# Electronic Supplementary Material (ESI) for Green Chemistry
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Green Chemistry'
_journal_coden_cambridge         1048
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       albertovpuga@hotmail.com
loop_
_publ_author_name
T.Belhocine
S.A.Forsyth
H.Q.N.Gunaratne
M.Nieuwenhuyzen
;
P.Nockemann
;
A.V.Puga
K.R.Seddon
G.Srinivasan
K.Whiston

# Attachment '- k09prr34.cif'

data_k09prr34
_database_code_depnum_ccdc_archive 'CCDC 812182'
#TrackingRef '- k09prr34.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H24 I N'
_chemical_formula_weight         297.21

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   14.0810(2)
_cell_length_b                   14.0810(2)
_cell_length_c                   27.3030(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5413.49(13)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       colourless
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2400
_exptl_absorpt_coefficient_mu    2.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_T_max  0.6527
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_diffrn_ambient_temperature      150(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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30345
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3096
_reflns_number_gt                2476
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       KappaCCD
_computing_cell_refinement       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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^)+(0.0712P)^2^+5.1775P] 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    geom
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3096
_refine_ls_number_parameters     106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.1224
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.144
_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
N1 N 0.6437(7) 0.0926(7) 0.5835(3) 0.032(3) Uiso 0.50 1 d P A 1
C2 C 0.6380(5) -0.0154(5) 0.5919(2) 0.0264(14) Uiso 0.50 1 d P A 1
H2A H 0.6569 -0.0483 0.5614 0.032 Uiso 0.50 1 calc PR A 1
H2B H 0.6842 -0.0332 0.6176 0.032 Uiso 0.50 1 calc PR A 1
C3 C 0.5394(6) -0.0507(6) 0.6071(3) 0.0352(17) Uiso 0.50 1 d P A 1
H3A H 0.4908 -0.0090 0.5921 0.042 Uiso 0.50 1 calc PR A 1
H3B H 0.5299 -0.1155 0.5939 0.042 Uiso 0.50 1 calc PR A 1
C4 C 0.5236(8) -0.0530(8) 0.6626(4) 0.041(2) Uiso 0.50 1 d P A 1
H4A H 0.5791 -0.0838 0.6783 0.049 Uiso 0.50 1 calc PR A 1
H4B H 0.4671 -0.0925 0.6697 0.049 Uiso 0.50 1 calc PR A 1
C5 C 0.5094(7) 0.0453(9) 0.6855(4) 0.038(2) Uiso 0.50 1 d P A 1
H5A H 0.5054 0.0384 0.7215 0.046 Uiso 0.50 1 calc PR A 1
H5B H 0.4482 0.0718 0.6739 0.046 Uiso 0.50 1 calc PR A 1
C6 C 0.5894(6) 0.1158(6) 0.6731(3) 0.0352(17) Uiso 0.50 1 d P A 1
H6A H 0.6516 0.0853 0.6791 0.042 Uiso 0.50 1 calc PR A 1
H6B H 0.5845 0.1719 0.6948 0.042 Uiso 0.50 1 calc PR A 1
C7 C 0.5839(5) 0.1489(5) 0.6185(2) 0.0243(14) Uiso 0.50 1 d P A 1
H7A H 0.5169 0.1455 0.6077 0.029 Uiso 0.50 1 calc PR A 1
H7B H 0.6037 0.2163 0.6168 0.029 Uiso 0.50 1 calc PR A 1
C8 C 0.7458(5) 0.1220(5) 0.5905(3) 0.0268(14) Uiso 0.50 1 d P A 1
H8A H 0.7616 0.1153 0.6256 0.032 Uiso 0.50 1 calc PR A 1
