 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-06-21 at 14:26:31
#  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  : ljf009 dreduc datcol struct
 
 
data_ljf009
 
_audit_creation_date            2000-06-21T14:26:31-00:00
_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                'C5 H12 O4'
_chemical_formula_structural            'C5 H12 O4'
_chemical_formula_sum                   'C5 H12 O4'
_chemical_formula_weight                136.15
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  tetragonal
_symmetry_space_group_name_H-M          'I -4'
_symmetry_space_group_name_Hall         'I -4'
_symmetry_Int_Tables_number             82
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
 
_cell_length_a                          6.0817(5)
_cell_length_b                          6.0817(5)
_cell_length_c                          8.7430(12)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            323.38(6)
_cell_formula_units_Z                   2
_cell_measurement_temperature           291(2)
_cell_measurement_reflns_used           25
_cell_measurement_theta_min             18.22
_cell_measurement_theta_max             24.85
_cell_measurement_wavelength            0.7093
loop_
    _cell_measurement_refln_index_h
    _cell_measurement_refln_index_k
    _cell_measurement_refln_index_l
    _cell_measurement_refln_theta
-7 0 1 24.35
1 0 7 24.35
7 0 -1 24.35
-6 1 -1 20.92
6 -1 1 20.92
-1 -1 6 20.92
-1 1 6 20.91
6 1 1 20.92
-7 2 1 24.85
1 2 7 24.85
7 2 -1 24.85
-1 3 6 22.02
-6 3 -1 22.03
6 3 1 22.03
-5 1 4 22.06
4 -1 5 22.06
-5 -1 4 22.06
4 1 5 22.06
6 1 3 23.16
6 -1 3 23.16
-3 1 6 23.16
-3 -1 6 23.16
-4 3 5 23.12
0 10 0 23.93
1 7 2 18.22
 
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.5
_exptl_crystal_size_mid                 0.5
_exptl_crystal_size_min                 0.4
_exptl_crystal_density_diffrn           1.398
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    148
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.121
_exptl_absorpt_correction_type          none
_exptl_absorpt_correction_T_min         0.9422
_exptl_absorpt_correction_T_max         0.9533
 
#----------------------------------------------------------------------------#
#                   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                        'scintillation LiI'
_diffrn_detector_dtime                  1.195
loop_
    _diffrn_attenuator_code
    _diffrn_attenuator_scale
0 0
 
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_ub_11             -0.14893
_diffrn_orient_matrix_ub_12             0.47661E-1
_diffrn_orient_matrix_ub_13             -0.11038E-1
_diffrn_orient_matrix_ub_21             -0.69343E-1
_diffrn_orient_matrix_ub_22             -0.101211
_diffrn_orient_matrix_ub_23             0.32086E-1
_diffrn_orient_matrix_ub_31             0.3775E-2
_diffrn_orient_matrix_ub_32             0.02359
_diffrn_orient_matrix_ub_33             0.160865
loop_
    _diffrn_orient_refln_angle_chi
    _diffrn_orient_refln_angle_kappa
    _diffrn_orient_refln_angle_phi
    _diffrn_orient_refln_angle_psi
    _diffrn_orient_refln_index_h
    _diffrn_orient_refln_index_k
    _diffrn_orient_refln_index_l
6.719 8.772 -66.178 0 -7 0 1
76.334 107.504 14.294 0.126 1 0 7
-6.722 -8.775 119.453 -0.001 7 0 -1
-9.081 -11.859 -69.652 -0.001 -6 1 -1
9.077 11.855 102.712 0.004 6 -1 1
68.753 94.93 -40.577 0.16 -1 -1 6
78.154 110.703 -82.065 0.217 -1 1 6
11.792 15.408 114.535 0.005 6 1 1
8.885 11.604 -78.127 0.004 -7 2 1
83.242 120.181 61.674 0.092 1 2 7
-4.311 -5.626 129.354 -0.002 7 2 -1
77.477 109.503 -142.771 0.06 -1 3 6
-6.068 -7.922 -83.072 0 -6 3 -1
13.834 18.085 126.226 0.008 6 3 1
37.813 50.032 -80.152 0.022 -5 1 4
48.673 65.068 69.004 0.039 4 -1 5
34.668 45.764 -63.745 0.026 -5 -1 4
52.688 70.778 85.345 0.032 4 1 5
28.416 37.364 103.327 0.014 6 1 3
25.685 33.725 91.623 0.01 6 -1 3
61.897 84.31 -85.247 0.068 -3 1 6
57.112 77.193 -60.717 0.063 -3 -1 6
51.018 68.392 -102.493 0.039 -4 3 5
11.861 15.499 -159.764 0.002 0 10 0
33.856 44.666 178.245 -0.114 1 7 2
 
