data_kalpi _audit_update_record ; 2010-12-29 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'H3.50 Al2 K1.50 O10.50 P2' _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 9.4309(7) _cell_length_b 9.5254(10) _cell_length_c 9.4352(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 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 '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 -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _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 ? _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^)+(0.0400P)^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 0.0159(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 0.0389 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.983 _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 Al1 Al -0.17830(7) 0.21231(6) 0.59812(6) 0.01435(14) Uani 1 1 d . . . Al2 Al 0.12784(7) 0.45731(5) 0.60657(6) 0.01368(14) Uani 1 1 d . . . P1 P -0.15420(6) 0.51448(5) 0.70677(5) 0.01378(12) Uani 1 1 d . . . P2 P 0.13951(6) 0.19175(4) 0.79228(5) 0.01327(12) Uani 1 1 d . . . K1 K -0.14254(8) 0.34895(6) 1.01718(6) 0.04241(18) Uani 1 1 d . . . K2 K 0.0000 0.0000 1.0000 0.0625(4) Uani 1 2 d S . . O1 O -0.19802(17) 0.59570(14) 0.82877(15) 0.0183(3) Uani 1 1 d . . . O2 O -0.20912(16) 0.58379(13) 0.55815(14) 0.0164(3) Uani 1 1 d . . . O3 O -0.21997(16) 0.36671(13) 0.70464(15) 0.0173(3) Uani 1 1 d . . . O4 O 0.01164(16) 0.50534(14) 0.73925(14) 0.0168(3) Uani 1 1 d . . . O5 O 0.16752(17) 0.24613(14) 0.94750(14) 0.0174(3) Uani 1 1 d . . . O6 O 0.19726(16) 0.29067(13) 0.69023(15) 0.0167(3) Uani 1 1 d . . . O7 O -0.02218(17) 0.16809(14) 0.74449(15) 0.0175(3) Uani 1 1 d . . . O8 O 0.21456(16) 0.04888(13) 0.78898(15) 0.0167(3) Uani 1 1 d . . . O9 O -0.4890(5) 0.3245(4) 0.7417(5) 0.0395(9) Uani 0.50 1 d PD . . H9A H -0.4056(19) 0.335(6) 0.738(7) 0.034(12) Uiso 0.50 1 d PD . . H9B H -0.494(7) 0.364(6) 0.815(4) 0.034(12) Uiso 0.50 1 d PD . . O10 O -0.1103(2) 0.07693(16) 0.48314(17) 0.0246(3) Uani 1 1 d D . . H10A H -0.153(4) 0.061(4) 0.4028(17) 0.065(11) Uiso 1 1 d D . . H10B H -0.041(6) 0.028(7) 0.507(10) 0.065(11) Uiso 0.50 1 d PD . . O11 O 0.44917(16) 0.13328(14) 0.99911(14) 0.0161(3) Uani 1 1 d D . . H11 H 0.484(3) 0.185(2) 0.948(3) 0.033(8) Uiso 1 1 d 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 Al1 0.0154(3) 0.0106(2) 0.0168(3) 0.00041(18) 