Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_General author K.Nomiya operator KenjiNomiya data_B102942H-K10H2[P2W18Ti6O77].17H2O _database_code_CSD 165396 #============================================================================== _audit_creation_date '2001-03-26' _audit_creation_method 'by teXsan for Windows v1.06' _audit_update_record ; ? ; #============================================================================== # SUBMISSION DETAILS _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _journal_coden_Cambridge 186 _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Kenji Nomiya' _publ_contact_author_address ; Department of Materials Science, Faculty of Science, Kanagawa University, Tsuchiya, Hiratsuka, Kanagawa Japan ; _publ_contact_letter ; Dear Sir: We have submitted our article to J. Chem. Soc., Dalton Trans. (the MS number was B1-2942H). Herein we deposit crystal data in CIF file. Kenji Nomiya ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' +81-463/59-4111 (Ext. 2717) ' _publ_contact_author_fax ' +81-463/58-9684 ' _publ_contact_author_email ' nomiya@chem.kanagawa-u.ac.jp ' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and characterization of tri-titanium(IV)-1,2,3- substituted alpha-Keggin polyoxotungstates with heteroatoms P and Si. Crystal structure of the dimeric, Ti-O-Ti bridged anhydride form K10H2[alpha,alpha-P2W18Ti6O77].17H2O and ultracentrifugation molecular weight measurements in detecting the dimeric forms in aqueous solution ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_address ' Kenji Nomiya ' ; Department of Materials Science, Faculty of Science, Kanagawa University, Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Mizuto Takahashi ' ; Department of Materials Science, Faculty of Science, Kanagawa University, Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Katsunori Ohsawa ' ; Department of Materials Science, Faculty of Science, Kanagawa University, Tsuchiya, Hiratsuka, Kanagawa 259-1293, Japan ; ' Jason A. Widegren ' ; Department of Chemistry, Colorado State University, Fort Collins, CO 80523, USA ; #============================================================================== # TEXT _publ_section_abstract ; ; _publ_section_exptl_refinement ; ; _publ_section_comment ; ; _publ_section_references ; Molecular Structure Corporation. (1997-1999). teXsan for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; _publ_section_figure_captions ; ; #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_structure_solution ? _computing_structure_refinement 'teXsan for Windows version 1.06 (MSC, 1997-1999)' _computing_publication_material 'teXsan for Windows version 1.06 (MSC, 1997-1999)' #------------------------------------------------------------------------------ _cell_length_a 18.586(6) _cell_length_b 20.544(7) _cell_length_c 12.877(9) _cell_angle_alpha 99.50(4) _cell_angle_beta 105.71(4) _cell_angle_gamma 105.54(2) _cell_volume 4408(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.7 _cell_measurement_theta_max 14.7 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 4.211 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 5589.86 _chemical_formula_analytical ? _chemical_formula_sum 'H36 K10 O94 P2 Ti6 W18 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 4944.00 _exptl_absorpt_coefficient_mu 24.545 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.407 _exptl_special_details ; The scan width was (1.37+0.30tan\q)\% with an \w scan speed of 4\% per minute (up to 6 scans to achieve I/\22s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #=========================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.02 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -3 3 3 -2 2 5 -3 2 _diffrn_reflns_number 20861 _reflns_number_total 20239 _reflns_number_gt 20236 _reflns_threshold_expression I>-10.00\s(I) _diffrn_reflns_av_R_equivalents 0.05276 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04832 _diffrn_orient_matrix_UB_12 -0.01433 _diffrn_orient_matrix_UB_13 0.01919 _diffrn_orient_matrix_UB_21 0.03291 _diffrn_orient_matrix_UB_22 0.04697 _diffrn_orient_matrix_UB_23 -0.00129 _diffrn_orient_matrix_UB_31 0.00926 _diffrn_orient_matrix_UB_32 0.01789 _diffrn_orient_matrix_UB_33 0.08120 #---------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K 0 20 0.179 0.250 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; P 0 4 0.090 0.095 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; W 0 36 -1.421 6.872 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 188 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Ti 0 12 0.248 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 72 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #===================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom W(1) 0.47390(4) 0.44475(4) 0.72803(7) 0.0172(2) 1.000 . Uani d ? W(2) 0.47637(4) 0.34184(4) 0.49246(6) 0.0171(2) 1.000 . Uani d ? W(3) 0.37516(4) 0.14879(4) 0.41545(6) 0.0165(2) 1.000 . Uani d ? W(4) 0.28041(4) 0.07540(4) 0.57986(7) 0.0171(2) 1.000 . Uani d ? W(5) 0.27293(4) 0.18577(4) 0.83524(6) 0.0168(2) 1.000 . Uani d ? W(6) 0.36847(4) 0.36233(4) 0.90739(6) 0.0174(2) 1.000 . Uani d ? W(7) 0.25380(4) 0.37170(4) 0.62690(7) 0.0197(2) 1.000 . Uani d ? W(8) 0.25641(4) 0.26933(4) 0.39021(6) 0.0186(2) 1.000 . Uani d ? W(9) 0.15993(4) 0.19449(4) 0.55415(7) 0.0186(2) 1.000 . Uani d ? W(10) 0.91685(4) 0.29698(4) 0.89193(7) 0.0202(2) 1.000 . Uani d ? W(11) 0.81875(4) 0.10296(4) 0.81457(6) 0.0173(2) 1.000 . Uani d ? W(12) 0.72090(4) 0.02897(4) 0.97459(6) 0.0168(2) 1.000 . Uani d ? W(13) 0.71004(4) 0.13910(4) 1.22846(6) 0.0179(2) 1.000 . Uani d ? W(14) 0.79679(5) 0.31589(4) 1.29593(7) 0.0200(2) 1.000 . Uani d ? W(15) 0.90620(5) 0.39804(4) 1.12099(7) 0.0218(2) 1.000 . Uani d ? W(16) 0.99978(4) 0.18910(4) 1.06655(7) 0.0202(2) 1.000 . Uani d ? W(17) 0.89981(5) 0.11374(5) 1.22787(7) 0.0208(2) 1.000 . Uani d ? W(18) 0.98829(5) 0.29057(5) 1.29708(7) 0.0218(2) 1.000 . Uani d ? Ti(1) 0.5748(2) 0.3302(2) 0.7438(3) 0.0180(8) 1.000 . Uani d ? Ti(2) 0.4801(2) 0.1478(2) 0.6738(3) 0.0153(8) 1.000 . Uani d ? Ti(3) 0.4714(2) 0.2498(2) 0.9143(3) 0.0167(8) 1.000 . Uani d ? Ti(4) 0.7425(2) 0.3155(2) 0.8950(3) 0.0189(8) 1.000 . Uani d ? Ti(5) 0.6482(2) 0.1293(2) 0.8229(3) 0.0163(8) 1.000 . Uani d ? Ti(6) 0.6388(2) 0.2339(2) 1.0636(3) 0.0176(8) 1.000 . Uani d ? K(1) 0.3317(5) -0.0750(4) 0.4859(5) 0.063(2) 1.000 . Uani d ? K(2) 0.5119(5) -0.0840(5) 0.8045(8) 0.082(3) 1.000 . Uani d ? K(3) 0.7711(4) -0.1361(4) 0.8770(5) 0.056(2) 1.000 . Uani d ? K(4) 1.0291(7) 0.0624(5) 0.8153(9) 0.106(4) 1.000 . Uani d ? K(5) 1.1183(5) 0.3851(5) 1.1338(9) 0.098(3) 1.000 . Uani d ? K(6) 0.6187(7) -0.0563(5) 1.1485(9) 0.100(4) 1.000 . Uani d ? K(7) 0.5660(5) 0.3637(5) 1.2106(7) 0.074(3) 1.000 . Uani d ? K(8) 0.3500(5) 0.3688(5) 1.2068(8) 0.083(3) 1.000 . Uani d ? K(9) -0.0842(4) 0.1165(4) 0.5343(6) 0.060(2) 1.000 . Uani d ? K(10) 0.030(1) 0.327(1) 0.621(2) 0.121(8) 0.500 S Uiso d ? P(1) 0.3706(3) 0.2604(3) 0.6559(4) 0.013(1) 1.000 . Uani d ? P(2) 0.8160(3) 0.2131(3) 1.0583(4) 0.014(1) 1.000 . Uani d ? O(1) 0.5447(7) 0.2360(7) 0.684(1) 0.016(3) 1.000 . Uiso d ? O(2) 0.4692(8) 0.1779(7) 0.812(1) 0.019(3) 1.000 . Uiso d ? O(3) 0.5418(7) 0.3168(7) 0.869(1) 0.017(3) 1.000 . Uiso d ? O(4) 0.5704(8) 0.3473(7) 0.595(1) 0.020(3) 1.000 . Uiso d ? O(5) 0.3776(8) 0.0671(7) 0.635(1) 0.020(3) 1.000 . Uiso d ? O(6) 0.4526(7) 0.1245(7) 0.507(1) 0.018(3) 1.000 . Uiso d ? O(7) 0.4458(7) 0.3335(7) 0.986(1) 0.019(3) 1.000 . Uiso d ? O(8) 0.3699(8) 0.1949(7) 0.931(1) 0.021(3) 1.000 . Uiso d ? O(9) 0.5655(7) 0.4275(7) 0.780(1) 0.016(3) 1.000 . Uiso d ? O(10) 0.4816(8) 0.4306(7) 0.578(1) 0.021(3) 1.000 . Uiso d ? O(11) 0.4458(7) 0.2433(7) 0.447(1) 0.018(3) 1.000 . Uiso d ? O(12) 0.2958(8) 0.0759(7) 0.439(1) 0.021(3) 1.000 . Uiso d ? O(13) 0.2792(7) 0.1163(7) 0.726(1) 0.016(3) 1.000 . Uiso d ? O(14) 0.2872(8) 0.2798(7) 0.907(1) 0.020(3) 1.000 . Uiso d ? O(15) 0.4397(7) 0.4186(7) 0.845(1) 0.019(3) 1.000 . Uiso d ? O(16) 0.3629(8) 0.3275(7) 0.431(1) 0.022(3) 1.000 . Uiso d ? O(17) 0.2927(8) 0.1916(7) 0.376(1) 0.020(3) 1.000 . Uiso d ? O(18) 0.2015(7) 0.1211(7) 0.528(1) 0.019(3) 1.000 . Uiso d ? O(19) 0.1993(8) 0.1996(7) 0.709(1) 0.021(3) 1.000 . Uiso d ? O(20) 