C26 C27 118.2(11) . . ?
C31 C26 C20 123.4(10) . . ?
C27 C26 C20 118.3(11) . . ?
C28 C27 C26 119.7(12) . . ?
C27 C28 C29 121.4(13) . . ?
C30 C29 C28 119.3(13) . . ?
C29 C30 C31 120.0(12) . . ?
C26 C31 C30 121.4(11) . . ?
C26 C31 N4 118.9(10) . . ?
C30 C31 N4 119.6(11) . . ?
C37 C32 C33 122.0(11) . . ?
C37 C32 S2 119.7(9) . . ?
C33 C32 S2 118.3(9) . . ?
C32 C33 C34 117.3(12) . . ?
C35 C34 C33 121.1(12) . . ?
C34 C35 C36 120.5(12) . . ?
C34 C35 C38 120.4(12) . . ?
C36 C35 C38 119.0(11) . . ?
C37 C36 C35 118.9(12) . . ?
C32 C37 C36 120.2(12) . . ?
C45 C46 N3 116.5(10) . . ?
C44 C45 C46 110.6(11) . . ?
C43 C44 C45 115.3(11) . . ?
C49 C50 N3 116.7(10) . . ?
C48 C49 C50 110.7(11) . . ?
C49 C48 C47 114.9(12) . . ?
C53 C54 N3 115.5(9) . . ?
C54 C53 C52 109.9(10) . . ?
C51 C52 C53 113.8(11) . . ?
N3 C42 C41 116.8(10) . . ?
C40 C41 C42 110.4(10) . . ?
C41 C40 C39 111.7(11) . . ?
C57 C58 N2 115.0(9) . . ?
C58 C57 C56 109.8(10) . . ?
C55 C56 C57 115.1(11) . . ?
N2 C62 C61 117.0(9) . . ?
C60 C61 C62 110.9(10) . . ?
N2 C70 C69 116.6(9) . . ?
C68 C69 C70 108.9(10) . . ?
C69 C68 C67 111.3(10) . . ?
N2 C66 C65 116.1(9) . . ?
C64 C65 C66 110.7(10) . . ?
C65 C64 C63 114.5(11) . . ?
C61 C60 C59 113.7(11) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        19.78
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.169
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.132