# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 1145/191 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Wenqin Pang Department of Chemistry Jilin University Jiefang Road 119 Changchun 130023 China ; _publ_contact_author_phone ? _publ_contact_author_fax '86 431 5671974' _publ_contact_author_email zhaoyn@263.net _publ_contact_letter ;please consider this CIF submission for publication in Journal of Materials Chemistry.This is a resubmission of a revised version of the paper Ref 9/04837E, as requested by the coeditor. ; _publ_requested_journal 'Journal of Materials CHemistry' #================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_comment ; The coordination geometry at titanium is distorted octahedra.The layer was constructed by trans corner-shared TiO5N octahedra linked by PO4 tetrahedra.Ethylenediamine intercalated between layers by hydrogen bond. ; _publ_section_experimental ; The compound was synthesized from tetrabutyltitanate,phosphorous acid,n-butanol,ethylenediamine and hydrogen peroxide under solvothermal conditions ; _publ_section_acknowledgements ; We thank the Fonds of the National Nature Science Foudation of China the Key Laboratory of Inorganic Synthesis and Preparation Chemistry of Jilin University. ; #================================================================ data_TP-J1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [H3NC2H4NH2]TiOPO4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 N4 O10 P2 Ti2' _chemical_formula_weight 439.66 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 '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 9.2457(19) _cell_length_b 7.3465(16) _cell_length_c 9.929(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.702(5) _cell_angle_gamma 90.00 _cell_volume 662.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 51 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 23.25 _exptl_crystal_description plate _exptl_crystal_colour pale _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 1.485 _exptl_absorpt_correction_type 'empirical omega scan' _exptl_absorpt_correction_T_min 0.419066 _exptl_absorpt_correction_T_max 0.530120 _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 CCD smart 1k ' _diffrn_measurement_method 'omega scan ' _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 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 23.25 _reflns_number_total 803 _reflns_number_gt 617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart program ' _computing_cell_refinement 'Smart program ' _computing_data_reduction 'Saint program ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodn ess of fit S are based on F^2^, conventional R-factors R are based on F, with F s et 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^)+(0.0827P)^2^+1.6617P] 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 803 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 0.710 _refine_ls_restrained_S_all 0.710 _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 Ti1 Ti 0.49330(10) 0.14599(11) 0.23206(10) 0.0137(4) Uani 1 1 d . . . P1 P 0.29181(16) 0.13199(15) -0.08724(14) 0.0120(4) Uani 1 1 d . . . O5 O 0.3351(4) 0.1450(4) 0.0698(3) 0.0191(9) Uani 1 1 d . . . O4 O 