 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H33.33 Al K O10 S2' 
_chemical_formula_weight          323.80 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'K'  'K'   0.2009   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Al'  'Al'   0.0645   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   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' 
 '-x, y+1/2, -z+1/2' 
 '-x+1/2, -y, z+1/2' 
 'z, x, y' 
 'z+1/2, -x+1/2, -y' 
 '-z, x+1/2, -y+1/2' 
 '-z+1/2, -x, y+1/2' 
 'y, z, x' 
 'y+1/2, -z+1/2, -x' 
 '-y, z+1/2, -x+1/2' 
 '-y+1/2, -z, x+1/2' 
 '-x, -y, -z' 
 '-x-1/2, y-1/2, z' 
 'x, -y-1/2, z-1/2' 
 'x-1/2, y, -z-1/2' 
 '-z, -x, -y' 
 '-z-1/2, x-1/2, y' 
 'z, -x-1/2, y-1/2' 
 'z-1/2, x, -y-1/2' 
 '-y, -z, -x' 
 '-y-1/2, z-1/2, x' 
 'y, -z-1/2, x-1/2' 
 'y-1/2, z, -x-1/2' 
 
_cell_length_a                    12.1544(4) 
_cell_length_b                    12.1544(4) 
_cell_length_c                    12.1544(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1795.56(10) 
_cell_formula_units_Z             6 
_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     1.797 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1064 
_exptl_absorpt_coefficient_mu     0.898 
_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             11748 
_diffrn_reflns_av_R_equivalents   0.0219 
_diffrn_reflns_av_sigmaI/netI     0.0075 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          2.90 
_diffrn_reflns_theta_max          25.95 
_reflns_number_total              589 
_reflns_number_gt                 566 
_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)+(0.0284P)²+1.0017P] 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        0.0130(14) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          589 
_refine_ls_number_parameters      68 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0302 
_refine_ls_R_factor_gt            0.0279 
_refine_ls_wR_factor_ref          0.0638 
_refine_ls_wR_factor_gt           0.0623 
_refine_ls_goodness_of_fit_ref    1.161 
_refine_ls_restrained_S_all       1.161 
_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 
K1 K 0.5000 0.0000 0.0000 0.0444(3) Uani 1 6 d S . . 
Al1 Al 0.0000 0.5000 0.5000 0.0162(3) Uani 1 6 d S . . 
S1 S 0.30770(3) 0.30770(3) 0.30770(3) 0.0216(3) Uani 1 3 d S . . 
O1 O 0.2655(3) 0.4211(2) 0.31028(19) 0.0430(9) Uani 0.691(6) 1 d P . . 
O2 O 0.23932(19) 0.23932(19) 0.23932(19) 0.0597(13) Uani 0.691(6) 3 d SP . . 
O11 O 0.2047(5) 0.3653(6) 0.2853(4) 0.046(2) Uani 0.309(6) 1 d P . . 
O22 O 0.3749(4) 0.3749(4) 0.3749(4) 0.077(4) Uani 0.309(6) 3 d SP . . 
O3 O 0.15172(10) 0.48023(11) 0.48141(12) 0.0258(3) Uani 1 1 d . . . 
O4 O 0.13344(13) 0.30261(12) 0.04605(17) 0.0373(4) Uani 1 1 d . . . 
H11 H 0.1736(19) 0.461(2) 0.429(2) 0.040(7) Uiso 1 1 d . . . 
H12 H 0.199(2) 0.471(2) 0.536(2) 0.058(8) Uiso 1 1 d . . . 
H21 H 0.153(3) 0.299(2) 0.097(3) 0.057(10) Uiso 1 1 d . . . 
H22 H 0.182(2) 0.293(2) 0.007(2) 0.056(9) 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 
K1 O22 2.634(9) 15_565 ? 
K1 O22 2.634(9) 3_645 ? 
K1 O4 2.9496(16) 20_656 ? 
K1 O4 2.9496(16) 8_554 ? 
K1 O4 2.9496(16) 2 ? 
K1 O4 2.9496(16) 14_655 ? 
K1 O4 2.9496(16) 21_655 ? 
K1 O4 2.9496(16) 9 ? 
Al1 O3 1.8733(12) 24_556 ? 
Al1 O3 1.8733(12) 12_565 ? 
Al1 O3 1.8733(12) 18_665 ? 
Al1 O3 1.8733(12) 6_456 ? 
Al1 O3 1.8733(12) . ? 
Al1 O3 1.8733(12) 13_566 ? 
S1 O22 1.414(9) . ? 
S1 O2 1.440(4) . ? 
S1 O11 1.460(4) 9 ? 
S1 O11 1.460(4) . ? 
S1 O11 1.460(4) 5 ? 
S1 O1 1.471(2) . ? 
S1 O1 1.471(2) 9 ? 
S1 O1 1.471(2) 5 ? 
O1 O11 1.048(7) . ? 
O1 O22 1.643(6) . ? 
O2 O11 1.684(7) 9 ? 
O2 O11 1.684(7) . ? 
O2 O11 1.684(7) 5 ? 
O22 O1 1.643(6) 9 ? 
O22 O1 1.643(6) 5 ? 
O22 K1 2.634(9) 3_655 ? 
O4 K1 2.9496(16) 2_455 ? 
 
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 
O22 K1 O22 180.0(6) 15_565 3_645 ? 
O22 K1 O4 105.17(3) 15_565 20_656 ? 
O22 K1 O4 74.83(3) 3_645 20_656 ? 
O22 K1 O4 74.83(3) 15_565 8_554 ? 
