 
data_sl97 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C12 H24 I K O6' 
_chemical_formula_weight          430.31 
 
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' 
 'I'  'I'  -0.4742   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' 
 '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, z+1/2' 
 'x+1/2, -y+1/2, -z' 
 '-x, y+1/2, -z+1/2' 
 
_cell_length_a                    8.4246(10) 
_cell_length_b                    13.0061(14) 
_cell_length_c                    17.674(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.040(11) 
_cell_angle_gamma                 90.00 
_cell_volume                      1936.6(4) 
_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     1.476 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              864 
_exptl_absorpt_coefficient_mu     1.885 
_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             10547 
_diffrn_reflns_av_R_equivalents   0.1111 
_diffrn_reflns_av_sigmaI/netI     0.0828 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.30 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              1953 
_reflns_number_gt                 1265 
_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)+(0.0550P)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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0(10) 
_refine_ls_number_reflns          1953 
_refine_ls_number_parameters      185 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1186 
_refine_ls_R_factor_gt            0.0746 
_refine_ls_wR_factor_ref          0.1395 
_refine_ls_wR_factor_gt           0.1255 
_refine_ls_goodness_of_fit_ref    1.091 
_refine_ls_restrained_S_all       1.091 
_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 
I1 I 0.82248(15) 0.65384(9) 0.84225(8) 0.1078(6) Uani 1 1 d . . . 
K1 K 0.6549(3) 0.44781(19) 0.92832(14) 0.0498(7) Uani 1 1 d . . . 
O1 O 0.4202(18) 0.5367(10) 1.0147(9) 0.113(5) Uani 1 1 d . . . 
O2 O 0.3352(17) 0.4617(11) 0.8735(9) 0.112(5) Uani 1 1 d . . . 
O3 O 0.564(2) 0.3700(8) 0.7870(5) 0.104(5) Uani 1 1 d . . . 
O4 O 0.8176(17) 0.2763(7) 0.8588(7) 0.097(4) Uani 1 1 d . . . 
O5 O 0.9094(13) 0.3554(11) 1.0020(8) 0.106(4) Uani 1 1 d . . . 
O6 O 0.681(2) 0.4478(10) 1.0882(5) 0.107(5) Uani 1 1 d . . . 
C12 C 0.266(4) 0.533(3) 0.994(3) 0.23(3) Uani 1 1 d . . . 
H12A H 0.2051 0.5829 1.0222 0.281 Uiso 1 1 calc R . . 
H12B H 0.2232 0.4649 1.0039 0.281 Uiso 1 1 calc R . . 
C21 C 0.261(4) 0.554(3) 0.917(3) 0.22(2) Uani 1 1 d . . . 
H21A H 0.3198 0.6168 0.9062 0.262 Uiso 1 1 calc R . . 
H21B H 0.1516 0.5646 0.9010 0.262 Uiso 1 1 calc R . . 
C23 C 0.340(3) 0.4801(18) 0.802(2) 0.156(12) Uani 1 1 d . . . 
H23A H 0.4082 0.5384 0.7918 0.188 Uiso 1 1 calc R . . 
H23B H 0.2339 0.4964 0.7835 0.188 Uiso 1 1 calc R . . 
C32 C 0.400(3) 0.389(2) 0.7631(9) 0.119(9) Uani 1 1 d . . . 
H32A H 0.3962 0.3990 0.7088 0.143 Uiso 1 1 calc R . . 
H32B H 0.3347 0.3297 0.7755 0.143 Uiso 1 1 calc R . . 
C34 C 0.629(5) 0.2899(17) 0.7567(12) 0.174(18) Uani 1 1 d . . . 
H34A H 0.6165 0.2929 0.7022 0.208 Uiso 1 1 calc R . . 
H34B H 0.5756 0.2284 0.7747 0.208 Uiso 1 1 calc R . . 
C43 C 0.809(4) 0.2846(18) 0.7773(11) 0.131(10) Uani 1 1 d . . . 
H43A H 0.8583 0.2252 0.7537 0.157 Uiso 1 1 calc R . . 
H43B H 0.8636 0.3460 0.7602 0.157 Uiso 1 1 calc R . . 
C45 C 0.967(3) 0.2805(15) 0.8785(15) 0.124(8) Uani 1 1 d . . . 
H45A H 1.0102 0.3458 0.8620 0.149 Uiso 1 1 calc R . . 
H45B H 1.0239 0.2265 0.8523 0.149 Uiso 1 1 calc R . . 
C54 C 0.995(2) 0.2696(15) 0.9604(13) 0.110(7) Uani 1 1 d . . . 
H54A H 1.1075 0.2728 0.9708 0.132 Uiso 1 1 calc R . . 
H54B H 0.9553 0.2035 0.9775 0.132 Uiso 1 1 calc R . . 
C56 C 0.921(3) 0.348(3) 1.0744(18) 0.180(17) Uani 1 1 d . . . 
H56A H 1.0318 0.3404 1.0880 0.216 Uiso 1 1 calc R . . 
H56B H 0.8659 0.2861 1.0908 0.216 Uiso 1 1 calc R . . 
C65 C 0.853(3) 0.438(3) 1.1152(9) 0.150(13) Uani 1 1 d . . . 
H65A H 0.9126 0.5000 1.1031 0.180 Uiso 1 1 calc R . . 
H65B H 0.8573 0.4273 1.1695 0.180 Uiso 1 1 calc R . . 
C61 C 0.610(5) 0.526(2) 1.1193(13) 0.157(14) Uani 1 1 d . . . 
H61A H 0.6619 0.5887 1.1032 0.189 Uiso 1 1 calc R . . 
H61B H 0.6202 0.5209 1.1738 0.189 Uiso 1 1 calc R . . 
C16 C 0.439(4) 0.531(2) 1.0992(18) 0.164(14) Uani 1 1 d . . . 
H16A H 0.3916 0.5919 1.1222 0.197 Uiso 1 1 calc R . . 
H16B H 0.3841 0.4713 1.1184 0.197 Uiso 1 1 calc R . . 
O11 O 0.460(3) 0.7897(17) 0.9543(11) 0.205(8) 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 
I1 K1 3.390(3) . ? 
K1 O1 2.754(12) . ? 
K1 O5 2.781(11) . ? 
K1 O3 2.800(10) . ? 
K1 O6 2.834(9) . ? 
K1 O2 2.868(13) . ? 
K1 O4 2.893(11) . ? 
K1 C23 3.50(3) . ? 
K1 C45 3.52(2) . ? 
O1 C12 1.35(4) . ? 
O1 C16 1.50(3) . ? 
O2 C23 1.29(3) . ? 
O2 C21 1.56(4) . ? 
O3 C34 1.29(3) . ? 
O3 C32 1.47(2) . ? 
O4 C45 1.30(3) . ? 
O4 C43 1.45(2) . ? 
O5 C56 1.29(3) . ? 
O5 C54 1.52(2) . ? 
O6 C61 1.30(3) . ? 
O6 C65 1.54(3) . ? 
C12 C21 1.39(5) . ? 
C23 C32 1.46(3) . ? 
C34 C43 1.57(4) . ? 
C45 C54 1.47(3) . ? 
C56 C65 1.49(4) . ? 
C61 C16 1.49(4) . ? 
 