H8B H 0.7512 0.1902 0.5821 0.032 Uiso 0.50 1 calc PR A 1
C9 C 0.8215(6) 0.0668(8) 0.5603(3) 0.036(2) Uiso 0.50 1 d P A 1
H9A H 0.8246 -0.0003 0.5711 0.044 Uiso 0.50 1 calc PR A 1
H9B H 0.8059 0.0685 0.5250 0.044 Uiso 0.50 1 calc PR A 1
C10 C 0.9164(8) 0.1172(8) 0.5701(4) 0.057(2) Uiso 0.50 1 d P A 1
H10A H 0.9116 0.1845 0.5599 0.069 Uiso 0.50 1 calc PR A 1
H10B H 0.9305 0.1157 0.6056 0.069 Uiso 0.50 1 calc PR A 1
C11 C 0.9965(9) 0.0691(10) 0.5420(4) 0.066(3) Uiso 0.50 1 d P A 1
H11A H 1.0563 0.1023 0.5485 0.098 Uiso 0.50 1 calc PR A 1
H11B H 0.9827 0.0712 0.5068 0.098 Uiso 0.50 1 calc PR A 1
H11C H 1.0019 0.0028 0.5525 0.098 Uiso 0.50 1 calc PR A 1
C71 C 0.6057(10) 0.1240(11) 0.5372(5) 0.034(4) Uiso 0.50 1 d P A 1
H71A H 0.6118 0.1932 0.5347 0.050 Uiso 0.50 1 calc PR A 1
H71B H 0.5385 0.1063 0.5350 0.050 Uiso 0.50 1 calc PR A 1
H71C H 0.6409 0.0939 0.5104 0.050 Uiso 0.50 1 calc PR A 1
N1' N 0.6412(7) 0.0715(8) 0.5824(4) 0.034(3) Uiso 0.50 1 d P B 2
C2' C 0.5733(7) -0.0179(7) 0.5863(3) 0.044(2) Uiso 0.50 1 d P B 2
H2'A H 0.5086 0.0018 0.5763 0.053 Uiso 0.50 1 calc PR B 2
H2'B H 0.5953 -0.0662 0.5625 0.053 Uiso 0.50 1 calc PR B 2
C3' C 0.5669(8) -0.0640(7) 0.6363(4) 0.053(2) Uiso 0.50 1 d P B 2
H3'A H 0.5460 -0.1305 0.6316 0.064 Uiso 0.50 1 calc PR B 2
H3'B H 0.6316 -0.0659 0.6504 0.064 Uiso 0.50 1 calc PR B 2
C4' C 0.5031(7) -0.0191(9) 0.6726(4) 0.045(2) Uiso 0.50 1 d P B 2
H4'A H 0.4388 -0.0174 0.6580 0.054 Uiso 0.50 1 calc PR B 2
H4'B H 0.4999 -0.0621 0.7012 0.054 Uiso 0.50 1 calc PR B 2
C5' C 0.5236(10) 0.0764(10) 0.6912(4) 0.055(3) Uiso 0.50 1 d P B 2
H5'A H 0.5756 0.0720 0.7155 0.065 Uiso 0.50 1 calc PR B 2
H5'B H 0.4666 0.1006 0.7084 0.065 Uiso 0.50 1 calc PR B 2
C6' C 0.5510(9) 0.1451(9) 0.6530(5) 0.067(3) Uiso 0.50 1 d P B 2
H6'A H 0.4992 0.1469 0.6285 0.080 Uiso 0.50 1 calc PR B 2
H6'B H 0.5536 0.2086 0.6685 0.080 Uiso 0.50 1 calc PR B 2
C7' C 0.6386(7) 0.1314(8) 0.6269(4) 0.052(2) Uiso 0.50 1 d P B 2
H7'A H 0.6850 0.1044 0.6503 0.063 Uiso 0.50 1 calc PR B 2
H7'B H 0.6624 0.1950 0.6176 0.063 Uiso 0.50 1 calc PR B 2
C8' C 0.7390(7) 0.0307(7) 0.5721(3) 0.047(2) Uiso 0.50 1 d P B 2
H8'A H 0.7541 -0.0169 0.5977 0.056 Uiso 0.50 1 calc PR B 2
H8'B H 0.7372 -0.0028 0.5403 0.056 Uiso 0.50 1 calc PR B 2
C9' C 0.8156(7) 0.1018(8) 0.5707(5) 0.049(3) Uiso 0.50 1 d P B 2
H9'A H 0.8209 0.1320 0.6034 0.059 Uiso 0.50 1 calc PR B 2
H9'B H 0.7985 0.1519 0.5469 0.059 Uiso 0.50 1 calc PR B 2
C10' C 0.9112(9) 0.0604(10) 0.5568(4) 0.066(3) Uiso 0.50 1 d P B 2
H10C H 0.9289 0.0125 0.5817 0.079 Uiso 0.50 1 calc PR B 2
H10D H 0.9041 0.0267 0.5251 0.079 Uiso 0.50 1 calc PR B 2
C11' C 0.9906(9) 0.1293(9) 0.5521(4) 0.068(3) Uiso 0.50 1 d P B 2
H11D H 1.0491 0.0953 0.5436 0.102 Uiso 0.50 1 calc PR B 2
H11E H 0.9995 0.1625 0.5833 0.102 Uiso 0.50 1 calc PR B 2
H11F H 0.9757 0.1755 0.5264 0.102 Uiso 0.50 1 calc PR B 2
C71' C 0.6136(12) 0.1129(13) 0.5322(6) 0.045(5) Uiso 0.50 1 d P B 2
H71D H 0.6519 0.1696 0.5256 0.067 Uiso 0.50 1 calc PR B 2
H71E H 0.5462 0.1301 0.5323 0.067 Uiso 0.50 1 calc PR B 2
H71F H 0.6252 0.0654 0.5066 0.067 Uiso 0.50 1 calc PR B 2
I1 I 0.188919(19) -0.102462(18) 0.054391(9) 0.03574(14) Uani 1 1 d . . .

