# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wen-Dan Cheng' _publ_contact_author_address ; Fuzhou 350002 ; _publ_contact_author_email cwd@fjirsm.ac.cn loop_ _publ_author_name 'Song-Lin Yang' 'Wen-Dan Cheng' 'Hao Zhang' 'Wei-Long Zhang' ; Zhang-Zhen He ; # Attachment '- Dalton Trans-CIF.txt' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 776166' #TrackingRef '- Dalton Trans-CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'O7 Sb Zn4, K' _chemical_formula_sum 'K O7 Sb Zn4' _chemical_formula_weight 534.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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)mc 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 6.141(3) _cell_length_b 6.141(3) _cell_length_c 9.948(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 324.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 3.8309 _cell_measurement_theta_max 27.4449 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 5.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 19.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.381 _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_standards_number 1939 _diffrn_reflns_number 2327 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.45 _reflns_number_total 311 _reflns_number_gt 300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0181P)^2^+0.0000P] 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 0.0416(11) _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 0.04(4) _refine_ls_number_reflns 311 _refine_ls_number_parameters 32 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0537 _refine_ls_wR_factor_gt 0.0528 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 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 Sb1 Sb 0.3333 0.6667 0.30524(6) 0.00557(15) Uani 1 6 d S . . Zn2 Zn 0.0000 0.0000 0.24722(15) 0.0088(3) Uani 1 6 d S . . Zn3 Zn 0.34583(11) 0.17292(6) 0.49287(10) 0.00752(17) Uani 1 2 d S . . K4 K 0.3333 0.6667 0.6774(3) 0.0133(6) Uani 1 6 d S . . O1 O 0.0000 0.0000 0.4436(7) 0.0069(7) Uani 1 6 d SU . . O2 O 0.1781(4) 0.3563(8) 0.1886(5) 0.0057(7) Uani 1 2 d SU . . O3 O 0.4893(4) 0.9786(8) 0.4206(5) 0.0070(7) Uani 1 2 d SU . . 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 Sb1 0.00625(19) 0.00625(19) 0.0042(3) 0.000 0.000 0.00312(9) Zn2 0.0093(3) 0.0093(3) 0.0078(6) 0.000 0.000 0.00466(17) Zn3 0.0079(4) 0.0083(3) 0.0062(3) -0.0002(2) -0.0004(4) 0.00397(18) K4 0.0133(7) 0.0133(7) 0.0132(14) 0.000 0.000 0.0067(4) O1 0.0069(7) 0.0069(7) 0.0068(11) 0.000 0.000 0.0034(4) O2 0.0066(9) 0.0052(8) 0.0048(10) -0.0004(7) -0.0002(3) 0.0026(4) O3 0.0070(9) 0.0065(8) 0.0071(10) -0.0004(7) -0.0002(3) 0.0033(4) _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 Sb1 O3 2.017(5) . Yes Sb1 O3 2.017(5) 2_665 Yes Sb1 O3 2.017(5) 3_565 Yes Sb1 O2 2.018(4) 3_565 Yes Sb1 O2 2.018(4) . Yes Sb1 O2 2.018(4) 2_665 Yes Sb1 K4 3.702(4) . Yes Sb1 K4 3.7669(18) 4_564 Yes Sb1 K4 3.7669(18) 4_674 Yes Sb1 K4 3.7669(18) 4_664 Yes Zn2 O1 1.954(8) . Yes Zn2 O2 1.982(4) 2 Yes Zn2 O2 1.982(4) 3 Yes