# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Fu, Zhiyong' _publ_contact_author_email zyfu@scut.edu.cn _publ_section_title ; Nitrogen-Containing Porous Cerium Trimetaphosphate as a New Efficient Base Catalyst ; loop_ _publ_author_name 'Jianglong Yi' 'Zhiyong Fu' 'Desheng Song' 'Shijun Liao' 'Yuan Chen' # Attachment '- SUBMISSION.cif' data_y1 _database_code_depnum_ccdc_archive 'CCDC 794008' #TrackingRef '- SUBMISSION.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ce H13 N3 O11 P3 ' _chemical_formula_weight 464.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ce Ce -0.2486 2.6331 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3040(15) _cell_length_b 9.1675(18) _cell_length_c 9.5663(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 640.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 450 _exptl_absorpt_coefficient_mu 3.982 _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 298(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 4785 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1081 _reflns_number_gt 1066 _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^)+(0.0258P)^2^+0.2377P] 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 _chemical_absolute_configuration unk _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(18) _refine_ls_number_reflns 1081 _refine_ls_number_parameters 110 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0473 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.059 _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 Ce1 Ce 0.0000 0.0000 0.30366(2) 0.01308(11) Uani 1 2 d S . . P1 P 0.5000 0.0000 0.27775(11) 0.0148(2) Uani 1 2 d S . . P2 P 0.38061(14) -0.12641(9) 0.53561(9) 0.0134(2) Uani 1 1 d . . . O1 O 0.3235(4) 0.0119(3) 0.1984(2) 0.0187(5) Uani 1 1 d . . . O2 O 0.1942(4) -0.0694(3) 0.4973(3) 0.0198(6) Uani 1 1 d . . . O3 O 0.3814(4) -0.2631(3) 0.6192(3) 0.0206(6) Uani 1 1 d . . . O4 O -0.0178(8) 0.1793(4) 0.1046(4) 0.0495(10) Uani 1 1 d D . . H3 H 0.051(6) 0.253(4) 0.117(5) 0.033(15) Uiso 1 1 d D . . H4 H -0.119(5) 0.194(7) 0.063(6) 0.050(18) Uiso 1 1 d D . . O5 O 0.2038(6) 0.4192(5) 0.0805(4) 0.0512(10) Uani 1 1 d D . . H6 H 0.200(8) 0.473(6) 0.011(4) 0.048(16) Uiso 1 1 d D . . H5 H 0.291(6) 0.452(5) 0.128(5) 0.040(16) Uiso 1 1 d D . . O6 O 0.5436(11) 0.4467(8) 0.2406(7) 0.047(2) Uani 0.50 1 d P . . N1 N 0.4914(7) -0.1451(3) 0.3850(3) 0.0160(6) Uani 1 1 d D . . H1 H 0.590(4) -0.191(5) 0.380(5) 0.032(13) Uiso 1 1 d D . . N2 N 0.5000 0.0000 0.6209(4) 0.0172(8) Uani 1 2 d SD . . H2 H 0.5000 0.0000 0.707(2) 0.022(15) Uiso 1 2 d SD . . 