data_2007src1287

#Dr. I. Collins
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C18 H14 N4 O'
_chemical_formula_weight          302.33
 
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'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    Pbca
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    14.7295(4)
_cell_length_b                    14.7023(4)
_cell_length_c                    26.7711(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      5797.5(3)
_cell_formula_units_Z             16
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6689
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Slab
_exptl_crystal_colour             Colourless
_exptl_crystal_size_max           0.34
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.386
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2528
_exptl_absorpt_coefficient_mu     0.090
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9700
_exptl_absorpt_correction_T_max   0.9955
_exptl_absorpt_process_details       'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details
;
SADABS was used to perform the Absorption correction
Estimated minimum and maximum transmission: 0.6766 0.7456
The given Tmin and Tmax were generated using the SHELX SIZE command
;


_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type   
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             26155
_diffrn_reflns_av_R_equivalents   0.0498
_diffrn_reflns_av_sigmaI/netI     0.0516
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          3.01
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6537
_reflns_number_gt                 5012
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   'WinGX (Farrugia, 1999)'
 
_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)+(0.0100P)²+9.3860P] 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      SHELXL
_refine_ls_extinction_coef        0.00071(13)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6537
_refine_ls_number_parameters      428
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0912
_refine_ls_R_factor_gt            0.0654
_refine_ls_wR_factor_ref          0.1346
_refine_ls_wR_factor_gt           0.1202
_refine_ls_goodness_of_fit_ref    1.107
_refine_ls_restrained_S_all       1.107
_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
C1 C 0.18630(15) 0.44979(15) 0.04885(8) 0.0178(5) Uani 1 1 d . . .
C2 C 0.25282(15) 0.45040(15) 0.08744(8) 0.0176(4) Uani 1 1 d . . .
C3 C 0.33021(16) 0.50722(16) 0.08666(8) 0.0200(5) Uani 1 1 d . . .
C4 C 0.33766(16) 0.57449(16) 0.04786(8) 0.0206(5) Uani 1 1 d . . .
H4 H 0.3859 0.6174 0.0476 0.025 Uiso 1 1 calc R . .
C5 C 0.27359(16) 0.57441(15) 0.01178(8) 0.0189(5) Uani 1 1 d . . .
C6 C 0.26521(16) 0.39097(15) 0.12721(8) 0.0194(5) Uani 1 1 d . . .
C7 C 0.27546(15) 0.63762(16) -0.03149(8) 0.0192(5) Uani 1 1 d . . .
C8 C 0.30167(16) 0.72824(16) -0.02487(9) 0.0238(5) Uani 1 1 d . . .
H8 H 0.3199 0.7488 0.0072 0.029 Uiso 1 1 calc R . .
C9 C 0.30119(17) 0.78809(17) -0.06475(9) 0.0258(5) Uani 1 1 d . . .
H9 H 0.3181 0.8498 -0.0597 0.031 Uiso 1 1 calc R . .
C10 C 0.27623(17) 0.75875(17) -0.11196(9) 0.0263(5) Uani 1 1 d . . .
H10 H 0.2758 0.8000 -0.1393 0.032 Uiso 1 1 calc R . .
C11 C 0.25184(18) 0.66855(17) -0.11896(9) 0.0256(5) Uani 1 1 d . . .
H11 H 0.2357 0.6478 -0.1514 0.031 Uiso 1 1 calc R . .
C12 C 0.25075(17) 0.60842(16) -0.07927(8) 0.0227(5) Uani 1 1 d . . .
H12 H 0.2331 0.5470 -0.0845 0.027 Uiso 1 1 calc R . .
C13 C 0.39651(17) 0.36522(16) 0.18478(8) 0.0219(5) Uani 1 1 d . . .
C14 C 0.48728(18) 0.34668(18) 0.17617(9) 0.0287(6) Uani 1 1 d . . .
H14 H 0.5165 0.3689 0.1470 0.034 Uiso 1 1 calc R . .
C15 C 0.53512(19) 0.2952(2) 0.21072(10) 0.0353(7) Uani 1 1 d . . .
H15 H 0.5975 0.2821 0.2052 0.042 Uiso 1 1 calc R . .