Zn2 O2 1.982(4) . Yes Zn2 Zn3 3.059(2) . Yes Zn2 Zn3 3.059(2) 2 Yes Zn2 Zn3 3.059(2) 3 Yes Zn2 Zn3 3.128(2) 4_554 Yes Zn2 Zn3 3.128(2) 5_554 Yes Zn2 Zn3 3.128(2) 6_554 Yes Zn2 K4 3.6131(16) 4_564 Yes Zn2 K4 3.6131(16) 4_554 Yes Zn3 O1 1.903(2) . Yes Zn3 O3 1.942(3) 1_545 Yes Zn3 O3 1.942(3) 3_565 Yes Zn3 O2 1.948(5) 5 Yes Zn3 Zn3 2.9556(17) 3_665 Yes Zn3 Zn3 2.9556(17) 2_655 Yes Zn3 Zn2 3.128(2) 4 Yes Zn3 K4 3.572(3) 4_664 Yes Zn3 K4 3.578(2) 1_545 Yes Zn3 K4 3.578(2) . Yes K4 O3 3.046(5) 2_665 Yes K4 O3 3.046(5) . Yes K4 O3 3.046(5) 3_565 Yes K4 O3 3.068(5) 4_675 Yes K4 O3 3.068(5) 5_455 Yes K4 O3 3.068(5) 6_655 Yes K4 O2 3.0751(14) 5_565 Yes K4 O2 3.0751(14) 4_565 Yes K4 O2 3.0751(14) 6 Yes K4 O2 3.0751(14) 6_665 Yes K4 O2 3.0751(14) 5 Yes K4 O2 3.0751(14) 4_665 Yes O1 Zn3 1.903(2) 3 Yes O1 Zn3 1.903(2) 2 Yes O2 Zn3 1.948(5) 6_554 Yes O2 K4 3.0751(14) 4_564 Yes O2 K4 3.0751(14) 4_664 Yes O3 Zn3 1.942(3) 1_565 Yes O3 Zn3 1.942(3) 2_665 Yes O3 K4 3.068(5) 4_674 Yes 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 O3 Sb1 O3 90.85(18) . 2_665 Yes O3 Sb1 O3 90.85(18) . 3_565 Yes O3 Sb1 O3 90.85(18) 2_665 3_565 Yes O3 Sb1 O2 89.46(14) . 3_565 Yes O3 Sb1 O2 89.46(14) 2_665 3_565 Yes O3 Sb1 O2 179.57(19) 3_565 3_565 Yes O3 Sb1 O2 179.57(19) . . Yes O3 Sb1 O2 89.46(14) 2_665 . Yes O3 Sb1 O2 89.46(14) 3_565 . Yes O2 Sb1 O2 90.2(2) 3_565 . Yes O3 Sb1 O2 89.46(14) . 2_665 Yes O3 Sb1 O2 179.57(19) 2_665 2_665 Yes O3 Sb1 O2 89.46(14) 3_565 2_665 Yes O2 Sb1 O2 90.2(2) 3_565 2_665 Yes O2 Sb1 O2 90.2(2) . 2_665 Yes O3 Sb1 K4 55.34(13) . . Yes O3 Sb1 K4 55.34(13) 2_665 . Yes O3 Sb1 K4 55.34(13) 3_565 . Yes O2 Sb1 K4 125.10(14) 3_565 . Yes O2 Sb1 K4 125.10(14) . . Yes O2 Sb1 K4 125.10(14) 2_665 . Yes O3 Sb1 K4 125.39(2) . 4_564 Yes O3 Sb1 K4 54.40(13) 2_665 4_564 Yes O3 Sb1 K4 125.39(2) 3_565 4_564 Yes O2 Sb1 K4 54.61(2) 3_565 4_564 Yes O2 Sb1 K4 54.61(2) . 4_564 Yes O2 Sb1 K4 125.17(15) 2_665 4_564 Yes K4 Sb1 K4 109.73(4) . 4_564 Yes O3 Sb1 K4 54.40(13) . 4_674 Yes O3 Sb1 K4 125.39(2) 2_665 4_674 Yes O3 Sb1 K4 125.39(2) 3_565 4_674 Yes O2 Sb1 K4 54.61(2) 3_565 4_674 Yes O2 Sb1 K4 125.17(15) . 4_674 Yes O2 Sb1 K4 54.61(2) 2_665 4_674 Yes K4 Sb1 K4 109.73(4) . 4_674 Yes K4 Sb1 K4 109.21(4) 4_564 4_674 Yes O3 Sb1 K4 125.39(2) . 4_664 Yes O3 Sb1 K4 125.39(2) 2_665 4_664 Yes O3 Sb1 K4 54.40(13) 3_565 4_664 Yes O2 Sb1 K4 125.17(15) 3_565 4_664 Yes O2 Sb1 K4 54.61(2) . 4_664 Yes O2 Sb1 K4 54.61(2) 2_665 4_664 Yes K4 Sb1 K4 109.73(4) . 4_664 Yes K4 Sb1 K4 109.21(4) 4_564 4_664 Yes K4 Sb1 K4 109.21(4) 4_674 4_664 Yes O1 Zn2 O2 107.10(15) . 2 Yes O1 Zn2 O2 107.10(15) . 3 Yes O2 Zn2 O2 111.73(14) 2 3 Yes O1 Zn2 O2 107.10(15) . . Yes O2 Zn2 O2 111.73(14) 2 . Yes O2 Zn2 O2 111.73(14) 3 . Yes O1 Zn2 Zn3 36.97(3) . . Yes O2 Zn2 Zn3 144.07(16) 2 . Yes O2 Zn2 Zn3 86.99(13) 3 . Yes O2 Zn2 Zn3 86.99(13) . . Yes O1 Zn2 Zn3 36.97(3) . 2 Yes O2 Zn2 Zn3 86.99(13) 2 2 Yes O2 Zn2 Zn3 144.07(16) 3 2 Yes O2 Zn2 Zn3 86.99(13) . 2 Yes Zn3 Zn2 Zn3 62.77(5) . 2 Yes O1 Zn2 Zn3 36.97(3) . 