 
data_182 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             (K3I)In4(B12Se12)
_chemical_melting_point           ?                
_chemical_formula_moiety          (K3I)In4(B12Se12)
_chemical_formula_sum 
 'B12 I In4 K3 Se12' 
_chemical_formula_weight          1780.72 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Se'  'Se'  -0.0929   2.2259 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'In'  'In'  -0.7276   1.3100 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal 
_symmetry_space_group_name_H-M    P6(3)22   
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 'y, x, -z' 
 'x-y, -y, -z' 
 '-x, -x+y, -z' 
 '-y, -x, -z+1/2' 
 '-x+y, y, -z+1/2' 
 'x, x-y, -z+1/2' 
 
_cell_length_a                    13.896(5) 
_cell_length_b                    13.896(5) 
_cell_length_c                    9.687(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1619.9(13) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     10430 
_cell_measurement_theta_min       2.70  
_cell_measurement_theta_max       25.50 
 
_exptl_crystal_description        prism	 
_exptl_crystal_colour             yellow  
_exptl_crystal_size_max           0.20    
_exptl_crystal_size_mid           0.10    
_exptl_crystal_size_min           0.06    
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.651 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1548 
_exptl_absorpt_coefficient_mu     17.630 
_exptl_absorpt_correction_type    'Multi-scan'                    
_exptl_absorpt_correction_T_min   0.3033                          
_exptl_absorpt_correction_T_max   1.0000                          
_exptl_absorpt_process_details    'Sphere (Rigaku CrystalClear)'  
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'rotating-anode generator' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku Mercury CCD'   
_diffrn_measurement_method        ω                     
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10403 
_diffrn_reflns_av_R_equivalents   0.1354 
_diffrn_reflns_av_sigmaI/netI     0.0651 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.70 
_diffrn_reflns_theta_max          25.50 
_reflns_number_total              1013 
_reflns_number_gt                 820 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear (Rigaku Corp., 2002)'  
_computing_cell_refinement        'CrystalClear (Rigaku Corp., 2002)'  
_computing_data_reduction         'CrystalClear (Rigaku Corp., 2002)'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   'Siemens SHELXTLTM 5' 
 
_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)+(0.1399P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    ? 
_refine_ls_hydrogen_treatment     ?
_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    0.01(6) 
_refine_ls_number_reflns          1013 
_refine_ls_number_parameters      54 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0732 
_refine_ls_R_factor_gt            0.0668 
_refine_ls_wR_factor_ref          0.1903 
_refine_ls_wR_factor_gt           0.1841 
_refine_ls_goodness_of_fit_ref    0.977 
_refine_ls_restrained_S_all       0.976 
_refine_ls_shift/su_max           0.077 
_refine_ls_shift/su_mean          0.004 
 
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 
In1 In 0.3333 0.6667 0.2500 0.0395(8) Uani 1 6 d S . . 
In2 In 0.0000 0.52979(13) 0.5000 0.0462(6) Uani 1 2 d S . . 
Se1 Se 0.17373(15) 0.50541(14) 0.43588(16) 0.0370(5) Uani 1 1 d . . . 
Se2 Se 0.06973(14) 0.67654(16) 0.69289(19) 0.0446(6) Uani 1 1 d . . . 
B1 B 0.2097(15) 0.6657(18) 0.7158(17) 0.039(5) Uani 1 1 d . . . 
B2 B 0.2560(14) 0.5888(15) 0.6099(18) 0.031(4) Uani 1 1 d . . . 
K1 K 0.0000 0.2020(13) 0.5000 0.198(7) Uani 1 2 d S . . 
I1A I 0.0000 0.0000 0.7500 0.286(9) Uani 0.679(4) 6 d SP . . 
I1B I 0.0000 0.0000 0.606(7) 0.286(9) Uani 0.1603(19) 3 d SP . . 
 
 
_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 
In1 Se1 2.8657(19) 3_565 ? 