0.2862(8) 0.3632(7) 0.773(1) 0.023(3) 1.000 . Uiso d ? O(21) 0.3586(8) 0.4220(7) 0.647(1) 0.020(3) 1.000 . Uiso d ? O(22) 0.2368(8) 0.3456(8) 0.471(1) 0.023(3) 1.000 . Uiso d ? O(23) 0.1655(8) 0.2114(7) 0.414(1) 0.020(3) 1.000 . Uiso d ? O(24) 0.1638(8) 0.2899(7) 0.593(1) 0.021(3) 1.000 . Uiso d ? O(25) 0.4429(7) 0.3185(6) 0.6537(9) 0.010(2) 1.000 . Uiso d ? O(26) 0.3743(7) 0.1886(6) 0.603(1) 0.012(2) 1.000 . Uiso d ? O(27) 0.3722(7) 0.2638(7) 0.777(1) 0.016(3) 1.000 . Uiso d ? O(28) 0.2948(7) 0.2707(7) 0.589(1) 0.017(3) 1.000 . Uiso d ? O(29) 0.5035(8) 0.3673(8) 0.384(1) 0.025(3) 1.000 . Uiso d ? O(30) 0.3741(8) 0.1132(8) 0.285(1) 0.027(3) 1.000 . Uiso d ? O(31) 0.2215(9) -0.0098(8) 0.550(1) 0.030(3) 1.000 . Uiso d ? O(32) 0.2091(8) 0.1413(7) 0.892(1) 0.022(3) 1.000 . Uiso d ? O(33) 0.3596(8) 0.4250(8) 1.008(1) 0.026(3) 1.000 . Uiso d ? O(34) 0.5024(8) 0.5352(8) 0.769(1) 0.027(3) 1.000 . Uiso d ? O(35) 0.2189(9) 0.2716(8) 0.254(1) 0.029(3) 1.000 . Uiso d ? O(36) 0.0628(9) 0.1477(8) 0.521(1) 0.028(3) 1.000 . Uiso d ? O(37) 0.2125(8) 0.4377(8) 0.637(1) 0.028(3) 1.000 . Uiso d ? O(38) 0.6832(8) 0.3546(7) 0.807(1) 0.023(3) 1.000 . Uiso d ? O(39) 0.5554(7) 0.1038(7) 0.708(1) 0.017(3) 1.000 . Uiso d ? O(40) 0.5423(7) 0.2463(7) 1.041(1) 0.017(3) 1.000 . Uiso d ? O(41) 0.6966(7) 0.2210(7) 0.816(1) 0.018(3) 1.000 . Uiso d ? O(42) 0.6194(7) 0.1625(7) 0.945(1) 0.018(3) 1.000 . Uiso d ? O(43) 0.6897(8) 0.3017(8) 0.999(1) 0.026(3) 1.000 . Uiso d ? O(44) 0.8299(7) 0.3220(7) 0.831(1) 0.017(3) 1.000 . Uiso d ? O(45) 0.7180(7) 0.0998(7) 0.743(1) 0.019(3) 1.000 . Uiso d ? O(46) 0.6400(7) 0.0423(7) 0.873(1) 0.016(3) 1.000 . Uiso d ? O(47) 0.6272(7) 0.1661(7) 1.158(1) 0.014(2) 1.000 . Uiso d ? O(48) 0.6951(8) 0.3050(8) 1.211(1) 0.026(3) 1.000 . Uiso d ? O(49) 0.8224(8) 0.4012(7) 1.008(1) 0.022(3) 1.000 . Uiso d ? O(50) 0.9581(8) 0.3814(7) 1.013(1) 0.023(3) 1.000 . Uiso d ? O(51) 0.8625(7) 0.2011(7) 0.823(1) 0.015(3) 1.000 . Uiso d ? O(52) 0.7795(7) 0.0246(7) 0.872(1) 0.018(3) 1.000 . Uiso d ? O(53) 0.6914(7) 0.0723(7) 1.096(1) 0.019(3) 1.000 . Uiso d ? O(54) 0.7572(8) 0.2270(8) 1.334(1) 0.026(3) 1.000 . Uiso d ? O(55) 0.8409(8) 0.3743(7) 1.210(1) 0.020(3) 1.000 . Uiso d ? O(56) 0.9846(8) 0.2603(8) 0.995(1) 0.025(3) 1.000 . Uiso d ? O(57) 0.9178(7) 0.1265(7) 0.942(1) 0.019(3) 1.000 . Uiso d ? O(58) 0.8250(8) 0.0557(7) 1.091(1) 0.019(3) 1.000 . Uiso d ? O(59) 0.8158(8) 0.1325(7) 1.269(1) 0.023(3) 1.000 . Uiso d ? O(60) 0.8957(7) 0.2964(7) 1.328(1) 0.016(3) 1.000 . Uiso d ? O(61) 0.9730(8) 0.3546(8) 1.209(1) 0.027(3) 1.000 . Uiso d ? O(62) 1.0443(9) 0.2585(8) 1.203(1) 0.028(3) 1.000 . Uiso d ? O(63) 0.9775(8) 0.1246(7) 1.153(1) 0.022(3) 1.000 . Uiso d ? O(64) 0.9671(9) 0.2017(8) 1.330(1) 0.030(3) 1.000 . Uiso d ? O(65) 