 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-10-03 at 15:36:20
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf023 dreduc struct sortav
 
 
data_ljf023
 
_audit_creation_date            2000-10-03T15:36:20-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 6,7-diphenyl-13H-dibenzo[a,i]carbazole
;
_chemical_formula_moiety                'C32 H21 N'
_chemical_formula_structural            'C32 H21 N'
_chemical_formula_sum                   'C32 H21 N'
_chemical_formula_weight                419.5
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  orthorhombic
_symmetry_space_group_name_H-M          'P c a b'
_symmetry_space_group_name_Hall         '-P 2bc 2ac'
_symmetry_Int_Tables_number             61
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, z'
 
_cell_length_a                          13.6545(3)
_cell_length_b                          15.2033(3)
_cell_length_c                          20.1647(5)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            4186.06(16)
_cell_formula_units_Z                   8
_cell_measurement_temperature           150(2)
_cell_measurement_reflns_used           5221
_cell_measurement_theta_min             3.395
_cell_measurement_theta_max             27.485
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   pale-yellow
_exptl_crystal_size_max                 0.4
_exptl_crystal_size_mid                 0.27
_exptl_crystal_size_min                 0.15
_exptl_crystal_density_diffrn           1.331
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1760
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.077
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.922
_exptl_absorpt_correction_T_max         1.052
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             150(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             0.20799E-1
_diffrn_orient_matrix_ub_12             0.25881E-1
_diffrn_orient_matrix_ub_13             0.652775E-1
_diffrn_orient_matrix_ub_21             -0.617793E-1
_diffrn_orient_matrix_ub_22             0.190405E-1
_diffrn_orient_matrix_ub_23             0.121352E-1
_diffrn_orient_matrix_ub_31             -0.95623E-2
_diffrn_orient_matrix_ub_32             -0.441152E-1
_diffrn_orient_matrix_ub_33             0.205374E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_number                   30310
_diffrn_reflns_av_R_equivalents         0.0816
_diffrn_reflns_av_unetI/netI            0.0705
_diffrn_reflns_limit_h_min              0
_diffrn_reflns_limit_h_max              17
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              19
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              26
_diffrn_reflns_theta_min                3.42
_diffrn_reflns_theta_max                27.46
_diffrn_reflns_theta_full               27.46
_diffrn_measured_fraction_theta_full
                                        0.997
_diffrn_measured_fraction_theta_max
                                        0.997
_reflns_number_total                    4781
_reflns_number_gt                       3030
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution           'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_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)+(0.0644P)²+0.0000P] 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_number_reflns                4781
_refine_ls_number_parameters            302
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0952
_refine_ls_R_factor_gt                  0.0479
_refine_ls_wR_factor_ref                0.1179
_refine_ls_wR_factor_gt                 0.1054
_refine_ls_goodness_of_fit_ref          0.981
_refine_ls_restrained_S_all             0.981
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.231
_refine_diff_density_min                -0.212
_refine_diff_density_rms                0.045
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
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 0 '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'
 
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 0.14765(9) 0.19030(10) 0.17180(7) 0.0262(3) Uani 1 1 d . . .
H1 H 0.1717 0.2267 0.1372 0.031 Uiso 1 1 calc R . .
C2 C 0.10957(9) 0.11012(10) 0.15698(7) 0.0291(4) Uani 1 1 d . . .
H2 H 0.1096 0.0901 0.1124 0.035 Uiso 1 1 calc R . .
C3 C 0.07008(10) 0.05644(10) 0.20732(7) 0.0296(4) Uani 1 1 d . . .
H3 H 0.0426 0.0008 0.1965 0.036 Uiso 1 1 calc R . .
C4 C 0.07143(9) 0.08475(10) 0.27213(7) 0.0269(4) Uani 1 1 d . . .
H4 H 0.0429 0.0491 0.3056 0.032 Uiso 1 1 calc R . .
C4A C 0.11443(9) 0.16584(9) 0.28971(7) 0.0236(3) Uani 1 1 d . . .
C5 C 0.11924(9) 0.19517(9) 0.35664(7) 0.0238(3) Uani 1 1 d . . .
H5 H 0.0902 0.1596 0.39 0.029 Uiso 1 1 calc R . .
C6 C 0.16369(9) 0.27234(9) 0.37551(7) 0.0218(3) Uani 1 1 d . . .
C6A C 0.20955(9) 0.32500(9) 0.32513(7) 0.0217(3) Uani 1 1 d . . .
C7 C 0.32067(9) 0.45592(9) 0.37209(7) 0.0220(3) Uani 1 1 d . . .