In1 Se1 2.8657(19) 12_565 ? 
In1 Se1 2.8657(19) 10_665 ? 
In1 Se1 2.8657(19) . ? 
In1 Se1 2.8657(19) 2_665 ? 
In1 Se1 2.8657(19) 11 ? 
In2 Se2 2.571(2) . ? 
In2 Se2 2.571(2) 9_556 ? 
In2 Se1 2.673(2) 9_556 ? 
In2 Se1 2.673(2) . ? 
Se1 B2 2.041(17) . ? 
Se1 K1 3.716(15) . ? 
Se2 B1 2.037(18) . ? 
Se2 K1 3.778(10) 4_565 ? 
B1 B2 1.80(2) 12_566 ? 
B1 B1 1.82(4) 12_566 ? 
B1 B2 1.82(2) . ? 
B1 B2 1.82(3) 3_565 ? 
B1 B1 1.85(4) 10_666 ? 
B2 B1 1.80(2) 12_566 ? 
B2 B1 1.82(3) 2_665 ? 
B2 B2 1.87(3) 3_565 ? 
B2 B2 1.87(3) 2_665 ? 
K1 I1B 2.99(3) 7_556 ? 
K1 I1B 2.99(3) . ? 
K1 I1A 3.707(14) 4_554 ? 
K1 I1A 3.707(14) . ? 
K1 Se1 3.716(15) 9_556 ? 
K1 Se2 3.778(10) 12_566 ? 
K1 Se2 3.778(10) 4_564 ? 
K1 K1 4.86(3) 2 ? 
K1 K1 4.86(3) 3 ? 
I1A I1B 1.39(6) 10_556 ? 
I1A I1B 1.39(6) . ? 
I1A K1 3.707(14) 5 ? 
I1A K1 3.707(14) 2 ? 
I1A K1 3.707(14) 3 ? 
I1A K1 3.707(14) 4 ? 
I1A K1 3.707(14) 6 ? 
I1B I1B 2.06(13) 7_556 ? 
I1B K1 2.99(3) 2 ? 
I1B K1 2.99(3) 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 
Se1 In1 Se1 94.75(7) 3_565 12_565 ? 
Se1 In1 Se1 95.83(8) 3_565 10_665 ? 
Se1 In1 Se1 84.71(6) 12_565 10_665 ? 
Se1 In1 Se1 84.71(6) 3_565 . ? 
Se1 In1 Se1 95.83(8) 12_565 . ? 
Se1 In1 Se1 179.20(7) 10_665 . ? 
Se1 In1 Se1 84.71(6) 3_565 2_665 ? 
Se1 In1 Se1 179.20(7) 12_565 2_665 ? 
Se1 In1 Se1 94.75(7) 10_665 2_665 ? 
Se1 In1 Se1 84.71(6) . 2_665 ? 
Se1 In1 Se1 179.20(7) 3_565 11 ? 
Se1 In1 Se1 84.71(6) 12_565 11 ? 
Se1 In1 Se1 84.71(6) 10_665 11 ? 
Se1 In1 Se1 94.75(7) . 11 ? 
Se1 In1 Se1 95.83(8) 2_665 11 ? 
Se2 In2 Se2 105.60(11) . 9_556 ? 
Se2 In2 Se1 115.85(6) . 9_556 ? 
Se2 In2 Se1 105.26(5) 9_556 9_556 ? 
Se2 In2 Se1 105.26(5) . . ? 
Se2 In2 Se1 115.85(6) 9_556 . ? 
Se1 In2 Se1 109.34(9) 9_556 . ? 
B2 Se1 In2 91.2(5) . . ? 
B2 Se1 In1 94.6(5) . . ? 
In2 Se1 In1 116.21(7) . . ? 
B2 Se1 K1 111.6(5) . . ? 
In2 Se1 K1 89.39(17) . . ? 