0.8376(7) 0.2766(7) 1.012(1) 0.014(3) 1.000 . Uiso d ? O(66) 0.7709(7) 0.1478(7) 0.961(1) 0.016(3) 1.000 . Uiso d ? O(67) 0.7627(7) 0.2216(6) 1.129(1) 0.012(2) 1.000 . Uiso d ? O(68) 0.8911(7) 0.2047(7) 1.130(1) 0.016(3) 1.000 . Uiso d ? O(69) 0.9730(9) 0.3187(8) 0.811(1) 0.032(3) 1.000 . Uiso d ? O(70) 0.8474(8) 0.0658(8) 0.709(1) 0.028(3) 1.000 . Uiso d ? O(71) 0.6850(8) -0.0567(8) 0.972(1) 0.024(3) 1.000 . Uiso d ? O(72) 0.6692(9) 0.0879(8) 1.303(1) 0.029(3) 1.000 . Uiso d ? O(73) 0.8132(9) 0.3768(8) 1.418(1) 0.030(3) 1.000 . Uiso d ? O(74) 0.9545(9) 0.4863(9) 1.182(1) 0.034(4) 1.000 . Uiso d ? O(75) 1.0816(8) 0.1768(8) 1.042(1) 0.025(3) 1.000 . Uiso d ? O(76) 0.9205(8) 0.0558(8) 1.303(1) 0.027(3) 1.000 . Uiso d ? O(77) 1.0624(9) 0.3446(9) 1.417(1) 0.036(4) 1.000 . Uiso d ? O(78) 0.084(1) 0.026(1) 1.007(2) 0.066(6) 1.000 . Uiso d ? O(79) 0.138(2) 0.314(2) 0.827(3) 0.14(1) 1.000 . Uiso d ? O(80) 0.019(2) 0.183(1) 0.759(2) 0.083(7) 1.000 . Uiso d ? O(81) 0.044(1) -0.004(1) 0.416(2) 0.059(5) 1.000 . Uiso d ? O(82) 0.188(2) 0.439(2) 0.355(3) 0.13(1) 1.000 . Uiso d ? O(83) 0.195(1) 0.308(1) 0.045(2) 0.066(6) 1.000 . Uiso d ? O(84) 0.270(2) 0.480(2) 0.130(3) 0.15(1) 1.000 . Uiso d ? O(85) 0.368(1) 0.473(1) 0.425(2) 0.056(5) 1.000 . Uiso d ? O(86) 0.379(1) 0.242(1) 0.162(2) 0.062(6) 1.000 . Uiso d ? O(87) 0.594(1) 0.440(1) 0.033(2) 0.069(6) 1.000 . Uiso d ? O(88) 0.550(2) 0.233(2) 0.300(3) 0.104(9) 1.000 . Uiso d ? O(89) 0.683(2) 0.436(1) 0.412(2) 0.090(8) 1.000 . Uiso d ? O(90) 0.516(1) 0.041(1) 0.396(2) 0.058(5) 1.000 . Uiso d ? O(91) 0.622(2) 0.211(2) 0.516(3) 0.14(1) 1.000 . Uiso d ? O(92) 0.726(1) 0.439(1) 0.650(2) 0.082(7) 1.000 . Uiso d ? O(93) 0.880(2) 0.233(2) 0.533(3) 0.13(1) 1.000 . Uiso d ? O(94) 0.123(1) 0.073(1) 0.252(2) 0.066(6) 1.000 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W(1) 0.0154(3) 0.0108(4) 0.0228(4) 0.0021(3) 0.0035(3) 0.0058(3) W(2) 0.0130(3) 0.0181(4) 0.0185(4) 0.0015(3) 0.0040(3) 0.0084(3) W(3) 0.0141(3) 0.0177(4) 0.0143(3) 0.0032(3) 0.0032(3) 0.0016(3) W(4) 0.0124(3) 0.0130(4) 0.0213(4) -0.0004(3) 0.0042(3) 0.0024(3) W(5) 0.0130(3) 0.0181(4) 0.0188(4) 0.0024(3) 0.0065(3) 0.0061(3) W(6) 0.0179(4) 0.0167(4) 0.0183(4) 0.0076(3) 0.0059(3) 0.0036(3) W(7) 0.0155(4) 0.0196(4) 0.0243(4) 0.0077(3) 0.0043(3) 0.0072(3) W(8) 0.0125(3) 0.0236(4) 0.0182(4) 0.0043(3) 0.0029(3) 0.0078(3) W(9) 0.0104(3) 0.0212(4) 0.0217(4) 0.0022(3) 0.0038(3) 0.0063(3) W(10) 0.0136(3) 0.0209(4) 0.0258(4) 0.0025(3) 0.0080(3) 0.0083(3) W(11) 0.0135(3) 0.0183(4) 0.0180(4) 0.0045(3) 0.0042(3) 0.0014(3) W(12) 0.0161(3) 0.0124(4) 0.0202(4) 0.0039(3) 0.0043(3) 0.0039(3) W(13) 0.0175(4) 0.0207(4) 0.0188(4) 0.0077(3) 0.0077(3) 0.0088(3) W(14) 0.0162(4) 0.0211(4) 0.0171(4) 0.0048(3) 0.0024(3) -0.0021(3) W(15) 