# 1. SUBMISSION DETAILS _publ_contact_autor ; YU, Jihong State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; _publ_contact_author_phone '86 431 5168608' _publ_contact_author_fax '86 431 5168608' _publ_contact_author_email 'jihong@mail.jlu.edu.cn' _publ_requested_journal 'Inorg.Chem.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; synthesis, crystal structure, and solid-state NMR spectroscopy of a new open-framework aluminophosphate (NH4)2Al4(PO4)4(HPO4)H2O ; loop_ _publ_author_name _publ_author_address 'ZHOU, Dan' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; 'CHEN, Lei' ; State Key Lab of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics, The Chinese Academy of Sciences Wuhan 430071 P. R. China ; YU, Jihong' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; 'LI, Yi' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; 'YAN, Wenfu' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; 'DENG, Feng' ; State Key Lab of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics, The Chinese Academy of Sciences Wuhan 430071 P. R. China ; 'XU, Ruren' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry Jilin University Changchun 130012 P. R. China ; #complex AlPO-CJ19 data_P2(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H11 Al4 N2 O21 P5' _chemical_formula_weight 637.88 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' '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' '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.0568(3) _cell_length_b 21.6211(18) _cell_length_c 8.1724(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.361(4) _cell_angle_gamma 90.00 _cell_volume 893.27(10) _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 platelike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type none _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4664 _diffrn_reflns_av_R_equivalents 0.0655 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2046 _reflns_number_gt 1485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0837P)^2^+2.8701P] 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 0.6(3) _refine_ls_number_reflns 2046 _refine_ls_number_parameters 289 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_restrained_S_all 0.783 _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 Al1 Al 2.0276(8) 0.33558(16) 1.6854(4) 0.0143(8) Uani 1 1 d . . . Al2 Al 0.9624(7) 0.58026(15) 1.0340(4) 0.0115(8) Uani 1 1 d . . . Al3 Al 1.4642(6) 0.17269(16) 1.5289(4) 0.0108(8) Uani 1 1 d . . . Al4 Al 1.5293(7) 0.41577(16) 1.1811(4) 0.0112(8) Uani 