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 
O1 K1 O5 118.4(5) . . ? 
O1 K1 O3 116.8(5) . . ? 
O5 K1 O3 118.1(5) . . ? 
O1 K1 O6 60.1(5) . . ? 
O5 K1 O6 58.3(5) . . ? 
O3 K1 O6 155.5(3) . . ? 
O1 K1 O2 59.1(5) . . ? 
O5 K1 O2 155.4(4) . . ? 
O3 K1 O2 57.7(5) . . ? 
O6 K1 O2 114.1(5) . . ? 
O1 K1 O4 154.2(4) . . ? 
O5 K1 O4 60.0(5) . . ? 
O3 K1 O4 58.1(4) . . ? 
O6 K1 O4 112.8(4) . . ? 
O2 K1 O4 110.5(5) . . ? 
O1 K1 I1 102.5(3) . . ? 
O5 K1 I1 103.3(3) . . ? 
O3 K1 I1 89.9(2) . . ? 
O6 K1 I1 114.6(2) . . ? 
O2 K1 I1 100.9(2) . . ? 
O4 K1 I1 102.8(2) . . ? 
O1 K1 C23 76.0(8) . . ? 
O5 K1 C23 159.5(6) . . ? 
O3 K1 C23 42.8(7) . . ? 
O6 K1 C23 134.1(7) . . ? 
O2 K1 C23 20.5(6) . . ? 
O4 K1 C23 100.4(7) . . ? 
I1 K1 C23 86.3(4) . . ? 
O1 K1 C45 159.0(5) . . ? 
O5 K1 C45 43.6(6) . . ? 
O3 K1 C45 75.9(6) . . ? 
O6 K1 C45 101.1(6) . . ? 
O2 K1 C45 130.9(6) . . ? 
O4 K1 C45 20.6(5) . . ? 
I1 K1 C45 93.7(4) . . ? 
C23 K1 C45 118.7(8) . . ? 
C12 O1 C16 112(3) . . ? 
C12 O1 K1 122(2) . . ? 
C16 O1 K1 117.2(14) . . ? 
C23 O2 C21 111(2) . . ? 
C23 O2 K1 108.4(17) . . ? 
C21 O2 K1 105.0(13) . . ? 
C34 O3 C32 114(2) . . ? 
C34 O3 K1 123.2(18) . . ? 
C32 O3 K1 117.0(11) . . ? 
C45 O4 C43 108.0(19) . . ? 
C45 O4 K1 108.1(12) . . ? 
C43 O4 K1 110.1(11) . . ? 
C56 O5 C54 113(2) . . ? 
C56 O5 K1 123.8(17) . . ? 
C54 O5 K1 117.1(10) . . ? 
C61 O6 C65 112(2) . . ? 
C61 O6 K1 112.7(14) . . ? 
C65 O6 K1 112.4(10) . . ? 
O1 C12 C21 107(3) . . ? 
C12 C21 O2 108(3) . . ? 
O2 C23 C32 108.6(19) . . ? 
O2 C23 K1 51.1(13) . . ? 
C32 C23 K1 86.4(13) . . ? 
C23 C32 O3 109.2(15) . . ? 
O3 C34 C43 110(2) . . ? 
O4 C43 C34 106.4(19) . . ? 
O4 C45 C54 114.3(19) . . ? 
O4 C45 K1 51.3(9) . . ? 
C54 C45 K1 86.1(12) . . ? 
C45 C54 O5 109.3(14) . . ? 
O5 C56 C65 113(2) . . ? 
C56 C65 O6 106.0(16) . . ? 
O6 C61 C16 113(3) . . ? 
C61 C16 O1 109.9(19) . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.444 
_refine_diff_density_min   -0.323 
_refine_diff_density_rms    0.078 
