 
data_udel2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C7 H5 O2' 
_chemical_formula_weight          121.11 
 
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' 
 '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' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    5.4266(11) 
_cell_length_b                    5.0403(10) 
_cell_length_c                    21.695(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.268(16) 
_cell_angle_gamma                 90.00 
_cell_volume                      589.9(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.364 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              252 
_exptl_absorpt_coefficient_mu     0.841 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.8141 
_exptl_absorpt_correction_T_max   0.9817 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      1.54178 
_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_reflns_number             3703 
_diffrn_reflns_av_R_equivalents   0.0545 
_diffrn_reflns_av_sigmaI/netI     0.0558 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        5 
_diffrn_reflns_limit_k_min        -5 
_diffrn_reflns_limit_k_max        5 
_diffrn_reflns_limit_l_min        -25 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          4.10 
_diffrn_reflns_theta_max          68.95 
_reflns_number_total              1001 
_reflns_number_gt                 789 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_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)+(0.1197P)²+1.4383P] 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_extinction_coef        ? 
_refine_ls_number_reflns          1001 
_refine_ls_number_parameters      106 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0967 
_refine_ls_R_factor_gt            0.0838 
_refine_ls_wR_factor_ref          0.2655 
_refine_ls_wR_factor_gt           0.2567 
_refine_ls_goodness_of_fit_ref    1.171 
_refine_ls_restrained_S_all       1.171 
_refine_ls_shift/su_max           0.397 
_refine_ls_shift/su_mean          0.018 
 
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 0.5436(8) 1.0295(9) 0.1534(2) 0.0327(11) Uani 1 1 d . . . 
H1 H 0.394(8) 0.930(9) 0.1566(19) 0.021(11) Uiso 1 1 d . . . 
C2 C 0.6220(9) 1.2244(10) 0.1971(2) 0.0375(12) Uani 1 1 d . . . 
H2 H 0.519(11) 1.260(12) 0.230(3) 0.054(17) Uiso 1 1 d . . . 
C3 C 0.8266(9) 1.3783(10) 0.1910(2) 0.0372(12) Uani 1 1 d . . . 
H3 H 0.885(10) 1.511(12) 0.222(3) 0.050(16) Uiso 1 1 d . . . 
C4 C 0.9576(9) 1.3399(9) 0.1418(2) 0.0364(12) Uani 1 1 d . . . 
H4 H 1.107(8) 1.457(10) 0.1393(19) 0.027(11) Uiso 1 1 d . . . 
C5 C 0.8828(8) 1.1458(9) 0.0979(2) 0.0340(11) Uani 1 1 d . . . 
H5 H 0.986(8) 1.103(9) 0.063(2) 0.023(11) Uiso 1 1 d . . . 
C6 C 0.6764(8) 0.9897(9) 0.1039(2) 0.0303(11) Uani 1 1 d . . . 
C7 C 0.5953(8) 0.7806(8) 0.0573(2) 0.0301(11) Uani 1 1 d . . . 
O1 O 0.7168(6) 0.7440(7) 0.01320(15) 0.0376(10) Uani 1 1 d . . . 
O2 O 0.4027(6) 0.6438(6) 0.06543(16) 0.0380(10) Uani 1 1 d . . . 
H2O H 0.337(19) 0.42(3) 0.028(5) 0.17(4) 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 0.031(2) 0.023(2) 0.045(3) 0.0030(18) 0.0081(19) -0.0017(18) 
C2 0.041(3) 0.031(3) 0.041(3) -0.001(2) 0.009(2) 0.004(2) 
C3 0.040(3) 0.026(2) 0.045(3) -0.003(2) 0.000(2) 0.003(2) 
C4 0.031(2) 0.023(2) 0.056(3) 0.001(2) 0.007(2) -0.0009(18) 
C5 0.029(2) 0.026(2) 0.048(3) 0.000(2) 0.0092(19) -0.0003(18) 
C6 0.030(2) 0.022(2) 0.039(3) 0.0030(17) 0.0046(18) 0.0017(18) 
C7 0.032(2) 0.019(2) 0.041(3) 0.0033(18) 0.0066(18) 0.0013(17) 
O1 0.0407(19) 0.0307(19) 0.044(2) -0.0031(14) 0.0142(14) -0.0060(15) 
O2 0.0360(19) 0.0297(19) 0.050(2) -0.0028(14) 0.0116(14) -0.0066(14) 
 
_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 C6 1.371(6) . ? 
C1 C2 1.399(7) . ? 
C1 H1 0.96(4) . ? 
C2 C3 1.372(7) . ? 
C2 H2 0.97(6) . ? 
C3 C4 1.361(7) . ? 
C3 H3 0.97(6) . ? 
C4 C5 1.394(7) . ? 
C4 H4 1.01(5) . ? 
C5 C6 1.387(6) . ? 
C5 H5 1.01(4) . ? 
C6 C7 1.493(6) . ? 
C7 O1 1.233(5) . ? 
C7 O2 1.281(5) . ? 
O2 H2O 1.41(12) . ? 
 
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 
C6 C1 C2 119.1(4) . . ? 
C6 C1 H1 120(3) . . ? 
C2 C1 H1 121(3) . . ? 
C3 C2 C1 121.4(4) . . ? 
C3 C2 H2 120(4) . . ? 
C1 C2 H2 118(4) . . ? 
C4 C3 C2 119.5(5) . . ? 
C4 C3 H3 118(3) . . ? 
C2 C3 H3 122(3) . . ? 
C3 C4 C5 119.8(5) . . ? 
C3 C4 H4 117(3) . . ? 
C5 C4 H4 123(3) . . ? 
C6 C5 C4 120.8(4) . . ? 
C6 C5 H5 118(3) . . ? 
C4 C5 H5 121(3) . . ? 
C1 C6 C5 119.3(4) . . ? 
C1 C6 C7 119.5(4) . . ? 
C5 C6 C7 121.2(4) . . ? 
O1 C7 O2 122.7(4) . . ? 
O1 C7 C6 119.2(4) . . ? 
O2 C7 C6 118.1(4) . . ? 
C7 O2 H2O 121(4) . . ? 
 
_diffrn_measured_fraction_theta_max    0.918 
_diffrn_reflns_theta_full              68.95 
_diffrn_measured_fraction_theta_full   0.918 
_refine_diff_density_max    0.410 
_refine_diff_density_min   -0.288 
_refine_diff_density_rms    0.081 
