data_comp1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 I4 K2 Mn O14' _chemical_formula_weight 868.77 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' 'H' 'H' 0.0000 0.0000 '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' 'Mn' 'Mn' 0.3368 0.7283 '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 monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.356(5) _cell_length_b 7.7609(18) _cell_length_c 11.166(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.09(3) _cell_angle_gamma 90.00 _cell_volume 724.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1149 _cell_measurement_theta_min 3.0425 _cell_measurement_theta_max 27.4797 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'White' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 10.081 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7249 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury70 _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2779 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1385 _reflns_number_gt 1376 _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^)+(0.0148P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00350(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 0.00 _refine_ls_number_reflns 1385 _refine_ls_number_parameters 102 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0140 _refine_ls_R_factor_gt 0.0139 _refine_ls_wR_factor_ref 0.0314 _refine_ls_wR_factor_gt 0.0313 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _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 1.0000 1.8709(3) 1.0000 0.0183(5) Uani 1 2 d S . . K2 K 1.0000 1.3455(3) 1.0000 0.0209(5) Uani 1 2 d S . . Mn1 Mn 0.5000 1.41278(18) 1.0000 0.0118(2) Uani 1 2 d S . . I1 I 1.24082(3) 2.08972(4) 0.72314(2) 0.01122(8) Uani 1 1 d . . . I2 I 0.74786(3) 1.60457(4) 0.76076(2) 0.01160(9) Uani 1 1 d . . . O1 O 1.4385(3) 2.1056(6) 0.6599(3) 0.0190(7) Uani 1 1 d . . . O2 O 1.1756(4) 1.8963(5) 0.6429(3) 0.0178(8) Uani 1 1 d . . . O3 O 1.2781(4) 1.9912(5) 0.8662(3) 0.0192(8) Uani 1 1 d . . . O4 O 0.7303(4) 1.7914(5) 0.8575(4) 0.0166(8) Uani 1 1 d . . . O5 O 0.7065(4) 1.4425(5) 0.8745(4) 0.0171(9) Uani 1 1 d . . . O6 O 0.5591(3) 1.6155(6) 0.6826(3) 0.0173(7) Uani 1 1 d . . . O1W O 0.5000 1.6878(8) 1.0000 0.0330(15) Uani 1 2 d S . . H1WA H 0.4252 1.7244 1.0457 0.049 Uiso 0.50 1 d PR . . H1WB H 0.5904 1.7244 1.0257 0.049 Uiso 0.50 1 d PR . . O2W O 0.5000 1.1423(6) 1.0000 0.0323(15) Uani 1 2 d S . . H2WA H 0.5904 1.1057 1.0257 0.048 Uiso 0.50 1 d PR . . H2WB H 0.4844 1.1057 0.9286 0.048 Uiso 0.50 1 d PR . . 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 0.0210(9) 0.0153(9) 0.0185(11) 0.000 -0.0016(7) 0.000 K2 0.0303(11) 0.0163(10) 0.0161(11) 0.000 -0.0043(9) 0.000 Mn1 0.0120(5) 0.0113(6) 0.0120(5) 0.000 -0.0026(5) 0.000 I1 0.01113(12) 0.01077(17) 0.01175(13) 0.00032(18) -0.00143(10) -0.00060(19) I2 0.01006(12) 0.0135(2) 0.01130(13) 0.0009(2) 0.00047(11) 0.0000(2) O1 0.0134(13) 0.0219(19) 0.0218(15) 0.000(2) 0.0037(11) -0.0015(19) O2 0.0222(17) 0.0132(19) 0.0182(17) -0.0028(15) -0.0081(14) -0.0018(16) O3 0.0253(19) 0.0175(18) 0.0148(17) 0.0070(14) -0.0049(14) -0.0045(15) O4 0.021(2) 0.0139(18) 0.015(2) -0.0024(15) 0.0014(17) -0.0029(18) O5 0.019(2) 0.016(2) 0.0163(19) 0.0018(16) 0.0037(15) 0.0014(15) O6 0.0130(13) 0.023(2) 0.0160(14) 0.0020(18) -0.0024(11) -0.0003(17) O1W 0.042(3) 0.020(3) 0.036(4) 0.000 0.022(3) 0.000 O2W 0.048(3) 0.011(3) 0.038(3) 0.000 -0.031(3) 0.000 _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 2.773(5) 4_746 ? K1 O1 2.773(5) 3_445 ? K1 O4 2.825(4) . ? K1 O4 2.825(4) 2_757 ? K1 O6 2.828(4) 3 ? K1 O6 2.828(4) 4_656 ? K1 O3 2.919(4) . ? K1 O3 2.919(4) 2_757 ? K1 K2 3.684(2) 1_565 ? K1 I1 3.9593(19) 3_445 ? K1 I1 3.9593(19) 4_746 ? K1 I2 3.9785(18) . ? K2 O1 2.744(5) 3_445 ? K2 O1 2.744(5) 4_746 ? K2 O6 2.754(4) 4_646 ? K2 O6 2.754(4) 3_545 ? K2 O5 2.921(4) 2_757 ? K2 O5 2.921(4) . ? K2 O2 3.172(4) 3_445 ? K2 O2 3.172(4) 4_746 ? K2 K1 3.684(2) 1_545 ? K2 I1 3.8089(18) 3_445 ? K2 I1 3.8089(18) 4_746 ? K2 I2 3.9496(18) 2_757 ? Mn1 O2W 2.099(5) . ? Mn1 O1W 2.134(6) . ? Mn1 O2 2.170(3) 3_445 ? Mn1 O2 2.170(3) 4_646 ? Mn1 O5 2.236(4) 2_657 ? Mn1 O5 2.236(4) . ? I1 O3 1.797(3) . ? I1 O1 1.802(3) . ? I1 O2 1.830(4) . ? I1 K2 3.8089(18) 3_554 ? I1 K1 3.9593(19) 3_554 ? I2 O6 1.804(3) . ? I2 O4 1.814(4) . ? I2 O5 1.821(4) . ? I2 K1 4.0047(18) 3_444 ? I2 K2 4.0304(17) 3_454 ? O1 K2 2.744(4) 3_554 ? O1 K1 2.773(5) 3_554 ? O2 Mn1 2.170(3) 3_554 ? O2 K2 3.172(4) 3_554 ? O6 K2 2.754(4) 3_454 ? O6 K1 2.828(4) 3_444 ? O1W H1WA 0.8561 . ? O1W H1WB 0.8566 . ? O2W H2WA 0.8566 . ? O2W H2WB 0.8563 . ? 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 84.15(18) 4_746 3_445 ? O1 K1 O4 67.90(11) 4_746 . ? O1 K1 O4 92.99(11) 3_445 . ? O1 K1 O4 92.99(11) 4_746 2_757 ? O1 K1 O4 67.90(11) 3_445 2_757 ? O4 K1 O4 154.77(18) . 2_757 ? O1 K1 O6 158.41(9) 4_746 3 ? O1 K1 O6 93.81(11) 3_445 3 ? O4 K1 O6 133.69(11) . 3 ? O4 K1 O6 66.57(11) 2_757 3 ? O1 K1 O6 93.81(10) 4_746 4_656 ? O1 K1 O6 158.41(9) 3_445 4_656 ? O4 K1 O6 66.57(11) . 4_656 ? O4 K1 O6 133.69(12) 2_757 4_656 ? O6 K1 O6 95.69(17) 3 4_656 ? O1 K1 O3 76.08(11) 4_746 . ? O1 K1 O3 135.69(10) 3_445 . ? O4 K1 O3 114.62(11) . . ? O4 K1 O3 73.93(11) 2_757 . ? O6 K1 O3 90.92(10) 3 . ? O6 K1 O3 63.54(10) 4_656 . ? O1 K1 O3 135.69(11) 4_746 2_757 ? O1 K1 O3 76.08(11) 3_445 2_757 ? O4 K1 O3 73.93(11) . 