# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'John Ellis' 'William W. Brennessel' 'Robert E. Jilek' 'Giovanna Tripepi' 'Eugenijus Urnezius' 'Victor G. Young' _publ_contact_author_name 'John Ellis' _publ_contact_author_address ; Department of Chemistry University of Minnesota 139 Smith Hall 207 Pleasant Street SE Minneapolis Minnesota 55455 UNITED STATES OF AMERICA ; _publ_contact_author_email ELLIS@CHEM.UMN.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Zerovalent titanium-sulfur complexes. Novel dithiocarbamato derivatives of Ti(CO)6: [Ti(CO)4(S2CNR2)]- ; data_05242m _database_code_depnum_ccdc_archive 'CCDC 637410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 05242 _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N P2, C10 H10 N O4 S2 Ti' _chemical_formula_sum 'C46 H40 N2 O4 P2 S2 Ti' _chemical_formula_weight 858.76 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' S S 0.1246 0.1234 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8175(8) _cell_length_b 22.0718(17) _cell_length_c 19.6526(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.1920(10) _cell_angle_gamma 90.00 _cell_volume 4257.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3776 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.46 _exptl_crystal_description Needles _exptl_crystal_colour Green _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7039 _exptl_absorpt_correction_T_max 0.8844 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens, SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49057 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9768 _reflns_number_gt 7916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0354P)^2^+2.6830P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9768 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _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 0.69387(3) 0.521409(15) 0.722620(17) 0.02868(9) Uani 1 1 d . . . S1 S 0.50324(6) 0.59469(2) 0.69456(3) 0.03841(12) Uani 1 1 d . . . S2 S 0.51137(6) 0.46813(2) 0.65215(3) 0.04639(15) Uani 1 1 d . . . P1 P 0.24579(5) 0.13250(2) 0.57012(2) 0.02430(10) Uani 1 1 d . . . P2 P 0.16327(5) 0.24587(2) 0.63839(2) 0.02549(10) Uani 1 1 d . . . O1 O 0.77528(16) 0.57244(7) 0.86906(7) 0.0472(4) Uani 1 1 d . . . O2 O 0.77433(16) 0.40626(7) 0.81219(7) 0.0423(4) Uani 1 1 d . . . O3 O 0.95816(16) 0.46068(7) 0.66347(8) 0.0441(4) Uani 1 1 d . . . O4 O 0.94457(16) 0.61121(7) 0.71662(9) 0.0478(4) Uani 1 1 d . . . N1 N 0.30639(18) 0.54306(8) 0.61801(9) 0.0392(4) Uani 1 1 d . . . N2 N 0.18629(16) 0.17599(7) 0.62616(8) 0.0289(3) Uani 1 1 d . . . C1 C 0.7429(2) 0.55365(9) 0.81605(10) 0.0328(4) Uani 1 1 d . . . C2 C 0.7434(2) 0.44811(9) 0.77963(9) 0.0321(4) Uani 1 1 d . . . C3 C 0.8577(2) 0.48169(9) 0.68394(9) 0.0326(4) Uani 1 1 d . . . C4 C 0.8498(2) 0.57923(9) 0.71864(10) 0.0342(4) Uani 1 1 d . . . C5 C 0.4251(2) 0.53625(9) 0.65039(10) 0.0346(4) Uani 1 1 d . . . C6 C 0.2321(2) 0.60087(12) 0.61609(12) 0.0504(6) Uani 1 1 d . . . H6A H 0.2812 0.6313 0.6444 0.060 Uiso 1 1 calc R . . H6B H 0.1401 0.5953 0.6348 0.060 Uiso 1 1 calc R . . C7 C 0.2201(3) 0.62287(12) 0.54392(14) 0.0597(7) Uani 1 1 d . . . H7A H 0.3119 0.6325 0.5270 0.072 Uiso 1 1 calc R . . H7B H 0.1650 0.6604 0.5423 0.072 Uiso 1 1 calc R . . C8 C 0.1540(4) 0.57544(14) 0.49831(16) 0.0877(11) Uani 1 1 d . . . H8A H 0.1541 0.5896 0.4505 0.105 Uiso 1 1 calc R . . H8B H 0.0582 0.5695 0.5115 0.105 Uiso 1 1 calc R . . C9 C 0.2298(3) 0.51576(12) 0.50389(13) 0.0620(7) Uani 1 1 d . . . H9A H 0.1809 0.4846 0.4766 0.074 Uiso 1 1 calc R . . H9B H 0.3221 0.5205 0.4852 0.074 Uiso 1 1 calc R . . C10 C 0.2416(2) 0.49525(11) 0.57674(11) 0.0443(5) Uani 1 1 d . . . H10A H 0.1499 0.4863 0.5942 0.053 Uiso 1 1 calc R . . H10B H 0.2968 0.4578 0.5797 0.053 Uiso 1 1 calc R . . C11 C 0.31871(18) 0.06810(8) 0.61346(9) 0.0255(4) Uani 1 1 d . . . C12 C 0.2738(2) 0.05353(9) 0.67800(9) 0.0309(4) Uani 1 1 d . . . H12A H 0.2099 0.0789 0.6998 0.037 Uiso 1 1 calc R . . C13 C 0.3223(2) 0.00181(9) 0.71056(10) 0.0349(4) Uani 1 1 d . . . H13A H 0.2920 -0.0080 0.7548 0.042 Uiso 1 1 calc R . . C14 C 0.4146(2) -0.03545(9) 0.67882(10) 0.0343(4) Uani 1 1 d . . . H14A H 0.4472 -0.0709 0.7011 0.041 Uiso 1 1 calc R . . C15 C 0.4595(2) -0.02107(9) 0.61464(11) 0.0369(5) Uani 1 1 d . . . H15A H 0.5226 -0.0468 0.5928 0.044 Uiso 1 1 calc R . . C16 C 0.41289(19) 0.03074(9) 0.58197(10) 0.0324(4) Uani 1 1 d . . . H16A H 0.4451 0.0408 0.5381 0.039 Uiso 1 1 calc R . . C17 C 0.11239(18) 0.10493(8) 0.51422(9) 0.0248(4) Uani 1 1 d . . . C18 C -0.02132(19) 0.12275(9) 0.52468(10) 0.0314(4) Uani 1 1 d . . . H18A H -0.0408 0.1509 0.5598 0.038 Uiso 1 1 calc R . . C19 C -0.1263(2) 0.09972(9) 0.48419(10) 0.0354(4) Uani 1 1 d . . . H19A H -0.2176 0.1118 0.4918 0.042 Uiso 1 1 calc R . . C20 C -0.0982(2) 0.05925(9) 0.43280(9) 0.0324(4) Uani 1 1 d . . . H20A H -0.1703 0.0439 0.4048 0.039 Uiso 1 1 calc R . . C21 C 0.0338(2) 0.04102(9) 0.42184(9) 0.0319(4) Uani 1 1 d . . . H21A H 0.0526 0.0132 0.3864 0.038 Uiso 1 1 calc R . . C22 C 0.13915(19) 0.06334(9) 0.46263(9) 0.0300(4) Uani 