3 Yes O2 Zn2 Zn3 86.99(13) 2 3 Yes O2 Zn2 Zn3 86.99(13) 3 3 Yes O2 Zn2 Zn3 144.07(16) . 3 Yes Zn3 Zn2 Zn3 62.77(5) . 3 Yes Zn3 Zn2 Zn3 62.77(5) 2 3 Yes O1 Zn2 Zn3 143.98(3) . 4_554 Yes O2 Zn2 Zn3 36.88(15) 2 4_554 Yes O2 Zn2 Zn3 92.47(13) 3 4_554 Yes O2 Zn2 Zn3 92.47(13) . 4_554 Yes Zn3 Zn2 Zn3 179.05(4) . 4_554 Yes Zn3 Zn2 Zn3 118.00(4) 2 4_554 Yes Zn3 Zn2 Zn3 118.00(4) 3 4_554 Yes O1 Zn2 Zn3 143.98(3) . 5_554 Yes O2 Zn2 Zn3 92.47(13) 2 5_554 Yes O2 Zn2 Zn3 36.88(15) 3 5_554 Yes O2 Zn2 Zn3 92.47(13) . 5_554 Yes Zn3 Zn2 Zn3 118.00(4) . 5_554 Yes Zn3 Zn2 Zn3 179.05(4) 2 5_554 Yes Zn3 Zn2 Zn3 118.00(4) 3 5_554 Yes Zn3 Zn2 Zn3 61.23(5) 4_554 5_554 Yes O1 Zn2 Zn3 143.98(3) . 6_554 Yes O2 Zn2 Zn3 92.47(13) 2 6_554 Yes O2 Zn2 Zn3 92.47(13) 3 6_554 Yes O2 Zn2 Zn3 36.88(15) . 6_554 Yes Zn3 Zn2 Zn3 118.00(4) . 6_554 Yes Zn3 Zn2 Zn3 118.00(4) 2 6_554 Yes Zn3 Zn2 Zn3 179.05(4) 3 6_554 Yes Zn3 Zn2 Zn3 61.23(5) 4_554 6_554 Yes Zn3 Zn2 Zn3 61.23(5) 5_554 6_554 Yes O1 Zn2 K4 101.08(5) . 4_564 Yes O2 Zn2 K4 58.297(15) 2 4_564 Yes O2 Zn2 K4 151.81(17) 3 4_564 Yes O2 Zn2 K4 58.297(15) . 4_564 Yes Zn3 Zn2 K4 116.66(4) . 4_564 Yes Zn3 Zn2 K4 64.11(5) 2 4_564 Yes Zn3 Zn2 K4 116.66(4) 3 4_564 Yes Zn3 Zn2 K4 63.64(4) 4_554 4_564 Yes Zn3 Zn2 K4 114.93(7) 5_554 4_564 Yes Zn3 Zn2 K4 63.64(4) 6_554 4_564 Yes O1 Zn2 K4 101.08(5) . 4_554 Yes O2 Zn2 K4 58.297(15) 2 4_554 Yes O2 Zn2 K4 58.297(15) 3 4_554 Yes O2 Zn2 K4 151.81(17) . 4_554 Yes Zn3 Zn2 K4 116.66(4) . 4_554 Yes Zn3 Zn2 K4 116.66(4) 2 4_554 Yes Zn3 Zn2 K4 64.11(5) 3 4_554 Yes Zn3 Zn2 K4 63.64(4) 4_554 4_554 Yes Zn3 Zn2 K4 63.64(4) 5_554 4_554 Yes Zn3 Zn2 K4 114.93(7) 6_554 4_554 Yes K4 Zn2 K4 116.40(3) 4_564 4_554 Yes O1 Zn3 O3 106.53(15) . 1_545 Yes O1 Zn3 O3 106.53(15) . 3_565 Yes O3 Zn3 O3 114.6(3) 1_545 3_565 Yes O1 Zn3 O2 106.5(2) . 5 Yes O3 Zn3 O2 111.04(14) 1_545 5 Yes O3 Zn3 O2 111.04(14) 3_565 5 Yes O1 Zn3 Zn3 146.81(9) . 3_665 Yes O3 Zn3 Zn3 94.62(11) 1_545 3_665 Yes O3 Zn3 Zn3 40.43(10) 3_565 3_665 Yes O2 Zn3 Zn3 88.59(11) 5 3_665 Yes O1 Zn3 Zn3 146.81(9) . 2_655 Yes O3 Zn3 Zn3 40.43(10) 1_545 2_655 Yes O3 Zn3 Zn3 94.62(11) 3_565 2_655 Yes O2 Zn3 Zn3 88.59(11) 5 2_655 Yes Zn3 Zn3 Zn3 60.0 3_665 2_655 Yes O1 Zn3 Zn2 38.1(2) . . Yes O3 Zn3 Zn2 86.58(12) 1_545 . Yes O3 Zn3 Zn2 86.58(12) 3_565 . Yes O2 Zn3 Zn2 144.66(13) 5 . Yes Zn3 Zn3 Zn2 121.39(2) 3_665 . Yes Zn3 Zn3 Zn2 121.39(2) 2_655 . Yes O1 Zn3 Zn2 68.9(2) . 4 Yes O3 Zn3 Zn2 122.05(13) 1_545 4 Yes O3 Zn3 Zn2 122.05(13) 3_565 4 Yes O2 Zn3 Zn2 37.65(13) 5 4 Yes Zn3 Zn3 Zn2 120.61(2) 3_665 4 Yes Zn3 Zn3 Zn2 120.61(2) 2_655 4 Yes Zn2 Zn3 Zn2 107.01(5) . 4 Yes O1 Zn3 K4 103.6(2) . 4_664 Yes O3 Zn3 K4 59.12(13) 1_545 4_664 Yes O3 Zn3 K4 59.12(13) 3_565 4_664 Yes O2 Zn3 K4 149.83(13) 5 4_664 Yes Zn3 Zn3 K4 65.56(3) 3_665 4_664 Yes Zn3 Zn3 K4 65.56(3) 2_655 4_664 Yes Zn2 Zn3 K4 65.50(5) . 4_664 Yes Zn2 Zn3 K4 172.52(4) 4 4_664 Yes O1 Zn3 K4 96.55(11) . 1_545 Yes O3 Zn3 K4 58.34(14) 1_545 1_545 Yes O3 Zn3 K4 156.87(10) 3_565 1_545 Yes O2 Zn3 K4 59.19(5) 5 1_545 Yes Zn3 Zn3 K4 116.435(17) 3_665 1_545 Yes Zn3 Zn3 K4 65.606(15) 2_655 1_545 Yes Zn2 Zn3 K4 113.50(4) . 