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
I1 0.04077(19) 0.03213(18) 0.03433(19) -0.00118(9) 0.00335(10) 0.00022(10)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C71 1.441(17) . ?
N1 C7 1.501(12) . ?
N1 C8 1.508(12) . ?
N1 C2 1.541(12) . ?
C2 C3 1.533(11) . ?
C3 C4 1.531(12) . ?
C4 C5 1.533(14) . ?
C5 C6 1.539(14) . ?
C6 C7 1.563(10) . ?
C8 C9 1.555(12) . ?
C9 C10 1.536(15) . ?
C10 C11 1.523(16) . ?
N1' C7' 1.478(15) . ?
N1' C8' 1.519(14) . ?
N1' C71' 1.54(2) . ?
N1' C2' 1.584(14) . ?
C2' C3' 1.513(14) . ?
C3' C4' 1.480(14) . ?
C4' C5' 1.466(16) . ?
C5' C6' 1.474(16) . ?
C6' C7' 1.438(15) . ?
C8' C9' 1.472(15) . ?
C9' C10' 1.516(17) . ?
C10' C11' 1.486(18) . ?

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
C71 N1 C7 100.9(9) . . ?
C71 N1 C8 112.4(9) . . ?
C7 N1 C8 108.0(7) . . ?
C71 N1 C2 114.5(9) . . ?
C7 N1 C2 113.4(7) . . ?
C8 N1 C2 107.5(7) . . ?
C3 C2 N1 114.1(7) . . ?
C4 C3 C2 114.0(7) . . ?
C3 C4 C5 113.8(8) . . ?
C4 C5 C6 113.4(8) . . ?
C5 C6 C7 111.5(7) . . ?
N1 C7 C6 115.0(7) . . ?
N1 C8 C9 116.7(7) . . ?
C10 C9 C8 105.9(8) . . ?
C11 C10 C9 110.5(10) . . ?
C7' N1' C8' 113.0(9) . . ?
C7' N1' C71' 120.6(11) . . ?
C8' N1' C71' 101.9(9) . . ?
C7' N1' C2' 112.6(8) . . ?
C8' N1' C2' 105.0(8) . . ?
C71' N1' C2' 102.0(9) . . ?
C3' C2' N1' 115.9(8) . . ?
C4' C3' C2' 117.2(9) . . ?
C5' C4' C3' 120.3(9) . . ?
C4' C5' C6' 114.1(10) . . ?
C7' C6' C5' 119.2(11) . . ?
C6' C7' N1' 120.3(9) . . ?
C9' C8' N1' 114.3(9) . . ?
C8' C9' C10' 113.3(10) . . ?
C11' C10' C9' 116.0(12) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.845
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.173


data_2010src0804
_database_code_depnum_ccdc_archive 'CCDC 812183'
#TrackingRef '- 2010src0804.cif'

_audit_creation_date             2010-12-20
_audit_creation_method           
;
Olex2 1.1
(compiled 2010.09.30 svn.r1450, GUI svn.r3284)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C13 H28 N, C2 F6 N O4 S2'
_chemical_formula_sum            'C15 H28 F6 N2 O4 S2'
_chemical_formula_weight         478.51
_chemical_melting_point          ?
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   9.7447(15)
_cell_length_b                   10.720(2)
_cell_length_c                   21.453(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.948(10)
_cell_angle_gamma                90.00
_cell_volume                     2192.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    84
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      12.61
_cell_measurement_theta_min      2.50
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
?