1 1 d . . . H22A H 0.2299 0.0503 0.4555 0.036 Uiso 1 1 calc R . . C23 C 0.37784(19) 0.16534(8) 0.51916(10) 0.0293(4) Uani 1 1 d . . . C24 C 0.5015(2) 0.18021(9) 0.55146(12) 0.0390(5) Uani 1 1 d . . . H24A H 0.5162 0.1708 0.5982 0.047 Uiso 1 1 calc R . . C25 C 0.6020(2) 0.20851(11) 0.51527(14) 0.0503(6) Uani 1 1 d . . . H25A H 0.6855 0.2192 0.5374 0.060 Uiso 1 1 calc R . . C26 C 0.5821(3) 0.22143(11) 0.44715(14) 0.0552(7) Uani 1 1 d . . . H26A H 0.6524 0.2405 0.4224 0.066 Uiso 1 1 calc R . . C27 C 0.4605(3) 0.20673(11) 0.41486(13) 0.0530(6) Uani 1 1 d . . . H27A H 0.4470 0.2156 0.3679 0.064 Uiso 1 1 calc R . . C28 C 0.3578(2) 0.17898(10) 0.45093(11) 0.0389(5) Uani 1 1 d . . . H28A H 0.2736 0.1693 0.4288 0.047 Uiso 1 1 calc R . . C29 C 0.2654(2) 0.27022(8) 0.71037(9) 0.0318(4) Uani 1 1 d . . . C30 C 0.3430(2) 0.22847(9) 0.74636(10) 0.0354(4) Uani 1 1 d . . . H30A H 0.3422 0.1871 0.7332 0.042 Uiso 1 1 calc R . . C31 C 0.4223(2) 0.24718(10) 0.80196(11) 0.0441(5) Uani 1 1 d . . . H31A H 0.4748 0.2183 0.8269 0.053 Uiso 1 1 calc R . . C32 C 0.4253(3) 0.30697(11) 0.82104(12) 0.0515(6) Uani 1 1 d . . . H32A H 0.4787 0.3193 0.8595 0.062 Uiso 1 1 calc R . . C33 C 0.3507(3) 0.34899(12) 0.78438(14) 0.0708(9) Uani 1 1 d . . . H33A H 0.3548 0.3906 0.7968 0.085 Uiso 1 1 calc R . . C34 C 0.2699(3) 0.33101(11) 0.72956(12) 0.0617(8) Uani 1 1 d . . . H34A H 0.2174 0.3601 0.7049 0.074 Uiso 1 1 calc R . . C35 C 0.20533(19) 0.29305(8) 0.56732(9) 0.0278(4) Uani 1 1 d . . . C36 C 0.3294(2) 0.32243(10) 0.56381(12) 0.0425(5) Uani 1 1 d . . . H36A H 0.3914 0.3215 0.6016 0.051 Uiso 1 1 calc R . . C37 C 0.3632(3) 0.35334(11) 0.50499(15) 0.0570(7) Uani 1 1 d . . . H37A H 0.4486 0.3734 0.5027 0.068 Uiso 1 1 calc R . . C38 C 0.2748(3) 0.35510(12) 0.45042(13) 0.0576(7) Uani 1 1 d . . . H38A H 0.2989 0.3763 0.4103 0.069 Uiso 1 1 calc R . . C39 C 0.1522(3) 0.32649(12) 0.45357(11) 0.0542(6) Uani 1 1 d . . . H39A H 0.0907 0.3282 0.4157 0.065 Uiso 1 1 calc R . . C40 C 0.1162(2) 0.29509(10) 0.51123(10) 0.0416(5) Uani 1 1 d . . . H40A H 0.0308 0.2749 0.5127 0.050 Uiso 1 1 calc R . . C41 C -0.0128(2) 0.25903(8) 0.65748(9) 0.0298(4) Uani 1 1 d . . . C42 C -0.0716(2) 0.31578(9) 0.64847(12) 0.0409(5) Uani 1 1 d . . . H42A H -0.0195 0.3481 0.6305 0.049 Uiso 1 1 calc R . . C43 C -0.2062(2) 0.32531(10) 0.66560(14) 0.0505(6) Uani 1 1 d . . . H43A H -0.2461 0.3642 0.6593 0.061 Uiso 1 1 calc R . . C44 C -0.2818(3) 0.27870(11) 0.69159(13) 0.0525(6) Uani 1 1 d . . . H44A H -0.3742 0.2853 0.7029 0.063 Uiso 1 1 calc R . . C45 C -0.2244(2) 0.22246(11) 0.70126(13) 0.0496(6) Uani 1 1 d . . . H45A H -0.2770 0.1905 0.7197 0.060 Uiso 1 1 calc R . . C46 C -0.0901(2) 0.21220(9) 0.68428(11) 0.0385(5) Uani 1 1 d . . . H46A H -0.0508 0.1733 0.6909 0.046 Uiso 1 1 calc R . . 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 0.02977(18) 0.03033(18) 0.02589(17) 0.00303(14) -0.00060(13) -0.00420(14) S1 0.0385(3) 0.0378(3) 0.0387(3) -0.0046(2) -0.0048(2) 0.0024(2) S2 0.0455(3) 0.0334(3) 0.0594(4) -0.0008(3) -0.0215(3) -0.0013(2) P1 0.0269(2) 0.0220(2) 0.0240(2) -0.00304(18) -0.00029(18) 0.00234(18) P2 0.0332(3) 0.0212(2) 0.0220(2) -0.00193(17) -0.00094(18) 0.00408(19) O1 0.0492(9) 0.0558(10) 0.0363(8) -0.0133(7) -0.0019(7) 0.0014(8) O2 0.0505(9) 0.0392(8) 0.0369(8) 0.0100(7) -0.0013(7) -0.0002(7) O3 0.0426(9) 0.0473(9) 0.0429(8) -0.0092(7) 0.0095(7) -0.0039(7) O4 0.0419(9) 0.0364(8) 0.0655(11) 0.0009(7) 0.0100(8) -0.0110(7) N1 0.0360(9) 0.0456(10) 0.0359(9) -0.0020(8) -0.0046(7) 0.0026(8) N2 0.0375(9) 0.0225(8) 0.0269(8) -0.0034(6) 0.0018(7) 0.0030(7) C1 0.0306(10) 0.0331(10) 0.0349(10) 0.0005(8) 0.0038(8) -0.0007(8) C2 0.0322(10) 0.0379(11) 0.0263(9) -0.0018(8) 0.0029(8) -0.0065(8) C3 0.0403(11) 0.0324(10) 0.0250(9) 0.0000(8) -0.0010(8) -0.0089(9) C4 0.0380(11) 0.0313(10) 0.0333(10) 0.0028(8) 0.0042(8) 0.0016(9) C5 0.0327(10) 0.0401(11) 0.0309(10) 0.0037(8) -0.0002(8) -0.0012(9) C6 0.0395(13) 0.0606(15) 0.0507(14) -0.0120(12) -0.0064(10) 0.0160(11) C7 0.0690(18) 0.0469(14) 0.0629(16) 0.0022(12) -0.0112(13) 0.0147(13) C8 0.137(3) 0.0627(19) 0.0612(18) -0.0019(15) -0.0493(19) 0.025(2) C9 0.092(2) 0.0521(15) 0.0414(13) -0.0060(11) -0.0174(13) 0.0063(14) C10 0.0353(11) 0.0501(13) 0.0471(13) 0.0025(10) -0.0069(10) -0.0069(10) C11 0.0260(9) 0.0232(9) 0.0273(9) -0.0046(7) -0.0037(7) 0.0009(7) C12 0.0360(10) 0.0287(10) 0.0280(9) -0.0057(8) -0.0006(8) 0.0039(8) C13 0.0427(11) 0.0358(11) 0.0260(9) -0.0005(8) -0.0045(8) 0.0017(9) C14 0.0347(10) 0.0296(10) 0.0381(11) 0.0026(8) -0.0086(8) 0.0043(8) C15 0.0324(10) 0.0338(11) 0.0444(12) -0.0011(9) 0.0009(9) 0.0114(8) C16 0.0312(10) 0.0337(10) 0.0322(10) -0.0003(8) 0.0023(8) 0.0061(8) C17 0.0284(9) 0.0221(9) 0.0238(8) 0.0008(7) -0.0009(7) 0.0000(7) C18 0.0323(10) 0.0293(10) 0.0327(10) -0.0049(8) -0.0008(8) 0.0052(8) C19 0.0284(10) 0.0370(11) 0.0405(11) 0.0006(9) -0.0031(8) 0.0039(8) C20 0.0361(11) 0.0320(10) 0.0289(9) 0.0053(8) -0.0076(8) -0.0065(8) C21 0.0405(11) 0.0307(10) 0.0244(9) -0.0033(8) 0.0004(8) -0.0033(8) C22 0.0286(10) 0.0316(10) 0.0299(9) -0.0036(8) 0.0028(8) 0.0018(8) C23 