# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               J.Mater.Chem.

_journal_coden_Cambridge         1145
loop_
_publ_author_name
_publ_author_address
'Neil B. McKeown'
;
FIRST AUTHORS ADDRESS
;
'Samer Badriya' ''
'Madeleine Helliwell' ''
'Maxim Shkunov' ''

_publ_contact_author_name        'Neil B. McKeown'
_publ_contact_author_address     
;
School of Chemistry
Cardiff University
Cardiff
CF10 3AT
UNITED KINGDOM
;

_publ_contact_author_email       MCKEOWNNB@CARDIFF.AC.UK

_publ_section_title              
;
The synthesis of robust, polymeric hole-transport
materials from oligoarylamine substituted styrenes.
;

_publ_section_exptl_refinement   
;
The data were collected using the RAXIS in 124 x 2 degree
phi oscillations of 20 minutes per exposure. The structure was solved by
direct methods.
H atoms were included in calculated positions.
The non-H atoms were refined anisotropically.
;

_publ_section_references         
;
Molecular Structure Corporation. (1995). teXsan.
Single Crystal Structure Analysis Software. Version 1.7.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.

Altomare, A., Cascarano, M.,
Giacovazzo, C., Guagliardi, A. (1993).
J. Appl. Cryst., 26, 343.
;

_publ_contact_author             
;
ENTER NAME
ENTER ADDRESS
;
_publ_contact_author_fax         ' ENTER FAX NUMBER '
_publ_contact_author_phone       ' ENTER PHONE NUMBER '
_publ_contact_letter             
;
ENTER TEXT OF LETTER
;

_publ_requested_coeditor_name    ?

data_s990
_database_code_depnum_ccdc_archive 'CCDC 610508'

#------------------------------------------------------------------------------
_audit_creation_date             19101-03-07
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             
;
?
;

_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H17 N'
_chemical_formula_weight         271.35

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  ?

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                   8.09(2)
_cell_length_b                   18.71(2)
_cell_length_c                   10.16(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.091(19)
_cell_angle_gamma                90.00
_cell_volume                     1539(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18132
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.43

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
The data were collected on a Rigaku RAXIS II which has a single
(phi) axis of rotation leading to a low data completeness arising
from a large number of data being in the blind region. However,
the connectivity was unabiguously determined.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'image plate'
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '80 x 4 degree phi scans'

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            18132
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         24.43
_reflns_number_total             1416
_reflns_number_gt                1023
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MSC RAXIS11 Control'
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_structure_solution    
;
SHELXS86 (Sheldrick, 1985)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'teXsan (MSC, 1995)'

_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 w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.6399P] 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     SHELXL
_refine_ls_extinction_coef       0.017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1416
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1133
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N -0.0045(3) 0.22500(15) 0.0396(3) 0.0705(9) Uani 1 d . . .
C1 C 0.0562(5) 0.29377(19) 0.0665(3) 0.0643(10) Uani 1 d . . .
C2 C -0.0472(5) 0.3502(2) 0.0968(3) 0.0790(11) Uani 1 d . . .
H2 H -0.1606 0.3424 0.1010 0.095 Uiso 1 calc R . .
C3 C 0.0122(7) 0.4160(3) 0.1204(4) 0.0991(14) Uani 1 d . . .
H3 H -0.0614 0.4528 0.1388 0.119 Uiso 1 calc R . .
C4 C 0.1760(9) 0.4303(2) 0.1181(4) 0.1001(17) Uani 1 d . . .
C5 C 0.2854(5) 0.3745(3) 0.0900(4) 0.0905(13) Uani 1 d . . .
H5 H 0.3986 0.3830 0.0891 0.109 Uiso 1 calc R . .
C6 C 0.2253(5) 0.3062(2) 0.0632(3) 0.0772(11) Uani 1 d . . .
H6 H 0.2979 0.2693 0.0432 0.093 Uiso 1 calc R . .
C7 C 0.2294(9) 0.5067(4) 0.1464(5) 0.148(2) Uani 1 d . . .
H7 H 0.1445 0.5392 0.1614 0.178 Uiso 1 calc R . .
C8 C 0.3553(8) 0.5284(4) 0.1513(6) 0.183(3) Uani 1 d . . .
H8A H 0.4456 0.4987 0.1371 0.219 Uiso 1 calc R . .
H8B H 0.3717 0.5766 0.1695 0.219 Uiso 1 calc R . .
C9 C 0.0878(4) 0.16311(18) 0.0739(4) 0.0615(9) Uani 1 d . . .
C10 C 0.1542(4) 0.1559(2) 0.1978(4) 0.0709(10) Uani 1 d . . .
H10 H 0.1434 0.1925 0.2592 0.085 Uiso 1 calc R . .
C11 C 0.2367(4) 0.0941(2) 0.2304(4) 0.0833(12) Uani 1 d . . .
H11 H 0.2820 0.0895 0.3141 0.100 Uiso 1 calc R . .
C12 C 0.2536(5) 0.0393(2) 0.1420(5) 0.0851(12) Uani 1 d . . .
H12 H 0.3076 -0.0026 0.1658 0.102 Uiso 1 calc R . .
C13 C 0.1897(5) 0.0473(2) 0.0182(5) 0.0824(12) Uani 1 d . . .
H13 H 0.2020 0.0109 -0.0432 0.099 Uiso 1 calc R . .
C14 C 0.1075(4) 0.1087(2) -0.0161(4) 0.0737(11) Uani 1 d . . .
H14 H 0.0649 0.1136 -0.1007 0.088 Uiso 1 calc R . .
C15 C -0.1639(4) 0.21475(19) -0.0161(3) 0.0645(10) Uani 1 d . . .
C16 C -0.2619(4) 0.1594(2) 0.0292(4) 0.0761(11) Uani 1 d . . .
H16 H -0.2245 0.1303 0.0972 0.091 Uiso 1 calc R . .
C17 C -0.4148(5) 0.1474(2) -0.0262(4) 0.0880(12) Uani 1 d . . .
H17 H -0.4797 0.1099 0.0045 0.106 Uiso 1 calc R . .
C18 C -0.4721(5) 0.1896(3) -0.1254(4) 0.0926(13) Uani 1 d . . .
H18 H -0.5753 0.1812 -0.1626 0.111 Uiso 1 calc R . .
C19 C -0.3757(5) 0.2445(3) -0.1696(4) 0.0929(13) Uani 1 d . . .
H19 H -0.4147 0.2740 -0.2365 0.112 Uiso 1 calc R . .
C20 C -0.2215(5) 0.2570(2) -0.1165(4) 0.0819(12) Uani 1 d . . .
H20 H -0.1565 0.2941 -0.1487 0.098 Uiso 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
N1 0.0669(19) 0.057(2) 0.088(2) -0.0044(16) -0.0183(16) -0.0058(16)
C1 0.077(3) 0.057(3) 0.059(2) 0.0005(18) -0.0076(18) -0.008(2)
C2 0.098(3) 0.066(3) 0.072(3) -0.007(2) -0.006(2) 0.003(3)
C3 0.154(5) 0.072(4) 0.071(3) -0.007(2) -0.016(3) -0.007(3)
C4 0.191(6) 0.051(3) 0.059(3) 0.003(2) -0.030(3) -0.039(4)
C5 0.111(4) 0.094(4) 0.067(3) 0.015(2) -0.024(2) -0.043(3)
C6 0.081(3) 0.078(3) 0.073(3) 0.003(2) -0.011(2) -0.015(2)
C7 0.175(6) 0.186(7) 0.083(4) 0.023(4) -0.024(4) -0.041(5)
C8 0.161(6) 0.248(8) 0.139(5) 0.017(5) -0.016(5) -0.090(6)
C9 0.062(2) 0.056(3) 0.066(3) -0.003(2) -0.0036(19) -0.0083(18)
C10 0.078(3) 0.073(3) 0.062(3) -0.0069(19) -0.001(2) 0.001(2)
C11 0.091(3) 0.088(3) 0.071(3) 0.009(3) -0.004(2) 0.007(3)
C12 0.092(3) 0.064(3) 0.099(4) 0.008(3) 0.003(3) 0.000(2)
C13 0.082(3) 0.069(3) 0.096(4) -0.017(2) 0.001(2) -0.008(2)
C14 0.078(3) 0.071(3) 0.072(3) -0.008(2) -0.0096(19) -0.007(2)
C15 0.063(2) 0.069(3) 0.062(3) -0.0089(19) -0.0036(19) -0.005(2)
C16 0.072(3) 0.081(3) 0.075(3) -0.004(2) -0.001(2) -0.013(2)
C17 0.072(3) 0.101(3) 0.091(3) -0.012(3) 0.011(2) -0.021(2)
C18 0.063(3) 0.128(4) 0.086(4) -0.021(3) -0.006(2) -0.009(3)
C19 0.073(3) 0.131(4) 0.075(3) 0.008(2) -0.010(2) -0.001(3)
C20 0.070(3) 0.098(3) 0.077(3) 0.013(2) -0.003(2) -0.010(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.404(4) . ?
N1 C15 1.420(5) . ?
N1 C9 1.422(4) . ?
C1 C2 1.382(5) . ?
C1 C6 1.389(6) . ?
C2 C3 1.344(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.352(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(6) . ?
C4 C7 1.522(8) . ?
C5 C6 1.393(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.098(7) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9300 . ?
C8 H8B 0.9300 . ?
C9 C10 1.375(10) . ?
C9 C14 1.378(7) . ?
C10 C11 1.375(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.371(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.367(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.372(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C20 1.371(7) . ?
C15 C16 1.383(5) . ?
C16 C17 1.377(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.362(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.366(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.379(6) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C15 121.2(3) . . ?
C1 N1 C9 121.0(3) . . ?
C15 N1 C9 117.7(3) . . ?
C2 C1 C6 118.3(4) . . ?
C2 C1 N1 122.1(4) . . ?
C6 C1 N1 119.6(3) . . ?
C3 C2 C1 121.6(4) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 121.9(5) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 118.5(4) . . ?
C3 C4 C7 117.4(6) . . ?
C5 C4 C7 124.1(6) . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C1 C6 C5 119.5(4) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C8 C7 C4 128.3(9) . . ?
C8 C7 H7 115.8 . . ?
C4 C7 H7 115.8 . . ?
C7 C8 H8A 120.0 . . ?
C7 C8 H8B 120.0 . . ?
H8A C8 H8B 120.0 . . ?
C10 C9 C14 119.3(5) . . ?
C10 C9 N1 120.6(3) . . ?
C14 C9 N1 120.0(5) . . ?
C9 C10 C11 119.5(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 121.3(5) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 C11 118.9(5) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 120.5(4) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C9 120.4(5) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
C20 C15 C16 119.0(4) . . ?
C20 C15 N1 121.7(4) . . ?
C16 C15 N1 119.3(4) . . ?
C17 C16 C15 120.1(4) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C18 C19 C20 121.0(4) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C15 C20 C19 120.0(4) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C1 C2 29.0(5) . . . . ?
C9 N1 C1 C2 -147.4(4) . . . . ?
C15 N1 C1 C6 -151.1(4) . . . . ?
C9 N1 C1 C6 32.4(5) . . . . ?
C6 C1 C2 C3 1.2(5) . . . . ?
N1 C1 C2 C3 -179.0(3) . . . . ?
C1 C2 C3 C4 -1.3(6) . . . . ?
C2 C3 C4 C5 0.2(6) . . . . ?
C2 C3 C4 C7 -180.0(4) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C7 C4 C5 C6 -179.0(4) . . . . ?
C2 C1 C6 C5 -0.1(5) . . . . ?
N1 C1 C6 C5 -180.0(3) . . . . ?
C4 C5 C6 C1 -0.9(5) . . . . ?
C3 C4 C7 C8 178.5(7) . . . . ?
C5 C4 C7 C8 -1.7(9) . . . . ?
C1 N1 C9 C10 48.7(5) . . . . ?
C15 N1 C9 C10 -127.9(3) . . . . ?
C1 N1 C9 C14 -133.2(3) . . . . ?
C15 N1 C9 C14 50.2(4) . . . . ?
C14 C9 C10 C11 -1.0(5) . . . . ?
N1 C9 C10 C11 177.1(3) . . . . ?
C9 C10 C11 C12 -0.3(5) . . . . ?
C10 C11 C12 C13 1.4(6) . . . . ?
C11 C12 C13 C14 -1.1(6) . . . . ?
C12 C13 C14 C9 -0.2(5) . . . . ?
C10 C9 C14 C13 1.3(5) . . . . ?
N1 C9 C14 C13 -176.9(3) . . . . ?
C1 N1 C15 C20 42.3(5) . . . . ?
C9 N1 C15 C20 -141.1(4) . . . . ?
C1 N1 C15 C16 -139.6(4) . . . . ?
C9 N1 C15 C16 37.0(5) . . . . ?
C20 C15 C16 C17 0.0(5) . . . . ?
N1 C15 C16 C17 -178.1(3) . . . . ?
C15 C16 C17 C18 -0.3(6) . . . . ?
C16 C17 C18 C19 -0.1(6) . . . . ?
C17 C18 C19 C20 0.9(6) . . . . ?
C16 C15 C20 C19 0.7(5) . . . . ?
N1 C15 C20 C19 178.8(3) . . . . ?
C18 C19 C20 C15 -1.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.538
_diffrn_reflns_theta_full        24.43
_diffrn_measured_fraction_theta_full 0.538
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.028

# Attachment '1ds927.txt'

data_s927
_database_code_depnum_ccdc_archive 'CCDC 610509'

#------------------------------------------------------------------------------
_audit_creation_date             19101-03-07
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             
;
?
;

_publ_section_abstract           
;
ENTER ABSTRACT
;

_publ_section_exptl_prep         
;
ENTER EXPERIMENTAL SECTION
;

_publ_section_exptl_refinement   
;
The data were collected using the RAXIS in 106 x 3 degree
phi oscillations of 10 minutes per exposure. The structure was
solved by direct methods. There are 2 molecules in the asymmetric unit.
For the second, the atoms C39 and C40 are disordered over two sites each,
whose occupancies were constrained to sum to 1.0. H atoms were included
in calculated positions.
The non-H atoms were refined anisotropically, except those of the
disordered sites.