1_545 Yes Zn2 Zn3 K4 64.79(4) 4 1_545 Yes K4 Zn3 K4 117.36(4) 4_664 1_545 Yes O1 Zn3 K4 96.55(11) . . Yes O3 Zn3 K4 156.87(10) 1_545 . Yes O3 Zn3 K4 58.34(14) 3_565 . Yes O2 Zn3 K4 59.19(5) 5 . Yes Zn3 Zn3 K4 65.606(15) 3_665 . Yes Zn3 Zn3 K4 116.435(17) 2_655 . Yes Zn2 Zn3 K4 113.50(4) . . Yes Zn2 Zn3 K4 64.79(4) 4 . Yes K4 Zn3 K4 117.36(4) 4_664 . Yes K4 Zn3 K4 118.23(9) 1_545 . Yes O3 K4 O3 56.28(15) 2_665 . Yes O3 K4 O3 56.28(15) 2_665 3_565 Yes O3 K4 O3 56.28(15) . 3_565 Yes O3 K4 O3 145.97(3) 2_665 4_675 Yes O3 K4 O3 109.05(4) . 4_675 Yes O3 K4 O3 145.97(3) 3_565 4_675 Yes O3 K4 O3 109.05(4) 2_665 5_455 Yes O3 K4 O3 145.97(3) . 5_455 Yes O3 K4 O3 145.97(3) 3_565 5_455 Yes O3 K4 O3 64.37(15) 4_675 5_455 Yes O3 K4 O3 145.97(3) 2_665 6_655 Yes O3 K4 O3 145.97(3) . 6_655 Yes O3 K4 O3 109.05(4) 3_565 6_655 Yes O3 K4 O3 64.37(15) 4_675 6_655 Yes O3 K4 O3 64.37(15) 5_455 6_655 Yes O3 K4 O2 92.98(9) 2_665 5_565 Yes O3 K4 O2 63.17(12) . 5_565 Yes O3 K4 O2 119.38(13) 3_565 5_565 Yes O3 K4 O2 55.06(12) 4_675 5_565 Yes O3 K4 O2 89.76(9) 5_455 5_565 Yes O3 K4 O2 119.41(13) 6_655 5_565 Yes O3 K4 O2 63.17(12) 2_665 4_565 Yes O3 K4 O2 92.98(10) . 4_565 Yes O3 K4 O2 119.38(13) 3_565 4_565 Yes O3 K4 O2 89.76(9) 4_675 4_565 Yes O3 K4 O2 55.06(12) 5_455 4_565 Yes O3 K4 O2 119.41(13) 6_655 4_565 Yes O2 K4 O2 64.50(15) 5_565 4_565 Yes O3 K4 O2 63.17(12) 2_665 6 Yes O3 K4 O2 119.38(13) . 6 Yes O3 K4 O2 92.98(10) 3_565 6 Yes O3 K4 O2 119.41(13) 4_675 6 Yes O3 K4 O2 55.06(12) 5_455 6 Yes O3 K4 O2 89.76(9) 6_655 6 Yes O2 K4 O2 119.870(14) 5_565 6 Yes O2 K4 O2 55.41(15) 4_565 6 Yes O3 K4 O2 119.38(13) 2_665 6_665 Yes O3 K4 O2 63.17(12) . 6_665 Yes O3 K4 O2 92.98(10) 3_565 6_665 Yes O3 K4 O2 55.06(12) 4_675 6_665 Yes O3 K4 O2 119.41(13) 5_455 6_665 Yes O3 K4 O2 89.76(10) 6_655 6_665 Yes O2 K4 O2 55.41(15) 5_565 6_665 Yes O2 K4 O2 119.870(14) 4_565 6_665 Yes O2 K4 O2 173.84(18) 6 6_665 Yes O3 K4 O2 92.98(10) 2_665 5 Yes O3 K4 O2 119.38(13) . 5 Yes O3 K4 O2 63.17(12) 3_565 5 Yes O3 K4 O2 119.41(13) 4_675 5 Yes O3 K4 O2 89.76(9) 5_455 5 Yes O3 K4 O2 55.06(12) 6_655 5 Yes O2 K4 O2 173.84(18) 5_565 5 Yes O2 K4 O2 119.870(14) 4_565 5 Yes O2 K4 O2 64.50(15) 6 5 Yes O2 K4 O2 119.870(14) 6_665 5 Yes O3 K4 O2 119.38(13) 2_665 4_665 Yes O3 K4 O2 92.98(10) . 4_665 Yes O3 K4 O2 63.17(12) 3_565 4_665 Yes O3 K4 O2 89.76(9) 4_675 4_665 Yes O3 K4 O2 119.41(13) 5_455 4_665 Yes O3 K4 O2 55.06(12) 6_655 4_665 Yes O2 K4 O2 119.870(14) 5_565 4_665 Yes O2 K4 O2 173.84(18) 4_565 4_665 Yes O2 K4 O2 119.870(13) 6 4_665 Yes O2 K4 O2 64.50(15) 6_665 4_665 Yes O2 K4 O2 55.41(15) 5 4_665 Yes Zn3 O1 Zn3 113.62(18) . 3 Yes Zn3 O1 Zn3 113.62(18) . 2 Yes Zn3 O1 Zn3 113.62(18) 3 2 Yes Zn3 O1 Zn2 104.9(2) . . Yes Zn3 O1 Zn2 104.9(2) 3 . Yes Zn3 O1 Zn2 104.9(2) 2 . Yes Zn3 O2 Zn2 105.5(2) 6_554 . Yes Zn3 O2 Sb1 126.7(2) 6_554 . Yes Zn2 O2 Sb1 127.8(3) . . Yes Zn3 O2 K4 87.86(10) 6_554 4_564 Yes Zn2 O2 K4 88.44(8) . 4_564 Yes Sb1 O2 K4 93.06(8) . 