Electronic Supplementary Information for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Yoichi Habata'
_publ_contact_author_address     
;
Department of Chemistry
Toho University
2-2-1 Miyama
Funabashi
Chiba 274-8510
JAPAN
;

_publ_contact_author_email       HABATA@CHEM.SCI.TOHO-U.AC.JP

_publ_section_title              
;
Synthesis of diazahexathia-24-crown-8 derivatives and
structures of Ag+ complexes
;
loop_
_publ_author_name
'Yoichi Habata'
'Shim Sung Lee'
'Kanae Noto'
'Futoshi Osaka'
'Satoshi Otawa'
'Joobeom Seo'

# Attachment '5b_AgOTf.cif'

data_phetn2s_p21_c
_database_code_depnum_ccdc_archive 'CCDC 284338'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H50 Ag2 F6 N2 O6 S8'
_chemical_formula_weight         1168.98

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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   6.4971(3)
_cell_length_b                   17.1739(9)
_cell_length_c                   19.2924(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.8450(10)
_cell_angle_gamma                90.00
_cell_volume                     2152.42(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1184
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4937
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
SADABS, Sheldrick, 1996
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15693
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         28.31
_reflns_number_total             5327
_reflns_number_gt                4345
_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^)+(0.0342P)^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         5327
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0667
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.002
_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
C8 C 0.5772(3) -0.22670(14) 0.06792(11) 0.0147(5) Uani 1 1 d . . .
H8A H 0.6755 -0.2239 0.1076 0.018 Uiso 1 1 calc R . .
H8B H 0.5057 -0.2775 0.0706 0.018 Uiso 1 1 calc R . .
C7 C 0.4187(3) -0.16219(13) 0.07582(12) 0.0145(4) Uani 1 1 d . . .
H7A H 0.3480 -0.1697 0.1204 0.017 Uiso 1 1 calc R . .
H7B H 0.3140 -0.1678 0.0383 0.017 Uiso 1 1 calc R . .
S3 S 0.51905(9) -0.06376(3) 0.07343(3) 0.01259(11) Uani 1 1 d . . .
C6 C 0.7008(4) -0.06047(14) 0.14656(11) 0.0147(5) Uani 1 1 d . . .
H6A H 0.6552 -0.0208 0.1803 0.018 Uiso 1 1 calc R . .
H6B H 0.7027 -0.1116 0.1702 0.018 Uiso 1 1 calc R . .
Ag1 Ag 1.27828(3) 0.079652(10) 0.034076(8) 0.01435(6) Uani 1 1 d . . .
S1 S 1.38580(8) 0.14187(3) 0.14921(3) 0.01361(12) Uani 1 1 d . . .
S2 S 0.92816(8) 0.05584(3) 0.08325(3) 0.01289(11) Uani 1 1 d . . .
N1 N 1.3049(3) 0.22433(11) -0.00301(9) 0.0120(4) Uani 1 1 d . . .
C12 C 0.7689(4) 0.42361(14) -0.05075(12) 0.0174(5) Uani 1 1 d . . .
H12 H 0.7978 0.4465 -0.0069 0.021 Uiso 1 1 calc R . .
C5 C 0.9176(3) -0.04067(13) 0.12263(11) 0.0134(4) Uani 1 1 d . . .
H5A H 0.9624 -0.0800 0.0885 0.016 Uiso 1 1 calc R . .
H5B H 1.0139 -0.0427 0.1628 0.016 Uiso 1 1 calc R . .
C2 C 1.3363(4) 0.24324(13) 0.12597(11) 0.0140(4) Uani 1 1 d . . .
H2A H 1.1863 0.2532 0.1261 0.017 Uiso 1 1 calc R . .
H2B H 1.4021 0.2779 0.1608 0.017 Uiso 1 1 calc R . .
C4 C 0.9523(4) 0.11707(14) 0.15985(12) 0.0164(5) Uani 1 1 d . . .
H4A H 0.9236 0.1715 0.1459 0.020 Uiso 1 1 calc R . .
H4B H 0.8446 0.1014 0.1928 0.020 Uiso 1 1 calc R . .
C15 C 0.6766(4) 0.35553(15) -0.17732(12) 0.0205(5) Uani 1 1 d . . .
H15 H 0.6437 0.3312 -0.2203 0.025 Uiso 1 1 calc R . .
C9 C 1.0993(3) 0.25919(13) -0.01479(12) 0.0148(5) Uani 1 1 d . . .
H9A H 1.0215 0.2554 0.0288 0.018 Uiso 1 1 calc R . .