0.0308(10) 0.0229(9) 0.0343(10) -0.0044(8) 0.0033(8) 0.0026(7) C24 0.0332(11) 0.0350(11) 0.0488(12) -0.0026(9) -0.0008(9) 0.0004(9) C25 0.0314(12) 0.0422(13) 0.0777(18) -0.0073(12) 0.0083(11) -0.0043(9) C26 0.0477(14) 0.0443(14) 0.0747(18) -0.0022(12) 0.0275(13) -0.0088(11) C27 0.0635(16) 0.0511(14) 0.0450(13) 0.0024(11) 0.0168(12) -0.0095(12) C28 0.0429(12) 0.0372(11) 0.0369(11) -0.0004(9) 0.0054(9) -0.0042(9) C29 0.0431(11) 0.0273(9) 0.0248(9) -0.0061(7) -0.0054(8) 0.0078(8) C30 0.0458(12) 0.0266(10) 0.0334(10) -0.0013(8) -0.0063(9) 0.0056(9) C31 0.0538(14) 0.0407(12) 0.0372(11) 0.0001(9) -0.0153(10) 0.0107(10) C32 0.0643(16) 0.0507(14) 0.0386(12) -0.0162(11) -0.0210(11) 0.0114(12) C33 0.111(2) 0.0395(14) 0.0598(16) -0.0250(12) -0.0417(16) 0.0233(15) C34 0.099(2) 0.0341(12) 0.0507(14) -0.0144(11) -0.0383(14) 0.0246(13) C35 0.0342(10) 0.0232(9) 0.0261(9) -0.0008(7) 0.0009(7) 0.0053(7) C36 0.0375(12) 0.0368(11) 0.0531(13) 0.0052(10) -0.0037(10) -0.0017(9) C37 0.0470(14) 0.0484(14) 0.0764(18) 0.0205(13) 0.0189(13) -0.0028(11) C38 0.0796(19) 0.0503(15) 0.0438(14) 0.0162(11) 0.0238(13) 0.0102(14) C39 0.0769(18) 0.0569(15) 0.0285(11) 0.0074(10) -0.0037(11) 0.0037(14) C40 0.0483(13) 0.0445(12) 0.0317(10) 0.0030(9) -0.0054(9) -0.0043(10) C41 0.0364(10) 0.0256(9) 0.0276(9) -0.0009(7) 0.0048(8) 0.0036(8) C42 0.0410(12) 0.0258(10) 0.0563(14) 0.0040(9) 0.0125(10) 0.0039(9) C43 0.0450(13) 0.0304(11) 0.0765(17) 0.0003(11) 0.0151(12) 0.0094(10) C44 0.0444(13) 0.0452(13) 0.0686(16) -0.0077(12) 0.0216(12) 0.0019(11) C45 0.0523(14) 0.0394(12) 0.0580(15) 0.0024(11) 0.0214(12) -0.0063(11) C46 0.0499(13) 0.0264(10) 0.0396(11) 0.0035(8) 0.0099(9) 0.0029(9) _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 C3 1.996(2) . ? Ti1 C4 1.996(2) . ? Ti1 C1 2.018(2) . ? Ti1 C2 2.021(2) . ? Ti1 S1 2.5258(6) . ? Ti1 S2 2.5313(6) . ? S1 C5 1.726(2) . ? S2 C5 1.726(2) . ? P1 N2 1.5818(15) . ? P1 C17 1.7979(18) . ? P1 C11 1.7980(18) . ? P1 C23 1.8065(19) . ? P2 N2 1.5780(15) . ? P2 C35 1.7971(19) . ? P2 C29 1.7989(19) . ? P2 C41 1.800(2) . ? O1 C1 1.160(2) . ? O2 C2 1.161(2) . ? O3 C3 1.169(2) . ? O4 C4 1.169(2) . ? N1 C5 1.324(3) . ? N1 C10 1.468(3) . ? N1 C6 1.470(3) . ? C6 C7 1.501(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.516(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.504(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.389(3) . ? C11 C16 1.393(3) . ? C12 C13 1.388(3) . ? C12 H12A 0.9500 . ? C13 C14 1.382(3) . ? C13 H13A 0.9500 . ? C14 C15 1.382(3) . ? C14 H14A 0.9500 . ? C15 C16 1.384(3) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.390(3) . ? C17 C22 1.397(2) . ? C18 C19 1.386(3) . ? C18 H18A 0.9500 . ? C19 C20 1.381(3) . ? C19 H19A 0.9500 . ? C20 C21 1.378(3) . ? C20 H20A 0.9500 . ? C21 C22 1.386(3) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.384(3) . ? C23 C24 1.397(3) . ? C24 C25 1.378(3) . ? C24 H24A 0.9500 . ? C25 C26 1.379(4) . ? C25 H25A 0.9500 . ? C26 C27 1.379(4) . ? C26 H26A 0.9500 . ? C27 C28 1.387(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.381(3) . ? C29 C34 1.394(3) . ? C30 C31 1.391(3) . ? C30 H30A 0.9500 . ? C31 C32 1.372(3) . ? C31 H31A 0.9500 . ? C32 C33 1.376(3) . ? C32 H32A 0.9500 . ? C33 C34 1.383(3) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.383(3) . ? C35 C40 1.394(3) . ? C36 C37 1.389(3) . ? C36 H36A 0.9500 . ? C37 C38 1.366(4) . ? C37 H37A 0.9500 . ? C38 C39 1.363(4) . ? C38 H38A 0.9500 . ? C39 C40 1.381(3) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.389(3) . ? C41 C46 1.392(3) . ? C42 C43 1.386(3) . ? C42 H42A 0.9500 . ? C43 C44 1.373(3) . ? C43 H43A 0.9500 . ? C44 C45 1.375(3) . ? C44 H44A 0.9500 . ? C45 C46 1.385(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? 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 C3 Ti1 C4 68.97(8) . . ? C3 Ti1 C1 108.82(8) . . ? C4 Ti1 C1 69.00(8) . . ? C3 Ti1 C2 70.92(8) . . ? C4 Ti1 C2 110.96(8) . . ? C1 Ti1 C2 74.21(8) . . ? C3 Ti1 S1 142.87(6) . . ? C4 Ti1 S1 98.48(6) . . ? C1 Ti1 S1 97.73(6) . . ? C2 Ti1 S1 143.33(6) . . ? C3 Ti1 S2 98.88(6) . . ? C4 Ti1 S2 144.13(6) . . ? C1 Ti1 S2 144.52(6) . . ? C2 Ti1 S2 95.21(6) . . ? S1 Ti1 S2 70.44(2) . . ? C5 S1 Ti1 87.19(7) . . ? C5 S2 Ti1 87.02(7) . . ? N2 P1 C17 110.85(9) . . ? N2 P1 C11 107.40(8) . . ? C17 P1 C11 107.44(8) . . ? N2 P1 C23 114.97(8) . . ? C17 P1 C23 108.61(8) . . ? C11 P1 C23 107.25(9) . . ? N2 P2 C35 114.33(8) . . ? N2 P2 C29 109.43(9) . . ? C35 P2 C29 107.74(9) . . ? N2 P2 C41 109.31(9) . . ? C35 P2 C41 107.80(9) . . ? C29 P2 C41 108.04(9) . . ? C5 N1 C10 123.41(19) . . ? C5 N1 C6 122.83(19) . . ? C10 N1 C6 113.62(17) . . ? P2 N2 P1 139.06(11) . . ? O1 C1 Ti1 177.82(17) . . ? O2 C2 Ti1 178.75(17) . . ? O3 C3 Ti1 176.13(17) . . ? O4 C4 Ti1 177.36(18) . . ? N1 C5 S2 122.36(16) . . ? N1 C5 S1 122.30(16) . . ? S2 C5 S1 115.33(11) . . ? N1 C6 C7 109.50(19) . . ? N1 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? N1 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? C6 C7 C8 111.1(2) . