 
data_ss 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Cl6 K3 Mn Na' 
_chemical_formula_weight          407.93 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Mn'  'Mn'   0.3368   0.7283 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Na'  'Na'   0.0362   0.0249 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    R-3c  
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x+y, y, z+1/2' 
 'x, x-y, z+1/2' 
 '-y, -x, z+1/2' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 '-x+y+2/3, y+1/3, z+5/6' 
 'x+2/3, x-y+1/3, z+5/6' 
 '-y+2/3, -x+1/3, z+5/6' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-x+y+1/3, y+2/3, z+7/6' 
 'x+1/3, x-y+2/3, z+7/6' 
 '-y+1/3, -x+2/3, z+7/6' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 'x-y, -y, -z-1/2' 
 '-x, -x+y, -z-1/2' 
 'y, x, -z-1/2' 
 '-x+2/3, -y+1/3, -z+1/3' 
 'y+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, x+1/3, -z+1/3' 
 'x-y+2/3, -y+1/3, -z-1/6' 
 '-x+2/3, -x+y+1/3, -z-1/6' 
 'y+2/3, x+1/3, -z-1/6' 
 '-x+1/3, -y+2/3, -z+2/3' 
 'y+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, x+2/3, -z+2/3' 
 'x-y+1/3, -y+2/3, -z+1/6' 
 '-x+1/3, -x+y+2/3, -z+1/6' 
 'y+1/3, x+2/3, -z+1/6' 
 
_cell_length_a                    12.0966(5) 
_cell_length_b                    12.0966(5) 
_cell_length_c                    13.9555(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1768.48(16) 
_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           0.23 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.298 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1170 
_exptl_absorpt_coefficient_mu     3.513 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4988 
_exptl_absorpt_correction_T_max   0.6208 
_exptl_absorpt_process_details    Higashi2001 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71075 
_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             7087 
_diffrn_reflns_av_R_equivalents   0.0197 
_diffrn_reflns_av_sigmaI/netI     0.0085 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          4.87 
_diffrn_reflns_theta_max          30.48 
_reflns_number_total              585 
_reflns_number_gt                 558 
_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 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^)+(0.0110P)^2^+0.7260P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          585 
_refine_ls_number_parameters      19 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0117 
_refine_ls_R_factor_gt            0.0108 
_refine_ls_wR_factor_ref          0.0247 
_refine_ls_wR_factor_gt           0.0245 
_refine_ls_goodness_of_fit_ref    1.114 
_refine_ls_restrained_S_all       1.114 
_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 
K K 0.29052(2) 0.3333 0.0833 0.02685(7) Uani 1 2 d S . . 
Na Na 0.0000 0.0000 0.2500 0.02882(17) Uani 1 6 d S . . 
Mn Mn 0.0000 0.0000 0.0000 0.01644(6) Uani 1 6 d S . . 
Cl Cl 0.181550(17) 0.027130(18) 0.108876(12) 0.02324(6) Uani 1 1 d . . . 
 
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 
K 0.02627(9) 0.02558(12) 0.02846(12) -0.00548(8) -0.00274(4) 0.01279(6) 
Na 0.0344(3) 0.0344(3) 0.0178(3) 0.000 0.000 0.01718(13) 
Mn 0.01713(8) 0.01713(8) 0.01504(11) 0.000 0.000 0.00857(4) 
Cl 0.02080(9) 0.02933(10) 0.02162(9) -0.00062(6) -0.00331(6) 0.01406(7) 
 
_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 
K Cl 3.2022(2) 18_554 ? 
K Cl 3.2022(2) 21 ? 
K Cl 3.2093(3) 10_554 ? 
K Cl 3.2093(3) 25 ? 
K Cl 3.2713(2) 34 ? 
K Cl 3.2714(2) . ? 
K Cl 3.3555(3) 35 ? 
K Cl 3.3556(3) 2 ? 
Na Cl 2.8440(2) 3 ? 
Na Cl 2.8440(2) 24_556 ? 
Na Cl 2.8440(2) 22_556 ? 
Na Cl 2.8440(2) 23_556 ? 
Na Cl 2.8440(2) 2 ? 
Na Cl 2.8441(2) . ? 
Mn Cl 2.55315(19) . ? 
Mn Cl 2.55317(19) 19 ? 
Mn Cl 2.55317(19) 20 ? 