0.0024(2) -0.00007(19) Al2 0.0148(3) 0.0096(2) 0.0165(3) 0.00053(18) 0.0028(2) -0.00004(19) P1 0.0156(3) 0.0097(2) 0.0161(2) -0.00042(15) 0.00313(16) 0.00067(15) P2 0.0148(3) 0.0088(2) 0.0160(2) 0.00014(15) 0.00241(16) 0.00014(15) K1 0.0649(5) 0.0344(3) 0.0277(3) 0.0000(2) 0.0085(2) -0.0206(3) K2 0.0262(6) 0.0674(6) 0.0972(8) 0.0597(6) 0.0199(5) 0.0094(4) O1 0.0224(9) 0.0146(6) 0.0183(6) -0.0023(5) 0.0050(5) 0.0037(5) O2 0.0188(8) 0.0131(6) 0.0173(6) 0.0012(5) 0.0037(5) 0.0020(5) O3 0.0216(9) 0.0099(5) 0.0212(6) -0.0008(5) 0.0062(5) -0.0016(5) O4 0.0168(9) 0.0151(6) 0.0182(6) -0.0007(5) 0.0030(5) 0.0007(5) O5 0.0176(8) 0.0164(6) 0.0178(6) -0.0019(5) 0.0026(5) 0.0011(5) O6 0.0182(8) 0.0112(6) 0.0214(7) 0.0029(5) 0.0053(5) 0.0005(5) O7 0.0161(8) 0.0149(6) 0.0208(7) 0.0020(5) 0.0019(5) -0.0006(5) O8 0.0194(8) 0.0097(5) 0.0196(6) -0.0003(4) 0.0006(5) 0.0016(5) O9 0.024(3) 0.0297(18) 0.069(3) -0.0139(17) 0.0203(19) -0.0022(14) O10 0.0271(10) 0.0220(7) 0.0228(7) -0.0056(6) 0.0004(6) 0.0092(6) O11 0.0173(8) 0.0125(6) 0.0185(6) 0.0017(5) 0.0039(5) -0.0010(5) _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 Al1 O1 1.8408(15) 2_446 ? Al1 O7 1.8566(16) . ? Al1 O5 1.8634(15) 4_565 ? Al1 O3 1.8665(14) . ? Al1 O10 1.8778(16) . ? Al1 O11 2.2195(15) 4_565 ? Al1 K1 3.9102(9) 2_446 ? Al2 O8 1.8333(15) 2_556 ? Al2 O6 1.8348(14) . ? Al2 O4 1.8764(15) . ? Al2 O2 1.9047(15) 3_566 ? Al2 O11 1.9837(16) 4_565 ? Al2 O11 2.0111(15) 2_556 ? Al2 Al2 2.9325(12) 3_566 ? Al2 K1 3.8255(8) 4_665 ? Al2 K2 3.8591(7) 2_556 ? Al2 K1 3.9790(8) 3_567 ? P1 O1 1.5109(14) . ? P1 O4 1.5355(16) . ? P1 O3 1.5367(14) . ? P1 O2 1.5436(14) . ? P1 K1 3.3088(7) . ? P1 K2 3.4556(6) 2_456 ? P1 K1 3.6635(9) 3_567 ? P2 O7 1.5189(16) . ? P2 O6 1.5229(14) . ? P2 O5 1.5264(14) . ? P2 O8 1.5371(14) . ? P2 K2 3.1511(5) . ? P2 K1 3.6367(8) 4_665 ? K1 O4 2.7583(14) 3_567 ? K1 O6 2.7738(15) 4_566 ? K1 O9 2.845(4) 4_666 ? K1 O3 2.8991(15) . ? K1 O2 2.9066(14) 2_446 ? K1 O1 2.9309(15) . ? K1 O10 3.185(2) 2_456 ? K1 O5 3.2716(17) . ? K1 O8 3.2724(16) 4_566 ? K1 O1 3.2951(18) 3_567 ? K1 K2 3.6011(8) . ? K2 O2 2.8049(15) 4_666 ? K2 O2 2.8049(15) 2_446 ? K2 O9 2.813(5) 2_446 ? K2 O9 2.813(5) 4_666 ? K2 O7 2.8670(14) . ? K2 O7 2.8670(14) 3_557 ? K2 O5 2.9237(15) 3_557 ? K2 O5 2.9237(15) . ? K2 O8 3.1419(15) . ? K2 O8 3.1419(15) 3_557 ? K2 P2 3.1511(5) 3_557 ? O1 Al1 1.8408(15) 2_456 ? O1 K1 3.2951(18) 3_567 ? O2 Al2 