data_kalpi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H3.50 Al2 K1.50 O10.50 P2' _chemical_formula_weight 346.08 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4352(7) _cell_length_b 9.5254(10) _cell_length_c 9.4309(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.421(7) _cell_angle_gamma 90.00 _cell_volume 830.81(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 9535 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 32.03 _exptl_crystal_description cube-like _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.539 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_T_max 0.919 _exptl_absorpt_process_details 'Coppens et al. (1965)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'IPDS-II (Stoe)' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean 6.7 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8523 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 29.99 _reflns_number_total 2250 _reflns_number_gt 1833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XAREA (Stoe 2001)' _computing_cell_refinement 'XAREA (Stoe 2001)' _computing_data_reduction 'XAREA (Stoe 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND 3.2 g (Brandenburg 2011)' _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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0152(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2250 _refine_ls_number_parameters 170 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0703 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.003 _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 0.51717(6) 0.15105(6) 0.85742(9) 0.04225(18) Uani 1 1 d . . . K2 K 0.0000 0.0000 0.5000 0.0626(4) Uani 1 2 d S . . Al1 Al 0.39343(6) 0.54272(5) 0.37218(7) 0.01362(14) Uani 1 1 d . . . Al2 Al 0.59812(6) 0.21233(6) 0.32170(7) 0.01431(14) Uani 1 1 d . . . P1 P 0.79323(5) 0.01448(5) 0.15419(6) 0.01374(12) Uani 1 1 d . . . P2 P 0.79228(5) 0.19176(4) 0.63950(6) 0.01323(12) Uani 1 1 d . . . O1 O 0.94184(14) 0.08387(14) 0.20914(17) 0.0163(3) Uani 1 1 d . . . O2 O 0.67123(15) 0.09581(14) 0.19799(18) 0.0182(3) Uani 1 1 d . . . O3 O 0.76075(14) 0.00533(14) -0.01157(16) 0.0166(3) Uani 1 1 d . . . O4 O 0.70465(15) 0.36666(13) 0.28015(17) 0.0172(3) Uani 1 1 d . . . O5 O 0.94750(15) 