# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

 
data_zhn20150918_3_0m 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B6 Br0.67 Cl0.33 K3 O10' 
_chemical_formula_weight          407.25 
 
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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Trigonal 
_symmetry_space_group_name_H-M    R3m 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-y, -x, z' 
 '-x+y, y, z' 
 'x, x-y, z' 
 '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' 
 '-y+2/3, -x+1/3, z+1/3' 
 '-x+y+2/3, y+1/3, z+1/3' 
 'x+2/3, x-y+1/3, z+1/3' 
 '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' 
 '-y+1/3, -x+2/3, z+2/3' 
 '-x+y+1/3, y+2/3, z+2/3' 
 'x+1/3, x-y+2/3, z+2/3' 
 
_cell_length_a                    10.0990(4) 
_cell_length_b                    10.0990(4) 
_cell_length_c                    8.8580(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      782.39(6) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     1823 
_cell_measurement_theta_min       3.27 
_cell_measurement_theta_max       28.22 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.593 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              588 
_exptl_absorpt_coefficient_mu     3.991 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       296(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   Bruker 
_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             2092 
_diffrn_reflns_av_R_equivalents   0.0313 
_diffrn_reflns_av_sigmaI/netI     0.0407 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.27 
_diffrn_reflns_theta_max          28.28 
_reflns_number_total              491 
_reflns_number_gt                 481 
_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)+(0.0191P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.334(11) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.014(13) 
_refine_ls_number_reflns          491 
_refine_ls_number_parameters      42 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0202 
_refine_ls_R_factor_gt            0.0200 
_refine_ls_wR_factor_ref          0.0484 
_refine_ls_wR_factor_gt           0.0483 
_refine_ls_goodness_of_fit_ref    1.126 
_refine_ls_restrained_S_all       1.125 
_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 
Br1 Br 0.0000 0.0000 0.99481(8) 0.0222(3) Uani 0.651(5) 6 d SP . . 
Cl1 Cl 0.0000 0.0000 0.99481(8) 0.0222(3) Uani 0.349(5) 6 d SP . . 
K1 K 0.17982(4) 0.35964(8) 0.88081(7) 0.0170(3) Uani 1 2 d S . . 
O1 O 0.0000 0.0000 0.5491(5) 0.0051(8) Uani 1 6 d S . . 
O2 O 0.44468(11) 0.55532(11) 1.0538(2) 0.0104(5) Uani 1 2 d S . . 
O3 O 0.23332(17) 0.23384(16) 0.62221(18) 0.0103(4) Uani 1 1 d . . . 
B1 B 0.08719(18) 0.1744(4) 0.5429(3) 0.0061(6) Uani 1 2 d S . . 
B2 B 0.3000(4) 0.15002(18) 0.6581(4) 0.0080(7) Uani 1 2 d S . . 
 
 
_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 
Br1 K1 3.3035(8) 2 ? 
Br1 K1 3.3035(8) . ? 
Br1 K1 3.3035(8) 3 ? 
Br1 K1 3.3144(9) 8 ? 
Br1 K1 3.3144(9) 7_445 ? 
Br1 K1 3.3144(9) 9_455 ? 
K1 O3 2.7807(15) 8 ? 
K1 O3 2.7808(15) 12_455 ? 
K1 O3 2.8000(16) 5 ? 
K1 O3 2.8000(16) . ? 
K1 O2 2.8500(13) . ? 
K1 O2 2.8500(13) 3_565 ? 
K1 B2 3.137(2) 8 ? 
K1 B2 3.137(2) 7_455 ? 
K1 Br1 3.3144(9) 13_554 ? 
K1 Cl1 3.3144(9) 13_554 ? 
O1 B1 1.526(3) 2 ? 
O1 B1 1.526(3) . ? 
O1 B1 1.526(3) 3 ? 
O2 B2 1.375(4) 8 ? 
O2 B1 1.443(4) 15 ? 
O2 K1 2.8500(13) 2_665 ? 
O3 B2 1.357(2) . ? 
