# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email liniu@nankai.edu.cn _publ_contact_author_name 'Niu Li' loop_ _publ_author_name 'Niu Li' 'Jinxiong Wu' 'Chenguang Wang' 'Qianqian Luo' 'Chunqian He' ; Xionghou Gao ; 'Haitao Zhang' 'Naijia Guan' 'Shouhe Xiang' data_shelx _database_code_depnum_ccdc_archive 'CCDC 852532' #TrackingRef 'm1012209b-- AlPO4-34FF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H10.50 Al3 N O14 P3' _chemical_formula_weight 470.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.200(3) _cell_length_b 9.208(3) _cell_length_c 9.269(3) _cell_angle_alpha 77.953(8) _cell_angle_beta 86.586(11) _cell_angle_gamma 88.716(10) _cell_volume 766.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 475 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8939 _exptl_absorpt_correction_T_max 0.9274 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8795 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3598 _reflns_number_gt 2691 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0414P)^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_number_reflns 3598 _refine_ls_number_parameters 234 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.06278(7) 0.36769(7) 0.58819(7) 0.00654(15) Uani 1 1 d . . . Al2 Al -0.34271(7) 0.13182(7) 0.57642(7) 0.00676(15) Uani 1 1 d . . . Al3 Al -0.12369(7) 0.10289(7) 0.15974(7) 0.00655(15) Uani 1 1 d . . . P1 P 0.31252(6) 0.11774(6) 0.59752(6) 0.00647(13) Uani 1 1 d . . . P2 P -0.11663(6) 0.12644(6) 0.81947(6) 0.00637(13) Uani 1 1 d . . . P3 P -0.14891(6) 0.33257(6) 0.35429(6) 0.00653(13) Uani 1 1 d . . . O1 O 0.30132(17) 0.04237(16) 0.46496(17) 0.0119(3) Uani 1 1 d . . . O2 O 0.47259(16) 0.14244(17) 0.61771(18) 0.0114(3) Uani 1 1 d . . . O3 O 0.25279(16) 0.01335(16) 0.73776(17) 0.0105(3) Uani 1 1 d . . . O4 O 0.23436(16) 0.26477(16) 0.56777(17) 0.0082(3) Uani 1 1 d . . . O5 O -0.00180(16) 0.24108(16) 0.76034(16) 0.0083(3) Uani 1 1 d . . . O6 O -0.05358(16) -0.03072(16) 0.82148(18) 0.0101(3) Uani 1 1 d . . . O7 O -0.16787(16) 0.13560(17) 0.97747(17) 0.0103(3) Uani 1 1 d . . . O8 O -0.25195(16) 0.14687(16) 0.72990(17) 0.0094(3) Uani 1 1 d . . . O9 O -0.03283(16) 0.26736(16) 0.46021(17) 0.0088(3) Uani 1 1 d . . . O10 O 0.11115(16) 0.50915(16) 0.40632(17) 0.0081(3) Uani 1 1 d D . . H10A H 0.1902 0.5569 0.3970 0.010 Uiso 0.50 