H9B H 1.0251 0.2277 -0.0501 0.018 Uiso 1 1 calc R . .
C11 C 0.9000(3) 0.36726(13) -0.07644(11) 0.0134(4) Uani 1 1 d . . .
C14 C 0.5495(4) 0.41331(15) -0.15195(13) 0.0215(5) Uani 1 1 d . . .
H14 H 0.4319 0.4296 -0.1779 0.026 Uiso 1 1 calc R . .
C1 C 1.4206(3) 0.26168(13) 0.05441(11) 0.0140(4) Uani 1 1 d . . .
H1A H 1.4181 0.3188 0.0475 0.017 Uiso 1 1 calc R . .
H1B H 1.5659 0.2446 0.0528 0.017 Uiso 1 1 calc R . .
C16 C 0.8518(4) 0.33277(14) -0.14046(11) 0.0163(5) Uani 1 1 d . . .
H16 H 0.9392 0.2937 -0.1587 0.020 Uiso 1 1 calc R . .
C3 C 1.1603(4) 0.11514(15) 0.19801(11) 0.0184(5) Uani 1 1 d . . .
H3A H 1.1816 0.0618 0.2162 0.022 Uiso 1 1 calc R . .
H3B H 1.1520 0.1504 0.2385 0.022 Uiso 1 1 calc R . .
C13 C 0.5952(4) 0.44709(15) -0.08845(13) 0.0200(5) Uani 1 1 d . . .
H13 H 0.5079 0.4864 -0.0705 0.024 Uiso 1 1 calc R . .
C10 C 1.0969(4) 0.34468(14) -0.03858(12) 0.0167(5) Uani 1 1 d . . .
H10A H 1.1152 0.3787 0.0024 0.020 Uiso 1 1 calc R . .
H10B H 1.2148 0.3537 -0.0695 0.020 Uiso 1 1 calc R . .
S4 S 0.13526(9) 0.84774(4) 0.28165(3) 0.01671(12) Uani 1 1 d . . .
F2 F -0.0630(2) 0.98140(8) 0.28738(7) 0.0243(3) Uani 1 1 d . . .
F3 F -0.1363(2) 0.90182(9) 0.36905(8) 0.0266(3) Uani 1 1 d . . .
F1 F 0.1520(3) 0.96282(10) 0.37130(8) 0.0324(4) Uani 1 1 d . . .
O1 O -0.0327(3) 0.81695(10) 0.24045(9) 0.0230(4) Uani 1 1 d . . .
C17 C 0.0155(4) 0.92714(14) 0.32991(12) 0.0163(5) Uani 1 1 d . . .
O3 O 0.2921(3) 0.88681(12) 0.24289(10) 0.0286(4) Uani 1 1 d . . .
O2 O 0.2072(3) 0.79704(11) 0.33658(9) 0.0253(4) 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
C8 0.0158(11) 0.0133(12) 0.0149(10) 0.0022(9) 0.0026(9) 0.0008(9)
C7 0.0135(11) 0.0140(12) 0.0161(11) 0.0005(9) 0.0001(9) -0.0034(9)
S3 0.0134(3) 0.0122(3) 0.0122(2) 0.0014(2) 0.0001(2) 0.0004(2)
C6 0.0175(11) 0.0162(12) 0.0104(10) 0.0016(8) -0.0003(8) -0.0024(9)
Ag1 0.01599(9) 0.01568(10) 0.01144(8) -0.00100(6) 0.00219(6) -0.00281(7)
S1 0.0130(3) 0.0155(3) 0.0123(3) -0.0004(2) -0.0015(2) -0.0002(2)
S2 0.0125(3) 0.0139(3) 0.0122(2) 0.0014(2) 0.0000(2) -0.0009(2)
N1 0.0118(9) 0.0113(9) 0.0129(9) -0.0007(7) 0.0002(7) 0.0002(7)
C12 0.0177(12) 0.0167(12) 0.0178(11) -0.0001(9) -0.0002(9) -0.0001(9)
C5 0.0159(11) 0.0119(11) 0.0124(10) 0.0020(8) -0.0019(8) 0.0011(9)
C2 0.0163(11) 0.0118(11) 0.0139(10) -0.0017(9) -0.0004(9) 0.0005(8)
C4 0.0152(11) 0.0167(12) 0.0175(11) -0.0036(9) 0.0052(9) -0.0019(9)
C15 0.0233(13) 0.0254(14) 0.0128(11) 0.0041(10) -0.0013(9) -0.0099(10)
C9 0.0138(11) 0.0140(12) 0.0165(11) 0.0002(9) -0.0003(9) 0.0007(8)
C11 0.0142(11) 0.0129(11) 0.0132(10) 0.0037(9) 0.0006(8) -0.0022(8)
C14 0.0165(12) 0.0254(14) 0.0224(12) 0.0126(10) -0.0057(10) -0.0043(10)
C1 0.0124(10) 0.0117(11) 0.0178(11) 0.0004(9) -0.0011(9) -0.0019(8)
C16 0.0190(12) 0.0158(12) 0.0144(11) 0.0013(9) 0.0019(9) -0.0028(9)
C3 0.0215(12) 0.0214(13) 0.0123(11) -0.0012(9) 0.0028(9) -0.0051(10)
C13 0.0165(12) 0.0171(13) 0.0266(13) 0.0041(10) 0.0023(10) 0.0040(9)
C10 0.0161(11) 0.0147(12) 0.0192(11) -0.0009(9) -0.0035(9) 0.0007(9)
S4 0.0169(3) 0.0163(3) 0.0170(3) 0.0006(2) 0.0011(2) 0.0021(2)
F2 0.0371(9) 0.0173(8) 0.0185(7) 0.0044(6) 0.0030(6) 0.0076(6)
F3 0.0344(9) 0.0190(8) 0.0269(8) 0.0002(6) 0.0162(7) -0.0027(6)
F1 0.0384(9) 0.0312(10) 0.0274(8) -0.0099(7) -0.0092(7) -0.0074(7)
O1 0.0276(10) 0.0205(10) 0.0207(9) -0.0065(7) -0.0062(8) 0.0032(7)
C17 0.0210(12) 0.0150(12) 0.0129(10) 0.0008(9) 0.0005(9) -0.0030(9)
O3 0.0249(10) 0.0297(11) 0.0315(10) 0.0023(8) 0.0128(8) -0.0007(8)
O2 0.0255(10) 0.0229(10) 0.0273(10) 0.0061(8) -0.0058(8) 0.0040(7)

