# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Wolfgang H. Runde' 'Amanda C. Bean' 'Brian L. Scott' _publ_contact_author_name 'Wolfgang H Runde' _publ_contact_author_address ; Environmental and Chemistry Divisions Los Alamos National Laboratory Los Alamos New Mexico 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email RUNDE@LANL.GOV _publ_section_title ; Synthesis and characterization of a channel framework in K3Am3(I03)12.HIO3 ; data_ccd681 _database_code_CSD 209298 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H Am3 I13 K3 O39' _chemical_formula_weight 3121.01 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' I I -0.4742 1.8119 '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' Am Am -7.8986 4.5125 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 22.096(6) _cell_length_b 22.096(6) _cell_length_c 13.436(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5681(3) _cell_formula_units_Z 6 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8064 _exptl_absorpt_coefficient_mu 17.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.07 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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/CCD' _diffrn_measurement_method '/w and /f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 8749 _diffrn_reflns_av_R_equivalents 0.0908 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1930 _reflns_number_gt 1804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material '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. Light atoms (O and K) were refined isotropically due to absorption problems ; _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^)+(0.0566P)^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 mixed _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 0.00(7) _refine_ls_number_reflns 1930 _refine_ls_number_parameters 106 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1328 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.545 _refine_ls_restrained_S_all 1.544 _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 Am1 Am 0.63065(5) 0.49707(5) 0.85926(8) 0.0102(3) Uani 1 1 d . . . K1 K 0.5528(3) 0.3231(3) 1.0700(6) 0.0113(14) Uiso 1 1 d . . . I1 I 0.6667 0.3333 0.8753(6) 0.070(2) Uani 1 3 d S . . I2 I 0.55008(11) 0.47729(10) 1.11671(17) 0.0147(5) Uani 1 1 d . . . I3 I 0.78254(11) 0.62195(10) 1.04311(16) 0.0133(5) Uani 1 1 d . . . I4 I 0.63386(10) 0.66219(10) 0.98632(17) 0.0143(5) Uani 1 1 d . . . I5 I 0.47899(13) 0.29004(13) 0.7918(2) 0.0277(6) Uani 1 1 d . . . O1 O 0.672(2) 0.405(2) 0.960(3) 