_diffrn_measurement_device              'κ-geometry diffractometer'
_diffrn_measurement_device_type         'Enraf Nonius CAD4'
_diffrn_measurement_method              'non-profiled omega/2theta scans'
_diffrn_standards_number                3
_diffrn_standards_interval_time         120
_diffrn_standards_decay_%               1
_diffrn_standards_decay_corr_max        1.015
_diffrn_standards_decay_corr_min        0.987
loop_
    _diffrn_standard_refln_index_h
    _diffrn_standard_refln_index_k
    _diffrn_standard_refln_index_l
-2 -2 2
-2 -1 -3
1 -4 -1
 
_diffrn_reflns_number                   692
_diffrn_reflns_av_R_equivalents         0.0164
_diffrn_reflns_av_unetI/netI            0.013
_diffrn_reflns_limit_h_min              -8
_diffrn_reflns_limit_h_max              1
_diffrn_reflns_limit_k_min              -8
_diffrn_reflns_limit_k_max              8
_diffrn_reflns_limit_l_min              -12
_diffrn_reflns_limit_l_max              1
_diffrn_reflns_theta_min                4.08
_diffrn_reflns_theta_max                29.88
_diffrn_reflns_theta_full               29.88
_diffrn_measured_fraction_theta_full
                                        1
_diffrn_measured_fraction_theta_max
                                        1
_reflns_number_total                    470
_reflns_number_gt                       458
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'CAD4 Express (Enraf Nonius, 1994)'
_computing_cell_refinement              'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction               'XCAD4 (Harms & Wocadlo, 1995)'
_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)+(0.0875P)²+0.1419P] 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              0.41(8)
_refine_ls_number_reflns                470
_refine_ls_number_parameters            34
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0509
_refine_ls_R_factor_gt                  0.05
_refine_ls_wR_factor_ref                0.161
_refine_ls_wR_factor_gt                 0.1604
_refine_ls_goodness_of_fit_ref          1.269
_refine_ls_restrained_S_all             1.269
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack          0(3)
_refine_diff_density_max                0.341
_refine_diff_density_min                -0.217
_refine_diff_density_rms                0.092
 
#----------------------------------------------------------------------------#
#                   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'
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 0 0 0.0250(7) Uani 1 4 d S . .
C2 C -0.1267(3) 0.1581(3) 0.1039(3) 0.0351(5) Uani 1 1 d . . .
H2A H -0.241(4) 0.064(4) 0.172(3) 0.023(6) Uiso 1 1 d . . .
H2B H -0.004(7) 0.252(8) 0.168(5) 0.060(9) Uiso 1 1 d . . .
O1 O -0.2463(2) 0.3185(2) 0.0188(3) 0.0485(7) Uani 1 1 d . . .
H1 H -0.393(8) 0.258(6) 0.009(6) 0.063(10) Uiso 1 1 d . . .
 
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_23
    _atom_site_aniso_U_13
    _atom_site_aniso_U_12
C1 0.0224(8) 0.0224(8) 0.0303(15) 0 0 0
C2 0.0297(10) 0.0343(10) 0.0414(9) -0.0083(8) 0.0038(7) 0.0062(8)
O1 0.0293(8) 0.0259(7) 0.0904(16) 0.0013(8) -0.0043(8) 0.0066(6)
 
 
#----------------------------------------------------------------------------#
#                   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 1.531(2) 4 ?
C1 C2 1.531(2) . ?
C1 C2 1.531(2) 3 ?
C1 C2 1.531(2) 2 ?
C2 O1 1.427(3) . ?
 
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 C2 110.61(9) 4 . ?
C2 C1 C2 107.22(17) 4 3 ?
C2 C1 C2 110.61(9) . 3 ?
C2 C1 C2 110.61(9) 4 2 ?
C2 C1 C2 107.22(17) . 2 ?
C2 C1 C2 110.61(9) 3 2 ?
O1 C2 C1 112.15(17) . . ?
 