1.9047(15) 3_566 ? O2 K2 2.8049(15) 2_456 ? O2 K1 2.9066(14) 2_456 ? O3 K2 3.2086(15) 2_456 ? O4 K1 2.7583(14) 3_567 ? O5 Al1 1.8634(15) 4_666 ? O6 K1 2.7738(15) 4_665 ? O8 Al2 1.8333(15) 2_546 ? O8 K1 3.2724(16) 4_665 ? O9 K2 2.813(5) 2_456 ? O9 K1 2.845(4) 4_565 ? O9 H9A 0.8000(11) . ? O9 H9B 0.8000(11) . ? O10 K1 3.185(2) 2_446 ? O10 H10A 0.8000(10) . ? O10 H10B 0.8000(11) . ? O11 Al2 1.9837(16) 4_666 ? O11 Al2 2.0111(15) 2_546 ? O11 Al1 2.2195(15) 4_666 ? O11 H11 0.7999(10) . ? 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 Al1 O7 93.00(7) 2_446 . ? O1 Al1 O5 87.55(7) 2_446 4_565 ? O7 Al1 O5 178.36(7) . 4_565 ? O1 Al1 O3 93.27(7) 2_446 . ? O7 Al1 O3 89.93(7) . . ? O5 Al1 O3 91.58(7) 4_565 . ? O1 Al1 O10 96.68(8) 2_446 . ? O7 Al1 O10 87.87(7) . . ? O5 Al1 O10 90.54(7) 4_565 . ? O3 Al1 O10 169.91(8) . . ? O1 Al1 O11 173.61(7) 2_446 4_565 ? O7 Al1 O11 92.73(6) . 4_565 ? O5 Al1 O11 86.79(6) 4_565 4_565 ? O3 Al1 O11 83.90(6) . 4_565 ? O10 Al1 O11 86.37(7) . 4_565 ? O1 Al1 K1 45.51(5) 2_446 2_446 ? O7 Al1 K1 103.98(5) . 2_446 ? O5 Al1 K1 75.34(5) 4_565 2_446 ? O3 Al1 K1 136.20(5) . 2_446 ? O10 Al1 K1 53.81(6) . 2_446 ? O11 Al1 K1 135.21(4) 4_565 2_446 ? O8 Al2 O6 89.89(7) 2_556 . ? O8 Al2 O4 92.51(7) 2_556 . ? O6 Al2 O4 97.45(7) . . ? O8 Al2 O2 97.01(7) 2_556 3_566 ? O6 Al2 O2 90.36(6) . 3_566 ? O4 Al2 O2 167.70(7) . 3_566 ? O8 Al2 O11 176.25(7) 2_556 4_565 ? O6 Al2 O11 92.19(6) . 4_565 ? O4 Al2 O11 84.14(6) . 4_565 ? O2 Al2 O11 86.09(6) 3_566 4_565 ? O8 Al2 O11 92.56(6) 2_556 2_556 ? O6 Al2 O11 175.86(6) . 2_556 ? O4 Al2 O11 85.77(6) . 2_556 ? O2 Al2 O11 86.04(6) 3_566 2_556 ? O11 Al2 O11 85.54(6) 4_565 2_556 ? O8 Al2 Al2 134.89(5) 2_556 3_566 ? O6 Al2 Al2 135.22(6) . 3_566 ? O4 Al2 Al2 83.13(5) . 3_566 ? O2 Al2 Al2 84.64(5) 3_566 3_566 ? O11 Al2 Al2 43.13(4) 4_565 3_566 ? O11 Al2 Al2 42.41(4) 2_556 3_566 ? O8 Al2 K1 92.71(5) 2_556 4_665 ? O6 Al2 K1 42.76(5) . 4_665 ? O4 Al2 K1 139.81(5) . 4_665 ? O2 Al2 K1 47.67(4) 3_566 4_665 ? O11 Al2 K1 90.93(4) 4_565 4_665 ? O11 Al2 K1 133.70(5) 2_556 4_665 ? Al2 Al2 K1 119.00(3) 3_566 4_665 ? O8 Al2 K2 53.67(5) 2_556 2_556 ? O6 Al2 K2 86.44(5) . 2_556 ? O4 Al2 K2 146.06(5) . 2_556 ? O2 Al2 K2 43.56(5) 3_566 2_556 ? O11 Al2 K2 129.57(5) 4_565 2_556 ? O11 Al2 K2 92.34(5) 2_556 2_556 ? Al2 Al2 K2 117.31(3) 3_566 2_556 ? K1 Al2 K2 55.887(15) 4_665 2_556 ? O8 Al2 K1 54.44(5) 2_556 3_567 ? O6 Al2 K1 94.07(5) . 