0.075(11) Uiso 1 1 d . . . O2 O 0.4691(13) 0.4676(14) 1.081(2) 0.030(6) Uiso 1 1 d . . . O3 O 0.5693(12) 0.4393(12) 1.0109(19) 0.025(6) Uiso 1 1 d . . . O4 O 0.5179(12) 0.3931(12) 1.1815(18) 0.021(5) Uiso 1 1 d . . . O5 O 0.8522(11) 0.6949(11) 0.9772(17) 0.014(5) Uiso 1 1 d . . . O6 O 0.8308(12) 0.5827(12) 1.0882(18) 0.021(5) Uiso 1 1 d . . . O7 O 0.7458(11) 0.5655(11) 0.9381(17) 0.014(5) Uiso 1 1 d . . . O8 O 0.7299(14) 0.7105(14) 0.997(2) 0.036(7) Uiso 1 1 d . . . O9 O 0.6265(10) 0.5768(10) 0.9824(17) 0.011(5) Uiso 1 1 d . . . O10 O 0.6096(12) 0.6623(11) 1.1137(18) 0.018(5) Uiso 1 1 d . . . O11 O 0.5579(17) 0.3632(17) 0.828(3) 0.050(8) Uiso 1 1 d . . . O12 O 0.4803(15) 0.3181(16) 0.667(3) 0.042(8) Uiso 1 1 d . . . O13 O 0.5179(14) 0.2344(13) 0.768(2) 0.034(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Am1 0.0075(5) 0.0109(6) 0.0098(6) -0.0020(5) 0.0006(5) 0.0028(5) I1 0.055(2) 0.055(2) 0.101(6) 0.000 0.000 0.0273(11) I2 0.0143(10) 0.0124(10) 0.0137(12) 0.0030(9) 0.0003(9) 0.0039(9) I3 0.0111(10) 0.0125(10) 0.0120(12) -0.0001(8) 0.0003(8) 0.0026(8) I4 0.0166(10) 0.0121(10) 0.0165(13) 0.0001(9) -0.0030(9) 0.0089(9) I5 0.0362(14) 0.0246(12) 0.0288(16) 0.0023(11) 0.0000(11) 0.0201(11) _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 Am1 O13 2.42(3) 3_665 ? Am1 O3 2.43(3) . ? Am1 O4 2.43(2) 4_664 ? Am1 O9 2.45(2) . ? Am1 O7 2.46(2) . ? Am1 O5 2.49(2) 12_454 ? Am1 O10 2.51(2) 14_654 ? Am1 O11 2.60(3) . ? Am1 O1 2.93(4) . ? Am1 K1 4.300(8) 4_664 ? Am1 K1 4.375(7) . ? K1 O1 2.40(4) 2_655 ? K1 O3 2.53(3) . ? K1 O4 2.53(2) . ? K1 O6 2.61(2) 2_655 ? K1 O1 2.75(4) . ? K1 O13 2.78(3) 6 ? K1 O12 3.35(3) 6 ? K1 O11 3.36(4) . ? K1 O7 3.42(2) 2_655 ? K1 I2 3.494(7) . ? K1 I1 3.557(10) . ? K1 I3 3.751(7) 2_655 ? I1 O1 1.92(4) 3_665 ? I1 O1 1.92(4) 2_655 ? I1 O1 1.92(4) . ? I1 K1 3.557(10) 2_655 ? I1 K1 3.557(10) 3_665 ? I2 O2 1.76(3) . ? I2 O3 1.81(3) . ? I2 O4 1.84(2) . ? I3 O6 1.78(2) . ? I3 O7 1.79(2) . ? I3 O5 1.81(2) . ? I3 K1 3.751(7) 3_665 ? I4 O10 1.79(2) . ? I4 O9 1.81(2) . ? I4 O8 1.84(3) . ? I5 O11 1.75(3) . ? I5 O12 1.78(3) . ? I5 O13 1.85(3) . ? I5 K1 3.936(8) 6_554 ? O1 K1 2.40(4) 3_665 ? O4 Am1 2.43(2) 4_665 ? O5 Am1 2.49(2) 18_554 ? O6 K1 2.61(2) 3_665 ? O7 K1 3.42(2) 3_665 ? O10 Am1 2.51(2) 9_565 ? O12 K1 3.35(3) 6_554 ? O13 Am1 2.42(3) 2_655 ? O13 K1 2.78(3) 6_554 ? 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 O13 Am1 O3 128.6(9) 3_665 . ? O13 Am1 O4 67.2(8) 3_665 4_664 ? O3 Am1 O4 136.7(8) . 