Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 # 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 'J. Mater. Chem.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; A new layered aluminophosphate [C4H12N2][Al2P2O8(OH)2] templated by piperazine ; loop_ _publ_author_name _publ_author_address 'Wang, Kaixue' ; 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 ; 'Miao, Peng' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; 'Song, Yu' ; Key Lab of Inorganic Synthesis and Preparative Chemistry Department of Chemistry Jilin University Changchun 130023 P. R. China ; 'Li, Jiyang' ; 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 B010206G data_CJ9 _database_code_CSD 163034 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H7 Al N O5 P' _chemical_formula_weight 183.04 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' '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8835(19) _cell_length_b 6.8743(15) _cell_length_c 9.5526(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.820(5) _cell_angle_gamma 90.00 _cell_volume 582.1(2) _cell_formula_units_Z 4 _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 0.320 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.583 _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 1310 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 23.23 _reflns_number_total 692 _reflns_number_gt 568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material '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^)+(0.0370P)^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 692 _refine_ls_number_parameters 119 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.098 _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 0.79719(10) -0.39663(12) 0.93101(11) 0.0156(3) Uani 1 1 d . . . Al1 Al 0.96428(11) -0.13980(14) 0.71953(12) 0.0156(4) Uani 1 1 d . . . O1 O 0.8797(3) -0.2160(3) 0.8796(3) 0.0208(7) Uani 1 1 d . . . O2 O 0.6317(3) -0.3899(3) 0.8815(3) 0.0218(7) Uani 1 1 d . . . O3 O 0.8104(3) -0.3961(3) 1.0920(3) 0.0178(7) Uani 1 1 d . . . O4 O 0.8697(3) -0.5813(3) 0.8763(3) 0.0204(7) Uani 1 1 d . . . O5 O 1.0155(3) -0.3992(3) 0.6913(4) 0.0221(8) Uani 1 1 d . . . N1 N 0.5154(4) -0.5468(5) 0.6451(4) 0.0212(9) Uani 1 1 d D . . C1 C 0.4242(5) -0.3763(6) 0.5939(5) 0.0258(11) Uani 1 1 d . . . C2 C 0.6393(4) -0.5915(6) 0.5542(4) 0.0245(11) Uani 1 1 d . . . H1 H 0.460(5) -0.656(6) 0.650(4) 0.034(12) Uiso 1 1 d . . . H2 H 0.541(4) -0.525(6) 0.730(3) 0.024(13) Uiso 1 1 d D . . H3 H 0.343(5) -0.359(5) 0.650(4) 0.029(12) Uiso 1 1 d . . . H4 H 0.495(4) -0.260(6) 0.593(4) 0.029(10) Uiso 1 1 d . . . H5 H 0.709(4) -0.477(5) 0.553(3) 0.018(9) Uiso 1 1 d . . . H6 H 0.686(4) -0.716(5) 0.587(3) 0.016(9) Uiso 1 1 d . . . H7 H 1.046(5) -0.399(6) 0.612(5) 0.039(18) Uiso 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 0.0151(5) 0.0131(5) 0.0184(8) -0.0001(4) -0.0007(5) 0.0005(4) Al1 0.0157(6) 0.0122(6) 0.0183(9) 0.0000(5) -0.0025(5) -0.0001(4) O1 0.0282(15) 0.0161(13) 0.0187(19) -0.0010(11) 0.0058(13) -0.0012(10) O2 0.0162(13) 0.0234(15) 0.0249(19) -0.0044(11) -0.0059(12) 0.0034(10) O3 0.0180(14) 0.0217(14) 0.013(2) 0.0005(10) -0.0011(12) -0.0022(10) O4 0.0190(14) 0.0158(13) 0.0268(19) 0.0000(11) 0.0043(12) -0.0012(10) O5 0.0320(17) 0.0166(15) 0.019(2) 0.0035(12) 0.0079(15) 0.0051(11) N1 0.027(2) 0.0222(18) 0.014(3) 0.0002(16) -0.0054(18) -0.0037(15) C1 0.026(2) 0.022(2) 0.030(4) -0.0034(18) 0.001(2) 0.0024(18) C2 0.027(2) 0.024(2) 0.022(3) -0.0003(18) -0.001(2) 0.0006(18) _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 1.514(3) . ? P1 O4 1.531(2) . ? P1 O3 1.535(3) . ? P1 O1 1.539(3) . ? Al1 O3 1.787(2) 4 ? Al1 O1 1.825(3) . ? Al1 O4 1.831(3) 2_756 ? Al1 O5 1.863(3) 2_756 ? Al1 O5 1.864(2) . ? O3 Al1 1.787(2) 4_556 ? O4 Al1 1.831(3) 2_746 ? O5 Al1 1.863(3) 2_746 ? O5 H7 0.82(5) . ? N1 C2 1.479(5) . ? N1 C1 1.489(5) . ? N1 H1 0.90(4) . ? N1 H2 0.84(3) . ? C1 C2 1.504(6) 3_646 ? C1 H3 0.94(4) . ? C1 H4 1.02(4) . ? C2 C1 1.504(6) 3_646 ? C2 H5 1.00(4) . ? C2 H6 0.99(3) . ? 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 109.90(13) . . ? O2 P1 O3 108.68(15) . . ? O4 P1 O3 109.79(14) . . ? O2 P1 O1 110.41(14) . . ? O4 P1 O1 109.87(15) . . ? O3 P1 O1 108.15(13) . . ? O3 Al1 O1 105.77(12) 4 . ? O3 Al1 O4 103.54(13) 4 2_756 ? O1 Al1 O4 150.69(12) . 2_756 ? O3 Al1 O5 103.59(12) 4 2_756 ? O1 Al1 O5 84.51(14) . 2_756 ? O4 Al1 O5 88.69(13) 2_756 2_756 ? O3 Al1 O5 102.51(12) 4 . ? O1 Al1 O5 87.98(14) . . ? O4 Al1 O5 85.72(13) 2_756 . ? O5 Al1 O5 153.89(7) 2_756 . ? P1 O1 Al1 136.91(16) . . ? P1 O3 Al1 133.42(16) . 4_556 ? P1 O4 Al1 136.38(15) . 2_746 ? Al1 O5 Al1 143.1(2) 2_746 . ? Al1 O5 H7 113(3) 2_746 . ? Al1 O5 H7 103(3) . . ? C2 N1 C1 112.4(3) . . ? C2 N1 H1 106(3) . . ? C1 N1 H1 113(3) . . ? C2 N1 H2 116(3) . . ? C1 N1 H2 106(3) . . ? H1 N1 H2 102(4) . . ? N1 C1 C2 110.8(3) . 3_646 ? N1 C1 H3 109(2) . . ? C2 C1 H3 108(3) 3_646 . ? N1 C1 H4 107(2) . . ? C2 C1 H4 108(2) 3_646 . ? H3 C1 H4 114(3) . . ? N1 C2 C1 109.6(3) . 3_646 ? N1 C2 H5 109(2) . . ? C1 C2 H5 107(2) 3_646 . ? N1 C2 H6 107.9(19) . . ? C1 C2 H6 107.0(19) 3_646 . ? H5 C2 H6 116(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 O2 0.90(4) 1.82(4) 2.700(4) 166(4) 2_646 N1 H2 O2 0.84(3) 1.86(3) 2.650(4) 156(4) . _diffrn_measured_fraction_theta_max 0.831 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.831 _refine_diff_density_max 0.322 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.065