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 110.7(2) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 111.0(2) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N1 C10 C9 109.49(19) . . ? N1 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? N1 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C16 119.65(17) . . ? C12 C11 P1 118.98(14) . . ? C16 C11 P1 121.25(14) . . ? C13 C12 C11 119.90(18) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C14 C13 C12 120.23(19) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C15 C14 C13 119.99(18) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.30(18) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C15 C16 C11 119.92(18) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C18 C17 C22 119.07(17) . . ? C18 C17 P1 119.47(14) . . ? C22 C17 P1 121.36(14) . . ? C19 C18 C17 120.32(18) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C20 C19 C18 119.98(18) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C21 C20 C19 120.42(18) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.91(18) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C21 C22 C17 120.29(17) . . ? C21 C22 H22A 119.9 . . ? C17 C22 H22A 119.9 . . ? C28 C23 C24 119.60(19) . . ? C28 C23 P1 122.33(15) . . ? C24 C23 P1 117.97(15) . . ? C25 C24 C23 119.8(2) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 120.5(2) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C25 C26 C27 120.1(2) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C28 120.0(2) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C23 C28 C27 120.0(2) . . ? C23 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C30 C29 C34 119.30(18) . . ? C30 C29 P2 119.72(14) . . ? C34 C29 P2 120.96(15) . . ? C29 C30 C31 119.86(19) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C32 C31 C30 120.58(19) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 H32A 120.1 . . ? C33 C32 H32A 120.1 . . ? C32 C33 C34 120.3(2) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C33 C34 C29 120.1(2) . . ? C33 C34 H34A 119.9 . . ? C29 C34 H34A 119.9 . . ? C36 C35 C40 118.99(19) . . ? C36 C35 P2 121.82(15) . . ? C40 C35 P2 118.86(15) . . ? C35 C36 C37 119.9(2) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 120.6(2) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C39 C38 C37 119.9(2) . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? C38 C39 C40 120.8(2) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C39 C40 C35 119.9(2) . . ? C39 C40 H40A 120.1 . . ? C35 C40 H40A 120.1 . . ? C42 C41 C46 119.30(19) . . ? C42 C41 P2 121.15(15) . . ? C46 C41 P2 119.50(15) . . ? C43 C42 C41 120.1(2) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C42 120.1(2) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C43 C44 C45 120.3(2) . . ? C43 C44 H44A 119.9 . . ? C45 C44 H44A 119.9 . . ? C44 C45 C46 120.3(2) . . ? C44 C45 H45A 119.9 . . ? C46 C45 H45A 119.9 . . ? C45 C46 C41 119.91(19) . . ? C45 C46 H46A 120.0 . . ? C41 C46 H46A 120.0 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Ti1 S1 C5 77.80(12) . . . . ? C4 Ti1 S1 C5 143.96(9) . . . . ? C1 Ti1 S1 C5 -146.25(9) . . . . ? C2 Ti1 S1 C5 -72.36(12) . . . . ? S2 Ti1 S1 C5 -0.77(7) . . . . ? C3 Ti1 S2 C5 -142.45(9) . . . . ? C4 Ti1 S2 C5 -76.26(13) . . . . ? C1 Ti1 S2 C5 76.14(12) . . . . ? C2 Ti1 S2 C5 146.09(9) . . . . ? S1 Ti1 S2 C5 0.77(7) . . . . ? C35 P2 N2 P1 5.1(2) . . . . ? C29 P2 N2 P1 -115.88(16) . . . . ? C41 P2 N2 P1 125.99(16) . . . . ? C17 P1 N2 P2 -94.71(17) . . . . ? C11 P1 N2 P2 148.20(15) . . . . ? C23 P1 N2 P2 28.9(2) . . . . ? C3 Ti1 C1 O1 30(5) . . . . ? C4 Ti1 C1 O1 -27(5) . . . . ? C2 Ti1 C1 O1 93(5) . . . . ? S1 Ti1 C1 O1 -123(5) . . . . ? S2 Ti1 C1 O1 170(5) . . . . ? C3 Ti1 C2 O2 37(8) . . . . ? C4 Ti1 C2 O2 -20(8) . . . . ? C1 Ti1 C2 O2 -80(8) . . . . ? S1 Ti1 C2 O2 -161(8) . . . . ? S2 Ti1 C2 O2 135(8) . . . . ? C4 Ti1 C3 O3 29(3) . . . . ? C1 Ti1 C3 O3 -29(3) . . . . ? C2 Ti1 C3 O3 -94(3) . . . . ? S1 Ti1 C3 O3 104(3) . . . . ? S2 Ti1 C3 O3 174(3) . . . . ? C3 Ti1 C4 O4 -30(4) . . . . ? C1 Ti1 C4 O4 91(4) . . . . ? C2 Ti1 C4 O4 29(4) . . . . ? S1 Ti1 C4 O4 -174(100) . . . . ? S2 Ti1 C4 O4 -105(4) . . . . ? C10 N1 C5 S2 -4.5(3) . . . . ? C6 N1 C5 S2 -179.91(17) . . . . ? C10 N1 C5 S1 176.23(16) . . . . ? C6 N1 C5 S1 0.8(3) . . . . ? Ti1 S2 C5 N1 179.51(17) . . . . ? Ti1 S2 C5 S1 -1.18(10) . . . . ? Ti1 S1 C5 N1 -179.50(17) . . . . ? Ti1 S1 C5 S2 1.18(10) . . . . ? C5 N1 C6 C7 117.0(2) . . . . ? C10 N1 C6 C7 -58.8(3) . . . . ? N1 C6 C7 C8 55.5(3) . . . . ? C6 C7 C8 C9 -54.6(4) . . . . ? C7 C8 C9 C10 54.6(4) . . . . ? C5 N1 C10 C9 -117.0(2) . . . . ? C6 N1 C10 C9 58.8(3) . . . . ? C8 C9 C10 N1 -55.5(3) . . . . ? N2 P1 C11 C12 22.90(17) . . . . ? C17 P1 C11 C12 -96.40(16) . . . . ? C23 P1 C11 C12 147.00(15) . . . . ? N2 P1 C11 C16 -160.98(15) . . . . ? C17 P1 C11 C16 79.72(17) . . . . ? C23 P1 C11 C16 -36.88(17) . . . . ? C16 C11 C12 C13 -0.3(3) . . . . ? P1 C11 C12 C13 175.90(15) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C11 -1.0(3) . . . . ? C12 C11 C16 C15 1.0(3) . . . . ? P1 C11 C16 C15 -175.12(15) . . . . ? N2 P1 C17 C18 -0.29(18) . . . . ? C11 P1 C17 C18 