1 d PRD . . O11 O -0.14989(16) 0.50075(15) 0.31161(17) 0.0083(3) Uani 1 1 d . . . O12 O -0.12650(16) 0.27335(16) 0.21044(17) 0.0089(3) Uani 1 1 d . . . O13 O -0.29966(16) 0.27760(16) 0.42794(17) 0.0090(3) Uani 1 1 d . . . O14 O 0.45227(19) 0.3287(2) -0.0201(2) 0.0236(4) Uani 1 1 d . . . N1 N 0.2342(2) 0.3373(2) 0.2106(2) 0.0196(5) Uani 1 1 d D . . C1 C 0.4866(3) 0.2896(3) 0.1317(3) 0.0269(6) Uani 1 1 d . . . H1A H 0.5895 0.3136 0.1408 0.032 Uiso 1 1 calc R . . H1B H 0.4744 0.1814 0.1681 0.032 Uiso 1 1 calc R . . C2 C 0.3887(3) 0.3726(3) 0.2258(3) 0.0234(6) Uani 1 1 d . . . H2A H 0.4130 0.3428 0.3306 0.028 Uiso 1 1 calc R . . H2B H 0.4041 0.4808 0.1932 0.028 Uiso 1 1 calc R . . C3 C 0.2005(3) 0.3725(3) 0.0504(3) 0.0200(6) Uani 1 1 d . . . H3A H 0.2085 0.4807 0.0111 0.024 Uiso 1 1 calc R . . H3B H 0.0996 0.3427 0.0399 0.024 Uiso 1 1 calc R . . C4 C 0.3062(3) 0.2900(3) -0.0361(3) 0.0213(6) Uani 1 1 d . . . H4A H 0.2939 0.1817 -0.0003 0.026 Uiso 1 1 calc R . . H4B H 0.2847 0.3148 -0.1419 0.026 Uiso 1 1 calc R . . H1 H 0.224(3) 0.2398(11) 0.252(3) 0.029(8) Uiso 1 1 d D . . H2 H 0.186(3) 0.395(2) 0.267(3) 0.055(11) 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 0.0069(3) 0.0051(3) 0.0075(3) -0.0011(3) -0.0008(3) -0.0001(2) Al2 0.0064(3) 0.0072(3) 0.0067(3) -0.0014(3) -0.0004(3) -0.0008(2) Al3 0.0073(3) 0.0060(3) 0.0063(3) -0.0015(3) 0.0006(3) -0.0004(2) P1 0.0059(3) 0.0061(3) 0.0072(3) -0.0011(2) 0.0002(2) 0.0002(2) P2 0.0061(3) 0.0066(3) 0.0063(3) -0.0010(2) -0.0005(2) 0.0000(2) P3 0.0075(3) 0.0054(3) 0.0069(3) -0.0016(2) -0.0004(2) -0.0003(2) O1 0.0160(9) 0.0098(8) 0.0109(8) -0.0043(6) -0.0018(7) 0.0020(6) O2 0.0051(8) 0.0149(8) 0.0133(9) -0.0007(7) -0.0001(7) 0.0001(6) O3 0.0103(8) 0.0088(8) 0.0107(8) 0.0009(6) 0.0020(7) -0.0010(6) O4 0.0082(8) 0.0069(7) 0.0091(8) -0.0013(6) -0.0001(6) 0.0014(6) O5 0.0080(8) 0.0084(7) 0.0078(8) -0.0002(6) -0.0006(6) -0.0017(6) O6 0.0081(8) 0.0067(7) 0.0157(9) -0.0025(6) -0.0017(7) 0.0002(6) O7 0.0106(8) 0.0141(8) 0.0061(8) -0.0018(6) 0.0005(6) -0.0012(6) O8 0.0068(8) 0.0137(8) 0.0086(8) -0.0037(6) -0.0024(6) 0.0008(6) O9 0.0086(8) 0.0068(8) 0.0110(8) -0.0015(6) -0.0026(6) 0.0006(6) O10 0.0083(8) 0.0070(7) 0.0088(8) -0.0013(6) 0.0000(6) -0.0002(6) O11 0.0089(8) 0.0059(7) 0.0104(8) -0.0016(6) -0.0021(6) -0.0003(6) O12 0.0127(8) 0.0063(7) 0.0078(8) -0.0021(6) 