

 
 
data_aw0101 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C24 H56 O5 Zn4' 
_chemical_formula_weight          686.17 
 
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'   0.0000   0.0000 
 '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' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Tetragonal
_symmetry_space_group_name_H-M    I4(1)/acd 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, z+1/2' 
 'y+1/4, x+1/4, z+1/4' 
 '-y+3/4, x+1/4, z+3/4' 
 'x, -y+1/2, z+1/2' 
 '-x, -y+1/2, z' 
 'y+1/4, -x+1/4, z+3/4' 
 '-y+3/4, -x+1/4, z+1/4' 
 'x+1/2, y+1/2, z+1/2' 
 '-x+1/2, y+1/2, z+1' 
 'y+3/4, x+3/4, z+3/4' 
 '-y+5/4, x+3/4, z+5/4' 
 'x+1/2, -y+1, z+1' 
 '-x+1/2, -y+1, z+1/2' 
 'y+3/4, -x+3/4, z+5/4' 
 '-y+5/4, -x+3/4, z+3/4' 
 '-x, -y, -z' 
 'x, -y, -z-1/2' 
 '-y-1/4, -x-1/4, -z-1/4' 
 'y-3/4, -x-1/4, -z-3/4' 
 '-x, y-1/2, -z-1/2' 
 'x, y-1/2, -z' 
 '-y-1/4, x-1/4, -z-3/4' 
 'y-3/4, x-1/4, -z-1/4' 
 '-x+1/2, -y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-y+1/4, -x+1/4, -z+1/4' 
 'y-1/4, -x+1/4, -z-1/4' 
 '-x+1/2, y, -z' 
 'x+1/2, y, -z+1/2' 
 '-y+1/4, x+1/4, -z-1/4' 
 'y-1/4, x+1/4, -z+1/4' 
 