3_567 ? O4 Al2 K1 38.14(5) . 3_567 ? O2 Al2 K1 151.02(5) 3_566 3_567 ? O11 Al2 K1 122.26(5) 4_565 3_567 ? O11 Al2 K1 90.06(4) 2_556 3_567 ? Al2 Al2 K1 111.21(3) 3_566 3_567 ? K1 Al2 K1 128.988(18) 4_665 3_567 ? K2 Al2 K1 108.107(18) 2_556 3_567 ? O1 P1 O4 107.36(8) . . ? O1 P1 O3 107.96(8) . . ? O4 P1 O3 110.07(8) . . ? O1 P1 O2 112.32(8) . . ? O4 P1 O2 110.54(8) . . ? O3 P1 O2 108.54(8) . . ? O1 P1 K1 62.34(5) . . ? O4 P1 K1 86.69(5) . . ? O3 P1 K1 61.16(5) . . ? O2 P1 K1 162.60(6) . . ? O1 P1 K2 94.62(6) . 2_456 ? O4 P1 K2 157.00(5) . 2_456 ? O3 P1 K2 67.83(6) . 2_456 ? O2 P1 K2 52.76(6) . 2_456 ? K1 P1 K2 110.056(19) . 2_456 ? O1 P1 K1 64.04(6) . 3_567 ? O4 P1 K1 43.43(5) . 3_567 ? O3 P1 K1 125.74(6) . 3_567 ? O2 P1 K1 124.45(6) . 3_567 ? K1 P1 K1 69.702(19) . 3_567 ? K2 P1 K1 156.667(19) 2_456 3_567 ? O7 P2 O6 111.58(8) . . ? O7 P2 O5 107.94(8) . . ? O6 P2 O5 112.40(8) . . ? O7 P2 O8 107.57(8) . . ? O6 P2 O8 108.13(8) . . ? O5 P2 O8 109.09(8) . . ? O7 P2 K2 65.19(5) . . ? O6 P2 K2 175.96(6) . . ? O5 P2 K2 67.30(6) . . ? O8 P2 K2 75.53(6) . . ? O7 P2 K1 116.64(6) . 4_665 ? O6 P2 K1 44.87(5) . 4_665 ? O5 P2 K1 134.92(6) . 4_665 ? O8 P2 K1 64.12(6) . 4_665 ? K2 P2 K1 138.309(17) . 4_665 ? O4 K1 O6 87.53(4) 3_567 4_566 ? O4 K1 O9 66.05(9) 3_567 4_666 ? O6 K1 O9 62.59(9) 4_566 4_666 ? O4 K1 O3 143.05(4) 3_567 . ? O6 K1 O3 124.74(5) 4_566 . ? O9 K1 O3 141.22(10) 4_666 . ? O4 K1 O2 139.06(4) 3_567 2_446 ? O6 K1 O2 55.63(4) 4_566 2_446 ? O9 K1 O2 80.03(9) 4_666 2_446 ? O3 K1 O2 77.87(4) . 2_446 ? O4 K1 O1 95.65(4) 3_567 . ? O6 K1 O1 133.54(5) 4_566 . ? O9 K1 O1 156.99(9) 4_666 . ? O3 K1 O1 50.02(4) . . ? O2 K1 O1 121.94(5) 2_446 . ? O4 K1 O10 82.21(4) 3_567 2_456 ? O6 K1 O10 81.01(4) 4_566 2_456 ? O9 K1 O10 131.36(9) 4_666 2_456 ? O3 K1 O10 85.55(4) . 2_456 ? O2 K1 O10 106.00(5) 2_446 2_456 ? O1 K1 O10 53.84(4) . 2_456 ? O4 K1 O5 92.73(4) 3_567 . ? O6 K1 O5 125.98(4) 4_566 . ? O9 K1 O5 68.44(9) 4_666 . ? O3 K1 O5 82.43(4) . . ? O2 K1 O5 95.55(4) 2_446 . ? O1 K1 O5 100.23(4) . . ? O10 K1 O5 152.48(4) 2_456 . ? O4 K1 O8 51.92(4) 3_567 4_566 ? O6 K1 O8 47.50(4) 4_566 4_566 ? O9 K1 O8 79.46(9) 4_666 4_566 ? O3 K1 O8 136.05(5) . 4_566 ? O2 K1 O8 101.37(4) 2_446 4_566 ? O1 K1 O8 100.66(4) . 4_566 ? O10 K1 O8 51.91(4) 2_456 4_566 ? O5 K1 O8 140.33(4) . 4_566 ? O4 K1 O1 46.81(4) 3_567 3_567 ? O6 K1 O1 114.46(4) 4_566 3_567 ? O9 K1 O1 57.09(9) 4_666 3_567 ? O3 K1 O1 117.81(4) . 