0.0006(7) 0.0006(6) O13 0.0068(8) 0.0104(8) 0.0086(8) 0.0004(6) 0.0002(6) -0.0010(6) O14 0.0185(10) 0.0320(11) 0.0175(10) -0.0007(8) 0.0058(8) 0.0007(8) N1 0.0215(12) 0.0184(12) 0.0176(12) -0.0024(9) 0.0045(10) -0.0043(9) C1 0.0185(14) 0.0375(17) 0.0210(15) 0.0021(12) -0.0034(12) 0.0064(12) C2 0.0203(14) 0.0305(15) 0.0166(14) 0.0015(11) -0.0003(11) -0.0037(11) C3 0.0147(13) 0.0210(13) 0.0211(14) 0.0027(11) 0.0005(11) -0.0007(10) C4 0.0239(14) 0.0234(14) 0.0166(14) -0.0038(11) -0.0025(12) -0.0023(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 Al1 O4 1.8434(17) . ? Al1 O5 1.8439(16) . ? Al1 O11 1.8907(16) 2_566 ? Al1 O9 1.9112(16) . ? Al1 O10 1.9382(17) . ? Al1 O10 1.9449(17) 2_566 ? Al1 Al1 2.8950(15) 2_566 ? Al2 O8 1.7232(17) . ? Al2 O2 1.7246(17) 1_455 ? Al2 O13 1.7437(17) . ? Al2 O1 1.7541(17) 2_556 ? Al3 O3 1.7197(17) 2_556 ? Al3 O7 1.7246(17) 1_554 ? Al3 O12 1.7291(17) . ? Al3 O6 1.7518(17) 2_556 ? P1 O4 1.5001(15) . ? P1 O2 1.5236(16) . ? P1 O3 1.5274(16) . ? P1 O1 1.5416(17) . ? P2 O5 1.5068(16) . ? P2 O8 1.5239(16) . ? P2 O7 1.5303(16) . ? P2 O6 1.5439(16) . ? P3 O11 1.5162(16) . ? P3 O9 1.5216(16) . ? P3 O12 1.5439(16) . ? P3 O13 1.5557(16) . ? O1 Al2 1.7542(17) 2_556 ? O2 Al2 1.7246(17) 1_655 ? O3 Al3 1.7197(17) 2_556 ? O6 Al3 1.7518(17) 2_556 ? O7 Al3 1.7247(17) 1_556 ? O10 Al1 1.9448(17) 2_566 ? O10 H10A 0.8491 . ? O11 Al1 1.8907(16) 2_566 ? O14 C4 1.422(3) . ? O14 C1 1.431(3) . ? N1 C2 1.486(3) . ? N1 C3 1.502(3) . ? N1 H1 0.904(9) . ? N1 H2 0.915(10) . ? C1 C2 1.520(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Al1 O5 94.67(7) . . ? O4 Al1 O11 93.06(7) . 2_566 ? O5 Al1 O11 93.66(7) . 2_566 ? O4 Al1 O9 92.16(7) . . ? O5 Al1 O9 95.19(7) . . ? O11 Al1 O9 169.32(7) 2_566 . ? O4 Al1 O10 90.93(7) . . ? O5 Al1 O10 174.27(7) . . ? O11 Al1 O10 87.27(7) 2_566 . ? O9 Al1 O10 83.35(7) . . ? O4 Al1 O10 174.46(7) . 2_566 ? O5 Al1 O10 90.83(7) . 2_566 ? O11 Al1 O10 85.91(7) 2_566 2_566 ? O9 Al1 O10 88.00(7) . 2_566 ? O10 Al1 O10 83.59(7) . 2_566 ? O4 Al1 Al1 132.81(6) . 2_566 ? O5 Al1 Al1 132.52(6) . 2_566 ? O11 Al1 Al1 85.42(6) 2_566 2_566 ? O9 Al1 Al1 84.20(6) . 2_566 ? O10 Al1 Al1 41.88(5) . 2_566 ? O10 Al1 Al1 41.71(5) 2_566 2_566 ? O8 Al2 O2 108.62(8) . 1_455 ? O8 Al2 O13 111.29(8) . . ? O2 Al2 O13 107.24(8) 1_455 . ? O8 Al2 O1 108.38(8) . 