C16 C 0.4923(2) 0.26287(18) 0.25329(10) 0.0320(6) Uani 1 1 d . . .
H16 H 0.5250 0.2272 0.2767 0.038 Uiso 1 1 calc R . .
C17 C 0.40159(19) 0.28281(17) 0.26151(9) 0.0289(6) Uani 1 1 d . . .
H17 H 0.3723 0.2605 0.2907 0.035 Uiso 1 1 calc R . .
C18 C 0.35322(18) 0.33493(17) 0.22763(8) 0.0251(5) Uani 1 1 d . . .
H18 H 0.2914 0.3497 0.2337 0.030 Uiso 1 1 calc R . .
N1 N 0.20129(13) 0.51286(12) 0.01196(7) 0.0186(4) Uani 1 1 d . . .
H1 H 0.1629 0.5147 -0.0132 0.022 Uiso 1 1 calc R . .
N2 N 0.38922(14) 0.48588(13) 0.12268(7) 0.0234(4) Uani 1 1 d . . .
N3 N 0.34645(13) 0.41422(13) 0.14767(7) 0.0208(4) Uani 1 1 d . . .
N4 N 0.20923(14) 0.32281(14) 0.14405(7) 0.0220(4) Uani 1 1 d D . .
H4A H 0.1666(14) 0.3123(19) 0.1214(8) 0.033 Uiso 1 1 d D . .
H4B H 0.2383(17) 0.2731(12) 0.1543(10) 0.033 Uiso 1 1 d D . .
O1 O 0.12093(11) 0.39600(11) 0.04734(6) 0.0215(4) Uani 1 1 d . . .
C21 C -0.00594(15) 0.57234(15) 0.06987(8) 0.0186(5) Uani 1 1 d . . .
C22 C 0.05742(16) 0.58833(15) 0.10927(8) 0.0188(5) Uani 1 1 d . . .
C23 C 0.12219(16) 0.65933(15) 0.10768(8) 0.0196(5) Uani 1 1 d . . .
C24 C 0.12292(16) 0.72042(16) 0.06631(8) 0.0215(5) Uani 1 1 d . . .
H24 H 0.1640 0.7702 0.0651 0.026 Uiso 1 1 calc R . .
C25 C 0.06341(16) 0.70509(15) 0.02902(8) 0.0193(5) Uani 1 1 d . . .
C26 C 0.07589(16) 0.54107(15) 0.15310(8) 0.0196(5) Uani 1 1 d . . .
C27 C 0.05898(15) 0.76322(16) -0.01631(8) 0.0200(5) Uani 1 1 d . . .
C28 C 0.07493(17) 0.85692(16) -0.01251(10) 0.0260(5) Uani 1 1 d . . .
H28 H 0.0883 0.8831 0.0191 0.031 Uiso 1 1 calc R . .
C29 C 0.07135(17) 0.91171(17) -0.05465(10) 0.0296(6) Uani 1 1 d . . .
H29 H 0.0823 0.9752 -0.0518 0.036 Uiso 1 1 calc R . .
C30 C 0.05185(17) 0.87387(18) -0.10090(9) 0.0290(6) Uani 1 1 d . . .
H30 H 0.0488 0.9114 -0.1297 0.035 Uiso 1 1 calc R . .
C31 C 0.03687(17) 0.78124(19) -0.10493(9) 0.0281(6) Uani 1 1 d . . .
H31 H 0.0236 0.7554 -0.1366 0.034 Uiso 1 1 calc R . .
C32 C 0.04107(16) 0.72572(17) -0.06311(8) 0.0220(5) Uani 1 1 d . . .
H32 H 0.0317 0.6621 -0.0664 0.026 Uiso 1 1 calc R . .
C33 C 0.19391(16) 0.56466(16) 0.22021(8) 0.0207(5) Uani 1 1 d . . .
C34 C 0.28659(17) 0.58129(16) 0.22188(9) 0.0242(5) Uani 1 1 d . . .
H34 H 0.3174 0.6035 0.1932 0.029 Uiso 1 1 calc R . .
