# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2002 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; YU, Jihong 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 'jihong@mail.jlu.edu.cn' _publ_requested_journal 'J. C. S. Dalton Trans' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; A new layered aluminophosphate [AlP2O8][C4H16N3] with 4.12-net porous sheets ; loop_ _publ_author_name _publ_author_address 'WEI, Bo' ; 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 ; 'QIU, Shilun' ; 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 ; #complex B00315530 data_p21n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H16 Al N3 O8 P2' _chemical_formula_weight 323.12 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)/n 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 10.8264(11) _cell_length_b 8.1432(8) _cell_length_c 13.7698(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.104(2) _cell_angle_gamma 90.00 _cell_volume 1209.2(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 block _exptl_crystal_colour none _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.471 _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 2736 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1679 _reflns_number_gt 1511 _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^)+(0.0518P)^2^+0.8064P] 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 1679 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 P1 P 2.16356(6) -0.07658(9) -0.08430(5) 0.0201(2) Uani 1 1 d . . . P2 P 1.66115(6) -0.24880(8) -0.21874(5) 0.0208(2) Uani 1 1 d . . . Al Al 1.86773(7) -0.02915(9) -0.12782(5) 0.0179(2) Uani 1 1 d . . . O1 O 2.02456(17) -0.0722(2) -0.11980(14) 0.0304(5) Uani 1 1 d . . . O2 O 2.20512(18) -0.2509(2) -0.06524(15) 0.0322(5) Uani 1 1 d . . . O3 O 2.18233(17) 0.0241(2) 0.01111(13) 0.0271(5) Uani 1 1 d . . . O4 O 2.23394(17) 0.0076(2) -0.16048(13) 0.0301(5) Uani 1 1 d . . . O5 O 1.79682(16) -0.1947(2) -0.18981(13) 0.0255(5) Uani 1 1 d . . . O6 O 1.66658(18) -0.3420(2) -0.31627(13) 0.0282(5) Uani 1 1 d . . . O7 O 1.62099(17) -0.3630(2) -0.14059(14) 0.0304(5) Uani 1 1 d . . . O8 O 1.57949(18) -0.1001(2) -0.23779(14) 0.0316(5) Uani 1 1 d . . . N1 N 1.3731(2) 0.5523(3) -0.15708(19) 0.0264(6) Uani 1 1 d . . . N2 N 1.4638(2) 0.1064(3) -0.12018(16) 0.0250(5) Uani 1 1 d . . . N3 N 1.6524(2) -0.0212(3) -0.4267(2) 0.0336(6) Uani 1 1 d . . . C1 C 1.3736(3) 0.3870(4) -0.1129(2) 0.0313(7) Uani 1 1 d . . . C2 C 1.4691(3) 0.2790(4) -0.1559(2) 0.0296(7) Uani 1 1 d . . . C3 C 1.5018(3) 0.0891(4) -0.0142(2) 0.0285(7) Uani 1 1 d . . . C4 C 1.5543(3) 0.0578(4) -0.4909(3) 0.0365(8) Uani 1 1 d . . . H1NA H 1.342(3) 0.551(4) -0.226(3) 0.048(10) Uiso 1 1 d . . . H1NB H 1.324(3) 0.618(4) -0.132(3) 0.048(11) Uiso 1 1 d . . . H1NC H 1.458(3) 0.589(4) -0.150(2) 0.043(9) Uiso 1 1 d . . . H2NA H 1.371(3) 0.065(4) -0.138(2) 0.044(9) Uiso 1 1 d . . . H2NB H 1.512(3) 0.036(4) -0.156(2) 0.046(10) Uiso 1 1 d . . . H3NA H 1.676(4) -0.116(5) -0.462(3) 0.073(13) Uiso 1 1 d . . . H3NB H 1.730(4) 0.040(5) -0.406(3) 0.061(11) Uiso 1 1 d . . . H3NC H 1.618(4) -0.037(6) -0.363(3) 0.097(16) Uiso 1 1 d . . . H1CA H 1.394(3) 0.399(4) -0.042(3) 0.042(9) Uiso 1 1 d . . . H1CB H 1.293(3) 0.346(4) -0.125(2) 0.032(8) Uiso 1 1 d . . . H2CA H 1.553(3) 0.320(4) -0.140(2) 0.036(8) Uiso 1 1 d . . . H2CB H 1.451(3) 0.271(4) -0.224(3) 0.045(10) Uiso 1 1 d . . . H3CA H 1.451(3) 0.156(4) 0.018(2) 0.030(8) Uiso 1 1 d . . . H3CB H 1.585(3) 0.134(4) -0.002(2) 0.032(8) Uiso 1 1 d . . . H4CA H 1.585(3) 0.084(4) -0.564(2) 0.039(8) Uiso 1 1 d . . . H4CB H 1.534(3) 0.154(5) -0.458(3) 0.056(11) 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 0.0176(4) 0.0244(4) 0.0187(4) 0.0004(3) 0.0029(3) -0.0004(3) P2 0.0211(4) 0.0204(4) 0.0207(4) -0.0022(3) 0.0006(3) -0.0016(3) Al 0.0179(4) 0.0190(4) 0.0167(4) 0.0005(3) 0.0003(3) -0.0006(3) O1 0.0197(10) 0.0380(11) 0.0332(11) -0.0022(9) 0.0004(8) -0.0012(8) O2 0.0335(11) 0.0270(11) 0.0368(12) 0.0009(9) 0.0077(9) 0.0065(8) O3 0.0300(10) 0.0318(11) 0.0199(10) -0.0015(8) 0.0043(8) -0.0041(8) O4 0.0258(10) 0.0443(12) 0.0204(10) 0.0039(9) 0.0033(8) -0.0081(9) O5 0.0230(10) 0.0266(10) 0.0267(11) -0.0047(8) 0.0009(8) -0.0036(8) O6 0.0363(11) 0.0238(10) 0.0237(10) -0.0043(8) -0.0022(8) -0.0011(8) O7 0.0295(11) 0.0333(11) 0.0286(11) 0.0044(9) 0.0044(8) -0.0043(9) O8 0.0317(11) 0.0290(11) 0.0339(11) -0.0002(9) 0.0026(9) 0.0084(9) N1 0.0277(14) 0.0271(14) 0.0244(15) -0.0004(11) 0.0030(12) 0.0020(11) N2 0.0267(13) 0.0245(12) 0.0243(13) 0.0004(10) 0.0042(10) 0.0020(10) N3 0.0319(15) 0.0334(15) 0.0347(16) -0.0025(12) -0.0018(13) -0.0002(12) C1 0.0342(18) 0.0284(16) 0.0321(18) 0.0037(14) 0.0078(14) 0.0017(13) C2 0.0318(17) 0.0275(15) 0.0305(19) 0.0056(13) 0.0081(14) 0.0023(13) C3 0.0295(16) 0.0276(15) 0.0279(17) -0.0001(13) 0.0001(13) 0.0006(13) C4 0.0353(17) 0.0291(17) 0.044(2) -0.0016(15) -0.0028(15) 0.0004(14) _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 1.505(2) . ? P1 O4 1.5142(19) . ? P1 O1 1.5408(19) . ? P1 O3 1.5468(19) . ? P2 O8 1.508(2) . ? P2 O7 1.5150(19) . ? P2 O6 1.5483(19) . ? P2 O5 1.5512(18) . ? Al O1 1.7277(19) . ? Al O6 1.7327(19) 2_854 ? Al O5 1.7373(19) . ? Al O3 1.7415(19) 3_955 ? O3 Al 1.7415(19) 3_955 ? O6 Al 1.7327(19) 2_844 ? N1 C1 1.477(4) . ? N1 H1NA 0.98(4) . ? N1 H1NB 0.85(4) . ? N1 H1NC 0.97(4) . ? N2 C3 1.488(4) . ? N2 C2 1.492(4) . ? N2 H2NA 1.07(3) . ? N2 H2NB 0.94(4) . ? N3 C4 1.468(4) . ? N3 H3NA 0.96(4) . ? N3 H3NB 1.00(4) . ? N3 H3NC 0.99(5) . ? C1 C2 1.516(4) . ? C1 H1CA 0.98(3) . ? C1 H1CB 0.93(3) . ? C2 H2CA 0.97(3) . ? C2 H2CB 0.94(3) . ? C3 C3 1.504(6) 3_855 ? C3 H3CA 0.91(3) . ? C3 H3CB 0.98(3) . ? C4 C4 1.510(6) 3_854 ? C4 H4CA 1.10(3) . ? C4 H4CB 0.94(4) . ? 