_cell_length_a                    14.8323(7) 
_cell_length_b                    14.8323(7) 
_cell_length_c                    30.0976(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      6621.4(5) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     180(2) 
_cell_measurement_reflns_used     6316
_cell_measurement_theta_min       1.0 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.23 
_exptl_crystal_size_min           0.23 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.377 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2880 
_exptl_absorpt_coefficient_mu     2.889 
_exptl_absorpt_correction_type 'multiscan' 
_exptl_absorpt_correction_T_max  1.105
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_process_details 
;
multi-scan from symmetry-related measurements (Blessing 1995)
;
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       180(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_measurement_device_type   'KappaCCD'
_diffrn_measurement_device        '95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean  9
_diffrn_radiation_monochromator   'horizonally mounted graphite crystal'
_diffrn_measurement_method        'CCD'
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10143 
_diffrn_reflns_av_R_equivalents   0.0553 
_diffrn_reflns_av_sigmaI/netI     0.0351 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        19 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -38 
_diffrn_reflns_limit_l_max        39 
_diffrn_reflns_theta_min          3.68 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              1876 
_reflns_number_gt                 1421 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'Collect (Nonius BV, 1997-2000)' 
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution     teXsan
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ 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/[\s^2^(Fo^2^)+(0.0531P)^2^+5.7780P] where P=(Fo^2^+2Fc^2^)/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          1876 
_refine_ls_number_parameters      85 
_refine_ls_number_restraints      10 
_refine_ls_R_factor_all           0.0587 
_refine_ls_R_factor_gt            0.0390 
_refine_ls_wR_factor_ref          0.1099 
_refine_ls_wR_factor_gt           0.0978 
_refine_ls_goodness_of_fit_ref    1.079 
_refine_ls_restrained_S_all       1.078 
_refine_ls_shift/su_max           0.001 
_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 
Zn1 Zn 0.92093(2) 0.31641(2) 0.411142(11) 0.04360(17) Uani 1 1 d . . . 
O1 O 0.92857(12) 0.30983(13) 0.34258(6) 0.0379(5) Uani 1 1 d . . . 
C1 C 0.8386(3) 0.3859(3) 0.44905(15) 0.0946(14) Uani 1 1 d . . . 
H1A H 0.8559 0.3783 0.4802 0.142 Uiso 1 1 calc R . . 
H1B H 0.7768 0.3642 0.4448 0.142 Uiso 1 1 calc R . . 
H1C H 0.8419 0.4499 0.4410 0.142 Uiso 1 1 calc R . . 
C2 C 0.8667(2) 0.3621(2) 0.31474(11) 0.0675(10) Uani 1 1 d . . . 
C3 C 0.7720(3) 0.3322(3) 0.32614(16) 0.0913(14) Uani 1 1 d . . . 
H3A H 0.7605 0.3429 0.3578 0.137 Uiso 1 1 calc R . . 
H3B H 0.7654 0.2677 0.3197 0.137 Uiso 1 1 calc R . . 
H3C H 0.7286 0.3665 0.3083 0.137 Uiso 1 1 calc R . . 
C4 C 0.8815(3) 0.4603(3) 0.32557(16) 0.0968(15) Uani 1 1 d . . . 
H4A H 0.8681 0.4709 0.3570 0.145 Uiso 1 1 calc R . . 
H4B H 0.8417 0.4975 0.3072 0.145 Uiso 1 1 calc R . . 
H4C H 0.9444 0.4764 0.3195 0.145 Uiso 1 1 calc R . . 
C5 C 0.8898(4) 0.3403(3) 0.26667(13) 0.0998(16) Uani 1 1 d . . . 
H5A H 0.8811 0.2757 0.2613 0.150 Uiso 1 1 calc R . . 
H5B H 0.9528 0.3564 0.2609 0.150 Uiso 1 1 calc R . . 
H5C H 0.8503 0.3749 0.2469 0.150 Uiso 1 1 calc R . . 
O2 O 0.5473(14) 0.1892(11) 0.3922(8) 0.123(4) Uiso 0.25 1 d PD A -1 
C6 C 0.542(2) 0.2795(17) 0.4085(7) 0.123(4) Uiso 0.25 1 d PD A -1 
H6A H 0.5090 0.2805 0.4372 0.148 Uiso 0.25 1 calc PR A -1 
H6B H 0.6032 0.3038 0.4135 0.148 Uiso 0.25 1 calc PR A -1 
C7 C 0.496(3) 0.3330(14) 0.3768(9) 0.123(4) Uiso 0.25 1 d PD A -1 
H7A H 0.5355 0.3817 0.3658 0.148 Uiso 0.25 1 calc PR A -1 
H7B H 0.4415 0.3607 0.3903 0.148 Uiso 0.25 1 calc PR A -1 
C8 C 0.470(2) 0.2737(16) 0.3407(7) 0.123(4) Uiso 0.25 1 d PD A -1 
H8A H 0.4061 0.2831 0.3327 0.148 Uiso 0.25 1 calc PR A -1 
H8B H 0.5076 0.2860 0.3141 0.148 Uiso 0.25 1 calc PR A -1 
C9 C 0.4840(19) 0.1837(13) 0.3556(11) 0.123(4) Uiso 0.25 1 d PD A -1 
H9A H 0.5089 0.1461 0.3313 0.148 Uiso 0.25 1 calc PR A -1 
H9B H 0.4264 0.1568 0.3656 0.148 Uiso 0.25 1 calc PR A -1 
 
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 
Zn1 0.0424(2) 0.0425(2) 0.0458(3) -0.00553(13) 0.00716(14) 0.00873(13) 
O1 0.0360(10) 0.0374(10) 0.0403(10) 0.0077(8) -0.0077(7) 0.0039(7) 
C1 0.091(3) 0.098(3) 0.095(3) -0.030(2) 0.029(2) 0.034(3) 
C2 0.061(2) 0.069(2) 0.073(2) 0.0262(18) -0.0219(17) 0.0132(18) 
C3 0.050(2) 0.106(3) 0.118(3) 0.023(3) -0.030(2) 0.018(2) 
C4 0.099(3) 0.058(2) 0.133(4) 0.039(2) -0.018(3) 0.025(2) 
C5 0.110(4) 0.131(4) 0.058(2) 0.036(2) -0.033(2) 0.009(3) 
 
