data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Zhang S.-L.Pan X.Fan Z.Zhou K.Poeppelmeier _publ_contact_author_name 'Pan, Shi-Lie' _publ_contact_author_email slpan@ms.xjb.ac.cn data_1 _database_code_depnum_ccdc_archive 'CCDC 796881' #TrackingRef '- Xray crystallographic file.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B6 Br K3 O10' _chemical_formula_weight 422.07 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' 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 10.1153(8) _cell_length_b 10.1153(8) _cell_length_c 8.8592(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 785.02(15) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2314 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 24.93 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.678 _exptl_crystal_density_method ? _exptl_crystal_F_000 606 _exptl_absorpt_coefficient_mu 5.165 _exptl_absorpt_correction_type none _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1915 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 24.93 _reflns_number_total 332 _reflns_number_gt 330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto Version 3.0 (Rigaku 2004)' _computing_cell_refinement 'Rapid Auto Version 3.0 (Rigaku 2004)' _computing_data_reduction 'Rapid Auto Version 3.0 (Rigaku 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS, 2000)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS, 2000)' _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^)+(0.0146P)^2^+2.0967P] where P=(Fo^2^+2Fc^2^)/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 0.296(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.029(15) _refine_ls_number_reflns 332 _refine_ls_number_parameters 26 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.155 _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 0.84691(7) 0.15309(7) 0.20948(17) 0.0139(5) Uani 1 2 d S . . Br1 Br 0.6667 0.3333 0.32183(8) 0.0203(5) Uani 1 6 d S . . B1 B 0.7545(3) 0.2455(3) -0.1300(7) 0.0049(12) Uiso 1 2 d S . . B2 B 0.9656(7) 0.4828(3) -0.0132(8) 0.0074(15) Uiso 1 2 d S . . O1 O 0.8995(3) 0.3331(3) -0.0483(3) 0.0082(7) Uiso 1 1 d . . . O2 O 0.7782(2) 0.2218(2) -0.2835(5) 0.0082(9) Uiso 1 2 d S . . O3 O 0.6667 0.3333 -0.1232(8) 0.0017(14) Uiso 1 6 d S . . 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 K1 0.0121(6) 0.0121(6) 0.0131(8) 0.0018(3) -0.0018(3) 0.0026(6) Br1 0.0198(5) 0.0198(5) 0.0214(7) 0.000 0.000 0.0099(3) _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 O1 2.793(3) 9_665 ? K1 O1 2.793(3) 12_445 ? K1 O1 2.801(3) 4_665 ? K1 O1 2.801(3) . ? K1 O2 2.853(3) 14_645 ? K1 O2 2.853(3) 15_655 ? K1 Br1 3.3111(14) . ? K1 Br1 3.3207(15) 13_544 ? Br1 K1 3.3111(14) 3_665 ? Br1 K1 3.3111(14) 2_655 ? Br1 K1 3.3206(15) 9_665 ? Br1 K1 3.3206(15) 8_545 ? Br1 K1 3.3207(15) 7_455 ? B1 O2 1.422(8) . ? B1 O1 1.470(4) . ? B1 O1 1.470(4) 4_665 ? B1 O3 1.539(6) . ? B2 O1 1.351(4) 6 ? B2 O1 1.351(4) . ? B2 O2 1.385(7) 9_665 ? O1 K1 2.793(2) 14_644 ? O2 B2 1.385(7) 14_644 ? O2 K1 2.853(3) 8_544 ? O2 K1 2.853(3) 9_664 ? O3 B1 1.539(6) 2_655 ? O3 B1 1.539(6) 3_665 ? 