# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

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

data_p
_database_code_depnum_ccdc_archive 'CCDC 1445532'
_audit_update_record             
;
2016-01-06 deposited with the CCDC.	2020-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 N6 S'
_chemical_formula_sum            'C16 H12 N6 S'
_chemical_formula_weight         320.38

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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  '-P 1   '

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

_cell_length_a                   8.5846(17)
_cell_length_b                   8.7889(18)
_cell_length_c                   10.622(2)
_cell_angle_alpha                71.38(3)
_cell_angle_beta                 76.72(3)
_cell_angle_gamma                82.17(3)
_cell_volume                     737.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1921
_cell_measurement_theta_min      2.0641
_cell_measurement_theta_max      27.8621

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             332
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.9473
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5332
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2801
_reflns_number_gt                2237
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0748P)²+0.2712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2801
_refine_ls_number_parameters     208
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0670
_refine_ls_wR_factor_ref         0.1831
_refine_ls_wR_factor_gt          0.1617
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_restrained_S_all      1.199
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.004

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7852(5) 0.7318(5) -0.2222(4) 0.0730(12) Uani 1 1 d . . .
H1A H 0.7681 0.8285 -0.2879 0.088 Uiso 1 1 calc R . .
C2 C 0.9055(5) 0.6268(5) -0.2577(4) 0.0723(12) Uani 1 1 d . . .
H2A H 0.9698 0.6518 -0.3440 0.087 Uiso 1 1 calc R . .
C3 C 0.9289(4) 0.4819(5) -0.1614(5) 0.0744(13) Uani 1 1 d . . .
H3A H 1.0105 0.4071 -0.1818 0.089 Uiso 1 1 calc R . .
C4 C 0.8304(4) 0.4486(5) -0.0345(4) 0.0621(10) Uani 1 1 d . . .
H4A H 0.8426 0.3507 0.0312 0.075 Uiso 1 1 calc R . .
C5 C 0.7126(4) 0.5653(4) -0.0079(3) 0.0491(8) Uani 1 1 d . . .
C6 C 0.4924(3) 0.6276(4) 0.1745(3) 0.0421(7) Uani 1 1 d . . .
C7 C 0.4417(4) 0.7841(4) 0.1133(3) 0.0440(7) Uani 1 1 d . . .
H7A H 0.4935 0.8372 0.0261 0.053 Uiso 1 1 calc R . .
C8 C 0.3123(4) 0.8659(4) 0.1809(3) 0.0463(7) Uani 1 1 d . . .
H8A H 0.2853 0.9727 0.1366 0.056 Uiso 1 1 calc R . .
C9 C 0.2250(3) 0.7977(4) 0.3068(3) 0.0401(7) Uani 1 1 d . . .
C10 C 0.2747(3) 0.6363(4) 0.3736(3) 0.0403(7) Uani 1 1 d . . .
C11 C 0.4076(3) 0.5542(4) 0.3077(3) 0.0443(7) Uani 1 1 d . . .
C12 C -0.0426(3) 0.9422(3) 0.3240(3) 0.0399(7) Uani 1 1 d . . .
C13 C -0.0753(4) 0.9257(4) 0.2060(3) 0.0505(8) Uani 1 1 d . . .
H13A H 0.0006 0.8760 0.1512 0.061 Uiso 1 1 calc R . .
C14 C -0.2207(4) 0.9842(5) 0.1732(4) 0.0672(10) Uani 1 1 d . . .
H14A H -0.2457 0.9712 0.0968 0.081 Uiso 1 1 calc R . .
