 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2001-05-09 at 11:55:51
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.2
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf039 dreduc struct sortav absorb
 
 
data_ljf039
 
_audit_creation_date            2001-05-09T11:55:51-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C29 H24 O5'
_chemical_formula_structural            'C29 H24 O5'
_chemical_formula_sum                   'C29 H24 O5'
_chemical_formula_weight                452.48
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  triclinic
_symmetry_space_group_name_H-M          'P -1'
_symmetry_space_group_name_Hall         '-P 1'
_symmetry_Int_Tables_number             2
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
 
_cell_length_a                          9.9550(3)
_cell_length_b                          10.1416(3)
_cell_length_c                          12.9122(4)
_cell_angle_alpha                       87.059(1)
_cell_angle_beta                        79.815(1)
_cell_angle_gamma                       63.839(1)
_cell_volume                            1151.11(6)
_cell_formula_units_Z                   2
_cell_measurement_temperature           291(2)
_cell_measurement_reflns_used           3601
_cell_measurement_theta_min             1
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   yellow
_exptl_crystal_size_max                 0.45
_exptl_crystal_size_mid                 0.42
_exptl_crystal_size_min                 0.25
_exptl_crystal_density_diffrn           1.305
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    476
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.089
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.954
_exptl_absorpt_correction_T_max         0.99
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             291(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             0.107482
_diffrn_orient_matrix_ub_12             -0.143808E-1
_diffrn_orient_matrix_ub_13             -0.192643E-1
_diffrn_orient_matrix_ub_21             -0.02994
_diffrn_orient_matrix_ub_22             0.989369E-1
_diffrn_orient_matrix_ub_23             0.318475E-1
_diffrn_orient_matrix_ub_31             0.214152E-1
_diffrn_orient_matrix_ub_32             -0.456549E-1
_diffrn_orient_matrix_ub_33             0.693668E-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_av_R_equivalents         0.0303
_diffrn_reflns_av_unetI/netI            0.0425
_diffrn_reflns_number                   5196
_diffrn_reflns_limit_h_min              -12
_diffrn_reflns_limit_h_max              14
_diffrn_reflns_limit_k_min              -14
_diffrn_reflns_limit_k_max              17
_diffrn_reflns_limit_l_min              -18
_diffrn_reflns_limit_l_max              16
_diffrn_reflns_theta_min                2.24
_diffrn_reflns_theta_max                27.49
_diffrn_reflns_theta_full               27.49
_diffrn_measured_fraction_theta_full
                                        0.983
_diffrn_measured_fraction_theta_max
                                        0.983
_reflns_number_total                    5196
_reflns_number_gt                       3396
_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)+(0.0426P)²+0.2415P] 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              0.027(9)
_refine_ls_number_reflns                5196
_refine_ls_number_parameters            316
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0879
_refine_ls_R_factor_gt                  0.0505
_refine_ls_wR_factor_ref                0.1258
_refine_ls_wR_factor_gt                 0.1086
_refine_ls_goodness_of_fit_ref          1.02
_refine_ls_restrained_S_all             1.02
_refine_ls_shift/su_max                 0.003
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.147
_refine_diff_density_min                -0.131
_refine_diff_density_rms                0.027
 
#----------------------------------------------------------------------------#
#                   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
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
 
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 0.80086(13) 0.08994(13) 0.53165(9) 0.0625(3) Uani 1 1 d . . .
O2 O 0.69899(15) -0.03255(14) 0.67306(10) 0.0674(4) Uani 1 1 d . . .
O3 O 0.92128(13) 0.21357(14) 0.40024(11) 0.0690(4) Uani 1 1 d . . .
O4 O 0.18375(15) 0.05723(14) 0.71379(8) 0.0659(3) Uani 1 1 d . . .
O5 O 0.36751(12) 0.31478(12) 0.45921(8) 0.0573(3) Uani 1 1 d . . .
C1 C 0.66867(18) 0.17446(16) 0.51101(11) 0.0472(4) Uani 1 1 d . . .
C1A C 0.53964(17) 0.14877(15) 0.56333(11) 0.0444(3) Uani 1 1 d . . .
C1B C 0.77239(17) 0.41583(16) 0.30677(12) 0.0477(4) Uani 1 1 d . . .
