# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Prof Mustafa M El-Abadelah'
_publ_contact_author_address     
;
Chemistry
University of Jordan
Faculty of Science
University of Jordan
Amman
Amman 11942
JORDAN
;

_publ_contact_author_email       MUSTELAB@JU.EDU.JO

_publ_section_title              
;
3-Mercaptopropionic Acid Nitrile Imine Adducts. An
Unprecedented Cyclization into 1,3,4-Thiadiazol-2(3H)-ones and
2(3H)-thiones
;
loop_
_publ_author_name
'Mustafa M. El-Abadelah'
'Bassam A. Abu Thaher'
'Roland Boese'
'Jalal A. Zahra'

data_ubkabam
_database_code_depnum_ccdc_archive 'CCDC 260037'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
5-Acetyl-3-(4-methylphenyl)-1,3,4-thiadiazol-2(3H)-one
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H20 N4 O4 S2'
_chemical_formula_weight         468.54
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           ?
_symmetry_space_group_name_H-M   ?
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                   11.9376(16)
_cell_length_b                   14.0036(19)
_cell_length_c                   13.9101(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.916(2)
_cell_angle_gamma                90.00
_cell_volume                     2212.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.278

_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      203(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27847
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         28.41
_reflns_number_total             5545
_reflns_number_gt                4467
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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 Rfactors
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^)+(0.0515P)^2^+0.8776P] where
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5545
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.32583(13) 0.26521(11) 0.95020(10) 0.0591(4) Uani 1 1 d . . .
O2 O -0.05751(12) 0.16324(13) 0.61999(12) 0.0696(4) Uani 1 1 d . . .
O3 O 0.38849(10) 0.04332(9) 0.02194(8) 0.0446(3) Uani 1 1 d . . .
O4 O 0.78113(10) 0.05973(9) 0.36509(9) 0.0469(3) Uani 1 1 d . . .
S1 S 0.12090(4) 0.21521(4) 0.81647(4) 0.05210(14) Uani 1 1 d . . .
C2 C 0.27540(15) 0.23208(12) 0.86810(13) 0.0439(4) Uani 1 1 d . . .
N3 N 0.32583(11) 0.20108(9) 0.79529(10) 0.0372(3) Uani 1 1 d . . .
N4 N 0.25043(12) 0.17297(10) 0.70491(10) 0.0390(3) Uani 1 1 d . . .
C5 C 0.14246(14) 0.17728(12) 0.70496(13) 0.0407(3) Uani 1 1 d . . .
C6 C 0.04154(15) 0.15595(13) 0.61381(14) 0.0467(4) Uani 1 1 d . . .
C7 C 0.06852(16) 0.12819(15) 0.52000(14) 0.0542(5) Uani 1 1 d . . .
H7A H 0.1017 0.0644 0.5276 0.081 Uiso 1 1 d R . .
H7B H 0.1246 0.1730 0.5077 0.081 Uiso 1 1 d R . .
H7C H -0.0034 0.1293 0.4634 0.081 Uiso 1 1 d R . .
C8 C 0.44919(14) 0.20188(11) 0.80492(12) 0.0372(3) Uani 1 1 d . . .
C9 C 0.53312(16) 0.19804(14) 0.89951(14) 0.0486(4) Uani 1 1 d . . .
H9 H 0.5101 0.1940 0.9597 0.058 Uiso 1 1 d R . .
C10 C 0.65158(16) 0.19904(14) 0.90574(16) 0.0535(5) Uani 1 1 d . . .
H10 H 0.7100 0.1979 0.9710 0.064 Uiso 1 1 d R . .
C11 C 0.68832(15) 0.20244(12) 0.82052(16) 0.0485(4) Uani 1 1 d . . .
C12 C 0.60220(16) 0.20442(12) 0.72684(15) 0.0467(4) Uani 1 1 d . . .
H12 H 0.6257 0.2059 0.6668 0.056 Uiso 1 1 d R . .
C13 C 0.48303(15) 0.20454(11) 0.71802(13) 0.0406(3) Uani 1 1 d . . .
H13 H 0.4247 0.2066 0.6527 0.049 Uiso 1 1 d R . .
C14 C 0.81798(17) 0.20539(16) 0.8296(2) 0.0678(6) Uani 1 1 d . . .
H14A H 0.8552 0.2581 0.8729 0.102 Uiso 1 1 d R . .
H14B H 0.8274 0.2138 0.7633 0.102 Uiso 1 1 d R . .
H14C H 0.8545 0.1458 0.8587 0.102 Uiso 1 1 d R . .
S21 S 0.59882(3) 0.04597(3) 0.16449(3) 0.03562(11) Uani 1 1 d . . .