0.0151(4) 0.0139(4) 0.0270(4) -0.0015(3) 0.0010(3) 0.0013(3) W(16) 0.0123(3) 0.0219(4) 0.0240(4) 0.0057(3) 0.0036(3) 0.0037(3) W(17) 0.0174(4) 0.0230(4) 0.0223(4) 0.0087(3) 0.0035(3) 0.0087(3) W(18) 0.0145(4) 0.0241(4) 0.0203(4) 0.0051(3) -0.0004(3) 0.0005(3) Ti(1) 0.012(1) 0.015(2) 0.022(2) 0.001(1) -0.000(1) 0.006(1) Ti(2) 0.011(1) 0.014(2) 0.016(2) 0.002(1) 0.001(1) 0.000(1) Ti(3) 0.013(1) 0.019(2) 0.017(2) 0.007(1) 0.003(1) 0.003(1) Ti(4) 0.011(1) 0.015(2) 0.028(2) 0.001(1) 0.003(1) 0.010(1) Ti(5) 0.014(2) 0.013(2) 0.017(2) 0.005(1) 0.001(1) 0.001(1) Ti(6) 0.015(2) 0.019(2) 0.018(2) 0.007(1) 0.004(1) 0.004(1) K(1) 0.073(5) 0.080(6) 0.041(4) 0.031(4) 0.020(3) 0.018(4) K(2) 0.060(5) 0.072(6) 0.091(6) -0.010(4) 0.039(4) -0.010(5) K(3) 0.062(4) 0.062(5) 0.039(3) 0.025(4) 0.012(3) -0.000(3) K(4) 0.120(8) 0.079(7) 0.099(7) 0.044(6) -0.003(6) 0.017(6) K(5) 0.064(5) 0.086(7) 0.114(8) -0.010(5) 0.030(5) 0.005(6) K(6) 0.135(9) 0.070(6) 0.106(8) 0.034(6) 0.049(7) 0.040(6) K(7) 0.085(6) 0.083(6) 0.068(5) 0.048(5) 0.031(4) 0.007(4) K(8) 0.070(5) 0.073(6) 0.091(6) -0.000(4) 0.025(5) 0.028(5) K(9) 0.031(3) 0.057(4) 0.080(5) 0.003(3) 0.017(3) 0.011(4) P(1) 0.011(2) 0.013(2) 0.017(2) 0.003(2) 0.005(2) 0.005(2) P(2) 0.012(2) 0.014(2) 0.016(2) 0.005(2) 0.005(2) 0.004(2) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.000000003 _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 20236 _refine_ls_number_parameters 697 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt ? _refine_ls_wR_factor_all 0.1600 _refine_ls_wR_factor_ref ? _refine_ls_goodness_of_fit_all 1.452 _refine_ls_goodness_of_fit_ref 1.450 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -4.60 _refine_diff_density_max 5.36 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(1) . . yes #---------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(3) . . . yes ? ? ? ? ? ? ? ? #---------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag W(4) K(1) 3.590(8) . . no K(1) O(90) 2.65(2) . 2_656 no K(1) O(45) 2.75(1) . 2_656 no K(1) O(72) 2.77(2) . 2_657 no K(1) O(31) 2.95(2) . . no K(1) O(5) 2.98(2) . . no K(1) O(91) 3.14(4) . 2_656 no K(1) O(12) 3.45(2) . . no K(2) O(30) 2.82(2) . 2_656 no K(2) O(46) 2.82(1) . . no K(2) O(90) 2.83(2) . 2_656 no K(2) O(88) 2.89(3) . 2_656 no K(2) O(47) 2.90(1) . 2_657 no K(2) O(71) 3.19(2) . . no K(2) O(72) 3.25(2) . 2_657 no K(3) O(78) 2.84(2) . 2_657 no K(3) O(86) 2.90(2) . 2_656 no K(3) O(71) 2.92(1) . . no K(3) O(32) 2.92(1) . 2_657 no K(3) O(75) 3.04(1) . 2_757 no K(3) O(17) 3.05(1) . 2_656 no K(3) O(94) 3.07(2) . 2_656 no K(3) O(35) 3.08(2) . 2_656 no K(3) O(30) 3.13(2) . 2_656 no K(3) O(52) 3.28(1) . . no K(4) O(78) 2.70(2) . 1_655 no K(4) O(80) 2.74(3) . 1_655 no K(4) O(81) 2.82(2) . 