C2 C 0.65731(18) 0.28878(17) 0.43820(11) 0.0488(4) Uani 1 1 d . . .
H2 H 0.5615 0.3558 0.4264 0.059 Uiso 1 1 calc R . .
C2A C 0.56188(19) 0.04454(17) 0.64385(11) 0.0501(4) Uani 1 1 d . . .
C2B C 0.6417(2) 0.4972(2) 0.26553(16) 0.0721(5) Uani 1 1 d . . .
H2B H 0.5559 0.4818 0.2883 0.086 Uiso 1 1 calc R . .
C3 C 0.78049(18) 0.30332(17) 0.38580(12) 0.0480(4) Uani 1 1 d . . .
C3A C 0.4458(2) 0.01403(17) 0.69747(12) 0.0548(4) Uani 1 1 d . . .
H3A H 0.4637 -0.0529 0.7513 0.066 Uiso 1 1 calc R . .
C3B C 0.6369(2) 0.6010(2) 0.19111(17) 0.0828(6) Uani 1 1 d . . .
H3B H 0.5479 0.6551 0.1644 0.099 Uiso 1 1 calc R . .
C4A C 0.3046(2) 0.08328(18) 0.67041(11) 0.0516(4) Uani 1 1 d . . .
C4B C 0.7621(2) 0.6248(2) 0.15629(15) 0.0686(5) Uani 1 1 d . . .
H4B H 0.7588 0.6944 0.1057 0.082 Uiso 1 1 calc R . .
C5A C 0.27523(18) 0.18666(17) 0.59145(11) 0.0507(4) Uani 1 1 d . . .
H5A H 0.1784 0.234 0.5743 0.061 Uiso 1 1 calc R . .
C5B C 0.8920(2) 0.5457(2) 0.19642(15) 0.0677(5) Uani 1 1 d . . .
H5B H 0.9772 0.5621 0.1735 0.081 Uiso 1 1 calc R . .
C6A C 0.38994(18) 0.21817(16) 0.53924(11) 0.0455(4) Uani 1 1 d . . .
C6B C 0.8976(2) 0.44169(19) 0.27069(13) 0.0578(4) Uani 1 1 d . . .
H6B H 0.9871 0.388 0.297 0.069 Uiso 1 1 calc R . .
C41 C 0.2044(2) -0.0526(2) 0.79271(13) 0.0667(5) Uani 1 1 d . . .
H41A H 0.3022 -0.1362 0.7722 0.08 Uiso 1 1 calc R . .
H41B H 0.1263 -0.0861 0.7961 0.08 Uiso 1 1 calc R . .
C51 C 0.22243(19) 0.3819(2) 0.42619(13) 0.0595(4) Uani 1 1 d . . .
H51A H 0.1466 0.4502 0.4804 0.071 Uiso 1 1 calc R . .
H51B H 0.1906 0.3077 0.4125 0.071 Uiso 1 1 calc R . .
C411 C 0.1972(2) 0.00367(17) 0.89965(12) 0.0527(4) Uani 1 1 d . . .
C412 C 0.0725(2) 0.12816(19) 0.94282(13) 0.0603(4) Uani 1 1 d . . .
H412 H -0.0047 0.1778 0.904 0.072 Uiso 1 1 calc R . .
C413 C 0.0591(2) 0.1810(2) 1.04176(14) 0.0693(5) Uani 1 1 d . . .
H413 H -0.0265 0.2654 1.0691 0.083 Uiso 1 1 calc R . .
C414 C 0.1707(3) 0.1101(2) 1.09971(15) 0.0755(6) Uani 1 1 d . . .
H414 H 0.1614 0.1458 1.1668 0.091 Uiso 1 1 calc R . .
C415 C 0.2961(3) -0.0130(3) 1.05951(16) 0.0878(7) Uani 1 1 d . . .
H415 H 0.3728 -0.0612 1.099 0.105 Uiso 1 1 calc R . .
C416 C 0.3097(2) -0.0672(2) 0.95901(15) 0.0767(6) Uani 1 1 d . . .
H416 H 0.3954 -0.1517 0.932 0.092 Uiso 1 1 calc R . .