_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
C8 N1 1.478(3) 3_755 ?
C8 C7 1.522(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 S3 1.813(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
S3 C6 1.827(2) . ?
S3 Ag1 2.4881(6) 3_755 ?
C6 C5 1.527(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
Ag1 S3 2.4881(6) 3_755 ?
Ag1 S2 2.5112(6) . ?
Ag1 S1 2.5530(6) . ?
Ag1 N1 2.5921(19) . ?
S1 C3 1.812(2) . ?
S1 C2 1.825(2) . ?
S2 C4 1.819(2) . ?
S2 C5 1.825(2) . ?
N1 C1 1.476(3) . ?
N1 C8 1.478(3) 3_755 ?
N1 C9 1.479(3) . ?
C12 C11 1.386(3) . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C2 C1 1.526(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C4 C3 1.530(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C15 C14 1.385(4) . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C9 C10 1.538(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C16 1.401(3) . ?
C11 C10 1.514(3) . ?
C14 C13 1.384(4) . ?
C14 H14 0.9500 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C16 H16 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C13 H13 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
S4 O3 1.4388(18) . ?
S4 O1 1.4410(18) . ?
S4 O2 1.4439(18) . ?
S4 C17 1.831(2) . ?
F2 C17 1.338(3) . ?
F3 C17 1.324(3) . ?
F1 C17 1.334(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
N1 C8 C7 115.13(18) 3_755 . ?
N1 C8 H8A 108.5 3_755 . ?
C7 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 3_755 . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C7 S3 115.59(16) . . ?
C8 C7 H7A 108.4 . . ?
S3 C7 H7A 108.4 . . ?
C8 C7 H7B 108.4 . . ?
S3 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
C7 S3 C6 103.76(11) . . ?
C7 S3 Ag1 96.54(7) . 3_755 ?
C6 S3 Ag1 107.64(8) . 3_755 ?
C5 C6 S3 111.22(15) . . ?
C5 C6 H6A 109.4 . . ?
S3 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
S3 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
S3 Ag1 S2 142.241(19) 3_755 . ?
S3 Ag1 S1 129.035(19) 3_755 . ?
S2 Ag1 S1 88.695(18) . . ?
S3 Ag1 N1 80.60(4) 3_755 . ?
S2 Ag1 N1 108.96(4) . . ?
S1 Ag1 N1 79.66(4) . . ?
C3 S1 C2 103.21(11) . . ?
C3 S1 Ag1 97.64(8) . . ?
C2 S1 Ag1 98.08(7) . . ?
C4 S2 C5 100.97(11) . . ?
C4 S2 Ag1 98.35(8) . . ?
C5 S2 Ag1 110.19(7) . . ?
C1 N1 C8 111.08(17) . 3_755 ?
C1 N1 C9 112.84(17) . . ?
C8 N1 C9 109.69(17) 3_755 . ?
C1 N1 Ag1 104.16(13) . . ?
C8 N1 Ag1 107.33(13) 3_755 . ?
C9 N1 Ag1 111.51(13) . . ?
C11 C12 C13 120.9(2) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C6 C5 S2 111.64(16) . . ?
C6 C5 H5A 109.3 . . ?
S2 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
S2 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C1 C2 S1 110.86(15) . . ?
C1 C2 H2A 109.5 . . ?
S1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
S1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C3 C4 S2 116.32(16) . . ?
C3 C4 H4A 108.2 . . ?
S2 C4 H4A 108.2 . . ?
C3 C4 H4B 108.2 . . ?
S2 C4 H4B 108.2 . . ?
H4A C4 H4B 107.4 . . ?
C14 C15 C16 120.6(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
N1 C9 C10 115.93(19) . . ?
N1 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N1 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C12 C11 C16 118.7(2) . . ?
C12 C11 C10 121.7(2) . . ?
C16 C11 C10 119.6(2) . . ?
C13 C14 C15 119.5(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N1 C1 C2 113.80(18) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C15 C16 C11 120.2(2) . . ?
C15 C16 H16 119.9 . . ?
C11 C16 H16 119.9 . . ?
C4 C3 S1 117.37(16) . . ?
C4 C3 H3A 108.0 . . ?
S1 C3 H3A 108.0 . . ?
C4 C3 H3B 108.0 . . ?
S1 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C11 C10 C9 113.13(19) . . ?
C11 C10 H10A 109.0 . . ?
C9 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
C9 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O3 S4 O1 114.89(11) . . ?
O3 S4 O2 116.02(12) . . ?
O1 S4 O2 114.69(11) . . ?
O3 S4 C17 103.09(11) . . ?
O1 S4 C17 103.28(11) . . ?
O2 S4 C17 102.19(11) . . ?
F3 C17 F1 107.68(18) . . ?
F3 C17 F2 107.4(2) . . ?
F1 C17 F2 106.9(2) . . ?
F3 C17 S4 111.78(16) . . ?
F1 C17 S4 111.27(17) . . ?
F2 C17 S4 111.59(15) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.098


# Attachment '5a_AgOTf.cif'

data_h:\dalton_s_paper\n2s6bzcl2ag\work\n2s6bzclagot_p_1
_database_code_depnum_ccdc_archive 'CCDC 284339'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H42 Ag2 Cl4 F6 N2 O6 S8'
_chemical_formula_weight         1278.70