2_757 ? O4 K1 O3 114.62(11) 2_757 2_757 ? O6 K1 O3 63.54(10) 3 2_757 ? O6 K1 O3 90.92(10) 4_656 2_757 ? O3 K1 O3 142.68(17) . 2_757 ? O1 K1 K2 137.93(9) 4_746 1_565 ? O1 K1 K2 137.93(9) 3_445 1_565 ? O4 K1 K2 102.61(9) . 1_565 ? O4 K1 K2 102.61(9) 2_757 1_565 ? O6 K1 K2 47.84(8) 3 1_565 ? O6 K1 K2 47.84(9) 4_656 1_565 ? O3 K1 K2 71.34(8) . 1_565 ? O3 K1 K2 71.34(8) 2_757 1_565 ? O1 K1 I1 95.63(10) 4_746 3_445 ? O1 K1 I1 23.62(6) 3_445 3_445 ? O4 K1 I1 78.32(9) . 3_445 ? O4 K1 I1 87.81(9) 2_757 3_445 ? O6 K1 I1 90.65(8) 3 3_445 ? O6 K1 I1 136.75(6) 4_656 3_445 ? O3 K1 I1 159.29(8) . 3_445 ? O3 K1 I1 54.36(8) 2_757 3_445 ? K2 K1 I1 123.44(3) 1_565 3_445 ? O1 K1 I1 23.62(6) 4_746 4_746 ? O1 K1 I1 95.63(10) 3_445 4_746 ? O4 K1 I1 87.81(9) . 4_746 ? O4 K1 I1 78.32(9) 2_757 4_746 ? O6 K1 I1 136.75(6) 3 4_746 ? O6 K1 I1 90.65(7) 4_656 4_746 ? O3 K1 I1 54.36(8) . 4_746 ? O3 K1 I1 159.29(8) 2_757 4_746 ? K2 K1 I1 123.44(3) 1_565 4_746 ? I1 K1 I1 113.12(7) 3_445 4_746 ? O1 K1 I2 44.00(6) 4_746 . ? O1 K1 I2 87.02(9) 3_445 . ? O4 K1 I2 24.10(8) . . ? O4 K1 I2 133.31(10) 2_757 . ? O6 K1 I2 157.55(7) 3 . ? O6 K1 I2 76.88(8) 4_656 . ? O3 K1 I2 104.11(7) . . ? O3 K1 I2 95.09(7) 2_757 . ? K2 K1 I2 121.30(3) 1_565 . ? I1 K1 I2 81.17(4) 3_445 . ? I1 K1 I2 65.22(4) 4_746 . ? O1 K2 O1 85.26(18) 3_445 4_746 ? O1 K2 O6 157.67(9) 3_445 4_646 ? O1 K2 O6 91.66(11) 4_746 4_646 ? O1 K2 O6 91.66(11) 3_445 3_545 ? O1 K2 O6 157.67(9) 4_746 3_545 ? O6 K2 O6 99.17(17) 4_646 3_545 ? O1 K2 O5 69.91(10) 3_445 2_757 ? O1 K2 O5 87.96(11) 4_746 2_757 ? O6 K2 O5 132.17(10) 4_646 2_757 ? O6 K2 O5 70.29(11) 3_545 2_757 ? O1 K2 O5 87.96(11) 3_445 . ? O1 K2 O5 69.91(10) 4_746 . ? O6 K2 O5 70.29(11) 4_646 . ? O6 K2 O5 132.17(10) 3_545 . ? O5 K2 O5 150.14(17) 2_757 . ? O1 K2 O2 54.56(10) 3_445 3_445 ? O1 K2 O2 113.38(11) 4_746 3_445 ? O6 K2 O2 107.50(10) 4_646 3_445 ? O6 K2 O2 81.98(10) 3_545 3_445 ? O5 K2 O2 116.37(10) 2_757 3_445 ? O5 K2 O2 59.45(10) . 3_445 ? O1 K2 O2 113.38(11) 3_445 4_746 ? O1 K2 O2 54.56(9) 4_746 4_746 ? O6 K2 O2 81.98(10) 4_646 4_746 ? O6 K2 O2 107.50(10) 3_545 4_746 ? O5 K2 O2 59.45(10) 2_757 4_746 ? O5 K2 O2 116.37(10) . 4_746 ? O2 K2 O2 165.71(16) 3_445 4_746 ? O1 K2 K1 137.37(9) 3_445 1_545 ? O1 K2 K1 137.37(9) 4_746 1_545 ? O6 K2 K1 49.59(8) 4_646 1_545 ? O6 K2 K1 49.59(8) 3_545 1_545 ? O5 K2 K1 104.93(8) 2_757 1_545 ? O5 K2 K1 104.93(8) . 1_545 ? O2 K2 K1 97.14(8) 3_445 1_545 ? O2 K2 K1 97.14(8) 4_746 1_545 ? O1 K2 I1 25.98(7) 3_445 3_445 ? O1 K2 I1 99.60(10) 4_746 3_445 ? O6 K2 I1 134.86(6) 4_646 3_445 ? O6 K2 I1 86.55(8) 3_545 3_445 ? O5 K2 I1 92.06(9) 2_757 3_445 ? O5 K2 I1 73.00(9) . 3_445 ? O2 K2 I1 28.58(7) 3_445 3_445 ? O2 K2 I1 138.97(9) 4_746 3_445 ? K1 K2 I1 119.84(3) 1_545 3_445 ? O1 K2 I1 99.60(10) 3_445 4_746 ? O1 K2 I1 25.98(7) 4_746 4_746 ? O6 K2 I1 86.55(8) 4_646 4_746 ? O6 K2 I1 134.86(6) 3_545 4_746 ? O5 K2 I1 73.00(9) 2_757 4_746 ? O5 K2 I1 92.06(9) . 4_746 ? O2 K2 I1 138.97(9) 3_445 4_746 ? O2 K2 I1 28.58(6) 4_746 4_746 ? K1 K2 I1 119.84(3) 1_545 4_746 ? I1 K2 I1 120.31(7) 3_445 4_746 ? O1 K2 I2 44.42(6) 3_445 2_757 ? O1 K2 I2 88.00(9) 4_746 2_757 ? O6 K2 I2 157.74(7) 4_646 2_757 ? O6 K2 I2 74.61(8) 3_545 2_757 ? O5 K2 I2 25.57(7) 2_757 2_757 ? O5 K2 I2 129.78(10) . 2_757 ? O2 K2 I2 92.97(7) 3_445 2_757 ? O2 K2 I2 79.72(7) 4_746 2_757 ? K1 K2 I2 120.60(3) 1_545 2_757 ? I1 K2 I2 66.89(4) 3_445 2_757 ? I1 K2 I2 83.44(4) 4_746 2_757 ? O2W Mn1 O1W 180.000(3) . . ? O2W Mn1 O2 86.63(11) . 3_445 ? O1W Mn1 O2 93.37(11) . 3_445 ? O2W Mn1 O2 86.63(11) . 4_646 ? O1W Mn1 O2 93.37(11) . 4_646 ? O2 Mn1 O2 173.3(2) 3_445 4_646 ? O2W Mn1 O5 95.91(10) . 2_657 ? O1W Mn1 O5 84.09(10) . 2_657 ? O2 Mn1 O5 93.84(15) 3_445 2_657 ? O2 Mn1 O5 86.85(15) 4_646 2_657 ? O2W Mn1 O5 95.91(10) . . ? O1W Mn1 O5 84.09(10) . . ? O2 Mn1 O5 86.85(15) 3_445 . ? O2 Mn1 O5 93.84(15) 4_646 . ? O5 Mn1 O5 168.2(2) 2_657 . ? O3 I1 O1 102.68(16) . . ? O3 I1 O2 97.88(16) . . ? O1 I1 O2 97.85(18) . . ? O3 I1 K2 105.75(13) . 3_554 ? O1 I1 K2 41.85(15) . 3_554 ? O2 I1 K2 56.01(11) . 3_554 ? O3 I1 K1 134.36(11) . 3_554 ? O1 I1 K1 38.08(14) . 3_554 ? O2 I1 K1 107.86(11) . 3_554 ? K2 I1 K1 63.29(4) 3_554 3_554 ? O3 I1 K1 39.80(11) . . ? O1 I1 K1 141.48(12) . . ? O2 I1 K1 83.23(12) . . ? K2 I1 K1 124.92(6) 3_554 . ? K1 I1 K1 168.86(5) 3_554 . ? O6 I2 O4 100.33(18) . . ? O6 I2 O5 101.72(17) . . ? O4 I2 O5 96.97(16) . . ? O6 I2 K2 144.73(14) . . ? O4 I2 K2 92.74(13) . . ? O5 I2 K2 43.80(12) . . ? O6 I2 K1 139.68(14) . . ? O4 I2 K1 39.48(12) . . ? O5 I2 K1 89.51(13) . . ? K2 I2 K1 61.90(4) . . ? O6 I2 K1 38.60(13) . 3_444 ? O4 I2 K1 138.82(12) . 3_444 ? O5 I2 K1 95.50(13) . 3_444 ? K2 I2 K1 122.41(6) . 3_444 ? K1 I2 K1 174.97(5) . 3_444 ? O6 I2 K2 34.97(12) . 3_454 ? O4 I2 K2 90.99(13) . 3_454 ? O5 I2 K2 136.59(12) . 3_454 ? K2 I2 K2 176.14(5) . 3_454 ? K1 I2 K2 121.00(6) . 3_454 ? K1 I2 K2 54.57(4) 3_444 3_454 ? I1 O1 K2 112.17(19) . 3_554 ? I1 O1 K1 118.30(18) . 3_554 ? K2 O1 K1 95.30(10) 3_554 3_554 ? I1 O2 Mn1 120.80(19) . 3_554 ? I1 O2 K2 95.41(13) . 3_554 ? Mn1 O2 K2 102.40(12) 3_554 3_554 ? I1 O3 K1 116.99(15) . . ? I2 O4 K1 116.42(17) . . ? I2 O5 Mn1 130.96(19) . . ? I2 O5 K2 110.63(15) . . ? Mn1 O5 K2 108.73(16) . . ? I2 O6 K2 122.97(17) . 