data_4000032 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _publ_section_title ; Solvothermal Synthesis and Characterization of a New Titanium Phosphate with 1-D Chiral Chain ; loop_ _publ_author_name 'Guo, Yanghong' 'Shi, Zhan' 'Yu, Jihong' 'Liu, Yunling' 'Pang, Wenqin' _chemical_formula_sum 'C10 H56 N10 O29 P6 Ti3' _chemical_formula_weight 1110.17 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1800(6) _cell_length_b 15.8992(9) _cell_length_c 23.2271(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3759.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description columnar _exptl_crystal_colour none _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.993 _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_reflns_number 18584 _diffrn_reflns_av_R_equivalents 0.1222 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5413 _reflns_number_gt 4493 _reflns_threshold_expression >2sigma(I) _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^)+(0.0363P)^2^+4.4393P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(5) _refine_ls_number_reflns 5413 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 -0.08637(12) 0.39210(8) 0.63967(6) 0.0202(3) Uani 1 1 d . . . Ti2 Ti -0.09689(12) 0.61716(7) 0.64299(6) 0.0168(3) Uani 1 1 d . . . Ti3 Ti -0.00433(15) 0.75660(9) 0.75014(6) 0.0229(3) Uani 1 1 d . . . P1 P -0.36500(16) 0.49462(13) 0.65521(7) 0.0200(4) Uani 1 1 d . . . P2 P -0.14896(15) 0.50247(13) 0.52005(6) 0.0179(3) Uani 1 1 d . . . P3 P 0.18911(17) 0.71004(11) 0.64102(9) 0.0189(4) Uani 1 1 d . . . P4 P -0.18857(18) 0.81716(11) 0.63984(8) 0.0182(4) Uani 1 1 d . . . P5 P 0.15378(19) 0.68495(11) 0.86382(9) 0.0220(5) Uani 1 1 d . . . P6 P -0.18498(19) 0.78274(12) 0.86503(9) 0.0247(5) Uani 1 1 d . . . O1 O -0.0603(5) 0.3511(3) 0.71250(19) 0.0191(12) Uani 1 1 d . . . O2 O 0.0936(5) 0.3559(3) 0.6178(2) 0.0242(12) Uani 1 1 d . . . O3 O -0.1567(5) 0.2759(3) 0.6152(2) 0.0247(12) Uani 1 1 d . . . O4 O -0.1148(5) 0.4246(3) 0.55554(19) 0.0245(12) Uani 1 1 d . . . O5 O -0.2740(5) 0.4181(3) 0.6557(2) 0.0249(12) Uani 1 1 d . . . O6 O -0.0368(4) 0.5016(3) 0.65547(15) 0.0200(9) Uani 1 1 d . . . O7 O -0.4422(4) 0.4939(4) 0.59726(18) 0.0307(11) Uani 1 1 d . . . O8 O -0.4607(5) 0.4914(3) 0.7041(2) 0.0359(12) Uani 1 1 d . . . O9 O -0.2823(5) 0.5756(3) 0.6578(2) 0.0208(11) Uani 1 1 d . . . O10 O -0.1250(5) 0.5821(3) 0.55563(19) 0.0218(12) Uani 1 1 d . . . O11 O -0.0738(4) 0.5042(4) 0.46401(17) 0.0307(11) Uani 1 1 d . . . O12 O -0.2990(4) 0.4976(4) 0.50539(16) 0.0261(10) Uani 1 1 d . . . O13 O -0.0700(5) 0.6543(3) 0.71338(19) 0.0182(11) Uani 