# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Warren Oldham' 'David A. Costa' 'Brian L. Scott' 'Michael E. Stoll' 'D. Bridget Williams' _publ_contact_author_name 'Dr Warren Oldham' _publ_contact_author_address ; Chemistry Division Los Alamos National Laboratory Mail Stop J514 Los Alamos New Mexico 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email WOLDHAM@LANL.GOV _publ_requested_journal 'Chemical Communications' _publ_section_title ; Coordination chemistry of the bis(trifluoromethylsulfonyl)imide anion: molecular interactions in room temperature ionic liquids ; data_ccd683s _database_code_depnum_ccdc_archive 'CCDC 255445' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34 F12 N3 O8 S4 Si Ti' _chemical_formula_weight 900.75 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.244(3) _cell_length_b 12.187(3) _cell_length_c 15.560(4) _cell_angle_alpha 92.299(5) _cell_angle_beta 102.362(4) _cell_angle_gamma 114.124(4) _cell_volume 1713.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 918 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 0.8822 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 with SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 11041 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5780 _reflns_number_gt 4962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Part of one of the NTf ligands was refined in two, one-half occupancy postions. The two sets of atomic positions were labeled as primed and unprimed S2, O3, O4, C17, F4, F5, and F6. The electron density for one n-hexane molecule per unit cell (123 \%A^3^; 34 electrons), centered at 0 0 0.5, was removed using the SQUEEZE facility in the program PLATON (Spek, A.L. (1990), Acta Cryst. A46, C-34). ; _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^)+(0.0637P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5780 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1541 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.677 _refine_ls_restrained_S_all 1.677 _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 Si1 Si -0.25923(11) 0.13425(10) 0.24177(7) 0.0297(3) Uani 1 1 d . . . Ti1 Ti 0.04143(7) 0.29622(6) 0.23493(4) 0.02106(19) Uani 1 1 d . . . S1 S 0.07775(12) 0.58878(9) 0.26059(7) 0.0366(3) Uani 1 1 d . . . S2 S 0.3423(3) 0.7387(2) 0.39448(15) 0.0428(5) Uani 0.50 1 d P . . S2' S 0.2646(3) 0.8000(2) 0.3690(3) 0.0722(10) Uani 0.50 1 d P . . S3 S 0.23282(10) 0.21050(9) 0.11414(6) 0.0288(2) Uani 1 1 d . . . S4 S 0.39221(10) 0.44349(9) 0.20849(7) 0.0322(3) Uani 1 1 d . . . N1 N -0.1602(3) 0.2162(3) 0.16874(19) 0.0233(6) Uani 1 1 d . . . N2 N 0.1688(4) 0.6515(3) 0.3554(3) 0.0478(10) Uani 1 1 d . . . N3 N 0.3769(3) 0.3292(3) 0.1504(2) 0.0349(8) Uani 1 1 d . . . O1 O 0.0241(3) 0.4584(2) 0.25892(17) 0.0314(6) Uani 1 1 d . . . O2 O 0.1298(4) 0.6349(3) 0.1869(2) 0.0636(10) Uani 1 1 d . . . O3 O 0.431(2) 0.733(3) 0.3340(16) 0.081(5) Uani 0.50 1 d P . . O3' O 0.240(2) 0.8445(14) 0.4515(14) 0.160(10) Uani 0.50 1 d P . . O4 O 0.4557(16) 0.7477(18) 0.4709(11) 0.118(6) Uani 0.50 1 d P . . O4' O 0.270(3) 0.8778(14) 0.3086(17) 0.104(9) Uani 0.50 1 d P . . O5 O 0.1041(3) 0.2115(2) 0.13854(16) 0.0278(6) Uani 1 1 d . . . O6 O 0.2569(3) 0.1057(3) 0.1248(2) 0.0407(7) Uani 1 1 d . . . O7 O 0.2552(3) 0.4302(2) 0.22887(18) 0.0325(6) Uani 1 1 d . . . O8 O 0.5198(3) 0.4883(3) 0.2789(2) 0.0519(8) Uani 1 1 d . . . C1 C -0.0795(4) 0.1710(3) 0.3243(2) 0.0263(8) Uani 1 1 d . . . C2 C 0.0214(4) 0.1266(3) 0.3031(2) 0.0290(8) Uani 1 1 d . . . C3 C 0.1670(4) 0.2115(4) 0.3441(2) 0.0322(9) Uani 1 1 d . . . C4 C 0.1594(4) 0.3110(4) 0.3914(2) 0.0342(9) Uani 1 1 d . . . C5 C 0.0087(4) 0.2839(4) 0.3803(2) 0.0294(8) Uani 1 1 d . . . C6 C -0.0200(5) 0.0069(4) 0.2485(3) 0.0407(10) Uani 