3_454 ? I2 O6 K1 117.96(18) . 3_444 ? K2 O6 K1 82.57(9) 3_454 3_444 ? Mn1 O1W H1WA 109.4 . . ? Mn1 O1W H1WB 109.4 . . ? H1WA O1W H1WB 109.6 . . ? Mn1 O2W H2WA 109.4 . . ? Mn1 O2W H2WB 109.4 . . ? H2WA O2W H2WB 109.6 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.607 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.133 #===end data_comp2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 Co I4 K2 O14' _chemical_formula_weight 872.76 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' 'H' 'H' 0.0000 0.0000 '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' 'Co' 'Co' 0.3494 0.9721 '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 monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.285(7) _cell_length_b 7.738(3) _cell_length_c 11.043(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.06(5) _cell_angle_gamma 90.00 _cell_volume 708.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1132 _cell_measurement_theta_min 3.0721 _cell_measurement_theta_max 27.4487 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'red purple' _exptl_crystal_size_max 0.0800 _exptl_crystal_size_mid 0.0600 _exptl_crystal_size_min 0.0400 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 10.589 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.4849 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury70 _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2790 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1497 _reflns_number_gt 1465 _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^)+(0.0243P)^2^+2.6402P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00094(13) _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 0.00 _refine_ls_number_reflns 1497 _refine_ls_number_parameters 102 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.0000 -0.8711(9) 0.0000 0.0233(17) Uani 1 2 d S . . K2 K 0.0000 -0.3434(11) 0.0000 0.031(2) Uani 1 2 d S . . Co1 Co 0.5000 -0.4165(6) 0.0000 0.0171(7) Uani 1 2 d S . . I1 I -0.23899(10) -1.09191(16) 0.27865(6) 0.0134(2) Uani 1 1 d . . . I2 I 0.25183(12) -0.60150(18) 0.23854(6) 0.0160(3) Uani 1 1 d . . . O1 O -0.4379(9) -1.107(2) 0.3435(9) 0.022(2) Uani 1 1 d . . . O2 O -0.1702(11) -0.9007(15) 0.3581(8) 0.016(2) Uani 1 1 d . . . O3 O -0.2803(11) -0.9955(13) 0.1354(8) 0.020(2) Uani 1 1 d . . . O4 O 0.2678(13) -0.789(2) 0.1457(11) 0.022(3) Uani 1 1 d . . . O5 O 0.2964(13) -0.4314(15) 0.1217(11) 0.017(3) Uani 1 1 d . . . O6 O 0.4409(10) -0.6155(17) 0.3181(8) 0.020(2) Uani 1 1 d . . . O1W O 0.5000 -0.688(2) 0.0000 0.022(4) Uani 1 2 d S . . H1WA H 0.5749 -0.7245 -0.0457 0.033 Uiso 0.50 1 d PR . . H1WB H 0.4096 -0.7245 -0.0258 0.033 Uiso 0.50 1 d PR . . O2W O 0.5000 -0.1540(15) 0.0000 0.035(5) Uani 1 2 d S . . H2WA H 0.4096 -0.1174 -0.0258 0.052 Uiso 0.50 1 d PR . . H2WB H 0.5156 -0.1174 0.0714 0.052 Uiso 0.50 1 d PR . . 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 0.027(3) 0.016(4) 0.027(4) 0.000 -0.010(3) 0.000 K2 0.033(4) 0.035(5) 0.023(4) 0.000 0.002(5) 0.000 Co1 0.0134(13) 0.0201(18) 0.0179(15) 0.000 -0.0017(19) 0.000 I1 0.0131(3) 0.0133(5) 0.0139(3) 0.0008(6) -0.0001(4) 0.0002(7) I2 0.0130(4) 0.0190(6) 0.0161(4) -0.0038(9) 0.0005(5) 0.0017(9) O1 0.011(4) 0.024(6) 0.031(5) 0.018(8) 0.002(3) 0.008(6) O2 0.016(4) 0.011(6) 0.022(5) -0.004(5) -0.004(4) -0.001(4) O3 0.022(5) 0.018(5) 0.020(5) 0.008(4) -0.008(5) -0.014(4) O4 0.020(6) 0.030(6) 0.017(6) -0.003(5) 0.001(6) -0.012(6) O5 0.014(6) 0.032(7) 0.006(5) 0.009(5) 0.005(4) 0.000(5) O6 0.023(4) 0.011(6) 0.026(5) -0.002(6) -0.010(4) -0.007(5) O1W 0.035(8) 0.023(8) 0.008(7) 0.000 0.015(7) 0.000 O2W 0.052(10) 0.009(9) 0.044(10) 0.000 -0.042(9) 0.000 _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 2.726(14) 4_455 ? K1 O1 2.726(14) 3_554 ? K1 O6 2.801(12) 3_444 ? K1 O6 2.801(12) 4_545 ? K1 O4 2.811(12) . ? K1 O4 2.811(12) 2 ? K1 O3 2.926(10) . ? K1 O3 2.926(10) 2 ? K1 K2 3.655(7) 1_545 ? K1 I1 3.915(4) 4_455 ? K1 I1 3.915(4) 3_554 ? K1 I2 3.954(4) . ? K2 O6 2.717(11) 4 ? K2 O6 2.717(11) 3_454 ? K2 O1 2.724(15) 3_554 ? K2 O1 2.724(15) 4_455 ? K2 O5 2.880(12) 2 ? K2 O5 2.880(12) . ? K2 O2 3.182(10) 4_455 ? K2 O2 3.182(10) 3_554 ? K2 K1 3.655(7) 1_565 ? K2 I1 3.790(5) 4_455 ? K2 I1 3.790(5) 3_554 ? K2 I2 3.908(5) 2 ? Co1 O2W 2.031(13) . ? Co1 O1W 2.100(18) . ? Co1 O2 2.110(9) 4 ? Co1 O2 2.110(9) 3_554 ? Co1 O5 2.161(11) . ? Co1 O5 2.161(11) 2_655 ? I1 O3 1.782(9) . ? I1 O1 1.801(8) . ? I1 O2 1.812(10) . ? I1 K2 3.790(5) 3_445 ? I1 K1 3.915(4) 3_445 ? I2 O4 1.784(14) . ? I2 O6 1.799(8) . ? I2 O5 1.880(11) . ? I2 K1 3.966(4) 3 ? I2 K2 4.007(4) 3_545 ? O1 K2 2.724(15) 3_445 ? O1 K1 2.726(14) 3_445 ? O2 Co1 2.110(9) 3_445 ? O2 K2 3.182(10) 3_445 ? O6 K2 2.717(11) 3_545 ? O6 K1 2.801(12) 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 O1 K1 O1 82.9(6) 4_455 3_554 ? O1 K1 O6 158.1(3) 4_455 3_444 ? O1 K1 O6 94.8(3) 3_554 3_444 ? O1 K1 O6 94.8(3) 4_455 4_545 ? O1 K1 O6 158.1(3) 3_554 4_545 ? O6 K1 O6 95.1(5) 3_444 4_545 ? O1 K1 O4 67.5(4) 4_455 . ? O1 K1 O4 92.6(4) 3_554 . ? O6 K1 O4 134.4(4) 3_444 . ? O6 K1 O4 66.7(4) 4_545 . ? O1 K1 O4 92.6(4) 4_455 2 ? O1 K1 O4 67.5(4) 3_554 2 ? O6 K1 O4 66.7(4) 3_444 2 ? O6 K1 O4 134.4(4) 4_545 2 ? O4 K1 O4 154.0(7) . 