In1 Se1 K1 143.31(13) . . ? 
B1 Se2 In2 90.9(5) . . ? 
B1 Se2 K1 114.5(5) . 4_565 ? 
In2 Se2 K1 147.92(9) . 4_565 ? 
B2 B1 B1 60.2(11) 12_566 12_566 ? 
B2 B1 B2 107.9(13) 12_566 . ? 
B1 B1 B2 59.5(11) 12_566 . ? 
B2 B1 B2 107.4(12) 12_566 3_565 ? 
B1 B1 B2 109.0(11) 12_566 3_565 ? 
B2 B1 B2 61.9(12) . 3_565 ? 
B2 B1 B1 59.6(10) 12_566 10_666 ? 
B1 B1 B1 107.7(10) 12_566 10_666 ? 
B2 B1 B1 108.1(11) . 10_666 ? 
B2 B1 B1 58.8(12) 3_565 10_666 ? 
B2 B1 Se2 116.7(10) 12_566 . ? 
B1 B1 Se2 123.6(6) 12_566 . ? 
B2 B1 Se2 127.9(11) . . ? 
B2 B1 Se2 122.8(12) 3_565 . ? 
B1 B1 Se2 116.8(6) 10_666 . ? 
B1 B2 B1 60.2(14) 12_566 . ? 
B1 B2 B1 61.6(13) 12_566 2_665 ? 
B1 B2 B1 109.3(14) . 2_665 ? 
B1 B2 B2 107.3(9) 12_566 3_565 ? 
B1 B2 B2 59.1(12) . 3_565 ? 
B1 B2 B2 107.5(10) 2_665 3_565 ? 
B1 B2 B2 108.0(8) 12_566 2_665 ? 
B1 B2 B2 107.6(10) . 2_665 ? 
B1 B2 B2 59.0(11) 2_665 2_665 ? 
B2 B2 B2 60.000(7) 3_565 2_665 ? 
B1 B2 Se1 125.1(11) 12_566 . ? 
B1 B2 Se1 122.6(11) . . ? 
B1 B2 Se1 122.2(11) 2_665 . ? 
B2 B2 Se1 119.3(8) 3_565 . ? 
B2 B2 Se1 119.1(7) 2_665 . ? 
I1B K1 I1B 40(2) 7_556 . ? 
I1B K1 I1A 20.7(12) 7_556 4_554 ? 
I1B K1 I1A 60.9(12) . 4_554 ? 
I1B K1 I1A 60.9(12) 7_556 . ? 
I1B K1 I1A 20.7(12) . . ? 
I1A K1 I1A 81.6(4) 4_554 . ? 
I1B K1 Se1 134.7(7) 7_556 . ? 
I1B K1 Se1 144.9(3) . . ? 
I1A K1 Se1 120.26(4) 4_554 . ? 
I1A K1 Se1 136.24(4) . . ? 
I1B K1 Se1 144.9(3) 7_556 9_556 ? 
I1B K1 Se1 134.7(7) . 9_556 ? 
I1A K1 Se1 136.24(4) 4_554 9_556 ? 
I1A K1 Se1 120.26(4) . 9_556 ? 
Se1 K1 Se1 71.9(3) . 9_556 ? 
I1B K1 Se2 144.2(11) 7_556 12_566 ? 
I1B K1 Se2 105.6(11) . 12_566 ? 
I1A K1 Se2 161.8(3) 4_554 12_566 ? 
I1A K1 Se2 85.47(7) . 12_566 ? 
Se1 K1 Se2 62.7(2) . 12_566 ? 
Se1 K1 Se2 61.8(2) 9_556 12_566 ? 
I1B K1 Se2 105.6(11) 7_556 4_564 ? 
I1B K1 Se2 144.2(11) . 4_564 ? 
I1A K1 Se2 85.47(7) 4_554 4_564 ? 
I1A K1 Se2 161.8(3) . 4_564 ? 