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.4064(5)
_cell_length_b                   10.4171(6)
_cell_length_c                   13.9910(8)
_cell_angle_alpha                70.3250(10)
_cell_angle_beta                 81.8880(10)
_cell_angle_gamma                79.2430(10)
_cell_volume                     1129.33(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             640
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_T_max  0.6589
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1996'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8419
_diffrn_reflns_av_R_equivalents  0.0118
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         28.28
_reflns_number_total             5518
_reflns_number_gt                5203
_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^)+(0.0341P)^2^+0.3947P] 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         5518
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0216
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0574
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.12208(19) 0.76336(16) -0.36307(11) 0.0145(3) Uani 1 1 d . . .
H1A H 0.1284 0.8289 -0.4332 0.017 Uiso 1 1 calc R . .
H1B H 0.0941 0.6771 -0.3670 0.017 Uiso 1 1 calc R . .
Ag1 Ag -0.051812(14) 0.292792(11) 0.115702(9) 0.01637(5) Uani 1 1 d . . .
C8 C -0.00434(19) 0.03329(15) 0.31669(12) 0.0145(3) Uani 1 1 d . . .
H8A H -0.1194 0.0281 0.3125 0.017 Uiso 1 1 calc R . .
H8B H 0.0244 -0.0236 0.3862 0.017 Uiso 1 1 calc R . .
C7 C 0.1008(2) -0.02941(16) 0.24060(12) 0.0158(3) Uani 1 1 d . . .
H7A H 0.1001 -0.1302 0.2649 0.019 Uiso 1 1 calc R . .
H7B H 0.2142 -0.0138 0.2378 0.019 Uiso 1 1 calc R . .
C6 C 0.22065(19) 0.05982(16) 0.03102(12) 0.0164(3) Uani 1 1 d . . .
H6A H 0.2961 -0.0274 0.0551 0.020 Uiso 1 1 calc R . .
H6B H 0.1968 0.0696 -0.0386 0.020 Uiso 1 1 calc R . .
C5 C 0.30960(19) 0.17800(16) 0.02362(12) 0.0156(3) Uani 1 1 d . . .
H5A H 0.4028 0.1797 -0.0285 0.019 Uiso 1 1 calc R . .
H5B H 0.3542 0.1584 0.0897 0.019 Uiso 1 1 calc R . .
C4 C 0.1428(2) 0.38072(17) -0.13829(12) 0.0165(3) Uani 1 1 d . . .
H4A H 0.1361 0.2922 -0.1482 0.020 Uiso 1 1 calc R . .
H4B H 0.0359 0.4398 -0.1502 0.020 Uiso 1 1 calc R . .
C3 C 0.2722(2) 0.45101(16) -0.21443(12) 0.0177(3) Uani 1 1 d . . .
H3A H 0.2400 0.4732 -0.2842 0.021 Uiso 1 1 calc R . .
H3B H 0.3758 0.3867 -0.2082 0.021 Uiso 1 1 calc R . .
C2 C 0.28968(19) 0.73149(16) -0.32296(12) 0.0156(3) Uani 1 1 d . . .
H2A H 0.3213 0.8188 -0.3239 0.019 Uiso 1 1 calc R . .
H2B H 0.3692 0.6946 -0.3701 0.019 Uiso 1 1 calc R . .
C9 C 0.16907(19) 0.18283(16) 0.33579(12) 0.0158(3) Uani 1 1 d . . .
H9A H 0.2571 0.1320 0.3017 0.019 Uiso 1 1 calc R . .
H9B H 0.1691 0.1351 0.4101 0.019 Uiso 1 1 calc R . .
C10 C 0.20493(18) 0.32778(16) 0.31296(12) 0.0148(3) Uani 1 1 d . . .
C11 C 0.25793(19) 0.40191(17) 0.21443(13) 0.0166(3) Uani 1 1 d . . .
H11 H 0.2735 0.3612 0.1618 0.020 Uiso 1 1 calc R . .
C12 C 0.28801(19) 0.53571(17) 0.19342(13) 0.0171(3) Uani 1 1 d . . .
C13 C 0.27304(19) 0.59689(17) 0.26862(14) 0.0189(3) Uani 1 1 d . . .
H13 H 0.2962 0.6878 0.2537 0.023 Uiso 1 1 calc R . .
C14 C 0.2228(2) 0.52004(18) 0.36660(14) 0.0196(3) Uani 1 1 d . . .