2 ? O1 K1 O3 76.8(3) 4_455 . ? O1 K1 O3 136.2(3) 3_554 . ? O6 K1 O3 90.3(3) 3_444 . ? O6 K1 O3 63.2(3) 4_545 . ? O4 K1 O3 114.1(3) . . ? O4 K1 O3 74.9(3) 2 . ? O1 K1 O3 136.2(3) 4_455 2 ? O1 K1 O3 76.8(3) 3_554 2 ? O6 K1 O3 63.2(3) 3_444 2 ? O6 K1 O3 90.3(3) 4_545 2 ? O4 K1 O3 74.9(3) . 2 ? O4 K1 O3 114.1(3) 2 2 ? O3 K1 O3 141.6(5) . 2 ? O1 K1 K2 138.6(3) 4_455 1_545 ? O1 K1 K2 138.6(3) 3_554 1_545 ? O6 K1 K2 47.5(3) 3_444 1_545 ? O6 K1 K2 47.5(3) 4_545 1_545 ? O4 K1 K2 103.0(3) . 1_545 ? O4 K1 K2 103.0(3) 2 1_545 ? O3 K1 K2 70.8(2) . 1_545 ? O3 K1 K2 70.8(2) 2 1_545 ? O1 K1 I1 23.89(19) 4_455 4_455 ? O1 K1 I1 95.0(3) 3_554 4_455 ? O6 K1 I1 136.37(18) 3_444 4_455 ? O6 K1 I1 91.2(2) 4_545 4_455 ? O4 K1 I1 87.4(3) . 4_455 ? O4 K1 I1 78.3(3) 2 4_455 ? O3 K1 I1 54.8(2) . 4_455 ? O3 K1 I1 160.0(2) 2 4_455 ? K2 K1 I1 123.49(9) 1_545 4_455 ? O1 K1 I1 95.0(3) 4_455 3_554 ? O1 K1 I1 23.89(19) 3_554 3_554 ? O6 K1 I1 91.2(2) 3_444 3_554 ? O6 K1 I1 136.37(18) 4_545 3_554 ? O4 K1 I1 78.3(3) . 3_554 ? O4 K1 I1 87.4(3) 2 3_554 ? O3 K1 I1 160.0(2) . 3_554 ? O3 K1 I1 54.8(2) 2 3_554 ? K2 K1 I1 123.49(9) 1_545 3_554 ? I1 K1 I1 113.02(19) 4_455 3_554 ? O1 K1 I2 44.10(17) 4_455 . ? O1 K1 I2 85.8(3) 3_554 . ? O6 K1 I2 157.75(19) 3_444 . ? O6 K1 I2 77.7(2) 4_545 . ? O4 K1 I2 23.7(3) . . ? O4 K1 I2 132.7(4) 2 . ? O3 K1 I2 104.58(18) . . ? O3 K1 I2 95.48(19) 2 . ? K2 K1 I2 121.85(9) 1_545 . ? I1 K1 I2 65.44(9) 4_455 . ? I1 K1 I2 80.41(11) 3_554 . ? O6 K2 O6 99.1(5) 4 3_454 ? O6 K2 O1 157.1(3) 4 3_554 ? O6 K2 O1 92.9(3) 3_454 3_554 ? O6 K2 O1 92.9(3) 4 4_455 ? O6 K2 O1 157.1(3) 3_454 4_455 ? O1 K2 O1 83.0(6) 3_554 4_455 ? O6 K2 O5 130.7(3) 4 2 ? O6 K2 O5 69.9(3) 3_454 2 ? O1 K2 O5 71.8(3) 3_554 2 ? O1 K2 O5 87.5(3) 4_455 2 ? O6 K2 O5 69.9(3) 4 . ? O6 K2 O5 130.7(3) 3_454 . ? O1 K2 O5 87.5(3) 3_554 . ? O1 K2 O5 71.8(3) 4_455 . ? O5 K2 O5 152.6(5) 2 . ? O6 K2 O2 83.1(3) 4 4_455 ? O6 K2 O2 107.5(3) 3_454 4_455 ? O1 K2 O2 111.8(4) 3_554 4_455 ? O1 K2 O2 54.6(3) 4_455 4_455 ? O5 K2 O2 57.6(3) 2 4_455 ? O5 K2 O2 118.0(3) . 4_455 ? O6 K2 O2 107.5(3) 4 3_554 ? O6 K2 O2 83.1(3) 3_454 3_554 ? O1 K2 O2 54.6(3) 3_554 3_554 ? O1 K2 O2 111.8(4) 4_455 3_554 ? O5 K2 O2 118.0(3) 2 3_554 ? O5 K2 O2 57.6(3) . 3_554 ? O2 K2 O2 164.0(5) 4_455 3_554 ? O6 K2 K1 49.5(3) 4 1_565 ? O6 K2 K1 49.5(3) 3_454 1_565 ? O1 K2 K1 138.5(3) 3_554 1_565 ? O1 K2 K1 138.5(3) 4_455 1_565 ? O5 K2 K1 103.7(3) 2 1_565 ? O5 K2 K1 103.7(3) . 1_565 ? O2 K2 K1 98.0(2) 4_455 1_565 ? O2 K2 K1 98.0(2) 3_554 1_565 ? O6 K2 I1 87.4(2) 4 4_455 ? O6 K2 I1 134.72(19) 3_454 4_455 ? O1 K2 I1 97.9(3) 3_554 4_455 ? O1 K2 I1 26.1(2) 4_455 4_455 ? O5 K2 I1 72.2(2) 2 4_455 ? O5 K2 I1 93.8(2) . 4_455 ? O2 K2 I1 28.46(19) 4_455 4_455 ? O2 K2 I1 137.5(3) 3_554 4_455 ? K1 K2 I1 120.50(11) 1_565 4_455 ? O6 K2 I1 134.72(18) 4 3_554 ? O6 K2 I1 87.4(2) 3_454 3_554 ? O1 K2 I1 26.1(2) 3_554 3_554 ? O1 K2 I1 97.9(3) 4_455 3_554 ? O5 K2 I1 93.8(2) 2 3_554 ? O5 K2 I1 72.2(2) . 3_554 ? O2 K2 I1 137.5(3) 4_455 3_554 ? O2 K2 I1 28.46(19) 3_554 3_554 ? K1 K2 I1 120.50(11) 1_565 3_554 ? I1 K2 I1 119.0(2) 4_455 3_554 ? O6 K2 I2 157.8(2) 4 2 ? O6 K2 I2 74.8(2) 3_454 2 ? O1 K2 I2 44.80(17) 3_554 2 ? O1 K2 I2 86.8(3) 4_455 2 ? O5 K2 I2 27.1(2) 2 2 ? O5 K2 I2 130.4(3) . 2 ? O2 K2 I2 78.6(2) 4_455 2 ? O2 K2 I2 93.2(2) 3_554 2 ? K1 K2 I2 120.74(11) 1_565 2 ? I1 K2 I2 82.57(12) 4_455 2 ? I1 K2 I2 67.07(10) 3_554 2 ? O2W Co1 O1W 180.000(1) . . ? O2W Co1 O2 86.7(3) . 4 ? O1W Co1 O2 93.3(3) . 4 ? O2W Co1 O2 86.7(3) . 3_554 ? O1W Co1 O2 93.3(3) . 3_554 ? O2 Co1 O2 173.4(7) 4 3_554 ? O2W Co1 O5 93.1(3) . . ? O1W Co1 O5 86.9(3) . . ? O2 Co1 O5 93.6(4) 4 . ? O2 Co1 O5 86.7(4) 3_554 . ? O2W Co1 O5 93.1(3) . 2_655 ? O1W Co1 O5 86.9(3) . 2_655 ? O2 Co1 O5 86.7(4) 4 2_655 ? O2 Co1 O5 93.6(4) 3_554 2_655 ? O5 Co1 O5 173.9(6) . 2_655 ? O3 I1 O1 101.8(4) . . ? O3 I1 O2 98.5(4) . . ? O1 I1 O2 98.5(6) . . ? O3 I1 K2 104.6(4) . 3_445 ? O1 I1 K2 41.7(5) . 3_445 ? O2 I1 K2 56.8(3) . 3_445 ? O3 I1 K1 132.8(3) . 3_445 ? O1 I1 K1 37.8(4) . 3_445 ? O2 I1 K1 108.8(3) . 3_445 ? K2 I1 K1 63.99(9) 3_445 3_445 ? O3 I1 K1 40.6(3) . . ? O1 I1 K1 141.2(4) . . ? O2 I1 K1 82.5(3) . . ? K2 I1 K1 123.86(19) 3_445 . ? K1 I1 K1 168.62(14) 3_445 . ? O4 I2 O6 99.6(6) . . ? O4 I2 O5 99.3(5) . . ? O6 I2 O5 101.9(5) . . ? O4 I2 K2 94.0(5) . . ? O6 I2 K2 145.5(4) . . ? O5 I2 K2 44.3(3) . . ? O4 I2 K1 39.3(4) . . ? O6 I2 K1 138.8(4) . . ? O5 I2 K1 90.9(4) . . ? K2 I2 K1 62.59(9) . . ? O4 I2 K1 138.2(4) . 3 ? O6 I2 K1 38.8(4) . 3 ? O5 I2 K1 94.8(4) . 3 ? K2 I2 K1 122.48(19) . 3 ? K1 I2 K1 174.27(16) . 3 ? O4 I2 K2 89.7(4) . 3_545 ? O6 I2 K2 34.3(4) . 3_545 ? O5 I2 K2 136.1(3) . 3_545 ? K2 I2 K2 176.14(16) . 3_545 ? K1 I2 K2 120.24(18) . 3_545 ? K1 I2 K2 54.56(9) 3 3_545 ? I1 O1 K2 112.2(6) . 3_445 ? I1 O1 K1 118.3(6) . 3_445 ? K2 O1 K1 97.1(3) 3_445 3_445 ? I1 O2 Co1 121.5(6) . 3_445 ? I1 O2 K2 94.7(4) . 3_445 ? Co1 O2 K2 102.5(3) 3_445 3_445 ? I1 O3 K1 116.1(4) . . ? I2 O4 K1 116.9(6) . . ? I2 O5 Co1 128.2(6) . . ? I2 O5 K2 108.5(4) . . ? Co1 O5 K2 111.3(5) . . ? I2 O6 K2 123.8(5) . 3_545 ? I2 O6 K1 117.5(6) . 