;
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12561
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_reflns_number_gt                2952
_reflns_number_total             3684
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         3684
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0655
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+6.5972P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1721
_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.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.26324(10) 0.08746(9) 0.34984(4) 0.0296(3) Uani 1 1 d U . .
S2 S 0.29048(10) 0.34742(10) 0.34697(5) 0.0313(3) Uani 1 1 d U . .
N1 N 0.2104(3) 0.2238(3) 0.35640(15) 0.0292(7) Uani 1 1 d . A .
N14 N 0.2288(3) 0.7205(3) 0.21236(14) 0.0265(7) Uani 1 1 d . . .
C15 C 0.1264(4) 0.7213(4) 0.25558(19) 0.0321(9) Uani 1 1 d . . .
H15B H 0.0370 0.7563 0.2329 0.048 Uiso 1 1 calc R . .
H15C H 0.1635 0.7723 0.2932 0.048 Uiso 1 1 calc R . .
H15A H 0.1116 0.6357 0.2689 0.048 Uiso 1 1 calc R . .
C16 C 0.2445(4) 0.8514(4) 0.18831(18) 0.0305(9) Uani 1 1 d . . .
H16A H 0.2491 0.9101 0.2243 0.037 Uiso 1 1 calc R . .
H16B H 0.3351 0.8567 0.1744 0.037 Uiso 1 1 calc R . .
C17 C 0.3693(4) 0.6720(4) 0.24783(17) 0.0281(8) Uani 1 1 d . . .
H17A H 0.3550 0.5884 0.2650 0.034 Uiso 1 1 calc R . .
H17B H 0.4312 0.6617 0.2169 0.034 Uiso 1 1 calc R . .
C18 C 0.4442(4) 0.7525(4) 0.30200(18) 0.0337(9) Uani 1 1 d . . .
H18A H 0.3882 0.7564 0.3355 0.040 Uiso 1 1 calc R . .
H18B H 0.4532 0.8383 0.2863 0.040 Uiso 1 1 calc R . .
C19 C 0.9190(5) 0.7519(5) 0.3657(2) 0.0498(12) Uani 1 1 d . . .
H19A H 0.8840 0.6999 0.3282 0.075 Uiso 1 1 calc R . .
H19C H 1.0121 0.7226 0.3871 0.075 Uiso 1 1 calc R . .
H19B H 0.9253 0.8388 0.3524 0.075 Uiso 1 1 calc R . .
C20 C 0.5894(4) 0.7011(4) 0.33034(18) 0.0341(9) Uani 1 1 d . . .
H20A H 0.5798 0.6169 0.3480 0.041 Uiso 1 1 calc R . .
H20B H 0.6433 0.6928 0.2962 0.041 Uiso 1 1 calc R . .
C21 C 0.2351(4) 0.6432(4) 0.09943(19) 0.0386(10) Uani 1 1 d . . .
H21A H 0.2386 0.5600 0.0798 0.046 Uiso 1 1 calc R . .
H21B H 0.3326 0.6740 0.1124 0.046 Uiso 1 1 calc R . .
C22 C 0.1297(4) 0.8943(4) 0.1340(2) 0.0373(10) Uani 1 1 d . . .
H22B H 0.1159 0.9852 0.1381 0.045 Uiso 1 1 calc R . .
H22A H 0.0410 0.8523 0.1374 0.045 Uiso 1 1 calc R . .
C23 C 0.1728(4) 0.6300(4) 0.15814(19) 0.0344(9) Uani 1 1 d . . .
H23A H 0.1900 0.5438 0.1745 0.041 Uiso 1 1 calc R . .
H23B H 0.0700 0.6412 0.1454 0.041 Uiso 1 1 calc R . .
C24 C 0.1526(5) 0.7320(5) 0.0497(2) 0.0475(12) Uani 1 1 d . . .
H24B H 0.1876 0.7229 0.0098 0.057 Uiso 1 1 calc R . .
H24A H 0.0529 0.7061 0.0405 0.057 Uiso 1 1 calc R . .
C25 C 0.8188(4) 0.7432(5) 0.4114(2) 0.0452(12) Uani 1 1 d . . .
H25B H 0.8554 0.7956 0.4492 0.054 Uiso 1 1 calc R . .
H25A H 0.8168 0.6558 0.4261 0.054 Uiso 1 1 calc R . .
C26 C 0.6691(4) 0.7842(5) 0.3824(2) 0.0460(11) Uani 1 1 d . . .
