# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1697 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; XU, Ruren Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; _publ_contact_author_phone '86 431 8922331 2479' _publ_contact_author_fax '86 431 5671974' _publ_contact_author_email 'rrxu@mail.jlu.edu.cn' _publ_requested_journal 'Chem. Commun.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; A Novel Open-framework Aluminophosphate [AlP2O6(OH)2][H3O] Containing Propeller-like Chiral Motifs ; loop_ _publ_author_name _publ_author_address 'YAN, Wenfu' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; 'YU, Jihong' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; 'SHI, Zhan' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; 'XU, Ruren' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; #complex yp-1 data_yp-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H7.50 Al1.50 O13.50 P3' _chemical_formula_weight 356.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' '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' _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 7.1177(18) _cell_length_b 8.6729(16) _cell_length_c 9.220(3) _cell_angle_alpha 65.108(16) _cell_angle_beta 70.521(13) _cell_angle_gamma 68.504(16) _cell_volume 469.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.859 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1114 _diffrn_reflns_av_R_equivalents 0.0115 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 23.25 _reflns_number_total 1107 _reflns_number_gt 963 _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^)+(0.0667P)^2^+1.3544P] 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 1107 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1098 _refine_ls_wR_factor_gt 0.1050 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 P1 P 0.0792(2) 0.62331(17) 1.27025(16) 0.0134(4) Uani 1 1 d . . . P2 P 0.0858(2) 0.85076(17) 0.71774(16) 0.0136(4) Uani 1 1 d . . . P3 P 0.5559(2) 0.94611(17) 0.27960(16) 0.0138(5) Uani 1 1 d . . . Al1 Al 0.0000 1.0000 1.0000 0.0145(6) Uani 1 2 d S . . Al2 Al 0.2021(3) 1.21624(19) 0.44701(18) 0.0145(5) Uani 1 1 d . . . O1 O -0.1116(6) 0.5853(4) 1.2498(4) 0.0193(10) Uani 1 1 d . . . H1 H -0.1493 0.5072 1.3322 0.080 Uiso 1 1 calc . . . O2 O 0.0196(6) 0.6828(4) 1.4162(4) 0.0157(10) Uani 1 1 d . . . O3 O 0.2476(6) 0.4483(4) 1.2962(4) 0.0145(9) Uani 1 1 d . . . O4 O 0.1487(6) 0.7648(4) 1.1114(4) 0.0166(10) Uani 1 1 d . . . O5 O -0.0542(6) 0.9166(4) 0.8581(4) 0.0153(9) Uani 1 1 d . . . O6 O -0.0232(6) 0.7508(4) 0.6849(4) 0.0150(9) Uani 1 1 d . . . O7 O 0.2814(6) 0.7025(5) 0.7777(4) 0.0187(10) Uani 1 1 d . . . H7 H 0.3527 0.6620 0.7049 0.080 Uiso 1 1 calc . . . O8 O 0.1649(6) 0.9908(4) 0.5683(4) 0.0163(10) Uani 1 1 d . . . O9 O 0.4296(6) 1.1277(4) 0.2933(4) 0.0152(9) Uani 1 1 d . . . O10 O 0.6083(6) 0.8108(4) 0.4395(4) 0.0150(10) Uani 1 1 d . . . O11 O 0.4164(6) 0.8695(5) 0.2393(4) 0.0224(10) Uani 1 1 d . . . H11 H 0.3816 0.9366 0.1527 0.080 Uiso 1 1 calc . . . O12 O 0.7423(6) 0.9683(4) 0.1400(4) 0.0183(10) Uani 1 1 d . . . O1W O 0.5000 0.5000 0.5000 0.057(2) Uani 1 2 d S . . O2W O 0.3799(9) 0.3387(6) 0.9742(6) 0.0543(15) Uani 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 P1 0.0215(12) 0.0074(7) 0.0109(7) -0.0018(6) -0.0053(6) -0.0032(7) P2 0.0205(12) 0.0084(7) 0.0126(7) -0.0023(6) -0.0056(7) -0.0041(7) P3 0.0224(12) 0.0090(7) 0.0102(7) -0.0019(5) -0.0049(7) -0.0047(7) Al1 0.0219(19) 0.0100(11) 0.0116(11) -0.0032(9) -0.0053(10) -0.0033(11) Al2 0.0232(14) 0.0092(8) 0.0109(8) -0.0024(6) -0.0048(8) -0.0043(8) O1 0.026(3) 0.0122(19) 