1 1 d . . . P1 P 1.5073(6) 0.32133(14) 1.4718(3) 0.0131(7) Uani 1 1 d . . . P2 P 1.9621(6) 0.20053(14) 1.7574(3) 0.0097(7) Uani 1 1 d . . . P3 P 1.4730(6) 0.55315(14) 1.2506(4) 0.0107(7) Uani 1 1 d . . . P4 P 1.0042(6) 0.42942(14) 0.9724(3) 0.0093(7) Uani 1 1 d . . . P5 P 0.9735(5) 0.11932(13) 1.3276(3) 0.0156(6) Uani 1 1 d . . . O1 O 1.7999(14) 0.3323(4) 1.5225(8) 0.0075(16) Uani 1 1 d . . . O2 O 1.4551(17) 0.3553(4) 1.3103(9) 0.0171(19) Uani 1 1 d . . . O3 O 1.4336(16) 0.2546(4) 1.4472(9) 0.0171(19) Uani 1 1 d . . . O4 O 1.3411(16) 0.3516(4) 1.6049(9) 0.021(2) Uani 1 1 d . . . O5 O 1.6733(16) 0.1974(4) 1.7035(9) 0.0151(19) Uani 1 1 d . . . O6 O 2.0252(17) 0.2686(4) 1.8028(10) 0.021(2) Uani 1 1 d . . . O7 O 2.0158(17) 0.1649(4) 1.9192(9) 0.019(2) Uani 1 1 d . . . O8 O 1.1471(16) 0.1788(4) 1.6297(10) 0.026(2) Uani 1 1 d . . . O9 O 1.5469(15) 0.4840(4) 1.2864(9) 0.0167(19) Uani 1 1 d U . . O10 O 1.5228(16) 0.5883(4) 1.4065(10) 0.020(2) Uani 1 1 d . . . O11 O 1.6326(16) 0.5752(4) 1.1065(11) 0.026(2) Uani 1 1 d U . . O12 O 1.1777(14) 0.5568(4) 1.2054(9) 0.0102(18) Uani 1 1 d . . . O13 O 0.9288(17) 0.4961(4) 0.9572(9) 0.022(2) Uani 1 1 d . . . O14 O 0.9497(15) 0.4001(4) 0.8052(9) 0.018(2) Uani 1 1 d . . . O15 O 0.8332(17) 0.3971(4) 1.1019(9) 0.019(2) Uani 1 1 d . . . O16 O 1.2907(17) 0.4211(4) 1.0172(10) 0.023(2) Uani 1 1 d . . . O17 O 1.2460(13) 0.1474(3) 1.3336(7) 0.0198(16) Uani 1 1 d . . . O18 O 1.0991(16) 0.5956(4) 0.8445(8) 0.0266(19) Uani 1 1 d . . . O19 O 1.7550(15) 0.1610(4) 1.3840(7) 0.0236(18) Uani 1 1 d . . . O20 O 0.9740(18) 0.0558(5) 1.4318(11) 0.030(2) Uani 1 1 d . . . H1 H 0.9383 0.0268 1.3707 0.080 Uiso 1 1 calc . . . O1W O 1.512(2) 0.4922(7) 0.6813(13) 0.065(4) Uani 1 1 d . . . N2 N 1.987(3) 0.2650(9) 1.1874(19) 0.063(5) Uani 1 1 d . . . N3 N 1.505(2) 0.2110(6) 1.0781(12) 0.030(3) 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 Al1 0.024(2) 0.0082(18) 0.0105(16) -0.0013(16) 0.0037(14) -0.0008(17) Al2 0.0165(19) 0.008(2) 0.0103(17) -0.0019(14) -0.0016(14) 0.0015(16) Al3 0.0009(16) 0.016(2) 0.0158(17) 0.0023(16) 0.0030(13) 0.0001(16) Al4 0.0037(16) 0.015(2) 0.0153(17) 0.0022(16) -0.0004(12) 0.0010(16) P1 0.0112(17) 0.0136(19) 0.0147(16) -0.0002(13) 0.0006(13) -0.0001(13) P2 0.0121(16) 0.0086(17) 0.0086(14) 0.0013(11) 0.0042(12) -0.0017(13) P3 0.0071(15) 0.0078(18) 0.0171(15) 0.0000(13) -0.0047(12) -0.0023(13) P4 0.0075(15) 0.0120(17) 0.0086(15) -0.0033(13) 0.0029(11) -0.0015(13) P5 0.0171(13) 0.0167(14) 0.0131(12) -0.0013(11) -0.0007(9) 0.0017(11) O1 0.003(4) 0.014(4) 