C15 C -0.3313(5) 1.0625(5) 0.2522(4) 0.0715(11) Uani 1 1 d . . .
H15A H -0.4311 1.1026 0.2311 0.086 Uiso 1 1 calc R . .
C16 C -0.2876(4) 1.0784(4) 0.3630(4) 0.0598(9) Uani 1 1 d . . .
H16A H -0.3600 1.1336 0.4156 0.072 Uiso 1 1 calc R . .
N1 N 0.6890(4) 0.7063(4) -0.0991(3) 0.0609(8) Uani 1 1 d . . .
N2 N 0.6164(3) 0.5342(3) 0.1207(3) 0.0556(8) Uani 1 1 d . . .
H2B H 0.6373 0.4419 0.1759 0.067 Uiso 1 1 calc R . .
N3 N 0.4404(3) 0.4033(3) 0.3832(3) 0.0562(8) Uani 1 1 d . . .
N4 N 0.2092(3) 0.5454(3) 0.4982(3) 0.0527(7) Uani 1 1 d . . .
N5 N 0.0939(3) 0.8786(3) 0.3725(2) 0.0453(6) Uani 1 1 d . . .
H5A H 0.1006 0.8885 0.4490 0.054 Uiso 1 1 calc R . .
N6 N -0.1478(3) 1.0200(3) 0.4008(3) 0.0488(7) Uani 1 1 d . . .
S1 S 0.31025(12) 0.37423(11) 0.52351(9) 0.0659(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.346(4) . ?
C1 C2 1.357(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.379(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.382(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(4) . ?
C4 H4A 0.9300 . ?
C5 N1 1.330(5) . ?
C5 N2 1.388(4) . ?
C6 C7 1.378(4) . ?
C6 N2 1.384(4) . ?
C6 C11 1.421(4) . ?
C7 C8 1.418(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.363(4) . ?
C8 H8A 0.9300 . ?
C9 N5 1.413(3) . ?
C9 C10 1.424(4) . ?
C10 N4 1.346(4) . ?
C10 C11 1.429(4) . ?
C11 N3 1.343(4) . ?
C12 N6 1.341(4) . ?
C12 N5 1.366(4) . ?
C12 C13 1.400(4) . ?
C13 C14 1.361(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.380(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.366(5) . ?
C15 H15A 0.9300 . ?
C16 N6 1.337(4) . ?
C16 H16A 0.9300 . ?
N2 H2B 0.8600 . ?
N3 S1 1.614(3) . ?
N4 S1 1.606(3) . ?
N5 H5A 0.8600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.8(4) . . ?
N1 C1 H1A 117.6 . . ?
C2 C1 H1A 117.6 . . ?
C1 C2 C3 117.7(3) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.2(4) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 N2 118.5(3) . . ?
N1 C5 C4 123.1(3) . . ?
N2 C5 C4 118.3(3) . . ?
C7 C6 N2 127.3(3) . . ?
C7 C6 C11 116.2(3) . . ?
N2 C6 C11 116.5(3) . . ?
C6 C7 C8 121.3(3) . . ?
C6 C7 H7A 119.4 . . ?
C8 C7 H7A 119.4 . . ?
C9 C8 C7 124.1(3) . . ?
C9 C8 H8A 118.0 . . ?
C7 C8 H8A 118.0 . . ?
C8 C9 N5 123.9(3) . . ?
C8 C9 C10 116.2(2) . . ?
N5 C9 C10 119.9(3) . . ?
N4 C10 C9 126.9(3) . . ?
N4 C10 C11 112.9(3) . . ?
C9 C10 C11 120.2(3) . . ?
N3 C11 C6 124.7(3) . . ?
N3 C11 C10 113.3(3) . . ?
C6 C11 C10 122.0(3) . . ?
N6 C12 N5 114.6(3) . . ?
N6 C12 C13 121.5(3) . . ?
N5 C12 C13 123.9(3) . . ?
C14 C13 C12 118.5(3) . . ?
C14 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
C13 C14 C15 120.7(3) . . ?
C13 C14 H14A 119.6 . . ?
C15 C14 H14A 119.6 . . ?
C16 C15 C14 117.0(3) . . ?
C16 C15 H15A 121.5 . . ?
C14 C15 H15A 121.5 . . ?
N6 C16 C15 124.4(3) . . ?
N6 C16 H16A 117.8 . . ?
C15 C16 H16A 117.8 . . ?
C5 N1 C1 116.6(3) . . ?
C6 N2 C5 130.5(3) . . ?
C6 N2 H2B 114.8 . . ?
C5 N2 H2B 114.8 . . ?
C11 N3 S1 106.2(2) . . ?
C10 N4 S1 106.5(2) . . ?
C12 N5 C9 125.1(2) . . ?
C12 N5 H5A 117.4 . . ?
C9 N5 H5A 117.4 . . ?
C16 N6 C12 117.8(3) . . ?
N4 S1 N3 101.01(14) . . ?