C15 C 0.1877(2) 0.38718(17) 0.39005(13) 0.0179(3) Uani 1 1 d . . .
H15 H 0.1525 0.3375 0.4578 0.022 Uiso 1 1 calc R . .
C16 C 0.5378(2) 0.84428(18) 0.39005(13) 0.0209(3) Uani 1 1 d . . .
Cl1 Cl 0.34593(5) 0.62975(5) 0.06873(3) 0.02488(9) Uani 1 1 d . . .
Cl2 Cl 0.20071(6) 0.59433(5) 0.46260(4) 0.03065(11) Uani 1 1 d . . .
F1 F 0.61838(15) 0.89280(13) 0.44344(9) 0.0316(3) Uani 1 1 d . . .
F2 F 0.57194(14) 0.70710(11) 0.42280(9) 0.0304(2) Uani 1 1 d . . .
F3 F 0.37904(13) 0.87810(12) 0.41340(8) 0.0275(2) Uani 1 1 d . . .
N1 N 0.01059(15) 0.17801(13) 0.30207(10) 0.0127(2) Uani 1 1 d . . .
O1 O 0.49520(14) 0.85580(13) 0.20757(10) 0.0204(2) Uani 1 1 d . . .
O2 O 0.54919(16) 1.06220(13) 0.23420(10) 0.0240(3) Uani 1 1 d . . .
O3 O 0.76509(15) 0.86639(14) 0.24577(10) 0.0249(3) Uani 1 1 d . . .
S3 S 0.03226(5) 0.04249(4) 0.11251(3) 0.01440(8) Uani 1 1 d . . .
S2 S 0.18892(5) 0.34862(4) -0.00833(3) 0.01484(8) Uani 1 1 d . . .
S1 S 0.30367(5) 0.60953(4) -0.19527(3) 0.01505(8) Uani 1 1 d . . .
S4 S 0.59348(5) 0.91548(4) 0.25349(3) 0.01548(8) 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
C1 0.0162(7) 0.0161(7) 0.0113(7) -0.0053(6) 0.0002(5) -0.0018(6)
Ag1 0.01836(7) 0.01462(7) 0.01394(7) -0.00493(5) 0.00292(4) 0.00037(4)
C8 0.0171(7) 0.0125(7) 0.0144(7) -0.0047(5) 0.0002(6) -0.0040(5)
C7 0.0178(7) 0.0147(7) 0.0141(7) -0.0043(6) -0.0021(6) -0.0005(6)
C6 0.0179(7) 0.0163(7) 0.0155(7) -0.0075(6) 0.0022(6) -0.0022(6)
C5 0.0151(7) 0.0158(7) 0.0161(7) -0.0058(6) -0.0006(6) -0.0018(6)
C4 0.0168(7) 0.0169(7) 0.0162(7) -0.0062(6) -0.0035(6) -0.0002(6)
C3 0.0232(8) 0.0140(7) 0.0149(7) -0.0063(6) 0.0014(6) 0.0005(6)
C2 0.0159(7) 0.0161(7) 0.0134(7) -0.0033(6) 0.0013(5) -0.0033(6)
C9 0.0158(7) 0.0149(7) 0.0179(7) -0.0059(6) -0.0048(6) -0.0014(6)
C10 0.0121(7) 0.0136(7) 0.0199(8) -0.0070(6) -0.0034(6) -0.0002(5)
C11 0.0145(7) 0.0189(8) 0.0192(8) -0.0090(6) -0.0027(6) -0.0029(6)
C12 0.0130(7) 0.0194(8) 0.0182(8) -0.0048(6) -0.0017(6) -0.0032(6)
C13 0.0148(7) 0.0157(7) 0.0281(9) -0.0097(6) -0.0007(6) -0.0026(6)
C14 0.0170(7) 0.0216(8) 0.0253(8) -0.0151(7) 0.0011(6) -0.0031(6)
C15 0.0164(7) 0.0199(8) 0.0195(8) -0.0091(6) 0.0001(6) -0.0037(6)
C16 0.0213(8) 0.0206(8) 0.0192(8) -0.0050(6) -0.0016(6) -0.0019(6)
Cl1 0.0285(2) 0.0256(2) 0.0205(2) -0.00295(16) -0.00245(16) -0.01198(17)
Cl2 0.0378(3) 0.0328(2) 0.0323(2) -0.0246(2) 0.00787(19) -0.01331(19)
F1 0.0386(7) 0.0395(7) 0.0213(5) -0.0121(5) -0.0084(5) -0.0081(5)
F2 0.0335(6) 0.0200(5) 0.0301(6) 0.0011(4) -0.0053(5) -0.0007(4)
F3 0.0221(5) 0.0306(6) 0.0234(5) -0.0049(4) 0.0065(4) -0.0011(4)
N1 0.0130(6) 0.0119(6) 0.0142(6) -0.0054(5) -0.0013(5) -0.0016(5)
O1 0.0181(6) 0.0238(6) 0.0231(6) -0.0114(5) -0.0027(5) -0.0044(5)
O2 0.0333(7) 0.0165(6) 0.0225(6) -0.0063(5) -0.0016(5) -0.0050(5)
O3 0.0151(6) 0.0337(7) 0.0315(7) -0.0183(6) 0.0024(5) -0.0057(5)
S3 0.01547(18) 0.01513(17) 0.01411(18) -0.00625(14) -0.00017(13) -0.00378(13)
S2 0.01781(18) 0.01444(17) 0.01270(17) -0.00515(14) 0.00084(13) -0.00350(14)
S1 0.01450(18) 0.01613(18) 0.01399(18) -0.00560(14) -0.00080(13) 0.00022(14)
S4 0.01531(18) 0.01695(18) 0.01619(18) -0.00784(14) 0.00093(14) -0.00420(14)

