# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2001 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Prof Ruren Xu Key Lab of Inorg Synth & Preparative Chem Jilin University Changchun 130023 CHINA ; _publ_contact_author_email 'RRXU@MAIL.JLU.EDU.CN' _publ_requested_journal 'J. C. S. Dalton Trans' _journal_coden_Cambridge 186 _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and characterization of a new three-dimensional aluminophosphate [Al11P12O48][C4H12N2][C4H11N2] with an Al/P ratio of 11/12 ; 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 ; 'Shi, Zhan' ; 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 ; 'Yan, Wenfu' ; 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 AlPO-CJ11 data_r-3c _database_code_CSD 154045 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H23 Al11 N4 O48 P12' _chemical_formula_weight 1611.72 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 Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 14.0454(17) _cell_length_b 14.0454(17) _cell_length_c 42.091(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7191.0(16) _cell_formula_units_Z 6 _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 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4836 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8872 _exptl_absorpt_correction_T_max 0.8872 _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 8009 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 11.40 _diffrn_reflns_theta_max 30.03 _reflns_number_total 2122 _reflns_number_gt 1348 _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^)+(0.1008P)^2^+70.6550P] 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 2122 _refine_ls_number_parameters 108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1908 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 0.24000(10) 0.81597(10) 0.02068(3) 0.0178(4) Uani 1 1 d . . . P2 P 0.08880(10) 0.57061(10) 0.08424(3) 0.0156(3) Uani 1 1 d . . . Al1 Al 0.3333 0.6667 0.05125(6) 0.0131(5) Uani 1 3 d S . . Al2 Al 0.00224(12) 0.66631(13) 0.03091(4) 0.0186(4) Uani 1 1 d . . . Al3 Al 0.04015(15) 0.3333 0.0833 0.0177(5) Uani 1 2 d S . . O1 O 0.2401(4) 0.8752(4) 0.05107(12) 0.0410(12) Uani 1 1 d . . . O2 O 0.3097(4) 0.8988(4) -0.00509(12) 0.0352(10) Uani 1 1 d . . . O3 O 0.2830(3) 0.7394(3) 0.02537(9) 0.0229(8) Uani 1 1 d . . . O4 O 0.1198(3) 0.7541(3) 0.00941(9) 0.0240(8) Uani 1 1 d . . . O5 O 0.2091(3) 0.6134(3) 0.07856(9) 0.0247(8) Uani 1 1 d . . . O6 O 0.0317(4) 0.5870(3) 0.05564(10) 0.0293(9) Uani 1 1 d . . . O7 O 0.0281(3) 0.4476(3) 0.09181(11) 0.0284(9) Uani 1 1 d . . . O8 O 0.0777(3) 0.6303(3) 0.11310(10) 0.0273(9) 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 0.0185(6) 0.0132(6) 0.0222(7) 0.0015(5) -0.0040(5) 0.0084(5) P2 0.0172(6) 0.0139(6) 0.0183(7) 0.0033(4) 0.0039(5) 0.0095(5) Al1 