 
data_dsak-50_rep
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C25.78 H18.67 N4.44 O2.67'
_chemical_formula_weight          433.34
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 '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'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 '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'
 '-y+1/4, x+3/4, z+1/4'
 '-x, -y+1/2, z'
 'y+1/4, -x+1/4, z+3/4'
 'x, -y, -z+1/2'
 '-x+1/2, y, -z'
 'y+3/4, x+1/4, -z+1/4'
 '-y+1/4, -x+1/4, -z+1/4'
 'x+1/2, y+1/2, z+1/2'
 '-y+3/4, x+5/4, z+3/4'
 '-x+1/2, -y+1, z+1/2'
 'y+3/4, -x+3/4, z+5/4'
 'x+1/2, -y+1/2, -z+1'
 '-x+1, y+1/2, -z+1/2'
 'y+5/4, x+3/4, -z+3/4'
 '-y+3/4, -x+3/4, -z+3/4'
 '-x, -y, -z'
 'y-1/4, -x-3/4, -z-1/4'
 'x, y-1/2, -z'
 '-y-1/4, x-1/4, -z-3/4'
 '-x, y, z-1/2'
 'x-1/2, -y, z'
 '-y-3/4, -x-1/4, z-1/4'
 'y-1/4, x-1/4, z-1/4'
 '-x+1/2, -y+1/2, -z+1/2'
 'y+1/4, -x-1/4, -z+1/4'
 'x+1/2, y, -z+1/2'
 '-y+1/4, x+1/4, -z-1/4'
 '-x+1/2, y+1/2, z'
 'x, -y+1/2, z+1/2'
 '-y-1/4, -x+1/4, z+1/4'
 'y+1/4, x+1/4, z+1/4'
 
_cell_length_a                    28.2864(11)
_cell_length_b                    28.2864(11)
_cell_length_c                    13.3571(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      10687.3(8)
_cell_formula_units_Z             18
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.212
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              4064
_exptl_absorpt_coefficient_mu     0.658
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   0.8269
_exptl_absorpt_correction_T_max   0.9371
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\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             12797
_diffrn_reflns_av_R_equivalents   0.0489
_diffrn_reflns_av_sigmaI/netI     0.0263
_diffrn_reflns_limit_h_min        -32
_diffrn_reflns_limit_h_max        33
_diffrn_reflns_limit_k_min        -32
_diffrn_reflns_limit_k_max        33
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.12
_diffrn_reflns_theta_max          66.27
_reflns_number_total              2335
_reflns_number_gt                 1872
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_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)+(0.1666P)²+20.9487P] 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        0.00001(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2335
_refine_ls_number_parameters      186
_refine_ls_number_restraints      31
_refine_ls_R_factor_all           0.1009
_refine_ls_R_factor_gt            0.0868
_refine_ls_wR_factor_ref          0.2672
_refine_ls_wR_factor_gt           0.2502
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.067
_refine_ls_shift/su_max           0.753
_refine_ls_shift/su_mean          0.011
 
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
N2 N 0.37859(9) 0.56788(10) 0.53039(18) 0.0416(7) Uani 1 1 d . . .
H1B H 0.3838 0.5405 0.5562 0.050 Uiso 1 1 calc R . .
N1 N 0.33924(10) 0.62706(10) 0.45797(19) 0.0415(7) Uani 1 1 d . . .
C1 C 0.2500 0.58043(16) 0.5000 0.0356(10) Uani 1 2 d S . .
H1 H 0(154) 0.6133(19) 1(154) 0.043 Uiso 1 2 calc S . .
C2 C 0.29284(11) 0.55627(11) 0.49736(19) 0.0362(8) Uani 1 1 d . . .
C4 C 0.2500 0.48209(16) 0.5000 0.0423(11) Uani 1 2 d S . .
C3 C 0.29259(12) 0.50696(11) 0.4983(2) 0.0404(8) Uani 1 1 d . . .
H3 H 0.3211 0.4905 0.4977 0.048 Uiso 1 1 calc R . .
C11 C 0.41109(12) 0.60372(13) 0.5188(2) 0.0448(8) Uani 1 1 d . . .
C5 C 0.33685(11) 0.58384(12) 0.4935(2) 0.0371(7) Uani 1 1 d . . .
C6 C 0.38617(12) 0.64064(13) 0.4719(2) 0.0441(8) Uani 1 1 d . . .
C7 C 0.40950(14) 0.68271(14) 0.4481(3) 0.0562(10) Uani 1 1 d . . .
H7 H 0.3938 0.7073 0.4159 0.067 Uiso 1 1 calc R . .
C10 C 0.45832(13) 0.60754(16) 0.5449(3) 0.0571(10) Uani 1 1 d . . .
H10 H 0.4744 0.5830 0.5764 0.069 Uiso 1 1 calc R . .
N3 N 0.2500 0.43283(18) 0.5000 0.0773(19) Uani 1 2 d S . .
C9 C 0.48018(15) 0.64987(18) 0.5216(3) 0.0694(13) Uani 1 1 d . . .
H9 H 0.5118 0.6540 0.5383 0.083 Uiso 1 1 calc R . .
C8 C 0.45625(15) 0.68649(16) 0.4738(3) 0.0658(11) Uani 1 1 d . . .
H8 H 0.4724 0.7143 0.4590 0.079 Uiso 1 1 calc R . .
C12 C 0.2745(3) 0.4042(3) 0.5103(4) 0.0481(16) Uani 0.50 1 d PU . .
O2 O 0.27198(10) 0.65692(10) 0.3293(2) 0.0710(10) Uani 1 1 d . . .
C17 C 0.29098(16) 0.68924(15) 0.2592(3) 0.0665(12) Uani 1 1 d . . .
O1 O 0.3170(2) 0.3605(2) 0.5246(4) 0.0618(14) Uani 0.50 1 d P . .
C16 C 0.2500 0.2549(2) 0.5000 0.080(2) Uani 1 2 d SU . .
H16 H 0(153) 0.222(3) 1(153) 0.096 Uiso 1 2 calc S . .
C15 C 0.2913(3) 0.2794(2) 0.5168(3) 0.0975(19) Uani 1 1 d U . .
H15 H 0.3195 0.2632 0.5281 0.117 Uiso 1 1 calc R . .
C14 C 0.2906(4) 0.3279(2) 0.5167(4) 0.140(3) Uani 1 1 d U . .
C13 C 0.2500 0.3527(3) 0.5000 0.163(5) Uani 1 2 d SU . .
 