0.005(3) 0.000(3) 0.002(3) -0.002(3) O2 0.028(5) 0.003(4) 0.020(4) 0.005(4) 0.002(4) -0.004(4) O3 0.020(5) 0.018(5) 0.013(4) 0.002(4) -0.009(3) 0.001(4) O4 0.010(4) 0.034(6) 0.020(4) -0.010(4) 0.008(3) -0.012(4) O5 0.018(5) 0.012(5) 0.015(4) 0.008(4) -0.002(4) 0.001(4) O6 0.029(5) 0.017(5) 0.017(4) 0.010(4) -0.014(4) -0.006(4) O7 0.028(5) 0.007(4) 0.023(5) 0.002(4) -0.006(4) 0.002(4) O8 0.024(4) 0.024(5) 0.031(5) 0.002(4) 0.018(4) 0.003(4) O9 0.017(3) 0.009(4) 0.024(3) 0.005(3) -0.005(3) 0.005(3) O10 0.018(5) 0.020(5) 0.022(5) -0.008(4) -0.011(4) 0.002(4) O11 0.016(4) 0.031(4) 0.033(4) 0.003(3) 0.012(3) -0.006(3) O12 0.003(4) 0.019(5) 0.009(4) 0.006(3) 0.004(3) 0.001(4) O13 0.024(5) 0.017(5) 0.025(5) -0.004(4) -0.011(4) 0.009(4) O14 0.005(4) 0.034(6) 0.013(4) -0.009(4) -0.002(3) 0.011(4) O15 0.021(5) 0.014(5) 0.020(4) 0.005(4) 0.001(4) -0.014(4) O16 0.022(5) 0.026(6) 0.022(4) 0.005(4) -0.002(3) 0.007(4) O17 0.023(4) 0.025(4) 0.011(3) 0.002(3) 0.003(3) -0.001(3) O18 0.029(5) 0.033(5) 0.018(4) 0.005(3) 0.007(3) -0.008(4) O19 0.036(5) 0.022(4) 0.013(3) -0.005(3) 0.002(3) 0.009(4) O20 0.026(5) 0.037(6) 0.028(5) -0.003(4) 0.013(4) -0.014(4) O1W 0.070(8) 0.093(10) 0.031(6) 0.023(7) -0.006(5) 0.018(8) N2 0.035(8) 0.079(12) 0.075(11) -0.001(10) 0.011(8) 0.002(8) N3 0.007(5) 0.073(9) 0.009(5) 0.005(5) -0.004(4) -0.001(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 O6 1.738(8) . ? Al1 O1 1.741(8) . ? Al1 O14 1.755(9) 1_656 ? Al1 O4 1.764(8) 1_655 ? Al2 O18 1.742(7) . ? Al2 O11 1.787(8) 1_455 ? Al2 O12 1.826(8) . ? Al2 O7 1.873(9) 2_858 ? Al2 O13 1.932(10) . ? Al3 O8 1.825(8) . ? Al3 O5 1.835(9) . ? Al3 O3 1.897(10) . ? Al3 O10 1.900(10) 2_848 ? Al3 O19 1.926(8) . ? Al3 O17 1.995(7) . ? Al4 O9 1.709(9) . ? Al4 O2 1.728(8) . ? Al4 O15 1.729(9) 1_655 ? Al4 O16 1.785(9) . ? P1 O3 1.503(10) . ? P1 O2 1.527(8) . ? P1 O4 1.537(8) . ? P1 O1 1.546(8) . ? P2 O8 1.494(8) 1_655 ? P2 O5 1.517(9) . ? P2 O7 1.548(8) . ? P2 O6 1.549(9) . ? P3 O10 1.500(9) . ? P3 O11 1.519(8) . ? P3 O12 1.532(8) . ? P3 O9 1.568(9) . ? P4 O13 1.495(10) . ? P4 O16 1.496(9) . ? P4 O14 1.525(8) . ? P4 O15 1.549(8) . ? P5 O17 1.506(7) . ? P5 O19 1.506(7) 1_455 ? P5 O18 1.533(7) 2_747 ? P5 O20 1.615(10) . ? O4 Al1 1.764(8) 1_455 ? O7 Al2 1.873(9) 2_848 ? O8 P2 1.494(8) 1_455 ? O10 Al3 1.900(10) 2_858 ? O11 Al2 1.787(8) 1_655 ? O14 Al1 1.755(9) 1_454 ? O15 Al4 1.729(9) 1_455 ? O18 P5 1.533(7) 2_757 ? O19 P5 1.506(7) 1_655 ? O20 H1 0.8200 . ? 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 O6 Al1 O1 112.1(4) . . ? O6 Al1 O14 110.5(4) . 