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
N1 C1 C2 C3 1.4(7) . . . . ?
C1 C2 C3 C4 0.4(6) . . . . ?
C2 C3 C4 C5 -1.4(6) . . . . ?
C3 C4 C5 N1 0.9(6) . . . . ?
C3 C4 C5 N2 -178.2(3) . . . . ?
N2 C6 C7 C8 -179.8(3) . . . . ?
C11 C6 C7 C8 0.1(5) . . . . ?
C6 C7 C8 C9 -2.3(5) . . . . ?
C7 C8 C9 N5 -178.6(3) . . . . ?
C7 C8 C9 C10 2.7(5) . . . . ?
C8 C9 C10 N4 179.0(3) . . . . ?
N5 C9 C10 N4 0.2(5) . . . . ?
C8 C9 C10 C11 -1.0(4) . . . . ?
N5 C9 C10 C11 -179.8(3) . . . . ?
C7 C6 C11 N3 -179.6(3) . . . . ?
N2 C6 C11 N3 0.3(5) . . . . ?
C7 C6 C11 C10 1.6(4) . . . . ?
N2 C6 C11 C10 -178.5(3) . . . . ?
N4 C10 C11 N3 0.0(4) . . . . ?
C9 C10 C11 N3 179.9(3) . . . . ?
N4 C10 C11 C6 178.9(3) . . . . ?
C9 C10 C11 C6 -1.1(5) . . . . ?
N6 C12 C13 C14 -3.1(5) . . . . ?
N5 C12 C13 C14 175.2(3) . . . . ?
C12 C13 C14 C15 2.1(6) . . . . ?
C13 C14 C15 C16 0.2(6) . . . . ?
C14 C15 C16 N6 -1.7(7) . . . . ?
N2 C5 N1 C1 179.7(3) . . . . ?
C4 C5 N1 C1 0.7(5) . . . . ?
C2 C1 N1 C5 -1.9(6) . . . . ?
C7 C6 N2 C5 -5.6(6) . . . . ?
C11 C6 N2 C5 174.5(3) . . . . ?
N1 C5 N2 C6 0.6(5) . . . . ?
C4 C5 N2 C6 179.8(3) . . . . ?
C6 C11 N3 S1 -178.7(3) . . . . ?
C10 C11 N3 S1 0.2(4) . . . . ?
C9 C10 N4 S1 179.8(3) . . . . ?
C11 C10 N4 S1 -0.2(3) . . . . ?
N6 C12 N5 C9 -177.1(3) . . . . ?
C13 C12 N5 C9 4.6(5) . . . . ?
C8 C9 N5 C12 59.7(5) . . . . ?
C10 C9 N5 C12 -121.6(3) . . . . ?
C15 C16 N6 C12 0.8(6) . . . . ?
N5 C12 N6 C16 -176.7(3) . . . . ?
C13 C12 N6 C16 1.6(5) . . . . ?
C10 N4 S1 N3 0.3(3) . . . . ?
C11 N3 S1 N4 -0.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5A N6 0.86 2.14 2.967(4) 162.5 2_576

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.068
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1449464'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.	2020-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H12 N6 O0 S'
_chemical_formula_sum            'C16 H12 N6 O0 S'
_chemical_formula_weight         320.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_HALL  '-P 1   '

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

_cell_length_a                   8.8290(18)
_cell_length_b                   10.340(2)
_cell_length_c                   16.666(3)
_cell_angle_alpha                96.61(3)
_cell_angle_beta                 90.45(3)
_cell_angle_gamma                102.67(3)
_cell_volume                     1473.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3852
_cell_measurement_theta_min      2.2473
_cell_measurement_theta_max      27.8644