C511 C 0.24093(18) 0.46154(18) 0.32745(13) 0.0541(4) Uani 1 1 d . . .
C512 C 0.2954(2) 0.3867(2) 0.23147(15) 0.0661(5) Uani 1 1 d . . .
H512 H 0.3187 0.2874 0.228 0.079 Uiso 1 1 calc R . .
C513 C 0.3156(2) 0.4585(3) 0.14049(16) 0.0828(6) Uani 1 1 d . . .
H513 H 0.3529 0.4072 0.0761 0.099 Uiso 1 1 calc R . .
C514 C 0.2810(2) 0.6042(3) 0.14461(19) 0.0868(7) Uani 1 1 d . . .
H514 H 0.2952 0.6518 0.0831 0.104 Uiso 1 1 calc R . .
C515 C 0.2257(3) 0.6801(2) 0.2388(2) 0.0860(7) Uani 1 1 d . . .
H515 H 0.2017 0.7796 0.2414 0.103 Uiso 1 1 calc R . .
C516 C 0.2052(2) 0.6092(2) 0.33039(16) 0.0719(5) Uani 1 1 d . . .
H516 H 0.1671 0.6614 0.3944 0.086 Uiso 1 1 calc R . .
H11 H 0.906(3) 0.145(3) 0.4552(18) 0.110(8) Uiso 1 1 d . . .
H10 H 0.770(3) -0.004(2) 0.6239(19) 0.111(8) 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
O1 C1 1.2819(18) . ?
O2 C2A 1.3518(19) . ?
O2 H10 0.99(2) . ?
O3 C3 1.3333(18) . ?
O3 H11 1.01(2) . ?
O4 C4A 1.3628(19) . ?
O4 C41 1.4409(19) . ?
O5 C6A 1.3647(16) . ?
O5 C51 1.4325(18) . ?
C1 C2 1.432(2) . ?
C1 C1A 1.464(2) . ?
C1A C2A 1.4176(19) . ?
C1A C6A 1.425(2) . ?
C1B C6B 1.382(2) . ?
C1B C2B 1.382(2) . ?
C1B C3 1.476(2) . ?
C2 C3 1.356(2) . ?
C2 H2 0.93 . ?
C2A C3A 1.386(2) . ?
C2B C3B 1.378(2) . ?
C2B H2B 0.93 . ?
C3A C4A 1.367(2) . ?
C3A H3A 0.93 . ?
C3B C4B 1.368(3) . ?
C3B H3B 0.93 . ?
C4A C5A 1.396(2) . ?
C4B C5B 1.365(3) . ?
C4B H4B 0.93 . ?
C5A C6A 1.374(2) . ?
C5A H5A 0.93 . ?
C5B C6B 1.378(2) . ?
C5B H5B 0.93 . ?
C6B H6B 0.93 . ?
C41 C411 1.499(2) . ?
C41 H41A 0.97 . ?
C41 H41B 0.97 . ?
C51 C511 1.501(2) . ?
C51 H51A 0.97 . ?
C51 H51B 0.97 . ?
C411 C412 1.375(2) . ?
C411 C416 1.377(2) . ?
C412 C413 1.373(2) . ?
C412 H412 0.93 . ?
C413 C414 1.359(3) . ?
C413 H413 0.93 . ?
C414 C415 1.360(3) . ?
C414 H414 0.93 . ?
C415 C416 1.396(3) . ?
C415 H415 0.93 . ?
C416 H416 0.93 . ?
C511 C516 1.379(2) . ?
C511 C512 1.379(2) . ?
C512 C513 1.382(3) . ?
C512 H512 0.93 . ?
C513 C514 1.362(3) . ?
C513 H513 0.93 . ?
C514 C515 1.364(3) . ?
C514 H514 0.93 . ?
C515 C516 1.384(3) . ?
C515 H515 0.93 . ?
C516 H516 0.93 . ?
 
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
C2A O2 H10 105.2(14) . . ?
C3 O3 H11 103.5(13) . . ?
C4A O4 C41 118.67(14) . . ?
C6A O5 C51 119.48(12) . . ?
O1 C1 C2 117.39(14) . . ?
O1 C1 C1A 118.28(13) . . ?
C2 C1 C1A 124.33(13) . . ?