1 1 d . . . O14 O 0.0748(5) 0.6571(3) 0.61658(19) 0.0199(11) Uani 1 1 d . . . O15 O -0.1797(5) 0.7252(3) 0.6179(2) 0.0231(12) Uani 1 1 d . . . O16 O 0.3028(5) 0.6517(3) 0.6554(2) 0.0303(12) Uani 1 1 d . . . O17 O 0.2348(5) 0.7747(3) 0.5967(2) 0.0311(13) Uani 1 1 d . . . O18 O 0.1440(5) 0.7572(3) 0.6962(2) 0.0226(12) Uani 1 1 d . . . O19 O -0.1376(5) 0.8750(3) 0.5922(2) 0.0291(12) Uani 1 1 d . . . O20 O -0.3336(5) 0.8369(3) 0.6529(2) 0.0307(13) Uani 1 1 d . . . O21 O -0.1066(5) 0.8283(3) 0.6953(2) 0.0272(13) Uani 1 1 d . . . O22 O 0.1021(6) 0.6810(3) 0.8020(2) 0.0295(13) Uani 1 1 d . . . O23 O -0.1512(5) 0.7525(3) 0.8049(2) 0.0311(14) Uani 1 1 d . . . O25 O 0.0589(6) 0.6343(3) 0.9033(2) 0.0400(14) Uani 1 1 d . . . O24 O 0.2875(5) 0.6442(3) 0.8686(2) 0.0335(13) Uani 1 1 d . . . O26 O -0.1671(6) 0.7089(3) 0.9076(2) 0.0409(15) Uani 1 1 d . . . O27 O -0.3248(5) 0.8127(4) 0.8679(2) 0.0492(16) Uani 1 1 d . . . O1W O 0.0090(9) 0.0351(5) 0.1497(3) 0.104(3) Uani 1 1 d . . . O2W O 0.3215(18) 0.5109(11) 0.2429(6) 0.274(11) Uani 1 1 d . . . N1 N 0.944(3) 0.7029(15) 0.1005(11) 0.116(8) Uiso 0.50 1 d P . . N1' N 0.8218(17) 0.6850(10) 0.0230(7) 0.058(4) Uiso 0.50 1 d P . . N2 N 1.0379(10) 0.8318(6) 0.0733(4) 0.091(3) Uani 1 1 d . . . N3 N -0.2230(6) 1.0024(5) 0.3963(2) 0.0322(13) Uani 1 1 d . . . H3A H -0.2404 0.9629 0.3703 0.080 Uiso 1 1 calc . . . H3B H -0.1371 1.0127 0.3968 0.080 Uiso 1 1 calc . . . H3C H -0.2661 1.0493 0.3873 0.080 Uiso 1 1 calc . . . N4 N -0.2935(6) 1.0080(4) 0.5553(2) 0.0321(14) Uani 1 1 d . . . H4A H -0.2769 1.0463 0.5823 0.080 Uiso 1 1 calc . . . H4B H -0.2566 0.9594 0.5652 0.080 Uiso 1 1 calc . . . H4C H -0.3799 1.0011 0.5520 0.080 Uiso 1 1 calc . . . N5 N 0.2524(15) 0.0826(9) 0.2135(6) 0.051(4) Uiso 0.50 1 d P . . N5' N 0.4880(11) 0.0007(10) 0.2206(5) 0.034(3) Uiso 0.50 1 d P . . N6 N 0.3736(8) 0.0680(4) 0.1023(3) 0.0468(19) Uani 1 1 d . . . H6A H 0.3606 0.0527 0.0659 0.080 Uiso 1 1 calc . . . H6B H 0.4582 0.0798 0.1076 0.080 Uiso 1 1 calc . . . H6C H 0.3255 0.1133 0.1102 0.080 Uiso 1 1 calc . . . N7 N 1.0615(7) 0.6597(4) 0.2365(3) 0.0491(19) Uani 1 1 d . . . H7A H 1.0234 0.6093 0.2365 0.080 Uiso 1 1 calc . . . H7B H 1.1109 0.6652 0.2679 0.080 Uiso 1 1 calc . . . H7C H 1.1117 0.6648 0.2053 0.080 Uiso 1 1 calc . . . N8 N 0.9173(7) 0.8784(4) 0.2394(3) 0.0379(17) Uani 1 1 d . . . H8A H 0.9557 0.9287 0.2394 0.080 Uiso 1 1 calc . . . H8B H 0.8709 0.8722 0.2716 0.080 Uiso 1 1 calc . . . H8C H 0.8642 0.8743 0.2091 0.080 Uiso 1 1 calc . . . N9 N -0.1119(6) 0.7308(4) 0.4980(2) 0.0274(14) Uani 1 1 d . . . H9A H -0.1301 0.6828 