_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             664
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.9536
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2006)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         6972
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14404
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.50
_reflns_number_total             5476
_reflns_number_gt                4143
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0728P)²+0.1966P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5476
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.46835(8) -0.22066(7) 0.42331(4) 0.0524(2) Uani 1 1 d . . .
S2 S 0.78939(9) 0.48997(8) -0.05225(4) 0.0587(2) Uani 1 1 d . . .
N1 N 0.9213(3) 0.6268(2) -0.03954(13) 0.0484(6) Uani 1 1 d . . .
N2 N 0.7056(2) 0.4964(2) 0.03323(13) 0.0463(6) Uani 1 1 d . . .
N3 N 0.6252(2) 0.5825(2) 0.19799(13) 0.0398(5) Uani 1 1 d . . .
H3A H 0.6407 0.5086 0.2118 0.048 Uiso 1 1 calc R . .
N4 N 0.3844(2) 0.5170(2) 0.24828(12) 0.0393(5) Uani 1 1 d . . .
N5 N 1.1095(2) 0.8739(2) 0.02333(13) 0.0463(6) Uani 1 1 d . . .
H5 H 1.1192 0.8290 -0.0223 0.056 Uiso 1 1 calc R . .
C13 C 1.3165(3) 1.0361(3) -0.02220(18) 0.0518(7) Uani 1 1 d . . .
H13 H 1.3162 0.9816 -0.0707 0.062 Uiso 1 1 calc R . .
N7 N 0.6189(2) -0.0973(2) 0.43496(12) 0.0435(5) Uani 1 1 d . . .
N8 N 0.4562(2) -0.2654(2) 0.51279(13) 0.0456(6) Uani 1 1 d . . .
N9 N 0.5120(2) -0.2748(2) 0.68708(12) 0.0399(5) Uani 1 1 d . . .
H9A H 0.5380 -0.3476 0.6955 0.048 Uiso 1 1 calc R . .
N10 N 0.3033(2) -0.3367(2) 0.76591(13) 0.0429(5) Uani 1 1 d . . .
N11 N 0.8719(2) 0.1025(2) 0.50100(12) 0.0411(5) Uani 1 1 d . . .
H11A H 0.8404 0.0873 0.4511 0.049 Uiso 1 1 calc R . .
C29 C 1.0362(4) 0.2980(3) 0.46000(18) 0.0606(8) Uani 1 1 d . . .
H29 H 0.9882 0.2781 0.4088 0.073 Uiso 1 1 calc R . .
C1 C 0.9027(3) 0.6857(2) 0.03520(15) 0.0370(6) Uani 1 1 d . . .
C2 C 0.9938(3) 0.8112(2) 0.07072(15) 0.0362(6) Uani 1 1 d . . .
C3 C 0.9584(3) 0.8540(2) 0.14761(15) 0.0402(6) Uani 1 1 d . . .
H3 H 1.0151 0.9350 0.1733 0.048 Uiso 1 1 calc R . .
C4 C 0.8371(3) 0.7775(2) 0.18919(15) 0.0396(6) Uani 1 1 d . . .
H4 H 0.8194 0.8103 0.2418 0.048 Uiso 1 1 calc R . .
C5 C 0.7453(3) 0.6594(2) 0.15676(15) 0.0345(5) Uani 1 1 d . . .
C6 C 0.7798(3) 0.6111(2) 0.07717(15) 0.0359(6) Uani 1 1 d . . .
C7 C 0.4870(3) 0.6141(2) 0.21808(14) 0.0337(5) Uani 1 1 d . . .
C8 C 0.4534(3) 0.7374(3) 0.20791(15) 0.0412(6) Uani 1 1 d . . .