C2A C1A C6A 115.39(14) . . ?
C2A C1A C1 119.00(14) . . ?
C6A C1A C1 125.61(13) . . ?
C6B C1B C2B 117.79(15) . . ?
C6B C1B C3 120.41(14) . . ?
C2B C1B C3 121.79(14) . . ?
C3 C2 C1 122.73(14) . . ?
C3 C2 H2 118.6 . . ?
C1 C2 H2 118.6 . . ?
O2 C2A C3A 115.48(13) . . ?
O2 C2A C1A 121.88(15) . . ?
C3A C2A C1A 122.64(15) . . ?
C3B C2B C1B 120.90(17) . . ?
C3B C2B H2B 119.6 . . ?
C1B C2B H2B 119.6 . . ?
O3 C3 C2 122.18(14) . . ?
O3 C3 C1B 114.04(14) . . ?
C2 C3 C1B 123.77(14) . . ?
C4A C3A C2A 119.36(14) . . ?
C4A C3A H3A 120.3 . . ?
C2A C3A H3A 120.3 . . ?
C4B C3B C2B 120.44(18) . . ?
C4B C3B H3B 119.8 . . ?
C2B C3B H3B 119.8 . . ?
O4 C4A C3A 124.70(14) . . ?
O4 C4A C5A 114.42(15) . . ?
C3A C4A C5A 120.86(15) . . ?
C5B C4B C3B 119.44(17) . . ?
C5B C4B H4B 120.3 . . ?
C3B C4B H4B 120.3 . . ?
C6A C5A C4A 119.73(15) . . ?
C6A C5A H5A 120.1 . . ?
C4A C5A H5A 120.1 . . ?
C4B C5B C6B 120.38(17) . . ?
C4B C5B H5B 119.8 . . ?
C6B C5B H5B 119.8 . . ?
O5 C6A C5A 121.64(14) . . ?
O5 C6A C1A 116.33(13) . . ?
C5A C6A C1A 122.00(13) . . ?
C5B C6B C1B 121.05(16) . . ?
C5B C6B H6B 119.5 . . ?
C1B C6B H6B 119.5 . . ?
O4 C41 C411 112.67(14) . . ?
O4 C41 H41A 109.1 . . ?
C411 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C411 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
O5 C51 C511 106.69(13) . . ?
O5 C51 H51A 110.4 . . ?
C511 C51 H51A 110.4 . . ?
O5 C51 H51B 110.4 . . ?
C511 C51 H51B 110.4 . . ?
H51A C51 H51B 108.6 . . ?
C412 C411 C416 117.76(16) . . ?
C412 C411 C41 119.75(16) . . ?
C416 C411 C41 122.47(17) . . ?
C413 C412 C411 121.70(17) . . ?
C413 C412 H412 119.1 . . ?
C411 C412 H412 119.1 . . ?
C414 C413 C412 120.04(19) . . ?
C414 C413 H413 120 . . ?
C412 C413 H413 120 . . ?
C413 C414 C415 119.97(19) . . ?
C413 C414 H414 120 . . ?
C415 C414 H414 120 . . ?
C414 C415 C416 120.04(19) . . ?
C414 C415 H415 120 . . ?
C416 C415 H415 120 . . ?
C411 C416 C415 120.48(19) . . ?
C411 C416 H416 119.8 . . ?
C415 C416 H416 119.8 . . ?
C516 C511 C512 118.74(17) . . ?
C516 C511 C51 121.30(17) . . ?
C512 C511 C51 119.96(16) . . ?
C511 C512 C513 120.32(19) . . ?
C511 C512 H512 119.8 . . ?
C513 C512 H512 119.8 . . ?
C514 C513 C512 120.3(2) . . ?
C514 C513 H513 119.8 . . ?
C512 C513 H513 119.8 . . ?
C513 C514 C515 120.1(2) . . ?
C513 C514 H514 120 . . ?
C515 C514 H514 120 . . ?
C514 C515 C516 120.0(2) . . ?
C514 C515 H515 120 . . ?
C516 C515 H515 120 . . ?
C511 C516 C515 120.5(2) . . ?
C511 C516 H516 119.8 . . ?
C515 C516 H516 119.8 . . ?
 