0.24627(14) 0.66752(17) 0.0173(3) Uani 1 1 d . . . O6 O 0.78896(15) 0.04882(13) 0.71448(17) 0.0166(3) Uani 1 1 d . . . O7 O 0.69021(15) 0.29077(13) 0.69719(17) 0.0166(3) Uani 1 1 d . . . O8 O 0.74451(15) 0.16809(14) 0.47788(17) 0.0173(3) Uani 1 1 d . . . O9 O 0.49908(15) 0.36676(14) 0.44906(17) 0.0161(3) Uani 1 1 d D . . H1 H 0.448(3) 0.314(3) 0.482(4) 0.039(9) Uiso 1 1 d D . . O10 O 0.48311(17) 0.07691(16) 0.3896(2) 0.0245(3) Uani 1 1 d D . . H2 H 0.4046(19) 0.054(4) 0.347(4) 0.064(11) Uiso 1 1 d D . . H3 H 0.508(9) 0.033(9) 0.463(6) 0.064(11) Uiso 0.50 1 d PD . . O11 O 0.2415(5) 0.1755(4) 0.5107(5) 0.0389(10) Uani 0.50 1 d PD . . H4 H 0.235(7) 0.162(6) 0.593(2) 0.028(11) Uiso 0.50 1 d PD . . H5 H 0.317(3) 0.139(6) 0.506(7) 0.028(11) Uiso 0.50 1 d PD . . 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 0.0276(3) 0.0343(3) 0.0645(5) 0.0205(3) 0.0085(3) 0.0000(2) K2 0.0970(9) 0.0675(7) 0.0264(6) 0.0094(4) 0.0200(5) 0.0598(6) Al1 0.0165(3) 0.0095(2) 0.0148(3) -0.00010(19) 0.0028(2) 0.00053(18) Al2 0.0167(3) 0.0106(2) 0.0154(3) -0.00006(19) 0.0024(2) 0.00042(18) P1 0.0160(2) 0.0096(2) 0.0156(3) -0.00066(16) 0.00312(16) 0.00041(15) P2 0.0159(2) 0.0087(2) 0.0148(3) 0.00014(16) 0.00239(16) 0.00013(15) O1 0.0173(6) 0.0131(6) 0.0188(8) -0.0022(5) 0.0037(5) -0.0012(5) O2 0.0183(6) 0.0145(6) 0.0223(9) -0.0039(5) 0.0050(5) 0.0022(5) O3 0.0183(6) 0.0149(6) 0.0163(9) -0.0007(5) 0.0029(5) 0.0007(5) O4 0.0212(7) 0.0099(6) 0.0213(9) -0.0018(5) 0.0062(5) -0.0008(5) O5 0.0177(6) 0.0164(6) 0.0176(8) 0.0011(5) 0.0026(5) -0.0019(5) O6 0.0195(6) 0.0097(5) 0.0192(9) 0.0017(5) 0.0006(5) -0.0003(4) O7 0.0214(7) 0.0110(6) 0.0179(8) 0.0003(5) 0.0052(5) 0.0029(5) O8 0.0210(7) 0.0148(6) 0.0156(8) -0.0006(5) 0.0018(5) 0.0020(5) O9 0.0184(6) 0.0125(6) 0.0175(8) 0.0011(5) 0.0038(5) -0.0017(5) O10 0.0228(7) 0.0219(7) 0.0270(10) 0.0095(6) 0.0003(6) -0.0056(6) O11 0.069(3) 0.0295(18) 0.022(3) 0.0024(14) 0.020(2) 0.0139(17) _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 O3 2.7587(15) 1_556 ? K1 O7 2.7744(15) . ? K1 O11 2.844(4) 4_666 ? K1 O4 2.8988(15) 4_566 ? K1 O1 2.9057(15) 4_566 ? K1 O2 2.9316(15) 3_656 ? K1 O10 3.184(2) 3_656 ? K1 O5 3.2715(18) 4_566 ? K1 O6 3.2727(16) . ? K1 O2 3.2950(18) 1_556 ? K1 P1 3.3088(8) 3_656 ? K1 K2 