_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 
Zn1 C1 1.964(3) . ? 
Zn1 O1 2.0647(19) 28_666 ? 
Zn1 O1 2.0673(18) 31_646 ? 
Zn1 O1 2.0690(19) . ? 
Zn1 Zn1 3.0633(7) 6_755 ? 
Zn1 Zn1 3.0700(6) 31_646 ? 
Zn1 Zn1 3.0700(6) 28_666 ? 
O1 C2 1.465(3) . ? 
O1 Zn1 2.0647(19) 31_646 ? 
O1 Zn1 2.0674(18) 28_666 ? 
C2 C4 1.510(6) . ? 
C2 C3 1.512(5) . ? 
C2 C5 1.522(6) . ? 
O2 C6 1.429(17) . ? 
O2 C9 1.450(17) . ? 
C6 C7 1.418(18) . ? 
C7 C8 1.449(17) . ? 
C8 C9 1.423(18) . ? 
 
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 
C1 Zn1 O1 129.30(15) . 28_666 ? 
C1 Zn1 O1 129.53(15) . 31_646 ? 
O1 Zn1 O1 83.97(8) 28_666 31_646 ? 
C1 Zn1 O1 129.66(15) . . ? 
O1 Zn1 O1 83.85(7) 28_666 . ? 
O1 Zn1 O1 83.78(8) 31_646 . ? 
C1 Zn1 Zn1 144.48(14) . 6_755 ? 
O1 Zn1 Zn1 42.19(5) 28_666 6_755 ? 
O1 Zn1 Zn1 42.12(5) 31_646 6_755 ? 
O1 Zn1 Zn1 85.85(5) . 6_755 ? 
C1 Zn1 Zn1 144.96(14) . 31_646 ? 
O1 Zn1 Zn1 85.75(5) 28_666 31_646 ? 
O1 Zn1 Zn1 42.10(5) 31_646 31_646 ? 
O1 Zn1 Zn1 41.98(5) . 31_646 ? 
Zn1 Zn1 Zn1 60.073(7) 6_755 31_646 ? 
C1 Zn1 Zn1 144.77(14) . 28_666 ? 
O1 Zn1 Zn1 42.09(5) 28_666 28_666 ? 
O1 Zn1 Zn1 85.70(5) 31_646 28_666 ? 
O1 Zn1 Zn1 42.06(5) . 28_666 ? 
Zn1 Zn1 Zn1 60.073(7) 6_755 28_666 ? 
Zn1 Zn1 Zn1 59.854(13) 31_646 28_666 ? 
C2 O1 Zn1 121.28(19) . 31_646 ? 
C2 O1 Zn1 121.07(19) . 28_666 ? 
Zn1 O1 Zn1 95.69(8) 31_646 28_666 ? 
C2 O1 Zn1 120.74(19) . . ? 
Zn1 O1 Zn1 95.92(8) 31_646 . ? 
Zn1 O1 Zn1 95.84(7) 28_666 . ? 
O1 C2 C4 107.2(3) . . ? 
O1 C2 C3 107.3(3) . . ? 
C4 C2 C3 111.7(4) . . ? 
O1 C2 C5 106.9(3) . . ? 
C4 C2 C5 112.1(4) . . ? 
C3 C2 C5 111.3(4) . . ? 
C6 O2 C9 106.2(10) . . ? 
C7 C6 O2 108.6(10) . . ? 
C6 C7 C8 107.0(10) . . ? 
C9 C8 C7 107.2(12) . . ? 
C8 C9 O2 106.3(12) . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.401 
_refine_diff_density_min   -0.530 
_refine_diff_density_rms    0.093 