H26A H 0.6158 0.7890 0.4169 0.055 Uiso 1 1 calc R . .
H26B H 0.6725 0.8693 0.3649 0.055 Uiso 1 1 calc R . .
C27 C 0.1603(5) 0.8676(5) 0.0683(2) 0.0455(12) Uani 1 1 d . . .
H27A H 0.0926 0.9148 0.0361 0.055 Uiso 1 1 calc R . .
H27B H 0.2553 0.8991 0.0673 0.055 Uiso 1 1 calc R . .
C13A C 0.383(2) 0.3926(15) 0.4307(9) 0.045(3) Uani 0.449(12) 1 d PU A 1
F6A F 0.4362(15) 0.5054(13) 0.4290(7) 0.075(4) Uani 0.449(12) 1 d PU A 1
F10A F 0.2879(14) 0.3965(9) 0.4687(5) 0.069(3) Uani 0.449(12) 1 d PU A 1
F8A F 0.4783(9) 0.3111(10) 0.4544(4) 0.062(3) Uani 0.449(12) 1 d PU A 1
C11A C 0.327(2) 0.0418(19) 0.4330(11) 0.056(4) Uani 0.449(12) 1 d PU A 1
F12A F 0.2279(17) 0.0595(9) 0.4664(5) 0.083(4) Uani 0.449(12) 1 d PU A 1
F4A F 0.2966(12) -0.0980(15) 0.4260(10) 0.048(3) Uani 0.449(12) 1 d PU A 1
F7A F 0.4393(14) 0.1047(8) 0.4588(5) 0.079(4) Uani 0.449(12) 1 d PU A 1
O2A O 0.4101(19) 0.082(2) 0.3443(9) 0.039(3) Uani 0.449(12) 1 d PU A 1
O3A O 0.402(2) 0.337(3) 0.3149(8) 0.033(3) Uani 0.449(12) 1 d PU A 1
O5A O 0.1685(15) 0.0168(18) 0.3090(7) 0.038(3) Uani 0.449(12) 1 d PU A 1
O9A O 0.1912(18) 0.4260(15) 0.3023(5) 0.039(3) Uani 0.449(12) 1 d PU A 1
C13B C 0.3137(15) 0.4221(12) 0.4234(7) 0.049(3) Uani 0.551(12) 1 d PU A 2
F6B F 0.3697(10) 0.5315(10) 0.4197(6) 0.069(3) Uani 0.551(12) 1 d PU A 2
F10B F 0.1947(10) 0.4342(8) 0.4416(4) 0.077(3) Uani 0.551(12) 1 d PU A 2
F8B F 0.3979(14) 0.3566(9) 0.4667(4) 0.085(4) Uani 0.551(12) 1 d PU A 2
C11B C 0.2673(13) 0.0211(13) 0.4281(6) 0.036(3) Uani 0.551(12) 1 d PU A 2
F12B F 0.1373(8) 0.0252(6) 0.4404(4) 0.052(2) Uani 0.551(12) 1 d PU A 2
F4B F 0.3516(13) -0.0828(13) 0.4349(8) 0.063(3) Uani 0.551(12) 1 d PU A 2
F7B F 0.3509(10) 0.0814(7) 0.4733(3) 0.057(2) Uani 0.551(12) 1 d PU A 2
O2B O 0.3815(17) 0.0652(19) 0.3239(8) 0.042(3) Uani 0.551(12) 1 d PU A 2
O3B O 0.4276(19) 0.335(2) 0.3345(8) 0.046(4) Uani 0.551(12) 1 d PU A 2
O5B O 0.1381(12) 0.0143(14) 0.3250(8) 0.057(4) Uani 0.551(12) 1 d PU A 2
O9B O 0.1938(14) 0.4420(13) 0.3292(6) 0.055(3) Uani 0.551(12) 1 d PU A 2

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 0.0294(5) 0.0308(6) 0.0313(5) -0.0015(4) 0.0125(4) 0.0013(4)
S2 0.0273(5) 0.0310(6) 0.0384(5) 0.0014(4) 0.0134(4) -0.0026(4)
N1 0.0227(15) 0.0301(19) 0.0373(17) -0.0019(15) 0.0116(13) -0.0034(13)
N14 0.0214(15) 0.0306(18) 0.0297(16) 0.0018(14) 0.0104(12) -0.0003(13)