4_564 Yes Zn3 O2 K4 87.86(10) 6_554 4_664 Yes Zn2 O2 K4 88.44(8) . 4_664 Yes Sb1 O2 K4 93.06(8) . 4_664 Yes K4 O2 K4 173.84(18) 4_564 4_664 Yes Zn3 O3 Zn3 99.1(2) 1_565 2_665 Yes Zn3 O3 Sb1 130.43(10) 1_565 . Yes Zn3 O3 Sb1 130.43(10) 2_665 . Yes Zn3 O3 K4 88.81(15) 1_565 . Yes Zn3 O3 K4 88.81(15) 2_665 . Yes Sb1 O3 K4 91.67(16) . . Yes Zn3 O3 K4 87.98(15) 1_565 4_674 Yes Zn3 O3 K4 87.98(15) 2_665 4_674 Yes Sb1 O3 K4 93.29(16) . 4_674 Yes K4 O3 K4 175.04(18) . 4_674 Yes _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.636 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.164 #===end data_Comp2 _database_code_depnum_ccdc_archive 'CCDC 776167' #TrackingRef '- Dalton Trans-CIF.txt' _refine_ls_number_constraints ? #Added by publCIF _diffrn_ambient_pressure ? #Added by publCIF _cell_measurement_pressure ? #Added by publCIF _symmetry_space_group_name_hall R3 #Added by publCIF _audit_update_record ; 2009-06-09 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common none _chemical_melting_point none _chemical_formula_moiety 'O12 Sb3 Zn4, K' _chemical_formula_sum 'K O12 Sb3 Zn4' _chemical_formula_weight 857.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, 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' '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' _cell_length_a 10.867(9) _cell_length_b 10.867(9) _cell_length_c 7.301(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 746.7(11) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 750 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 5.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 17.975 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.354 _exptl_absorpt_correction_T_max 0.407 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 1723 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 750 _reflns_number_gt 722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0134P)^2^+0.0000P] 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 0.0140(3) _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 0.02(3) _refine_ls_number_reflns 750 _refine_ls_number_parameters 62 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0414 _refine_ls_wR_factor_gt 0.0412 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.005 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 Sb1 Sb 0.68189(5) 0.77711(4) 0.971320(8) 0.00357(15) Uani 1 1 d . . . Zn2 Zn 0.78369(8) 1.08591(8) 0.72262(12) 0.0054(2) Uani 1 1 d . . . Zn3 Zn 1.0000 1.0000 0.9883(2) 0.0068(3) Uani 1 3 d S . . K1 K 1.0000 1.0000 0.5070(5) 0.0170(7) Uani 1 3 d S . . O1 O 0.9255(5) 1.2768(5) 0.8093(8) 0.0064(11) Uani 1 1 d U . . O2 O 0.8436(5) 0.8195(5) 1.1415(8) 0.0062(12) Uani 1 1 d U . . O3 O 0.6053(6) 0.8707(6) 1.1231(7) 0.0079(11) Uani 1 1 d U . . O4 O 0.8168(5) 0.9432(6) 0.8391(7) 0.0062(11) Uani 1 1 d U . . 