C22 C 0.44327(13) 0.04865(10) 0.11046(11) 0.0326(3) Uani 1 1 d . . .
N23 N 0.39553(11) 0.05871(9) 0.19013(8) 0.0303(2) Uani 1 1 d . . .
N24 N 0.47267(11) 0.06094(9) 0.28538(9) 0.0319(3) Uani 1 1 d . . .
C25 C 0.57981(13) 0.05601(10) 0.28254(10) 0.0316(3) Uani 1 1 d . . .
C26 C 0.68332(14) 0.05689(11) 0.37483(11) 0.0367(3) Uani 1 1 d . . .
C27 C 0.66154(17) 0.05118(16) 0.47520(12) 0.0535(5) Uani 1 1 d . . .
H27A H 0.6462 -0.0146 0.4890 0.080 Uiso 1 1 d R . .
H27B H 0.5940 0.0902 0.4738 0.080 Uiso 1 1 d R . .
H27C H 0.7302 0.0741 0.5277 0.080 Uiso 1 1 d R . .
C28 C 0.27203(13) 0.06209(10) 0.17890(10) 0.0302(3) Uani 1 1 d . . .
C29 C 0.19116(14) 0.09454(13) 0.09063(12) 0.0416(4) Uani 1 1 d . . .
H29 H 0.2169 0.1154 0.0351 0.050 Uiso 1 1 d R . .
C30 C 0.07234(15) 0.09607(14) 0.08289(13) 0.0454(4) Uani 1 1 d . . .
H30 H 0.0165 0.1174 0.0210 0.054 Uiso 1 1 d R . .
C31 C 0.03223(14) 0.06727(12) 0.16232(13) 0.0411(4) Uani 1 1 d . . .
C32 C 0.11491(16) 0.03612(13) 0.24962(13) 0.0452(4) Uani 1 1 d . . .
H32 H 0.0892 0.0157 0.3053 0.054 Uiso 1 1 d R . .
C33 C 0.23403(15) 0.03307(12) 0.25911(12) 0.0400(3) Uani 1 1 d . . .
H33 H 0.2897 0.0109 0.3207 0.048 Uiso 1 1 d R . .
C34 C -0.09780(17) 0.07166(16) 0.15284(17) 0.0579(5) Uani 1 1 d . . .
H34A H -0.1092 0.0534 0.2164 0.087 Uiso 1 1 d R . .
H34B H -0.1412 0.0284 0.1000 0.087 Uiso 1 1 d R . .
H34C H -0.1260 0.1363 0.1358 0.087 Uiso 1 1 d 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
O1 0.0599(8) 0.0688(9) 0.0453(7) -0.0085(6) 0.0111(6) 0.0019(7)
O2 0.0357(7) 0.0928(12) 0.0771(10) 0.0026(9) 0.0125(7) -0.0098(7)
O3 0.0401(6) 0.0665(8) 0.0266(5) -0.0048(5) 0.0091(4) 0.0063(5)
O4 0.0347(6) 0.0566(7) 0.0460(7) 0.0001(5) 0.0075(5) -0.0020(5)
S1 0.0419(2) 0.0619(3) 0.0545(3) 0.0024(2) 0.0178(2) 0.0021(2)
C2 0.0439(9) 0.0419(9) 0.0450(9) 0.0048(7) 0.0124(7) 0.0021(7)
N3 0.0332(7) 0.0366(7) 0.0394(7) 0.0050(5) 0.0073(5) -0.0019(5)
N4 0.0352(7) 0.0374(7) 0.0405(7) 0.0048(5) 0.0057(5) -0.0032(5)
C5 0.0360(8) 0.0383(8) 0.0459(9) 0.0085(7) 0.0098(7) -0.0014(6)
C6 0.0348(8) 0.0453(9) 0.0543(10) 0.0102(8) 0.0052(7) -0.0061(7)
C7 0.0406(9) 0.0626(12) 0.0494(10) 0.0043(9) -0.0010(8) -0.0025(8)
C8 0.0327(7) 0.0298(7) 0.0453(8) 0.0049(6) 0.0063(6) -0.0033(6)
C9 0.0417(9) 0.0530(10) 0.0453(9) 0.0118(8) 0.0047(7) -0.0032(8)
C10 0.0380(9) 0.0505(10) 0.0599(11) 0.0103(8) -0.0028(8) -0.0020(8)
C11 0.0337(8) 0.0335(8) 0.0754(13) -0.0013(8) 0.0123(8) -0.0017(6)
C12 0.0423(9) 0.0388(9) 0.0615(11) -0.0054(7) 0.0199(8) -0.0015(7)
C13 0.0369(8) 0.0357(8) 0.0461(9) -0.0027(6) 0.0081(7) -0.0018(6)
