#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003374.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003374 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 560 _journal_page_last 562 _publ_section_title ; Hexaaquatitanium(III) Tris(para-Toluenesulfonate) Trihydrate ; _chemical_formula_moiety 'C21 H39 O20 S9 Ti1' _chemical_formula_sum 'C21 H39 O18 S3 Ti' _[local]_cod_chemical_formula_sum_orig 'C21 H39 O18 S3 Ti1' _chemical_formula_weight 723.61 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/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 17.519(2) _cell_length_b 7.1971(8) _cell_length_c 25.835(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.487(11) _cell_angle_gamma 90.00 _cell_volume 3257.3(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 10.74 _cell_measurement_theta_max 12.44 _exptl_absorpt_coefficient_mu 0.51 _cell_measurement_temperature 240(2) _exptl_crystal_description needle _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_colour purple _chemical_compound_source ? _diffrn_measurement_device 'Stoe Siemens diffractometer' _diffrn_measurement_method '\w/\q scans with on-line profile fitting (Clegg,' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.682 _diffrn_reflns_number 5555 _reflns_number_total 4260 _reflns_number_observed 2663 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_theta_max 22.50 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0656 _refine_ls_wR_factor_obs 0.1722 _refine_ls_wR_factor_all 0.2280 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_number_reflns 4252 _refine_ls_number_parameters 421 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0994P)^2^ + 13.4428P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max <0.001 _refine_diff_density_max .94 _refine_diff_density_min -.51 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0106 .0060 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1246 .1234 'Ti' 'Ti' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .2776 .445 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ti1 1 0.0000 0.0000 0.0000 0.0294(4) O1 1 0.0564(2) 0.2035(7) 0.0381(2) 0.0417(12) H1A 1 0.1017(19) 0.2209(92) 0.0357(27) 0.050 H1B 1 0.0335(32) 0.2868(76) 0.0516(27) 0.050 O2 1 0.0607(3) -0.1990(7) 0.0388(2) 0.0448(12) H2A 1 0.1066(18) -0.2043(97) 0.0396(28) 0.054 H2B 1 0.0408(33) -0.2898(73) 0.0517(28) 0.054 O3 1 0.0822(3) 0.0078(7) -0.0546(2) 0.0402(11) H3A 1 0.1002(37) -0.0797(62) -0.0690(25) 0.048 H3B 1 0.1008(38) 0.1062(54) -0.0616(27) 0.048 Ti2 1 0.5000 0.5000 0.0000 0.0469(5) O4 1 0.5930(3) 0.6280(10) 0.0315(2) 0.074(2) O5 1 0.5227(3) 0.2717(10) 0.0440(3) 0.076(2) H5A 1 0.5666(24) 0.2586(116) 0.0542(35) 0.091 H5B 1 0.4987(42) 0.1761(82) 0.0480(40) 0.091 O6 1 0.4288(4) 0.6034(13) 0.0554(2) 0.106(3) O7 1 0.7322(3) 0.4942(13) 0.0320(3) 0.112(3) O8 1 0.2002(4) 0.2376(17) 0.0352(4) 0.178(6) O9 1 0.2056(4) -0.2408(17) 