C7A C 0.26804(9) 0.40526(9) 0.32384(7) 0.0222(3) Uani 1 1 d . . .
C8 C 0.36331(9) 0.53338(10) 0.35176(7) 0.0245(3) Uani 1 1 d . . .
H8 H 0.3949 0.5689 0.3841 0.029 Uiso 1 1 calc R . .
C8A C 0.36261(9) 0.56301(9) 0.28472(7) 0.0240(3) Uani 1 1 d . . .
C9 C 0.40948(10) 0.64173(10) 0.26547(7) 0.0269(4) Uani 1 1 d . . .
H9 H 0.4396 0.6776 0.2982 0.032 Uiso 1 1 calc R . .
C10 C 0.41226(10) 0.66738(10) 0.20018(8) 0.0304(4) Uani 1 1 d . . .
H10 H 0.4429 0.7212 0.1882 0.037 Uiso 1 1 calc R . .
C11 C 0.36924(10) 0.61338(10) 0.15043(7) 0.0273(4) Uani 1 1 d . . .
H11 H 0.372 0.6305 0.1052 0.033 Uiso 1 1 calc R . .
C12 C 0.32391(10) 0.53680(10) 0.16813(7) 0.0278(4) Uani 1 1 d . . .
H12 H 0.2944 0.5014 0.1348 0.033 Uiso 1 1 calc R . .
C12A C 0.31997(9) 0.50920(10) 0.23498(7) 0.0228(3) Uani 1 1 d . . .
C12B C 0.27616(9) 0.42970(9) 0.25704(7) 0.0219(3) Uani 1 1 d . . .
C13A C 0.19513(9) 0.30127(9) 0.25848(7) 0.0220(3) Uani 1 1 d . . .
C13B C 0.15191(9) 0.22018(9) 0.23817(7) 0.0229(3) Uani 1 1 d . . .
C14 C 0.15130(9) 0.30118(10) 0.44571(7) 0.0227(3) Uani 1 1 d . . .
C15 C 0.16951(9) 0.24371(10) 0.49786(7) 0.0267(4) Uani 1 1 d . . .
H15 H 0.1968 0.1875 0.4888 0.032 Uiso 1 1 calc R . .
C16 C 0.14871(10) 0.26672(11) 0.56253(7) 0.0313(4) Uani 1 1 d . . .
H16 H 0.1619 0.2265 0.5974 0.038 Uiso 1 1 calc R . .
C17 C 0.10893(10) 0.34780(12) 0.57664(8) 0.0341(4) Uani 1 1 d . . .
H17 H 0.0936 0.3634 0.6211 0.041 Uiso 1 1 calc R . .
C18 C 0.09138(10) 0.40649(11) 0.52543(8) 0.0335(4) Uani 1 1 d . . .
H18 H 0.0652 0.463 0.535 0.04 Uiso 1 1 calc R . .
C19 C 0.11172(10) 0.38347(10) 0.46038(7) 0.0280(4) Uani 1 1 d . . .
H19 H 0.0986 0.424 0.4256 0.034 Uiso 1 1 calc R . .
C20 C 0.34588(9) 0.42345(10) 0.43961(7) 0.0237(3) Uani 1 1 d . . .
C21 C 0.38141(9) 0.33769(10) 0.44774(7) 0.0263(4) Uani 1 1 d . . .
H21 H 0.3812 0.2984 0.4111 0.032 Uiso 1 1 calc R . .
C22 C 0.41673(10) 0.30940(11) 0.50824(8) 0.0335(4) Uani 1 1 d . . .
H22 H 0.4407 0.251 0.5129 0.04 Uiso 1 1 calc R . .
C23 C 0.41739(11) 0.36556(12) 0.56200(8) 0.0360(4) Uani 1 1 d . . .
H23 H 0.4423 0.3462 0.6035 0.043 Uiso 1 1 calc R . .
C24 C 0.38180(11) 0.44966(12) 0.55510(8) 0.0374(4) Uani 1 1 d . . .
H24 H 0.3815 0.4882 0.5922 0.045 Uiso 1 1 calc R . .
C25 C 0.34618(10) 0.47882(11) 0.49439(7) 0.0328(4) Uani 1 1 d . . .
H25 H 0.3218 0.5371 0.4903 0.039 Uiso 1 1 calc R . .
N13 N 0.23329(8) 0.36560(8) 0.21862(6) 0.0249(3) Uani 1 1 d . . .
H13 H 0.2302(10) 0.3650(9) 0.1754(8) 0.034(5) Uiso 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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 C2 1.359(2) . ?