H8 H 0.5282 0.8050 0.1899 0.049 Uiso 1 1 calc R . .
C9 C 0.2437(3) 0.5405(3) 0.26521(16) 0.0490(7) Uani 1 1 d . . .
H9 H 0.1715 0.4739 0.2859 0.059 Uiso 1 1 calc R . .
C10 C 0.1998(3) 0.6568(3) 0.25386(18) 0.0555(8) Uani 1 1 d . . .
H10 H 0.1002 0.6679 0.2653 0.067 Uiso 1 1 calc R . .
C11 C 0.3079(3) 0.7563(3) 0.22507(17) 0.0500(7) Uani 1 1 d . . .
H11 H 0.2821 0.8366 0.2172 0.060 Uiso 1 1 calc R . .
C12 C 1.2117(3) 0.9972(3) 0.03774(16) 0.0407(6) Uani 1 1 d . . .
N6 N 1.2057(3) 1.0731(2) 0.10706(14) 0.0535(6) Uani 1 1 d . . .
C14 C 1.4197(3) 1.1574(3) -0.0072(2) 0.0625(9) Uani 1 1 d . . .
H14 H 1.4920 1.1853 -0.0454 0.075 Uiso 1 1 calc R . .
C15 C 1.4161(3) 1.2379(3) 0.06476(19) 0.0627(9) Uani 1 1 d . . .
H15 H 1.4854 1.3201 0.0761 0.075 Uiso 1 1 calc R . .
C16 C 1.3078(4) 1.1923(3) 0.11806(19) 0.0636(9) Uani 1 1 d . . .
H16 H 1.3035 1.2473 0.1658 0.076 Uiso 1 1 calc R . .
C17 C 0.6671(3) -0.0880(2) 0.51240(14) 0.0351(6) Uani 1 1 d . . .
C18 C 0.5746(3) -0.1842(2) 0.55739(15) 0.0354(6) Uani 1 1 d . . .
C19 C 0.6100(3) -0.1850(2) 0.64062(15) 0.0367(6) Uani 1 1 d . . .
C20 C 0.7365(3) -0.0928(3) 0.67297(15) 0.0412(6) Uani 1 1 d . . .
H20 H 0.7633 -0.0927 0.7271 0.049 Uiso 1 1 calc R . .
C21 C 0.8300(3) 0.0031(2) 0.62920(15) 0.0405(6) Uani 1 1 d . . .
H21 H 0.9157 0.0624 0.6551 0.049 Uiso 1 1 calc R . .
C22 C 0.7966(3) 0.0103(2) 0.54958(14) 0.0347(6) Uani 1 1 d . . .
C23 C 0.3781(3) -0.2487(2) 0.71858(14) 0.0341(6) Uani 1 1 d . . .
C24 C 0.3211(3) -0.1381(3) 0.70224(16) 0.0444(6) Uani 1 1 d . . .
H24 H 0.3752 -0.0773 0.6698 0.053 Uiso 1 1 calc R . .
C25 C 0.1704(3) -0.3153(3) 0.79767(18) 0.0527(7) Uani 1 1 d . . .
H25 H 0.1186 -0.3758 0.8309 0.063 Uiso 1 1 calc R . .
C26 C 0.1064(3) -0.2107(3) 0.78442(18) 0.0561(8) Uani 1 1 d . . .
H26 H 0.0140 -0.1999 0.8078 0.067 Uiso 1 1 calc R . .
C27 C 0.1841(3) -0.1212(3) 0.73499(18) 0.0539(7) Uani 1 1 d . . .
H27 H 0.1432 -0.0494 0.7240 0.065 Uiso 1 1 calc R . .
C28 C 0.9905(3) 0.2157(2) 0.51981(15) 0.0373(6) Uani 1 1 d . . .
N12 N 1.0560(3) 0.2398(2) 0.59316(14) 0.0508(6) Uani 1 1 d . . .
C30 C 1.1533(4) 0.4089(3) 0.4780(2) 0.0734(10) Uani 1 1 d . . .
H30 H 1.1860 0.4653 0.4389 0.088 Uiso 1 1 calc R . .
C31 C 1.2229(4) 0.4369(3) 0.5542(2) 0.0643(9) Uani 1 1 d . . .
H31 H 1.3026 0.5118 0.5680 0.077 Uiso 1 1 calc R . .
C32 C 1.1701(4) 0.3502(3) 0.60797(19) 0.0633(9) Uani 1 1 d . . .
H32 H 1.2166 0.3687 0.6595 0.076 Uiso 1 1 calc R . .


