 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 H8 Cu O5' 
_chemical_formula_weight          199.64 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Cu'  'Cu'   0.3240   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0056   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'C'  'C'   0.0015   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, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    13.1541(7) 
_cell_length_b                    8.5540(7) 
_cell_length_c                    13.8403(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  117.047(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      1386.99(15) 
_cell_formula_units_Z             8 
_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     1.912 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              808 
_exptl_absorpt_coefficient_mu     1.636 
_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      0.56083 
_diffrn_radiation_type            AgK\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             18145 
_diffrn_reflns_av_R_equivalents   0.0576 
_diffrn_reflns_av_sigmaI/netI     0.0347 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        19 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.33 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              2379 
_reflns_number_gt                 1723 
_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)+(0.0415P)²+0.0000P] 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_coef        0.0182(9) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          2379 
_refine_ls_number_parameters      100 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0478 
_refine_ls_R_factor_gt            0.0270 
_refine_ls_wR_factor_ref          0.0667 
_refine_ls_wR_factor_gt           0.0625 
_refine_ls_goodness_of_fit_ref    0.911 
_refine_ls_restrained_S_all       0.911 
_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 
Cu1 Cu 0.049886(17) 0.91599(3) 0.455017(19) 0.01773(8) Uani 1 1 d . . . 
O1 O 0.18379(11) 0.91127(18) 0.60039(12) 0.0256(3) Uani 1 1 d . . . 
O2 O -0.10017(12) 0.93967(18) 0.32426(13) 0.0274(3) Uani 1 1 d . . . 
O3 O 0.09511(13) 1.12072(18) 0.42525(14) 0.0307(3) Uani 1 1 d . . . 
O4 O -0.00759(13) 0.73592(18) 0.49990(14) 0.0305(3) Uani 1 1 d . . . 
O5 O 0.12419(17) 0.7923(2) 0.36724(17) 0.0364(4) Uani 1 1 d . . . 
H51 H 0.120(3) 0.835(4) 0.315(3) 0.041(9) Uiso 1 1 d . . . 
H52 H 0.174(3) 0.739(5) 0.384(3) 0.065(12) Uiso 1 1 d . . . 
C1 C 0.18237(15) 0.9792(2) 0.68042(17) 0.0221(3) Uani 1 1 d . . . 
C2 C -0.06563(15) 0.7514(2) 0.55060(17) 0.0245(4) Uani 1 1 d . . . 
C3 C -0.1038(2) 0.6047(3) 0.5842(2) 0.0382(6) Uani 1 1 d . . . 
H3A H -0.0764 0.5153 0.5611 0.057 Uiso 1 1 calc R . . 
H3B H -0.1857 0.6021 0.5512 0.057 Uiso 1 1 calc R . . 
H3C H -0.0738 0.6030 0.6617 0.057 Uiso 1 1 calc R . . 
C4 C 0.2842(2) 0.9631(4) 0.7887(2) 0.0433(6) Uani 1 1 d . . . 
H4A H 0.2716 1.0203 0.8419 0.065 Uiso 1 1 calc R . . 
H4B H 0.3503 1.0037 0.7849 0.065 Uiso 1 1 calc R . . 
H4C H 0.2961 0.8547 0.8087 0.065 Uiso 1 1 calc R . . 
 
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 
Cu1 0.01687(10) 0.01942(11) 0.01766(13) 0.00020(10) 0.00851(8) 0.00119(9) 
O1 0.0203(5) 0.0332(7) 0.0202(7) -0.0014(6) 0.0064(5) 0.0038(6) 
O2 0.0221(6) 0.0361(9) 0.0196(8) -0.0035(5) 0.0055(5) 0.0051(5) 
O3 0.0327(7) 0.0272(7) 0.0372(10) 0.0056(6) 0.0202(7) -0.0021(6) 
O4 0.0355(7) 0.0230(7) 0.0366(9) 0.0024(6) 0.0194(7) -0.0037(6) 
O5 0.0486(10) 0.0401(9) 0.0329(10) 0.0130(7) 0.0293(9) 0.0224(8) 
C1 0.0190(7) 0.0254(8) 0.0196(10) 0.0021(7) 0.0066(7) 0.0002(6) 
C2 0.0201(8) 0.0242(8) 0.0234(10) 0.0061(7) 0.0049(7) -0.0043(7) 
C3 0.0386(11) 0.0315(12) 0.0429(15) 0.0122(10) 0.0172(10) -0.0073(9) 
C4 0.0304(11) 0.0631(16) 0.0231(13) -0.0029(10) 0.0005(9) 0.0143(10) 
 
_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 
Cu1 O4 1.9383(15) . ? 
Cu1 O3 1.9528(15) . ? 
Cu1 O1 1.9823(14) . ? 
Cu1 O2 1.9909(15) . ? 
Cu1 O5 2.1518(17) . ? 
Cu1 Cu1 2.6125(4) 5_576 ? 
O1 C1 1.259(3) . ? 
O2 C1 1.261(2) 5_576 ? 
O3 C2 1.256(3) 5_576 ? 
O4 C2 1.257(3) . ? 
C1 O2 1.261(2) 5_576 ? 
C1 C4 1.494(3) . ? 
C2 O3 1.256(3) 5_576 ? 
C2 C3 1.502(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 
O4 Cu1 O3 168.78(7) . . ? 
O4 Cu1 O1 87.40(7) . . ? 
O3 Cu1 O1 90.98(7) . . ? 
O4 Cu1 O2 90.13(7) . . ? 
O3 Cu1 O2 89.32(7) . . ? 
O1 Cu1 O2 168.76(6) . . ? 
O4 Cu1 O5 97.69(7) . . ? 
O3 Cu1 O5 93.53(7) . . ? 
O1 Cu1 O5 98.10(7) . . ? 
O2 Cu1 O5 93.09(7) . . ? 
O4 Cu1 Cu1 86.03(5) . 5_576 ? 
O3 Cu1 Cu1 82.79(5) . 5_576 ? 
O1 Cu1 Cu1 86.25(4) . 5_576 ? 
O2 Cu1 Cu1 82.64(4) . 5_576 ? 
O5 Cu1 Cu1 174.37(5) . 5_576 ? 
C1 O1 Cu1 121.46(12) . . ? 
C1 O2 Cu1 125.10(14) 5_576 . ? 
C2 O3 Cu1 124.37(14) 5_576 . ? 
C2 O4 Cu1 121.32(14) . . ? 
O1 C1 O2 124.36(18) . 5_576 ? 
O1 C1 C4 118.32(18) . . ? 
O2 C1 C4 117.3(2) 5_576 . ? 
O3 C2 O4 125.43(18) 5_576 . ? 
O3 C2 C3 117.28(19) 5_576 . ? 
O4 C2 C3 117.3(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.957 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.957 
_refine_diff_density_max    0.446 
_refine_diff_density_min   -0.540 
_refine_diff_density_rms    0.094 