2_556 ? O2 Al2 O1 108.84(8) 1_455 2_556 ? O13 Al2 O1 112.37(8) . 2_556 ? O3 Al3 O7 107.85(8) 2_556 1_554 ? O3 Al3 O12 111.14(8) 2_556 . ? O7 Al3 O12 106.72(8) 1_554 . ? O3 Al3 O6 112.91(8) 2_556 2_556 ? O7 Al3 O6 110.61(8) 1_554 2_556 ? O12 Al3 O6 107.46(8) . 2_556 ? O4 P1 O2 109.27(9) . . ? O4 P1 O3 112.86(9) . . ? O2 P1 O3 107.17(9) . . ? O4 P1 O1 109.49(9) . . ? O2 P1 O1 108.81(9) . . ? O3 P1 O1 109.14(9) . . ? O5 P2 O8 113.15(9) . . ? O5 P2 O7 110.31(9) . . ? O8 P2 O7 106.43(9) . . ? O5 P2 O6 109.95(9) . . ? O8 P2 O6 108.48(9) . . ? O7 P2 O6 108.35(9) . . ? O11 P3 O9 114.31(8) . . ? O11 P3 O12 107.45(9) . . ? O9 P3 O12 109.77(9) . . ? O11 P3 O13 109.69(9) . . ? O9 P3 O13 107.89(9) . . ? O12 P3 O13 107.54(9) . . ? P1 O1 Al2 137.22(11) . 2_556 ? P1 O2 Al2 154.80(11) . 1_655 ? P1 O3 Al3 153.54(11) . 2_556 ? P1 O4 Al1 147.02(10) . . ? P2 O5 Al1 141.36(10) . . ? P2 O6 Al3 131.79(10) . 2_556 ? P2 O7 Al3 145.96(11) . 1_556 ? P2 O8 Al2 151.60(11) . . ? P3 O9 Al1 126.44(9) . . ? Al1 O10 Al1 96.41(7) . 2_566 ? Al1 O10 H10A 119.6 . . ? Al1 O10 H10A 114.0 2_566 . ? P3 O11 Al1 126.62(10) . 2_566 ? P3 O12 Al3 137.33(10) . . ? P3 O13 Al2 130.13(10) . . ? C4 O14 C1 110.27(19) . . ? C2 N1 C3 109.79(19) . . ? C2 N1 H1 105.9(18) . . ? C3 N1 H1 112.3(17) . . ? C2 N1 H2 102(2) . . ? C3 N1 H2 115(2) . . ? H1 N1 H2 111.2(15) . . ? O14 C1 C2 111.0(2) . . ? O14 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? O14 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C1 109.2(2) . . ? N1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? N1 C3 C4 109.7(2) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O14 C4 C3 110.7(2) . . ? O14 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? O14 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 P1 O1 Al2 -170.91(13) . . . 2_556 ? O2 P1 O1 Al2 69.73(17) . . . 2_556 ? O3 P1 O1 Al2 -46.92(17) . . . 2_556 ? O4 P1 O2 Al2 -121.1(3) . . . 1_655 ? O3 P1 O2 Al2 116.3(3) . . . 1_655 ? O1 P1 O2 Al2 -1.6(3) . . . 1_655 ? O4 P1 O3 Al3 71.8(3) . . . 2_556 ? O2 P1 O3 Al3 -167.8(2) . . . 2_556 ? O1 P1 O3 Al3 -50.1(3) . . . 