0.5160 0.080 Uiso 1 1 calc . . . H9B H -0.1594 0.7341 0.4659 0.080 Uiso 1 1 calc . . . H9C H -0.1313 0.7740 0.5208 0.080 Uiso 1 1 calc . . . N10 N 0.0439(7) 0.8057(4) 0.3909(3) 0.0397(18) Uani 1 1 d . . . H10A H 0.0656 0.8539 0.3738 0.080 Uiso 1 1 calc . . . H10B H -0.0405 0.7946 0.3843 0.080 Uiso 1 1 calc . . . H10C H 0.0931 0.7643 0.3767 0.080 Uiso 1 1 calc . . . C1 C 0.9491(14) 0.6953(7) 0.0343(5) 0.079(4) Uani 1 1 d . . . C2 C 0.967(2) 0.7900(14) 0.0160(10) 0.053(6) Uiso 0.50 1 d P . . C2' C 1.021(2) 0.7762(11) 0.0171(8) 0.031(4) Uiso 0.50 1 d P . . C3 C -0.2653(8) 0.9732(4) 0.4536(3) 0.034(2) Uani 1 1 d . . . H3D H -0.2195 0.9213 0.4627 0.080 Uiso 1 1 calc . . . H3E H -0.3586 0.9609 0.4525 0.080 Uiso 1 1 calc . . . C4 C -0.2396(9) 1.0361(5) 0.5005(3) 0.041(2) Uani 1 1 d . . . H4D H -0.1457 1.0445 0.5044 0.080 Uiso 1 1 calc . . . H4E H -0.2789 1.0895 0.4901 0.080 Uiso 1 1 calc . . . C5 C 0.3468(11) 0.0067(10) 0.1990(4) 0.095(4) Uani 1 1 d . . . C6 C 0.3323(12) -0.0058(8) 0.1434(6) 0.101(4) Uani 1 1 d . . . H6D H 0.2406 -0.0186 0.1362 0.080 Uiso 1 1 calc . . . H6E H 0.3828 -0.0552 0.1329 0.080 Uiso 1 1 calc . . . C7 C 0.9594(9) 0.7258(5) 0.2361(4) 0.049(2) Uani 1 1 d . . . H7D H 0.9037 0.7194 0.2697 0.080 Uiso 1 1 calc . . . H7E H 0.9049 0.7193 0.2021 0.080 Uiso 1 1 calc . . . C8 C 1.0193(8) 0.8120(5) 0.2362(3) 0.038(2) Uani 1 1 d . . . H8D H 1.0779 0.8173 0.2689 0.080 Uiso 1 1 calc . . . H8E H 1.0707 0.8196 0.2015 0.080 Uiso 1 1 calc . . . C9 C 0.0305(7) 0.7332(5) 0.4832(3) 0.035(2) Uani 1 1 d . . . H9D H 0.0517 0.6857 0.4587 0.080 Uiso 1 1 calc . . . H9E H 0.0820 0.7283 0.5181 0.080 Uiso 1 1 calc . . . C10 C 0.0663(8) 0.8127(5) 0.4530(4) 0.039(2) Uani 1 1 d . . . H10D H 0.0140 0.8586 0.4683 0.080 Uiso 1 1 calc . . . H10E H 0.1580 0.8254 0.4601 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 0.0171(7) 0.0248(7) 0.0187(7) -0.0025(6) -0.0024(6) 0.0015(6) Ti2 0.0155(7) 0.0178(7) 0.0172(7) 0.0015(5) -0.0020(6) -0.0006(5) Ti3 0.0272(7) 0.0267(7) 0.0150(5) 0.0006(5) 0.0017(5) 0.0067(5) P1 0.0150(8) 0.0194(8) 0.0256(8) 0.0058(10) 0.0012(6) -0.0003(9) P2 0.0196(9) 0.0195(8) 0.0145(7) -0.0008(10) -0.0029(6) -0.0017(10) P3 0.0141(9) 0.0216(10) 0.0209(10) -0.0011(8) 0.0033(9) -0.0027(8) P4 0.0193(10) 0.0167(9) 0.0186(10) 0.0005(8) -0.0002(9) 0.0019(8) P5 0.0279(11) 0.0188(9) 0.0193(10) -0.0003(8) -0.0007(9) 0.0021(8) P6 0.0229(11) 0.0269(11) 0.0243(11) -0.0081(9) 0.0030(10) -0.0062(9) O1 0.024(3) 0.015(2) 0.018(3) 0.003(2) -0.001(2) -0.001(2) O2 0.024(3) 0.025(3) 0.024(3) 0.008(2) 0.002(2) 0.008(2) O3 0.037(3) 0.015(2) 