Se1 K1 Se2 61.8(2) . 4_564 ? 
Se1 K1 Se2 62.7(2) 9_556 4_564 ? 
Se2 K1 Se2 109.8(5) 12_566 4_564 ? 
I1B K1 K1 35.6(6) 7_556 2 ? 
I1B K1 K1 35.6(6) . 2 ? 
I1A K1 K1 49.02(14) 4_554 2 ? 
I1A K1 K1 49.02(14) . 2 ? 
Se1 K1 K1 169.26(11) . 2 ? 
Se1 K1 K1 114.83(16) 9_556 2 ? 
Se2 K1 K1 127.52(18) 12_566 2 ? 
Se2 K1 K1 112.76(19) 4_564 2 ? 
I1B K1 K1 35.6(6) 7_556 3 ? 
I1B K1 K1 35.6(6) . 3 ? 
I1A K1 K1 49.02(14) 4_554 3 ? 
I1A K1 K1 49.02(14) . 3 ? 
Se1 K1 K1 114.83(16) . 3 ? 
Se1 K1 K1 169.26(11) 9_556 3 ? 
Se2 K1 K1 112.76(19) 12_566 3 ? 
Se2 K1 K1 127.52(18) 4_564 3 ? 
K1 K1 K1 60.0 2 3 ? 
I1B I1A I1B 180.000(11) 10_556 . ? 
I1B I1A K1 49.22(19) 10_556 5 ? 
I1B I1A K1 130.78(19) . 5 ? 
I1B I1A K1 130.78(19) 10_556 2 ? 
I1B I1A K1 49.22(19) . 2 ? 
K1 I1A K1 180.000(1) 5 2 ? 
I1B I1A K1 130.78(18) 10_556 3 ? 
I1B I1A K1 49.22(18) . 3 ? 
K1 I1A K1 98.0(3) 5 3 ? 
K1 I1A K1 82.0(3) 2 3 ? 
I1B I1A K1 130.78(18) 10_556 . ? 
I1B I1A K1 49.22(18) . . ? 
K1 I1A K1 98.0(3) 5 . ? 
K1 I1A K1 82.0(3) 2 . ? 
K1 I1A K1 82.0(3) 3 . ? 
I1B I1A K1 49.22(18) 10_556 4 ? 
I1B I1A K1 130.78(18) . 4 ? 
K1 I1A K1 82.0(3) 5 4 ? 
K1 I1A K1 98.0(3) 2 4 ? 
K1 I1A K1 98.0(3) 3 4 ? 
K1 I1A K1 180.000(1) . 4 ? 
I1B I1A K1 49.22(18) 10_556 6 ? 
I1B I1A K1 130.78(18) . 6 ? 
K1 I1A K1 82.0(3) 5 6 ? 
K1 I1A K1 98.0(3) 2 6 ? 
K1 I1A K1 180.0(4) 3 6 ? 
K1 I1A K1 98.0(3) . 6 ? 
K1 I1A K1 82.0(3) 4 6 ? 
I1A I1B I1B 180.000(18) . 7_556 ? 
I1A I1B K1 110.1(12) . 2 ? 
I1B I1B K1 69.9(12) 7_556 2 ? 
I1A I1B K1 110.1(12) . 3 ? 
I1B I1B K1 69.9(12) 7_556 3 ? 
K1 I1B K1 108.8(12) 2 3 ? 
I1A I1B K1 110.1(12) . . ? 
I1B I1B K1 69.9(12) 7_556 . ? 
K1 I1B K1 108.8(12) 2 . ? 
K1 I1B K1 108.8(12) 3 . ? 
 
_diffrn_measured_fraction_theta_max    0.989 
_diffrn_reflns_theta_full              25.50 
_diffrn_measured_fraction_theta_full   0.989 
_refine_diff_density_max    3.891 
_refine_diff_density_min   -2.118 
_refine_diff_density_rms    0.331 