4_664 ? O13 Am1 O9 139.1(8) 3_665 . ? O3 Am1 O9 66.4(7) . . ? O4 Am1 O9 132.6(7) 4_664 . ? O13 Am1 O7 70.2(8) 3_665 . ? O3 Am1 O7 95.5(8) . . ? O4 Am1 O7 126.4(8) 4_664 . ? O9 Am1 O7 70.5(7) . . ? O13 Am1 O5 133.0(8) 3_665 12_454 ? O3 Am1 O5 85.0(8) . 12_454 ? O4 Am1 O5 66.0(7) 4_664 12_454 ? O9 Am1 O5 80.0(7) . 12_454 ? O7 Am1 O5 147.3(7) . 12_454 ? O13 Am1 O10 91.5(8) 3_665 14_654 ? O3 Am1 O10 135.6(8) . 14_654 ? O4 Am1 O10 70.5(8) 4_664 14_654 ? O9 Am1 O10 70.5(7) . 14_654 ? O7 Am1 O10 79.8(7) . 14_654 ? O5 Am1 O10 77.3(7) 12_454 14_654 ? O13 Am1 O11 80.9(10) 3_665 . ? O3 Am1 O11 70.9(10) . . ? O4 Am1 O11 73.6(10) 4_664 . ? O9 Am1 O11 134.7(9) . . ? O7 Am1 O11 129.1(9) . . ? O5 Am1 O11 82.0(9) 12_454 . ? O10 Am1 O11 143.4(9) 14_654 . ? O13 Am1 O1 66.9(10) 3_665 . ? O3 Am1 O1 62.0(10) . . ? O4 Am1 O1 118.8(10) 4_664 . ? O9 Am1 O1 108.6(9) . . ? O7 Am1 O1 69.1(10) . . ? O5 Am1 O1 136.2(10) 12_454 . ? O10 Am1 O1 146.5(10) 14_654 . ? O11 Am1 O1 61.2(11) . . ? O13 Am1 K1 37.1(7) 3_665 4_664 ? O3 Am1 K1 140.0(6) . 4_664 ? O4 Am1 K1 30.7(5) 4_664 4_664 ? O9 Am1 K1 153.3(5) . 4_664 ? O7 Am1 K1 104.0(5) . 4_664 ? O5 Am1 K1 96.0(5) 12_454 4_664 ? O10 Am1 K1 82.8(5) 14_654 4_664 ? O11 Am1 K1 69.6(8) . 4_664 ? O1 Am1 K1 92.7(8) . 4_664 ? O13 Am1 K1 101.5(6) 3_665 . ? O3 Am1 K1 28.8(6) . . ? O4 Am1 K1 123.6(6) 4_664 . ? O9 Am1 K1 93.2(5) . . ? O7 Am1 K1 95.3(5) . . ? O5 Am1 K1 100.2(5) 12_454 . ? O10 Am1 K1 163.7(5) 14_654 . ? O11 Am1 K1 50.0(8) . . ? O1 Am1 K1 38.2(8) . . ? K1 Am1 K1 113.51(12) 4_664 . ? O1 K1 O3 116.2(12) 2_655 . ? O1 K1 O4 175.1(12) 2_655 . ? O3 K1 O4 60.0(8) . . ? O1 K1 O6 110.1(11) 2_655 2_655 ? O3 K1 O6 102.1(7) . 2_655 ? O4 K1 O6 74.3(7) . 2_655 ? O1 K1 O1 62.0(18) 2_655 . ? O3 K1 O1 63.6(10) . . ? O4 K1 O1 113.1(10) . . ? O6 K1 O1 151.7(11) 2_655 . ? O1 K1 O13 122.6(11) 2_655 6 ? O3 K1 O13 119.6(8) . 6 ? O4 K1 O13 60.4(8) . 6 ? O6 K1 O13 70.2(8) 2_655 6 ? O1 K1 O13 137.8(11) . 6 ? O1 K1 O12 77.7(11) 2_655 6 ? O3 K1 O12 161.4(8) . 6 ? O4 K1 O12 106.7(8) . 6 ? O6 K1 O12 60.1(7) 2_655 6 ? O1 K1 O12 134.6(10) . 6 ? O13 K1 O12 52.0(8) 6 6 ? O1 K1 O11 64.8(11) 2_655 . ? O3 K1 O11 57.3(8) . . ? O4 K1 O11 113.1(8) . . ? O6 K1 O11 97.7(8) 2_655 . ? O1 K1 O11 54.0(10) . . ? O13 K1 O11 167.2(8) 6 . ? O12 K1 O11 126.3(8) 6 . ? O1 K1 O7 60.9(11) 2_655 2_655 ? O3 K1 O7 115.4(7) . 2_655 ? O4 K1 O7 122.9(7) . 2_655 ? O6 K1 O7 50.0(6) 2_655 2_655 ? O1 K1 O7 111.6(10) . 2_655 ? O13 K1 O7 104.0(7) 6 2_655 ? O12 K1 O7 58.8(7) 6 2_655 ? O11 K1 O7 69.5(7) . 