O22 K1 O4 105.17(3) 3_645 8_554 ? 
O4 K1 O4 180.00(3) 20_656 8_554 ? 
O22 K1 O4 74.83(3) 15_565 2 ? 
O22 K1 O4 105.17(3) 3_645 2 ? 
O4 K1 O4 66.59(3) 20_656 2 ? 
O4 K1 O4 113.41(3) 8_554 2 ? 
O22 K1 O4 105.17(3) 15_565 14_655 ? 
O22 K1 O4 74.83(3) 3_645 14_655 ? 
O4 K1 O4 113.41(3) 20_656 14_655 ? 
O4 K1 O4 66.59(3) 8_554 14_655 ? 
O4 K1 O4 180.00(9) 2 14_655 ? 
O22 K1 O4 105.17(3) 15_565 21_655 ? 
O22 K1 O4 74.83(3) 3_645 21_655 ? 
O4 K1 O4 113.41(3) 20_656 21_655 ? 
O4 K1 O4 66.59(3) 8_554 21_655 ? 
O4 K1 O4 66.59(3) 2 21_655 ? 
O4 K1 O4 113.41(3) 14_655 21_655 ? 
O22 K1 O4 74.83(3) 15_565 9 ? 
O22 K1 O4 105.17(3) 3_645 9 ? 
O4 K1 O4 66.59(3) 20_656 9 ? 
O4 K1 O4 113.41(3) 8_554 9 ? 
O4 K1 O4 113.41(3) 2 9 ? 
O4 K1 O4 66.59(3) 14_655 9 ? 
O4 K1 O4 180.00(6) 21_655 9 ? 
O3 Al1 O3 180.0 24_556 12_565 ? 
O3 Al1 O3 90.45(6) 24_556 18_665 ? 
O3 Al1 O3 89.55(6) 12_565 18_665 ? 
O3 Al1 O3 89.55(6) 24_556 6_456 ? 
O3 Al1 O3 90.45(6) 12_565 6_456 ? 
O3 Al1 O3 180.0 18_665 6_456 ? 
O3 Al1 O3 89.55(6) 24_556 . ? 
O3 Al1 O3 90.45(6) 12_565 . ? 
O3 Al1 O3 89.55(6) 18_665 . ? 
O3 Al1 O3 90.45(6) 6_456 . ? 
O3 Al1 O3 90.45(6) 24_556 13_566 ? 
O3 Al1 O3 89.55(6) 12_565 13_566 ? 
O3 Al1 O3 90.45(6) 18_665 13_566 ? 
O3 Al1 O3 89.55(6) 6_456 13_566 ? 
O3 Al1 O3 180.0 . 13_566 ? 
O22 S1 O2 180.0(2) . . ? 
O22 S1 O11 109.0(3) . 9 ? 
O2 S1 O11 71.0(3) . 9 ? 
O22 S1 O11 109.0(3) . . ? 
O2 S1 O11 71.0(3) . . ? 
O11 S1 O11 109.9(3) 9 . ? 
O22 S1 O11 109.0(3) . 5 ? 
O2 S1 O11 71.0(3) . 5 ? 
O11 S1 O11 109.9(3) 9 5 ? 
O11 S1 O11 109.9(3) . 5 ? 
O22 S1 O1 69.40(14) . . ? 
O2 S1 O1 110.60(14) . . ? 
O11 S1 O1 111.1(2) 9 . ? 
O11 S1 O1 41.9(3) . . ? 
O11 S1 O1 136.7(2) 5 . ? 
O22 S1 O1 69.40(14) . 9 ? 
O2 S1 O1 110.60(14) . 9 ? 
O11 S1 O1 41.9(3) 9 9 ? 
O11 S1 O1 136.7(2) . 9 ? 
O11 S1 O1 111.1(2) 5 9 ? 
O1 S1 O1 108.32(15) . 9 ? 
O22 S1 O1 69.40(14) . 5 ? 
O2 S1 O1 110.60(14) . 5 ? 
O11 S1 O1 136.7(2) 9 5 ? 
O11 S1 O1 111.1(2) . 5 ? 
O11 S1 O1 41.9(3) 5 5 ? 
O1 S1 O1 108.32(15) . 5 ? 
O1 S1 O1 108.32(15) 9 5 ? 
O11 O1 S1 68.5(3) . . ? 
O11 O1 O22 119.2(4) . . ? 
S1 O1 O22 53.7(3) . . ? 
S1 O2 O11 55.1(3) . 9 ? 
S1 O2 O11 55.1(3) . . ? 
O11 O2 O11 90.5(4) 9 . ? 
S1 O2 O11 55.1(3) . 5 ? 
O11 O2 O11 90.5(4) 9 5 ? 
O11 O2 O11 90.5(4) . 5 ? 
O1 O11 S1 69.6(3) . . ? 
O1 O11 O2 120.6(4) . . ? 
S1 O11 O2 53.9(2) . . ? 
S1 O22 O1 56.9(3) . 9 ? 
S1 O22 O1 56.9(3) . . ? 
O1 O22 O1 93.1(4) 9 . ? 
S1 O22 O1 56.9(3) . 5 ? 
O1 O22 O1 93.1(4) 9 5 ? 
O1 O22 O1 93.1(4) . 5 ? 
S1 O22 K1 180.0(8) . 3_655 ? 
O1 O22 K1 123.1(3) 9 3_655 ? 
O1 O22 K1 123.1(3) . 3_655 ? 
O1 O22 K1 123.1(3) 5 3_655 ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.95 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.276 
_refine_diff_density_min   -0.191 
_refine_diff_density_rms    0.040 