C14 0.0371(10) 0.0566(12) 0.1058(19) -0.0109(12) 0.0163(11) -0.0023(9)
S21 0.03328(19) 0.0436(2) 0.03110(18) -0.00381(14) 0.01156(14) -0.00022(15)
C22 0.0350(7) 0.0345(7) 0.0300(7) -0.0018(5) 0.0127(6) 0.0005(6)
N23 0.0310(6) 0.0348(6) 0.0250(5) -0.0001(4) 0.0086(5) -0.0013(5)
N24 0.0346(6) 0.0347(6) 0.0252(5) 0.0002(4) 0.0074(5) -0.0024(5)
C25 0.0356(7) 0.0306(7) 0.0287(6) -0.0004(5) 0.0099(6) -0.0010(5)
C26 0.0372(8) 0.0370(8) 0.0329(7) 0.0005(6) 0.0064(6) -0.0027(6)
C27 0.0483(10) 0.0771(13) 0.0300(8) 0.0053(8) 0.0047(7) -0.0071(9)
C28 0.0315(7) 0.0303(7) 0.0299(7) -0.0019(5) 0.0109(5) -0.0013(5)
C29 0.0379(8) 0.0541(10) 0.0329(7) 0.0073(7) 0.0112(6) 0.0018(7)
C30 0.0353(8) 0.0587(11) 0.0389(8) 0.0040(7) 0.0066(7) 0.0045(7)
C31 0.0342(8) 0.0402(8) 0.0509(9) -0.0070(7) 0.0159(7) -0.0008(6)
C32 0.0446(9) 0.0530(10) 0.0459(9) 0.0037(7) 0.0255(7) 0.0011(7)
C33 0.0399(8) 0.0506(9) 0.0317(7) 0.0064(6) 0.0145(6) 0.0048(7)
C34 0.0393(9) 0.0680(13) 0.0710(13) -0.0056(10) 0.0237(9) 0.0008(9)

_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
O1 C2 1.208(2) . ?
O2 C6 1.216(2) . ?
O3 C22 1.2058(17) . ?
O4 C26 1.2168(19) . ?
S1 C5 1.7321(18) . ?
S1 C2 1.7772(18) . ?
C2 N3 1.397(2) . ?
N3 N4 1.3600(18) . ?
N3 C8 1.437(2) . ?
N4 C5 1.291(2) . ?
C5 C6 1.486(2) . ?
C6 C7 1.489(3) . ?
C8 C13 1.388(2) . ?
C8 C9 1.388(2) . ?
C9 C10 1.390(3) . ?
C10 C11 1.386(3) . ?
C11 C12 1.390(3) . ?
C11 C14 1.514(3) . ?
C12 C13 1.390(2) . ?
S21 C25 1.7312(15) . ?
S21 C22 1.7765(16) . ?
C22 N23 1.4005(17) . ?
N23 N24 1.3616(16) . ?
N23 C28 1.4347(18) . ?
N24 C25 1.2936(19) . ?
C25 C26 1.483(2) . ?
C26 C27 1.499(2) . ?
C28 C29 1.385(2) . ?
C28 C33 1.388(2) . ?
C29 C30 1.389(2) . ?
C30 C31 1.392(2) . ?
C31 C32 1.379(2) . ?
C31 C34 1.518(2) . ?
C32 C33 1.388(2) . ?
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
C5 S1 C2 88.91(8) . . ?
O1 C2 N3 127.17(17) . . ?
O1 C2 S1 125.91(15) . . ?
N3 C2 S1 106.91(12) . . ?
N4 N3 C2 116.74(13) . . ?
N4 N3 C8 117.14(13) . . ?
C2 N3 C8 126.00(14) . . ?
C5 N4 N3 111.29(14) . . ?
N4 C5 C6 122.53(16) . . ?
N4 C5 S1 116.01(13) . . ?
C6 C5 S1 121.39(13) . . ?
O2 C6 C5 118.27(18) . . ?
O2 C6 C7 124.13(17) . . ?
C5 C6 C7 117.59(15) . . ?
C13 C8 C9 120.53(16) . . ?
C13 C8 N3 118.92(14) . . ?
C9 C8 N3 120.54(15) . . ?
C8 C9 C10 118.85(18) . . ?
C11 C10 C9 122.06(17) . . ?
C10 C11 C12 117.73(16) . . ?
C10 C11 C14 120.95(18) . . ?
C12 C11 C14 121.3(2) . . ?
C11 C12 C13 121.65(18) . . ?
C8 C13 C12 119.16(16) . . ?
C25 S21 C22 88.54(7) . . ?
O3 C22 N23 126.12(14) . . ?
O3 C22 S21 126.77(12) . . ?
N23 C22 S21 107.11(10) . . ?
N24 N23 C22 117.02(12) . . ?