3 ? K2 O6 K1 82.9(3) 3_545 3 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.994 _refine_diff_density_min -1.494 _refine_diff_density_rms 0.270 #===end data_comp3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 I4 K2 O14 Zn' _chemical_formula_weight 879.20 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' 'H' 'H' 0.0000 0.0000 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.289(4) _cell_length_b 7.733(8) _cell_length_c 11.080(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.12(3) _cell_angle_gamma 90.00 _cell_volume 710.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 526 _cell_measurement_theta_min 3.0659 _cell_measurement_theta_max 27.4642 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 11.078 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.5671 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury2 _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2626 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 27.44 _reflns_number_total 1193 _reflns_number_gt 1186 _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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0057(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 0.04(4) _refine_ls_number_reflns 1193 _refine_ls_number_parameters 100 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0453 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _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 0.0000 -0.8714(5) 0.0000 0.0183(8) Uani 1 2 d S . . K2 K 0.0000 -0.3423(6) 0.0000 0.0204(8) Uani 1 2 d S . . Zn1 Zn 0.5000 -0.4161(3) 0.0000 0.0139(3) Uani 1 2 d S . . I1 I -0.23907(6) -1.09112(8) 0.27879(4) 0.01097(13) Uani 1 1 d . . . I2 I 0.25225(7) -0.60232(9) 0.23821(4) 0.01147(13) Uani 1 1 d . . . O1 O -0.4377(6) -1.1044(12) 0.3439(5) 0.0195(12) Uani 1 1 d . . . O2 O -0.1703(7) -0.8954(8) 0.3586(5) 0.0165(13) Uani 1 1 d . . . O3 O -0.2816(7) -0.9918(8) 0.1363(5) 0.0181(14) Uani 1 1 d . . . O4 O 0.2710(6) -0.7905(9) 0.1416(6) 0.0154(14) Uani 1 1 d . . . O5 O 0.2947(7) -0.4380(8) 0.1252(6) 0.0155(15) Uani 1 1 d . . . O6 O 0.4426(6) -0.6129(10) 0.3181(5) 0.0154(12) Uani 1 1 d . . . O1W O 0.5000 -0.6840(14) 0.0000 0.030(2) Uani 1 2 d S . . H1WA H 0.5749 -0.7207 -0.0457 0.045 Uiso 0.50 1 d PR . . H1WB H 0.4096 -0.7207 -0.0258 0.045 Uiso 0.50 1 d PR . . O2W O 0.5000 -0.1551(12) 0.0000 0.036(3) Uani 1 2 d S . . H2WA H 0.4096 -0.1185 -0.0258 0.054 Uiso 0.50 1 d PR . . H2WB H 0.5156 -0.1185 0.0714 0.054 Uiso 0.50 1 d PR . . 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 0.0216(14) 0.0162(19) 0.0170(17) 0.000 -0.0019(15) 0.000 K2 0.0301(17) 0.0143(15) 0.0168(15) 0.000 -0.001(2) 0.000 Zn1 0.0163(6) 0.0094(6) 0.0161(8) 0.000 -0.0032(8) 0.000 I1 0.01081(19) 0.0093(3) 0.0128(2) 0.0000(3) 0.0010(2) -0.0006(3) I2 0.0102(2) 0.0125(3) 0.0117(2) 0.0006(4) 0.0017(3) 0.0000(4) O1 0.013(2) 0.022(3) 0.023(3) -0.007(4) 0.003(2) 0.003(3) O2 0.017(3) 0.010(3) 0.022(3) -0.007(3) -0.006(2) 0.000(3) O3 0.024(3) 0.016(3) 0.014(3) 0.005(2) -0.007(3) -0.005(2) O4 0.019(3) 0.013(3) 0.015(3) -0.006(3) 0.003(3) -0.004(3) O5 0.018(3) 0.012(3) 0.017(3) 0.000(3) 0.007(3) 0.006(2) O6 0.0114(19) 0.018(3) 0.017(3) 0.004(4) -0.002(2) 0.000(3) O1W 0.029(4) 0.023(5) 0.038(7) 0.000 0.022(5) 0.000 O2W 0.055(6) 0.011(5) 0.042(7) 0.000 -0.029(6) 0.000 _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 2.743(9) 4_455 ? K1 O1 2.743(9) 3_554 ? K1 O6 2.787(7) 3_444 ? K1 O6 2.787(7) 4_545 ? K1 O4 2.808(6) . ? K1 O4 2.808(6) 2 ? K1 O3 2.934(6) 2 ? K1 O3 2.934(6) . ? K1 K2 3.641(5) 1_545 ? K1 I1 3.925(3) 4_455 ? K1 I1 3.925(3) 3_554 ? K1 I2 3.956(3) . ? K2 O1 2.715(8) 3_554 ? K2 O1 2.715(8) 4_455 ? K2 O6 2.726(7) 4 ? K2 O6 2.726(7) 3_454 ? K2 O5 2.903(7) 2 ? K2 O5 2.903(7) . ? K2 O2 3.180(6) 3_554 ? K2 O2 3.180(6) 4_455 ? K2 K1 3.641(5) 1_565 ? K2 I1 3.796(3) 3_554 ? K2 I1 3.796(3) 4_455 ? K2 I2 3.919(3) 2 ? Zn1 O2W 2.018(9) . ? Zn1 O1W 2.072(12) . ? Zn1 O2 2.113(6) 4 ? Zn1 O2 2.113(6) 3_554 ? Zn1 O5 2.204(6) 2_655 ? Zn1 O5 2.204(6) . ? I1 O3 1.790(6) . ? I1 O1 1.802(5) . ? I1 O2 1.842(6) . ? I1 K2 3.796(3) 3_445 ? I1 K1 3.925(3) 3_445 ? I2 O6 1.810(5) . ? I2 O4 1.814(7) . ? I2 O5 1.819(7) . ? I2 K1 3.974(3) 3 ? I2 K2 4.006(3) 3_545 ? O1 K2 2.715(8) 3_445 ? O1 K1 2.743(9) 3_445 ? O2 Zn1 2.113(6) 3_445 ? O2 K2 3.180(6) 3_445 ? O6 K2 2.726(7) 3_545 ? O6 K1 2.787(7) 3 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? 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 82.4(3) 4_455 3_554 ? O1 K1 O6 158.12(16) 4_455 3_444 ? O1 K1 O6 94.6(2) 3_554 3_444 ? O1 K1 O6 94.6(2) 4_455 4_545 ? O1 K1 O6 158.12(16) 3_554 4_545 ? O6 K1 O6 95.9(3) 3_444 4_545 ? O1 K1 O4 68.37(19) 4_455 . ? O1 K1 O4 91.9(2) 3_554 . ? O6 K1 O4 133.49(19) 3_444 . ? O6 K1 O4 67.06(19) 4_545 . ? O1 K1 O4 91.9(2) 4_455 2 ? O1 K1 O4 68.37(19) 3_554 2 ? O6 K1 O4 67.06(19) 3_444 2 ? O6 K1 O4 133.49(19) 4_545 2 ? O4 K1 O4 154.3(3) . 2 ? O1 K1 O3 135.58(18) 4_455 2 ? O1 K1 O3 76.31(18) 3_554 2 ? O6 K1 O3 63.26(16) 3_444 2 ? O6 K1 O3 91.43(19) 4_545 2 ? O4 K1 O3 73.85(18) . 2 ? O4 K1 O3 114.81(19) 2 2 ? O1 K1 O3 76.31(18) 4_455 . ? O1 K1 O3 135.58(18) 3_554 . ? O6 K1 O3 91.43(19) 3_444 . ? O6 K1 O3 63.26(16) 4_545 . ? O4 K1 O3 114.81(19) . . ? O4 K1 O3 73.85(18) 2 . ? O3 K1 O3 143.0(3) 2 . ? O1 K1 K2 138.82(16) 4_455 1_545 ? O1 K1 K2 138.82(16) 3_554 1_545 ? O6 K1 K2 47.95(15) 3_444 1_545 ? O6 K1 K2 47.95(15) 4_545 1_545 ? O4 K1 K2 102.87(17) . 1_545 ? O4 K1 K2 102.87(17) 2 1_545 ? O3 K1 K2 71.50(13) 2 1_545 ? O3 K1 K2 71.50(13) . 