C35 C 0.33385(18) 0.56508(17) 0.26585(9) 0.0269(5) Uani 1 1 d . . .
H35 H 0.3973 0.5765 0.2673 0.032 Uiso 1 1 calc R . .
C36 C 0.28915(18) 0.53238(17) 0.30761(9) 0.0268(6) Uani 1 1 d . . .
H36 H 0.3217 0.5215 0.3377 0.032 Uiso 1 1 calc R . .
C37 C 0.19697(18) 0.51561(18) 0.30535(9) 0.0280(6) Uani 1 1 d . . .
H37 H 0.1664 0.4927 0.3340 0.034 Uiso 1 1 calc R . .
C38 C 0.14834(18) 0.53183(17) 0.26176(9) 0.0259(5) Uani 1 1 d . . .
H38 H 0.0849 0.5206 0.2605 0.031 Uiso 1 1 calc R . .
N21 N 0.00333(13) 0.63201(13) 0.03059(7) 0.0190(4) Uani 1 1 d . . .
H21 H -0.0315 0.6233 0.0043 0.023 Uiso 1 1 calc R . .
N22 N 0.17715(14) 0.65822(13) 0.14708(7) 0.0217(4) Uani 1 1 d . . .
N23 N 0.14644(14) 0.58497(13) 0.17519(7) 0.0208(4) Uani 1 1 d . . .
N24 N 0.03230(15) 0.46646(14) 0.17232(8) 0.0255(5) Uani 1 1 d D . .
H24A H -0.0069(16) 0.4430(18) 0.1506(9) 0.038 Uiso 1 1 d D . .
H24B H 0.0661(17) 0.4279(16) 0.1903(9) 0.038 Uiso 1 1 d D . .
O21 O -0.06539(11) 0.51175(11) 0.06957(6) 0.0230(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 O1 1.247(3) . ?
C1 N1 1.373(3) . ?
C1 C2 1.424(3) . ?
C2 C6 1.389(3) . ?
C2 C3 1.414(3) . ?
C3 N2 1.336(3) . ?
C3 C4 1.438(3) . ?
C4 C5 1.350(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.397(3) . ?
C5 C7 1.485(3) . ?
C6 N3 1.360(3) . ?
C6 N4 1.374(3) . ?
C7 C12 1.397(3) . ?
C7 C8 1.398(3) . ?
C8 C9 1.383(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.384(4) . ?
C13 C18 1.386(3) . ?
C13 N3 1.432(3) . ?
C14 C15 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
N1 H1 0.8800 . ?
N2 N3 1.398(3) . ?
N4 H4A 0.887(10) . ?
N4 H4B 0.891(10) . ?
C21 O21 1.249(3) . ?
C21 N21 1.376(3) . ?
C21 C22 1.428(3) . ?
C22 C26 1.391(3) . ?
C22 C23 1.415(3) . ?
C23 N22 1.330(3) . ?
C23 C24 1.426(3) . ?
C24 C25 1.347(3) . ?
C24 H24 0.9500 . ?
C25 N21 1.393(3) . ?
C25 C27 1.486(3) . ?
C26 N23 1.359(3) . ?
C26 N24 1.371(3) . ?
C27 C32 1.394(3) . ?
C27 C28 1.401(3) . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.384(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.387(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.386(3) . ?
C33 C34 1.388(3) . ?
C33 N23 1.425(3) . ?
C34 C35 1.388(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.390(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
N21 H21 0.8800 . ?
N22 N23 1.390(3) . ?
N24 H24A 0.890(10) . ?
N24 H24B 0.894(10) . ?
 
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
O1 C1 N1 122.0(2) . . ?
O1 C1 C2 124.0(2) . . ?
N1 C1 C2 114.0(2) . . ?
C6 C2 C3 106.1(2) . . ?
C6 C2 C1 130.0(2) . . ?
C3 C2 C1 123.2(2) . . ?
N2 C3 C2 112.0(2) . . ?
N2 C3 C4 129.3(2) . . ?
C2 C3 C4 118.6(2) . . ?
C5 C4 C3 117.5(2) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C4 C5 N1 122.1(2) . . ?
