 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12.50 H12.50 O2.50' 
_chemical_formula_weight          202.73 
 
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   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'C'  'C'   0.0033   0.0000 
 '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' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    6.0509(2) 
_cell_length_b                    18.1250(6) 
_cell_length_c                    10.3711(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.689(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1131.82(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.190 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              430 
_exptl_absorpt_coefficient_mu     0.082 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\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_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3890 
_diffrn_reflns_av_R_equivalents   0.0207 
_diffrn_reflns_av_sigmaI/netI     0.0300 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.57 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              1982 
_reflns_number_gt                 1545 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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)+(0.0603P)²+0.1764P] 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          1982 
_refine_ls_number_parameters      219 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0554 
_refine_ls_R_factor_gt            0.0391 
_refine_ls_wR_factor_ref          0.1102 
_refine_ls_wR_factor_gt           0.1028 
_refine_ls_goodness_of_fit_ref    1.107 
_refine_ls_restrained_S_all       1.107 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 0.1648(2) 0.91944(6) 0.67608(11) 0.0377(4) Uani 1 1 d . . . 
O2 O 0.02268(19) 0.97390(6) 0.85053(11) 0.0328(3) Uani 1 1 d . . . 
O3 O 0.2131(2) 0.86344(7) 0.87597(12) 0.0384(3) Uani 1 1 d . . . 
O4 O -0.1308(2) 0.87119(7) 0.76200(11) 0.0380(3) Uani 1 1 d . . . 
C1 C -0.1279(3) 0.81362(9) 0.85023(16) 0.0319(4) Uani 1 1 d . . . 
C2 C -0.2959(3) 0.76533(10) 0.86910(19) 0.0367(5) Uani 1 1 d . . . 
C3 C 0.2014(3) 1.02809(10) 0.86496(18) 0.0330(4) Uani 1 1 d . . . 
C4 C -0.0393(3) 0.70714(10) 1.03298(18) 0.0391(5) Uani 1 1 d . . . 
C5 C 0.1286(3) 0.75689(10) 1.01137(18) 0.0371(5) Uani 1 1 d . . . 
C6 C 0.1466(4) 1.05460(11) 0.64230(19) 0.0395(5) Uani 1 1 d . . . 
C7 C 0.5456(3) 1.07426(11) 0.8031(2) 0.0434(5) Uani 1 1 d . . . 
C8 C 0.1531(3) 1.09289(10) 0.77391(19) 0.0366(5) Uani 1 1 d . . . 
C9 C 0.3704(3) 1.13607(11) 0.7976(2) 0.0421(5) Uani 1 1 d . . . 
C10 C -0.2455(3) 0.71133(10) 0.96371(19) 0.0392(5) Uani 1 1 d . . . 
C11 C 0.4096(3) 1.00294(11) 0.80517(19) 0.0357(5) Uani 1 1 d . . . 
C12 C 0.2971(3) 0.98669(10) 0.67154(18) 0.0363(5) Uani 1 1 d . . . 
C13 C 0.0777(3) 0.80945(9) 0.91885(17) 0.0318(4) Uani 1 1 d . . . 
C14 C 0.0708(3) 0.90993(9) 0.78927(17) 0.0325(4) Uani 1 1 d . . . 
H1 H 0.485(3) 0.9627(12) 0.8457(19) 0.043(5) Uiso 1 1 d . . . 
H2 H 0.219(3) 1.0419(10) 0.957(2) 0.036(5) Uiso 1 1 d . . . 
H3 H 0.394(3) 0.9762(10) 0.606(2) 0.042(5) Uiso 1 1 d . . . 
H4 H -0.011(3) 0.6690(12) 1.100(2) 0.047(5) Uiso 1 1 d . . . 
H5 H -0.440(3) 0.7693(11) 0.8222(19) 0.041(5) Uiso 1 1 d . . . 
H6 H 0.017(3) 1.1207(11) 0.7879(19) 0.044(5) Uiso 1 1 d . . . 