C15 0.0254(19) 0.037(2) 0.037(2) 0.0010(19) 0.0145(16) 0.0003(17)
C16 0.0262(19) 0.030(2) 0.038(2) -0.0008(17) 0.0134(16) -0.0019(16)
C17 0.0223(18) 0.030(2) 0.033(2) 0.0015(17) 0.0080(15) 0.0031(15)
C18 0.028(2) 0.042(3) 0.032(2) -0.0061(18) 0.0083(16) 0.0024(17)
C19 0.034(2) 0.056(3) 0.059(3) 0.002(2) 0.010(2) -0.001(2)
C20 0.028(2) 0.043(3) 0.033(2) -0.0003(18) 0.0085(16) 0.0019(17)
C21 0.039(2) 0.039(3) 0.037(2) -0.0062(19) 0.0059(18) 0.0040(19)
C22 0.033(2) 0.032(2) 0.049(2) 0.006(2) 0.0127(19) 0.0044(17)
C23 0.029(2) 0.036(2) 0.038(2) -0.0045(18) 0.0061(17) -0.0020(17)
C24 0.039(2) 0.067(3) 0.034(2) -0.001(2) 0.0033(19) 0.004(2)
C25 0.030(2) 0.065(3) 0.038(2) -0.017(2) 0.0018(18) 0.006(2)
C26 0.036(2) 0.060(3) 0.039(2) -0.013(2) 0.0019(18) 0.008(2)
C27 0.040(2) 0.055(3) 0.043(2) 0.017(2) 0.0119(19) 0.011(2)
C13A 0.071(10) 0.040(7) 0.037(8) -0.006(5) 0.038(8) -0.017(6)
F6A 0.104(10) 0.060(6) 0.067(6) -0.028(5) 0.033(7) -0.055(6)
F10A 0.085(8) 0.081(6) 0.057(5) -0.021(5) 0.051(6) -0.027(6)
F8A 0.048(5) 0.087(6) 0.044(4) -0.002(4) -0.007(3) -0.017(4)
C11A 0.078(11) 0.035(8) 0.062(10) 0.001(7) 0.030(9) -0.003(8)
F12A 0.149(12) 0.057(6) 0.062(6) 0.018(5) 0.067(9) 0.036(8)
F4A 0.057(6) 0.033(5) 0.060(7) 0.012(4) 0.030(7) 0.014(5)
F7A 0.094(7) 0.059(5) 0.061(5) -0.005(4) -0.034(5) 0.012(5)
O2A 0.028(5) 0.038(9) 0.058(10) -0.012(7) 0.025(6) -0.003(5)
O3A 0.034(8) 0.039(6) 0.031(6) -0.006(6) 0.020(5) -0.013(6)
O5A 0.032(7) 0.045(5) 0.040(5) -0.015(4) 0.016(4) 0.003(5)
O9A 0.052(5) 0.023(5) 0.040(6) 0.007(5) 0.002(5) -0.004(3)
C13B 0.047(6) 0.042(6) 0.058(7) -0.018(5) 0.013(5) -0.019(5)
F6B 0.070(6) 0.051(5) 0.091(6) -0.022(4) 0.029(6) -0.034(4)
F10B 0.074(5) 0.091(5) 0.082(5) -0.056(4) 0.050(4) -0.036(4)
F8B 0.112(8) 0.079(6) 0.050(5) -0.001(4) -0.021(6) -0.026(6)
C11B 0.048(6) 0.030(6) 0.035(5) 0.001(4) 0.022(5) 0.004(5)
F12B 0.064(4) 0.046(4) 0.060(4) 0.012(3) 0.041(3) 0.010(3)
F4B 0.095(8) 0.039(5) 0.056(5) 0.018(4) 0.021(7) 0.034(6)
F7B 0.081(6) 0.049(4) 0.035(3) -0.002(3) -0.001(4) 0.007(4)
O2B 0.048(7) 0.025(5) 0.066(9) -0.014(6) 0.040(6) -0.002(5)
O3B 0.025(6) 0.042(5) 0.078(11) -0.014(9) 0.027(7) -0.005(4)
O5B 0.024(4) 0.029(4) 0.121(11) -0.026(7) 0.020(5) -0.005(3)
O9B 0.041(4) 0.039(6) 0.086(8) 0.024(7) 0.016(7) 0.002(3)

_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 N1 1.566(3) . ?
S1 C11A 1.83(2) . ?
S1 O2A 1.462(19) . ?