0.0120(7) 0.0120(7) 0.0151(12) 0.000 0.000 0.0060(3) Al2 0.0187(7) 0.0233(8) 0.0185(8) -0.0028(6) -0.0029(6) 0.0138(6) Al3 0.0170(7) 0.0125(9) 0.0221(11) 0.0027(8) 0.0013(4) 0.0063(5) O1 0.049(3) 0.046(3) 0.042(3) -0.024(2) -0.019(2) 0.034(2) O2 0.030(2) 0.028(2) 0.044(3) 0.0166(19) -0.0017(19) 0.0115(18) O3 0.028(2) 0.0250(19) 0.0239(19) 0.0066(15) 0.0022(15) 0.0189(16) O4 0.0214(18) 0.032(2) 0.0210(19) -0.0019(15) -0.0030(14) 0.0148(16) O5 0.0175(17) 0.027(2) 0.0274(19) 0.0058(16) 0.0066(15) 0.0091(15) O6 0.033(2) 0.031(2) 0.028(2) 0.0048(17) -0.0053(17) 0.0183(18) O7 0.027(2) 0.0186(19) 0.041(2) 0.0089(16) 0.0091(17) 0.0120(16) O8 0.031(2) 0.029(2) 0.026(2) -0.0035(16) 0.0045(16) 0.0188(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 O3 1.486(4) . ? P1 O1 1.526(5) . ? P1 O2 1.533(5) . ? P1 O4 1.538(4) . ? P2 O5 1.503(4) . ? P2 O6 1.526(4) . ? P2 O8 1.527(4) . ? P2 O7 1.530(4) . ? Al1 O3 1.858(4) . ? Al1 O3 1.858(4) 2_665 ? Al1 O3 1.858(4) 3_565 ? Al1 O5 1.902(4) 3_565 ? Al1 O5 1.902(4) . ? Al1 O5 1.902(4) 2_665 ? Al2 O2 1.700(4) 20_455 ? Al2 O6 1.719(4) . ? Al2 O8 1.732(4) 16_454 ? Al2 O4 1.740(4) . ? Al3 O1 1.711(5) 18_544 ? Al3 O1 1.711(5) 2_665 ? Al3 O7 1.733(4) . ? Al3 O7 1.733(4) 17_554 ? O1 Al3 1.711(5) 3_565 ? O2 Al2 1.700(4) 21_665 ? O8 Al2 1.732(4) 16_454 ? 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 O3 P1 O1 113.2(3) . . ? O3 P1 O2 107.9(2) . . ? O1 P1 O2 110.7(3) . . ? O3 P1 O4 111.2(2) . . ? O1 P1 O4 105.6(3) . . ? O2 P1 O4 108.3(2) . . ? O5 P2 O6 112.6(2) . . ? O5 P2 O8 108.1(2) . . ? O6 P2 O8 109.8(2) . . ? O5 P2 O7 111.4(2) . . ? O6 P2 O7 107.3(2) . . ? O8 P2 O7 107.6(2) . . ? O3 Al1 O3 89.12(19) . 2_665 ? O3 Al1 O3 89.12(19) . 3_565 ? O3 Al1 O3 89.12(19) 2_665 3_565 ? O3 Al1 O5 91.06(18) . 3_565 ? O3 Al1 O5 178.3(2) 2_665 3_565 ? O3 Al1 O5 92.56(17) 3_565 3_565 ? O3 Al1 O5 92.56(17) . . ? O3 Al1 O5 91.06(18) 2_665 . ? O3 Al1 O5 178.3(2) 3_565 . ? O5 Al1 O5 87.26(19) 3_565 . ? O3 Al1 O5 178.3(2) . 2_665 ? O3 Al1 O5 92.56(17) 2_665 2_665 ? O3 Al1 O5 91.06(18) 3_565 2_665 ? O5 Al1 O5 87.26(19) 3_565 2_665 ? O5 Al1 O5 87.26(19) . 2_665 ? O2 Al2 O6 112.3(2) 20_455 . ? O2 Al2 O8 108.5(2) 20_455 16_454 ? O6 Al2 O8 109.2(2) . 16_454 ? O2 Al2 O4 108.9(2) 20_455 . ? O6 Al2 O4 108.9(2) . . ? O8 Al2 O4 108.9(2) 16_454 . ? O1 Al3 O1 111.2(4) 18_544 2_665 ? O1 Al3 O7 109.5(2) 18_544 . ? O1 Al3 O7 107.5(2) 2_665 . ? O1 Al3 O7 107.5(2) 18_544 17_554 ? O1 Al3 O7 109.5(2) 2_665 17_554 ? O7 Al3 O7 111.8(3) . 17_554 ? P1 O1 Al3 157.8(4) . 3_565 ? P1 O2 Al2 152.2(3) . 21_665 ? P1 O3 Al1 151.6(3) . . ? P1 O4 Al2 128.7(3) . . ? P2 O5 Al1 151.6(3) . . ? P2 O6 Al2 152.9(3) . . ? P2 O7 Al3 138.2(3) . . ? P2 O8 Al2 149.8(3) . 16_454 ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 2.691 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.156