Mn Cl 2.55317(19) 2 ? 
Mn Cl 2.55317(19) 21 ? 
Mn Cl 2.55317(19) 3 ? 
Cl K 3.2022(2) 20 ? 
Cl K 3.2093(3) 25 ? 
Cl K 3.3556(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 
Cl K Cl 153.706(11) 18_554 21 ? 
Cl K Cl 130.430(6) 18_554 10_554 ? 
Cl K Cl 73.046(6) 21 10_554 ? 
Cl K Cl 73.044(6) 18_554 25 ? 
Cl K Cl 130.432(6) 21 25 ? 
Cl K Cl 76.635(9) 10_554 25 ? 
Cl K Cl 68.992(6) 18_554 34 ? 
Cl K Cl 115.641(6) 21 34 ? 
Cl K Cl 73.635(6) 10_554 34 ? 
Cl K Cl 91.471(6) 25 34 ? 
Cl K Cl 115.642(6) 18_554 . ? 
Cl K Cl 68.991(6) 21 . ? 
Cl K Cl 91.472(6) 10_554 . ? 
Cl K Cl 73.637(6) 25 . ? 
Cl K Cl 161.217(10) 34 . ? 
Cl K Cl 67.947(7) 18_554 35 ? 
Cl K Cl 90.071(7) 21 35 ? 
Cl K Cl 122.056(3) 10_554 35 ? 
Cl K Cl 139.472(5) 25 35 ? 
Cl K Cl 64.847(6) 34 35 ? 
Cl K Cl 133.909(7) . 35 ? 
Cl K Cl 90.072(7) 18_554 2 ? 
Cl K Cl 67.946(7) 21 2 ? 
Cl K Cl 139.472(5) 10_554 2 ? 
Cl K Cl 122.057(3) 25 2 ? 
Cl K Cl 133.910(7) 34 2 ? 
Cl K Cl 64.846(6) . 2 ? 
Cl K Cl 69.302(8) 35 2 ? 
Cl K Mn 39.892(3) 18_554 16_554 ? 
Cl K Mn 126.565(6) 21 16_554 ? 
Cl K Mn 113.426(4) 10_554 16_554 ? 
Cl K Mn 101.188(4) 25 16_554 ? 
Cl K Mn 39.803(3) 34 16_554 ? 
Cl K Mn 153.038(5) . 16_554 ? 
Cl K Mn 39.656(3) 35 16_554 ? 
Cl K Mn 98.604(6) 2 16_554 ? 
Cl K Mn 126.566(6) 18_554 . ? 
Cl K Mn 39.892(3) 21 . ? 
Cl K Mn 101.189(4) 10_554 . ? 
Cl K Mn 113.428(4) 25 . ? 
Cl K Mn 153.036(5) 34 . ? 
Cl K Mn 39.802(3) . . ? 
Cl K Mn 98.603(6) 35 . ? 
Cl K Mn 39.655(3) 2 . ? 
Mn K Mn 135.701(7) 16_554 . ? 
Cl K Na 88.375(5) 18_554 13_554 ? 
Cl K Na 82.841(6) 21 13_554 ? 
Cl K Na 82.764(5) 10_554 13_554 ? 
Cl K Na 130.816(5) 25 13_554 ? 
Cl K Na 39.594(3) 34 13_554 ? 
Cl K Na 151.682(4) . 13_554 ? 
Cl K Na 39.654(3) 35 13_554 ? 
Cl K Na 102.511(6) 2 13_554 ? 
Mn K Na 48.489(4) 16_554 13_554 ? 
Mn K Na 114.154(4) . 13_554 ? 
Cl K Na 82.842(5) 18_554 . ? 
Cl K Na 88.374(5) 21 . ? 
Cl K Na 130.817(5) 10_554 . ? 
Cl K Na 82.765(4) 25 . ? 
Cl K Na 151.684(4) 34 . ? 
Cl K Na 39.594(3) . . ? 
Cl K Na 102.511(6) 35 . ? 
Cl K Na 39.654(3) 2 . ? 
Mn K Na 114.154(4) 16_554 . ? 
Mn K Na 48.488(3) . . ? 
Na K Na 140.698(6) 13_554 . ? 
Cl Na Cl 148.588(8) 3 24_556 ? 
Cl Na Cl 127.308(8) 3 22_556 ? 