2_556 ? O2 P1 O4 Al1 -148.32(17) . . . . ? O3 P1 O4 Al1 -29.2(2) . . . . ? O1 P1 O4 Al1 92.6(2) . . . . ? O5 Al1 O4 P1 28.4(2) . . . . ? O11 Al1 O4 P1 122.36(19) 2_566 . . . ? O9 Al1 O4 P1 -67.0(2) . . . . ? O10 Al1 O4 P1 -150.33(19) . . . . ? O10 Al1 O4 P1 -158.5(7) 2_566 . . . ? Al1 Al1 O4 P1 -151.05(15) 2_566 . . . ? O8 P2 O5 Al1 -25.09(19) . . . . ? O7 P2 O5 Al1 -144.18(14) . . . . ? O6 P2 O5 Al1 96.38(16) . . . . ? O4 Al1 O5 P2 -110.75(16) . . . . ? O11 Al1 O5 P2 155.87(15) 2_566 . . . ? O9 Al1 O5 P2 -18.15(17) . . . . ? O10 Al1 O5 P2 56.7(8) . . . . ? O10 Al1 O5 P2 69.92(16) 2_566 . . . ? Al1 Al1 O5 P2 68.73(18) 2_566 . . . ? O5 P2 O6 Al3 28.81(16) . . . 2_556 ? O8 P2 O6 Al3 153.02(13) . . . 2_556 ? O7 P2 O6 Al3 -91.82(14) . . . 2_556 ? O5 P2 O7 Al3 -71.4(2) . . . 1_556 ? O8 P2 O7 Al3 165.49(17) . . . 1_556 ? O6 P2 O7 Al3 49.0(2) . . . 1_556 ? O5 P2 O8 Al2 76.4(2) . . . . ? O7 P2 O8 Al2 -162.3(2) . . . . ? O6 P2 O8 Al2 -45.9(2) . . . . ? O2 Al2 O8 P2 161.3(2) 1_455 . . . ? O13 Al2 O8 P2 -80.9(2) . . . . ? O1 Al2 O8 P2 43.2(2) 2_556 . . . ? O11 P3 O9 Al1 21.41(15) . . . . ? O12 P3 O9 Al1 142.20(11) . . . . ? O13 P3 O9 Al1 -100.89(12) . . . . ? O4 Al1 O9 P3 -146.12(12) . . . . ? O5 Al1 O9 P3 118.99(12) . . . . ? O11 Al1 O9 P3 -26.8(5) 2_566 . . . ? O10 Al1 O9 P3 -55.44(12) . . . . ? O10 Al1 O9 P3 28.34(12) 2_566 . . . ? Al1 Al1 O9 P3 -13.30(11) 2_566 . . . ? O4 Al1 O10 Al1 -179.21(8) . . . 2_566 ? O5 Al1 O10 Al1 13.3(7) . . . 2_566 ? O11 Al1 O10 Al1 -86.19(7) 2_566 . . 2_566 ? O9 Al1 O10 Al1 88.72(7) . . . 2_566 ? O10 Al1 O10 Al1 0.0 2_566 . . 2_566 ? O9 P3 O11 Al1 -17.89(15) . . . 2_566 ? O12 P3 O11 Al1 -139.96(11) . . . 2_566 ? O13 P3 O11 Al1 103.42(12) . . . 2_566 ? O11 P3 O12 Al3 -174.96(13) . . . . ? O9 P3 O12 Al3 60.19(17) . . . . ? O13 P3 O12 Al3 -56.94(17) . . . . ? O3 Al3 O12 P3 37.77(17) 2_556 . . . ? O7 Al3 O12 P3 155.11(14) 1_554 . . . ? O6 Al3 O12 P3 -86.23(16) 2_556 . . . ? O11 P3 O13 Al2 -141.75(12) . . . . ? O9 P3 O13 Al2 -16.65(15) . . . . ? O12 P3 O13 Al2 101.69(13) . . . . ? O8 Al2 O13 P3 54.39(15) . . . . ? O2 Al2 O13 P3 173.07(12) 1_455 . . . ? O1 Al2 O13 P3 -67.37(14) 2_556 . . . ? C4 O14 C1 C2 -61.2(3) . . . . ? C3 N1 C2 C1 -55.5(3) . . . . ? O14 C1 C2 N1 58.5(3) . . . . ? C2 N1 C3 C4 55.6(3) . . . . ? C1 O14 C4 C3 60.9(3) . . . . ? N1 C3 C4 O14 -58.2(3) . . . . ? 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 N1 H1 O1 0.904(9) 2.516(19) 3.277(3) 142(2) . N1 H2 O10 0.915(10) 1.913(12) 2.820(3) 170(3) . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.551 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.095