 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C4 H0 Cu O8' 
_chemical_formula_weight          239.58 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 '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'   0.0000   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' 
 
_cell_length_a                    6.5186(5) 
_cell_length_b                    7.0637(6) 
_cell_length_c                    18.4024(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.138(6) 
_cell_angle_gamma                 90.00 
_cell_volume                      847.34(11) 
_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     1.878 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              468 
_exptl_absorpt_coefficient_mu     2.590 
_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             6712 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.1573 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        8 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.88 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              6712 
_reflns_number_gt                 3342 
_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)+(0.0178P)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        0.0054(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00 
_refine_ls_number_reflns          6712 
_refine_ls_number_parameters      239 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.1029 
_refine_ls_R_factor_gt            0.0390 
_refine_ls_wR_factor_ref          0.0690 
_refine_ls_wR_factor_gt           0.0592 
_refine_ls_goodness_of_fit_ref    0.681 
_refine_ls_restrained_S_all       0.681 
_refine_ls_shift/su_max           1.977 
_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 
Cu1 Cu 0.07258(14) 0.5091(3) 0.09892(6) 0.0170(4) Uani 1 1 d . . . 
O111 O -0.2531(17) 0.4187(18) 0.2078(6) 0.024(3) Uani 1 1 d . . . 
O112 O 0.0574(19) 0.5318(17) 0.2065(6) 0.022(3) Uani 1 1 d . . . 
O141 O 0.0606(15) 0.5189(16) -0.0084(5) 0.012(2) Uani 1 1 d . . . 
O142 O -0.2698(14) 0.468(2) -0.0094(5) 0.036(4) Uani 1 1 d . . . 
C11 C -0.121(3) 0.487(3) 0.2368(9) 0.035(5) Uani 1 1 d . . . 
C12 C -0.109(2) 0.502(3) 0.3130(9) 0.020(3) Uani 1 1 d . . . 
C13 C -0.0817(17) 0.498(3) -0.1206(9) 0.013(3) Uani 1 1 d . . . 
C14 C -0.111(2) 0.490(3) -0.0433(7) 0.013(3) Uani 1 1 d . . . 
O11 O 0.073(2) 0.2382(15) 0.1052(6) 0.023(2) Uani 1 1 d . . . 
O12 O -0.0068(15) 0.7664(13) 0.0928(5) 0.020(2) Uani 1 1 d . . . 
O13 O -0.5855(12) 0.536(2) 0.1039(6) 0.024(3) Uani 1 1 d . . . 
Cu2 Cu 0.36950(15) 0.0101(4) 0.28238(6) 0.0195(5) Uani 1 1 d . . . 
O211 O 0.3548(15) -0.0186(18) 0.3893(6) 0.018(3) Uani 1 1 d . . . 
O212 O 0.7015(19) -0.022(3) 0.3873(7) 0.064(5) Uani 1 1 d . . . 
O241 O 0.3814(16) 0.030(2) 0.1793(6) 0.033(3) Uani 1 1 d . . . 
O242 O 0.7095(15) -0.080(2) 0.1745(6) 0.035(4) Uani 1 1 d . . . 
C21 C 0.525(2) -0.008(3) 0.4155(8) 0.025(4) Uani 1 1 d . . . 
C22 C -0.4434(19) 0.004(3) -0.0031(10) 0.030(3) Uani 1 1 d . . . 
C23 C -0.473(2) -0.018(2) 0.0595(10) 0.024(4) Uani 1 1 d . . . 
C24 C 0.5380(18) -0.024(2) 0.1448(6) 0.010(3) Uani 1 1 d . . . 
O21 O 0.4149(18) 0.2960(14) 0.2861(8) 0.033(3) Uani 1 1 d . . . 
O22 O 0.3514(16) -0.2773(16) 0.2800(7) 0.025(3) Uani 1 1 d . . . 
O23 O 1.0010(15) 0.039(2) 0.2731(7) 0.049(3) Uani 1 1 d . . . 
O1 O 0.3938(14) 0.515(2) 0.4017(6) 0.032(3) Uani 1 1 d . . . 