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 Sb1 0.0053(2) 0.0045(2) 0.0008(2) -0.00014(17) -0.00033(17) 0.00240(19) Zn2 0.0060(4) 0.0060(4) 0.0031(5) 0.0004(3) 0.0001(3) 0.0022(3) Zn3 0.0066(4) 0.0066(4) 0.0072(7) 0.000 0.000 0.0033(2) K1 0.0115(9) 0.0115(9) 0.0279(19) 0.000 0.000 0.0058(4) O1 0.0064(14) 0.0065(13) 0.0056(13) 0.0008(9) -0.0005(9) 0.0027(9) O2 0.0067(14) 0.0061(14) 0.0046(14) 0.0015(9) -0.0006(9) 0.0023(10) O3 0.0089(13) 0.0076(14) 0.0081(14) 0.0000(9) 0.0001(9) 0.0047(10) O4 0.0060(14) 0.0065(14) 0.0057(14) 0.0010(9) 0.0000(9) 0.0028(10) _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 Sb1 O4 1.922(5) . Yes Sb1 O3 1.949(6) . Yes Sb1 O2 1.980(5) 8_654 Yes Sb1 O2 2.009(5) . Yes Sb1 O1 2.010(5) 4_445 Yes Sb1 O1 2.043(5) 2_765 Yes Sb1 Zn3 3.076(2) . Yes Sb1 Sb1 3.119(2) 6_565 Yes Sb1 Sb1 3.119(2) 8_654 Yes Sb1 K1 3.664(3) 7_445 Yes Zn2 O3 1.953(5) 9_564 Yes Zn2 O3 1.965(6) 5_664 Yes Zn2 O4 1.953(6) . Yes Zn2 O1 1.970(5) . Yes Zn2 Zn2 3.135(2) 9_564 Yes Zn2 Zn2 3.135(2) 5_665 Yes Zn2 K1 3.327(3) . Yes Zn2 K1 3.606(3) 4_455 Yes Zn3 O4 2.074(5) . Yes Zn3 O4 2.074(5) 3_675 Yes Zn3 O4 2.074(5) 2_765 Yes Zn3 O2 2.158(5) 2_765 Yes Zn3 O2 2.158(5) . Yes Zn3 O2 2.158(5) 3_675 Yes Zn3 Sb1 3.076(2) 3_675 Yes Zn3 Sb1 3.076(2) 2_765 Yes Zn3 K1 3.514(5) . Yes Zn3 K1 3.787(5) 1_556 Yes K1 O3 2.690(6) 6_564 Yes K1 O3 2.690(6) 4_554 Yes K1 O3 2.690(6) 5_664 Yes K1 O4 2.999(6) 3_675 Yes K1 O4 2.999(6) 2_765 Yes K1 O4 2.999(6) . Yes K1 O1 3.173(6) 8_764 Yes K1 O1 3.173(6) 9_564 Yes K1 O1 3.173(6) 7_544 Yes K1 O2 3.243(6) 1_554 Yes K1 O2 3.243(6) 2_764 Yes K1 O2 3.243(6) 3_674 Yes O1 Sb1 2.010(5) 7_554 Yes O1 Sb1 2.043(5) 3_675 Yes O1 K1 3.173(6) 4_455 Yes O2 Sb1 1.980(5) 6_565 Yes O2 K1 3.243(6) 1_556 Yes O3 Zn2 1.954(5) 5_665 Yes O3 Zn2 1.965(6) 9_565 Yes O3 K1 2.690(6) 7_445 Yes 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 O4 Sb1 O3 96.9(2) . . Yes O4 Sb1 O2 103.5(2) . 8_654 Yes O3 Sb1 O2 93.2(2) . 8_654 Yes O4 Sb1 O2 85.8(2) . . Yes O3 Sb1 O2 94.7(2) . . Yes O2 Sb1 O2 167.06(14) 8_654 . Yes O4 Sb1 O1 163.5(2) . 4_445 Yes O3 Sb1 O1 88.6(2) . 4_445 Yes O2 Sb1 O1 91.7(2) 8_654 4_445 Yes O2 Sb1 O1 78.2(2) . 4_445 Yes O4 Sb1 O1 91.5(2) . 2_765 Yes O3 Sb1 O1 169.2(2) . 2_765 Yes O2 Sb1 O1 78.1(2) 8_654 2_765 Yes O2 Sb1 O1 92.8(2) . 2_765 Yes O1 Sb1 O1 85.22(6) 4_445 2_765 Yes O4 Sb1 Zn3 41.52(16) . . Yes O3 Sb1 Zn3 99.85(16) . . Yes O2 Sb1 Zn3 143.57(17) 8_654 . Yes O2 Sb1 Zn3 44.32(14) . . Yes O1 Sb1 Zn3 122.21(15) 4_445 . Yes O1 Sb1 Zn3 90.97(13) 2_765 . Yes O4 Sb1 Sb1 123.66(16) . 6_565 Yes O3 Sb1 Sb1 94.02(16) . 6_565 Yes O2 Sb1 Sb1 130.89(17) 8_654 6_565 Yes O2 Sb1 Sb1 38.22(14) . 6_565 Yes O1 Sb1 Sb1 40.08(15) 4_445 6_565 Yes O1 Sb1 Sb1 87.02(17) 2_765 6_565 Yes Zn3 Sb1 Sb1 82.18(3) . 6_565 Yes O4 Sb1 Sb1 97.84(18) . 8_654 Yes O3 Sb1 Sb1 131.99(16) . 8_654 Yes O2 Sb1 Sb1 38.88(13) 8_654 8_654 Yes O2 Sb1 Sb1 131.79(16) . 8_654 Yes O1 Sb1 Sb1 89.86(17) 4_445 8_654 Yes O1 Sb1 Sb1 39.28(14) 2_765 8_654 Yes Zn3 Sb1 Sb1 120.84(3) . 8_654 Yes Sb1 Sb1 Sb1 114.39(6) 6_565 8_654 Yes O4 Sb1 K1 133.50(16) . 7_445 Yes O3 Sb1 K1 45.64(17) . 7_445 Yes O2 Sb1 K1 61.95(17) 8_654 7_445 Yes O2 Sb1 K1 117.93(18) . 7_445 Yes O1 Sb1 K1 59.85(15) 4_445 7_445 Yes O1 Sb1 K1 123.63(13) 2_765 7_445 Yes Zn3 Sb1 K1 144.35(4) . 