O3 B1 1.465(2) . ? 
O3 K1 2.7807(15) 15_554 ? 
B1 O2 1.443(4) 8_554 ? 
B1 O3 1.465(2) 5 ? 
B2 O3 1.357(2) 6 ? 
B2 O2 1.375(4) 15_554 ? 
B2 K1 3.137(2) 15_554 ? 
B2 K1 3.137(2) 13_544 ? 
B2 K1 3.524(2) 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 
K1 Br1 K1 111.091(16) 2 . ? 
K1 Br1 K1 111.091(16) 2 3 ? 
K1 Br1 K1 111.091(16) . 3 ? 
K1 Br1 K1 161.91(3) 2 8 ? 
K1 Br1 K1 78.081(5) . 8 ? 
K1 Br1 K1 78.083(5) 3 8 ? 
K1 Br1 K1 78.081(5) 2 7_445 ? 
K1 Br1 K1 161.91(3) . 7_445 ? 
K1 Br1 K1 78.082(5) 3 7_445 ? 
K1 Br1 K1 89.12(2) 8 7_445 ? 
K1 Br1 K1 78.082(5) 2 9_455 ? 
K1 Br1 K1 78.082(5) . 9_455 ? 
K1 Br1 K1 161.91(3) 3 9_455 ? 
K1 Br1 K1 89.11(2) 8 9_455 ? 
K1 Br1 K1 89.11(2) 7_445 9_455 ? 
O3 K1 O3 150.74(7) 8 12_455 ? 
O3 K1 O3 124.60(6) 8 5 ? 
O3 K1 O3 75.84(2) 12_455 5 ? 
O3 K1 O3 75.84(2) 8 . ? 
O3 K1 O3 124.60(6) 12_455 . ? 
O3 K1 O3 49.65(6) 5 . ? 
O3 K1 O2 49.46(5) 8 . ? 
O3 K1 O2 119.69(6) 12_455 . ? 
O3 K1 O2 157.57(5) 5 . ? 
O3 K1 O2 115.30(5) . . ? 
O3 K1 O2 119.69(6) 8 3_565 ? 
O3 K1 O2 49.46(5) 12_455 3_565 ? 
O3 K1 O2 115.30(5) 5 3_565 ? 
O3 K1 O2 157.57(5) . 3_565 ? 
O2 K1 O2 72.58(8) . 3_565 ? 
O3 K1 B2 25.62(6) 8 8 ? 
O3 K1 B2 144.21(7) 12_455 8 ? 
O3 K1 B2 139.71(7) 5 8 ? 
O3 K1 B2 91.12(7) . 8 ? 
O2 K1 B2 25.98(7) . 8 ? 
O2 K1 B2 98.55(7) 3_565 8 ? 
O3 K1 B2 144.21(7) 8 7_455 ? 
O3 K1 B2 25.62(6) 12_455 7_455 ? 
O3 K1 B2 91.12(7) 5 7_455 ? 
O3 K1 B2 139.71(7) . 7_455 ? 
O2 K1 B2 98.55(7) . 7_455 ? 
O2 K1 B2 25.98(7) 3_565 7_455 ? 
B2 K1 B2 124.53(12) 8 7_455 ? 
O3 K1 Br1 81.19(4) 8 . ? 
O3 K1 Br1 81.19(4) 12_455 . ? 
O3 K1 Br1 82.87(4) 5 . ? 
O3 K1 Br1 82.87(4) . . ? 
O2 K1 Br1 114.04(4) . . ? 
O2 K1 Br1 114.04(4) 3_565 . ? 
B2 K1 Br1 103.47(4) 8 . ? 
B2 K1 Br1 103.47(4) 7_455 . ? 
O3 K1 Br1 102.00(4) 8 13_554 ? 
O3 K1 Br1 102.00(4) 12_455 13_554 ? 
O3 K1 Br1 80.72(4) 5 13_554 ? 
O3 K1 Br1 80.72(4) . 13_554 ? 