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 112.74(11) . . ? O2 P1 O1 110.20(12) . . ? O4 P1 O1 107.90(11) . . ? O2 P1 O3 109.71(11) . . ? O4 P1 O3 108.20(11) . . ? O1 P1 O3 107.95(11) . . ? O8 P2 O7 114.54(11) . . ? O8 P2 O6 108.03(11) . . ? O7 P2 O6 110.53(11) . . ? O8 P2 O5 110.09(11) . . ? O7 P2 O5 108.49(11) . . ? O6 P2 O5 104.71(10) . . ? O1 Al O6 112.19(10) . 2_854 ? O1 Al O5 105.22(9) . . ? O6 Al O5 113.34(9) 2_854 . ? O1 Al O3 109.30(10) . 3_955 ? O6 Al O3 108.51(10) 2_854 3_955 ? O5 Al O3 108.14(9) . 3_955 ? P1 O1 Al 162.08(14) . . ? P1 O3 Al 140.18(12) . 3_955 ? P2 O5 Al 135.53(12) . . ? P2 O6 Al 142.50(13) . 2_844 ? C1 N1 H1NA 112(2) . . ? C1 N1 H1NB 113(2) . . ? H1NA N1 H1NB 103(3) . . ? C1 N1 H1NC 105.6(19) . . ? H1NA N1 H1NC 110(3) . . ? H1NB N1 H1NC 113(3) . . ? C3 N2 C2 113.4(2) . . ? C3 N2 H2NA 111.4(16) . . ? C2 N2 H2NA 106.5(17) . . ? C3 N2 H2NB 110(2) . . ? C2 N2 H2NB 111(2) . . ? H2NA N2 H2NB 104(3) . . ? C4 N3 H3NA 105(2) . . ? C4 N3 H3NB 120(2) . . ? H3NA N3 H3NB 107(3) . . ? C4 N3 H3NC 106(3) . . ? H3NA N3 H3NC 119(4) . . ? H3NB N3 H3NC 101(3) . . ? N1 C1 C2 110.2(2) . . ? N1 C1 H1CA 107.9(19) . . ? C2 C1 H1CA 110.1(19) . . ? N1 C1 H1CB 106.6(18) . . ? C2 C1 H1CB 112.5(19) . . ? H1CA C1 H1CB 109(3) . . ? N2 C2 C1 111.7(2) . . ? N2 C2 H2CA 107.9(18) . . ? C1 C2 H2CA 111.7(18) . . ? N2 C2 H2CB 105(2) . . ? C1 C2 H2CB 110(2) . . ? H2CA C2 H2CB 111(3) . . ? N2 C3 C3 109.6(3) . 3_855 ? N2 C3 H3CA 107.2(18) . . ? C3 C3 H3CA 114.6(19) 3_855 . ? N2 C3 H3CB 107.8(17) . . ? C3 C3 H3CB 111.1(18) 3_855 . ? H3CA C3 H3CB 106(2) . . ? N3 C4 C4 109.8(3) . 3_854 ? N3 C4 H4CA 111.6(16) . . ? C4 C4 H4CA 105.2(16) 3_854 . ? N3 C4 H4CB 105(2) . . ? C4 C4 H4CB 113(2) 3_854 . ? H4CA C4 H4CB 112(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 H1NA O4 0.98(4) 1.74(4) 2.696(3) 166(3) 2_854 N1 H1NB O2 0.85(4) 1.96(4) 2.807(3) 173(3) 1_465 N1 H1NC O7 0.97(4) 1.80(4) 2.761(3) 175(3) 1_565 N2 H2NA O4 1.07(3) 1.56(3) 2.627(3) 178(3) 1_455 N2 H2NB O8 0.94(4) 1.78(4) 2.717(3) 170(3) . N3 H3NA O2 0.96(4) 1.84(4) 2.757(3) 160(4) 4 N3 H3NB O7 1.00(4) 1.86(4) 2.851(3) 174(3) 2_854 N3 H3NB O5 1.00(4) 2.57(4) 3.129(3) 116(3) 2_854 N3 H3NC O8 0.99(5) 1.89(5) 2.859(3) 168(4) . _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.270 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.057 #============================================================================