3_567 ? O2 K1 O1 128.82(5) 2_446 3_567 ? O1 K1 O1 100.40(4) . 3_567 ? O10 K1 O1 122.72(4) 2_456 3_567 ? O5 K1 O1 45.94(4) . 3_567 ? O8 K1 O1 97.09(4) 4_566 3_567 ? O4 K1 P1 115.38(3) 3_567 . ? O6 K1 P1 145.38(4) 4_566 . ? O9 K1 P1 149.13(9) 4_666 . ? O3 K1 P1 27.67(3) . . ? O2 K1 P1 105.52(3) 2_446 . ? O1 K1 P1 27.17(3) . . ? O10 K1 P1 77.19(3) 2_456 . ? O5 K1 P1 80.74(3) . . ? O8 K1 P1 127.25(3) 4_566 . ? O1 K1 P1 99.95(3) 3_567 . ? O4 K1 K2 113.11(4) 3_567 . ? O6 K1 K2 80.54(3) 4_566 . ? O9 K1 K2 50.08(9) 4_666 . ? O3 K1 K2 91.67(3) . . ? O2 K1 K2 49.67(3) 2_446 . ? O1 K1 K2 137.42(3) . . ? O10 K1 K2 155.35(3) 2_456 . ? O5 K1 K2 50.07(3) . . ? O8 K1 K2 121.68(3) 4_566 . ? O1 K1 K2 80.07(3) 3_567 . ? P1 K1 K2 110.320(19) . . ? O2 K2 O2 180.000(1) 4_666 2_446 ? O2 K2 O9 82.35(9) 4_666 2_446 ? O2 K2 O9 97.65(9) 2_446 2_446 ? O2 K2 O9 97.65(9) 4_666 4_666 ? O2 K2 O9 82.35(9) 2_446 4_666 ? O9 K2 O9 180.000(1) 2_446 4_666 ? O2 K2 O7 103.24(4) 4_666 . ? O2 K2 O7 76.76(4) 2_446 . ? O9 K2 O7 70.46(8) 2_446 . ? O9 K2 O7 109.54(8) 4_666 . ? O2 K2 O7 76.76(4) 4_666 3_557 ? O2 K2 O7 103.24(4) 2_446 3_557 ? O9 K2 O7 109.54(8) 2_446 3_557 ? O9 K2 O7 70.46(8) 4_666 3_557 ? O7 K2 O7 180.0 . 3_557 ? O2 K2 O5 106.21(4) 4_666 3_557 ? O2 K2 O5 73.79(4) 2_446 3_557 ? O9 K2 O5 74.12(8) 2_446 3_557 ? O9 K2 O5 105.88(8) 4_666 3_557 ? O7 K2 O5 129.67(4) . 3_557 ? O7 K2 O5 50.33(4) 3_557 3_557 ? O2 K2 O5 73.79(4) 4_666 . ? O2 K2 O5 106.21(4) 2_446 . ? O9 K2 O5 105.88(8) 2_446 . ? O9 K2 O5 74.12(8) 4_666 . ? O7 K2 O5 50.33(4) . . ? O7 K2 O5 129.67(4) 3_557 . ? O5 K2 O5 180.00(3) 3_557 . ? O2 K2 O8 55.84(4) 4_666 . ? O2 K2 O8 124.16(4) 2_446 . ? O9 K2 O8 59.95(8) 2_446 . ? O9 K2 O8 120.05(8) 4_666 . ? O7 K2 O8 48.19(4) . . ? O7 K2 O8 131.81(4) 3_557 . ? O5 K2 O8 131.58(4) 3_557 . ? O5 K2 O8 48.42(4) . . ? O2 K2 O8 124.16(4) 4_666 3_557 ? O2 K2 O8 55.84(4) 2_446 3_557 ? O9 K2 O8 120.05(8) 2_446 3_557 ? O9 K2 O8 59.95(8) 4_666 3_557 ? O7 K2 O8 131.81(4) . 3_557 ? O7 K2 O8 48.19(4) 3_557 3_557 ? O5 K2 O8 48.42(4) 3_557 3_557 ? O5 K2 O8 131.58(4) . 3_557 ? O8 K2 O8 180.0 . 3_557 ? O2 K2 P2 76.94(3) 4_666 . ? O2 K2 P2 103.06(3) 2_446 . ? O9 K2 P2 78.07(8) 2_446 . ? O9 K2 P2 101.93(8) 4_666 . ? O7 K2 P2 28.74(3) . . ? O7 K2 P2 151.26(3) 3_557 . ? O5 K2 P2 151.21(3) 3_557 . ? O5 K2 P2 28.79(3) . . ? O8 K2 P2 28.28(2) . . ? O8 K2 P2 151.72(2) 3_557 . ? O2 K2 P2 103.06(3) 4_666 3_557 ? O2 K2 P2 76.94(3) 2_446 3_557 ? O9 K2 P2 101.93(8) 2_446 3_557 ? O9 K2 P2 78.07(8) 4_666 3_557 ? O7 K2 P2 151.26(3) . 