0.0376(4) 0.183(6) S1 1 -0.08750(9) 0.4926(2) 0.10334(6) 0.0344(4) O11 1 -0.1321(2) 0.6522(6) 0.0849(2) 0.0409(12) O12 1 -0.1250(3) 0.3176(7) 0.0917(2) 0.0466(13) O13 1 -0.0087(2) 0.4996(7) 0.0849(2) 0.0441(12) C11 1 -0.0825(3) 0.5082(9) 0.1713(2) 0.035(2) C12 1 -0.1431(4) 0.4455(10) 0.2005(3) 0.041(2) H12 1 -0.1857(4) 0.3898(10) 0.1844(3) 0.049 C13 1 -0.1403(4) 0.4662(11) 0.2543(3) 0.049(2) H13 1 -0.1820(4) 0.4259(11) 0.2740(3) 0.059 C14 1 -0.0784(5) 0.5434(11) 0.2794(3) 0.051(2) C15 1 -0.0187(4) 0.6066(11) 0.2493(3) 0.050(2) H15 1 0.0239(4) 0.6615(11) 0.2656(3) 0.060 C16 1 -0.0201(4) 0.5910(10) 0.1958(3) 0.043(2) H16 1 0.0209(4) 0.6360(10) 0.1761(3) 0.052 C17 1 -0.0754(6) 0.5658(13) 0.3369(3) 0.077(3) H17A 0.74(11) -0.1156(47) 0.4926(145) 0.3525(5) 0.115 H17B 0.74(11) -0.0824(75) 0.6957(29) 0.3457(4) 0.115 H17C 0.74(11) -0.0262(29) 0.5238(171) 0.3499(6) 0.115 H17D 0.26(11) -0.0339(48) 0.6488(145) 0.3463(5) 0.115 H17E 0.26(11) -0.0671(75) 0.4457(30) 0.3530(4) 0.115 H17F 0.26(11) -0.1233(29) 0.6176(171) 0.3488(6) 0.115 S2 1 0.68085(10) 0.0168(3) 0.09762(7) 0.0488(5) O21 1 0.7422(3) -0.0484(8) 0.0656(2) 0.062(2) O22 1 0.6142(3) -0.1026(10) 0.0978(2) 0.072(2) O23 1 0.6585(3) 0.2090(9) 0.0855(2) 0.071(2) C21 1 0.7152(4) 0.0241(10) 0.1619(3) 0.041(2) C22 1 0.7840(4) -0.0592(11) 0.1748(3) 0.050(2) H22 1 0.8135(4) -0.1179(11) 0.1494(3) 0.060 C23 1 0.8085(4) -0.0544(11) 0.2259(3) 0.054(2) H23 1 0.8553(4) -0.1102(11) 0.2347(3) 0.064 C24 1 0.7665(4) 0.0297(11) 0.2647(3) 0.051(2) C25 1 0.6984(4) 0.1141(12) 0.2498(3) 0.057(2) H25 1 0.6690(4) 0.1748(12) 0.2749(3) 0.068 C26 1 0.6728(4) 0.1113(11) 0.1997(3) 0.051(2) H26 1 0.6263(4) 0.1689(11) 0.1909(3) 0.061 C27 1 0.7921(6) 0.0322(14) 0.3202(3) 0.076(3) H27A 0.63(11) 0.8382(72) -0.0413(256) 0.3240(16) 0.114 H27B 0.63(11) 0.7523(52) -0.0197(288) 0.3417(10) 0.114 H27C 0.63(11) 0.8023(123) 0.1591(34) 0.3307(26) 0.114 H27D 0.37(11) 0.7570(71) 0.1067(257) 0.3403(16) 0.114 H27E 0.37(11) 0.8429(51) 0.0851(287) 0.3226(10) 0.114 H27F 0.37(11) 0.7929(124) -0.0937(34) 0.3335(26) 0.114 S3 1 0.36136(13) 0.0680(6) 0.10830(10) 0.0958(11) O31 1 0.4216(4) 0.0047(12) 0.0763(3) 0.096(2) O32 1 0.3513(6) 0.2733(18) 0.0982(3) 0.159(5) O33 1 0.2905(5) -0.0133(21) 0.1040(3) 0.201(7) C31 1 0.3914(4) 0.0544(12) 0.1733(3) 0.052(2) C32 1 0.4629(4) -0.0146(11) 0.1866(3) 0.050(2) H32 1 0.4967(4) -0.0528(11) 0.1606(3) 0.060 C33 1 0.4840(4) -0.0268(11) 0.2373(3) 0.053(2) H33 1 0.5329(4) -0.0722(11) 0.2456(3) 0.063 C34 1 0.4360(5) 0.0250(11) 0.2771(3) 0.053(2) C35 1 0.3646(5) 0.0954(12) 0.2630(3) 0.057(2) H35 1 0.3311(5) 0.1336(12) 0.2891(3) 0.068 C36 1 0.3418(4) 0.1106(12) 0.2124(3) 0.055(2) H36 1 0.2934(4) 0.1585(12) 0.2040(3) 0.066 C37 1 0.4611(6) 0.0109(13) 0.3328(3) 0.073(3) H37A 0.60(11) 0.4945(120) 0.1144(200) 0.3412(28) 0.109 H37B 0.60(11) 0.4884(130) -0.1049(168) 0.3381(23) 0.109 H37C 0.60(11) 0.4167(12) 0.0141(367) 0.3549(6) 0.109 