116.78(15) . . . . ? C23 P1 C17 C18 -127.51(15) . . . . ? N2 P1 C17 C22 -176.80(15) . . . . ? C11 P1 C17 C22 -59.72(17) . . . . ? C23 P1 C17 C22 55.99(17) . . . . ? C22 C17 C18 C19 -0.3(3) . . . . ? P1 C17 C18 C19 -176.89(15) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C19 C20 C21 C22 0.1(3) . . . . ? C20 C21 C22 C17 -0.9(3) . . . . ? C18 C17 C22 C21 1.0(3) . . . . ? P1 C17 C22 C21 177.56(14) . . . . ? N2 P1 C23 C28 -110.59(17) . . . . ? C17 P1 C23 C28 14.23(19) . . . . ? C11 P1 C23 C28 130.06(16) . . . . ? N2 P1 C23 C24 65.89(17) . . . . ? C17 P1 C23 C24 -169.28(15) . . . . ? C11 P1 C23 C24 -53.45(17) . . . . ? C28 C23 C24 C25 0.3(3) . . . . ? P1 C23 C24 C25 -176.30(16) . . . . ? C23 C24 C25 C26 -1.0(3) . . . . ? C24 C25 C26 C27 0.8(4) . . . . ? C25 C26 C27 C28 0.1(4) . . . . ? C24 C23 C28 C27 0.6(3) . . . . ? P1 C23 C28 C27 177.02(17) . . . . ? C26 C27 C28 C23 -0.8(4) . . . . ? N2 P2 C29 C30 -2.3(2) . . . . ? C35 P2 C29 C30 -127.21(17) . . . . ? C41 P2 C29 C30 116.58(18) . . . . ? N2 P2 C29 C34 176.1(2) . . . . ? C35 P2 C29 C34 51.3(2) . . . . ? C41 P2 C29 C34 -64.9(2) . . . . ? C34 C29 C30 C31 1.4(3) . . . . ? P2 C29 C30 C31 179.87(17) . . . . ? C29 C30 C31 C32 -0.7(4) . . . . ? C30 C31 C32 C33 -0.9(4) . . . . ? C31 C32 C33 C34 1.8(5) . . . . ? C32 C33 C34 C29 -1.1(5) . . . . ? C30 C29 C34 C33 -0.5(4) . . . . ? P2 C29 C34 C33 -179.0(2) . . . . ? N2 P2 C35 C36 -97.75(18) . . . . ? C29 P2 C35 C36 24.12(19) . . . . ? C41 P2 C35 C36 140.49(17) . . . . ? N2 P2 C35 C40 75.62(18) . . . . ? C29 P2 C35 C40 -162.51(16) . . . . ? C41 P2 C35 C40 -46.14(18) . . . . ? C40 C35 C36 C37 0.0(3) . . . . ? P2 C35 C36 C37 173.39(18) . . . . ? C35 C36 C37 C38 0.1(4) . . . . ? C36 C37 C38 C39 0.2(4) . . . . ? C37 C38 C39 C40 -0.6(4) . . . . ? C38 C39 C40 C35 0.7(4) . . . . ? C36 C35 C40 C39 -0.4(3) . . . . ? P2 C35 C40 C39 -173.99(18) . . . . ? N2 P2 C41 C42 -158.49(17) . . . . ? C35 P2 C41 C42 -33.67(19) . . . . ? C29 P2 C41 C42 82.51(18) . . . . ? N2 P2 C41 C46 24.07(19) . . . . ? C35 P2 C41 C46 148.90(16) . . . . ? C29 P2 C41 C46 -94.93(17) . . . . ? C46 C41 C42 C43 -0.5(3) . . . . ? P2 C41 C42 C43 -177.92(18) . . . . ? C41 C42 C43 C44 0.1(4) . . . . ? C42 C43 C44 C45 0.5(4) . . . . ? C43 C44 C45 C46 -0.6(4) . . . . ? C44 C45 C46 C41 0.2(4) . . . . ? C42 C41 C46 C45 0.4(3) . . . . ? P2 C41 C46 C45 177.85(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.386 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.046 data_99185 _database_code_depnum_ccdc_archive 'CCDC 637821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 99185 _chemical_melting_point ? _chemical_formula_moiety 'C19 H30 K N O10 S2 Ti' _chemical_formula_sum 'C19 H30 K N O10 S2 Ti' _chemical_formula_weight 583.56 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 33.882(12) _cell_length_b 8.511(3) _cell_length_c 19.052(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5494(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7485 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green-black _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8624 _exptl_absorpt_correction_T_max 0.8899 _exptl_absorpt_process_details 'SADABS (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38486 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4854 _reflns_number_gt 3492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _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^)+(0.0503P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4854 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _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 0.637770(13) 0.72610(6) 0.11335(2) 0.03284(14) Uani 1 1 d . . . K1 K 0.596704(16) 1.00812(6) -0.12350(3) 0.03327(15) Uani 1 1 d . . . S1 S 0.69201(2) 0.57554(10) 0.17604(4) 0.0529(2) Uani 1 1 d . . . S2 S 0.69890(2) 0.71272(10) 0.03651(4) 0.0496(2) Uani 1 1 d . . . O1 O 0.61079(6) 1.0818(3) 0.10674(14) 0.0719(7) Uani 1 1 d . . . O2 O 0.59276(7) 0.8228(3) 0.25286(12) 0.0719(7) Uani 1 1 d . . . O3 O 0.56012(6) 0.5215(2) 0.13152(10) 0.0506(5) Uani 1 1 d . . . O4 O 0.57934(6) 0.7958(2) -0.01250(10) 0.0484(5) Uani 1 1 d . . . N1 N 0.76122(6) 0.6273(3) 0.11341(11) 0.0387(5) Uani 1 1 d . . . O5 O 0.52471(5) 1.1323(2) -0.08225(10) 0.0442(5) Uani 1 1 d . . . O6 O 0.59375(5) 1.3177(2) -0.07653(9) 0.0412(5) Uani 1 1 d . . . O7 O 0.66862(5) 1.17157(19) -0.09436(9) 0.0358(4) Uani 1 1 d . . . O8 O 0.67115(5) 0.89212(19) -0.17319(9) 0.0356(4) Uani 1 1 d . . . O9 O 0.60169(5) 0.7054(2) -0.17626(9) 0.0385(4) Uani 1 1 d . . . O10 O 0.52737(5) 0.8546(2) -0.16339(10) 0.0434(5) Uani 1 1 d . . . C1 C 0.62168(8) 0.9521(4) 0.10888(16) 0.0472(7) Uani 1 1 d . . . C2 C 0.61028(8) 0.7858(4) 0.20310(16) 0.0462(7) Uani 1 1 d . . . C3 C 0.58921(8) 0.5928(3) 0.12540(13) 0.0350(6) Uani 1 1 d . . . C4 C 0.60176(8) 0.7675(3) 0.03249(14) 0.0344(6) Uani 1 1 d . . . C5 C 0.72252(7) 0.6354(3) 0.10864(13) 0.0350(6) Uani 1 1 d . . . C6 C 0.78106(9) 0.5623(4) 0.17484(15) 0.0621(9) Uani 1 1 d . . . H6A H 0.7622 0.5008 0.2025 0.093 Uiso 1 1 calc R . . H6B H 0.7916 0.6481 0.2036 0.093 Uiso 1 1 calc R . . H6C H 0.8028 0.4942 0.1596 0.093 Uiso 1 1 calc R . . C7 C 0.78770(9) 0.6828(4) 0.05815(16) 0.0580(9) Uani 1 1 d . . . H7A H 0.7722 0.7320 0.0207 0.087 Uiso 1 1 calc R . . H7B H 0.8025 0.5936 0.0389 0.087 Uiso 1 1 calc R . . H7C H 0.8062 0.7598 0.0777 0.087 Uiso 1 1 calc R . . C8 C 0.52389(9) 1.2977(3) -0.07328(18) 0.0523(8) Uani 1 1 d . . . H8A H 0.5000 1.3284 -0.0468 0.063 Uiso 1 1 calc R . . H8B H 0.5231 1.3500 -0.1196 0.063 Uiso 1 1 calc R . . C9 C 0.56009(8) 1.3477(3) -0.03398(16) 0.0494(8) Uani 1 1 d . . . H9A H 0.5585 1.4610 -0.0227 0.059 Uiso 1 1 calc R . . H9B H 0.5621 1.2884 0.0106 0.059 Uiso 1 1 calc R . . C10 C 0.62902(8) 1.3751(3) -0.04533(16) 0.0463(7) Uani 1 1 d . . . H10A H 0.6329 1.3258 0.0012 0.056 Uiso 1 1 calc R . . H10B H 0.6271 1.4903 -0.0387 0.056 Uiso 1 1 calc R . . C11 C 0.66318(9) 1.3371(3) -0.09216(16) 0.0461(7) Uani 1 1 d . . . H11A H 0.6580 1.3774 -0.1400 0.055 Uiso 1 1 calc R . . H11B H 0.6874 1.3883 -0.0741 0.055 Uiso 1 1 calc R . . C12 C 0.70143(8) 1.1278(3) -0.13633(14) 0.0415(7) Uani 1 1 d . . . H12A H 0.7259 1.1736 -0.1167 0.050 Uiso 1 1 calc R . . H12B H 0.6980 1.1682 -0.1847 0.050 Uiso 1 1 calc R . . C13 C 0.70448(8) 0.9538(3) -0.13753(14) 0.0398(7) Uani 1 1 d . . . H13A H 0.7290 0.9217 -0.1619 0.048 Uiso 1 1 calc R . . H13B H 0.7054 0.9126 -0.0890 0.048 Uiso 1 1 calc R . . C14 C 0.67132(8) 0.7252(3) -0.17718(15) 0.0408(7) Uani 1 1 d . . . H14A H 0.6710 0.6798 -0.1293 0.049 Uiso 1 1 calc R . . H14B H 0.6956 0.6888 -0.2012 0.049 Uiso 1 1 calc R . . C15 C 0.63566(8) 0.6721(3) -0.21711(14) 0.0403(7) Uani 1 1 d . . . H15A H 0.6341 0.7279 -0.2626 0.048 Uiso 1 1 calc R . . H15B H 0.6373 0.5579 -0.2265 0.048 Uiso 1 1 calc R . . C16 C 0.56651(8) 0.6467(3) -0.20846(15) 0.0467(7) Uani 1 1 d . . . H16A H 0.5682 0.5312 -0.2136 0.056 Uiso 1 1 calc R . . H16B H 0.5633 0.6933 -0.2557 0.056 Uiso 1 1 calc R . . C17 C 0.53196(8) 0.6888(3) -0.16352(16) 0.0474(7) Uani 1 1 d . . . H17A H 0.5078 0.6384 -0.1821 0.057 Uiso 1 1 calc R . . H17B H 0.5363 0.6507 -0.1150 0.057 Uiso 1 1 calc R . . C18 C 0.49381(8) 0.9020(4) -0.12362(18) 0.0590(9) Uani 1 1 d . . . H18A H 0.4958 0.8606 -0.0752 0.071 Uiso 1 1 calc R . . H18B H 0.4695 0.8597 -0.1452 0.071 Uiso 1 1 calc R . . C19 C 0.49229(9) 1.0774(4) -0.12224(18) 0.0610(9) Uani 1 1 d . . . H19A H 0.4937 1.1194 -0.1706 0.073 Uiso 1 1 calc R . . H19B H 0.4672 1.1130 -0.1008 0.073 Uiso 1 1 calc R . . 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 0.0271(3) 0.0396(3) 0.0318(3) 0.0021(2) -0.0008(2) 0.0018(2) K1 0.0329(3) 0.0289(3) 0.0380(3) -0.0021(2) 0.0026(3) 0.0008(2) S1 0.0361(4) 0.0750(6) 0.0474(5) 0.0296(4) 0.0110(4) 0.0132(4) S2 0.0355(4) 0.0803(6) 0.0330(4) 0.0168(4) 0.0033(3) 0.0105(4) O1 0.0508(13) 0.0410(13) 0.124(2) -0.0024(14) -0.0029(14) 0.0015(11) O2 0.0748(17) 0.1000(19) 0.0409(13) -0.0259(13) 0.0059(12) 0.0108(14) O3 0.0426(12) 0.0551(13) 0.0540(13) 0.0128(10) -0.0023(10) -0.0114(10) O4 0.0508(13) 0.0599(13) 0.0346(11) 0.0040(9) -0.0063(10) 0.0097(10) N1 0.0306(13) 0.0547(14) 0.0308(13) -0.0008(11) 0.0023(10) 0.0051(11) O5 0.0346(11) 0.0453(12) 0.0526(12) -0.0055(10) -0.0036(9) 0.0062(9) O6 0.0455(12) 0.0365(10) 0.0416(11) -0.0082(9) -0.0037(10) 0.0049(9) O7 0.0399(11) 0.0295(10) 0.0379(10) 0.0017(8) 0.0014(9) -0.0024(8) O8 0.0350(10) 0.0333(10) 0.0386(11) -0.0007(8) -0.0001(8) 0.0032(8) O9 0.0399(11) 0.0394(10) 0.0364(10) -0.0100(8) 0.0013(9) -0.0015(8) O10 0.0362(11) 0.0463(12) 0.0479(12) -0.0059(10) 0.0007(9) -0.0032(9) C1 0.0301(15) 0.0457(18) 0.066(2) -0.0030(15) -0.0039(14) -0.0046(13) C2 0.0395(16) 0.0590(19) 0.0402(17) -0.0062(15) -0.0071(14) 0.0018(14) C3 0.0368(16) 0.0404(16) 0.0278(14) 0.0053(12) -0.0032(12) 0.0036(12) C4 0.0348(15) 0.0373(15) 0.0311(15) 0.0000(12) 0.0065(13) 0.0039(12) C5 0.0321(15) 0.0389(15) 0.0338(15) 0.0018(12) 0.0027(12) 0.0040(11) C6 0.0413(18) 0.104(3) 0.0411(19) 0.0031(18) -0.0076(15) 0.0200(18) C7 0.0379(17) 0.082(2) 0.054(2) 0.0085(17) 0.0126(16) -0.0006(16) C8 0.0493(18) 0.0450(18) 0.063(2) -0.0112(15) -0.0053(16) 0.0165(14) C9 0.055(2) 0.0408(17) 0.0521(19) -0.0100(14) -0.0029(16) 0.0115(14) C10 0.0500(18) 0.0333(15) 0.0556(19) -0.0124(14) -0.0072(15) 0.0017(13) C11 0.0485(18) 0.0325(15) 0.0573(19) -0.0009(14) -0.0058(15) -0.0075(13) C12 0.0406(17) 0.0465(17) 0.0374(16) 0.0028(13) 0.0026(13) -0.0066(13) C13 0.0373(16) 0.0462(17) 0.0359(16) 0.0019(13) 0.0013(12) 0.0032(12) C14 0.0428(16) 0.0331(15) 0.0465(17) -0.0002(13) 0.0039(14) 0.0102(12) C15 0.0491(18) 0.0333(15) 0.0384(16) -0.0063(12) 0.0044(14) 0.0064(13) C16 0.0521(18) 0.0431(17) 0.0449(18) -0.0135(14) -0.0051(15) -0.0069(14) C17 0.0442(17) 0.0486(19) 0.0495(19) -0.0078(14) -0.0015(15) -0.0138(14) C18 0.0305(16) 0.070(2) 0.076(2) -0.0218(18) 0.0065(16) -0.0041(15) C19 0.0341(17) 0.071(2) 0.077(2) -0.0247(19) -0.0031(16) 0.0083(16) _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 C4 1.997(3) . ? Ti1 C1 2.001(3) . ? Ti1 C3 2.012(3) . ? Ti1 C2 2.012(3) . ? Ti1 S1 2.5388(10) . ? Ti1 S2 2.5389(11) . ? K1 O2 2.764(2) 7_575 ? K1 O9 2.7704(19) . ? K1 O5 2.772(2) . ? K1 O6 2.785(2) . ? K1 