7_445 Yes Sb1 Sb1 K1 90.62(6) 6_565 7_445 Yes Sb1 Sb1 K1 93.97(6) 8_654 7_445 Yes O3 Zn2 O3 110.5(2) 9_564 5_664 Yes O3 Zn2 O4 111.6(2) 9_564 . Yes O3 Zn2 O4 107.7(2) 5_664 . Yes O3 Zn2 O1 105.8(2) 9_564 . Yes O3 Zn2 O1 111.5(2) 5_664 . Yes O4 Zn2 O1 109.8(2) . . Yes O3 Zn2 Zn2 88.11(17) 9_564 9_564 Yes O3 Zn2 Zn2 36.74(16) 5_664 9_564 Yes O4 Zn2 Zn2 90.76(17) . 9_564 Yes O1 Zn2 Zn2 147.80(17) . 9_564 Yes O3 Zn2 Zn2 36.99(16) 9_564 5_665 Yes O3 Zn2 Zn2 145.63(16) 5_664 5_665 Yes O4 Zn2 Zn2 84.40(15) . 5_665 Yes O1 Zn2 Zn2 93.22(17) . 5_665 Yes Zn2 Zn2 Zn2 113.83(7) 9_564 5_665 Yes O3 Zn2 K1 154.62(17) 9_564 . Yes O3 Zn2 K1 53.95(17) 5_664 . Yes O4 Zn2 K1 63.06(16) . . Yes O1 Zn2 K1 99.04(16) . . Yes Zn2 Zn2 K1 67.77(6) 9_564 . Yes Zn2 Zn2 K1 147.42(5) 5_665 . Yes O3 Zn2 K1 47.14(17) 9_564 4_455 Yes O3 Zn2 K1 112.11(16) 5_664 4_455 Yes O4 Zn2 K1 139.62(18) . 4_455 Yes O1 Zn2 K1 61.32(15) . 4_455 Yes Zn2 Zn2 K1 117.45(5) 9_564 4_455 Yes Zn2 Zn2 K1 58.66(5) 5_665 4_455 Yes K1 Zn2 K1 152.12(6) . 4_455 Yes O4 Zn3 O4 95.0(2) . 3_675 Yes O4 Zn3 O4 95.0(2) . 2_765 Yes O4 Zn3 O4 95.0(2) 3_675 2_765 Yes O4 Zn3 O2 170.99(18) . 2_765 Yes O4 Zn3 O2 91.72(19) 3_675 2_765 Yes O4 Zn3 O2 78.41(18) 2_765 2_765 Yes O4 Zn3 O2 78.41(18) . . Yes O4 Zn3 O2 170.99(18) 3_675 . Yes O4 Zn3 O2 91.72(19) 2_765 . Yes O2 Zn3 O2 95.5(2) 2_765 . Yes O4 Zn3 O2 91.72(18) . 3_675 Yes O4 Zn3 O2 78.41(18) 3_675 3_675 Yes O4 Zn3 O2 170.99(19) 2_765 3_675 Yes O2 Zn3 O2 95.5(2) 2_765 3_675 Yes O2 Zn3 O2 95.5(2) . 3_675 Yes O4 Zn3 Sb1 37.89(15) . . Yes O4 Zn3 Sb1 132.78(16) 3_675 . Yes O4 Zn3 Sb1 92.67(16) 2_765 . Yes O2 Zn3 Sb1 135.40(16) 2_765 . Yes O2 Zn3 Sb1 40.58(14) . . Yes O2 Zn3 Sb1 96.31(15) 3_675 . Yes O4 Zn3 Sb1 92.67(16) . 3_675 Yes O4 Zn3 Sb1 37.89(15) 3_675 3_675 Yes O4 Zn3 Sb1 132.78(16) 2_765 3_675 Yes O2 Zn3 Sb1 96.31(15) 2_765 3_675 Yes O2 Zn3 Sb1 135.40(16) . 3_675 Yes O2 Zn3 Sb1 40.58(14) 3_675 3_675 Yes Sb1 Zn3 Sb1 119.840(4) . 3_675 Yes O4 Zn3 Sb1 132.78(16) . 2_765 Yes O4 Zn3 Sb1 92.67(16) 3_675 2_765 Yes O4 Zn3 Sb1 37.89(15) 2_765 2_765 Yes O2 Zn3 Sb1 40.58(14) 2_765 2_765 Yes O2 Zn3 Sb1 96.31(15) . 2_765 Yes O2 Zn3 Sb1 135.40(16) 3_675 2_765 Yes Sb1 Zn3 Sb1 119.840(4) . 2_765 Yes Sb1 Zn3 Sb1 119.840(4) 3_675 2_765 Yes O4 Zn3 K1 58.34(14) . . Yes O4 Zn3 K1 58.34(14) 3_675 . Yes O4 Zn3 K1 58.34(14) 2_765 . Yes O2 Zn3 K1 121.24(15) 2_765 . Yes O2 Zn3 K1 121.24(15) . . Yes O2 Zn3 K1 121.24(15) 3_675 . Yes Sb1 Zn3 K1 87.70(3) . . Yes Sb1 Zn3 K1 87.70(3) 3_675 . Yes Sb1 Zn3 K1 87.70(3) 2_765 . Yes O4 Zn3 K1 121.66(14) . 1_556 Yes O4 Zn3 K1 121.66(14) 3_675 1_556 Yes O4 Zn3 K1 121.66(14) 2_765 1_556 Yes O2 Zn3 K1 58.76(15) 2_765 1_556 Yes O2 Zn3 K1 58.76(15) . 1_556 Yes O2 Zn3 K1 58.76(15) 3_675 1_556 Yes Sb1 Zn3 K1 92.30(3) . 1_556 Yes Sb1 Zn3 K1 92.30(3) 3_675 1_556 Yes Sb1 Zn3 K1 92.30(3) 2_765 1_556 Yes K1 Zn3 K1 180.000(2) . 