N24 N23 C28 118.03(11) . . ?
C22 N23 C28 124.88(12) . . ?
C25 N24 N23 110.37(11) . . ?
N24 C25 C26 122.78(13) . . ?
N24 C25 S21 116.92(11) . . ?
C26 C25 S21 120.29(11) . . ?
O4 C26 C25 118.46(14) . . ?
O4 C26 C27 123.56(15) . . ?
C25 C26 C27 117.96(14) . . ?
C29 C28 C33 119.85(14) . . ?
C29 C28 N23 121.35(13) . . ?
C33 C28 N23 118.80(13) . . ?
C28 C29 C30 119.37(14) . . ?
C29 C30 C31 121.76(15) . . ?
C32 C31 C30 117.56(15) . . ?
C32 C31 C34 121.67(16) . . ?
C30 C31 C34 120.76(16) . . ?
C31 C32 C33 121.90(15) . . ?
C32 C33 C28 119.55(15) . . ?
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
C5 S1 C2 O1 175.76(18) . . . . ?
C5 S1 C2 N3 -3.44(12) . . . . ?
O1 C2 N3 N4 -175.13(17) . . . . ?
S1 C2 N3 N4 4.06(17) . . . . ?
O1 C2 N3 C8 0.7(3) . . . . ?
S1 C2 N3 C8 179.88(11) . . . . ?
C2 N3 N4 C5 -2.38(19) . . . . ?
C8 N3 N4 C5 -178.58(13) . . . . ?
N3 N4 C5 C6 176.36(14) . . . . ?
N3 N4 C5 S1 -0.64(18) . . . . ?
C2 S1 C5 N4 2.51(14) . . . . ?
C2 S1 C5 C6 -174.54(14) . . . . ?
N4 C5 C6 O2 -178.82(17) . . . . ?
S1 C5 C6 O2 -2.0(2) . . . . ?
N4 C5 C6 C7 0.3(2) . . . . ?
S1 C5 C6 C7 177.19(13) . . . . ?
N4 N3 C8 C13 20.2(2) . . . . ?
C2 N3 C8 C13 -155.55(16) . . . . ?
N4 N3 C8 C9 -158.42(15) . . . . ?
C2 N3 C8 C9 25.8(2) . . . . ?
C13 C8 C9 C10 1.4(3) . . . . ?
N3 C8 C9 C10 -179.95(15) . . . . ?
C8 C9 C10 C11 -0.9(3) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C9 C10 C11 C14 178.80(18) . . . . ?
C10 C11 C12 C13 1.0(3) . . . . ?
C14 C11 C12 C13 -178.10(16) . . . . ?
C9 C8 C13 C12 -0.7(2) . . . . ?
N3 C8 C13 C12 -179.40(14) . . . . ?
C11 C12 C13 C8 -0.5(2) . . . . ?
C25 S21 C22 O3 -179.29(15) . . . . ?
C25 S21 C22 N23 1.04(10) . . . . ?
O3 C22 N23 N24 178.34(15) . . . . ?
S21 C22 N23 N24 -1.98(15) . . . . ?
O3 C22 N23 C28 1.5(2) . . . . ?
S21 C22 N23 C28 -178.78(11) . . . . ?
C22 N23 N24 C25 2.05(17) . . . . ?
C28 N23 N24 C25 179.08(12) . . . . ?
N23 N24 C25 C26 180.00(13) . . . . ?
N23 N24 C25 S21 -1.13(16) . . . . ?
C22 S21 C25 N24 0.03(12) . . . . ?
C22 S21 C25 C26 178.93(12) . . . . ?
N24 C25 C26 O4 -174.18(15) . . . . ?
S21 C25 C26 O4 7.0(2) . . . . ?
N24 C25 C26 C27 7.7(2) . . . . ?
S21 C25 C26 C27 -171.16(13) . . . . ?
N24 N23 C28 C29 156.13(14) . . . . ?
C22 N23 C28 C29 -27.1(2) . . . . ?
N24 N23 C28 C33 -23.12(19) . . . . ?
C22 N23 C28 C33 153.65(15) . . . . ?
C33 C28 C29 C30 -1.1(2) . . . . ?
N23 C28 C29 C30 179.65(15) . . . . ?
C28 C29 C30 C31 1.1(3) . . . . ?
C29 C30 C31 C32 -0.5(3) . . . . ?
C29 C30 C31 C34 178.65(17) . . . . ?
C30 C31 C32 C33 -0.1(3) . . . . ?
C34 C31 C32 C33 -179.20(17) . . . . ?
C31 C32 C33 C28 0.0(3) . . . . ?
C29 C28 C33 C32 0.6(2) . . . . ?
N23 C28 C33 C32 179.82(14) . . . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.047