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 O1 150.50(14) 9_665 12_445 ? O1 K1 O1 124.56(11) 9_665 4_665 ? O1 K1 O1 75.82(4) 12_445 4_665 ? O1 K1 O1 75.82(4) 9_665 . ? O1 K1 O1 124.56(11) 12_445 . ? O1 K1 O1 49.66(11) 4_665 . ? O1 K1 O2 49.34(9) 9_665 14_645 ? O1 K1 O2 119.73(11) 12_445 14_645 ? O1 K1 O2 157.98(10) 4_665 14_645 ? O1 K1 O2 115.38(10) . 14_645 ? O1 K1 O2 119.73(11) 9_665 15_655 ? O1 K1 O2 49.34(9) 12_445 15_655 ? O1 K1 O2 115.38(10) 4_665 15_655 ? O1 K1 O2 157.98(10) . 15_655 ? O2 K1 O2 72.79(15) 14_645 15_655 ? O1 K1 B2 144.34(13) 9_665 7_445 ? O1 K1 Br1 81.14(6) 9_665 . ? O1 K1 Br1 81.14(6) 12_445 . ? O1 K1 Br1 82.25(6) 4_665 . ? O1 K1 Br1 82.25(6) . . ? O2 K1 Br1 114.06(8) 14_645 . ? O2 K1 Br1 114.06(8) 15_655 . ? B2 K1 Br1 103.37(8) 7_445 . ? B2 K1 Br1 103.37(8) 9_665 . ? O1 K1 Br1 102.17(6) 9_665 13_544 ? O1 K1 Br1 102.17(6) 12_445 13_544 ? O1 K1 Br1 80.85(6) 4_665 13_544 ? O1 K1 Br1 80.85(6) . 13_544 ? O2 K1 Br1 80.52(7) 14_645 13_544 ? O2 K1 Br1 80.52(7) 15_655 13_544 ? B2 K1 Br1 84.76(9) 7_445 13_544 ? B2 K1 Br1 84.76(9) 9_665 13_544 ? Br1 K1 Br1 161.37(5) . 13_544 ? K1 Br1 K1 111.37(3) . 3_665 ? K1 Br1 K1 111.37(3) . 2_655 ? K1 Br1 K1 111.37(3) 3_665 2_655 ? K1 Br1 K1 77.999(9) . 9_665 ? K1 Br1 K1 161.37(5) 3_665 9_665 ? K1 Br1 K1 77.997(9) 2_655 9_665 ? K1 Br1 K1 77.998(9) . 8_545 ? K1 Br1 K1 77.997(9) 3_665 8_545 ? K1 Br1 K1 161.37(5) 2_655 8_545 ? K1 Br1 K1 88.77(4) 9_665 8_545 ? K1 Br1 K1 161.37(5) . 7_455 ? K1 Br1 K1 77.998(9) 3_665 7_455 ? K1 Br1 K1 77.998(9) 2_655 7_455 ? K1 Br1 K1 88.77(4) 9_665 7_455 ? K1 Br1 K1 88.77(4) 8_545 7_455 ? O2 B1 O1 111.7(3) . . ? O2 B1 O1 111.7(3) . 4_665 ? O1 B1 O1 106.3(4) . 4_665 ? O2 B1 O3 109.3(5) . . ? O1 B1 O3 108.9(3) . . ? O1 B1 O3 108.9(3) 4_665 . ? O1 B2 O1 121.8(5) 6 . ? O1 B2 O2 119.0(3) 6 9_665 ? O1 B2 O2 119.0(3) . 9_665 ? O1 B2 K1 62.6(2) 6 13_554 ? O1 B2 K1 146.1(4) . 13_554 ? O2 B2 K1 65.08(19) 9_665 13_554 ? O1 B2 K1 146.1(4) 6 14_644 ? O1 B2 K1 62.6(2) . 14_644 ? O2 B2 K1 65.09(19) 9_665 14_644 ? K1 B2 K1 95.21(17) 13_554 14_644 ? O1 B2 K1 47.6(2) 6 2_655 ? O1 B2 K1 132.8(4) . 2_655 ? O2 B2 K1 92.5(2) 9_665 2_655 ? K1 B2 K1 77.17(3) 13_554 2_655 ? K1 B2 K1 157.3(2) 14_644 2_655 ? B2 O1 B1 125.0(3) . . ? B2 O1 K1 92.0(3) . 14_644 ? B1 O1 K1 126.9(3) . 14_644 ? B2 O1 K1 111.6(3) . . ? B1 O1 K1 101.7(2) . . ? K1 O1 K1 96.50(8) 14_644 . ? B2 O2 B1 130.8(5) 14_644 . ? B2 O2 K1 88.8(2) 14_644 8_544 ? B1 O2 K1 116.92(14) . 8_544 ? B2 O2 K1 88.8(2) 14_644 9_664 ? B1 O2 K1 116.92(14) . 9_664 ? K1 O2 K1 109.00(15) 8_544 9_664 ? B1 O3 B1 119.85(5) . 2_655 ? B1 O3 B1 119.85(5) . 3_665 ? B1 O3 B1 119.85(5) 2_655 3_665 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.93 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.535 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.117