0.022(3) -0.001(2) -0.009(2) -0.003(2) O4 0.037(3) 0.019(3) 0.017(3) 0.001(2) -0.004(3) 0.002(3) O5 0.019(3) 0.016(2) 0.040(3) -0.006(2) 0.002(3) -0.003(2) O6 0.020(2) 0.020(2) 0.021(2) 0.003(3) -0.0009(17) -0.001(3) O7 0.023(2) 0.033(3) 0.036(3) 0.003(3) -0.008(2) 0.000(3) O8 0.030(3) 0.029(3) 0.049(3) 0.016(3) 0.017(2) 0.004(3) O9 0.015(2) 0.022(3) 0.025(3) 0.004(2) -0.004(2) -0.002(2) O10 0.031(3) 0.016(2) 0.018(3) 0.003(2) -0.005(2) 0.000(2) O11 0.034(3) 0.041(3) 0.018(2) 0.000(3) 0.001(2) 0.008(3) O12 0.027(3) 0.028(2) 0.022(2) 0.003(3) -0.0074(19) 0.000(3) O13 0.022(3) 0.014(2) 0.018(3) -0.001(2) 0.000(2) -0.005(2) O14 0.019(3) 0.026(3) 0.015(3) -0.003(2) -0.001(2) -0.003(2) O15 0.023(3) 0.022(3) 0.024(3) -0.001(2) -0.007(2) 0.009(2) O16 0.025(3) 0.031(3) 0.035(3) -0.006(2) -0.009(2) 0.006(2) O17 0.030(3) 0.036(3) 0.027(3) 0.001(2) 0.008(3) -0.011(3) O18 0.020(3) 0.029(3) 0.019(3) -0.006(2) 0.000(2) -0.007(2) O19 0.032(3) 0.027(3) 0.028(3) 0.013(2) -0.001(2) 0.002(3) O20 0.023(3) 0.036(3) 0.033(3) -0.006(2) 0.004(2) 0.005(2) O21 0.038(3) 0.021(3) 0.022(3) -0.002(2) -0.009(3) 0.003(3) O22 0.048(4) 0.019(3) 0.022(3) -0.003(2) -0.009(3) 0.004(3) O23 0.030(3) 0.035(3) 0.028(3) -0.013(3) 0.010(3) -0.011(3) O25 0.041(3) 0.039(3) 0.041(3) 0.020(3) 0.002(3) -0.006(3) O24 0.040(3) 0.035(3) 0.026(3) 0.001(2) -0.008(3) 0.014(3) O26 0.052(4) 0.031(3) 0.039(3) 0.005(3) 0.013(3) -0.011(3) O27 0.023(3) 0.078(4) 0.046(4) -0.017(3) 0.003(3) 0.002(3) O1W 0.119(8) 0.118(7) 0.075(5) -0.017(5) -0.022(5) 0.042(6) O2W 0.33(2) 0.293(19) 0.202(14) -0.102(14) 0.125(14) -0.209(19) N2 0.084(7) 0.094(7) 0.095(7) 0.024(6) 0.020(6) 0.035(6) N3 0.040(4) 0.032(3) 0.025(3) 0.006(4) 0.001(3) 0.002(4) N4 0.039(4) 0.029(3) 0.028(3) 0.000(3) -0.012(3) 0.004(4) N6 0.048(5) 0.048(4) 0.045(4) 0.010(4) -0.011(4) -0.013(4) N7 0.051(5) 0.052(4) 0.044(4) -0.016(4) 0.005(4) -0.009(4) N8 0.036(4) 0.046(4) 0.033(4) -0.006(3) 0.006(3) -0.008(3) N9 0.027(4) 0.037(4) 0.018(3) 0.003(3) 0.002(3) 0.004(3) N10 0.025(4) 0.037(4) 0.057(5) 0.014(3) 0.007(3) -0.009(3) C1 0.104(11) 0.074(8) 0.058(7) -0.002(6) -0.001(7) -0.015(8) C3 0.045(5) 0.023(4) 0.034(4) -0.006(3) -0.007(4) -0.006(3) C4 0.063(7) 0.022(4) 0.037(5) 0.005(3) -0.004(4) -0.001(4) C5 0.071(7) 0.164(12) 0.050(6) -0.061(9) 0.021(5) -0.024(10) C6 0.091(9) 0.084(8) 0.129(11) -0.049(10) -0.024(8) 0.033(9) C7 0.035(5) 0.037(5) 0.074(7) -0.027(5) 0.009(5) 0.001(4) C8 0.022(4) 0.049(5) 0.042(5) -0.009(4) 0.002(4) -0.009(4) C9 0.014(4) 0.054(5) 0.036(5) 0.014(4) 0.002(4) 0.001(4) C10 0.030(5) 0.041(5) 0.045(5) -0.008(4) -0.002(4) -0.008(4)