_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 N1 1.4742(19) 2_565 ?
C1 C2 1.527(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
Ag1 S1 2.4598(4) 2_565 ?
Ag1 S2 2.4927(4) . ?
Ag1 N1 2.5605(13) . ?
Ag1 S3 2.5849(4) . ?
C8 N1 1.4786(19) . ?
C8 C7 1.526(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C7 S3 1.8251(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C6 C5 1.524(2) . ?
C6 S3 1.8164(16) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 S2 1.8188(16) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 C3 1.516(2) . ?
C4 S2 1.8193(16) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C3 S1 1.8303(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 S1 1.8152(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C9 N1 1.4894(19) . ?
C9 C10 1.514(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.390(2) . ?
C10 C15 1.393(2) . ?
C11 C12 1.388(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(2) . ?
C12 Cl1 1.7401(17) . ?
C13 C14 1.387(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(2) . ?
C14 Cl2 1.7358(17) . ?
C15 H15 0.9500 . ?
C16 F2 1.333(2) . ?
C16 F3 1.338(2) . ?
C16 F1 1.341(2) . ?
C16 S4 1.8283(18) . ?
N1 C1 1.4742(19) 2_565 ?
O1 S4 1.4465(12) . ?
O2 S4 1.4442(13) . ?
O3 S4 1.4395(13) . ?
S1 Ag1 2.4598(4) 2_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
N1 C1 C2 115.35(13) 2_565 . ?
N1 C1 H1A 108.4 2_565 . ?
C2 C1 H1A 108.4 . . ?
N1 C1 H1B 108.4 2_565 . ?
C2 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
S1 Ag1 S2 144.798(14) 2_565 . ?
S1 Ag1 N1 81.82(3) 2_565 . ?
S2 Ag1 N1 115.30(3) . . ?
S1 Ag1 S3 127.864(13) 2_565 . ?
S2 Ag1 S3 86.336(13) . . ?
N1 Ag1 S3 81.79(3) . . ?
N1 C8 C7 115.25(12) . . ?
N1 C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C7 S3 113.08(11) . . ?
C8 C7 H7A 109.0 . . ?
S3 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
S3 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C5 C6 S3 117.81(11) . . ?
C5 C6 H6A 107.9 . . ?
S3 C6 H6A 107.9 . . ?
C5 C6 H6B 107.9 . . ?
S3 C6 H6B 107.9 . . ?
H6A C6 H6B 107.2 . . ?
C6 C5 S2 115.92(11) . . ?
C6 C5 H5A 108.3 . . ?
S2 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
S2 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C3 C4 S2 110.94(11) . . ?
C3 C4 H4A 109.5 . . ?
S2 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
S2 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
C4 C3 S1 112.41(11) . . ?
C4 C3 H3A 109.1 . . ?
S1 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
S1 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C1 C2 S1 115.04(11) . . ?
C1 C2 H2A 108.5 . . ?
S1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
S1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N1 C9 C10 113.51(13) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C15 119.50(15) . . ?
C11 C10 C9 119.84(14) . . ?
C15 C10 C9 120.65(15) . . ?
C12 C11 C10 119.67(15) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C13 C12 C11 122.01(15) . . ?
C13 C12 Cl1 118.86(13) . . ?
C11 C12 Cl1 119.13(13) . . ?
C12 C13 C14 117.23(15) . . ?
C12 C13 H13 121.4 . . ?
C14 C13 H13 121.4 . . ?
C13 C14 C15 122.38(15) . . ?
C13 C14 Cl2 118.44(13) . . ?
C15 C14 Cl2 119.17(14) . . ?
C14 C15 C10 119.16(16) . . ?
C14 C15 H15 120.4 . . ?
C10 C15 H15 120.4 . . ?
F2 C16 F3 107.55(14) . . ?
F2 C16 F1 107.80(14) . . ?
F3 C16 F1 107.13(14) . . ?
F2 C16 S4 111.66(12) . . ?
F3 C16 S4 111.72(12) . . ?
F1 C16 S4 110.76(12) . . ?
C1 N1 C8 109.99(12) 2_565 . ?
C1 N1 C9 108.96(12) 2_565 . ?
C8 N1 C9 109.31(12) . . ?
C1 N1 Ag1 106.38(9) 2_565 . ?
C8 N1 Ag1 100.87(9) . . ?
C9 N1 Ag1 120.86(9) . . ?
C6 S3 C7 103.32(7) . . ?
C6 S3 Ag1 100.15(5) . . ?
C7 S3 Ag1 96.26(5) . . ?
C5 S2 C4 103.19(7) . . ?
C5 S2 Ag1 98.72(5) . . ?
C4 S2 Ag1 111.66(5) . . ?
C2 S1 C3 101.54(7) . . ?
C2 S1 Ag1 97.62(5) . 2_565 ?
C3 S1 Ag1 109.30(5) . 2_565 ?
O3 S4 O2 115.68(8) . . ?
O3 S4 O1 114.94(8) . . ?
O2 S4 O1 114.63(8) . . ?
O3 S4 C16 102.36(8) . . ?
O2 S4 C16 102.89(8) . . ?
O1 S4 C16 103.80(8) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.083