H7 H -0.357(3) 0.6768(12) 0.9815(19) 0.044(5) Uiso 1 1 d . . . 
H8 H -0.008(3) 1.0374(10) 0.6070(18) 0.039(5) Uiso 1 1 d . . . 
H9 H 0.657(4) 1.0784(11) 0.882(2) 0.052(6) Uiso 1 1 d . . . 
H10 H 0.266(3) 0.7543(10) 1.055(2) 0.038(5) Uiso 1 1 d . . . 
H11 H 0.618(4) 1.0756(13) 0.724(2) 0.065(7) Uiso 1 1 d . . . 
H12 H 0.377(3) 1.1615(12) 0.881(2) 0.051(6) Uiso 1 1 d . . . 
H13 H 0.390(3) 1.1735(13) 0.726(2) 0.057(6) Uiso 1 1 d . . . 
H14 H 0.210(4) 1.0881(12) 0.573(2) 0.056(6) Uiso 1 1 d . . . 
 
 
_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 C14 1.365(2) . ? 
O1 C12 1.462(2) . ? 
O2 C14 1.367(2) . ? 
O2 C3 1.457(2) . ? 
O3 C13 1.378(2) . ? 
O3 C14 1.452(2) . ? 
O4 C1 1.387(2) . ? 
O4 C14 1.412(2) . ? 
C1 C2 1.370(3) . ? 
C1 C13 1.373(3) . ? 
C2 C10 1.398(3) . ? 
C3 C8 1.517(3) . ? 
C3 C11 1.528(3) . ? 
C4 C10 1.379(3) . ? 
C4 C5 1.393(3) . ? 
C5 C13 1.365(3) . ? 
C6 C8 1.528(3) . ? 
C6 C12 1.543(3) . ? 
C7 C11 1.534(3) . ? 
C7 C9 1.540(3) . ? 
C8 C9 1.529(3) . ? 
C11 C12 1.511(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 
C14 O1 C12 114.16(13) . . ? 
C14 O2 C3 115.42(13) . . ? 
C13 O3 C14 106.09(13) . . ? 
C1 O4 C14 106.72(13) . . ? 
C2 C1 C13 122.55(16) . . ? 
C2 C1 O4 127.85(17) . . ? 
C13 C1 O4 109.59(15) . . ? 
C1 C2 C10 115.72(19) . . ? 
O2 C3 C8 111.28(15) . . ? 
O2 C3 C11 112.99(14) . . ? 
C8 C3 C11 95.38(14) . . ? 
C10 C4 C5 121.15(18) . . ? 
C13 C5 C4 116.59(19) . . ? 
C8 C6 C12 102.96(15) . . ? 
C11 C7 C9 104.20(15) . . ? 
C3 C8 C6 100.99(14) . . ? 
C3 C8 C9 100.77(16) . . ? 
C6 C8 C9 108.79(16) . . ? 
C8 C9 C7 102.20(15) . . ? 
C4 C10 C2 121.83(18) . . ? 
C12 C11 C3 96.65(16) . . ? 
C12 C11 C7 110.19(16) . . ? 
C3 C11 C7 102.68(15) . . ? 
O1 C12 C11 109.35(14) . . ? 
O1 C12 C6 110.91(15) . . ? 
C11 C12 C6 103.19(15) . . ? 
C5 C13 C1 122.16(17) . . ? 
C5 C13 O3 128.50(17) . . ? 
C1 C13 O3 109.32(15) . . ? 
O1 C14 O2 114.74(14) . . ? 
O1 C14 O4 108.42(14) . . ? 
O2 C14 O4 107.19(14) . . ? 
O1 C14 O3 109.50(14) . . ? 
O2 C14 O3 110.18(14) . . ? 
O4 C14 O3 106.44(13) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.153 
_refine_diff_density_min   -0.186 
_refine_diff_density_rms    0.041 