1_656 ? O1 Al1 O14 107.8(4) . 1_656 ? O6 Al1 O4 112.8(5) . 1_655 ? O1 Al1 O4 107.9(4) . 1_655 ? O14 Al1 O4 105.5(4) 1_656 1_655 ? O18 Al2 O11 134.4(5) . 1_455 ? O18 Al2 O12 119.5(4) . . ? O11 Al2 O12 105.8(4) 1_455 . ? O18 Al2 O7 88.5(4) . 2_858 ? O11 Al2 O7 92.5(4) 1_455 2_858 ? O12 Al2 O7 94.8(4) . 2_858 ? O18 Al2 O13 85.7(4) . . ? O11 Al2 O13 88.5(4) 1_455 . ? O12 Al2 O13 92.0(4) . . ? O7 Al2 O13 172.7(4) 2_858 . ? O8 Al3 O5 97.1(4) . . ? O8 Al3 O3 91.5(4) . . ? O5 Al3 O3 92.4(4) . . ? O8 Al3 O10 88.2(4) . 2_848 ? O5 Al3 O10 92.7(4) . 2_848 ? O3 Al3 O10 174.8(4) . 2_848 ? O8 Al3 O19 168.2(4) . . ? O5 Al3 O19 94.7(4) . . ? O3 Al3 O19 87.9(4) . . ? O10 Al3 O19 91.3(4) 2_848 . ? O8 Al3 O17 84.6(4) . . ? O5 Al3 O17 177.9(4) . . ? O3 Al3 O17 86.3(3) . . ? O10 Al3 O17 88.5(4) 2_848 . ? O19 Al3 O17 83.6(3) . . ? O9 Al4 O2 110.8(4) . . ? O9 Al4 O15 110.7(4) . 1_655 ? O2 Al4 O15 105.1(4) . 1_655 ? O9 Al4 O16 110.4(4) . . ? O2 Al4 O16 110.8(5) . . ? O15 Al4 O16 109.0(4) 1_655 . ? O3 P1 O2 108.0(5) . . ? O3 P1 O4 111.4(5) . . ? O2 P1 O4 108.7(5) . . ? O3 P1 O1 114.6(5) . . ? O2 P1 O1 107.6(4) . . ? O4 P1 O1 106.3(4) . . ? O8 P2 O5 113.4(5) 1_655 . ? O8 P2 O7 109.9(5) 1_655 . ? O5 P2 O7 112.0(5) . . ? O8 P2 O6 109.7(5) 1_655 . ? O5 P2 O6 107.7(5) . . ? O7 P2 O6 103.7(5) . . ? O10 P3 O11 114.7(6) . . ? O10 P3 O12 108.8(5) . . ? O11 P3 O12 109.2(5) . . ? O10 P3 O9 106.9(5) . . ? O11 P3 O9 108.4(5) . . ? O12 P3 O9 108.8(5) . . ? O13 P4 O16 112.3(5) . . ? O13 P4 O14 106.6(5) . . ? O16 P4 O14 108.8(5) . . ? O13 P4 O15 110.2(5) . . ? O16 P4 O15 109.4(5) . . ? O14 P4 O15 109.5(5) . . ? O17 P5 O19 115.3(4) . 1_455 ? O17 P5 O18 111.3(4) . 2_747 ? O19 P5 O18 108.6(4) 1_455 2_747 ? O17 P5 O20 109.6(5) . . ? O19 P5 O20 109.8(4) 1_455 . ? O18 P5 O20 101.3(5) 2_747 . ? P1 O1 Al1 145.4(5) . . ? P1 O2 Al4 148.9(6) . . ? P1 O3 Al3 146.2(5) . . ? P1 O4 Al1 133.8(6) . 1_455 ? P2 O5 Al3 140.5(5) . . ? P2 O6 Al1 131.6(5) . . ? P2 O7 Al2 132.0(5) . 2_848 ? P2 O8 Al3 155.5(7) 1_455 . ? P3 O9 Al4 136.0(5) . . ? P3 O10 Al3 136.6(6) . 2_858 ? P3 O11 Al2 142.5(7) . 1_655 ? P3 O12 Al2 139.4(5) . . ? P4 O13 Al2 149.4(5) . . ? P4 O14 Al1 142.4(6) . 1_454 ? P4 O15 Al4 131.8(6) . 1_455 ? P4 O16 Al4 145.5(6) . . ? P5 O17 Al3 128.7(4) . . ? P5 O18 Al2 141.9(5) 2_757 . ? P5 O19 Al3 147.5(5) 1_655 . ? P5 O20 H1 109.5 . . ? 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 O20 H1 O1W 0.82 2.42 2.944(16) 122.4 2_747 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.493 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.121