2_655 ? O1 K1 I2 145.1(10) 2_655 . ? O3 K1 I2 29.8(6) . . ? O4 K1 I2 30.7(5) . . ? O6 K1 I2 91.6(5) 2_655 . ? O1 K1 I2 85.8(9) . . ? O13 K1 I2 89.8(6) 6 . ? O12 K1 I2 137.1(6) 6 . ? O11 K1 I2 86.1(6) . . ? O7 K1 I2 128.0(4) 2_655 . ? O1 K1 I1 30.4(10) 2_655 . ? O3 K1 I1 88.1(6) . . ? O4 K1 I1 144.8(6) . . ? O6 K1 I1 131.3(6) 2_655 . ? O1 K1 I1 32.4(9) . . ? O13 K1 I1 143.0(6) 6 . ? O12 K1 I1 107.6(6) 6 . ? O11 K1 I1 48.8(6) . . ? O7 K1 I1 82.4(4) 2_655 . ? I2 K1 I1 115.3(2) . . ? O1 K1 I3 85.4(10) 2_655 2_655 ? O3 K1 I3 119.8(6) . 2_655 ? O4 K1 I3 99.1(6) . 2_655 ? O6 K1 I3 25.3(5) 2_655 2_655 ? O1 K1 I3 139.9(9) . 2_655 ? O13 K1 I3 78.5(6) 6 2_655 ? O12 K1 I3 45.9(5) 6 2_655 ? O11 K1 I3 92.4(6) . 2_655 ? O7 K1 I3 28.4(4) 2_655 2_655 ? I2 K1 I3 116.04(18) . 2_655 ? I1 K1 I3 110.3(2) . 2_655 ? O1 I1 O1 88.2(17) 3_665 2_655 ? O1 I1 O1 88.2(17) 3_665 . ? O1 I1 O1 88.2(17) 2_655 . ? O1 I1 K1 39.3(12) 3_665 2_655 ? O1 I1 K1 50.1(13) 2_655 2_655 ? O1 I1 K1 95.8(12) . 2_655 ? O1 I1 K1 50.1(13) 3_665 3_665 ? O1 I1 K1 95.8(12) 2_655 3_665 ? O1 I1 K1 39.3(12) . 3_665 ? K1 I1 K1 71.9(2) 2_655 3_665 ? O1 I1 K1 95.8(12) 3_665 . ? O1 I1 K1 39.3(12) 2_655 . ? O1 I1 K1 50.1(13) . . ? K1 I1 K1 71.9(2) 2_655 . ? K1 I1 K1 71.9(2) 3_665 . ? O2 I2 O3 100.9(12) . . ? O2 I2 O4 98.7(12) . . ? O3 I2 O4 87.9(11) . . ? O2 I2 K1 110.1(9) . . ? O3 I2 K1 44.2(8) . . ? O4 I2 K1 44.5(7) . . ? O6 I3 O7 95.9(10) . . ? O6 I3 O5 98.6(10) . . ? O7 I3 O5 97.1(10) . . ? O6 I3 K1 38.7(8) . 3_665 ? O7 I3 K1 65.4(7) . 3_665 ? O5 I3 K1 123.8(7) . 3_665 ? O10 I4 O9 99.0(10) . . ? O10 I4 O8 100.7(12) . . ? O9 I4 O8 94.8(11) . . ? O11 I5 O12 95.9(15) . . ? O11 I5 O13 94.7(13) . . ? O12 I5 O13 97.9(13) . . ? O11 I5 K1 97.6(11) . 6_554 ? O12 I5 K1 57.9(10) . 6_554 ? O13 I5 K1 39.9(9) . 6_554 ? O11 I5 K1 56.3(12) . . ? O12 I5 K1 151.9(10) . . ? O13 I5 K1 90.0(9) . . ? K1 I5 K1 124.71(15) 6_554 . ? I1 O1 K1 110.3(17) . 3_665 ? I1 O1 K1 97.5(16) . . ? K1 O1 K1 107.9(15) 3_665 . ? I1 O1 Am1 112.9(17) . . ? K1 O1 Am1 123.7(16) 3_665 . ? K1 O1 Am1 100.6(12) . . ? I2 O3 Am1 128.0(12) . . ? I2 O3 K1 106.1(11) . . ? Am1 O3 K1 123.8(10) . . ? I2 O4 Am1 128.6(11) . 4_665 ? I2 O4 K1 104.8(11) . . ? Am1 O4 K1 119.9(9) 4_665 . ? I3 O5 Am1 135.1(12) . 18_554 ? I3 O6 K1 116.0(11) . 3_665 ? I3 O7 Am1 137.7(11) . . ? I3 O7 K1 86.2(8) . 3_665 ? Am1 O7 K1 105.3(7) . 3_665 ? I4 O9 Am1 138.8(11) . . ? I4 O10 Am1 131.2(11) . 9_565 ? I5 O11 Am1 149.1(17) . . ? I5 O11 K1 97.9(13) . . ? Am1 O11 K1 93.6(10) . . ? I5 O12 K1 95.3(11) . 6_554 ? I5 O13 Am1 129.1(14) . 2_655 ? I5 O13 K1 114.8(12) . 6_554 ? Am1 O13 K1 111.4(10) 2_655 6_554 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.321 _refine_diff_density_min -4.148 _refine_diff_density_rms 0.561