;

_publ_section_comment            
;
ENTER TEXT
;

_publ_section_references         
;
ENTER OTHER REFERENCES

Molecular Structure Corporation. (1995). teXsan.
Single Crystal Structure Analysis Software. Version 1.7.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.

Altomare, A., Cascarano, M.,
Giacovazzo, C., Guagliardi, A. (1993).
J. Appl. Cryst., 26, 343.
;

_publ_section_acknowledgements   
;
ENTER ACKNOWLEDGEMENTS
;

_publ_section_table_legends      
;
ENTER TABLE LEGENDS
;

_publ_section_figure_captions    
;
ENTER FIGURE CAPTIONS
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H15 N S'
_chemical_formula_weight         301.39

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'
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   'P 21/a '
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  ?

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

_cell_length_a                   14.178(6)
_cell_length_b                   14.05(3)
_cell_length_c                   15.909(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.62(3)
_cell_angle_gamma                90.00
_cell_volume                     3164(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    51660
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      26.34

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'scintillation counter'
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '95 x 3 degree phi scans'

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            51660
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         26.34
_reflns_number_total             6246
_reflns_number_gt                4989
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MSC RAXIS11 Control'
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_structure_solution    
;
SHELXS86 (Sheldrick, 1985)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'teXsan (MSC, 1995)'

_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 w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.8963P] 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     SHELXL
_refine_ls_extinction_coef       0.035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6246
_refine_ls_number_parameters     394
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1734
_refine_ls_wR_factor_gt          0.1631
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.121
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.53509(4) 0.16857(4) 0.63377(5) 0.0765(3) Uani 1 d . . .
N1 N 0.33553(11) 0.15114(11) 0.55007(11) 0.0527(4) Uani 1 d . . .
C1 C 0.44083(13) 0.24793(14) 0.64396(13) 0.0517(5) Uani 1 d . . .
C2 C 0.45701(16) 0.32895(15) 0.69301(15) 0.0609(5) Uani 1 d . . .
H2 H 0.5140 0.3356 0.7247 0.073 Uiso 1 calc R . .
C3 C 0.38958(18) 0.39971(16) 0.69536(17) 0.0684(6) Uani 1 d . . .
H3 H 0.4010 0.4539 0.7279 0.082 Uiso 1 calc R . .
C4 C 0.30562(17) 0.38870(16) 0.64891(18) 0.0696(6) Uani 1 d . . .
H4 H 0.2606 0.4368 0.6487 0.084 Uiso 1 calc R . .
C5 C 0.28686(15) 0.30675(15) 0.60218(15) 0.0600(5) Uani 1 d . . .
H5 H 0.2285 0.2999 0.5727 0.072 Uiso 1 calc R . .
C6 C 0.35370(13) 0.23474(13) 0.59864(12) 0.0476(4) Uani 1 d . . .
C7 C 0.38202(13) 0.06369(13) 0.57058(12) 0.0482(4) Uani 1 d . . .
C8 C 0.33975(15) -0.02390(14) 0.55100(14) 0.0566(5) Uani 1 d . . .
H8 H 0.2791 -0.0254 0.5250 0.068 Uiso 1 calc R . .
C9 C 0.38631(17) -0.10844(15) 0.56948(15) 0.0627(6) Uani 1 d . . .
H9 H 0.3569 -0.1658 0.5552 0.075 Uiso 1 calc R . .
C10 C 0.47547(17) -0.10891(16) 0.60866(16) 0.0649(6) Uani 1 d . . .
H10 H 0.5067 -0.1660 0.6207 0.078 Uiso 1 calc R . .
C11 C 0.51787(15) -0.02301(16) 0.62976(15) 0.0616(5) Uani 1 d . . .
H11 H 0.5777 -0.0225 0.6573 0.074 Uiso 1 calc R . .
C12 C 0.47274(14) 0.06269(15) 0.61062(13) 0.0530(5) Uani 1 d . . .
C13 C 0.24659(14) 0.14521(13) 0.50073(13) 0.0514(5) Uani 1 d . . .
C14 C 0.24460(15) 0.15792(14) 0.41490(14) 0.0556(5) Uani 1 d . . .
H14 H 0.3000 0.1717 0.3891 0.067 Uiso 1 calc R . .
C15 C 0.15983(17) 0.15016(15) 0.36696(15) 0.0613(5) Uani 1 d . . .
H15 H 0.1594 0.1581 0.3089 0.074 Uiso 1 calc R . .
C16 C 0.07565(15) 0.13087(15) 0.40347(14) 0.0588(5) Uani 1 d . . .
C17 C 0.07874(15) 0.11797(16) 0.49038(16) 0.0622(6) Uani 1 d . . .
H17 H 0.0233 0.1047 0.5163 0.075 Uiso 1 calc R . .
C18 C 0.16312(15) 0.12461(16) 0.53869(14) 0.0597(5) Uani 1 d . . .
H18 H 0.1641 0.1153 0.5966 0.072 Uiso 1 calc R . .
C19 C -0.01473(18) 0.12501(19) 0.35107(19) 0.0766(7) Uani 1 d D . .
H19 H -0.0091 0.1257 0.2931 0.092 Uiso 1 calc R . .
C20 C -0.0971(2) 0.1193(2) 0.3740(3) 0.1016(10) Uani 1 d D . .
H20A H -0.1078 0.1183 0.4310 0.122 Uiso 1 calc R . .
H20B H -0.1478 0.1161 0.3340 0.122 Uiso 1 calc R . .
S2 S 0.07502(7) 0.09399(7) 0.10950(5) 0.1014(3) Uani 1 d . . .
N2 N 0.16500(16) 0.28879(18) 0.11528(13) 0.0764(6) Uani 1 d . . .
C21 C 0.1960(2) 0.1181(2) 0.12821(16) 0.0845(8) Uani 1 d . . .
C22 C 0.2589(3) 0.0423(3) 0.1436(2) 0.1062(11) Uani 1 d . . .
H22 H 0.2373 -0.0200 0.1377 0.127 Uiso 1 calc R . .
C23 C 0.3524(3) 0.0595(4) 0.1673(2) 0.1191(13) Uani 1 d . . .
H23 H 0.3940 0.0091 0.1778 0.143 Uiso 1 calc R . .
C24 C 0.3835(3) 0.1512(4) 0.1754(2) 0.1120(12) Uani 1 d . . .
H24 H 0.4463 0.1627 0.1930 0.134 Uiso 1 calc R . .
C25 C 0.3232(2) 0.2279(3) 0.15803(19) 0.0912(9) Uani 1 d . . .
H25 H 0.3461 0.2898 0.1630 0.109 Uiso 1 calc R . .
C26 C 0.2284(2) 0.2119(2) 0.13309(15) 0.0756(7) Uani 1 d . . .
C27 C 0.08916(18) 0.2781(2) 0.05339(17) 0.0776(7) Uani 1 d . . .
C28 C 0.0552(2) 0.3541(3) 0.0045(2) 0.0975(9) Uani 1 d . . .
H28 H 0.0826 0.4139 0.0120 0.117 Uiso 1 calc R . .
C29 C -0.0194(3) 0.3415(3) -0.0557(3) 0.1205(13) Uani 1 d . . .
H29 H -0.0425 0.3933 -0.0870 0.145 Uiso 1 calc R . .
C30 C -0.0592(2) 0.2536(4) -0.0693(3) 0.1215(14) Uani 1 d . . .
H30 H -0.1074 0.2453 -0.1110 0.146 Uiso 1 calc R . .
C31 C -0.0273(2) 0.1779(3) -0.0209(2) 0.1036(11) Uani 1 d . . .
H31 H -0.0542 0.1182 -0.0300 0.124 Uiso 1 calc R . .
C32 C 0.04479(19) 0.1897(2) 0.04170(18) 0.0836(8) Uani 1 d . . .
C33 C 0.19831(17) 0.3842(2) 0.13199(15) 0.0712(6) Uani 1 d . . .
C34 C 0.1698(2) 0.4325(2) 0.20133(17) 0.0827(8) Uani 1 d . . .
H34 H 0.1300 0.4028 0.2375 0.099 Uiso 1 calc R . .
C35 C 0.1993(2) 0.5236(3) 0.2177(2) 0.0955(9) Uani 1 d . . .
H35 H 0.1788 0.5543 0.2650 0.115 Uiso 1 calc R . .
C36 C 0.2574(3) 0.5712(3) 0.1674(2) 0.0972(10) Uani 1 d . . .
C37 C 0.2873(3) 0.5228(3) 0.0975(2) 0.1067(11) Uani 1 d . . .
H37 H 0.3276 0.5531 0.0622 0.128 Uiso 1 calc R . .
C38 C 0.2584(2) 0.4301(3) 0.07952(19) 0.0927(9) Uani 1 d . . .
H38 H 0.2791 0.3990 0.0325 0.111 Uiso 1 calc R . .
C39A C 0.2685(4) 0.6739(4) 0.2043(4) 0.0800(14) Uiso 0.50 d PD A 1
H39A H 0.2370 0.6837 0.2531 0.096 Uiso 0.50 calc PR A 1
C40A C 0.3046(4) 0.7330(5) 0.1843(4) 0.141(4) Uiso 0.50 d PD A 1
H40A H 0.3381 0.7296 0.1360 0.169 Uiso 0.50 calc PR A 1
H40B H 0.3035 0.7895 0.2147 0.169 Uiso 0.50 calc PR A 1
C39B C 0.2997(4) 0.6685(5) 0.1694(4) 0.115(3) Uiso 0.50 d PRD A 2
H39B H 0.2958 0.6808 0.2265 0.138 Uiso 0.50 calc PR A 2
C40B C 0.3319(6) 0.7353(5) 0.1517(6) 0.113(2) Uiso 0.50 d PD A 2
H40C H 0.3456 0.7459 0.0961 0.136 Uiso 0.50 calc PR A 2
H40D H 0.3457 0.7818 0.1922 0.136 Uiso 0.50 calc PR 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 0.0391(3) 0.0633(4) 0.1257(6) -0.0264(3) -0.0058(3) -0.0019(2)
N1 0.0439(8) 0.0483(9) 0.0643(10) -0.0072(7) -0.0091(7) 0.0007(7)
C1 0.0434(10) 0.0488(10) 0.0622(12) -0.0031(8) -0.0017(8) -0.0052(8)
C2 0.0554(12) 0.0549(12) 0.0710(14) -0.0088(10) -0.0067(10) -0.0073(9)
C3 0.0748(15) 0.0497(11) 0.0796(16) -0.0143(10) -0.0047(12) -0.0018(10)
C4 0.0650(14) 0.0487(11) 0.0936(17) -0.0081(11) -0.0074(12) 0.0104(10)
C5 0.0533(11) 0.0508(11) 0.0741(14) -0.0010(9) -0.0100(10) 0.0029(9)
C6 0.0452(9) 0.0438(9) 0.0533(10) -0.0005(8) -0.0009(8) -0.0036(7)
C7 0.0443(10) 0.0477(10) 0.0523(10) -0.0033(8) 0.0008(8) 0.0001(7)
C8 0.0523(11) 0.0505(11) 0.0657(13) -0.0026(9) -0.0058(9) -0.0047(8)
C9 0.0691(14) 0.0477(11) 0.0704(14) -0.0008(9) -0.0018(11) -0.0051(9)
C10 0.0649(13) 0.0530(12) 0.0761(15) 0.0026(10) -0.0010(11) 0.0087(10)
C11 0.0485(11) 0.0645(13) 0.0710(14) -0.0026(10) -0.0043(9) 0.0087(9)
C12 0.0426(10) 0.0547(11) 0.0615(12) -0.0069(9) 0.0002(8) 0.0014(8)
C13 0.0440(9) 0.0469(10) 0.0620(12) -0.0056(8) -0.0068(8) 0.0008(8)
C14 0.0526(11) 0.0514(11) 0.0621(12) -0.0042(9) -0.0020(9) 0.0030(8)
C15 0.0661(13) 0.0581(12) 0.0585(12) -0.0053(9) -0.0064(10) 0.0072(10)
C16 0.0545(12) 0.0485(10) 0.0711(14) -0.0104(9) -0.0137(10) 0.0045(9)
C17 0.0467(11) 0.0630(13) 0.0763(15) -0.0083(10) -0.0011(10) -0.0054(9)
C18 0.0516(11) 0.0654(13) 0.0610(12) -0.0041(10) -0.0042(9) -0.0059(9)
C19 0.0637(15) 0.0716(15) 0.0907(18) -0.0142(13) -0.0236(12) 0.0052(12)
C20 0.0615(16) 0.108(2) 0.131(3) 0.004(2) -0.0303(17) -0.0090(15)
S2 0.1089(7) 0.1109(7) 0.0852(5) 0.0021(4) 0.0119(4) -0.0258(5)
N2 0.0680(12) 0.0951(16) 0.0653(12) 0.0011(11) -0.0008(10) -0.0018(11)
C21 0.100(2) 0.101(2) 0.0526(14) 0.0037(13) 0.0044(13) 0.0027(17)
C22 0.144(3) 0.103(2) 0.0702(18) 0.0022(16) -0.0003(19) 0.023(2)
C23 0.135(3) 0.137(4) 0.084(2) 0.009(2) -0.007(2) 0.047(3)
C24 0.091(2) 0.154(4) 0.089(2) 0.017(2) -0.0099(17) 0.027(2)
C25 0.0763(18) 0.120(2) 0.0758(17) 0.0121(16) -0.0062(14) 0.0038(17)
C26 0.0765(16) 0.0976(19) 0.0524(13) 0.0060(12) 0.0020(11) 0.0041(14)
C27 0.0586(13) 0.104(2) 0.0695(15) -0.0054(14) 0.0034(11) 0.0025(13)
C28 0.0799(19) 0.113(2) 0.097(2) -0.0021(18) -0.0155(16) 0.0115(17)
C29 0.088(2) 0.146(4) 0.123(3) 0.000(3) -0.031(2) 0.023(2)
C30 0.073(2) 0.170(4) 0.117(3) -0.020(3) -0.0271(19) 0.007(2)
C31 0.0666(17) 0.140(3) 0.103(2) -0.021(2) -0.0012(16) -0.0106(18)
C32 0.0621(14) 0.115(2) 0.0736(16) -0.0101(15) 0.0082(12) -0.0059(15)
C33 0.0610(13) 0.0936(18) 0.0588(13) 0.0020(12) 0.0018(10) -0.0020(12)
C34 0.0686(15) 0.116(2) 0.0640(15) -0.0018(15) 0.0070(12) -0.0003(15)
C35 0.093(2) 0.110(2) 0.082(2) -0.0203(18) -0.0079(16) 0.0022(19)
C36 0.092(2) 0.100(2) 0.094(2) -0.0004(18) -0.0346(18) 0.0001(18)
C37 0.090(2) 0.120(3) 0.108(3) 0.035(2) -0.0017(19) -0.027(2)
C38 0.092(2) 0.117(2) 0.0713(17) 0.0019(16) 0.0201(15) -0.0118(18)