1_545 ? O1 K1 I1 23.93(11) 4_455 4_455 ? O1 K1 I1 94.74(19) 3_554 4_455 ? O6 K1 I1 136.71(11) 3_444 4_455 ? O6 K1 I1 90.68(15) 4_545 4_455 ? O4 K1 I1 88.25(16) . 4_455 ? O4 K1 I1 77.55(16) 2 4_455 ? O3 K1 I1 159.48(14) 2 4_455 ? O3 K1 I1 54.12(13) . 4_455 ? K2 K1 I1 123.52(6) 1_545 4_455 ? O1 K1 I1 94.74(19) 4_455 3_554 ? O1 K1 I1 23.93(11) 3_554 3_554 ? O6 K1 I1 90.68(15) 3_444 3_554 ? O6 K1 I1 136.71(11) 4_545 3_554 ? O4 K1 I1 77.55(16) . 3_554 ? O4 K1 I1 88.25(16) 2 3_554 ? O3 K1 I1 54.12(13) 2 3_554 ? O3 K1 I1 159.48(14) . 3_554 ? K2 K1 I1 123.52(6) 1_545 3_554 ? I1 K1 I1 112.96(12) 4_455 3_554 ? O1 K1 I2 44.20(11) 4_455 . ? O1 K1 I2 85.69(16) 3_554 . ? O6 K1 I2 157.52(11) 3_444 . ? O6 K1 I2 77.33(15) 4_545 . ? O4 K1 I2 24.33(14) . . ? O4 K1 I2 132.59(19) 2 . ? O3 K1 I2 95.19(12) 2 . ? O3 K1 I2 104.09(12) . . ? K2 K1 I2 121.74(6) 1_545 . ? I1 K1 I2 65.42(6) 4_455 . ? I1 K1 I2 80.50(9) 3_554 . ? O1 K2 O1 83.4(3) 3_554 4_455 ? O1 K2 O6 157.49(16) 3_554 4 ? O1 K2 O6 92.7(2) 4_455 4 ? O1 K2 O6 92.7(2) 3_554 3_454 ? O1 K2 O6 157.49(16) 4_455 3_454 ? O6 K2 O6 98.8(3) 4 3_454 ? O1 K2 O5 70.49(16) 3_554 2 ? O1 K2 O5 87.3(2) 4_455 2 ? O6 K2 O5 131.66(17) 4 2 ? O6 K2 O5 70.57(18) 3_454 2 ? O1 K2 O5 87.3(2) 3_554 . ? O1 K2 O5 70.49(16) 4_455 . ? O6 K2 O5 70.57(18) 4 . ? O6 K2 O5 131.66(17) 3_454 . ? O5 K2 O5 150.4(3) 2 . ? O1 K2 O2 54.89(17) 3_554 3_554 ? O1 K2 O2 112.47(19) 4_455 3_554 ? O6 K2 O2 107.44(16) 4 3_554 ? O6 K2 O2 82.45(17) 3_454 3_554 ? O5 K2 O2 117.05(17) 2 3_554 ? O5 K2 O2 58.61(17) . 3_554 ? O1 K2 O2 112.47(19) 3_554 4_455 ? O1 K2 O2 54.89(17) 4_455 4_455 ? O6 K2 O2 82.45(17) 4 4_455 ? O6 K2 O2 107.44(16) 3_454 4_455 ? O5 K2 O2 58.61(17) 2 4_455 ? O5 K2 O2 117.05(17) . 4_455 ? O2 K2 O2 165.1(3) 3_554 4_455 ? O1 K2 K1 138.30(17) 3_554 1_565 ? O1 K2 K1 138.30(17) 4_455 1_565 ? O6 K2 K1 49.40(15) 4 1_565 ? O6 K2 K1 49.40(15) 3_454 1_565 ? O5 K2 K1 104.78(14) 2 1_565 ? O5 K2 K1 104.78(14) . 1_565 ? O2 K2 K1 97.43(13) 3_554 1_565 ? O2 K2 K1 97.43(13) 4_455 1_565 ? O1 K2 I1 25.96(13) 3_554 3_554 ? O1 K2 I1 98.2(2) 4_455 3_554 ? O6 K2 I1 135.11(11) 4 3_554 ? O6 K2 I1 87.21(15) 3_454 3_554 ? O5 K2 I1 92.42(15) 2 3_554 ? O5 K2 I1 72.49(15) . 3_554 ? O2 K2 I1 28.94(11) 3_554 3_554 ? O2 K2 I1 138.08(16) 4_455 3_554 ? K1 K2 I1 120.46(7) 1_565 3_554 ? O1 K2 I1 98.2(2) 3_554 4_455 ? O1 K2 I1 25.96(13) 4_455 4_455 ? O6 K2 I1 87.21(15) 4 4_455 ? O6 K2 I1 135.11(11) 3_454 4_455 ? O5 K2 I1 72.49(15) 2 4_455 ? O5 K2 I1 92.42(14) . 4_455 ? O2 K2 I1 138.08(16) 3_554 4_455 ? O2 K2 I1 28.94(11) 4_455 4_455 ? K1 K2 I1 120.46(7) 1_565 4_455 ? I1 K2 I1 119.08(14) 3_554 4_455 ? O1 K2 I2 44.74(11) 3_554 2 ? O1 K2 I2 86.79(18) 4_455 2 ? O6 K2 I2 157.50(11) 4 2 ? O6 K2 I2 75.16(15) 3_454 2 ? O5 K2 I2 25.84(12) 2 2 ? O5 K2 I2 129.66(18) . 2 ? O2 K2 I2 93.42(12) 3_554 2 ? O2 K2 I2 78.91(12) 4_455 2 ? K1 K2 I2 120.87(7) 1_565 2 ? I1 K2 I2 66.98(7) 3_554 2 ? I1 K2 I2 82.58(9) 4_455 2 ? O2W Zn1 O1W 180.000(1) . . ? O2W Zn1 O2 85.66(18) . 4 ? O1W Zn1 O2 94.34(18) . 4 ? O2W Zn1 O2 85.66(18) . 3_554 ? O1W Zn1 O2 94.34(18) . 3_554 ? O2 Zn1 O2 171.3(4) 4 3_554 ? O2W Zn1 O5 94.42(16) . 2_655 ? O1W Zn1 O5 85.58(16) . 2_655 ? O2 Zn1 O5 87.5(2) 4 2_655 ? O2 Zn1 O5 93.1(2) 3_554 2_655 ? O2W Zn1 O5 94.42(16) . . ? O1W Zn1 O5 85.58(16) . . ? O2 Zn1 O5 93.1(2) 4 . ? O2 Zn1 O5 87.5(2) 3_554 . ? O5 Zn1 O5 171.2(3) 2_655 . ? O3 I1 O1 101.5(3) . . ? O3 I1 O2 97.5(3) . . ? O1 I1 O2 97.9(3) . . ? O3 I1 K2 103.9(2) . 3_445 ? O1 I1 K2 41.3(3) . 3_445 ? O2 I1 K2 56.63(19) . 3_445 ? O3 I1 K1 132.85(19) . 3_445 ? O1 I1 K1 38.1(3) . 3_445 ? O2 I1 K1 108.9(2) . 3_445 ? K2 I1 K1 63.98(8) 3_445 3_445 ? O3 I1 K1 40.76(19) . . ? O1 I1 K1 141.1(2) . . ? O2 I1 K1 82.5(2) . . ? K2 I1 K1 124.10(12) 3_445 . ? K1 I1 K1 168.44(8) 3_445 . ? O6 I2 O4 100.2(3) . . ? O6 I2 O5 101.4(3) . . ? O4 I2 O5 97.9(3) . . ? O6 I2 K2 144.7(2) . . ? O4 I2 K2 93.5(2) . . ? O5 I2 K2 44.1(2) . . ? O6 I2 K1 139.6(2) . . ? O4 I2 K1 39.62(19) . . ? O5 I2 K1 90.6(2) . . ? K2 I2 K1 62.61(8) . . ? O6 I2 K1 38.2(2) . 3 ? O4 I2 K1 138.29(19) . 3 ? O5 I2 K1 95.1(2) . 3 ? K2 I2 K1 122.36(11) . 3 ? K1 I2 K1 174.27(8) . 3 ? O6 I2 K2 34.9(2) . 3_545 ? O4 I2 K2 90.7(2) . 3_545 ? O5 I2 K2 136.2(2) . 3_545 ? K2 I2 K2 175.75(9) . 3_545 ? K1 I2 K2 120.59(11) . 3_545 ? K1 I2 K2 54.28(7) 3 3_545 ? I1 O1 K2 112.8(3) . 3_445 ? I1 O1 K1 117.9(3) . 3_445 ? K2 O1 K1 97.1(2) 3_445 3_445 ? I1 O2 Zn1 119.9(3) . 3_445 ? I1 O2 K2 94.4(2) . 3_445 ? Zn1 O2 K2 102.6(2) 3_445 3_445 ? I1 O3 K1 115.8(3) . . ? I2 O4 K1 116.0(3) . . ? I2 O5 Zn1 129.6(3) . . ? I2 O5 K2 110.1(3) . . ? Zn1 O5 K2 109.3(3) . . ? I2 O6 K2 122.8(3) . 3_545 ? I2 O6 K1 118.1(3) . 3 ? K2 O6 K1 82.65(18) 3_545 3 ? Zn1 O1W H1WA 109.5 . . ? Zn1 O1W H1WB 109.5 . . ? H1WA O1W H1WB 109.5 . . ? Zn1 O2W H2WA 109.5 . . ? Zn1 O2W H2WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.761 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.195 #===end data_comp4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H4 I4 K2 Mg O14' _chemical_formula_weight 838.14 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' 'H' 'H' 0.0000 0.0000 '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' 'Mg' 'Mg' 0.0486 0.0363 '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 monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.305(9) _cell_length_b 7.760(8) _cell_length_c 11.101(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.009(18) _cell_angle_gamma 90.00 _cell_volume 715.