 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-09-15 at 14:12:42
#  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  : ljf021 dreduc sortav struct
 
 
data_ljf021
 
_audit_creation_date            2000-09-15T14:12:42-00:00
_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
;
 ?
;
_chemical_formula_moiety                'C13 H11 I O2'
_chemical_formula_structural            'C13 H11 I O2'
_chemical_formula_sum                   'C13 H11 I O2'
_chemical_formula_weight                326.12
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/c'
_symmetry_space_group_name_Hall         '-P 2ybc'
_symmetry_Int_Tables_number             14
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                          5.8709(2)
_cell_length_b                          14.9976(5)
_cell_length_c                          14.3802(5)
_cell_angle_alpha                       90
_cell_angle_beta                        100.5720(10)
_cell_angle_gamma                       90
_cell_volume                            1244.68(7)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)
_cell_measurement_reflns_used           4778
_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                   Colourless
_exptl_crystal_size_max                 0.25
_exptl_crystal_size_mid                 0.22
_exptl_crystal_size_min                 0.2
_exptl_crystal_density_diffrn           1.74
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    632
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           2.555
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.623
_exptl_absorpt_correction_T_max         0.74
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             293(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             0.240381E-1
_diffrn_orient_matrix_ub_12             -0.158091
_diffrn_orient_matrix_ub_13             -0.667306E-1
_diffrn_orient_matrix_ub_21             0.443408E-1
_diffrn_orient_matrix_ub_22             0.249364E-1
_diffrn_orient_matrix_ub_23             -0.431038E-1
_diffrn_orient_matrix_ub_31             0.528318E-1
_diffrn_orient_matrix_ub_32             -0.234145E-1
_diffrn_orient_matrix_ub_33             0.408023E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              CCD
_diffrn_reflns_number                   2758
_diffrn_reflns_av_R_equivalents         0.0424
_diffrn_reflns_av_unetI/netI            0.0394
_diffrn_reflns_limit_h_min              -7
_diffrn_reflns_limit_h_max              7
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              19
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              18
_diffrn_reflns_theta_min                3.53
_diffrn_reflns_theta_max                27.41
_diffrn_reflns_theta_full               27.41
_diffrn_measured_fraction_theta_full
                                        0.973
_diffrn_measured_fraction_theta_max
                                        0.973
_reflns_number_total                    2758
_reflns_number_gt                       2215
_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)+(0.0409P)²+0.6591P] 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_expression
                                    Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef              0.013(3)
_refine_ls_number_reflns                2758
_refine_ls_number_parameters            146
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0471
_refine_ls_R_factor_gt                  0.0346
_refine_ls_wR_factor_ref                0.0951
_refine_ls_wR_factor_gt                 0.0874
_refine_ls_goodness_of_fit_ref          1.038
_refine_ls_restrained_S_all             1.038
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.437
_refine_diff_density_min                -0.668
_refine_diff_density_rms                0.061
 