data_ns3_boc_p21_c
_database_code_depnum_ccdc_archive 'CCDC 284340'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H25 N O2 S3'
_chemical_formula_weight         323.52

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   21.1574(13)
_cell_length_b                   8.5512(6)
_cell_length_c                   9.2467(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.9910(10)
_cell_angle_gamma                90.00
_cell_volume                     1652.37(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7973
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
SADABS, Sheldrick, 1996
;

_diffrn_ambient_temperature      90
_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 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12033
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         0.97
_diffrn_reflns_theta_max         28.30
_reflns_number_total             4115
_reflns_number_gt                3501
_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^)+(0.0555P)^2^+0.5699P] 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         4115
_refine_ls_number_parameters     195
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.1053
_refine_ls_wR_factor_gt          0.0937
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.24178(7) 0.18994(18) 0.66005(19) 0.0184(3) Uani 1 1 d . . .
H1A H 0.2182 0.2609 0.5859 0.022 Uiso 1 1 calc R . .
H1B H 0.2627 0.1088 0.6076 0.022 Uiso 1 1 calc R . .
C2 C 0.29308(8) 0.28324(19) 0.75850(18) 0.0187(3) Uani 1 1 d . . .
H2A H 0.3073 0.2225 0.8489 0.022 Uiso 1 1 calc R . .
H2B H 0.2740 0.3819 0.7872 0.022 Uiso 1 1 calc R . .
C3 C 0.39859(8) 0.1363(2) 0.66648(19) 0.0213(3) Uani 1 1 d . . .
H3A H 0.3646 0.0583 0.6351 0.026 Uiso 1 1 calc R . .
H3B H 0.4280 0.1369 0.5932 0.026 Uiso 1 1 calc R . .
C4 C 0.43514(8) 0.0894(2) 0.8138(2) 0.0233(4) Uani 1 1 d . A .
H4A H 0.4075 0.1067 0.8895 0.028 Uiso 1 1 calc R . .
H4B H 0.4730 0.1581 0.8372 0.028 Uiso 1 1 calc R . .
C7 C 0.24460(8) -0.09152(19) 0.91813(18) 0.0198(3) Uani 1 1 d . . .
H7A H 0.2190 -0.0794 0.9984 0.024 Uiso 1 1 calc R . .
H7B H 0.2808 -0.0170 0.9359 0.024 Uiso 1 1 calc R . .
C8 C 0.20293(8) -0.05228(18) 0.77255(19) 0.0201(3) Uani 1 1 d . . .
H8A H 0.2215 -0.1029 0.6925 0.024 Uiso 1 1 calc R . .
H8B H 0.1598 -0.0973 0.7724 0.024 Uiso 1 1 calc R . .
C9 C 0.14523(7) 0.19170(18) 0.78129(18) 0.0175(3) Uani 1 1 d . . .
C10 C 0.09036(7) 0.44568(19) 0.75156(18) 0.0180(3) Uani 1 1 d . . .
C11 C 0.02730(8) 0.3749(2) 0.6792(2) 0.0241(4) Uani 1 1 d . . .
H11A H 0.0302 0.3480 0.5774 0.036 Uiso 1 1 calc R . .
H11B H -0.0073 0.4507 0.6813 0.036 Uiso 1 1 calc R . .
H11C H 0.0183 0.2802 0.7322 0.036 Uiso 1 1 calc R . .
C12 C 0.09163(10) 0.4816(2) 0.9133(2) 0.0296(4) Uani 1 1 d . . .
H12A H 0.0831 0.3857 0.9649 0.044 Uiso 1 1 calc R . .
H12B H 0.0588 0.5597 0.9240 0.044 Uiso 1 1 calc R . .
H12C H 0.1338 0.5225 0.9549 0.044 Uiso 1 1 calc R . .
C13 C 0.10618(8) 0.58940(19) 0.6680(2) 0.0215(3) Uani 1 1 d . . .
H13A H 0.1487 0.6281 0.7101 0.032 Uiso 1 1 calc R . .
H13B H 0.0742 0.6709 0.6750 0.032 Uiso 1 1 calc R . .
H13C H 0.1058 0.5621 0.5650 0.032 Uiso 1 1 calc R . .
C5A C 0.40180(11) -0.1966(2) 0.9237(2) 0.0220(6) Uani 0.808(6) 1 d P A 1
H5A1 H 0.4212 -0.2847 0.9846 0.026 Uiso 0.808(6) 1 calc PR A 1
H5A2 H 0.3887 -0.1162 0.9902 0.026 Uiso 0.808(6) 1 calc PR A 1
C6A C 0.34313(10) -0.2546(2) 0.8223(2) 0.0208(6) Uani 0.807(6) 1 d P A 1
H6A1 H 0.3538 -0.3527 0.7748 0.025 Uiso 0.807(6) 1 calc PR A 1
H6A2 H 0.3305 -0.1760 0.7445 0.025 Uiso 0.807(6) 1 calc PR A 1
C5B C 0.3801(4) -0.2154(9) 0.7923(9) 0.016(2) Uani 0.192(6) 1 d PU A 2
H5B1 H 0.3481 -0.1510 0.7290 0.019 Uiso 0.192(6) 1 calc PR A 2
H5B2 H 0.3833 -0.3183 0.7447 0.019 Uiso 0.192(6) 1 calc PR A 2
C6B C 0.3611(4) -0.2358(9) 0.9407(9) 0.016(2) Uani 0.193(6) 1 d PU A 2
H6B1 H 0.3684 -0.1372 0.9968 0.019 Uiso 0.193(6) 1 calc PR A 2
H6B2 H 0.3875 -0.3186 0.9952 0.019 Uiso 0.193(6) 1 calc PR A 2
N1 N 0.19639(6) 0.11484(15) 0.74212(16) 0.0182(3) Uani 1 1 d . . .
O1 O 0.10677(6) 0.13141(14) 0.84872(14) 0.0243(3) Uani 1 1 d . . .
O2 O 0.14431(5) 0.34087(13) 0.73486(13) 0.0179(2) Uani 1 1 d . . .
S1 S 0.362329(19) 0.32949(5) 0.67266(5) 0.02037(11) Uani 1 1 d . . .
S2 S 0.46161(2) -0.11308(5) 0.82283(6) 0.02634(13) Uani 1 1 d . . .
S3 S 0.27578(2) -0.29005(5) 0.92030(5) 0.02177(12) 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
C1 0.0151(7) 0.0174(7) 0.0228(8) -0.0014(6) 0.0034(6) 0.0020(6)
C2 0.0165(7) 0.0182(7) 0.0219(8) 0.0006(6) 0.0051(6) -0.0019(6)
C3 0.0184(8) 0.0216(8) 0.0240(8) -0.0010(6) 0.0041(7) 0.0027(6)
C4 0.0234(8) 0.0198(8) 0.0264(9) 0.0021(7) 0.0034(7) 0.0017(6)
C7 0.0221(8) 0.0165(7) 0.0209(8) -0.0004(6) 0.0038(6) 0.0022(6)
C8 0.0191(7) 0.0119(7) 0.0276(9) 0.0005(6) -0.0022(7) 0.0015(6)
C9 0.0138(7) 0.0165(7) 0.0210(8) 0.0012(6) -0.0012(6) -0.0007(6)
C10 0.0134(7) 0.0172(7) 0.0239(8) 0.0012(6) 0.0046(6) 0.0044(6)
C11 0.0138(7) 0.0237(8) 0.0340(10) 0.0033(7) 0.0013(7) 0.0012(6)
C12 0.0334(10) 0.0315(10) 0.0243(9) -0.0005(7) 0.0060(8) 0.0095(8)
C13 0.0183(8) 0.0161(7) 0.0305(9) 0.0012(6) 0.0049(7) 0.0032(6)
C5A 0.0226(13) 0.0198(10) 0.0231(11) 0.0025(8) 0.0019(9) 0.0013(8)
C6A 0.0202(12) 0.0172(10) 0.0252(12) -0.0009(8) 0.0047(9) 0.0013(8)
C5B 0.013(4) 0.012(3) 0.022(3) 0.000(2) -0.001(3) -0.001(2)
C6B 0.011(4) 0.013(3) 0.022(3) 0.001(2) -0.002(3) -0.002(2)
N1 0.0140(6) 0.0126(6) 0.0273(7) 0.0012(5) 0.0014(5) 0.0002(5)
O1 0.0192(6) 0.0222(6) 0.0323(7) 0.0077(5) 0.0064(5) -0.0004(5)
O2 0.0130(5) 0.0139(5) 0.0272(6) 0.0034(4) 0.0048(5) 0.0026(4)
S1 0.0171(2) 0.0171(2) 0.0278(2) 0.00523(16) 0.00622(16) 0.00028(14)
S2 0.0177(2) 0.0197(2) 0.0432(3) 0.00402(18) 0.00986(19) 0.00554(15)
S3 0.0200(2) 0.0161(2) 0.0290(2) 0.00771(16) 0.00327(17) 0.00055(14)