O10 2.794(2) . ? K1 O4 2.843(2) . ? K1 O7 2.860(2) . ? K1 O8 2.8693(19) . ? S1 C5 1.725(3) . ? S2 C5 1.721(3) . ? O1 C1 1.165(3) . ? O2 C2 1.162(3) . ? O2 K1 2.764(2) 7_576 ? O3 C3 1.163(3) . ? O4 C4 1.170(3) . ? N1 C5 1.316(3) . ? N1 C6 1.459(3) . ? N1 C7 1.461(3) . ? O5 C19 1.416(3) . ? O5 C8 1.418(3) . ? O6 C10 1.421(3) . ? O6 C9 1.422(3) . ? O7 C12 1.419(3) . ? O7 C11 1.422(3) . ? O8 C13 1.419(3) . ? O8 C14 1.423(3) . ? O9 C15 1.418(3) . ? O9 C16 1.431(3) . ? O10 C17 1.420(3) . ? O10 C18 1.424(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.499(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.497(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.484(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.498(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.494(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.494(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? 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 C4 Ti1 C1 68.34(11) . . ? C4 Ti1 C3 71.81(10) . . ? C1 Ti1 C3 108.91(11) . . ? C4 Ti1 C2 109.16(11) . . ? C1 Ti1 C2 70.58(13) . . ? C3 Ti1 C2 70.54(11) . . ? C4 Ti1 S1 153.44(8) . . ? C1 Ti1 S1 134.62(9) . . ? C3 Ti1 S1 104.70(8) . . ? C2 Ti1 S1 93.60(9) . . ? C4 Ti1 S2 93.53(8) . . ? C1 Ti1 S2 103.93(9) . . ? C3 Ti1 S2 135.05(8) . . ? C2 Ti1 S2 151.51(8) . . ? S1 Ti1 S2 70.01(3) . . ? O2 K1 O9 100.25(7) 7_575 . ? O2 K1 O5 90.03(7) 7_575 . ? O9 K1 O5 120.73(6) . . ? O2 K1 O6 77.25(7) 7_575 . ? O9 K1 O6 177.07(6) . . ? O5 K1 O6 61.09(6) . . ? O2 K1 O10 88.34(7) 7_575 . ? O9 K1 O10 61.16(5) . . ? O5 K1 O10 61.01(6) . . ? O6 K1 O10 119.98(6) . . ? O2 K1 O4 162.74(7) 7_575 . ? O9 K1 O4 72.04(6) . . ? O5 K1 O4 81.33(6) . . ? O6 K1 O4 110.78(6) . . ? O10 K1 O4 74.40(6) . . ? O2 K1 O7 87.33(6) 7_575 . ? O9 K1 O7 118.08(5) . . ? O5 K1 O7 120.61(6) . . ? O6 K1 O7 60.53(5) . . ? O10 K1 O7 175.37(6) . . ? O4 K1 O7 109.93(6) . . ? O2 K1 O8 86.59(7) 7_575 . ? O9 K1 O8 60.45(5) . . ? O5 K1 O8 176.59(6) . . ? O6 K1 O8 117.59(5) . . ? O10 K1 O8 119.25(6) . . ? O4 K1 O8 102.04(6) . . ? O7 K1 O8 58.83(5) . . ? C5 S1 Ti1 86.25(9) . . ? C5 S2 Ti1 86.33(9) . . ? C2 O2 K1 144.3(2) . 7_576 ? C4 O4 K1 122.77(18) . . ? C5 N1 C6 122.3(2) . . ? C5 N1 C7 123.0(2) . . ? C6 N1 C7 114.7(2) . . ? C19 O5 C8 112.2(2) . . ? C19 O5 K1 113.84(16) . . ? C8 O5 K1 115.45(16) . . ? C10 O6 C9 112.0(2) . . ? C10 O6 K1 115.43(14) . . ? C9 O6 K1 112.42(15) . . ? C12 O7 C11 112.23(19) . . ? C12 O7 K1 115.49(14) . . ? C11 O7 K1 112.17(15) . . ? C13 O8 C14 113.08(19) . . ? C13 O8 K1 114.49(14) . . ? C14 O8 K1 111.40(14) . . ? C15 O9 C16 111.77(19) . . ? C15 O9 K1 115.77(14) . . ? C16 O9 K1 115.44(15) . . ? C17 O10 C18 111.7(2) . . ? C17 O10 K1 111.92(15) . . ? C18 O10 K1 113.21(16) . . ? O1 C1 Ti1 177.3(2) . . ? O2 C2 Ti1 176.5(3) . . ? O3 C3 Ti1 176.9(2) . . ? O4 C4 Ti1 176.5(2) . . ? N1 C5 S2 122.6(2) . . ? N1 C5 S1 122.0(2) . . ? S2 C5 S1 115.38(15) . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O5 C8 C9 109.0(2) . . ? O5 C8 H8A 109.9 . . ? C9 C8 H8A 109.9 . . ? O5 C8 H8B 109.9 . . ? C9 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O6 C9 C8 108.7(2) . . ? O6 C9 H9A 109.9 . . ? C8 C9 H9A 109.9 . . ? O6 C9 H9B 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O6 C10 C11 109.1(2) . . ? O6 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? O6 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O7 C11 C10 109.4(2) . . ? O7 C11 H11A 109.8 . . ? C10 C11 H11A 109.8 . . ? O7 C11 H11B 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? O7 C12 C13 109.0(2) . . ? O7 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? O7 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O8 C13 C12 108.7(2) . . ? O8 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? O8 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? O8 C14 C15 109.0(2) . . ? O8 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? O8 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? O9 C15 C14 108.4(2) . . ? O9 C15 H15A 110.0 . . ? C14 C15 H15A 110.0 . . ? O9 C15 H15B 110.0 . . ? C14 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? O9 C16 C17 108.9(2) . . ? O9 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? O9 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O10 C17 C16 109.0(2) . . ? O10 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? O10 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? O10 C18 C19 108.7(3) . . ? O10 C18 H18A 110.0 . . ? C19 C18 H18A 110.0 . . ? O10 C18 H18B 110.0 . . ? C19 C18 H18B 110.0 . . ? H18A C18 H18B 108.3 . . ? O5 C19 C18 108.2(3) . . ? O5 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? O5 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Ti1 S1 C5 63.1(2) . . . . ? C1 Ti1 S1 C5 -81.40(16) . . . . ? C3 Ti1 S1 C5 141.75(12) . . . . ? C2 Ti1 S1 C5 -147.44(13) . . . . ? S2 Ti1 S1 C5 8.66(9) . . . . ? C4 Ti1 S2 C5 -167.30(12) . . . . ? C1 Ti1 S2 C5 124.15(13) . . . . ? C3 Ti1 S2 C5 -99.70(14) . . . . ? C2 Ti1 S2 C5 49.3(2) . . . . ? S1 Ti1 S2 C5 -8.68(9) . . . . ? O2 K1 O4 C4 170.2(2) 7_575 . . . ? O9 K1 O4 C4 