H37D 0.40(11) 0.4386(120) -0.0987(199) 0.3483(28) 0.109 H37E 0.40(11) 0.4447(130) 0.1206(168) 0.3514(23) 0.109 H37F 0.40(11) 0.5163(12) 0.0016(367) 0.3345(6) 0.109 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ti1 0.0267(8) 0.0015(8) 0.0042(6) 0.0334(9) -0.0020(8) 0.0282(8) O1 0.027(2) -0.006(2) 0.007(2) 0.052(3) -0.010(2) 0.047(3) O2 0.039(3) 0.002(2) -0.001(2) 0.044(3) 0.012(2) 0.051(3) O3 0.040(3) 0.000(2) 0.014(2) 0.036(3) -0.004(3) 0.045(3) Ti2 0.0340(9) 0.0102(10) -0.0089(7) 0.0720(14) -0.0076(10) 0.0347(10) O4 0.054(3) -0.005(3) -0.021(3) 0.099(5) 0.002(4) 0.069(4) O5 0.050(4) 0.005(3) -0.016(3) 0.096(5) 0.019(4) 0.081(4) O6 0.076(4) 0.045(5) -0.010(3) 0.183(8) -0.026(5) 0.059(4) O7 0.044(3) 0.001(4) -0.021(4) 0.172(8) -0.020(6) 0.121(6) O8 0.049(4) -0.043(6) -0.055(6) 0.234(12) 0.143(10) 0.250(12) O9 0.049(4) 0.049(6) -0.053(6) 0.245(13) -0.159(10) 0.254(12) S1 0.0340(9) 0.0026(8) 0.0060(7) 0.0340(9) -0.0003(8) 0.0354(9) O11 0.040(3) 0.011(2) 0.004(2) 0.042(3) 0.003(2) 0.040(3) O12 0.046(3) -0.006(2) 0.008(2) 0.046(3) -0.011(2) 0.049(3) O13 0.033(2) 0.001(2) 0.012(2) 0.049(3) -0.001(2) 0.050(3) C11 0.030(3) 0.000(3) -0.002(3) 0.036(4) 0.004(3) 0.040(4) C12 0.033(4) -0.006(3) -0.003(3) 0.047(4) 0.002(3) 0.041(4) C13 0.052(4) 0.002(4) 0.006(3) 0.056(5) 0.006(4) 0.038(4) C14 0.062(5) 0.002(4) -0.004(4) 0.048(5) -0.005(4) 0.043(4) C15 0.051(5) -0.003(4) -0.018(4) 0.048(5) -0.010(4) 0.051(5) C16 0.034(4) -0.006(3) 0.004(3) 0.044(4) -0.003(4) 0.052(5) C17 0.121(8) 0.007(6) -0.007(5) 0.070(6) 0.003(4) 0.039(5) S2 0.0345(10) 0.0045(10) -0.0008(8) 0.0633(13) -0.0030(10) 0.0486(11) O21 0.048(3) 0.011(3) 0.005(2) 0.091(5) -0.006(3) 0.048(3) O22 0.050(3) -0.015(3) 0.003(3) 0.100(5) -0.013(4) 0.068(4) O23 0.066(4) 0.018(3) -0.015(3) 0.075(4) 0.009(3) 0.070(4) C21 0.032(4) -0.001(3) 0.004(3) 0.038(4) 0.001(4) 0.052(4) C22 0.042(4) 0.003(4) 0.004(3) 0.059(5) -0.003(4) 0.048(5) C23 0.042(4) 0.002(4) -0.002(4) 0.057(5) 0.006(4) 0.063(5) C24 0.050(4) -0.011(4) -0.003(4) 0.047(5) 0.007(4) 0.055(5) C25 0.053(5) -0.007(4) 0.009(4) 0.062(6) -0.014(4) 0.055(5) C26 0.038(4) 0.010(4) 0.004(4) 0.058(5) -0.006(4) 0.057(5) C27 0.087(7) -0.015(6) -0.014(4) 0.096(8) 0.005(5) 0.045(5) S3 0.0474(14) 0.023(2) -0.0108(11) 0.184(4) -0.015(2) 0.0554(15) O31 0.072(4) 0.011(5) -0.004(3) 0.153(7) -0.015(4) 0.064(4) O32 0.140(8) 0.112(8) 0.016(6) 0.230(12) 0.039(7) 0.108(7) O33 0.091(6) -0.111(9) -0.030(5) 0.431(21) 0.025(9) 0.081(6) C31 0.036(4) 0.001(4) 0.002(4) 0.065(6) 0.000(4) 0.055(5) C32 0.038(4) 0.007(4) 0.001(3) 0.064(5) -0.005(4) 0.049(5) C33 0.042(4) 0.007(4) -0.007(4) 0.057(5) -0.001(4) 0.060(5) C34 0.067(5) -0.005(4) 0.000(4) 0.043(5) -0.005(4) 0.047(4) C35 0.057(5) 0.000(4) 0.019(4) 0.053(5) -0.004(4) 0.062(6) C36 0.038(4) 0.010(4) 0.005(4) 0.061(5) -0.001(4) 0.065(6) C37 0.103(7) -0.012(6) -0.008(5) 0.068(6) 0.005(5) 0.047(5) _cod_database_code 2003374