_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 C1 1.756(3) . ?
S1 C12 1.758(3) . ?
N1 C6 1.421(3) . ?
N1 C7 1.423(3) . ?
N1 C13 1.445(2) . ?
C1 C2 1.391(3) . ?
C1 C6 1.403(3) . ?
C2 C3 1.382(4) . ?
C3 C4 1.370(3) . ?
C4 C5 1.387(4) . ?
C5 C6 1.390(3) . ?
C7 C8 1.396(3) . ?
C7 C12 1.399(3) . ?
C8 C9 1.382(4) . ?
C9 C10 1.374(3) . ?
C10 C11 1.381(4) . ?
C11 C12 1.389(4) . ?
C13 C14 1.376(3) . ?
C13 C18 1.393(3) . ?
C14 C15 1.387(3) . ?
C15 C16 1.387(3) . ?
C16 C17 1.392(3) . ?
C16 C19 1.486(3) . ?
C17 C18 1.384(3) . ?
C19 C20 1.248(4) . ?
S2 C21 1.755(3) . ?
S2 C32 1.760(4) . ?
N2 C27 1.419(3) . ?
N2 C26 1.423(4) . ?
N2 C33 1.441(4) . ?
C21 C26 1.396(5) . ?
C21 C22 1.400(5) . ?
C22 C23 1.377(6) . ?
C23 C24 1.365(7) . ?
C24 C25 1.393(5) . ?
C25 C26 1.395(4) . ?
C27 C28 1.389(5) . ?
C27 C32 1.400(5) . ?
C28 C29 1.393(5) . ?
C29 C30 1.368(6) . ?
C30 C31 1.373(6) . ?
C31 C32 1.391(4) . ?
C33 C34 1.377(4) . ?
C33 C38 1.388(4) . ?
C34 C35 1.367(5) . ?
C35 C36 1.360(5) . ?
C36 C37 1.391(5) . ?
C36 C39B 1.492(7) . ?
C36 C39A 1.562(7) . ?
C37 C38 1.390(6) . ?
C39A C40A 1.036(6) . ?
C39B C40B 1.089(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C12 100.45(14) . . ?
C6 N1 C7 121.61(18) . . ?
C6 N1 C13 117.72(16) . . ?
C7 N1 C13 116.78(16) . . ?
C2 C1 C6 120.34(19) . . ?
C2 C1 S1 118.17(17) . . ?
C6 C1 S1 121.28(16) . . ?
C3 C2 C1 121.0(2) . . ?
C4 C3 C2 118.9(2) . . ?
C3 C4 C5 120.9(2) . . ?
C4 C5 C6 121.2(2) . . ?
C5 C6 C1 117.61(19) . . ?
C5 C6 N1 121.56(19) . . ?
C1 C6 N1 120.82(17) . . ?
C8 C7 C12 117.53(18) . . ?
C8 C7 N1 121.64(19) . . ?
C12 C7 N1 120.83(17) . . ?
C9 C8 C7 121.2(2) . . ?
C10 C9 C8 120.9(2) . . ?
C9 C10 C11 118.7(2) . . ?
C10 C11 C12 121.2(2) . . ?
C11 C12 C7 120.42(19) . . ?
C11 C12 S1 118.00(19) . . ?
C7 C12 S1 121.51(16) . . ?
C14 C13 C18 119.52(19) . . ?
C14 C13 N1 119.61(19) . . ?
C18 C13 N1 120.85(19) . . ?
C13 C14 C15 119.9(2) . . ?
C14 C15 C16 121.6(2) . . ?
C15 C16 C17 117.87(19) . . ?
C15 C16 C19 120.7(2) . . ?
C17 C16 C19 121.4(2) . . ?
C18 C17 C16 121.0(2) . . ?
C17 C18 C13 120.1(2) . . ?
C20 C19 C16 129.0(3) . . ?
C21 S2 C32 98.85(15) . . ?
C27 N2 C26 119.9(2) . . ?
C27 N2 C33 116.8(2) . . ?
C26 N2 C33 118.3(2) . . ?
C26 C21 C22 120.3(3) . . ?
C26 C21 S2 120.4(2) . . ?
C22 C21 S2 119.1(3) . . ?
C23 C22 C21 120.4(4) . . ?
C24 C23 C22 119.4(4) . . ?
C23 C24 C25 121.4(4) . . ?
C24 C25 C26 120.0(4) . . ?
C25 C26 C21 118.4(3) . . ?
C25 C26 N2 121.3(3) . . ?
C21 C26 N2 120.3(3) . . ?
C28 C27 C32 118.1(3) . . ?
C28 C27 N2 121.8(3) . . ?
C32 C27 N2 120.0(3) . . ?
C27 C28 C29 120.6(4) . . ?
C30 C29 C28 120.7(4) . . ?
C29 C30 C31 119.5(3) . . ?
C30 C31 C32 120.7(4) . . ?
C31 C32 C27 120.3(3) . . ?
C31 C32 S2 119.2(3) . . ?
C27 C32 S2 120.4(2) . . ?
C34 C33 C38 118.3(3) . . ?
C34 C33 N2 119.8(2) . . ?
C38 C33 N2 121.9(3) . . ?
C35 C34 C33 120.8(3) . . ?
C36 C35 C34 122.5(3) . . ?
C35 C36 C37 117.1(3) . . ?
C35 C36 C39B 134.0(4) . . ?
C37 C36 C39B 108.9(4) . . ?
C35 C36 C39A 106.4(4) . . ?
C37 C36 C39A 136.4(4) . . ?
C39B C36 C39A 27.7(3) . . ?
C38 C37 C36 121.5(3) . . ?
C33 C38 C37 119.7(3) . . ?
C40A C39A C36 131.7(7) . . ?
C40B C39B C36 163.5(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 S1 C1 C2 155.30(18) . . . . ?
C12 S1 C1 C6 -29.9(2) . . . . ?
C6 C1 C2 C3 -2.8(3) . . . . ?
S1 C1 C2 C3 172.09(19) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C3 C4 C5 2.0(4) . . . . ?
C3 C4 C5 C6 -2.2(4) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C4 C5 C6 N1 -179.2(2) . . . . ?
C2 C1 C6 C5 2.5(3) . . . . ?
S1 C1 C6 C5 -172.20(17) . . . . ?
C2 C1 C6 N1 -178.37(19) . . . . ?
S1 C1 C6 N1 6.9(3) . . . . ?
C7 N1 C6 C5 -154.0(2) . . . . ?
C13 N1 C6 C5 3.0(3) . . . . ?
C7 N1 C6 C1 26.9(3) . . . . ?
C13 N1 C6 C1 -176.08(19) . . . . ?
C6 N1 C7 C8 151.4(2) . . . . ?
C13 N1 C7 C8 -5.9(3) . . . . ?
C6 N1 C7 C12 -29.3(3) . . . . ?
C13 N1 C7 C12 173.44(19) . . . . ?
C12 C7 C8 C9 -0.8(3) . . . . ?
N1 C7 C8 C9 178.5(2) . . . . ?
C7 C8 C9 C10 0.7(4) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C9 C10 C11 C12 -1.2(4) . . . . ?
C10 C11 C12 C7 1.1(3) . . . . ?
C10 C11 C12 S1 -175.99(19) . . . . ?
C8 C7 C12 C11 -0.1(3) . . . . ?
N1 C7 C12 C11 -179.46(19) . . . . ?
C8 C7 C12 S1 176.94(16) . . . . ?
N1 C7 C12 S1 -2.4(3) . . . . ?
C1 S1 C12 C11 -155.22(18) . . . . ?
C1 S1 C12 C7 27.7(2) . . . . ?
C6 N1 C13 C14 104.6(2) . . . . ?
C7 N1 C13 C14 -97.2(2) . . . . ?
C6 N1 C13 C18 -76.9(3) . . . . ?
C7 N1 C13 C18 81.3(2) . . . . ?
C18 C13 C14 C15 0.0(3) . . . . ?
N1 C13 C14 C15 178.52(18) . . . . ?
C13 C14 C15 C16 0.8(3) . . . . ?
C14 C15 C16 C17 -0.9(3) . . . . ?
C14 C15 C16 C19 178.6(2) . . . . ?
C15 C16 C17 C18 0.3(3) . . . . ?
C19 C16 C17 C18 -179.3(2) . . . . ?
C16 C17 C18 C13 0.5(3) . . . . ?
C14 C13 C18 C17 -0.6(3) . . . . ?
N1 C13 C18 C17 -179.15(19) . . . . ?
C15 C16 C19 C20 -170.9(3) . . . . ?
C17 C16 C19 C20 8.6(4) . . . . ?
C32 S2 C21 C26 34.9(3) . . . . ?
C32 S2 C21 C22 -149.2(2) . . . . ?
C26 C21 C22 C23 2.9(5) . . . . ?
S2 C21 C22 C23 -173.0(3) . . . . ?
C21 C22 C23 C24 -0.3(5) . . . . ?
C22 C23 C24 C25 -1.7(6) . . . . ?
C23 C24 C25 C26 1.1(5) . . . . ?
C24 C25 C26 C21 1.5(4) . . . . ?
C24 C25 C26 N2 179.7(3) . . . . ?
C22 C21 C26 C25 -3.5(4) . . . . ?
S2 C21 C26 C25 172.4(2) . . . . ?
C22 C21 C26 N2 178.3(2) . . . . ?
S2 C21 C26 N2 -5.8(3) . . . . ?
C27 N2 C26 C25 148.2(3) . . . . ?
C33 N2 C26 C25 -6.4(4) . . . . ?
C27 N2 C26 C21 -33.7(4) . . . . ?
C33 N2 C26 C21 171.8(2) . . . . ?
C26 N2 C27 C28 -148.0(3) . . . . ?
C33 N2 C27 C28 6.9(4) . . . . ?
C26 N2 C27 C32 33.6(4) . . . . ?
C33 N2 C27 C32 -171.5(2) . . . . ?
C32 C27 C28 C29 -1.4(5) . . . . ?
N2 C27 C28 C29 -179.9(3) . . . . ?
C27 C28 C29 C30 -1.7(6) . . . . ?
C28 C29 C30 C31 2.4(7) . . . . ?
C29 C30 C31 C32 0.0(6) . . . . ?
C30 C31 C32 C27 -3.2(5) . . . . ?
C30 C31 C32 S2 173.4(3) . . . . ?
C28 C27 C32 C31 3.8(4) . . . . ?
N2 C27 C32 C31 -177.7(3) . . . . ?
C28 C27 C32 S2 -172.7(2) . . . . ?
N2 C27 C32 S2 5.8(4) . . . . ?
C21 S2 C32 C31 148.5(2) . . . . ?
C21 S2 C32 C27 -35.0(3) . . . . ?
C27 N2 C33 C34 100.1(3) . . . . ?
C26 N2 C33 C34 -104.6(3) . . . . ?
C27 N2 C33 C38 -79.4(3) . . . . ?
C26 N2 C33 C38 75.9(3) . . . . ?
C38 C33 C34 C35 0.6(4) . . . . ?
N2 C33 C34 C35 -178.9(3) . . . . ?
C33 C34 C35 C36 0.0(5) . . . . ?
C34 C35 C36 C37 -0.6(5) . . . . ?
C34 C35 C36 C39B 179.8(4) . . . . ?
C34 C35 C36 C39A 176.4(3) . . . . ?
C35 C36 C37 C38 0.6(5) . . . . ?
C39B C36 C37 C38 -179.7(4) . . . . ?
C39A C36 C37 C38 -175.3(4) . . . . ?
C34 C33 C38 C37 -0.5(5) . . . . ?
N2 C33 C38 C37 178.9(3) . . . . ?
C36 C37 C38 C33 0.0(5) . . . . ?
C35 C36 C39A C40A -177.8(9) . . . . ?
C37 C36 C39A C40A -1.6(12) . . . . ?
C39B C36 C39A C40A 7.4(3) . . . . ?
C35 C36 C39B C40B -158(3) . . . . ?
C37 C36 C39B C40B 23(3) . . . . ?
C39A C36 C39B C40B -151(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        26.34
_diffrn_measured_fraction_theta_full 0.927
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.037

# Attachment '1cs926.txt'

data_s926
_database_code_depnum_ccdc_archive 'CCDC 610510'

#------------------------------------------------------------------------------
_audit_creation_date             19101-03-07
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             
;
?
;

_publ_section_abstract           
;
ENTER ABSTRACT
;

_publ_section_exptl_prep         
;
ENTER EXPERIMENTAL SECTION
;

_publ_section_exptl_refinement   
;
The data were collected using the RAXIS in 120 x 2 degree
phi oscillations of 10 minutes per exposure. The structure was
solved by direct methods. H atoms were included
in calculated positions, and the non-H atoms were refined anisotropically.