#----------------------------------------------------------------------------#
#                   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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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 0.3835(6) 0.4031(2) 0.5700(3) 0.0633(8) Uani 1 1 d . . .
H1A H 0.3342 0.4143 0.5029 0.076 Uiso 1 1 calc R . .
H1B H 0.5251 0.3683 0.5789 0.076 Uiso 1 1 calc R . .
C111 C 0.1181(5) 0.15515(19) 0.4559(2) 0.0571(7) Uani 1 1 d . . .
C112 C -0.0685(6) 0.1198(2) 0.4882(3) 0.0657(8) Uani 1 1 d . . .
H112 H -0.1373 0.0676 0.4617 0.079 Uiso 1 1 calc R . .
C113 C -0.1537(6) 0.1617(2) 0.5599(3) 0.0680(9) Uani 1 1 d . . .
H113 H -0.2794 0.1374 0.5821 0.082 Uiso 1 1 calc R . .
C114 C -0.0530(5) 0.23966(19) 0.5991(2) 0.0584(7) Uani 1 1 d . . .
C115 C 0.1311(5) 0.27676(18) 0.5635(2) 0.0541(6) Uani 1 1 d . . .
C116 C 0.2200(6) 0.23508(19) 0.4926(2) 0.0575(7) Uani 1 1 d . . .
H116 H 0.3445 0.2595 0.4697 0.069 Uiso 1 1 calc R . .
C211 C 0.4249(5) 0.49004(19) 0.6232(2) 0.0556(7) Uani 1 1 d . . .
C212 C 0.6261(7) 0.5038(2) 0.6863(3) 0.0812(11) Uani 1 1 d . . .
H212 H 0.7368 0.4588 0.6972 0.097 Uiso 1 1 calc R . .
C213 C 0.6666(8) 0.5838(3) 0.7340(4) 0.0952(15) Uani 1 1 d . . .
H213 H 0.8052 0.5925 0.776 0.114 Uiso 1 1 calc R . .
C214 C 0.5056(7) 0.6500(2) 0.7199(3) 0.0749(9) Uani 1 1 d . . .
H214 H 0.5327 0.7036 0.7527 0.09 Uiso 1 1 calc R . .
C215 C 0.3053(7) 0.6370(3) 0.6577(3) 0.0833(11) Uani 1 1 d . . .
H215 H 0.1948 0.6821 0.6472 0.1 Uiso 1 1 calc R . .
C216 C 0.2646(6) 0.5567(3) 0.6098(3) 0.0777(10) Uani 1 1 d . . .
H216 H 0.1257 0.5482 0.5678 0.093 Uiso 1 1 calc R . .
I1 I 0.25931(5) 0.089239(16) 0.351027(17) 0.07804(17) Uani 1 1 d . . .
O1 O -0.1341(5) 0.27875(16) 0.6721(2) 0.0818(7) Uani 1 1 d . . .
H1 H -0.0596 0.3242 0.6883 0.123 Uiso 1 1 calc R . .
O2 O 0.2080(4) 0.35586(15) 0.60607(17) 0.0694(6) Uani 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 O2 1.424(4) . ?
C1 C211 1.509(4) . ?
C1 H1A 0.97 . ?
C1 H1B 0.97 . ?
C111 C112 1.372(5) . ?
C111 C116 1.399(4) . ?
C111 I1 2.098(3) . ?
C112 C113 1.377(5) . ?
C112 H112 0.93 . ?
C113 C114 1.383(4) . ?
C113 H113 0.93 . ?
C114 O1 1.362(4) . ?
C114 C115 1.394(4) . ?
C115 O2 1.373(3) . ?
C115 C116 1.378(4) . ?
C116 H116 0.93 . ?
C211 C216 1.362(5) . ?
C211 C212 1.366(5) . ?
C212 C213 1.381(5) . ?
C212 H212 0.93 . ?
C213 C214 1.360(5) . ?
C213 H213 0.93 . ?
C214 C215 1.354(5) . ?
C214 H214 0.93 . ?
C215 C216 1.387(6) . ?
C215 H215 0.93 . ?
C216 H216 0.93 . ?
O1 H1 0.82 . ?
 
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
O2 C1 C211 107.8(3) . . ?
O2 C1 H1A 110.1 . . ?
C211 C1 H1A 110.1 . . ?
O2 C1 H1B 110.1 . . ?
C211 C1 H1B 110.1 . . ?
H1A C1 H1B 108.5 . . ?
C112 C111 C116 121.1(3) . . ?
C112 C111 I1 120.5(2) . . ?
C116 C111 I1 118.5(2) . . ?
C111 C112 C113 120.0(3) . . ?
C111 C112 H112 120 . . ?
C113 C112 H112 120 . . ?
C112 C113 C114 120.2(3) . . ?
C112 C113 H113 119.9 . . ?
C114 C113 H113 119.9 . . ?
O1 C114 C113 119.6(3) . . ?
O1 C114 C115 121.0(3) . . ?
C113 C114 C115 119.4(3) . . ?
O2 C115 C116 125.7(3) . . ?
O2 C115 C114 113.3(3) . . ?
C116 C115 C114 121.0(3) . . ?
C115 C116 C111 118.3(3) . . ?
C115 C116 H116 120.9 . . ?
C111 C116 H116 120.9 . . ?
C216 C211 C212 118.3(3) . . ?
C216 C211 C1 121.3(3) . . ?
C212 C211 C1 120.4(3) . . ?
C211 C212 C213 120.6(3) . . ?
C211 C212 H212 119.7 . . ?
C213 C212 H212 119.7 . . ?
C214 C213 C212 120.6(4) . . ?
C214 C213 H213 119.7 . . ?
C212 C213 H213 119.7 . . ?
C215 C214 C213 119.2(3) . . ?
C215 C214 H214 120.4 . . ?
C213 C214 H214 120.4 . . ?
C214 C215 C216 120.2(4) . . ?
C214 C215 H215 119.9 . . ?
C216 C215 H215 119.9 . . ?
C211 C216 C215 121.0(3) . . ?
C211 C216 H216 119.5 . . ?
C215 C216 H216 119.5 . . ?
C114 O1 H1 109.5 . . ?
C115 O2 C1 117.9(2) . . ?
 