_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 N8 1.609(2) . ?
S1 N7 1.620(2) . ?
S2 N2 1.612(2) . ?
S2 N1 1.615(2) . ?
N1 C1 1.350(3) . ?
N2 C6 1.351(3) . ?
N3 C7 1.366(3) . ?
N3 C5 1.413(3) . ?
N3 H3A 0.8600 . ?
N4 C7 1.344(3) . ?
N4 C9 1.343(3) . ?
N5 C2 1.388(3) . ?
N5 C12 1.385(3) . ?
N5 H5 0.8600 . ?
C13 C14 1.374(4) . ?
C13 C12 1.399(4) . ?
C13 H13 0.9300 . ?
N7 C17 1.342(3) . ?
N8 C18 1.345(3) . ?
N9 C23 1.365(3) . ?
N9 C19 1.426(3) . ?
N9 H9A 0.8600 . ?
N10 C23 1.340(3) . ?
N10 C25 1.342(3) . ?
N11 C22 1.383(3) . ?
N11 C28 1.391(3) . ?
N11 H11A 0.8600 . ?
C29 C30 1.367(4) . ?
C29 C28 1.390(4) . ?
C29 H29 0.9300 . ?
C1 C6 1.425(3) . ?
C1 C2 1.428(3) . ?
C2 C3 1.368(3) . ?
C3 C4 1.421(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.422(3) . ?
C7 C8 1.398(3) . ?
C8 C11 1.369(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.374(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.374(4) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 N6 1.328(3) . ?
N6 C16 1.350(3) . ?
C14 C15 1.383(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.356(4) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C18 1.429(3) . ?
C17 C22 1.435(3) . ?
C18 C19 1.421(3) . ?
C19 C20 1.361(3) . ?
C20 C21 1.419(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.371(3) . ?
C21 H21 0.9300 . ?
C23 C24 1.399(3) . ?
C24 C27 1.368(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.363(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.382(4) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 N12 1.321(3) . ?
N12 C32 1.344(3) . ?
C30 C31 1.378(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.354(4) . ?
C31 H31 0.9300 . ?
C32 H32 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
N8 S1 N7 101.10(11) . . ?
N2 S2 N1 101.05(11) . . ?
C1 N1 S2 105.99(17) . . ?
C6 N2 S2 106.47(17) . . ?
C7 N3 C5 126.3(2) . . ?
C7 N3 H3A 116.9 . . ?
C5 N3 H3A 116.9 . . ?
C7 N4 C9 117.1(2) . . ?
C2 N5 C12 130.4(2) . . ?
C2 N5 H5 114.8 . . ?
C12 N5 H5 114.8 . . ?
C14 C13 C12 117.9(3) . . ?
C14 C13 H13 121.1 . . ?
C12 C13 H13 121.0 . . ?
C17 N7 S1 105.65(17) . . ?
C18 N8 S1 106.58(17) . . ?
C23 N9 C19 122.0(2) . . ?
C23 N9 H9A 119.0 . . ?
C19 N9 H9A 119.0 . . ?
C23 N10 C25 117.7(2) . . ?
C22 N11 C28 130.4(2) . . ?
C22 N11 H11A 114.8 . . ?
C28 N11 H11A 114.8 . . ?
C30 C29 C28 118.6(3) . . ?