;

_publ_section_comment            
;
ENTER TEXT
;

_publ_section_references         
;
ENTER OTHER REFERENCES

Molecular Structure Corporation. (1995). teXsan.
Single Crystal Structure Analysis Software. Version 1.7.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.

Altomare, A., Cascarano, M.,
Giacovazzo, C., Guagliardi, A. (1993).
J. Appl. Cryst., 26, 343.
;

_publ_section_acknowledgements   
;
ENTER ACKNOWLEDGEMENTS
;

_publ_section_table_legends      
;
ENTER TABLE LEGENDS
;

_publ_section_figure_captions    
;
ENTER FIGURE CAPTIONS
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H15 N'
_chemical_formula_weight         269.33

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  ?

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

_cell_length_a                   16.19(4)
_cell_length_b                   7.739(10)
_cell_length_c                   23.46(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2939(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    38287
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      26.30

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
The data were collected on a Rigaku RAXIS II which has a single
(phi) axis of rotation leading to a low data completeness arising
from a large number of data being in the blind region. However,
the connectivity was unabiguously determined.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'image plate'
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '120 x 2 degree phi scans'

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            38287
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         26.30
_reflns_number_total             1980
_reflns_number_gt                1497
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MSC RAXIS11 Control'
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_structure_solution    
;
SHELXS86 (Sheldrick, 1985)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'teXsan (MSC, 1995)'

_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 w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0974P] 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     SHELXL
_refine_ls_extinction_coef       0.0161(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         1980
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.45748(8) 0.02891(15) 0.63705(5) 0.0588(4) Uani 1 d . . .
C1 C 0.53342(10) -0.0518(2) 0.63069(7) 0.0586(4) Uani 1 d . . .
C2 C 0.59972(12) -0.0066(2) 0.59660(7) 0.0707(5) Uani 1 d . . .
H2 H 0.5977 0.0902 0.5732 0.085 Uiso 1 calc R . .
C3 C 0.66836(13) -0.1095(3) 0.59861(9) 0.0846(6) Uani 1 d . . .
H3 H 0.7138 -0.0821 0.5760 0.101 Uiso 1 calc R . .
C4 C 0.67169(14) -0.2534(3) 0.63344(10) 0.0917(7) Uani 1 d . . .
H4 H 0.7188 -0.3222 0.6333 0.110 Uiso 1 calc R . .
C5 C 0.60713(15) -0.2963(2) 0.66796(8) 0.0826(6) Uani 1 d . . .
H5 H 0.6103 -0.3924 0.6916 0.099 Uiso 1 calc R . .
C6 C 0.53656(11) -0.1945(2) 0.66728(7) 0.0621(5) Uani 1 d . . .
C7 C 0.45975(11) -0.19927(19) 0.69760(7) 0.0597(5) Uani 1 d . . .
C8 C 0.42744(14) -0.3071(2) 0.73915(8) 0.0742(5) Uani 1 d . . .
H8 H 0.4588 -0.3977 0.7536 0.089 Uiso 1 calc R . .
C9 C 0.34943(15) -0.2793(2) 0.75858(8) 0.0814(6) Uani 1 d . . .
H9 H 0.3277 -0.3507 0.7867 0.098 Uiso 1 calc R . .
C10 C 0.30213(12) -0.1461(2) 0.73703(8) 0.0767(5) Uani 1 d . . .
H10 H 0.2485 -0.1310 0.7503 0.092 Uiso 1 calc R . .
C11 C 0.33244(11) -0.0352(2) 0.69637(7) 0.0655(5) Uani 1 d . . .
H11 H 0.3004 0.0545 0.6821 0.079 Uiso 1 calc R . .
C12 C 0.41210(10) -0.06182(19) 0.67756(6) 0.0556(4) Uani 1 d . . .
C13 C 0.43177(10) 0.18146(18) 0.60834(7) 0.0555(4) Uani 1 d . . .
C14 C 0.40449(11) 0.32233(19) 0.63888(7) 0.0644(5) Uani 1 d . . .
H14 H 0.4027 0.3180 0.6785 0.077 Uiso 1 calc R . .
C15 C 0.37988(11) 0.4695(2) 0.61071(7) 0.0665(5) Uani 1 d . . .
H15 H 0.3604 0.5631 0.6316 0.080 Uiso 1 calc R . .
C16 C 0.38348(10) 0.48119(19) 0.55191(7) 0.0599(5) Uani 1 d . . .
C17 C 0.41251(11) 0.3398(2) 0.52252(7) 0.0680(5) Uani 1 d . . .
H17 H 0.4169 0.3454 0.4830 0.082 Uiso 1 calc R . .
C18 C 0.43515(10) 0.1906(2) 0.54999(7) 0.0637(5) Uani 1 d . . .
H18 H 0.4528 0.0956 0.5290 0.076 Uiso 1 calc R . .
C19 C 0.35663(12) 0.6356(2) 0.52072(8) 0.0791(6) Uani 1 d . . .
H19 H 0.3707 0.6399 0.4823 0.095 Uiso 1 calc R . .
C20 C 0.31609(14) 0.7654(3) 0.54010(10) 0.1011(7) Uani 1 d . . .
H20A H 0.3003 0.7683 0.5782 0.121 Uiso 1 calc R . .
H20B H 0.3025 0.8565 0.5160 0.121 Uiso 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
N1 0.0625(10) 0.0545(8) 0.0595(8) 0.0049(7) 0.0015(7) 0.0067(7)
C1 0.0599(12) 0.0589(10) 0.0569(10) -0.0091(8) -0.0049(9) 0.0045(9)
C2 0.0664(13) 0.0775(12) 0.0681(11) -0.0103(9) 0.0012(10) 0.0025(10)
C3 0.0661(14) 0.1069(16) 0.0807(13) -0.0239(13) -0.0032(10) 0.0074(12)
C4 0.0758(16) 0.1118(17) 0.0875(15) -0.0260(14) -0.0172(13) 0.0336(13)
C5 0.0915(16) 0.0804(13) 0.0759(13) -0.0096(10) -0.0234(12) 0.0233(12)
C6 0.0705(13) 0.0560(10) 0.0599(10) -0.0101(8) -0.0163(9) 0.0088(9)
C7 0.0719(12) 0.0521(9) 0.0551(9) -0.0034(8) -0.0128(9) -0.0017(9)
C8 0.1001(16) 0.0589(11) 0.0636(11) 0.0078(9) -0.0158(11) -0.0045(10)
C9 0.1007(17) 0.0732(13) 0.0704(12) 0.0097(10) 0.0009(12) -0.0193(12)
C10 0.0803(14) 0.0800(12) 0.0697(11) -0.0009(10) 0.0043(10) -0.0155(11)
C11 0.0669(13) 0.0647(10) 0.0650(11) 0.0022(9) -0.0025(9) -0.0013(9)
C12 0.0620(12) 0.0514(9) 0.0535(9) -0.0008(8) -0.0053(9) -0.0029(8)
C13 0.0601(11) 0.0505(10) 0.0558(10) 0.0016(8) -0.0014(8) 0.0002(8)
C14 0.0811(13) 0.0575(11) 0.0545(9) -0.0029(8) -0.0017(9) 0.0022(9)
C15 0.0790(13) 0.0517(10) 0.0688(12) -0.0068(8) -0.0038(9) 0.0013(9)
C16 0.0587(11) 0.0539(10) 0.0670(11) 0.0057(9) -0.0073(8) -0.0043(8)
C17 0.0788(13) 0.0703(12) 0.0549(10) 0.0036(9) -0.0020(9) 0.0006(10)
C18 0.0747(12) 0.0604(11) 0.0560(10) -0.0038(8) 0.0005(9) 0.0068(9)
C19 0.0817(14) 0.0707(12) 0.0849(13) 0.0113(11) -0.0021(11) 0.0014(11)
C20 0.1083(18) 0.0852(15) 0.1096(17) 0.0167(13) -0.0002(13) 0.0195(13)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1 1.387(3) . ?
N1 C12 1.391(2) . ?
N1 C13 1.421(2) . ?
C1 C2 1.383(3) . ?
C1 C6 1.400(2) . ?
C2 C3 1.368(3) . ?
C3 C4 1.382(3) . ?
C4 C5 1.363(3) . ?
C5 C6 1.388(3) . ?
C6 C7 1.433(4) . ?
C7 C8 1.386(3) . ?
C7 C12 1.395(3) . ?
C8 C9 1.360(4) . ?
C9 C10 1.380(3) . ?
C10 C11 1.374(3) . ?
C11 C12 1.378(4) . ?
C13 C18 1.372(3) . ?
C13 C14 1.377(2) . ?
C14 C15 1.375(2) . ?
C15 C16 1.384(3) . ?
C16 C17 1.376(2) . ?
C16 C19 1.467(3) . ?
C17 C18 1.372(2) . ?
C19 C20 1.283(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C12 108.30(16) . . ?
C1 N1 C13 125.63(14) . . ?
C12 N1 C13 126.04(17) . . ?
C2 C1 N1 129.48(19) . . ?
C2 C1 C6 121.74(17) . . ?
N1 C1 C6 108.76(15) . . ?
C3 C2 C1 117.6(2) . . ?
C2 C3 C4 121.4(2) . . ?
C5 C4 C3 121.2(2) . . ?
C4 C5 C6 119.1(2) . . ?
C5 C6 C1 119.00(18) . . ?
C5 C6 C7 133.9(2) . . ?
C1 C6 C7 107.06(15) . . ?
C8 C7 C12 119.2(2) . . ?
C8 C7 C6 133.80(17) . . ?
C12 C7 C6 107.02(18) . . ?
C9 C8 C7 119.39(18) . . ?
C8 C9 C10 120.72(19) . . ?
C11 C10 C9 121.5(2) . . ?
C10 C11 C12 117.60(17) . . ?
C11 C12 N1 129.59(16) . . ?
C11 C12 C7 121.53(17) . . ?
N1 C12 C7 108.85(19) . . ?
C18 C13 C14 119.40(15) . . ?
C18 C13 N1 120.28(14) . . ?
C14 C13 N1 120.32(16) . . ?
C15 C14 C13 119.88(17) . . ?
C14 C15 C16 121.41(16) . . ?
C17 C16 C15 117.49(15) . . ?
C17 C16 C19 119.93(18) . . ?
C15 C16 C19 122.57(17) . . ?
C18 C17 C16 121.66(17) . . ?
C17 C18 C13 120.12(15) . . ?
C20 C19 C16 127.8(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 C2 -178.16(15) . . . . ?
C13 N1 C1 C2 0.0(3) . . . . ?
C12 N1 C1 C6 -0.04(16) . . . . ?
C13 N1 C1 C6 178.10(13) . . . . ?
N1 C1 C2 C3 179.70(15) . . . . ?
C6 C1 C2 C3 1.8(2) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 -1.2(3) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C4 C5 C6 C1 0.7(2) . . . . ?
C4 C5 C6 C7 -178.87(17) . . . . ?
C2 C1 C6 C5 -2.1(2) . . . . ?
N1 C1 C6 C5 179.61(14) . . . . ?
C2 C1 C6 C7 177.57(14) . . . . ?
N1 C1 C6 C7 -0.72(16) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C1 C6 C7 C8 -179.26(16) . . . . ?
C5 C6 C7 C12 -179.19(17) . . . . ?
C1 C6 C7 C12 1.20(16) . . . . ?
C12 C7 C8 C9 1.5(2) . . . . ?
C6 C7 C8 C9 -178.02(17) . . . . ?
C7 C8 C9 C10 0.6(3) . . . . ?
C8 C9 C10 C11 -1.4(3) . . . . ?
C9 C10 C11 C12 0.2(3) . . . . ?
C10 C11 C12 N1 179.57(15) . . . . ?
C10 C11 C12 C7 1.9(2) . . . . ?
C1 N1 C12 C11 -177.07(15) . . . . ?
C13 N1 C12 C11 4.8(2) . . . . ?
C1 N1 C12 C7 0.81(16) . . . . ?
C13 N1 C12 C7 -177.32(13) . . . . ?
C8 C7 C12 C11 -2.8(2) . . . . ?
C6 C7 C12 C11 176.85(14) . . . . ?
C8 C7 C12 N1 179.14(13) . . . . ?
C6 C7 C12 N1 -1.24(16) . . . . ?
C1 N1 C13 C18 53.9(2) . . . . ?
C12 N1 C13 C18 -128.24(17) . . . . ?
C1 N1 C13 C14 -125.03(17) . . . . ?
C12 N1 C13 C14 52.8(2) . . . . ?
C18 C13 C14 C15 0.9(2) . . . . ?
N1 C13 C14 C15 179.89(15) . . . . ?
C13 C14 C15 C16 -1.4(3) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C14 C15 C16 C19 179.17(16) . . . . ?
C15 C16 C17 C18 1.6(2) . . . . ?
C19 C16 C17 C18 -177.43(16) . . . . ?
C16 C17 C18 C13 -2.2(3) . . . . ?
C14 C13 C18 C17 0.8(2) . . . . ?
N1 C13 C18 C17 -178.15(15) . . . . ?
C17 C16 C19 C20 167.6(2) . . . . ?
C15 C16 C19 C20 -11.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.584
_diffrn_reflns_theta_full        26.30
_diffrn_measured_fraction_theta_full 0.584
_refine_diff_density_max         0.093
_refine_diff_density_min         -0.129
_refine_diff_density_rms         0.027