C1 C13B 1.4145(19) . ?
C2 C3 1.410(2) . ?
C3 C4 1.3760(19) . ?
C4 C4A 1.4108(19) . ?
C4A C13B 1.4229(19) . ?
C4A C5 1.4228(19) . ?
C5 C6 1.3746(19) . ?
C6 C6A 1.4370(18) . ?
C6 C14 1.4916(19) . ?
C6A C13A 1.4055(19) . ?
C6A C7A 1.4587(19) . ?
C7 C8 1.3762(19) . ?
C7 C7A 1.4339(19) . ?
C7 C20 1.4887(19) . ?
C7A C12B 1.4017(19) . ?
C8 C8A 1.4250(19) . ?
C8A C9 1.412(2) . ?
C8A C12A 1.4192(19) . ?
C9 C10 1.374(2) . ?
C10 C11 1.423(2) . ?
C11 C12 1.366(2) . ?
C12 C12A 1.4128(18) . ?
C12A C12B 1.4201(19) . ?
C12B N13 1.3757(18) . ?
C13A N13 1.3688(18) . ?
C13A C13B 1.427(2) . ?
C14 C15 1.3897(19) . ?
C14 C19 1.394(2) . ?
C15 C16 1.3796(19) . ?
C16 C17 1.377(2) . ?
C17 C18 1.386(2) . ?
C18 C19 1.386(2) . ?
C20 C25 1.389(2) . ?
C20 C21 1.401(2) . ?
C21 C22 1.3805(19) . ?
C22 C23 1.380(2) . ?
C23 C24 1.375(2) . ?
C24 C25 1.390(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
C2 C1 C13B 120.80(14) . . ?
C1 C2 C3 120.49(14) . . ?
C4 C3 C2 119.84(14) . . ?
C3 C4 C4A 121.17(14) . . ?
C4 C4A C13B 118.26(13) . . ?
C4 C4A C5 122.10(13) . . ?
C13B C4A C5 119.62(13) . . ?
C6 C5 C4A 123.39(13) . . ?
C5 C6 C6A 118.18(12) . . ?
C5 C6 C14 117.62(12) . . ?
C6A C6 C14 123.82(13) . . ?
C13A C6A C6 118.17(12) . . ?
C13A C6A C7A 105.92(12) . . ?
C6 C6A C7A 135.83(13) . . ?
C8 C7 C7A 118.01(13) . . ?
C8 C7 C20 117.28(12) . . ?
C7A C7 C20 123.94(12) . . ?
C12B C7A C7 118.03(12) . . ?
C12B C7A C6A 106.39(12) . . ?
C7 C7A C6A 135.37(13) . . ?
C7 C8 C8A 123.38(13) . . ?
C9 C8A C12A 118.71(13) . . ?
C9 C8A C8 121.72(13) . . ?
C12A C8A C8 119.40(13) . . ?
C10 C9 C8A 121.11(14) . . ?
C9 C10 C11 120.03(14) . . ?
C12 C11 C10 119.63(14) . . ?
C11 C12 C12A 121.31(14) . . ?
C12 C12A C8A 119.17(13) . . ?
C12 C12A C12B 124.59(13) . . ?
C8A C12A C12B 116.24(12) . . ?
N13 C12B C7A 108.64(12) . . ?
N13 C12B C12A 127.29(13) . . ?
C7A C12B C12A 124.05(13) . . ?
N13 C13A C6A 108.95(12) . . ?
N13 C13A C13B 127.32(13) . . ?
C6A C13A C13B 123.65(13) . . ?
C1 C13B C4A 119.33(13) . . ?
C1 C13B C13A 124.48(13) . . ?
C4A C13B C13A 116.16(12) . . ?
C15 C14 C19 118.22(13) . . ?
C15 C14 C6 120.87(13) . . ?
C19 C14 C6 120.60(13) . . ?
C16 C15 C14 121.26(14) . . ?
C17 C16 C15 120.24(14) . . ?
C16 C17 C18 119.39(14) . . ?
C17 C18 C19 120.54(15) . . ?
C18 C19 C14 120.33(14) . . ?
C25 C20 C21 118.04(13) . . ?
C25 C20 C7 121.81(13) . . ?
C21 C20 C7 119.72(13) . . ?
C22 C21 C20 120.96(14) . . ?
C23 C22 C21 120.25(15) . . ?
C24 C23 C22 119.57(15) . . ?
C23 C24 C25 120.63(15) . . ?
C20 C25 C24 120.54(15) . . ?
C13A N13 C12B 109.73(12) . . ?
 