3.6013(8) 2_556 ? K2 O1 2.8049(16) 1_455 ? K2 O1 2.8049(16) 3_656 ? K2 O11 2.811(5) 3_556 ? K2 O11 2.811(5) . ? K2 O8 2.8669(14) 3_656 ? K2 O8 2.8669(14) 1_455 ? K2 O5 2.9247(15) 3_656 ? K2 O5 2.9247(15) 1_455 ? K2 O6 3.1413(15) 3_656 ? K2 O6 3.1413(15) 1_455 ? K2 P2 3.1511(5) 3_656 ? K2 P2 3.1511(5) 1_455 ? K2 H4 2.71(6) . ? Al1 O7 1.8336(14) 3_666 ? Al1 O6 1.8339(16) 4_565 ? Al1 O3 1.8768(15) 4_566 ? Al1 O1 1.9051(15) 2_655 ? Al1 O9 1.9842(16) 3_666 ? Al1 O9 2.0105(15) . ? Al1 Al1 2.9323(12) 3_666 ? Al1 K1 3.8252(8) 3_666 ? Al1 K2 3.8593(7) 2 ? Al1 K1 3.9791(8) 4_565 ? Al2 O2 1.8405(16) . ? Al2 O8 1.8572(16) . ? Al2 O5 1.8631(16) 4_565 ? Al2 O4 1.8657(14) . ? Al2 O10 1.8781(16) . ? Al2 O9 2.2191(15) . ? Al2 K1 3.9103(10) 3_656 ? P1 O2 1.5113(14) . ? P1 O3 1.5348(16) . ? P1 O4 1.5367(14) 2_645 ? P1 O1 1.5439(14) . ? P1 K1 3.3088(8) 3_656 ? P1 K2 3.4556(6) 1_655 ? P1 K1 3.6638(9) 1_554 ? P2 O8 1.5182(17) . ? P2 O7 1.5233(14) . ? P2 O5 1.5268(14) . ? P2 O6 1.5374(14) . ? P2 K2 3.1511(5) 1_655 ? O1 Al1 1.9051(15) 2_645 ? O1 K2 2.8049(16) 1_655 ? O1 K1 2.9057(15) 4_665 ? O2 K1 2.9316(15) 3_656 ? O2 K1 3.2950(18) 1_554 ? O3 Al1 1.8768(15) 4_665 ? O3 K1 2.7587(15) 1_554 ? O4 P1 1.5367(14) 2_655 ? O4 K1 2.8988(15) 4_665 ? O4 K2 3.2097(15) 2 ? O5 Al2 1.8631(16) 4_666 ? O5 K2 2.9247(15) 1_655 ? O5 K1 3.2715(18) 4_665 ? O6 Al1 1.8339(16) 4_666 ? O6 K2 3.1413(15) 1_655 ? O7 Al1 1.8336(14) 3_666 ? O8 K2 2.8669(14) 1_655 ? O9 Al1 1.9842(16) 3_666 ? O9 H1 0.7999(10) . ? O10 K1 3.184(2) 3_656 ? O10 H2 0.8000(10) . ? O10 H3 0.8000(10) . ? O11 K1 2.844(4) 4_565 ? O11 H4 0.8000(10) . ? O11 H5 0.8000(11) . ? 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 K1 O7 87.56(4) 1_556 . ? O3 K1 O11 66.08(10) 1_556 4_666 ? O7 K1 O11 62.57(9) . 4_666 ? O3 K1 O4 143.04(4) 1_556 4_566 ? O7 K1 O4 124.75(5) . 4_566 ? O11 K1 O4 141.18(10) 4_666 4_566 ? O3 K1 O1 139.07(4) 1_556 4_566 ? O7 K1 O1 55.62(4) . 4_566 ? O11 K1 O1 80.00(9) 4_666 4_566 ? O4 K1 O1 77.87(4) 4_566 4_566 ? O3 K1 O2 95.64(4) 1_556 3_656 ? O7 K1 O2 133.56(5) . 3_656 ? O11 K1 O2 157.01(9) 4_666 3_656 ? O4 K1 O2 50.05(4) 4_566 3_656 ? O1 K1 O2 121.96(5) 4_566 3_656 ? O3 K1 O10 82.21(5) 1_556 3_656 ? O7 K1 O10 81.02(4) . 