# Attachment '1gs979.txt'

data_s979
_database_code_depnum_ccdc_archive 'CCDC 610511'
#------------------------------------------------------------------------------
_audit_creation_date             19101-03-07
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             
;
?
;

_publ_section_abstract           
;
ENTER ABSTRACT
;

_publ_section_exptl_prep         
;
ENTER EXPERIMENTAL SECTION
;

_publ_section_exptl_refinement   
;
The data were collected using the RAXIS in 150 x 1 degree
phi oscillations of 20 minutes per exposure. The structure was solved by
direct methods.
H atoms were included in calculated positions.
The non-H atoms were refined anisotropically.
The absolute configuration could not be determined.

;

_publ_section_comment            
;
ENTER TEXT
;

_publ_section_references         
;
ENTER OTHER REFERENCES

Molecular Structure Corporation. (1995). teXsan.
Single Crystal Structure Analysis Software. Version 1.7.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.

Altomare, A., Cascarano, M.,
Giacovazzo, C., Guagliardi, A. (1993).
J. Appl. Cryst., 26, 343.
;

_publ_section_acknowledgements   
;
ENTER ACKNOWLEDGEMENTS
;

_publ_section_table_legends      
;
ENTER TABLE LEGENDS
;

_publ_section_figure_captions    
;
ENTER FIGURE CAPTIONS
;

_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H31 N3'
_chemical_formula_weight         601.72

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  ?

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

_cell_length_a                   8.616(10)
_cell_length_b                   9.832(10)
_cell_length_c                   38.95(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3299(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31171
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      24.91

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'image plate'
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '150 x 1 degree phi scans'

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            31171
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         24.91
_reflns_number_total             5080
_reflns_number_gt                4399
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'MSC RAXIS11 Control'
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_structure_solution    
;
SHELXS86 (Sheldrick, 1985)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'teXsan (MSC, 1995)'