C30 C29 H29 120.7 . . ?
C28 C29 H29 120.7 . . ?
N1 C1 C6 113.6(2) . . ?
N1 C1 C2 124.8(2) . . ?
C6 C1 C2 121.6(2) . . ?
C3 C2 N5 127.9(2) . . ?
C3 C2 C1 116.3(2) . . ?
N5 C2 C1 115.8(2) . . ?
C2 C3 C4 121.5(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 124.0(2) . . ?
C5 C4 H4 118.0 . . ?
C3 C4 H4 118.0 . . ?
C4 C5 N3 124.3(2) . . ?
C4 C5 C6 116.0(2) . . ?
N3 C5 C6 119.7(2) . . ?
N2 C6 C1 112.9(2) . . ?
N2 C6 C5 126.5(2) . . ?
C1 C6 C5 120.6(2) . . ?
N4 C7 N3 114.7(2) . . ?
N4 C7 C8 122.2(2) . . ?
N3 C7 C8 123.0(2) . . ?
C11 C8 C7 118.6(2) . . ?
C11 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
N4 C9 C10 124.1(3) . . ?
N4 C9 H9 118.0 . . ?
C10 C9 H9 118.0 . . ?
C9 C10 C11 117.9(3) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C8 C11 C10 120.1(3) . . ?
C8 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
N6 C12 N5 118.9(2) . . ?
N6 C12 C13 123.1(2) . . ?
N5 C12 C13 118.0(2) . . ?
C12 N6 C16 116.5(2) . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 117.4(3) . . ?
C16 C15 H15 121.3 . . ?
C14 C15 H15 121.3 . . ?
N6 C16 C15 125.0(3) . . ?
N6 C16 H16 117.5 . . ?
C15 C16 H16 117.5 . . ?
N7 C17 C18 114.0(2) . . ?
N7 C17 C22 124.6(2) . . ?
C18 C17 C22 121.4(2) . . ?
N8 C18 C19 126.9(2) . . ?
N8 C18 C17 112.7(2) . . ?
C19 C18 C17 120.4(2) . . ?
C20 C19 C18 116.4(2) . . ?
C20 C19 N9 123.0(2) . . ?
C18 C19 N9 120.6(2) . . ?
C19 C20 C21 124.0(2) . . ?
C19 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C22 C21 C20 121.4(2) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 N11 127.6(2) . . ?
C21 C22 C17 116.3(2) . . ?
N11 C22 C17 116.0(2) . . ?
N10 C23 N9 115.7(2) . . ?
N10 C23 C24 121.8(2) . . ?
N9 C23 C24 122.5(2) . . ?
C27 C24 C23 118.6(2) . . ?
C27 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
N10 C25 C26 124.3(3) . . ?
N10 C25 H25 117.9 . . ?
C26 C25 H25 117.9 . . ?
C25 C26 C27 117.5(3) . . ?
C25 C26 H26 121.3 . . ?
C27 C26 H26 121.3 . . ?
C24 C27 C26 120.2(3) . . ?
C24 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N12 C28 N11 118.9(2) . . ?
N12 C28 C29 122.7(2) . . ?
N11 C28 C29 118.3(2) . . ?
C28 N12 C32 116.4(2) . . ?
C31 C30 C29 119.9(3) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C32 C31 C30 116.9(3) . . ?
C32 C31 H31 121.5 . . ?
C30 C31 H31 121.5 . . ?
N12 C32 C31 125.5(3) . . ?
N12 C32 H32 117.3 . . ?
C31 C32 H32 117.3 . . ?