3_656 ? O11 K1 O10 131.37(9) 4_666 3_656 ? O4 K1 O10 85.58(5) 4_566 3_656 ? O1 K1 O10 106.01(5) 4_566 3_656 ? O2 K1 O10 53.85(4) 3_656 3_656 ? O3 K1 O5 92.70(5) 1_556 4_566 ? O7 K1 O5 125.98(4) . 4_566 ? O11 K1 O5 68.46(9) 4_666 4_566 ? O4 K1 O5 82.39(4) 4_566 4_566 ? O1 K1 O5 95.57(4) 4_566 4_566 ? O2 K1 O5 100.20(4) 3_656 4_566 ? O10 K1 O5 152.46(4) 3_656 4_566 ? O3 K1 O6 51.94(4) 1_556 . ? O7 K1 O6 47.53(4) . . ? O11 K1 O6 79.48(9) 4_666 . ? O4 K1 O6 136.07(5) 4_566 . ? O1 K1 O6 101.38(4) 4_566 . ? O2 K1 O6 100.65(4) 3_656 . ? O10 K1 O6 51.90(4) 3_656 . ? O5 K1 O6 140.33(4) 4_566 . ? O3 K1 O2 46.80(4) 1_556 1_556 ? O7 K1 O2 114.45(5) . 1_556 ? O11 K1 O2 57.11(9) 4_666 1_556 ? O4 K1 O2 117.78(5) 4_566 1_556 ? O1 K1 O2 128.80(5) 4_566 1_556 ? O2 K1 O2 100.40(4) 3_656 1_556 ? O10 K1 O2 122.72(4) 3_656 1_556 ? O5 K1 O2 45.92(4) 4_566 1_556 ? O6 K1 O2 97.10(4) . 1_556 ? O3 K1 P1 115.37(4) 1_556 3_656 ? O7 K1 P1 145.39(4) . 3_656 ? O11 K1 P1 149.13(9) 4_666 3_656 ? O4 K1 P1 27.67(3) 4_566 3_656 ? O1 K1 P1 105.52(3) 4_566 3_656 ? O2 K1 P1 27.18(3) 3_656 3_656 ? O10 K1 P1 77.19(3) 3_656 3_656 ? O5 K1 P1 80.73(3) 4_566 3_656 ? O6 K1 P1 127.24(3) . 3_656 ? O2 K1 P1 99.96(3) 1_556 3_656 ? O3 K1 K2 113.09(4) 1_556 2_556 ? O7 K1 K2 80.53(3) . 2_556 ? O11 K1 K2 50.05(9) 4_666 2_556 ? O4 K1 K2 91.65(3) 4_566 2_556 ? O1 K1 K2 49.67(3) 4_566 2_556 ? O2 K1 K2 137.42(3) 3_656 2_556 ? O10 K1 K2 155.36(4) 3_656 2_556 ? O5 K1 K2 50.09(3) 4_566 2_556 ? O6 K1 K2 121.69(3) . 2_556 ? O2 K1 K2 80.05(3) 1_556 2_556 ? P1 K1 K2 110.32(2) 3_656 2_556 ? O1 K2 O1 180.0 1_455 3_656 ? O1 K2 O11 97.70(9) 1_455 3_556 ? O1 K2 O11 82.30(9) 3_656 3_556 ? O1 K2 O11 82.30(9) 1_455 . ? O1 K2 O11 97.70(9) 3_656 . ? O11 K2 O11 180.0 3_556 . ? O1 K2 O8 103.24(4) 1_455 3_656 ? O1 K2 O8 76.76(4) 3_656 3_656 ? O11 K2 O8 109.53(8) 3_556 3_656 ? O11 K2 O8 70.47(8) . 3_656 ? O1 K2 O8 76.76(4) 1_455 1_455 ? O1 K2 O8 103.24(4) 3_656 1_455 ? O11 K2 O8 70.47(8) 3_556 1_455 ? O11 K2 O8 109.53(8) . 1_455 ? O8 K2 O8 180.0 3_656 1_455 ? O1 K2 O5 73.83(4) 1_455 3_656 ? O1 K2 O5 106.17(4) 3_656 3_656 ? O11 K2 O5 74.12(8) 3_556 3_656 ? O11 K2 O5 105.88(8) . 3_656 ? O8 K2 O5 50.32(4) 3_656 3_656 ? O8 K2 O5 129.68(4) 1_455 3_656 ? O1 K2 O5 106.17(4) 1_455 1_455 ? O1 K2 O5 73.83(4) 3_656 1_455 ? O11 K2 O5 105.88(8) 3_556 1_455 ? O11 K2 O5 74.12(8) . 