Cl Na Cl 77.333(7) 24_556 22_556 ? 
Cl Na Cl 88.797(8) 3 23_556 ? 
Cl Na Cl 77.333(6) 24_556 23_556 ? 
Cl Na Cl 77.333(6) 22_556 23_556 ? 
Cl Na Cl 77.333(6) 3 2 ? 
Cl Na Cl 88.797(8) 24_556 2 ? 
Cl Na Cl 148.588(8) 22_556 2 ? 
Cl Na Cl 127.308(8) 23_556 2 ? 
Cl Na Cl 77.333(6) 3 . ? 
Cl Na Cl 127.309(8) 24_556 . ? 
Cl Na Cl 88.798(8) 22_556 . ? 
Cl Na Cl 148.588(8) 23_556 . ? 
Cl Na Cl 77.333(6) 2 . ? 
Cl Na Mn 46.174(4) 3 . ? 
Cl Na Mn 133.826(4) 24_556 . ? 
Cl Na Mn 133.826(4) 22_556 . ? 
Cl Na Mn 133.826(4) 23_556 . ? 
Cl Na Mn 46.174(4) 2 . ? 
Cl Na Mn 46.173(4) . . ? 
Cl Na Mn 133.826(4) 3 4 ? 
Cl Na Mn 46.174(4) 24_556 4 ? 
Cl Na Mn 46.174(4) 22_556 4 ? 
Cl Na Mn 46.174(4) 23_556 4 ? 
Cl Na Mn 133.826(4) 2 4 ? 
Cl Na Mn 133.827(4) . 4 ? 
Mn Na Mn 180.0 . 4 ? 
Cl Na K 85.895(5) 3 7_445 ? 
Cl Na K 104.693(6) 24_556 7_445 ? 
Cl Na K 47.146(4) 22_556 7_445 ? 
Cl Na K 48.844(5) 23_556 7_445 ? 
Cl Na K 163.057(4) 2 7_445 ? 
Cl Na K 101.513(6) . 7_445 ? 
Mn Na K 121.473(2) . 7_445 ? 
Mn Na K 58.527(2) 4 7_445 ? 
Cl Na K 104.695(6) 3 . ? 
Cl Na K 85.894(5) 24_556 . ? 
Cl Na K 101.512(5) 22_556 . ? 
Cl Na K 163.056(4) 23_556 . ? 
Cl Na K 48.845(5) 2 . ? 
Cl Na K 47.147(4) . . ? 
Mn Na K 58.529(2) . . ? 
Mn Na K 121.471(2) 4 . ? 
K Na K 140.698(6) 7_445 . ? 
Cl Na K 48.845(5) 3 2 ? 
Cl Na K 101.511(5) 24_556 2 ? 
Cl Na K 163.056(4) 22_556 2 ? 
Cl Na K 85.894(5) 23_556 2 ? 
Cl Na K 47.147(5) 2 2 ? 
Cl Na K 104.695(6) . 2 ? 
Mn Na K 58.529(2) . 2 ? 
Mn Na K 121.471(2) 4 2 ? 
K Na K 118.586(5) 7_445 2 ? 
K Na K 95.231(3) . 2 ? 
Cl Na K 47.147(4) 3 3 ? 
Cl Na K 163.056(4) 24_556 3 ? 
Cl Na K 85.894(5) 22_556 3 ? 
Cl Na K 101.511(6) 23_556 3 ? 
Cl Na K 104.695(6) 2 3 ? 
Cl Na K 48.845(5) . 3 ? 
Mn Na K 58.529(2) . 3 ? 
Mn Na K 121.471(2) 4 3 ? 
K Na K 64.240(5) 7_445 3 ? 
K Na K 95.231(3) . 3 ? 
K Na K 95.231(3) 2 3 ? 
Cl Mn Cl 180.0 . 19 ? 
Cl Mn Cl 91.791(6) . 20 ? 
Cl Mn Cl 88.209(7) 19 20 ? 
Cl Mn Cl 88.209(6) . 2 ? 
Cl Mn Cl 91.791(7) 19 2 ? 
Cl Mn Cl 180.000(9) 20 2 ? 
Cl Mn Cl 91.791(6) . 21 ? 
Cl Mn Cl 88.209(6) 19 21 ? 
Cl Mn Cl 88.209(6) 20 21 ? 