O2 O 0.0251(15) 1.018(2) -0.0198(5) 0.029(3) Uani 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 
Cu1 O12 1.893(10) . ? 
Cu1 O11 1.917(11) . ? 
Cu1 O141 1.977(10) . ? 
Cu1 O112 1.989(11) . ? 
Cu1 O13 2.239(8) 1_655 ? 
O111 C11 1.12(2) . ? 
O112 C11 1.33(2) . ? 
O141 C14 1.304(18) . ? 
O142 C14 1.222(17) . ? 
C11 C12 1.41(2) . ? 
C12 C13 1.23(2) 2_565 ? 
C13 C12 1.23(2) 2_564 ? 
C13 C14 1.44(2) . ? 
O13 Cu1 2.239(8) 1_455 ? 
Cu2 O241 1.904(12) . ? 
Cu2 O211 1.981(11) . ? 
Cu2 O22 2.034(12) . ? 
Cu2 O21 2.042(11) . ? 
Cu2 O23 2.416(10) 1_455 ? 
O211 C21 1.207(18) . ? 
O212 C21 1.269(18) . ? 
O241 C24 1.262(18) . ? 
O242 C24 1.306(14) . ? 
C21 C22 1.51(2) 2_655 ? 
C22 C23 1.18(2) . ? 
C22 C21 1.51(2) 2_454 ? 
C23 C24 1.57(2) 1_455 ? 
C24 C23 1.57(2) 1_655 ? 
O23 Cu2 2.416(10) 1_655 ? 
 
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 
O12 Cu1 O11 164.2(5) . . ? 
O12 Cu1 O141 84.1(4) . . ? 
O11 Cu1 O141 95.5(5) . . ? 
O12 Cu1 O112 88.1(5) . . ? 
O11 Cu1 O112 91.2(5) . . ? 
O141 Cu1 O112 171.6(4) . . ? 
O12 Cu1 O13 101.1(5) . 1_655 ? 
O11 Cu1 O13 94.7(5) . 1_655 ? 
O141 Cu1 O13 94.3(4) . 1_655 ? 
O112 Cu1 O13 90.3(5) . 1_655 ? 
C11 O112 Cu1 116.3(11) . . ? 
C14 O141 Cu1 121.3(9) . . ? 
O111 C11 O112 125.0(15) . . ? 
O111 C11 C12 123.3(16) . . ? 
O112 C11 C12 110.6(15) . . ? 
C13 C12 C11 173(2) 2_565 . ? 
C12 C13 C14 164.0(14) 2_564 . ? 
O142 C14 O141 119.7(13) . . ? 
O142 C14 C13 128.7(12) . . ? 
O141 C14 C13 111.6(12) . . ? 
O241 Cu2 O211 178.2(6) . . ? 
O241 Cu2 O22 93.1(6) . . ? 
O211 Cu2 O22 85.2(5) . . ? 
O241 Cu2 O21 87.4(6) . . ? 
O211 Cu2 O21 94.3(5) . . ? 
O22 Cu2 O21 174.9(5) . . ? 
O241 Cu2 O23 88.1(5) . 1_455 ? 
O211 Cu2 O23 91.6(5) . 1_455 ? 
O22 Cu2 O23 91.4(5) . 1_455 ? 
O21 Cu2 O23 93.6(5) . 1_455 ? 
C21 O211 Cu2 110.0(10) . . ? 
C24 O241 Cu2 121.0(9) . . ? 
O211 C21 O212 131.8(14) . . ? 
O211 C21 C22 121.3(12) . 2_655 ? 
O212 C21 C22 106.4(12) . 2_655 ? 
C23 C22 C21 161.6(15) . 2_454 ? 
C22 C23 C24 166.7(17) . 1_455 ? 
O241 C24 O242 125.0(11) . . ? 
O241 C24 C23 117.4(11) . 1_655 ? 
O242 C24 C23 117.6(12) . 1_655 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.372 
_refine_diff_density_min   -0.390 
_refine_diff_density_rms    0.087 