C4 C5 C7 123.0(2) . . ?
N1 C5 C7 114.95(19) . . ?
N3 C6 N4 125.4(2) . . ?
N3 C6 C2 105.4(2) . . ?
N4 C6 C2 129.1(2) . . ?
C12 C7 C8 118.7(2) . . ?
C12 C7 C5 121.1(2) . . ?
C8 C7 C5 120.2(2) . . ?
C9 C8 C7 120.5(2) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 119.3(2) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 120.7(2) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 120.3(2) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 121.3(2) . . ?
C14 C13 N3 118.8(2) . . ?
C18 C13 N3 119.9(2) . . ?
C13 C14 C15 119.1(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 119.8(2) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C18 C17 C16 120.6(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 118.9(2) . . ?
C17 C18 H18 120.6 . . ?
C13 C18 H18 120.6 . . ?
C1 N1 C5 124.22(19) . . ?
C1 N1 H1 117.9 . . ?
C5 N1 H1 117.9 . . ?
C3 N2 N3 103.26(18) . . ?
C6 N3 N2 113.16(18) . . ?
C6 N3 C13 127.32(19) . . ?
N2 N3 C13 118.63(19) . . ?
C6 N4 H4A 109.2(18) . . ?
C6 N4 H4B 114.2(19) . . ?
H4A N4 H4B 114(3) . . ?
O21 C21 N21 121.3(2) . . ?
O21 C21 C22 125.5(2) . . ?
N21 C21 C22 113.24(19) . . ?
C26 C22 C23 105.2(2) . . ?
C26 C22 C21 132.0(2) . . ?
C23 C22 C21 122.7(2) . . ?
N22 C23 C22 112.2(2) . . ?
N22 C23 C24 128.3(2) . . ?
C22 C23 C24 119.6(2) . . ?
C25 C24 C23 117.7(2) . . ?
C25 C24 H24 121.1 . . ?
C23 C24 H24 121.1 . . ?
C24 C25 N21 121.3(2) . . ?
C24 C25 C27 122.5(2) . . ?
N21 C25 C27 116.14(19) . . ?
N23 C26 N24 125.1(2) . . ?
N23 C26 C22 106.2(2) . . ?
N24 C26 C22 128.7(2) . . ?
C32 C27 C28 119.1(2) . . ?
C32 C27 C25 121.0(2) . . ?
C28 C27 C25 119.9(2) . . ?
C29 C28 C27 120.4(2) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.1(2) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 119.8(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.6(2) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 120.1(2) . . ?
C31 C32 H32 120.0 . . ?
C27 C32 H32 120.0 . . ?
C38 C33 C34 120.8(2) . . ?
C38 C33 N23 120.9(2) . . ?
C34 C33 N23 118.2(2) . . ?
C33 C34 C35 119.4(2) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C36 C35 C34 120.4(2) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C37 C36 C35 119.6(2) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 120.9(2) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C33 C38 C37 119.0(2) . . ?
C33 C38 H38 120.5 . . ?
C37 C38 H38 120.5 . . ?
C21 N21 C25 125.31(19) . . ?
C21 N21 H21 117.3 . . ?
C25 N21 H21 117.3 . . ?
C23 N22 N23 103.94(18) . . ?
C26 N23 N22 112.43(18) . . ?
C26 N23 C33 130.1(2) . . ?
N22 N23 C33 117.43(18) . . ?
C26 N24 H24A 111.6(19) . . ?
C26 N24 H24B 116.6(19) . . ?
H24A N24 H24B 118(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
N1 H1 O21  0.88 2.12 2.984(2) 167.2 5_565
N4 H4A O1  0.887(10) 2.43(2) 3.091(3) 132(2) .
N4 H4B N22  0.891(10) 2.107(15) 2.943(3) 156(2) 8_655
N21 H21 O1  0.88 1.93 2.806(2) 172.7 5_565
N24 H24A O21  0.890(10) 2.54(2) 3.175(3) 129(2) .
 
_diffrn_measured_fraction_theta_max    0.985
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.985
_refine_diff_density_max    0.320
_refine_diff_density_min   -0.263
_refine_diff_density_rms    0.062