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 349 _cell_measurement_theta_min 3.0629 _cell_measurement_theta_max 27.4526 _exptl_crystal_description 'rectangle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.891 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 9.405 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.4358 _exptl_absorpt_correction_T_max 1.0000 _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 Mercury2 _diffrn_measurement_method 'CCD_Profile_fitting' _diffrn_detector_area_resol_mean 13.6612 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2785 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.77 _reflns_number_total 1650 _reflns_number_gt 1541 _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^)+(0.1192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _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 0.05(8) _refine_ls_number_reflns 1650 _refine_ls_number_parameters 98 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 1.0000 1.8678(8) 1.0000 0.0247(10) Uani 1 2 d S . . K2 K 1.0000 1.3402(8) 1.0000 0.0289(13) Uani 1 2 d S . . Mg1 Mg 0.5000 1.4170(10) 1.0000 0.0238(16) Uani 1 2 d S . . I1 I 1.23971(7) 2.09030(18) 0.72180(6) 0.0177(3) Uani 1 1 d . . . I2 I 0.74771(7) 1.59942(5) 0.76247(7) 0.0177(3) Uani 1 1 d . . . O1 O 1.4388(9) 2.0988(17) 0.6555(8) 0.0259(18) Uani 1 1 d . . . O2 O 1.1698(12) 1.9005(12) 0.6417(9) 0.025(2) Uani 1 1 d . . . O3 O 1.2783(12) 1.9904(15) 0.8643(9) 0.029(2) Uani 1 1 d . . . O4 O 0.7270(12) 1.7921(15) 0.8579(11) 0.025(2) Uani 1 1 d . . . O5 O 0.7056(13) 1.4380(13) 0.8767(9) 0.022(2) Uani 1 1 d . . . O6 O 0.5588(10) 1.6128(17) 0.6815(8) 0.028(2) Uani 1 1 d . . . O1W O 0.5000 1.6815(19) 1.0000 0.029(3) Uani 1 2 d S . . H1WA H 0.4252 1.7181 1.0457 0.044 Uiso 0.50 1 d PR . . H1WB H 0.5904 1.7181 1.0257 0.044 Uiso 0.50 1 d PR . . O2W O 0.5000 1.155(2) 1.0000 0.041(4) Uani 1 2 d S . . H2WA H 0.5904 1.1180 1.0257 0.061 Uiso 0.50 1 d PR . . H2WB H 0.4844 1.1180 0.9286 0.061 Uiso 0.50 1 d PR . . 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 0.028(3) 0.023(2) 0.022(2) 0.000 0.0008(18) 0.000 K2 0.043(3) 0.023(3) 0.021(2) 0.000 -0.004(2) 0.000 Mg1 0.020(3) 0.019(3) 0.032(4) 0.000 0.005(3) 0.000 I1 0.0187(4) 0.0171(5) 0.0174(4) 0.0002(6) 0.0040(3) -0.0007(4) I2 0.0179(4) 0.0182(6) 0.0169(4) 0.0021(6) 0.0052(3) 0.0001(4) O1 0.022(4) 0.027(4) 0.029(4) -0.004(6) -0.002(3) -0.001(5) O2 0.031(5) 0.021(5) 0.023(5) -0.002(4) 0.004(4) -0.002(4) O3 0.037(6) 0.023(5) 0.026(5) 0.012(5) 0.003(5) 0.003(4) O4 0.020(5) 0.027(5) 0.027(5) -0.002(5) -0.004(4) 0.000(5) O5 0.027(6) 0.023(5) 0.017(5) 0.007(4) 0.007(4) -0.003(4) O6 0.023(4) 0.037(6) 0.025(4) 0.005(5) -0.007(3) 0.000(5) O1W 0.042(8) 0.021(7) 0.026(7) 0.000 0.017(7) 0.000 O2W 0.047(9) 0.034(9) 0.042(9) 0.000 -0.023(8) 0.000 _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 2.756(12) 4_746 ? K1 O1 2.756(13) 3_445 ? K1 O6 2.813(12) 3 ? K1 O6 2.813(12) 4_656 ? K1 O4 2.824(11) . ? K1 O4 2.824(11) 2_757 ? K1 O3 2.918(10) . ? K1 O3 2.918(10) 2_757 ? K1 K2 3.666(7) 1_565 ? K1 I1 3.921(5) 4_746 ? K1 I1 3.921(5) 3_445 ? K1 I2 3.959(4) . ? K2 O1 2.696(12) 3_445 ? K2 O1 2.696(12) 4_746 ? K2 O6 2.723(11) 4_646 ? K2 O6 2.722(11) 3_545 ? K2 O5 2.903(12) 2_757 ? K2 O5 2.903(12) . ? K2 O2 3.196(10) 4_746 ? K2 O2 3.196(10) 3_445 ? K2 K1 3.666(7) 1_545 ? K2 I1 3.808(4) 3_445 ? K2 I1 3.808(4) 4_746 ? K2 I2 3.923(4) 2_757 ? Mg1 O2W 2.036(18) . ? Mg1 O1W 2.053(17) . ? Mg1 O2 2.116(11) 4_646 ? Mg1 O2 2.116(11) 3_445 ? Mg1 O5 2.195(10) . ? Mg1 O5 2.195(10) 2_657 ? Mg1 K2 4.195(5) 1_455 ? I1 O3 1.791(10) . ? I1 O1 1.811(8) . ? I1 O2 1.816(10) . ? I1 K2 3.808(4) 3_554 ? I1 K1 3.921(5) 3_554 ? I2 O6 1.811(8) . ? I2 O5 1.816(10) . ? I2 O4 1.840(12) . ? I2 K1 3.994(4) 3_444 ? I2 K2 4.026(4) 3_454 ? O1 K2 2.696(12) 3_554 ? O1 K1 2.756(12) 3_554 ? O2 Mg1 2.116(10) 3_554 ? O2 K2 3.196(10) 3_554 ? O6 K2 2.722(11) 3_454 ? O6 K1 2.813(12) 3_444 ? O1W H1WA 0.8510 . ? O1W H1WB 0.8523 . ? O2W H2WA 0.8523 . ? O2W H2WB 0.8520 . ? 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 81.5(5) 4_746 3_445 ? O1 K1 O6 158.2(3) 4_746 3 ? O1 K1 O6 95.5(3) 3_445 3 ? O1 K1 O6 95.5(3) 4_746 4_656 ? O1 K1 O6 158.2(3) 3_445 4_656 ? O6 K1 O6 94.9(5) 3 4_656 ? O1 K1 O4 68.9(3) 4_746 . ? O1 K1 O4 92.5(3) 3_445 . ? O6 K1 O4 132.9(3) 3 . ? O6 K1 O4 66.5(3) 4_656 . ? O1 K1 O4 92.5(3) 4_746 2_757 ? O1 K1 O4 68.9(3) 3_445 2_757 ? O6 K1 O4 66.5(3) 3 2_757 ? O6 K1 O4 132.9(3) 4_656 2_757 ? O4 K1 O4 156.0(5) . 2_757 ? O1 K1 O3 77.1(3) 4_746 . ? O1 K1 O3 135.7(3) 3_445 . ? O6 K1 O3 90.7(3) 3 . ? O6 K1 O3 63.1(3) 4_656 . ? O4 K1 O3 114.5(3) . . ? O4 K1 O3 73.8(3) 2_757 . ? O1 K1 O3 135.7(3) 4_746 2_757 ? O1 K1 O3 77.1(3) 3_445 2_757 ? O6 K1 O3 63.1(3) 3 2_757 ? O6 K1 O3 90.7(3) 4_656 2_757 ? O4 K1 O3 73.8(3) . 2_757 ? O4 K1 O3 114.5(3) 2_757 2_757 ? O3 K1 O3 141.9(5) . 2_757 ? O1 K1 K2 139.2(2) 4_746 1_565 ? O1 K1 K2 139.2(2) 3_445 1_565 ? O6 K1 K2 47.5(2) 3 1_565 ? O6 K1 K2 47.5(2) 4_656 1_565 ? O4 K1 K2 102.0(3) . 1_565 ? O4 K1 K2 102.0(3) 2_757 1_565 ? O3 K1 K2 71.0(3) . 1_565 ? O3 K1 K2 71.0(3) 2_757 1_565 ? O1 K1 I1 24.36(18) 4_746 4_746 ? O1 K1 I1 94.5(3) 3_445 4_746 ? O6 K1 I1 136.49(18) 3 4_746 ? O6 K1 I1 91.0(2) 4_656 4_746 ? O4 K1 I1 88.7(3) . 