104.6(2) . . . . ? O5 K1 O4 C4 -129.0(2) . . . . ? O6 K1 O4 C4 -74.6(2) . . . . ? O10 K1 O4 C4 168.8(2) . . . . ? O7 K1 O4 C4 -9.5(2) . . . . ? O8 K1 O4 C4 51.4(2) . . . . ? O2 K1 O5 C19 69.2(2) 7_575 . . . ? O9 K1 O5 C19 -32.7(2) . . . . ? O6 K1 O5 C19 144.6(2) . . . . ? O10 K1 O5 C19 -18.86(19) . . . . ? O4 K1 O5 C19 -95.8(2) . . . . ? O7 K1 O5 C19 156.13(19) . . . . ? O8 K1 O5 C19 76.5(10) . . . . ? O2 K1 O5 C8 -62.62(19) 7_575 . . . ? O9 K1 O5 C8 -164.59(17) . . . . ? O6 K1 O5 C8 12.77(17) . . . . ? O10 K1 O5 C8 -150.7(2) . . . . ? O4 K1 O5 C8 132.39(19) . . . . ? O7 K1 O5 C8 24.3(2) . . . . ? O8 K1 O5 C8 -55.3(10) . . . . ? O2 K1 O6 C10 -110.81(18) 7_575 . . . ? O9 K1 O6 C10 -79.0(12) . . . . ? O5 K1 O6 C10 151.98(19) . . . . ? O10 K1 O6 C10 168.68(17) . . . . ? O4 K1 O6 C10 85.17(18) . . . . ? O7 K1 O6 C10 -16.62(17) . . . . ? O8 K1 O6 C10 -31.58(19) . . . . ? O2 K1 O6 C9 119.06(17) 7_575 . . . ? O9 K1 O6 C9 150.9(11) . . . . ? O5 K1 O6 C9 21.85(16) . . . . ? O10 K1 O6 C9 38.55(18) . . . . ? O4 K1 O6 C9 -44.96(17) . . . . ? O7 K1 O6 C9 -146.76(18) . . . . ? O8 K1 O6 C9 -161.72(16) . . . . ? O2 K1 O7 C12 -71.53(16) 7_575 . . . ? O9 K1 O7 C12 28.66(17) . . . . ? O5 K1 O7 C12 -159.99(15) . . . . ? O6 K1 O7 C12 -148.39(17) . . . . ? O10 K1 O7 C12 -50.7(7) . . . . ? O4 K1 O7 C12 108.39(16) . . . . ? O8 K1 O7 C12 16.10(15) . . . . ? O2 K1 O7 C11 58.77(17) 7_575 . . . ? O9 K1 O7 C11 158.97(16) . . . . ? O5 K1 O7 C11 -29.69(18) . . . . ? O6 K1 O7 C11 -18.09(16) . . . . ? O10 K1 O7 C11 79.6(7) . . . . ? O4 K1 O7 C11 -121.31(17) . . . . ? O8 K1 O7 C11 146.40(18) . . . . ? O2 K1 O8 C13 107.85(16) 7_575 . . . ? O9 K1 O8 C13 -148.33(16) . . . . ? O5 K1 O8 C13 100.5(9) . . . . ? O6 K1 O8 C13 34.14(16) . . . . ? O10 K1 O8 C13 -165.97(14) . . . . ? O4 K1 O8 C13 -87.25(16) . . . . ? O7 K1 O8 C13 18.92(14) . . . . ? O2 K1 O8 C14 -122.27(17) 7_575 . . . ? O9 K1 O8 C14 -18.46(15) . . . . ? O5 K1 O8 C14 -129.6(9) . . . . ? O6 K1 O8 C14 164.02(15) . . . . ? O10 K1 O8 C14 -36.10(17) . . . . ? O4 K1 O8 C14 42.62(16) . . . . ? O7 K1 O8 C14 148.79(17) . . . . ? O2 K1 O9 C15 63.05(17) 7_575 . . . ? O5 K1 O9 C15 159.26(16) . . . . ? O6 K1 O9 C15 31.6(12) . . . . ? O10 K1 O9 C15 145.39(18) . . . . ? O4 K1 O9 C15 -132.90(17) . . . . ? O7 K1 O9 C15 -29.41(18) . . . . ? O8 K1 O9 C15 -17.05(15) . . . . ? O2 K1 O9 C16 -70.24(17) 7_575 . . . ? O5 K1 O9 C16 25.97(19) . . . . ? O6 K1 O9 C16 -101.7(11) . . . . ? O10 K1 O9 C16 12.10(16) . . . . ? O4 K1 O9 C16 93.82(17) . . . . ? O7 K1 O9 C16 -162.69(16) . . . . ? O8 K1 O9 C16 -150.34(18) . . . . ? O2 K1 O10 C17 125.03(17) 7_575 . . . ? O9 K1 O10 C17 22.37(16) . . . . ? O5 K1 O10 C17 -144.01(18) . . . . ? O6 K1 O10 C17 -160.73(16) . . . . ? O4 K1 O10 C17 -55.40(17) . . . . ? O7 K1 O10 C17 104.2(7) . . . . ? O8 K1 O10 C17 39.87(18) . . . . ? O2 K1 O10 C18 -107.7(2) 7_575 . . . ? O9 K1 O10 C18 149.7(2) . . . . ? O5 K1 O10 C18 -16.70(19) . . . . ? O6 K1 O10 C18 -33.4(2) . . . . ? O4 K1 O10 C18 71.91(19) . . . . ? O7 K1 O10 C18 -128.5(7) . . . . ? O8 K1 O10 C18 167.18(19) . . . . ? C4 Ti1 C1 O1 64(6) . . . . ? C3 Ti1 C1 O1 3(6) . . . . ? C2 Ti1 C1 O1 -57(6) . . . . ? S1 Ti1 C1 O1 -132(6) . . . . ? S2 Ti1 C1 O1 152(6) . . . . ? K1 O2 C2 Ti1 -130(4) 7_576 . . . ? C4 Ti1 C2 O2 -2(5) . . . . ? C1 Ti1 C2 O2 56(5) . . . . ? C3 Ti1 C2 O2 -64(5) . . . . ? S1 Ti1 C2 O2 -168(5) . . . . ? S2 Ti1 C2 O2 139(4) . . . . ? C4 Ti1 C3 O3 -44(4) . . . . ? C1 Ti1 C3 O3 15(4) . . . . ? C2 Ti1 C3 O3 75(4) . . . . ? S1 Ti1 C3 O3 164(4) . . . . ? S2 Ti1 C3 O3 -120(4) . . . . ? K1 O4 C4 Ti1 112(4) . . . . ? C1 Ti1 C4 O4 -49(4) . . . . ? C3 Ti1 C4 O4 70(4) . . . . ? C2 Ti1 C4 O4 9(4) . . . . ? S1 Ti1 C4 O4 157(4) . . . . ? S2 Ti1 C4 O4 -153(4) . . . . ? C6 N1 C5 S2 179.7(2) . . . . ? C7 N1 C5 S2 -0.1(4) . . . . ? C6 N1 C5 S1 2.2(4) . . . . ? C7 N1 C5 S1 -177.6(2) . . . . ? Ti1 S2 C5 N1 -164.3(2) . . . . ? Ti1 S2 C5 S1 13.35(14) . . . . ? Ti1 S1 C5 N1 164.3(2) . . . . ? Ti1 S1 C5 S2 -13.35(14) . . . . ? C19 O5 C8 C9 -177.0(3) . . . . ? K1 O5 C8 C9 -44.4(3) . . . . ? C10 O6 C9 C8 174.7(2) . . . . ? K1 O6 C9 C8 -53.4(3) . . . . ? O5 C8 C9 O6 65.8(3) . . . . ? C9 O6 C10 C11 179.0(2) . . . . ? K1 O6 C10 C11 48.6(3) . . . . ? C12 O7 C11 C10 -178.2(2) . . . . ? K1 O7 C11 C10 49.8(3) . . . . ? O6 C10 C11 O7 -66.7(3) . . . . ? C11 O7 C12 C13 -178.5(2) . . . . ? K1 O7 C12 C13 -48.2(2) . . . . ? C14 O8 C13 C12 180.0(2) . . . . ? K1 O8 C13 C12 -51.0(2) . . . . ? O7 C12 C13 O8 66.2(3) . . . . ? C13 O8 C14 C15 -178.6(2) . . . . ? K1 O8 C14 C15 50.8(2) . . . . ? C16 O9 C15 C14 -175.4(2) . . . . ? K1 O9 C15 C14 49.7(2) . . . . ? O8 C14 C15 O9 -68.1(3) . . . . ? C15 O9 C16 C17 -178.8(2) . . . . ? K1 O9 C16 C17 -43.7(3) . . . . ? C18 O10 C17 C16 177.6(2) . . . . ? K1 O10 C17 C16 -54.3(2) . . . . ? O9 C16 C17 O10 66.2(3) . . . . ? C17 O10 C18 C19 176.6(2) . . . . ? K1 O10 C18 C19 49.2(3) . . . . ? C8 O5 C19 C18 -175.2(3) . . . . ? K1 O5 C19 C18 51.4(3) . . . . ? O10 C18 C19 O5 -67.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.364 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.052