S1 O5A 1.363(16) . ?
S1 C11B 1.816(14) . ?
S1 O2B 1.400(17) . ?
S1 O5B 1.455(13) . ?
S2 N1 1.572(3) . ?
S2 C13A 1.90(2) . ?
S2 O3A 1.41(2) . ?
S2 O9A 1.477(15) . ?
S2 C13B 1.797(14) . ?
S2 O3B 1.423(19) . ?
S2 O9B 1.383(13) . ?
N14 C15 1.496(4) . ?
N14 C16 1.514(5) . ?
N14 C17 1.514(4) . ?
N14 C23 1.527(5) . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 H15A 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C22 1.511(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.509(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C20 1.523(5) . ?
C19 H19A 0.9800 . ?
C19 H19C 0.9800 . ?
C19 H19B 0.9800 . ?
C19 C25 1.523(6) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C26 1.512(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C23 1.514(6) . ?
C21 C24 1.528(6) . ?
C22 H22B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 C27 1.527(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 C27 1.506(7) . ?
C25 H25B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 C26 1.528(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C13A F6A 1.321(18) . ?
C13A F10A 1.351(16) . ?
C13A F8A 1.30(2) . ?
C11A F12A 1.33(2) . ?
C11A F4A 1.53(3) . ?
C11A F7A 1.31(2) . ?
C13B F6B 1.303(15) . ?
C13B F10B 1.304(15) . ?
C13B F8B 1.308(15) . ?
C11B F12B 1.348(12) . ?
C11B F4B 1.37(2) . ?
C11B F7B 1.302(14) . ?

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
S1 N1 S2 126.41(19) . . ?
N1 S1 C11A 102.3(7) . . ?
N1 S1 C11B 103.1(4) . . ?
N1 S2 C13A 104.1(4) . . ?
N1 S2 C13B 103.3(4) . . ?
N14 C15 H15B 109.5 . . ?
N14 C15 H15C 109.5 . . ?
N14 C15 H15A 109.5 . . ?
N14 C16 H16A 108.4 . . ?
N14 C16 H16B 108.4 . . ?
N14 C17 H17A 108.4 . . ?
N14 C17 H17B 108.4 . . ?
N14 C23 H23A 108.4 . . ?
N14 C23 H23B 108.4 . . ?
C15 N14 C16 109.5(3) . . ?
C15 N14 C17 109.9(3) . . ?
C15 N14 C23 107.2(3) . . ?
H15B C15 H15C 109.5 . . ?
H15B C15 H15A 109.5 . . ?
H15C C15 H15A 109.5 . . ?
C16 N14 C23 112.0(3) . . ?
C16 C22 H22B 108.8 . . ?
C16 C22 H22A 108.8 . . ?
C16 C22 C27 113.6(3) . . ?
H16A C16 H16B 107.4 . . ?
C17 N14 C16 110.2(3) . . ?
C17 N14 C23 107.9(3) . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C17 C18 C20 111.2(3) . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N14 115.7(3) . . ?
C18 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
C18 C20 H20A 109.2 . . ?
C18 C20 H20B 109.2 . . ?
H18A C18 H18B 108.0 . . ?
C19 C25 H25B 108.8 . . ?
C19 C25 H25A 108.8 . . ?
C19 C25 C26 113.9(4) . . ?
H19A C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19C C19 H19B 109.5 . . ?
C20 C18 H18A 109.4 . . ?
C20 C18 H18B 109.4 . . ?
C20 C26 C25 115.6(4) . . ?
C20 C26 H26A 108.4 . . ?
C20 C26 H26B 108.4 . . ?
H20A C20 H20B 107.9 . . ?
C21 C23 N14 115.6(3) . . ?
C21 C23 H23A 108.4 . . ?
C21 C23 H23B 108.4 . . ?
C21 C24 H24B 108.5 . . ?
C21 C24 H24A 108.5 . . ?
H21A C21 H21B 107.7 . . ?
C22 C16 N14 115.7(3) . . ?
C22 C16 H16A 108.4 . . ?
C22 C16 H16B 108.4 . . ?
C22 C27 H27A 108.6 . . ?
C22 C27 H27B 108.6 . . ?
H22B C22 H22A 107.7 . . ?
C23 C21 H21A 108.9 . . ?
C23 C21 H21B 108.9 . . ?
C23 C21 C24 113.3(3) . . ?