 
_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
N2 C5 1.357(4) . ?
N2 C11 1.377(5) . ?
N1 C5 1.313(4) . ?
N1 C6 1.395(4) . ?
C1 C2 1.392(4) . ?
C1 C2 1.392(4) 6_556 ?
C2 C3 1.395(4) . ?
C2 C5 1.470(4) . ?
C4 C3 1.395(4) 6_556 ?
C4 C3 1.395(4) . ?
C4 N3 1.393(7) . ?
C11 C10 1.385(5) . ?
C11 C6 1.407(5) . ?
C6 C7 1.397(5) . ?
C7 C8 1.371(6) . ?
C10 C9 1.383(6) . ?
N3 C12 1.074(8) . ?
N3 C12 1.074(8) 6_556 ?
C9 C8 1.392(7) . ?
C12 C12 1.411(16) 6_556 ?
C12 C13 1.619(11) . ?
C12 O1 1.735(10) . ?
O2 C17 1.415(5) . ?
O1 C14 1.192(9) . ?
C16 C15 1.377(7) 6_556 ?
C16 C15 1.377(7) . ?
C15 C14 1.371(8) . ?
C14 C13 1.365(10) . ?
C13 C14 1.365(10) 6_556 ?
C13 C12 1.619(11) 6_556 ?
 
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 N2 C11 107.2(3) . . ?
C5 N1 C6 104.9(3) . . ?
C2 C1 C2 121.2(4) . 6_556 ?
C1 C2 C3 119.1(3) . . ?
C1 C2 C5 118.5(3) . . ?
C3 C2 C5 122.4(3) . . ?
C3 C4 C3 119.4(4) 6_556 . ?
C3 C4 N3 120.3(2) 6_556 . ?
C3 C4 N3 120.3(2) . . ?
C4 C3 C2 120.6(3) . . ?
N2 C11 C10 132.3(3) . . ?
N2 C11 C6 105.2(3) . . ?
C10 C11 C6 122.5(4) . . ?
N1 C5 N2 113.4(3) . . ?
N1 C5 C2 123.4(3) . . ?
N2 C5 C2 123.2(3) . . ?
N1 C6 C7 130.8(3) . . ?
N1 C6 C11 109.4(3) . . ?
C7 C6 C11 119.8(3) . . ?
C8 C7 C6 117.7(4) . . ?
C11 C10 C9 116.2(4) . . ?
C12 N3 C12 82.2(9) . 6_556 ?
C12 N3 C4 138.9(4) . . ?
C12 N3 C4 138.9(4) 6_556 . ?
C10 C9 C8 122.0(4) . . ?
C7 C8 C9 121.7(4) . . ?
N3 C12 C12 48.9(4) . 6_556 ?
N3 C12 C13 113.1(6) . . ?
C12 C12 C13 64.2(3) 6_556 . ?
N3 C12 O1 176.2(7) . . ?
C12 C12 O1 134.5(3) 6_556 . ?
C13 C12 O1 70.4(4) . . ?
C14 O1 C12 96.2(7) . . ?
C15 C16 C15 119.7(7) 6_556 . ?
C16 C15 C14 119.3(8) . . ?
O1 C14 C13 98.2(6) . . ?
O1 C14 C15 139.9(12) . . ?
C13 C14 C15 121.9(9) . . ?
C14 C13 C14 118.0(8) 6_556 . ?
C14 C13 C12 95.2(4) 6_556 6_556 ?
C14 C13 C12 146.9(6) . 6_556 ?
C14 C13 C12 146.9(6) 6_556 . ?
C14 C13 C12 95.2(4) . . ?
C12 C13 C12 51.7(6) 6_556 . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              66.27
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.683
_refine_diff_density_min   -0.749
_refine_diff_density_rms    0.071