3_557 ? O7 K2 P2 28.74(3) 3_557 3_557 ? O5 K2 P2 28.79(3) 3_557 3_557 ? O5 K2 P2 151.21(3) . 3_557 ? O8 K2 P2 151.72(2) . 3_557 ? O8 K2 P2 28.28(2) 3_557 3_557 ? P2 K2 P2 180.0 . 3_557 ? P1 O1 Al1 152.09(10) . 2_456 ? P1 O1 K1 90.49(6) . . ? Al1 O1 K1 107.87(6) 2_456 . ? P1 O1 K1 91.62(7) . 3_567 ? Al1 O1 K1 111.89(6) 2_456 3_567 ? K1 O1 K1 79.60(4) . 3_567 ? P1 O2 Al2 122.44(9) . 3_566 ? P1 O2 K2 101.26(7) . 2_456 ? Al2 O2 K2 108.54(6) 3_566 2_456 ? P1 O2 K1 130.73(7) . 2_456 ? Al2 O2 K1 103.36(6) 3_566 2_456 ? K2 O2 K1 78.15(4) 2_456 2_456 ? P1 O3 Al1 126.96(9) . . ? P1 O3 K1 91.17(6) . . ? Al1 O3 K1 117.66(6) . . ? P1 O3 K2 85.84(6) . 2_456 ? Al1 O3 K2 102.93(6) . 2_456 ? K1 O3 K2 130.29(5) . 2_456 ? P1 O4 Al2 125.95(8) . . ? P1 O4 K1 114.07(7) . 3_567 ? Al2 O4 K1 117.02(7) . 3_567 ? P2 O5 Al1 139.87(10) . 4_666 ? P2 O5 K2 83.90(6) . . ? Al1 O5 K2 114.04(6) 4_666 . ? P2 O5 K1 107.62(7) . . ? Al1 O5 K1 112.13(6) 4_666 . ? K2 O5 K1 70.82(4) . . ? P2 O6 Al2 131.72(10) . . ? P2 O6 K1 112.34(7) . 4_665 ? Al2 O6 K1 110.55(6) . 4_665 ? P2 O7 Al1 142.07(9) . . ? P2 O7 K2 86.07(6) . . ? Al1 O7 K2 131.85(7) . . ? P2 O8 Al2 137.55(9) . 2_546 ? P2 O8 K2 76.20(6) . . ? Al2 O8 K2 98.29(6) 2_546 . ? P2 O8 K1 90.88(6) . 4_665 ? Al2 O8 K1 98.45(6) 2_546 4_665 ? K2 O8 K1 163.25(5) . 4_665 ? K2 O9 K1 79.05(13) 2_456 4_565 ? K2 O9 H9A 77(5) 2_456 . ? K1 O9 H9A 114(5) 4_565 . ? K2 O9 H9B 115(5) 2_456 . ? K1 O9 H9B 144(5) 4_565 . ? H9A O9 H9B 101(6) . . ? Al1 O10 K1 97.78(7) . 2_446 ? Al1 O10 H10A 121(3) . . ? K1 O10 H10A 69(3) 2_446 . ? Al1 O10 H10B 127(7) . . ? K1 O10 H10B 100(6) 2_446 . ? H10A O10 H10B 113(7) . . ? Al2 O11 Al2 94.46(6) 4_666 2_546 ? Al2 O11 Al1 123.31(7) 4_666 4_666 ? Al2 O11 Al1 126.05(8) 2_546 4_666 ? Al2 O11 H11 99(2) 4_666 . ? Al2 O11 H11 111(2) 2_546 . ? Al1 O11 H11 100(2) 4_666 . ? 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 H9A O3 0.8000(11) 1.865(10) 2.660(4) 172(7) . O9 H9B O10 0.8000(11) 2.17(3) 2.901(4) 151(6) 4_566 O10 H10A O8 0.8000(10) 2.072(16) 2.828(2) 157(4) 3_556 O10 H10B O10 0.8000(11) 1.73(2) 2.513(3) 167(10) 3_556 O11 H11 O9 0.7999(10) 2.416(12) 3.181(5) 160(3) 1_655 _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.480 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.106