H23A C23 H23B 107.4 . . ?
C24 C21 H21A 108.9 . . ?
C24 C21 H21B 108.9 . . ?
C24 C27 C22 114.7(4) . . ?
C24 C27 H27A 108.6 . . ?
C24 C27 H27B 108.6 . . ?
H24B C24 H24A 107.5 . . ?
C25 C19 H19A 109.5 . . ?
C25 C19 H19C 109.5 . . ?
C25 C19 H19B 109.5 . . ?
C25 C26 H26A 108.4 . . ?
C25 C26 H26B 108.4 . . ?
H25B C25 H25A 107.7 . . ?
C26 C20 C18 112.0(3) . . ?
C26 C20 H20A 109.2 . . ?
C26 C20 H20B 109.2 . . ?
C26 C25 H25B 108.8 . . ?
C26 C25 H25A 108.8 . . ?
H26A C26 H26B 107.4 . . ?
C27 C22 H22B 108.8 . . ?
C27 C22 H22A 108.8 . . ?
C27 C24 C21 115.2(4) . . ?
C27 C24 H24B 108.5 . . ?
C27 C24 H24A 108.5 . . ?
H27A C27 H27B 107.6 . . ?
F6A C13A S2 108.6(13) . . ?
F6A C13A F10A 108.2(12) . . ?
F10A C13A S2 109.3(14) . . ?
F8A C13A S2 111.0(9) . . ?
F8A C13A F6A 111.7(16) . . ?
F8A C13A F10A 108.0(15) . . ?
F12A C11A S1 110.4(15) . . ?
F12A C11A F4A 92.5(14) . . ?
F4A C11A S1 98.4(15) . . ?
F7A C11A S1 111.2(13) . . ?
F7A C11A F12A 109.6(19) . . ?
F7A C11A F4A 132.5(19) . . ?
O2A S1 N1 113.0(10) . . ?
O2A S1 C11A 85.9(11) . . ?
O2A S1 C11B 103.0(11) . . ?
O3A S2 N1 116.8(12) . . ?
O3A S2 C13A 102.8(9) . . ?
O3A S2 O9A 101.4(11) . . ?
O3A S2 C13B 121.2(9) . . ?
O3A S2 O3B 17.9(10) . . ?
O5A S1 N1 112.6(8) . . ?
O5A S1 C11A 121.7(10) . . ?
O5A S1 O2A 118.0(8) . . ?
O5A S1 C11B 105.0(8) . . ?
O5A S1 O2B 98.9(7) . . ?
O5A S1 O5B 20.1(7) . . ?
O9A S2 N1 106.8(7) . . ?
O9A S2 C13A 125.9(8) . . ?
O9A S2 C13B 106.3(7) . . ?
C13B S2 C13A 22.5(4) . . ?
F6B C13B S2 108.7(11) . . ?
F6B C13B F10B 109.8(11) . . ?
F6B C13B F8B 108.5(11) . . ?
F10B C13B S2 111.5(8) . . ?
F10B C13B F8B 107.8(13) . . ?
F8B C13B S2 110.5(11) . . ?
C11B S1 C11A 19.3(5) . . ?
F12B C11B S1 109.1(9) . . ?
F12B C11B F4B 124.8(13) . . ?
F4B C11B S1 108.3(10) . . ?
F7B C11B S1 112.7(9) . . ?
F7B C11B F12B 107.8(9) . . ?
F7B C11B F4B 93.1(11) . . ?
O2B S1 N1 120.5(9) . . ?
O2B S1 C11A 101.5(10) . . ?
O2B S1 O2A 20.0(8) . . ?
O2B S1 C11B 116.0(10) . . ?
O2B S1 O5B 117.4(7) . . ?
O3B S2 N1 117.2(10) . . ?
O3B S2 C13A 85.7(8) . . ?
O3B S2 O9A 116.5(10) . . ?
O3B S2 C13B 105.6(8) . . ?
O5B S1 N1 105.6(6) . . ?
O5B S1 C11A 107.6(10) . . ?
O5B S1 O2A 135.1(8) . . ?
O5B S1 C11B 89.0(8) . . ?
O9B S2 N1 109.0(6) . . ?
O9B S2 C13A 103.6(9) . . ?
O9B S2 O3A 118.4(12) . . ?
O9B S2 O9A 23.8(6) . . ?
O9B S2 C13B 82.8(8) . . ?
O9B S2 O3B 129.0(11) . . ?