2_656 no K(4) O(32) 3.09(2) . 1_655 no K(4) O(76) 3.14(2) . 2_757 no K(4) O(75) 3.16(2) . . no K(4) O(94) 3.18(3) . 2_656 no K(4) O(70) 3.31(2) . . no K(4) O(57) 3.36(2) . . no K(5) O(82) 2.68(4) . 1_656 no K(5) O(83) 2.71(2) . 1_656 no K(5) O(50) 2.94(2) . . no K(5) O(56) 2.94(2) . . no K(5) O(84) 2.99(4) . 1_656 no K(5) O(62) 2.99(2) . . no K(5) O(61) 3.06(2) . . no K(6) O(2) 2.80(2) . 2_657 no K(6) O(5) 2.82(2) . 2_657 no K(6) O(13) 2.83(2) . 2_657 no K(6) O(71) 2.87(2) . . no K(6) O(53) 2.90(2) . . no K(6) O(8) 2.95(2) . 2_657 no K(6) O(72) 3.03(2) . . no K(7) O(34) 2.72(2) . 2_667 no K(7) O(89) 2.75(3) . 1_556 no K(7) O(29) 2.78(2) . 1_556 no K(7) O(40) 2.82(1) . . no K(7) O(48) 2.96(2) . . no K(7) O(7) 2.98(1) . . no K(7) O(87) 3.06(3) . 1_556 no K(7) O(88) 3.07(3) . 1_556 no K(7) O(86) 3.52(2) . 1_556 no K(8) O(86) 2.79(2) . 1_556 no K(8) O(34) 2.82(2) . 2_667 no K(8) O(83) 2.86(2) . 1_556 no K(8) O(35) 2.98(2) . 1_556 no K(8) O(33) 3.00(2) . . no K(8) O(16) 3.11(2) . 1_556 no K(8) O(85) 3.12(2) . 1_556 no K(8) O(29) 3.14(2) . 1_556 no K(8) O(84) 3.20(4) . 1_556 no K(9) O(93) 2.65(4) . 1_455 no K(9) O(31) 2.69(2) . 2_556 no K(9) O(36) 2.69(2) . . no K(9) O(81) 2.74(2) . 2_556 no K(9) O(80) 2.87(3) . . no K(9) O(70) 3.06(2) . 1_455 no K(9) O(76) 3.07(2) . 1_454 no K(9) O(59) 3.54(2) . 1_454 no K(9) O(64) 3.59(2) . 1_454 no K(10) O(93) 2.73(4) . 1_455 no K(10) O(24) 2.88(3) . . no K(10) O(77) 2.90(3) . 1_454 no K(10) O(69) 2.93(3) . 1_455 no K(10) O(79) 2.96(4) . . no K(10) O(37) 3.47(3) . . no O(1) O(91) 2.95(4) . . no O(3) O(87) 2.77(3) . 1_556 no O(4) O(92) 2.83(3) . . no O(4) O(91) 3.29(4) . . no O(5) O(72) 3.36(2) . 2_657 no O(5) O(90) 3.37(2) . 2_656 no O(6) O(90) 2.76(2) . . no O(6) O(91) 3.13(4) . . no O(7) O(87) 2.86(3) . 1_556 no O(7) O(86) 3.44(3) . 1_556 no O(7) O(34) 3.51(2) . 2_667 no O(8) O(86) 2.92(2) . 1_556 no O(8) O(71) 3.32(2) . 2_657 no O(9) O(84) 2.92(4) . 2_666 no O(9) O(87) 3.11(3) . 1_556 no O(9) O(33) 3.39(2) . 2_667 no O(10) O(85) 2.90(2) . . no O(10) O(85) 2.97(3) . 2_666 no O(11) O(88) 3.08(3) . . no O(11) O(91) 3.42(4) . . no O(11) O(86) 3.54(2) . . no O(12) O(70) 3.23(2) . 2_656 no O(12) O(94) 3.43(3) . . no O(14) O(83) 2.87(3) . 1_556 no O(14) O(79) 3.00(4) . . no O(14) O(86) 3.57(2) . 1_556 no O(15) O(87) 3.08(3) . 1_556 no O(15) O(87) 3.35(3) . 2_666 no O(16) O(85) 2.99(2) . . no O(17) O(94) 3.22(3) . . no O(18) O(81) 3.11(3) . . no O(18) O(94) 3.32(3) . . no O(19) O(79) 3.21(4) . . no O(19) O(80) 3.51(3) . . no O(20) O(79) 2.96(4) . . no O(21) O(85) 3.23(2) . . no O(21) O(89) 3.35(3) . 2_666 no O(22) O(82) 2.81(4) . . no O(22) O(77) 3.12(2) . 1_454 no O(22) O(85) 3.32(3) . . no O(23) O(94) 3.01(3) . . no O(23) O(62) 3.49(2) . 1_454 no O(23) O(64) 3.49(2) . 