_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 w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+0.1023P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(3)
_refine_ls_number_reflns         5080
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0928
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.93533(19) 0.11178(18) 0.08774(4) 0.0620(4) Uani 1 d . . .
N2 N 1.50107(18) -0.16564(17) 0.10675(4) 0.0620(4) Uani 1 d . . .
N3 N 0.64133(18) 0.39883(17) 0.19548(4) 0.0582(4) Uani 1 d . . .
C1 C 0.8693(2) 0.10702(19) 0.05430(4) 0.0563(4) Uani 1 d . . .
C2 C 0.7102(2) 0.1021(2) 0.04963(5) 0.0680(5) Uani 1 d . . .
H2 H 0.6444 0.1029 0.0686 0.082 Uiso 1 calc R . .
C3 C 0.6481(3) 0.0960(2) 0.01661(6) 0.0784(6) Uani 1 d . . .
H3 H 0.5409 0.0947 0.0140 0.094 Uiso 1 calc R . .
C4 C 0.7408(3) 0.0918(2) -0.01241(5) 0.0775(6) Uani 1 d . . .
C5 C 0.9004(3) 0.0979(2) -0.00745(5) 0.0795(7) Uani 1 d . . .
H5 H 0.9661 0.0960 -0.0264 0.095 Uiso 1 calc R . .
C6 C 0.9641(3) 0.1068(2) 0.02549(5) 0.0716(6) Uani 1 d . . .
H6 H 1.0712 0.1127 0.0281 0.086 Uiso 1 calc R . .
C7 C 0.6717(4) 0.0795(3) -0.04691(7) 0.1044(9) Uani 1 d . . .
H7 H 0.5655 0.0957 -0.0483 0.125 Uiso 1 calc R . .
C8 C 0.7393(6) 0.0494(3) -0.07526(7) 0.1373(15) Uani 1 d . . .
H8A H 0.8454 0.0322 -0.0756 0.165 Uiso 1 calc R . .
H8B H 0.6822 0.0449 -0.0955 0.165 Uiso 1 calc R . .
C9 C 1.0759(2) 0.0408(2) 0.09425(4) 0.0566(5) Uani 1 d . . .
C10 C 1.1991(2) 0.1028(2) 0.11135(5) 0.0611(5) Uani 1 d . . .
H10 H 1.1872 0.1903 0.1200 0.073 Uiso 1 calc R . .
C11 C 1.3388(2) 0.0359(2) 0.11563(5) 0.0603(5) Uani 1 d . . .
H11 H 1.4208 0.0792 0.1267 0.072 Uiso 1 calc R . .
C12 C 1.3567(2) -0.0967(2) 0.10336(5) 0.0589(5) Uani 1 d . . .
C13 C 1.2325(2) -0.1595(2) 0.08708(5) 0.0670(5) Uani 1 d . . .
H13 H 1.2426 -0.2485 0.0793 0.080 Uiso 1 calc R . .
C14 C 1.0942(2) -0.0912(2) 0.08228(5) 0.0642(5) Uani 1 d . . .
H14 H 1.0127 -0.1340 0.0709 0.077 Uiso 1 calc R . .
C15 C 1.5812(2) -0.2297(2) 0.07984(5) 0.0590(5) Uani 1 d . . .
C16 C 1.5424(3) -0.2422(2) 0.04513(5) 0.0753(6) Uani 1 d . . .
H16 H 1.4500 -0.2070 0.0366 0.090 Uiso 1 calc R . .
C17 C 1.6468(3) -0.3090(3) 0.02392(6) 0.0852(7) Uani 1 d . . .
H17 H 1.6248 -0.3169 0.0006 0.102 Uiso 1 calc R . .
C18 C 1.7828(3) -0.3640(2) 0.03657(6) 0.0811(6) Uani 1 d . . .
H18 H 1.8490 -0.4106 0.0218 0.097 Uiso 1 calc R . .
C19 C 1.8221(3) -0.3511(2) 0.07071(6) 0.0712(6) Uani 1 d . . .
H19 H 1.9144 -0.3879 0.0789 0.085 Uiso 1 calc R . .
C20 C 1.7216(2) -0.28172(18) 0.09295(5) 0.0579(5) Uani 1 d . . .
C21 C 1.7266(2) -0.24748(19) 0.12923(5) 0.0570(4) Uani 1 d . . .
C22 C 1.8330(2) -0.2724(2) 0.15569(6) 0.0693(5) Uani 1 d . . .
H22 H 1.9254 -0.3178 0.1511 0.083 Uiso 1 calc R . .
C23 C 1.7996(3) -0.2288(2) 0.18852(6) 0.0726(6) Uani 1 d . . .
H23 H 1.8699 -0.2451 0.2062 0.087 Uiso 1 calc R . .
C24 C 1.6622(3) -0.1609(2) 0.19544(5) 0.0714(6) Uani 1 d . . .
H24 H 1.6420 -0.1327 0.2178 0.086 Uiso 1 calc R . .
C25 C 1.5547(2) -0.1339(2) 0.17016(5) 0.0648(5) Uani 1 d . . .
H25 H 1.4625 -0.0888 0.1751 0.078 Uiso 1 calc R . .
C26 C 1.5895(2) -0.17717(19) 0.13684(4) 0.0559(4) Uani 1 d . . .
C27 C 0.8607(2) 0.18342(19) 0.11513(4) 0.0531(4) Uani 1 d . . .
C28 C 0.8557(2) 0.12935(19) 0.14801(4) 0.0599(5) Uani 1 d . . .
H28 H 0.9016 0.0455 0.1524 0.072 Uiso 1 calc R . .
C29 C 0.7829(2) 0.19923(19) 0.17432(4) 0.0606(5) Uani 1 d . . .
H29 H 0.7795 0.1616 0.1962 0.073 Uiso 1 calc R . .
C30 C 0.7149(2) 0.32505(19) 0.16831(4) 0.0544(4) Uani 1 d . . .
C31 C 0.7182(2) 0.3784(2) 0.13518(4) 0.0595(5) Uani 1 d . . .
H31 H 0.6714 0.4618 0.1308 0.071 Uiso 1 calc R . .
C32 C 0.7904(2) 0.30852(19) 0.10880(4) 0.0585(5) Uani 1 d . . .
H32 H 0.7920 0.3452 0.0868 0.070 Uiso 1 calc R . .
C33 C 0.7154(2) 0.45289(19) 0.22472(4) 0.0555(4) Uani 1 d . . .
C34 C 0.8660(2) 0.4322(2) 0.23644(5) 0.0689(5) Uani 1 d . . .
H34 H 0.9343 0.3744 0.2251 0.083 Uiso 1 calc R . .
C35 C 0.9095(3) 0.5017(3) 0.26585(6) 0.0838(7) Uani 1 d . . .
H35 H 1.0094 0.4896 0.2744 0.101 Uiso 1 calc R . .
C36 C 0.8094(3) 0.5888(3) 0.28301(6) 0.0878(7) Uani 1 d . . .
H36 H 0.8430 0.6336 0.3027 0.105 Uiso 1 calc R . .
C37 C 0.6609(3) 0.6094(2) 0.27121(5) 0.0753(6) Uani 1 d . . .
H37 H 0.5938 0.6678 0.2827 0.090 Uiso 1 calc R . .
C38 C 0.6122(2) 0.5412(2) 0.24156(4) 0.0595(5) Uani 1 d . . .
C39 C 0.4712(2) 0.5441(2) 0.22179(4) 0.0618(5) Uani 1 d . . .
C40 C 0.3314(3) 0.6131(3) 0.22488(6) 0.0843(7) Uani 1 d . . .
H40 H 0.3153 0.6737 0.2429 0.101 Uiso 1 calc R . .
C41 C 0.2171(3) 0.5906(4) 0.20095(7) 0.1096(10) Uani 1 d . . .
H41 H 0.1235 0.6370 0.2029 0.132 Uiso 1 calc R . .
C42 C 0.2383(3) 0.5001(4) 0.17400(7) 0.1090(10) Uani 1 d . . .
H42 H 0.1573 0.4851 0.1587 0.131 Uiso 1 calc R . .
C43 C 0.3761(3) 0.4323(3) 0.16946(6) 0.0843(7) Uani 1 d . . .
H43 H 0.3911 0.3734 0.1511 0.101 Uiso 1 calc R . .
C44 C 0.4926(2) 0.4556(2) 0.19358(5) 0.0606(5) Uani 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
N1 0.0572(9) 0.0769(11) 0.0518(8) -0.0085(8) -0.0027(7) 0.0203(8)
N2 0.0577(9) 0.0674(11) 0.0608(9) -0.0060(8) -0.0016(7) 0.0153(8)
N3 0.0552(9) 0.0665(10) 0.0530(8) -0.0088(7) -0.0004(6) 0.0092(8)
C1 0.0614(11) 0.0572(11) 0.0503(9) -0.0040(8) -0.0027(8) 0.0068(9)
C2 0.0625(12) 0.0754(13) 0.0660(12) -0.0043(10) -0.0044(10) 0.0015(11)
C3 0.0755(14) 0.0783(15) 0.0813(15) -0.0024(12) -0.0237(12) -0.0024(12)
C4 0.1054(19) 0.0619(13) 0.0651(13) -0.0001(10) -0.0217(13) -0.0011(13)
C5 0.108(2) 0.0759(15) 0.0545(12) -0.0040(11) 0.0063(11) 0.0038(14)
C6 0.0728(13) 0.0822(15) 0.0597(11) -0.0063(10) 0.0042(10) 0.0049(12)
C7 0.161(3) 0.0740(16) 0.0783(17) -0.0019(13) -0.0420(17) -0.0096(17)
C8 0.234(4) 0.112(2) 0.0657(16) -0.0006(16) -0.029(2) -0.039(3)
C9 0.0544(11) 0.0600(11) 0.0555(10) -0.0048(9) -0.0015(8) 0.0097(9)
C10 0.0647(12) 0.0542(11) 0.0645(11) -0.0108(9) -0.0062(9) 0.0093(10)
C11 0.0595(12) 0.0562(11) 0.0652(11) -0.0080(9) -0.0060(9) 0.0049(9)
C12 0.0550(11) 0.0583(11) 0.0634(11) -0.0014(9) -0.0025(9) 0.0083(9)
C13 0.0640(12) 0.0541(11) 0.0829(13) -0.0111(10) -0.0064(10) 0.0058(10)
C14 0.0526(11) 0.0596(12) 0.0804(13) -0.0126(10) -0.0079(9) 0.0022(10)
C15 0.0638(12) 0.0534(11) 0.0597(11) -0.0040(9) 0.0030(9) 0.0051(9)
C16 0.0870(15) 0.0726(14) 0.0664(13) -0.0059(11) -0.0068(11) 0.0099(12)
C17 0.111(2) 0.0827(16) 0.0619(12) -0.0115(11) 0.0082(13) 0.0034(16)
C18 0.0919(16) 0.0727(14) 0.0786(14) -0.0116(11) 0.0227(13) 0.0071(14)
C19 0.0693(13) 0.0596(12) 0.0847(14) -0.0052(10) 0.0157(10) 0.0051(10)
C20 0.0557(11) 0.0461(10) 0.0719(12) -0.0002(8) 0.0057(9) 0.0005(9)
C21 0.0556(11) 0.0503(10) 0.0651(11) 0.0005(8) -0.0001(9) 0.0024(9)
C22 0.0594(12) 0.0651(13) 0.0834(14) -0.0001(10) -0.0079(10) 0.0122(10)
C23 0.0770(15) 0.0691(13) 0.0718(13) 0.0049(10) -0.0162(11) 0.0088(12)
C24 0.0847(15) 0.0698(13) 0.0597(11) 0.0010(10) -0.0028(10) 0.0034(12)
C25 0.0654(12) 0.0659(12) 0.0632(11) 0.0009(10) 0.0042(9) 0.0104(10)
C26 0.0556(11) 0.0531(11) 0.0589(10) 0.0018(8) 0.0001(8) 0.0053(9)
C27 0.0524(10) 0.0548(10) 0.0521(9) -0.0025(8) 0.0001(8) 0.0063(9)
C28 0.0713(13) 0.0526(11) 0.0559(10) 0.0034(8) -0.0022(9) 0.0156(10)
C29 0.0743(12) 0.0590(11) 0.0485(9) 0.0042(8) 0.0012(9) 0.0124(10)
C30 0.0549(10) 0.0573(10) 0.0510(9) -0.0044(8) 0.0009(8) 0.0072(9)
C31 0.0646(11) 0.0526(10) 0.0614(11) 0.0043(8) 0.0029(9) 0.0092(10)
C32 0.0663(11) 0.0601(11) 0.0492(9) 0.0063(8) 0.0032(8) 0.0090(10)
C33 0.0605(11) 0.0580(11) 0.0479(9) 0.0020(8) -0.0015(8) -0.0017(9)
C34 0.0658(12) 0.0718(13) 0.0691(12) -0.0007(10) -0.0044(10) 0.0036(11)
C35 0.0804(15) 0.0944(18) 0.0767(14) 0.0002(13) -0.0201(12) -0.0078(14)
C36 0.1031(18) 0.0967(18) 0.0637(13) -0.0141(12) -0.0105(13) -0.0060(16)
C37 0.0916(16) 0.0799(14) 0.0542(11) -0.0089(10) 0.0058(10) 0.0031(13)
C38 0.0706(12) 0.0620(11) 0.0461(9) 0.0029(9) 0.0088(9) 0.0002(10)
C39 0.0646(12) 0.0710(13) 0.0496(10) 0.0027(9) 0.0113(9) 0.0101(10)
C40 0.0824(15) 0.1039(17) 0.0667(12) -0.0055(12) 0.0170(11) 0.0310(14)
C41 0.0718(16) 0.173(3) 0.0840(16) -0.0057(18) 0.0033(13) 0.0525(19)
C42 0.0658(15) 0.180(3) 0.0817(15) -0.0190(18) -0.0097(13) 0.0362(18)
C43 0.0662(13) 0.121(2) 0.0653(12) -0.0176(13) -0.0053(10) 0.0155(14)
C44 0.0562(11) 0.0714(12) 0.0541(10) -0.0016(9) 0.0034(8) 0.0101(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 C1 1.422(3) . ?
N1 C9 1.421(3) . ?
N1 C27 1.431(3) . ?
N2 C26 1.403(3) . ?
N2 C15 1.404(3) . ?
N2 C12 1.423(3) . ?
N3 C44 1.399(3) . ?
N3 C33 1.409(3) . ?
N3 C30 1.431(3) . ?
C1 C2 1.384(3) . ?
C1 C6 1.388(3) . ?
C2 C3 1.394(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(4) . ?
C4 C7 1.475(4) . ?
C5 C6 1.398(4) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.283(5) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9300 . ?
C8 H8B 0.9300 . ?
C9 C14 1.389(3) . ?
C9 C10 1.393(3) . ?
C10 C11 1.381(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.397(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(3) . ?
C13 C14 1.380(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.398(4) . ?
C15 C20 1.410(3) . ?
C16 C17 1.387(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.382(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.378(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.402(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.453(4) . ?
C21 C22 1.401(3) . ?
C21 C26 1.400(3) . ?
C22 C23 1.379(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.386(3) . ?
C23 H23 0.9300 . ?
C24 C25 1.378(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.398(3) . ?
C25 H25 0.9300 . ?
C27 C28 1.388(3) . ?
C27 C32 1.393(3) . ?
C28 C29 1.384(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.389(3) . ?
C29 H29 0.9300 . ?
C30 C31 1.393(3) . ?
C31 C32 1.384(3) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C34 1.391(3) . ?
C33 C38 1.405(3) . ?
C34 C35 1.386(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.387(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.374(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.400(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.439(3) . ?
C39 C40 1.389(3) . ?
C39 C44 1.414(3) . ?
C40 C41 1.373(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.388(4) . ?
C41 H41 0.9300 . ?
C42 C43 1.373(4) . ?
C42 H42 0.9300 . ?
C43 C44 1.393(3) . ?
C43 H43 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C9 119.25(15) . . ?
C1 N1 C27 121.28(17) . . ?
C9 N1 C27 119.44(16) . . ?
C26 N2 C15 108.69(18) . . ?
C26 N2 C12 126.24(15) . . ?
C15 N2 C12 125.04(17) . . ?
C44 N3 C33 107.88(15) . . ?
C44 N3 C30 124.64(16) . . ?
C33 N3 C30 126.03(17) . . ?
C2 C1 C6 118.46(19) . . ?
C2 C1 N1 121.20(17) . . ?
C6 C1 N1 120.3(2) . . ?
C1 C2 C3 120.2(2) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C4 C3 C2 122.2(2) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 117.1(2) . . ?
C3 C4 C7 120.9(3) . . ?
C5 C4 C7 122.0(3) . . ?
C4 C5 C6 121.3(2) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 120.7(2) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C4 128.3(4) . . ?
C8 C7 H7 115.9 . . ?
C4 C7 H7 115.9 . . ?
C7 C8 H8A 120.0 . . ?
C7 C8 H8B 120.0 . . ?
H8A C8 H8B 120.0 . . ?
C14 C9 C10 118.86(18) . . ?
C14 C9 N1 119.74(18) . . ?
C10 C9 N1 121.36(18) . . ?
C11 C10 C9 120.90(18) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 119.93(19) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 119.09(19) . . ?
C13 C12 N2 120.27(18) . . ?
C11 C12 N2 120.62(18) . . ?
C14 C13 C12 120.69(19) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C9 120.50(19) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
C16 C15 N2 130.1(2) . . ?
C16 C15 C20 121.55(18) . . ?
N2 C15 C20 108.32(18) . . ?
C17 C16 C15 117.6(2) . . ?
C17 C16 H16 121.2 . . ?
C15 C16 H16 121.2 . . ?
C18 C17 C16 121.5(2) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C19 C18 C17 121.1(2) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C18 C19 C20 119.3(2) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C19 C20 C15 118.9(2) . . ?
C19 C20 C21 134.05(19) . . ?
C15 C20 C21 107.06(17) . . ?
C22 C21 C26 118.87(19) . . ?
C22 C21 C20 133.94(19) . . ?
C26 C21 C20 107.18(16) . . ?
C23 C22 C21 119.4(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C22 C23 C24 120.56(19) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 121.9(2) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C26 117.4(2) . . ?
C24 C25 H25 121.3 . . ?
C26 C25 H25 121.3 . . ?
C25 C26 N2 129.36(19) . . ?
C25 C26 C21 121.86(17) . . ?
N2 C26 C21 108.74(17) . . ?
C28 C27 C32 119.21(16) . . ?
C28 C27 N1 120.91(18) . . ?
C32 C27 N1 119.87(17) . . ?
C29 C28 C27 120.50(19) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.57(18) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 118.88(16) . . ?
C29 C30 N3 120.91(17) . . ?
C31 C30 N3 120.21(18) . . ?
C32 C31 C30 120.67(19) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C27 120.15(18) . . ?
C31 C32 H32 119.9 . . ?
C27 C32 H32 119.9 . . ?
C34 C33 C38 121.83(19) . . ?
C34 C33 N3 129.23(18) . . ?
C38 C33 N3 108.91(18) . . ?
C35 C34 C33 116.9(2) . . ?
C35 C34 H34 121.6 . . ?
C33 C34 H34 121.6 . . ?
C34 C35 C36 122.3(2) . . ?
C34 C35 H35 118.9 . . ?
C36 C35 H35 118.9 . . ?
C37 C36 C35 120.6(2) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C36 C37 C38 118.9(2) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C37 C38 C33 119.5(2) . . ?
C37 C38 C39 133.24(19) . . ?
C33 C38 C39 107.23(18) . . ?
C40 C39 C44 118.79(19) . . ?
C40 C39 C38 134.1(2) . . ?
C44 C39 C38 107.10(18) . . ?
C41 C40 C39 118.9(2) . . ?
C41 C40 H40 120.5 . . ?
C39 C40 H40 120.5 . . ?
C40 C41 C42 121.5(2) . . ?
C40 C41 H41 119.2 . . ?
C42 C41 H41 119.2 . . ?
C43 C42 C41 121.5(2) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C44 117.2(2) . . ?
C42 C43 H43 121.4 . . ?
C44 C43 H43 121.4 . . ?
C43 C44 N3 129.04(19) . . ?
C43 C44 C39 122.1(2) . . ?
N3 C44 C39 108.87(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C1 C2 143.3(2) . . . . ?
C27 N1 C1 C2 -35.0(3) . . . . ?
C9 N1 C1 C6 -36.6(3) . . . . ?
C27 N1 C1 C6 145.2(2) . . . . ?
C6 C1 C2 C3 0.5(3) . . . . ?
N1 C1 C2 C3 -179.30(19) . . . . ?
C1 C2 C3 C4 1.3(4) . . . . ?
C2 C3 C4 C5 -1.8(4) . . . . ?
C2 C3 C4 C7 177.4(2) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C7 C4 C5 C6 -178.7(2) . . . . ?
C2 C1 C6 C5 -1.8(3) . . . . ?
N1 C1 C6 C5 178.0(2) . . . . ?
C4 C5 C6 C1 1.3(4) . . . . ?
C3 C4 C7 C8 -165.9(3) . . . . ?
C5 C4 C7 C8 13.3(4) . . . . ?
C1 N1 C9 C14 -45.1(3) . . . . ?
C27 N1 C9 C14 133.2(2) . . . . ?
C1 N1 C9 C10 132.5(2) . . . . ?
C27 N1 C9 C10 -49.3(3) . . . . ?
C14 C9 C10 C11 1.7(3) . . . . ?
N1 C9 C10 C11 -175.85(17) . . . . ?
C9 C10 C11 C12 -1.4(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C10 C11 C12 N2 178.32(17) . . . . ?
C26 N2 C12 C13 -132.0(2) . . . . ?
C15 N2 C12 C13 50.4(3) . . . . ?
C26 N2 C12 C11 49.4(3) . . . . ?
C15 N2 C12 C11 -128.2(2) . . . . ?
C11 C12 C13 C14 1.6(3) . . . . ?
N2 C12 C13 C14 -177.03(18) . . . . ?
C12 C13 C14 C9 -1.2(3) . . . . ?
C10 C9 C14 C13 -0.4(3) . . . . ?
N1 C9 C14 C13 177.19(18) . . . . ?
C26 N2 C15 C16 -178.3(2) . . . . ?
C12 N2 C15 C16 -0.4(3) . . . . ?
C26 N2 C15 C20 -0.2(2) . . . . ?
C12 N2 C15 C20 177.77(17) . . . . ?
N2 C15 C16 C17 178.4(2) . . . . ?
C20 C15 C16 C17 0.5(3) . . . . ?
C15 C16 C17 C18 1.4(4) . . . . ?
C16 C17 C18 C19 -1.9(4) . . . . ?
C17 C18 C19 C20 0.5(3) . . . . ?
C18 C19 C20 C15 1.3(3) . . . . ?
C18 C19 C20 C21 -178.7(2) . . . . ?
C16 C15 C20 C19 -1.9(3) . . . . ?
N2 C15 C20 C19 179.81(17) . . . . ?
C16 C15 C20 C21 178.2(2) . . . . ?
N2 C15 C20 C21 -0.1(2) . . . . ?
C19 C20 C21 C22 -0.9(4) . . . . ?
C15 C20 C21 C22 179.0(2) . . . . ?
C19 C20 C21 C26 -179.5(2) . . . . ?
C15 C20 C21 C26 0.4(2) . . . . ?
C26 C21 C22 C23 0.8(3) . . . . ?
C20 C21 C22 C23 -177.7(2) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C22 C23 C24 C25 -0.2(3) . . . . ?
C23 C24 C25 C26 -0.4(3) . . . . ?
C24 C25 C26 N2 178.7(2) . . . . ?
C24 C25 C26 C21 1.2(3) . . . . ?
C15 N2 C26 C25 -177.3(2) . . . . ?
C12 N2 C26 C25 4.8(3) . . . . ?
C15 N2 C26 C21 0.4(2) . . . . ?
C12 N2 C26 C21 -177.49(17) . . . . ?
C22 C21 C26 C25 -1.4(3) . . . . ?
C20 C21 C26 C25 177.43(18) . . . . ?
C22 C21 C26 N2 -179.39(18) . . . . ?
C20 C21 C26 N2 -0.5(2) . . . . ?
C1 N1 C27 C28 139.0(2) . . . . ?
C9 N1 C27 C28 -39.2(3) . . . . ?
C1 N1 C27 C32 -40.2(3) . . . . ?
C9 N1 C27 C32 141.51(19) . . . . ?
C32 C27 C28 C29 -0.6(3) . . . . ?
N1 C27 C28 C29 -179.82(18) . . . . ?
C27 C28 C29 C30 -0.5(3) . . . . ?
C28 C29 C30 C31 1.4(3) . . . . ?
C28 C29 C30 N3 -179.12(18) . . . . ?
C44 N3 C30 C29 -130.5(2) . . . . ?
C33 N3 C30 C29 65.0(3) . . . . ?
C44 N3 C30 C31 49.0(3) . . . . ?
C33 N3 C30 C31 -115.5(2) . . . . ?
C29 C30 C31 C32 -1.2(3) . . . . ?
N3 C30 C31 C32 179.35(18) . . . . ?
C30 C31 C32 C27 0.1(3) . . . . ?
C28 C27 C32 C31 0.8(3) . . . . ?
N1 C27 C32 C31 -179.94(18) . . . . ?
C44 N3 C33 C34 -176.7(2) . . . . ?
C30 N3 C33 C34 -10.1(3) . . . . ?
C44 N3 C33 C38 1.2(2) . . . . ?
C30 N3 C33 C38 167.91(17) . . . . ?
C38 C33 C34 C35 0.7(3) . . . . ?
N3 C33 C34 C35 178.5(2) . . . . ?
C33 C34 C35 C36 -0.3(3) . . . . ?
C34 C35 C36 C37 0.0(4) . . . . ?
C35 C36 C37 C38 0.0(4) . . . . ?
C36 C37 C38 C33 0.4(3) . . . . ?
C36 C37 C38 C39 -176.6(2) . . . . ?
C34 C33 C38 C37 -0.8(3) . . . . ?
N3 C33 C38 C37 -178.91(17) . . . . ?
C34 C33 C38 C39 176.97(18) . . . . ?
N3 C33 C38 C39 -1.2(2) . . . . ?
C37 C38 C39 C40 -1.1(4) . . . . ?
C33 C38 C39 C40 -178.4(2) . . . . ?
C37 C38 C39 C44 178.0(2) . . . . ?
C33 C38 C39 C44 0.7(2) . . . . ?
C44 C39 C40 C41 1.7(4) . . . . ?
C38 C39 C40 C41 -179.4(2) . . . . ?
C39 C40 C41 C42 0.3(5) . . . . ?
C40 C41 C42 C43 -2.0(5) . . . . ?
C41 C42 C43 C44 1.6(5) . . . . ?
C42 C43 C44 N3 178.7(2) . . . . ?
C42 C43 C44 C39 0.5(4) . . . . ?
C33 N3 C44 C43 -179.3(2) . . . . ?
C30 N3 C44 C43 13.8(3) . . . . ?
C33 N3 C44 C39 -0.8(2) . . . . ?
C30 N3 C44 C39 -167.71(18) . . . . ?
C40 C39 C44 C43 -2.1(3) . . . . ?
C38 C39 C44 C43 178.7(2) . . . . ?
C40 C39 C44 N3 179.31(19) . . . . ?
C38 C39 C44 N3 0.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.929
_diffrn_reflns_theta_full        24.91
_diffrn_measured_fraction_theta_full 0.929
_refine_diff_density_max         0.099
_refine_diff_density_min         -0.121
_refine_diff_density_rms         0.026