0.0206(19) -0.0037(16) -0.0081(18) -0.0053(18) O2 0.023(3) 0.0118(18) 0.0130(19) -0.0049(15) -0.0048(17) -0.0033(18) O3 0.020(3) 0.0093(18) 0.0126(18) -0.0027(15) -0.0043(17) -0.0031(18) O4 0.025(3) 0.0102(18) 0.0120(19) -0.0011(15) -0.0043(17) -0.0042(18) O5 0.020(3) 0.0145(19) 0.0130(18) -0.0070(15) -0.0032(17) -0.0037(18) O6 0.023(3) 0.0088(17) 0.0132(18) -0.0014(15) -0.0076(17) -0.0040(18) O7 0.021(3) 0.0124(19) 0.019(2) -0.0050(16) -0.0057(18) 0.0006(18) O8 0.024(3) 0.0123(18) 0.0130(19) -0.0026(15) -0.0044(18) -0.0069(18) O9 0.020(3) 0.0096(18) 0.0129(19) -0.0037(15) -0.0030(17) -0.0007(18) O10 0.022(3) 0.0102(18) 0.0118(18) -0.0020(15) -0.0062(17) -0.0035(18) O11 0.034(3) 0.015(2) 0.023(2) -0.0052(17) -0.0137(19) -0.005(2) O12 0.027(3) 0.0129(19) 0.0127(19) -0.0028(15) -0.0035(18) -0.0053(19) O1W 0.080(7) 0.049(4) 0.049(4) -0.014(4) -0.009(4) -0.029(4) O2W 0.074(5) 0.043(3) 0.036(3) -0.007(2) -0.016(3) -0.007(3) _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 P1 O2 1.517(4) . ? P1 O4 1.531(4) . ? P1 O3 1.533(4) . ? P1 O1 1.593(4) . ? P2 O8 1.505(4) . ? P2 O6 1.522(4) . ? P2 O5 1.529(4) . ? P2 O7 1.581(4) . ? P3 O10 1.510(3) . ? P3 O12 1.514(4) . ? P3 O9 1.536(4) . ? P3 O11 1.582(4) . ? Al1 O12 1.897(4) 1_456 ? Al1 O12 1.897(4) 2_676 ? Al1 O4 1.927(4) 2_577 ? Al1 O4 1.927(4) . ? Al1 O5 1.929(3) 2_577 ? Al1 O5 1.929(3) . ? Al2 O2 1.854(4) 2_577 ? Al2 O10 1.864(4) 2_676 ? Al2 O8 1.867(3) . ? Al2 O6 1.912(4) 2_576 ? Al2 O9 1.922(4) . ? Al2 O3 1.978(3) 1_564 ? O1 H1 0.8200 . ? O2 Al2 1.854(4) 2_577 ? O3 Al2 1.978(3) 1_546 ? O6 Al2 1.912(4) 2_576 ? O7 H7 0.8200 . ? O10 Al2 1.864(4) 2_676 ? O11 H11 0.8200 . ? O12 Al1 1.897(4) 1_654 ? 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 O2 P1 O4 111.16(19) . . ? O2 P1 O3 110.4(2) . . ? O4 P1 O3 111.0(2) . . ? O2 P1 O1 110.9(2) . . ? O4 P1 O1 107.5(2) . . ? O3 P1 O1 105.6(2) . . ? O8 P2 O6 114.46(19) . . ? O8 P2 O5 114.2(2) . . ? O6 P2 O5 108.5(2) . . ? O8 P2 O7 106.9(2) . . ? O6 P2 O7 102.8(2) . . ? O5 P2 O7 109.2(2) . . ? O10 P3 O12 113.9(2) . . ? O10 P3 O9 113.0(2) . . ? O12 P3 O9 108.9(2) . . ? O10 P3 O11 103.7(2) . . ? O12 P3 O11 108.7(2) . . ? O9 P3 O11 108.4(2) . . ? O12 Al1 O12 180.000(1) 1_456 2_676 ? O12 Al1 O4 87.02(16) 1_456 2_577 ? O12 Al1 O4 92.98(16) 2_676 2_577 ? O12 Al1 O4 92.98(16) 1_456 . ? O12 Al1 O4 87.02(16) 2_676 . ? O4 Al1 O4 180.0(2) 2_577 . ? O12 Al1 O5 92.11(15) 1_456 2_577 ? O12 Al1 O5 87.89(15) 2_676 2_577 ? O4 Al1 O5 90.81(14) 2_577 2_577 ? O4 Al1 O5 89.19(14) . 2_577 ? O12 Al1 O5 87.89(15) 1_456 . ? O12 Al1 O5 92.11(15) 2_676 . ? O4 Al1 O5 89.19(14) 2_577 . ? O4 Al1 O5 90.81(14) . . ? O5 Al1 O5 180.000(1) 2_577 . ? O2 Al2 O10 92.79(17) 2_577 2_676 ? O2 Al2 O8 92.70(17) 2_577 . ? O10 Al2 O8 93.85(16) 2_676 . ? O2 Al2 O6 90.63(17) 2_577 2_576 ? O10 Al2 O6 175.53(19) 2_676 2_576 ? O8 Al2 O6 88.85(16) . 2_576 ? O2 Al2 O9 175.96(17) 2_577 . ? O10 Al2 O9 88.54(17) 2_676 . ? O8 Al2 O9 91.01(16) . . ? O6 Al2 O9 87.85(17) 2_576 . ? O2 Al2 O3 92.17(16) 2_577 1_564 ? O10 Al2 O3 90.19(15) 2_676 1_564 ? O8 Al2 O3 173.51(16) . 1_564 ? O6 Al2 O3 86.81(15) 2_576 1_564 ? O9 Al2 O3 84.01(15) . 1_564 ? P1 O1 H1 109.5 . . ? P1 O2 Al2 143.7(3) . 2_577 ? P1 O3 Al2 124.9(2) . 1_546 ? P1 O4 Al1 131.0(2) . . ? P2 O5 Al1 132.1(2) . . ? P2 O6 Al2 141.7(2) . 2_576 ? P2 O7 H7 109.5 . . ? P2 O8 Al2 155.1(2) . . ? P3 O9 Al2 136.6(2) . . ? P3 O10 Al2 130.8(2) . 2_676 ? P3 O11 H11 109.5 . . ? P3 O12 Al1 167.0(2) . 1_654 ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.824 _refine_diff_density_max 0.524 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.100