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 Ce1 0.01237(17) 0.01283(15) 0.01404(15) 0.000 0.000 -0.00049(13) P1 0.0123(6) 0.0180(5) 0.0142(5) 0.000 0.000 0.0020(8) P2 0.0127(5) 0.0113(4) 0.0163(4) 0.0009(3) -0.0002(4) -0.0007(4) O1 0.0159(15) 0.0224(12) 0.0179(12) -0.0004(19) -0.0023(8) 0.0013(12) O2 0.0135(15) 0.0206(12) 0.0253(13) 0.0007(12) -0.0005(11) 0.0009(11) O3 0.0215(17) 0.0168(12) 0.0235(14) 0.0031(11) 0.0027(12) -0.0005(11) O4 0.058(3) 0.0460(19) 0.0442(18) 0.0262(16) -0.025(3) -0.026(2) O5 0.050(3) 0.067(2) 0.036(2) 0.020(2) -0.0034(19) -0.019(2) O6 0.056(8) 0.057(4) 0.028(3) 0.003(3) 0.005(3) -0.016(4) N1 0.0166(17) 0.0149(12) 0.0166(12) -0.0001(10) 0.002(2) 0.0039(18) N2 0.019(2) 0.0201(17) 0.0126(17) 0.000 0.000 -0.005(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 Ce1 O2 2.418(3) 2 ? Ce1 O2 2.418(3) . ? Ce1 O3 2.452(3) 3_556 ? Ce1 O3 2.452(3) 4_446 ? Ce1 O4 2.519(3) 2 ? Ce1 O4 2.519(3) . ? Ce1 O1 2.571(3) . ? Ce1 O1 2.571(3) 2 ? P1 O1 1.500(3) . ? P1 O1 1.500(3) 2_655 ? P1 N1 1.681(3) 2_655 ? P1 N1 1.681(3) . ? P2 O3 1.487(3) . ? P2 O2 1.504(3) . ? P2 N1 1.662(3) . ? P2 N2 1.664(2) . ? O3 Ce1 2.452(3) 3_546 ? O4 H3 0.85(2) . ? O4 H4 0.85(2) . ? O5 H6 0.83(2) . ? O5 H5 0.83(2) . ? O6 O6 1.167(15) 2_665 ? N1 H1 0.83(2) . ? N2 P2 1.664(2) 2_655 ? N2 H2 0.83(2) . ? 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 Ce1 O2 80.01(13) 2 . ? O2 Ce1 O3 75.16(9) 2 3_556 ? O2 Ce1 O3 78.19(9) . 3_556 ? O2 Ce1 O3 78.19(9) 2 4_446 ? O2 Ce1 O3 75.16(9) . 4_446 ? O3 Ce1 O3 144.98(12) 3_556 4_446 ? O2 Ce1 O4 141.35(13) 2 2 ? O2 Ce1 O4 112.15(13) . 2 ? O3 Ce1 O4 141.94(11) 3_556 2 ? O3 Ce1 O4 70.58(10) 4_446 2 ? O2 Ce1 O4 112.15(13) 2 . ? O2 Ce1 O4 141.35(13) . . ? O3 Ce1 O4 70.58(10) 3_556 . ? O3 Ce1 O4 141.94(11) 4_446 . ? O4 Ce1 O4 81.79(19) 2 . ? O2 Ce1 O1 145.90(9) 2 . ? O2 Ce1 O1 76.82(8) . . ? O3 Ce1 O1 75.86(10) 3_556 . ? O3 Ce1 O1 118.69(10) 4_446 . ? O4 Ce1 O1 71.58(13) 2 . ? O4 Ce1 O1 73.96(14) . . ? O2 Ce1 O1 76.82(8) 2 2 ? O2 Ce1 O1 145.90(9) . 2 ? O3 Ce1 O1 118.69(10) 3_556 2 ? O3 Ce1 O1 75.86(10) 4_446 2 ? O4 Ce1 O1 73.96(14) 2 2 ? O4 Ce1 O1 71.58(13) . 2 ? O1 Ce1 O1 133.88(10) . 2 ? O1 P1 O1 119.20(19) . 2_655 ? O1 P1 N1 106.47(18) . 2_655 ? O1 P1 N1 109.51(19) 2_655 2_655 ? O1 P1 N1 109.51(19) . . ? O1 P1 N1 106.47(18) 2_655 . ? N1 P1 N1 104.80(19) 2_655 . ? O3 P2 O2 115.33(17) . . ? O3 P2 N1 112.19(14) . . ? O2 P2 N1 105.39(19) . . ? O3 P2 N2 108.74(15) . . ? O2 P2 N2 110.60(11) . . ? N1 P2 N2 103.99(17) . . ? P1 O1 Ce1 126.06(12) . . ? P2 O2 Ce1 144.02(17) . . ? P2 O3 Ce1 155.49(19) . 3_546 ? Ce1 O4 H3 113(3) . . ? Ce1 O4 H4 120(4) . . ? H3 O4 H4 117(5) . . ? H6 O5 H5 104(6) . . ? P2 N1 P1 117.75(18) . . ? P2 N1 H1 121(3) . . ? P1 N1 H1 109(3) . . ? P2 N2 P2 121.3(2) . 2_655 ? P2 N2 H2 119.35(11) . . ? P2 N2 H2 119.35(11) 2_655 . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.746 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.107