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
N2 S2 N1 C1 -0.6(2) . . . . ?
N1 S2 N2 C6 0.3(2) . . . . ?
N8 S1 N7 C17 0.62(19) . . . . ?
N7 S1 N8 C18 -0.7(2) . . . . ?
S2 N1 C1 C6 0.6(3) . . . . ?
S2 N1 C1 C2 -178.7(2) . . . . ?
C12 N5 C2 C3 -4.6(4) . . . . ?
C12 N5 C2 C1 176.6(2) . . . . ?
N1 C1 C2 C3 -179.4(3) . . . . ?
C6 C1 C2 C3 1.4(4) . . . . ?
N1 C1 C2 N5 -0.4(4) . . . . ?
C6 C1 C2 N5 -179.7(2) . . . . ?
N5 C2 C3 C4 -179.1(2) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 N3 179.5(2) . . . . ?
C3 C4 C5 C6 1.9(4) . . . . ?
C7 N3 C5 C4 70.5(4) . . . . ?
C7 N3 C5 C6 -112.0(3) . . . . ?
S2 N2 C6 C1 0.0(3) . . . . ?
S2 N2 C6 C5 179.7(2) . . . . ?
N1 C1 C6 N2 -0.4(3) . . . . ?
C2 C1 C6 N2 178.9(2) . . . . ?
N1 C1 C6 C5 179.9(2) . . . . ?
C2 C1 C6 C5 -0.8(4) . . . . ?
C4 C5 C6 N2 179.5(2) . . . . ?
N3 C5 C6 N2 1.8(4) . . . . ?
C4 C5 C6 C1 -0.8(4) . . . . ?
N3 C5 C6 C1 -178.6(2) . . . . ?
C9 N4 C7 N3 -176.7(2) . . . . ?
C9 N4 C7 C8 3.0(4) . . . . ?
C5 N3 C7 N4 172.2(2) . . . . ?
C5 N3 C7 C8 -7.5(4) . . . . ?
N4 C7 C8 C11 -3.8(4) . . . . ?
N3 C7 C8 C11 175.9(2) . . . . ?
C7 N4 C9 C10 -0.3(4) . . . . ?
N4 C9 C10 C11 -1.5(4) . . . . ?
C7 C8 C11 C10 1.9(4) . . . . ?
C9 C10 C11 C8 0.6(4) . . . . ?
C2 N5 C12 N6 0.4(4) . . . . ?
C2 N5 C12 C13 -179.2(3) . . . . ?
C14 C13 C12 N6 1.6(4) . . . . ?
C14 C13 C12 N5 -178.8(2) . . . . ?
N5 C12 N6 C16 -179.9(3) . . . . ?
C13 C12 N6 C16 -0.4(4) . . . . ?
C12 C13 C14 C15 -1.2(4) . . . . ?
C13 C14 C15 C16 -0.3(5) . . . . ?
C12 N6 C16 C15 -1.3(5) . . . . ?
C14 C15 C16 N6 1.6(5) . . . . ?
S1 N7 C17 C18 -0.3(3) . . . . ?
S1 N7 C17 C22 -178.7(2) . . . . ?
S1 N8 C18 C19 179.2(2) . . . . ?
S1 N8 C18 C17 0.6(3) . . . . ?
N7 C17 C18 N8 -0.2(3) . . . . ?
C22 C17 C18 N8 178.3(2) . . . . ?
N7 C17 C18 C19 -178.9(2) . . . . ?
C22 C17 C18 C19 -0.4(4) . . . . ?
N8 C18 C19 C20 179.9(2) . . . . ?
C17 C18 C19 C20 -1.5(4) . . . . ?
N8 C18 C19 N9 -2.8(4) . . . . ?
C17 C18 C19 N9 175.7(2) . . . . ?
C23 N9 C19 C20 95.9(3) . . . . ?
C23 N9 C19 C18 -81.1(3) . . . . ?
C18 C19 C20 C21 1.4(4) . . . . ?
N9 C19 C20 C21 -175.8(2) . . . . ?
C19 C20 C21 C22 0.9(4) . . . . ?
C20 C21 C22 N11 176.3(2) . . . . ?
C20 C21 C22 C17 -2.8(4) . . . . ?
C28 N11 C22 C21 -5.5(4) . . . . ?
C28 N11 C22 C17 173.6(2) . . . . ?
N7 C17 C22 C21 -179.1(2) . . . . ?
C18 C17 C22 C21 2.6(3) . . . . ?
N7 C17 C22 N11 1.7(4) . . . . ?
C18 C17 C22 N11 -176.6(2) . . . . ?
C25 N10 C23 N9 -179.5(2) . . . . ?
C25 N10 C23 C24 0.0(4) . . . . ?
C19 N9 C23 N10 -175.2(2) . . . . ?
C19 N9 C23 C24 5.3(4) . . . . ?
N10 C23 C24 C27 -0.9(4) . . . . ?
N9 C23 C24 C27 178.6(2) . . . . ?
C23 N10 C25 C26 0.5(4) . . . . ?
N10 C25 C26 C27 0.0(5) . . . . ?
C23 C24 C27 C26 1.3(4) . . . . ?
C25 C26 C27 C24 -0.9(5) . . . . ?
C22 N11 C28 N12 6.2(4) . . . . ?
C22 N11 C28 C29 -174.5(3) . . . . ?
C30 C29 C28 N12 -0.3(5) . . . . ?
C30 C29 C28 N11 -179.6(3) . . . . ?
N11 C28 N12 C32 179.8(3) . . . . ?
C29 C28 N12 C32 0.6(4) . . . . ?
C28 C29 C30 C31 -0.1(5) . . . . ?
C29 C30 C31 C32 0.3(5) . . . . ?
C28 N12 C32 C31 -0.5(5) . . . . ?
C30 C31 C32 N12 0.0(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N9 H9A N4 0.86 2.30 3.144(3) 165.3 2_656
N3 H3A N10 0.86 2.02 2.876(3) 173.1 2_656

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.043