1_455 ? O8 K2 O5 129.68(4) 3_656 1_455 ? O8 K2 O5 50.32(4) 1_455 1_455 ? O5 K2 O5 180.00(5) 3_656 1_455 ? O1 K2 O6 55.85(4) 1_455 3_656 ? O1 K2 O6 124.15(4) 3_656 3_656 ? O11 K2 O6 120.09(8) 3_556 3_656 ? O11 K2 O6 59.91(8) . 3_656 ? O8 K2 O6 48.17(4) 3_656 3_656 ? O8 K2 O6 131.83(4) 1_455 3_656 ? O5 K2 O6 48.45(4) 3_656 3_656 ? O5 K2 O6 131.55(4) 1_455 3_656 ? O1 K2 O6 124.15(4) 1_455 1_455 ? O1 K2 O6 55.85(4) 3_656 1_455 ? O11 K2 O6 59.91(8) 3_556 1_455 ? O11 K2 O6 120.09(8) . 1_455 ? O8 K2 O6 131.83(4) 3_656 1_455 ? O8 K2 O6 48.17(4) 1_455 1_455 ? O5 K2 O6 131.55(4) 3_656 1_455 ? O5 K2 O6 48.45(4) 1_455 1_455 ? O6 K2 O6 180.0 3_656 1_455 ? O1 K2 P2 76.95(3) 1_455 3_656 ? O1 K2 P2 103.05(3) 3_656 3_656 ? O11 K2 P2 101.94(8) 3_556 3_656 ? O11 K2 P2 78.06(8) . 3_656 ? O8 K2 P2 28.73(3) 3_656 3_656 ? O8 K2 P2 151.27(3) 1_455 3_656 ? O5 K2 P2 28.80(3) 3_656 3_656 ? O5 K2 P2 151.20(3) 1_455 3_656 ? O6 K2 P2 28.28(2) 3_656 3_656 ? O6 K2 P2 151.72(2) 1_455 3_656 ? O1 K2 P2 103.05(3) 1_455 1_455 ? O1 K2 P2 76.95(3) 3_656 1_455 ? O11 K2 P2 78.06(8) 3_556 1_455 ? O11 K2 P2 101.94(8) . 1_455 ? O8 K2 P2 151.27(3) 3_656 1_455 ? O8 K2 P2 28.73(3) 1_455 1_455 ? O5 K2 P2 151.20(3) 3_656 1_455 ? O5 K2 P2 28.80(3) 1_455 1_455 ? O6 K2 P2 151.72(2) 3_656 1_455 ? O6 K2 P2 28.28(2) 1_455 1_455 ? P2 K2 P2 180.0 3_656 1_455 ? O1 K2 H4 98.2(3) 1_455 . ? O1 K2 H4 81.8(3) 3_656 . ? O11 K2 H4 163.47(4) 3_556 . ? O11 K2 H4 16.53(4) . . ? O8 K2 H4 70.8(12) 3_656 . ? O8 K2 H4 109.2(12) 1_455 . ? O5 K2 H4 114.7(11) 3_656 . ? O5 K2 H4 65.3(11) 1_455 . ? O6 K2 H4 73.1(7) 3_656 . ? O6 K2 H4 106.9(7) 1_455 . ? P2 K2 H4 85.9(11) 3_656 . ? P2 K2 H4 94.1(11) 1_455 . ? O7 Al1 O6 89.87(7) 3_666 4_565 ? O7 Al1 O3 97.45(7) 3_666 4_566 ? O6 Al1 O3 92.53(7) 4_565 4_566 ? O7 Al1 O1 90.36(7) 3_666 2_655 ? O6 Al1 O1 96.99(7) 4_565 2_655 ? O3 Al1 O1 167.71(7) 4_566 2_655 ? O7 Al1 O9 92.22(7) 3_666 3_666 ? O6 Al1 O9 176.26(7) 4_565 3_666 ? O3 Al1 O9 84.12(7) 4_566 3_666 ? O1 Al1 O9 86.11(7) 2_655 3_666 ? O7 Al1 O9 175.88(7) 3_666 . ? O6 Al1 O9 92.56(6) 4_565 . ? O3 Al1 O9 85.78(6) 4_566 . ? O1 Al1 O9 86.04(6) 2_655 . ? O9 Al1 O9 85.55(6) 3_666 . ? O7 Al1 Al1 135.24(6) 3_666 3_666 ? O6 Al1 Al1 134.89(5) 4_565 3_666 ? O3 Al1 Al1 83.12(5) 4_566 3_666 ? O1 Al1 Al1 84.65(5) 2_655 3_666 ? O9 Al1 Al1 43.12(4) 3_666 3_666 ? O9 Al1 Al1 42.43(4) . 