# Attachment '1hs1033m.txt'

data_s1033m
_database_code_depnum_ccdc_archive 'CCDC 610512'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;

_publ_section_abstract           
;
ENTER ABSTRACT
;

_publ_section_exptl_prep         
;
ENTER EXPERIMENTAL SECTION
;

_publ_section_exptl_refinement   
;
The crystals were small and weakly diffracting, so that
the number of observed data was rather low.
The structure was solved by direct methods.
H atoms were included in calculated positions.
The non-H atoms were refined anisotropically.

;

_publ_section_comment            
;
ENTER TEXT
;

_publ_section_references         
;
ENTER OTHER REFERENCES

;

_publ_section_acknowledgements   
;
ENTER ACKNOWLEDGEMENTS
;

_publ_section_table_legends      
;
ENTER TABLE LEGENDS
;

_publ_section_figure_captions    
;
ENTER FIGURE CAPTIONS
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H31 N3 S2'
_chemical_formula_weight         665.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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                   10.985(4)
_cell_length_b                   24.813(8)
_cell_length_c                   13.194(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.149(7)
_cell_angle_gamma                90.00
_cell_volume                     3376.3(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    631
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      16.27

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
The crystals were small and weakly diffracting, so that
the number of observed data were rather low.

;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         '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_decay_%        ?
_diffrn_reflns_number            20836
_diffrn_reflns_av_R_equivalents  0.2716
_diffrn_reflns_av_sigmaI/netI    0.4784
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         28.24
_reflns_number_total             7817
_reflns_number_gt                1479
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_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^)+(0.0000P)^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         7817
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3273
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   0.611
_refine_ls_restrained_S_all      0.611
_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 -0.11990(19) 0.23774(7) 0.26201(13) 0.0768(6) Uani 1 1 d . . .
S2 S 0.6456(2) -0.04755(7) 1.32902(14) 0.0848(7) Uani 1 1 d . . .
N1 N 0.4748(4) 0.23323(18) 0.9077(3) 0.0449(13) Uani 1 1 d . . .
N2 N 0.0909(5) 0.2372(2) 0.4922(4) 0.0562(15) Uani 1 1 d . . .
N3 N 0.5912(6) 0.0480(2) 1.1718(4) 0.0553(15) Uani 1 1 d . . .
C1 C 0.3746(6) 0.2324(2) 0.8030(4) 0.0433(16) Uani 1 1 d . . .
C2 C 0.4035(6) 0.2494(2) 0.7152(4) 0.062(2) Uani 1 1 d . . .
H2 H 0.4883 0.2593 0.7242 0.075 Uiso 1 1 calc R . .
C3 C 0.3109(7) 0.2522(3) 0.6141(4) 0.071(2) Uani 1 1 d . . .
H3 H 0.3316 0.2653 0.5560 0.086 Uiso 1 1 calc R . .
C4 C 0.1860(6) 0.2351(2) 0.5999(4) 0.0511(17) Uani 1 1 d . . .
C5 C 0.1563(6) 0.2176(2) 0.6869(4) 0.0504(17) Uani 1 1 d . . .
H5 H 0.0724 0.2063 0.6773 0.060 Uiso 1 1 calc R . .
C6 C 0.2496(6) 0.2165(2) 0.7890(4) 0.0449(16) Uani 1 1 d . . .
H6 H 0.2281 0.2051 0.8478 0.054 Uiso 1 1 calc R . .
C7 C 0.0052(6) 0.2819(3) 0.4634(5) 0.0519(18) Uani 1 1 d . . .
C8 C 0.0205(6) 0.3235(3) 0.5357(5) 0.063(2) Uani 1 1 d . . .
H8 H 0.0852 0.3219 0.6032 0.076 Uiso 1 1 calc R . .
C9 C -0.0625(8) 0.3686(3) 0.5067(5) 0.083(2) Uani 1 1 d . . .
H9 H -0.0516 0.3966 0.5558 0.100 Uiso 1 1 calc R . .
C10 C -0.1578(7) 0.3721(3) 0.4086(5) 0.079(2) Uani 1 1 d . . .
H10 H -0.2113 0.4022 0.3912 0.095 Uiso 1 1 calc R . .
C11 C -0.1747(7) 0.3321(3) 0.3375(5) 0.065(2) Uani 1 1 d . . .
H11 H -0.2400 0.3343 0.2703 0.079 Uiso 1 1 calc R . .
C12 C -0.0928(6) 0.2865(3) 0.3646(4) 0.0486(17) Uani 1 1 d . . .
C13 C -0.0272(6) 0.1840(2) 0.3318(4) 0.0469(17) Uani 1 1 d . . .
C14 C -0.0495(6) 0.1345(3) 0.2797(5) 0.067(2) Uani 1 1 d . . .
H14 H -0.1188 0.1310 0.2151 0.080 Uiso 1 1 calc R . .
C15 C 0.0291(7) 0.0897(3) 0.3213(5) 0.075(2) Uani 1 1 d . . .
H15 H 0.0142 0.0569 0.2853 0.091 Uiso 1 1 calc R . .
C16 C 0.1292(6) 0.0962(3) 0.4176(5) 0.072(2) Uani 1 1 d . . .
H16 H 0.1842 0.0673 0.4462 0.086 Uiso 1 1 calc R . .
C17 C 0.1505(6) 0.1443(3) 0.4729(4) 0.0552(18) Uani 1 1 d . . .
H17 H 0.2191 0.1474 0.5380 0.066 Uiso 1 1 calc R . .
C18 C 0.0714(6) 0.1877(3) 0.4328(4) 0.0511(18) Uani 1 1 d . . .
C19 C 0.5092(5) 0.1862(3) 0.9708(4) 0.0423(16) Uani 1 1 d . . .
C20 C 0.4742(5) 0.1355(2) 0.9263(4) 0.0450(16) Uani 1 1 d . . .
H20 H 0.4321 0.1316 0.8523 0.054 Uiso 1 1 calc R . .
C21 C 0.5025(6) 0.0907(2) 0.9927(4) 0.0527(18) Uani 1 1 d . . .
H21 H 0.4779 0.0567 0.9628 0.063 Uiso 1 1 calc R . .
C22 C 0.5661(6) 0.0954(2) 1.1019(5) 0.0459(16) Uani 1 1 d . . .
C23 C 0.6050(5) 0.1450(2) 1.1455(4) 0.0470(17) Uani 1 1 d . . .
H23 H 0.6512 0.1483 1.2189 0.056 Uiso 1 1 calc R . .
C24 C 0.5761(5) 0.1904(2) 1.0808(4) 0.0439(16) Uani 1 1 d . . .
H24 H 0.6017 0.2242 1.1114 0.053 Uiso 1 1 calc R . .
C25 C 0.4874(7) 0.0303(3) 1.2046(5) 0.0518(18) Uani 1 1 d . . .
C26 C 0.3728(8) 0.0581(3) 1.1703(5) 0.074(2) Uani 1 1 d . . .
H26 H 0.3636 0.0878 1.1254 0.088 Uiso 1 1 calc R . .
C27 C 0.2716(8) 0.0425(3) 1.2016(6) 0.090(3) Uani 1 1 d . . .
H27 H 0.1953 0.0625 1.1799 0.108 Uiso 1 1 calc R . .
C28 C 0.2817(10) -0.0029(4) 1.2656(6) 0.099(3) Uani 1 1 d . . .
H28 H 0.2117 -0.0136 1.2851 0.119 Uiso 1 1 calc R . .
C29 C 0.3922(9) -0.0317(3) 1.2994(5) 0.076(2) Uani 1 1 d . . .
H29 H 0.3988 -0.0625 1.3410 0.091 Uiso 1 1 calc R . .
C30 C 0.4979(8) -0.0141(3) 1.2705(5) 0.063(2) Uani 1 1 d . . .
C31 C 0.7220(7) -0.0334(3) 1.2367(5) 0.065(2) Uani 1 1 d . . .
C32 C 0.8204(9) -0.0668(3) 1.2312(6) 0.087(3) Uani 1 1 d . . .
H32 H 0.8405 -0.0971 1.2752 0.105 Uiso 1 1 calc R . .
C33 C 0.8894(8) -0.0575(3) 1.1646(7) 0.089(3) Uani 1 1 d . . .
H33 H 0.9550 -0.0809 1.1634 0.107 Uiso 1 1 calc R . .
C34 C 0.8599(8) -0.0126(3) 1.0993(6) 0.079(2) Uani 1 1 d . . .
H34 H 0.9061 -0.0052 1.0535 0.095 Uiso 1 1 calc R . .
C35 C 0.7597(7) 0.0218(3) 1.1021(6) 0.063(2) Uani 1 1 d . . .
H35 H 0.7390 0.0517 1.0567 0.075 Uiso 1 1 calc R . .
C36 C 0.6912(7) 0.0125(3) 1.1705(5) 0.0574(19) Uani 1 1 d . . .
C37 C 0.5497(5) 0.2810(2) 0.9342(4) 0.0353(14) Uani 1 1 d . . .
C38 C 0.6849(6) 0.2788(2) 0.9700(4) 0.0435(16) Uani 1 1 d . . .
H38 H 0.7272 0.2458 0.9783 0.052 Uiso 1 1 calc R . .
C39 C 0.7552(6) 0.3260(3) 0.9932(4) 0.0466(16) Uani 1 1 d . . .
H39 H 0.8452 0.3239 1.0180 0.056 Uiso 1 1 calc R . .
C40 C 0.6976(6) 0.3765(3) 0.9810(4) 0.0465(17) Uani 1 1 d . . .
C41 C 0.5622(7) 0.3772(2) 0.9424(4) 0.0557(18) Uani 1 1 d . . .
H41 H 0.5194 0.4102 0.9309 0.067 Uiso 1 1 calc R . .
C42 C 0.4894(6) 0.3299(2) 0.9209(4) 0.0486(16) Uani 1 1 d . . .
H42 H 0.3993 0.3317 0.8973 0.058 Uiso 1 1 calc R . .
C43 C 0.7690(8) 0.4265(3) 0.9995(5) 0.067(2) Uani 1 1 d . . .
H43 H 0.7192 0.4577 0.9805 0.080 Uiso 1 1 calc R . .
C44 C 0.8915(8) 0.4335(3) 1.0386(6) 0.100(3) Uani 1 1 d . . .
H44A H 0.9466 0.4040 1.0591 0.120 Uiso 1 1 calc R . .
H44B H 0.9256 0.4682 1.0464 0.120 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
S1 0.0749(14) 0.0787(14) 0.0461(10) 0.0031(10) -0.0183(9) 0.0017(12)
S2 0.1226(19) 0.0658(14) 0.0467(12) 0.0101(10) 0.0045(12) 0.0062(13)
N1 0.047(3) 0.048(3) 0.029(3) 0.007(2) 0.000(2) -0.007(3)
N2 0.051(4) 0.067(4) 0.034(3) 0.006(3) -0.007(3) 0.001(3)
N3 0.068(4) 0.051(4) 0.037(3) -0.001(3) 0.006(3) 0.003(4)
C1 0.053(4) 0.056(4) 0.019(3) 0.000(3) 0.009(3) -0.006(4)
C2 0.054(5) 0.094(6) 0.029(4) 0.015(3) 0.004(3) -0.006(4)
C3 0.069(5) 0.112(6) 0.029(4) 0.020(4) 0.012(4) -0.017(5)
C4 0.051(4) 0.060(5) 0.033(4) -0.002(3) 0.003(3) 0.002(4)
C5 0.046(4) 0.063(5) 0.033(4) 0.004(3) 0.002(3) 0.004(3)
C6 0.046(4) 0.059(4) 0.029(3) 0.000(3) 0.012(3) -0.002(4)
C7 0.049(4) 0.061(5) 0.039(4) 0.002(3) 0.006(3) -0.016(4)
C8 0.068(5) 0.061(5) 0.049(4) 0.008(4) 0.006(4) -0.004(4)
C9 0.112(7) 0.077(6) 0.065(5) 0.002(4) 0.036(5) 0.026(5)
C10 0.096(6) 0.071(6) 0.049(5) 0.017(4) -0.003(4) 0.022(5)
C11 0.070(5) 0.073(5) 0.038(4) 0.014(4) -0.001(4) -0.013(5)
C12 0.041(4) 0.063(5) 0.034(4) 0.008(3) 0.004(3) -0.009(4)
C13 0.047(4) 0.052(4) 0.034(4) -0.002(3) 0.005(3) 0.001(3)
C14 0.051(4) 0.098(6) 0.041(4) -0.011(4) 0.002(3) 0.003(5)
C15 0.081(6) 0.078(6) 0.054(5) -0.018(4) 0.007(4) 0.020(5)
C16 0.063(5) 0.089(6) 0.044(4) -0.006(4) -0.006(4) 0.019(5)
C17 0.058(5) 0.062(5) 0.031(4) 0.006(3) -0.002(3) 0.006(4)
C18 0.045(4) 0.070(5) 0.029(4) -0.004(3) 0.001(3) -0.012(4)
C19 0.038(4) 0.058(5) 0.026(3) 0.003(3) 0.006(3) 0.004(3)
C20 0.044(4) 0.058(4) 0.024(3) -0.004(3) -0.001(3) -0.008(4)
C21 0.056(5) 0.047(4) 0.044(4) -0.006(3) 0.004(3) -0.009(4)
C22 0.042(4) 0.050(4) 0.034(4) 0.001(3) -0.002(3) -0.008(3)
C23 0.048(4) 0.065(5) 0.021(3) -0.003(3) 0.002(3) 0.007(4)
C24 0.046(4) 0.043(4) 0.036(4) 0.000(3) 0.006(3) 0.006(3)
C25 0.048(5) 0.059(5) 0.037(4) 0.002(3) 0.000(4) -0.005(4)
C26 0.080(6) 0.088(6) 0.058(5) 0.015(4) 0.032(5) -0.004(5)
C27 0.083(7) 0.118(8) 0.074(6) 0.008(5) 0.033(5) 0.005(6)
C28 0.122(9) 0.104(8) 0.085(7) 0.016(5) 0.052(6) -0.003(7)
C29 0.094(7) 0.075(6) 0.057(5) 0.002(4) 0.025(5) -0.012(6)
C30 0.093(6) 0.050(5) 0.031(4) 0.007(3) 0.003(4) 0.008(4)
C31 0.074(6) 0.036(5) 0.064(5) 0.005(4) -0.002(4) 0.006(4)
C32 0.086(7) 0.058(6) 0.093(7) -0.001(5) 0.000(5) -0.002(5)
C33 0.054(6) 0.076(7) 0.116(8) 0.001(6) 0.001(5) 0.010(5)
C34 0.067(6) 0.070(6) 0.090(6) -0.025(5) 0.013(5) -0.016(5)
C35 0.049(5) 0.048(5) 0.075(5) -0.009(4) -0.001(4) -0.008(4)
C36 0.063(5) 0.053(5) 0.047(4) -0.018(4) 0.007(4) -0.018(4)
C37 0.037(4) 0.044(4) 0.017(3) 0.005(3) 0.001(3) 0.003(3)
C38 0.055(4) 0.042(4) 0.030(3) -0.005(3) 0.009(3) 0.006(4)
C39 0.037(4) 0.065(5) 0.030(3) -0.008(3) 0.001(3) 0.004(4)
C40 0.055(5) 0.049(5) 0.028(3) 0.001(3) 0.005(3) -0.001(4)
C41 0.073(5) 0.046(4) 0.042(4) 0.005(3) 0.011(4) 0.018(4)
C42 0.043(4) 0.048(4) 0.046(4) 0.009(3) 0.003(3) 0.003(4)
C43 0.081(6) 0.057(5) 0.055(5) -0.002(4) 0.014(4) -0.011(5)
C44 0.087(7) 0.077(6) 0.129(7) -0.027(5) 0.027(6) -0.020(5)