1_556 Yes O3 K1 O3 118.15(6) 6_564 4_554 Yes O3 K1 O3 118.15(6) 6_564 5_664 Yes O3 K1 O3 118.15(6) 4_554 5_664 Yes O3 K1 O4 128.56(19) 6_564 3_675 Yes O3 K1 O4 67.29(15) 4_554 3_675 Yes O3 K1 O4 95.49(16) 5_664 3_675 Yes O3 K1 O4 67.29(14) 6_564 2_765 Yes O3 K1 O4 95.49(16) 4_554 2_765 Yes O3 K1 O4 128.56(19) 5_664 2_765 Yes O4 K1 O4 61.28(17) 3_675 2_765 Yes O3 K1 O4 95.49(16) 6_564 . Yes O3 K1 O4 128.56(19) 4_554 . Yes O3 K1 O4 67.29(15) 5_664 . Yes O4 K1 O4 61.28(18) 3_675 . Yes O4 K1 O4 61.28(17) 2_765 . Yes O3 K1 O1 167.3(2) 6_564 8_764 Yes O3 K1 O1 63.92(14) 4_554 8_764 Yes O3 K1 O1 55.57(14) 5_664 8_764 Yes O4 K1 O1 64.13(14) 3_675 8_764 Yes O4 K1 O1 125.40(17) 2_765 8_764 Yes O4 K1 O1 91.72(15) . 8_764 Yes O3 K1 O1 55.57(14) 6_564 9_564 Yes O3 K1 O1 167.3(2) 4_554 9_564 Yes O3 K1 O1 63.92(14) 5_664 9_564 Yes O4 K1 O1 125.40(17) 3_675 9_564 Yes O4 K1 O1 91.72(15) 2_765 9_564 Yes O4 K1 O1 64.13(14) . 9_564 Yes O1 K1 O1 119.50(3) 8_764 9_564 Yes O3 K1 O1 63.92(14) 6_564 7_544 Yes O3 K1 O1 55.58(14) 4_554 7_544 Yes O3 K1 O1 167.3(2) 5_664 7_544 Yes O4 K1 O1 91.72(15) 3_675 7_544 Yes O4 K1 O1 64.13(14) 2_765 7_544 Yes O4 K1 O1 125.40(17) . 7_544 Yes O1 K1 O1 119.50(3) 8_764 7_544 Yes O1 K1 O1 119.50(3) 9_564 7_544 Yes O3 K1 O2 56.61(14) 6_564 1_554 Yes O3 K1 O2 114.41(18) 4_554 1_554 Yes O3 K1 O2 78.37(15) 5_664 1_554 Yes O4 K1 O2 173.74(13) 3_675 1_554 Yes O4 K1 O2 123.61(14) 2_765 1_554 Yes O4 K1 O2 116.57(13) . 1_554 Yes O1 K1 O2 110.76(17) 8_764 1_554 Yes O1 K1 O2 52.99(11) 9_564 1_554 Yes O1 K1 O2 94.10(15) 7_544 1_554 Yes O3 K1 O2 78.37(15) 6_564 2_764 Yes O3 K1 O2 56.61(14) 4_554 2_764 Yes O3 K1 O2 114.41(18) 5_664 2_764 Yes O4 K1 O2 123.61(14) 3_675 2_764 Yes O4 K1 O2 116.57(13) 2_765 2_764 Yes O4 K1 O2 173.74(13) . 2_764 Yes O1 K1 O2 94.10(15) 8_764 2_764 Yes O1 K1 O2 110.76(17) 9_564 2_764 Yes O1 K1 O2 52.99(11) 7_544 2_764 Yes O2 K1 O2 59.02(16) 1_554 2_764 Yes O3 K1 O2 114.41(18) 6_564 3_674 Yes O3 K1 O2 78.37(15) 4_554 3_674 Yes O3 K1 O2 56.61(14) 5_664 3_674 Yes O4 K1 O2 116.57(13) 3_675 3_674 Yes O4 K1 O2 173.74(13) 2_765 3_674 Yes O4 K1 O2 123.61(14) . 3_674 Yes O1 K1 O2 52.99(11) 8_764 3_674 Yes O1 K1 O2 94.10(15) 9_564 3_674 Yes O1 K1 O2 110.76(17) 7_544 3_674 Yes O2 K1 O2 59.02(16) 1_554 3_674 Yes O2 K1 O2 59.02(16) 2_764 3_674 Yes Zn2 O1 Sb1 121.5(3) . 7_554 Yes Zn2 O1 Sb1 124.2(2) . 3_675 Yes Sb1 O1 Sb1 100.6(2) 7_554 3_675 Yes Zn2 O1 K1 85.67(17) . 4_455 Yes Sb1 O1 K1 86.94(17) 7_554 4_455 Yes Sb1 O1 K1 134.9(2) 3_675 4_455 Yes Sb1 O2 Sb1 102.90(19) 6_565 . Yes Sb1 O2 Zn3 159.5(3) 6_565 . Yes Sb1 O2 Zn3 95.1(2) . . Yes Sb1 O2 K1 85.5(2) 6_565 1_556 Yes Sb1 O2 K1 141.4(2) . 1_556 Yes Zn3 O2 K1 86.58(16) . 1_556 Yes Zn2 O3 Zn2 106.3(3) 5_665 9_565 Yes Zn2 O3 Sb1 127.4(3) 5_665 . Yes Zn2 O3 Sb1 119.8(3) 9_565 . Yes Zn2 O3 K1 100.7(2) 5_665 7_445 Yes Zn2 O3 K1 89.9(2) 9_565 7_445 Yes Sb1 O3 K1 103.2(2) . 7_445 Yes Sb1 O4 Zn2 127.4(3) . . Yes Sb1 O4 Zn3 100.6(2) . . Yes Zn2 O4 Zn3 121.5(3) . . Yes Sb1 O4 K1 135.7(3) . . Yes Zn2 O4 K1 81.46(18) . . Yes Zn3 O4 K1 85.61(17) . . Yes _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.774 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.209 #===end