3_666 ? O7 Al1 K1 42.77(5) 3_666 3_666 ? O6 Al1 K1 92.69(5) 4_565 3_666 ? O3 Al1 K1 139.82(5) 4_566 3_666 ? O1 Al1 K1 47.65(4) 2_655 3_666 ? O9 Al1 K1 90.95(5) 3_666 3_666 ? O9 Al1 K1 133.69(5) . 3_666 ? Al1 Al1 K1 119.00(3) 3_666 3_666 ? O7 Al1 K2 86.44(5) 3_666 2 ? O6 Al1 K2 53.65(5) 4_565 2 ? O3 Al1 K2 146.06(5) 4_566 2 ? O1 Al1 K2 43.56(5) 2_655 2 ? O9 Al1 K2 129.58(5) 3_666 2 ? O9 Al1 K2 92.31(5) . 2 ? Al1 Al1 K2 117.31(3) 3_666 2 ? K1 Al1 K2 55.890(15) 3_666 2 ? O7 Al1 K1 94.06(5) 3_666 4_565 ? O6 Al1 K1 54.45(5) 4_565 4_565 ? O3 Al1 K1 38.15(5) 4_566 4_565 ? O1 Al1 K1 151.01(5) 2_655 4_565 ? O9 Al1 K1 122.25(5) 3_666 4_565 ? O9 Al1 K1 90.06(4) . 4_565 ? Al1 Al1 K1 111.22(3) 3_666 4_565 ? K1 Al1 K1 128.985(18) 3_666 4_565 ? K2 Al1 K1 108.095(18) 2 4_565 ? O2 Al2 O8 93.02(7) . . ? O2 Al2 O5 87.51(7) . 4_565 ? O8 Al2 O5 178.33(7) . 4_565 ? O2 Al2 O4 93.26(7) . . ? O8 Al2 O4 89.90(7) . . ? O5 Al2 O4 91.65(7) 4_565 . ? O2 Al2 O10 96.68(8) . . ? O8 Al2 O10 87.87(7) . . ? O5 Al2 O10 90.50(7) 4_565 . ? O4 Al2 O10 169.91(8) . . ? O2 Al2 O9 173.57(7) . . ? O8 Al2 O9 92.75(6) . . ? O5 Al2 O9 86.81(6) 4_565 . ? O4 Al2 O9 83.89(6) . . ? O10 Al2 O9 86.38(7) . . ? O2 Al2 K1 45.53(5) . 3_656 ? O8 Al2 K1 103.97(5) . 3_656 ? O5 Al2 K1 75.30(5) 4_565 3_656 ? O4 Al2 K1 136.23(5) . 3_656 ? O10 Al2 K1 53.79(6) . 3_656 ? O9 Al2 K1 135.21(4) . 3_656 ? O2 P1 O3 107.35(8) . . ? O2 P1 O4 108.02(8) . 2_645 ? O3 P1 O4 110.02(8) . 2_645 ? O2 P1 O1 112.28(8) . . ? O3 P1 O1 110.55(8) . . ? O4 P1 O1 108.58(8) 2_645 . ? O2 P1 K1 62.37(6) . 3_656 ? O3 P1 K1 86.69(5) . 3_656 ? O4 P1 K1 61.15(5) 2_645 3_656 ? O1 P1 K1 162.59(7) . 3_656 ? O2 P1 K2 94.63(7) . 1_655 ? O3 P1 K2 157.01(5) . 1_655 ? O4 P1 K2 67.87(6) 2_645 1_655 ? O1 P1 K2 52.76(6) . 1_655 ? K1 P1 K2 110.05(2) 3_656 1_655 ? O2 P1 K1 64.03(7) . 1_554 ? O3 P1 K1 43.42(5) . 1_554 ? O4 P1 K1 125.71(6) 2_645 1_554 ? O1 P1 K1 124.43(6) . 1_554 ? K1 P1 K1 69.709(19) 3_656 1_554 ? K2 P1 K1 156.671(19) 1_655 1_554 ? O8 P2 O7 111.56(8) . . ? O8 P2 O5 107.95(9) . . ? O7 P2 O5 112.35(8) . . ? O8 P2 O6 107.53(8) . . ? O7 P2 O6 108.19(8) . . ? O5 P2 O6 109.14(8) . . ? O8 P2 K2 65.19(5) . 