0.4483(4) -0.1353(4) 0.2757(3) 0.0158(9) Uani 1 1 d . . . O3 O 0.1245(4) 0.1293(4) -0.1248(4) 0.0176(9) Uani 1 1 d . . . O2 O 0.6448(4) 0.0421(4) 0.1365(4) 0.0179(10) Uani 1 1 d . . . O1 O 0.3487(4) 0.1977(4) 0.3498(4) 0.0166(9) Uani 1 1 d . . . N1 N 0.6498(5) 0.1025(5) 0.4262(5) 0.0202(12) Uani 1 1 d . . . H1A H 0.6061 0.1412 0.4947 0.080 Uiso 1 1 calc . . . H1B H 0.6632 -0.0183 0.4370 0.080 Uiso 1 1 calc . . . N2 N 1.0073(5) 0.2903(5) 0.6240(5) 0.0196(11) Uani 1 1 d . . . H2A H 1.0555 0.2676 0.7086 0.080 Uiso 1 1 calc . . . H2B H 0.9713 0.4029 0.6200 0.080 Uiso 1 1 calc . . . H2C H 1.0687 0.2794 0.5652 0.080 Uiso 1 1 calc . . . C2 C 0.8831(6) 0.1566(6) 0.5871(6) 0.0192(13) Uani 1 1 d . . . H2D H 0.8179 0.1669 0.6529 0.080 Uiso 1 1 calc . . . H2E H 0.9228 0.0341 0.5931 0.080 Uiso 1 1 calc . . . C1 C 0.7961(6) 0.1875(7) 0.4452(5) 0.0207(14) Uani 1 1 d . . . H1C H 0.7849 0.3173 0.4287 0.080 Uiso 1 1 calc . . . H1D H 0.8500 0.1377 0.3787 0.080 Uiso 1 1 calc . . . 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 Ti1 0.0164(7) 0.0121(5) 0.0128(6) -0.0003(4) 0.0035(6) 0.0014(4) P1 0.0147(10) 0.0108(6) 0.0105(8) -0.0003(5) 0.0024(7) 0.0000(5) O5 0.021(2) 0.0216(19) 0.013(2) 0.0030(15) -0.003(2) 0.0016(15) O4 0.017(2) 0.0140(17) 0.016(2) 0.0020(14) 0.003(2) -0.0024(14) O3 0.009(2) 0.0215(19) 0.020(2) 0.0016(15) -0.0022(19) -0.0008(14) O2 0.020(2) 0.0139(18) 0.022(2) 0.0002(14) 0.008(2) -0.0010(15) O1 0.018(2) 0.0141(17) 0.020(2) 0.0004(14) 0.0086(19) -0.0008(15) N1 0.016(3) 0.024(2) 0.019(3) 0.0007(19) -0.003(3) -0.0053(19) N2 0.013(3) 0.021(2) 0.023(3) -0.0025(18) 0.000(2) 0.0002(19) C2 0.015(4) 0.020(3) 0.021(3) 0.001(2) -0.001(3) 0.001(2) C1 0.017(4) 0.028(3) 0.014(3) 0.003(2) -0.006(3) 0.000(2) _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 Ti1 O4 1.701(3) 2_655 ? Ti1 O5 1.965(4) . ? Ti1 O1 1.970(3) . ? Ti1 O2 1.984(3) . ? Ti1 O4 2.168(3) . ? Ti1 N1 2.208(5) . ? P1 O3 1.522(4) . ? P1 O2 1.525(3) 3_655 ? P1 O1 1.534(3) 4_565 ? P1 O5 1.539(4) . ? O4 Ti1 1.701(3) 2_645 ? O2 P1 1.525(3) 3_655 ? O1 P1 1.534(3) 4_566 ? N1 C1 1.469(7) . ? N2 C2 1.504(7) . ? C2 C1 1.504(8) . ? 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 O4 Ti1 O5 99.22(16) 2_655 . ? O4 Ti1 O1 95.78(14) 2_655 . ? O5 Ti1 O1 90.21(15) . . ? O4 Ti1 O2 94.79(14) 2_655 . ? O5 Ti1 O2 95.17(15) . . ? O1 Ti1 O2 167.22(13) . . ? O4 Ti1 O4 169.66(7) 2_655 . ? O5 Ti1 O4 91.11(14) . . ? O1 Ti1 O4 83.61(13) . . ? O2 Ti1 O4 84.70(13) . . ? O4 Ti1 N1 90.82(16) 2_655 . ? O5 Ti1 N1 169.36(14) . . ? O1 Ti1 N1 85.24(16) . . ? O2 Ti1 N1 87.44(16) . . ? O4 Ti1 N1 78.84(14) . . ? O3 P1 O2 110.1(2) . 3_655 ? O3 P1 O1 108.68(19) . 4_565 ? O2 P1 O1 111.83(18) 3_655 4_565 ? O3 P1 O5 108.1(2) . . ? O2 P1 O5 109.49(19) 3_655 . ? O1 P1 O5 108.52(19) 4_565 . ? P1 O5 Ti1 147.7(2) . . ? Ti1 O4 Ti1 144.80(19) 2_645 . ? P1 O2 Ti1 145.4(2) 3_655 . ? P1 O1 Ti1 136.14(19) 4_566 . ? C1 N1 Ti1 119.3(3) . . ? N2 C2 C1 112.4(4) . . ? N1 C1 C2 112.1(4) . . ? _diffrn_measured_fraction_theta_max 0.847 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.847 _refine_diff_density_max 0.371 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.082 #=======================================================================