Cl Mn Cl 91.791(6) 2 21 ? 
Cl Mn Cl 88.209(6) . 3 ? 
Cl Mn Cl 91.791(6) 19 3 ? 
Cl Mn Cl 91.791(6) 20 3 ? 
Cl Mn Cl 88.209(6) 2 3 ? 
Cl Mn Cl 180.000(10) 21 3 ? 
Cl Mn Na 53.479(4) . . ? 
Cl Mn Na 126.522(4) 19 . ? 
Cl Mn Na 126.522(4) 20 . ? 
Cl Mn Na 53.478(4) 2 . ? 
Cl Mn Na 126.522(4) 21 . ? 
Cl Mn Na 53.478(4) 3 . ? 
Cl Mn Na 126.521(4) . 19 ? 
Cl Mn Na 53.478(4) 19 19 ? 
Cl Mn Na 53.478(4) 20 19 ? 
Cl Mn Na 126.522(4) 2 19 ? 
Cl Mn Na 53.478(4) 21 19 ? 
Cl Mn Na 126.522(4) 3 19 ? 
Na Mn Na 180.0 . 19 ? 
Cl Mn K 55.106(5) . . ? 
Cl Mn K 124.894(5) 19 . ? 
Cl Mn K 122.995(5) 20 . ? 
Cl Mn K 57.005(5) 2 . ? 
Cl Mn K 53.550(5) 21 . ? 
Cl Mn K 126.450(5) 3 . ? 
Na Mn K 72.983(1) . . ? 
Na Mn K 107.017(1) 19 . ? 
Cl Mn K 124.894(5) . 19 ? 
Cl Mn K 55.106(5) 19 19 ? 
Cl Mn K 57.005(5) 20 19 ? 
Cl Mn K 122.995(5) 2 19 ? 
Cl Mn K 126.449(5) 21 19 ? 
Cl Mn K 53.551(5) 3 19 ? 
Na Mn K 107.017(1) . 19 ? 
Na Mn K 72.983(1) 19 19 ? 
K Mn K 180.0 . 19 ? 
Cl Mn K 126.450(5) . 2 ? 
Cl Mn K 53.551(5) 19 2 ? 
Cl Mn K 124.894(5) 20 2 ? 
Cl Mn K 55.106(5) 2 2 ? 
Cl Mn K 122.995(5) 21 2 ? 
Cl Mn K 57.005(5) 3 2 ? 
Na Mn K 72.983(1) . 2 ? 
Na Mn K 107.017(2) 19 2 ? 
K Mn K 111.810(1) . 2 ? 
K Mn K 68.190(1) 19 2 ? 
Cl Mn K 53.550(5) . 20 ? 
Cl Mn K 126.449(5) 19 20 ? 
Cl Mn K 55.106(5) 20 20 ? 
Cl Mn K 124.894(5) 2 20 ? 
Cl Mn K 57.005(5) 21 20 ? 
Cl Mn K 122.995(5) 3 20 ? 
Na Mn K 107.017(2) . 20 ? 
Na Mn K 72.983(1) 19 20 ? 
K Mn K 68.190(1) . 20 ? 
K Mn K 111.810(1) 19 20 ? 
K Mn K 180.0 2 20 ? 
Mn Cl Na 80.347(6) . . ? 
Mn Cl K 86.559(7) . 20 ? 
Na Cl K 166.832(6) . 20 ? 
Mn Cl K 168.461(8) . 25 ? 
Na Cl K 97.282(7) . 25 ? 
K Cl K 95.277(6) 20 25 ? 
Mn Cl K 85.092(6) . . ? 
Na Cl K 93.260(6) . . ? 
K Cl K 86.971(5) 20 . ? 
K Cl K 106.363(6) 25 . ? 
Mn Cl K 83.340(5) . 3 ? 
Na Cl K 91.501(5) . 3 ? 
K Cl K 85.556(5) 20 3 ? 
K Cl K 85.443(5) 25 3 ? 
K Cl K 166.573(6) . 3 ? 
 
_diffrn_measured_fraction_theta_max    0.972 
_diffrn_reflns_theta_full              30.48 
_diffrn_measured_fraction_theta_full   0.972 
_refine_diff_density_max    0.193 
_refine_diff_density_min   -0.207 
_refine_diff_density_rms    0.040 