O2 K1 Br1 80.14(4) . 13_554 ? 
O2 K1 Br1 80.14(4) 3_565 13_554 ? 
B2 K1 Br1 84.48(5) 8 13_554 ? 
B2 K1 Br1 84.48(5) 7_455 13_554 ? 
Br1 K1 Br1 161.91(3) . 13_554 ? 
O3 K1 Cl1 102.00(4) 8 13_554 ? 
O3 K1 Cl1 102.00(4) 12_455 13_554 ? 
O3 K1 Cl1 80.72(4) 5 13_554 ? 
O3 K1 Cl1 80.72(4) . 13_554 ? 
O2 K1 Cl1 80.14(4) . 13_554 ? 
O2 K1 Cl1 80.14(4) 3_565 13_554 ? 
B2 K1 Cl1 84.48(5) 8 13_554 ? 
B2 K1 Cl1 84.48(5) 7_455 13_554 ? 
Br1 K1 Cl1 161.91(3) . 13_554 ? 
Br1 K1 Cl1 0.00(2) 13_554 13_554 ? 
B1 O1 B1 119.87(3) 2 . ? 
B1 O1 B1 119.87(3) 2 3 ? 
B1 O1 B1 119.87(3) . 3 ? 
B2 O2 B1 130.7(3) 8 15 ? 
B2 O2 K1 88.76(11) 8 . ? 
B1 O2 K1 116.87(8) 15 . ? 
B2 O2 K1 88.76(11) 8 2_665 ? 
B1 O2 K1 116.87(8) 15 2_665 ? 
K1 O2 K1 109.36(7) . 2_665 ? 
B2 O3 B1 124.7(2) . . ? 
B2 O3 K1 92.03(15) . 15_554 ? 
B1 O3 K1 127.96(15) . 15_554 ? 
B2 O3 K1 111.09(18) . . ? 
B1 O3 K1 101.25(13) . . ? 
K1 O3 K1 96.65(5) 15_554 . ? 
O2 B1 O3 110.77(16) 8_554 5 ? 
O2 B1 O3 110.77(16) 8_554 . ? 
O3 B1 O3 106.7(2) 5 . ? 
O2 B1 O1 109.1(3) 8_554 . ? 
O3 B1 O1 109.72(17) 5 . ? 
O3 B1 O1 109.72(17) . . ? 
O2 B1 K1 134.54(19) 8_554 . ? 
O3 B1 K1 53.78(12) 5 . ? 
O3 B1 K1 53.78(12) . . ? 
O1 B1 K1 116.4(2) . . ? 
O3 B2 O3 121.4(3) 6 . ? 
O3 B2 O2 119.20(14) 6 15_554 ? 
O3 B2 O2 119.21(14) . 15_554 ? 
O3 B2 K1 145.9(2) 6 15_554 ? 
O3 B2 K1 62.35(11) . 15_554 ? 
O2 B2 K1 65.26(10) 15_554 15_554 ? 
O3 B2 K1 62.35(11) 6 13_544 ? 
O3 B2 K1 145.9(2) . 13_544 ? 
O2 B2 K1 65.26(10) 15_554 13_544 ? 
K1 B2 K1 95.67(9) 15_554 13_544 ? 
O3 B2 K1 132.60(19) 6 . ? 
O3 B2 K1 47.85(13) . . ? 
O2 B2 K1 92.77(13) 15_554 . ? 
K1 B2 K1 77.242(18) 15_554 . ? 
K1 B2 K1 157.70(11) 13_544 . ? 
O3 B2 K1 47.85(13) 6 3 ? 
O3 B2 K1 132.60(19) . 3 ? 
O2 B2 K1 92.77(13) 15_554 3 ? 
K1 B2 K1 157.70(11) 15_554 3 ? 
K1 B2 K1 77.241(18) 13_544 3 ? 
K1 B2 K1 101.26(8) . 3 ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              28.28 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.595 
_refine_diff_density_min   -0.233 
_refine_diff_density_rms    0.079 