1_655 ? O7 P2 K2 175.92(6) . 1_655 ? O5 P2 K2 67.34(6) . 1_655 ? O6 P2 K2 75.50(6) . 1_655 ? O8 P2 K1 116.64(6) . . ? O7 P2 K1 44.90(5) . . ? O5 P2 K1 134.91(7) . . ? O6 P2 K1 64.14(6) . . ? K2 P2 K1 138.306(18) 1_655 . ? P1 O1 Al1 122.41(9) . 2_645 ? P1 O1 K2 101.25(7) . 1_655 ? Al1 O1 K2 108.53(6) 2_645 1_655 ? P1 O1 K1 130.76(7) . 4_665 ? Al1 O1 K1 103.37(6) 2_645 4_665 ? K2 O1 K1 78.17(4) 1_655 4_665 ? P1 O2 Al2 152.09(11) . . ? P1 O2 K1 90.45(6) . 3_656 ? Al2 O2 K1 107.85(6) . 3_656 ? P1 O2 K1 91.62(7) . 1_554 ? Al2 O2 K1 111.92(6) . 1_554 ? K1 O2 K1 79.60(4) 3_656 1_554 ? P1 O3 Al1 125.95(8) . 4_665 ? P1 O3 K1 114.09(7) . 1_554 ? Al1 O3 K1 117.00(7) 4_665 1_554 ? P1 O4 Al2 127.01(9) 2_655 . ? P1 O4 K1 91.18(6) 2_655 4_665 ? Al2 O4 K1 117.70(6) . 4_665 ? P1 O4 K2 85.80(6) 2_655 2 ? Al2 O4 K2 102.91(6) . 2 ? K1 O4 K2 130.25(5) 4_665 2 ? P2 O5 Al2 139.85(10) . 4_666 ? P2 O5 K2 83.86(6) . 1_655 ? Al2 O5 K2 114.00(6) 4_666 1_655 ? P2 O5 K1 107.61(7) . 4_665 ? Al2 O5 K1 112.16(6) 4_666 4_665 ? K2 O5 K1 70.82(4) 1_655 4_665 ? P2 O6 Al1 137.51(9) . 4_666 ? P2 O6 K2 76.21(6) . 1_655 ? Al1 O6 K2 98.30(6) 4_666 1_655 ? P2 O6 K1 90.86(6) . . ? Al1 O6 K1 98.43(6) 4_666 . ? K2 O6 K1 163.25(5) 1_655 . ? P2 O7 Al1 131.76(10) . 3_666 ? P2 O7 K1 112.29(7) . . ? Al1 O7 K1 110.56(6) 3_666 . ? P2 O8 Al2 142.08(9) . . ? P2 O8 K2 86.08(6) . 1_655 ? Al2 O8 K2 131.84(7) . 1_655 ? Al1 O9 Al1 94.45(6) 3_666 . ? Al1 O9 Al2 123.28(7) 3_666 . ? Al1 O9 Al2 126.10(8) . . ? Al1 O9 H1 101(3) 3_666 . ? Al1 O9 H1 112(2) . . ? Al2 O9 H1 98(2) . . ? Al2 O10 K1 97.79(8) . 3_656 ? Al2 O10 H2 124(3) . . ? K1 O10 H2 65(3) 3_656 . ? Al2 O10 H3 124(6) . . ? K1 O10 H3 103(7) 3_656 . ? H2 O10 H3 112(7) . . ? K2 O11 K1 79.10(13) . 4_565 ? K2 O11 H4 74(4) . . ? K1 O11 H4 113(4) 4_565 . ? K2 O11 H5 118(4) . . ? K1 O11 H5 144(5) 4_565 . ? H4 O11 H5 103(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1 O11 0.7999(10) 2.413(12) 3.182(5) 162(3) . O10 H2 O6 0.8000(10) 2.052(13) 2.827(2) 163(4) 3_656 O10 H3 O10 0.8000(10) 1.73(2) 2.514(3) 165(9) 3_656 O11 H4 O4 0.8000(10) 1.864(7) 2.662(4) 175(6) 4_566 O11 H5 O10 0.8000(11) 2.17(3) 2.901(4) 152(6) . _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.494 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.106