1_454 no O(24) O(77) 3.10(2) . 1_454 no O(24) O(79) 3.15(4) . . no O(29) O(34) 3.03(2) . 2_666 no O(29) O(89) 3.14(3) . . no O(29) O(88) 3.22(3) . . no O(29) O(86) 3.31(3) . . no O(29) O(85) 3.53(3) . 2_666 no O(30) O(71) 3.09(2) . 2_656 no O(30) O(86) 3.30(3) . . no O(30) O(52) 3.30(2) . 2_656 no O(30) O(46) 3.40(2) . 2_656 no O(30) O(88) 3.46(3) . . no O(30) O(90) 3.47(2) . . no O(31) O(70) 3.12(2) . 2_656 no O(31) O(72) 3.31(2) . 2_657 no O(31) O(81) 3.33(2) . . no O(32) O(71) 3.31(2) . 2_657 no O(32) O(75) 3.58(2) . 1_455 no O(33) O(87) 2.85(3) . 2_666 no O(33) O(84) 2.90(4) . 1_556 no O(33) O(34) 3.10(2) . 2_667 no O(33) O(83) 3.55(3) . 1_556 no O(34) O(87) 3.53(3) . 2_666 no O(35) O(83) 2.86(3) . . no O(35) O(62) 3.06(2) . 1_454 no O(35) O(75) 3.09(2) . 1_454 no O(36) O(81) 3.06(3) . . no O(36) O(76) 3.16(2) . 1_454 no O(36) O(64) 3.17(2) . 1_454 no O(36) O(80) 3.38(3) . . no O(36) O(81) 3.45(3) . 2_556 no O(37) O(89) 3.07(3) . 2_666 no O(37) O(77) 3.25(2) . 1_454 no O(37) O(82) 3.54(4) . . no O(38) O(92) 3.01(3) . . no O(38) O(84) 3.17(4) . 2_666 no O(39) O(90) 2.82(3) . 2_656 no O(40) O(88) 3.36(3) . 1_556 no O(47) O(88) 2.98(3) . 1_556 no O(48) O(88) 3.30(3) . 1_556 no O(48) O(89) 3.52(3) . 1_556 no O(51) O(80) 3.33(3) . 1_655 no O(52) O(78) 3.13(2) . 2_657 no O(52) O(94) 3.50(2) . 2_656 no O(54) O(93) 2.90(4) . 1_556 no O(56) O(80) 3.49(3) . 1_655 no O(57) O(78) 3.30(3) . 2_657 no O(57) O(80) 3.56(3) . 1_655 no O(58) O(78) 3.04(2) . 2_657 no O(59) O(93) 3.38(4) . 1_556 no O(60) O(93) 3.17(4) . 1_556 no O(63) O(78) 3.14(3) . 2_657 no O(63) O(94) 3.19(2) . 1_656 no O(64) O(93) 3.49(4) . 1_556 no O(69) O(79) 3.05(4) . 1_655 no O(69) O(80) 3.15(3) . 1_655 no O(69) O(93) 3.44(4) . . no O(70) O(94) 3.13(3) . 2_656 no O(70) O(80) 3.27(3) . 1_655 no O(70) O(81) 3.28(2) . 2_656 no O(72) O(90) 3.34(3) . 1_556 no O(73) O(89) 2.99(3) . 1_556 no O(75) O(83) 2.93(3) . 1_656 no O(75) O(78) 3.07(3) . 1_655 no O(75) O(80) 3.55(3) . 1_655 no O(76) O(81) 3.03(2) . 1_656 no O(77) O(82) 2.98(4) . 1_656 no O(78) O(78) 2.96(4) . 2_557 no O(78) O(94) 2.97(3) . 1_556 no O(79) O(83) 2.76(4) . 1_556 no O(79) O(80) 2.81(5) . . no O(81) O(81) 3.05(4) . 2_556 no O(81) O(94) 3.26(3) . . no O(82) O(92) 2.60(5) . 2_666 no O(82) O(85) 3.08(4) . . no O(82) O(89) 3.41(4) . 2_666 no O(83) O(84) 3.31(5) . . no O(84) O(92) 3.01(5) . 2_666 no O(85) O(92) 2.93(3) . 2_666 no O(85) O(89) 3.08(3) . 2_666 no O(86) O(88) 3.28(4) . . no O(88) O(91) 2.90(5) . . no O(89) O(92) 2.94(4) . . no O(90) O(91) 3.38(4) . . no #------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? # -- ENTER TORSION ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 C4 52.8(1) . . . . yes #---------------------------------------------------------- # End of CIF