4_746 ? O4 K1 I1 78.1(3) 2_757 4_746 ? O3 K1 I1 54.4(2) . 4_746 ? O3 K1 I1 160.0(3) 2_757 4_746 ? K2 K1 I1 123.31(9) 1_565 4_746 ? O1 K1 I1 94.5(3) 4_746 3_445 ? O1 K1 I1 24.36(18) 3_445 3_445 ? O6 K1 I1 91.0(2) 3 3_445 ? O6 K1 I1 136.49(18) 4_656 3_445 ? O4 K1 I1 78.1(3) . 3_445 ? O4 K1 I1 88.7(3) 2_757 3_445 ? O3 K1 I1 160.0(3) . 3_445 ? O3 K1 I1 54.4(2) 2_757 3_445 ? K2 K1 I1 123.31(9) 1_565 3_445 ? I1 K1 I1 113.38(19) 4_746 3_445 ? O1 K1 I2 44.12(17) 4_746 . ? O1 K1 I2 85.5(2) 3_445 . ? O6 K1 I2 157.56(19) 3 . ? O6 K1 I2 77.7(2) 4_656 . ? O4 K1 I2 25.0(2) . . ? O4 K1 I2 133.4(3) 2_757 . ? O3 K1 I2 104.3(2) . . ? O3 K1 I2 95.5(2) 2_757 . ? K2 K1 I2 121.73(9) 1_565 . ? I1 K1 I2 65.46(10) 4_746 . ? I1 K1 I2 80.65(12) 3_445 . ? O1 K2 O1 83.8(5) 3_445 4_746 ? O1 K2 O6 157.3(3) 3_445 4_646 ? O1 K2 O6 92.4(3) 4_746 4_646 ? O1 K2 O6 92.4(3) 3_445 3_545 ? O1 K2 O6 157.3(3) 4_746 3_545 ? O6 K2 O6 99.2(5) 4_646 3_545 ? O1 K2 O5 70.3(3) 3_445 2_757 ? O1 K2 O5 87.1(3) 4_746 2_757 ? O6 K2 O5 132.0(3) 4_646 2_757 ? O6 K2 O5 70.7(3) 3_545 2_757 ? O1 K2 O5 87.1(3) 3_445 . ? O1 K2 O5 70.3(3) 4_746 . ? O6 K2 O5 70.7(3) 4_646 . ? O6 K2 O5 132.0(3) 3_545 . ? O5 K2 O5 149.7(4) 2_757 . ? O1 K2 O2 111.6(3) 3_445 4_746 ? O1 K2 O2 54.1(3) 4_746 4_746 ? O6 K2 O2 83.4(3) 4_646 4_746 ? O6 K2 O2 107.8(3) 3_545 4_746 ? O5 K2 O2 58.1(3) 2_757 4_746 ? O5 K2 O2 116.9(3) . 4_746 ? O1 K2 O2 54.1(3) 3_445 3_445 ? O1 K2 O2 111.6(3) 4_746 3_445 ? O6 K2 O2 107.8(3) 4_646 3_445 ? O6 K2 O2 83.4(3) 3_545 3_445 ? O5 K2 O2 116.9(3) 2_757 3_445 ? O5 K2 O2 58.1(3) . 3_445 ? O2 K2 O2 163.2(4) 4_746 3_445 ? O1 K2 K1 138.1(2) 3_445 1_545 ? O1 K2 K1 138.1(2) 4_746 1_545 ? O6 K2 K1 49.6(3) 4_646 1_545 ? O6 K2 K1 49.6(3) 3_545 1_545 ? O5 K2 K1 105.2(2) 2_757 1_545 ? O5 K2 K1 105.2(2) . 1_545 ? O2 K2 K1 98.4(2) 4_746 1_545 ? O2 K2 K1 98.4(2) 3_445 1_545 ? O1 K2 I1 25.77(19) 3_445 3_445 ? O1 K2 I1 98.1(3) 4_746 3_445 ? O6 K2 I1 134.99(19) 4_646 3_445 ? O6 K2 I1 87.3(2) 3_545 3_445 ? O5 K2 I1 92.3(2) 2_757 3_445 ? O5 K2 I1 72.2(2) . 3_445 ? O2 K2 I1 136.9(3) 4_746 3_445 ? O2 K2 I1 28.37(18) 3_445 3_445 ? K1 K2 I1 120.64(10) 1_545 3_445 ? O1 K2 I1 98.1(3) 3_445 4_746 ? O1 K2 I1 25.77(19) 4_746 4_746 ? O6 K2 I1 87.3(2) 4_646 4_746 ? O6 K2 I1 134.99(19) 3_545 4_746 ? O5 K2 I1 72.2(2) 2_757 4_746 ? O5 K2 I1 92.3(2) . 4_746 ? O2 K2 I1 28.37(17) 4_746 4_746 ? O2 K2 I1 136.9(3) 3_445 4_746 ? K1 K2 I1 120.64(10) 1_545 4_746 ? I1 K2 I1 118.72(19) 3_445 4_746 ? O1 K2 I2 44.64(17) 3_445 2_757 ? O1 K2 I2 87.0(2) 4_746 2_757 ? O6 K2 I2 157.76(19) 4_646 2_757 ? O6 K2 I2 74.9(2) 3_545 2_757 ? O5 K2 I2 25.74(18) 2_757 2_757 ? O5 K2 I2 129.2(3) . 2_757 ? O2 K2 I2 78.3(2) 4_746 2_757 ? O2 K2 I2 93.0(2) 3_445 2_757 ? K1 K2 I2 120.85(9) 1_545 2_757 ? I1 K2 I2 66.88(10) 3_445 2_757 ? I1 K2 I2 82.53(12) 4_746 2_757 ? O2W Mg1 O1W 180.000(10) . . ? O2W Mg1 O2 86.5(3) . 4_646 ? O1W Mg1 O2 93.5(3) . 4_646 ? O2W Mg1 O2 86.5(3) . 3_445 ? O1W Mg1 O2 93.5(3) . 3_445 ? O2 Mg1 O2 173.1(6) 4_646 3_445 ? O2W Mg1 O5 94.3(3) . . ? O1W Mg1 O5 85.7(3) . . ? O2 Mg1 O5 93.4(4) 4_646 . ? O2 Mg1 O5 87.1(4) 3_445 . ? O2W Mg1 O5 94.3(3) . 2_657 ? O1W Mg1 O5 85.7(3) . 2_657 ? O2 Mg1 O5 87.1(4) 4_646 2_657 ? O2 Mg1 O5 93.4(4) 3_445 2_657 ? O5 Mg1 O5 171.5(7) . 2_657 ? O2W Mg1 K2 81.83(14) . 1_455 ? O1W Mg1 K2 98.17(14) . 1_455 ? O2 Mg1 K2 48.1(3) 4_646 1_455 ? O2 Mg1 K2 130.6(3) 3_445 1_455 ? O5 Mg1 K2 141.3(3) . 1_455 ? O5 Mg1 K2 40.6(3) 2_657 1_455 ? O2W Mg1 K2 81.83(14) . . ? O1W Mg1 K2 98.17(14) . . ? O2 Mg1 K2 130.6(3) 4_646 . ? O2 Mg1 K2 48.1(3) 3_445 . ? O5 Mg1 K2 40.6(3) . . ? O5 Mg1 K2 141.3(3) 2_657 . ? K2 Mg1 K2 163.7(3) 1_455 . ? O3 I1 O1 102.2(5) . . ? O3 I1 O2 98.0(5) . . ? O1 I1 O2 97.0(5) . . ? O3 I1 K2 104.4(4) . 3_554 ? O1 I1 K2 40.3(4) . 3_554 ? O2 I1 K2 56.7(3) . 3_554 ? O3 I1 K1 133.9(3) . 3_554 ? O1 I1 K1 38.9(4) . 3_554 ? O2 I1 K1 108.3(3) . 3_554 ? K2 I1 K1 63.95(10) 3_554 3_554 ? O3 I1 K1 39.8(3) . . ? O1 I1 K1 140.6(4) . . ? O2 I1 K1 82.6(3) . . ? K2 I1 K1 123.60(17) 3_554 . ? K1 I1 K1 169.01(13) 3_554 . ? O6 I2 O5 102.7(5) . . ? O6 I2 O4 99.1(5) . . ? O5 I2 O4 98.1(5) . . ? O6 I2 K2 145.7(4) . . ? O5 I2 K2 43.9(4) . . ? O4 I2 K2 94.6(4) . . ? O6 I2 K1 139.4(4) . . ? O5 I2 K1 90.0(4) . . ? O4 I2 K1 40.4(3) . . ? K2 I2 K1 62.58(10) . . ? O6 I2 K1 38.5(4) . 3_444 ? O5 I2 K1 95.7(4) . 3_444 ? O4 I2 K1 137.5(3) . 3_444 ? K2 I2 K1 122.32(16) . 3_444 ? K1 I2 K1 174.27(14) . 3_444 ? O6 I2 K2 34.1(4) . 3_454 ? O5 I2 K2 136.6(4) . 3_454 ? O4 I2 K2 89.5(4) . 3_454 ? K2 I2 K2 175.73(12) . 3_454 ? K1 I2 K2 120.54(16) . 3_454 ? K1 I2 K2 54.40(10) 3_444 3_454 ? I1 O1 K2 113.9(5) . 3_554 ? I1 O1 K1 116.8(5) . 3_554 ? K2 O1 K1 97.3(3) 3_554 3_554 ? I1 O2 Mg1 121.9(5) . 3_554 ? I1 O2 K2 94.9(4) . 3_554 ? Mg1 O2 K2 102.4(4) 3_554 3_554 ? I1 O3 K1 117.1(5) . . ? I2 O4 K1 114.6(5) . . ? I2 O5 Mg1 129.5(6) . . ? I2 O5 K2 110.3(5) . . ? Mg1 O5 K2 110.0(4) . . ? I2 O6 K2 124.0(5) . 3_454 ? I2 O6 K1 117.8(5) . 3_444 ? K2 O6 K1 82.9(3) 3_454 3_444 ? Mg1 O1W H1WA 109.5 . . ? Mg1 O1W H1WB 109.5 . . ? H1WA O1W H1WB 109.4 . . ? Mg1 O2W H2WA 109.5 . . ? Mg1 O2W H2WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.520 _refine_diff_density_min -3.220 _refine_diff_density_rms 0.478 #===end