_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 N1 1.462(2) . ?
C1 C2 1.528(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 S1 1.8157(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.512(2) . ?
C3 S1 1.8257(17) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 S2 1.8176(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 C8 1.527(2) . ?
C7 S3 1.8203(17) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.459(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O1 1.214(2) . ?
C9 O2 1.3451(19) . ?
C9 N1 1.363(2) . ?
C10 O2 1.4781(18) . ?
C10 C13 1.516(2) . ?
C10 C11 1.522(2) . ?
C10 C12 1.523(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C5A C6A 1.517(3) . ?
C5A S2 1.831(2) . ?
C5A H5A1 0.9900 . ?
C5A H5A2 0.9900 . ?
C6A S3 1.830(2) . ?
C6A H6A1 0.9900 . ?
C6A H6A2 0.9900 . ?
C5B C6B 1.500(12) . ?
C5B S2 1.915(8) . ?
C5B H5B1 0.9900 . ?
C5B H5B2 0.9900 . ?
C6B S3 1.844(8) . ?
C6B H6B1 0.9900 . ?
C6B H6B2 0.9900 . ?

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
N1 C1 C2 112.52(13) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 S1 113.57(11) . . ?
C1 C2 H2A 108.9 . . ?
S1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
S1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 S1 111.73(12) . . ?
C4 C3 H3A 109.3 . . ?
S1 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
S1 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 S2 113.87(12) . . ?
C3 C4 H4A 108.8 . . ?
S2 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
S2 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C8 C7 S3 111.91(11) . . ?
C8 C7 H7A 109.2 . . ?
S3 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
S3 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N1 C8 C7 114.18(13) . . ?
N1 C8 H8A 108.7 . . ?
C7 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O1 C9 O2 126.09(15) . . ?
O1 C9 N1 123.74(15) . . ?
O2 C9 N1 110.18(13) . . ?
O2 C10 C13 101.70(12) . . ?
O2 C10 C11 110.55(13) . . ?
C13 C10 C11 110.28(14) . . ?
O2 C10 C12 109.24(13) . . ?
C13 C10 C12 111.41(15) . . ?
C11 C10 C12 113.06(14) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C6A C5A S2 112.10(15) . . ?
C6A C5A H5A1 109.2 . . ?
S2 C5A H5A1 109.2 . . ?
C6A C5A H5A2 109.2 . . ?
S2 C5A H5A2 109.2 . . ?
H5A1 C5A H5A2 107.9 . . ?
C5A C6A S3 111.91(15) . . ?
C5A C6A H6A1 109.2 . . ?
S3 C6A H6A1 109.2 . . ?
C5A C6A H6A2 109.2 . . ?
S3 C6A H6A2 109.2 . . ?
H6A1 C6A H6A2 107.9 . . ?
C6B C5B S2 106.4(6) . . ?
C6B C5B H5B1 110.5 . . ?
S2 C5B H5B1 110.5 . . ?
C6B C5B H5B2 110.5 . . ?
S2 C5B H5B2 110.5 . . ?
H5B1 C5B H5B2 108.6 . . ?
C5B C6B S3 109.5(6) . . ?
C5B C6B H6B1 109.8 . . ?
S3 C6B H6B1 109.8 . . ?
C5B C6B H6B2 109.8 . . ?
S3 C6B H6B2 109.8 . . ?
H6B1 C6B H6B2 108.2 . . ?
C9 N1 C8 118.45(14) . . ?
C9 N1 C1 122.65(13) . . ?
C8 N1 C1 118.69(13) . . ?
C9 O2 C10 120.96(12) . . ?
C2 S1 C3 100.86(8) . . ?
C4 S2 C5A 99.35(9) . . ?
C4 S2 C5B 99.5(2) . . ?
C5A S2 C5B 38.6(3) . . ?
C7 S3 C6A 98.56(9) . . ?
C7 S3 C6B 96.5(3) . . ?
C6A S3 C6B 35.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.071