_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 C13 1.737(6) . ?
S1 C12 1.763(6) . ?
S2 C31 1.736(8) . ?
S2 C30 1.748(7) . ?
N1 C19 1.407(6) . ?
N1 C37 1.417(6) . ?
N1 C1 1.439(6) . ?
N2 C7 1.420(7) . ?
N2 C18 1.432(6) . ?
N2 C4 1.445(6) . ?
N3 C36 1.413(8) . ?
N3 C25 1.421(7) . ?
N3 C22 1.460(6) . ?
C1 C2 1.370(6) . ?
C1 C6 1.378(7) . ?
C2 C3 1.372(6) . ?
C3 C4 1.385(8) . ?
C4 C5 1.368(7) . ?
C5 C6 1.383(6) . ?
C7 C8 1.376(7) . ?
C7 C12 1.380(7) . ?
C8 C9 1.411(8) . ?
C9 C10 1.358(8) . ?
C10 C11 1.334(7) . ?
C11 C12 1.414(7) . ?
C13 C14 1.388(7) . ?
C13 C18 1.402(7) . ?
C14 C15 1.398(7) . ?
C15 C16 1.374(7) . ?
C16 C17 1.377(7) . ?
C17 C18 1.370(7) . ?
C19 C20 1.386(6) . ?
C19 C24 1.387(6) . ?
C20 C21 1.383(6) . ?
C21 C22 1.373(7) . ?
C22 C23 1.364(7) . ?
C23 C24 1.384(6) . ?
C25 C26 1.369(8) . ?
C25 C30 1.383(8) . ?
C26 C27 1.368(9) . ?
C27 C28 1.390(9) . ?
C28 C29 1.344(9) . ?
C29 C30 1.410(9) . ?
C31 C32 1.383(9) . ?
C31 C36 1.404(8) . ?
C32 C33 1.363(9) . ?
C33 C34 1.376(9) . ?
C34 C35 1.405(9) . ?
C35 C36 1.380(8) . ?
C37 C42 1.365(6) . ?
C37 C38 1.396(7) . ?
C38 C39 1.376(7) . ?
C39 C40 1.388(7) . ?
C40 C41 1.396(7) . ?
C40 C43 1.444(8) . ?
C41 C42 1.393(7) . ?
C43 C44 1.277(9) . ?

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
C13 S1 C12 101.9(3) . . ?
C31 S2 C30 101.2(4) . . ?
C19 N1 C37 122.2(4) . . ?
C19 N1 C1 121.1(5) . . ?
C37 N1 C1 115.9(4) . . ?
C7 N2 C18 124.3(5) . . ?
C7 N2 C4 118.6(5) . . ?
C18 N2 C4 115.4(5) . . ?
C36 N3 C25 121.3(6) . . ?
C36 N3 C22 118.2(6) . . ?
C25 N3 C22 116.4(6) . . ?
C2 C1 C6 119.0(5) . . ?
C2 C1 N1 118.9(5) . . ?
C6 C1 N1 122.1(5) . . ?
C1 C2 C3 121.8(6) . . ?
C2 C3 C4 119.0(6) . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 N2 122.4(6) . . ?
C3 C4 N2 118.0(6) . . ?
C4 C5 C6 120.9(6) . . ?
C1 C6 C5 119.7(5) . . ?
C8 C7 C12 117.5(7) . . ?
C8 C7 N2 119.3(6) . . ?
C12 C7 N2 123.2(6) . . ?
C7 C8 C9 119.6(6) . . ?
C10 C9 C8 121.5(7) . . ?
C11 C10 C9 119.9(7) . . ?
C10 C11 C12 119.7(6) . . ?
C7 C12 C11 121.8(6) . . ?
C7 C12 S1 122.6(6) . . ?
C11 C12 S1 115.5(5) . . ?
C14 C13 C18 118.4(6) . . ?
C14 C13 S1 116.5(5) . . ?
C18 C13 S1 125.0(5) . . ?
C13 C14 C15 121.9(6) . . ?
C16 C15 C14 117.4(6) . . ?
C15 C16 C17 121.8(6) . . ?
C18 C17 C16 120.5(6) . . ?
C17 C18 C13 119.7(6) . . ?
C17 C18 N2 120.4(5) . . ?
C13 C18 N2 119.8(6) . . ?
C20 C19 C24 118.8(5) . . ?
C20 C19 N1 121.6(5) . . ?
C24 C19 N1 119.6(5) . . ?
C21 C20 C19 119.5(5) . . ?
C22 C21 C20 121.2(6) . . ?
C23 C22 C21 119.4(6) . . ?
C23 C22 N3 119.8(5) . . ?
C21 C22 N3 120.8(6) . . ?
C22 C23 C24 120.3(5) . . ?
C23 C24 C19 120.7(6) . . ?
C26 C25 C30 118.5(7) . . ?
C26 C25 N3 119.1(6) . . ?
C30 C25 N3 122.4(7) . . ?
C27 C26 C25 120.5(7) . . ?
C26 C27 C28 120.6(8) . . ?
C29 C28 C27 120.4(9) . . ?
C28 C29 C30 118.7(8) . . ?
C25 C30 C29 121.2(7) . . ?
C25 C30 S2 121.3(7) . . ?
C29 C30 S2 117.3(6) . . ?
C32 C31 C36 118.6(8) . . ?
C32 C31 S2 119.4(6) . . ?
C36 C31 S2 121.9(7) . . ?
C33 C32 C31 123.4(8) . . ?
C32 C33 C34 118.5(8) . . ?
C33 C34 C35 119.5(8) . . ?
C36 C35 C34 121.6(7) . . ?
C35 C36 C31 118.3(7) . . ?
C35 C36 N3 120.3(7) . . ?
C31 C36 N3 121.4(7) . . ?
C42 C37 C38 119.4(6) . . ?
C42 C37 N1 119.8(5) . . ?
C38 C37 N1 120.8(5) . . ?
C39 C38 C37 119.5(6) . . ?
C38 C39 C40 122.9(6) . . ?
C39 C40 C41 116.1(6) . . ?
C39 C40 C43 123.9(6) . . ?
C41 C40 C43 119.9(7) . . ?
C42 C41 C40 121.9(6) . . ?
C37 C42 C41 120.2(6) . . ?
C44 C43 C40 128.4(8) . . ?

_diffrn_measured_fraction_theta_max 0.935
_diffrn_reflns_theta_full        28.24
_diffrn_measured_fraction_theta_full 0.935
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.222
_refine_diff_density_rms         0.048