1 1 d . . . H6A H -0.1256 -0.0347 0.2271 0.061 Uiso 1 1 calc R . . H6B H 0.0155 -0.0421 0.2846 0.061 Uiso 1 1 calc R . . H6C H 0.0238 0.0211 0.1989 0.061 Uiso 1 1 calc R . . C7 C 0.3054(5) 0.1961(5) 0.3482(3) 0.0488(12) Uani 1 1 d . . . H7A H 0.2826 0.1228 0.3108 0.073 Uiso 1 1 calc R . . H7B H 0.3483 0.1915 0.4084 0.073 Uiso 1 1 calc R . . H7C H 0.3742 0.2643 0.3281 0.073 Uiso 1 1 calc R . . C8 C 0.2890(5) 0.4171(4) 0.4485(3) 0.0477(11) Uani 1 1 d . . . H8A H 0.2557 0.4710 0.4735 0.072 Uiso 1 1 calc R . . H8B H 0.3552 0.4593 0.4132 0.072 Uiso 1 1 calc R . . H8C H 0.3397 0.3891 0.4955 0.072 Uiso 1 1 calc R . . C9 C -0.0430(5) 0.3626(4) 0.4281(3) 0.0449(11) Uani 1 1 d . . . H9A H 0.0410 0.4335 0.4614 0.067 Uiso 1 1 calc R . . H9B H -0.0977 0.3176 0.4679 0.067 Uiso 1 1 calc R . . H9C H -0.1054 0.3867 0.3854 0.067 Uiso 1 1 calc R . . C10 C -0.3760(5) 0.1984(5) 0.2792(3) 0.0477(12) Uani 1 1 d . . . H10A H -0.3184 0.2836 0.3002 0.072 Uiso 1 1 calc R . . H10B H -0.4127 0.1577 0.3264 0.072 Uiso 1 1 calc R . . H10C H -0.4576 0.1873 0.2304 0.072 Uiso 1 1 calc R . . C11 C -0.3754(5) -0.0296(4) 0.2008(4) 0.0532(12) Uani 1 1 d . . . H11A H -0.3171 -0.0649 0.1806 0.080 Uiso 1 1 calc R . . H11B H -0.4568 -0.0388 0.1524 0.080 Uiso 1 1 calc R . . H11C H -0.4124 -0.0697 0.2480 0.080 Uiso 1 1 calc R . . C12 C -0.2181(4) 0.2293(4) 0.0750(2) 0.0305(9) Uani 1 1 d . . . C13 C -0.3650(4) 0.2380(4) 0.0651(3) 0.0417(10) Uani 1 1 d . . . H13A H -0.4345 0.1667 0.0819 0.063 Uiso 1 1 calc R . . H13B H -0.4030 0.2442 0.0044 0.063 Uiso 1 1 calc R . . H13C H -0.3499 0.3087 0.1028 0.063 Uiso 1 1 calc R . . C14 C -0.2441(5) 0.1147(4) 0.0154(3) 0.0403(10) Uani 1 1 d . . . H14A H -0.1522 0.1087 0.0211 0.060 Uiso 1 1 calc R . . H14B H -0.2833 0.1197 -0.0454 0.060 Uiso 1 1 calc R . . H14C H -0.3132 0.0443 0.0332 0.060 Uiso 1 1 calc R . . C15 C -0.1083(4) 0.3413(4) 0.0487(3) 0.0353(9) Uani 1 1 d . . . H15A H -0.0159 0.3358 0.0554 0.053 Uiso 1 1 calc R . . H15B H -0.0935 0.4121 0.0862 0.053 Uiso 1 1 calc R . . H15C H -0.1457 0.3473 -0.0121 0.053 Uiso 1 1 calc R . . C16 C -0.0939(6) 0.6060(5) 0.2547(4) 0.0552(13) Uani 1 1 d . . . C17 C 0.3404(14) 0.8873(12) 0.3757(9) 0.059(3) Uiso 0.50 1 d P . . C17' C 0.4431(15) 0.8002(13) 0.4072(9) 0.067(3) Uiso 0.50 1 d P . . C18 C 0.1892(5) 0.2108(4) -0.0067(3) 0.0413(10) Uani 1 1 d . . . C19 C 0.4243(5) 0.5563(4) 0.1328(3) 0.0487(12) Uani 1 1 d . . . F1 F -0.1911(4) 0.5432(3) 0.1809(2) 0.0798(10) Uani 1 1 d . . . F2 F -0.0673(5) 0.7206(3) 0.2537(3) 0.0982(13) Uani 1 1 d . . . F3 F -0.1467(3) 0.5686(3) 0.3225(2) 0.0704(9) Uani 1 1 d . . . F4 F 0.4763(10) 0.9727(6) 0.4032(6) 0.091(2) Uani 0.50 1 d P . . F4' F 0.5434(8) 0.9169(8) 0.4297(7) 0.104(3) Uani 0.50 1 d P . . F5 F 0.2593(13) 0.9060(9) 0.4207(8) 0.090(3) Uani 0.50 1 d P . . F5' F 0.3901(10) 0.7467(10) 0.4884(7) 0.070(3) Uani 0.50 1 d P . . F6 F 0.294(3) 0.8810(17) 0.2877(13) 0.096(6) Uani 0.50 1 d P . . F6' F 0.473(2) 0.741(3) 0.3552(17) 0.103(6) Uani 0.50 1 d P . . F7 F 0.0677(3) 0.1120(3) -0.04338(17) 0.0613(8) Uani 1 1 d . . . F8 F 0.2973(3) 0.2106(3) -0.03798(18) 0.0603(8) Uani 1 1 d . . . F9 F 0.1672(4) 0.3063(3) -0.02640(18) 0.0635(8) Uani 1 1 d . . . F10 F 0.5270(4) 0.5581(4) 0.0943(3) 0.0843(11) Uani 1 1 d . . . F11 F 0.3030(4) 0.5299(3) 0.0700(2) 0.0771(10) Uani 1 1 d . . . F12 F 0.4622(5) 0.6633(3) 0.1735(3) 0.0964(13) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0244(5) 0.0305(6) 0.0322(6) 0.0048(5) 0.0103(4) 0.0082(4) Ti1 0.0213(3) 0.0213(3) 0.0208(3) 0.0036(3) 0.0055(2) 0.0091(3) S1 0.0431(6) 0.0240(5) 0.0428(6) 0.0032(4) 0.0161(5) 0.0119(4) S2 0.0366(12) 0.0378(12) 0.0428(13) -0.0033(10) 0.0046(10) 0.0085(11) S2' 0.0453(15) 0.0314(14) 0.121(3) -0.0199(17) 0.0083(16) 0.0068(12) S3 0.0293(5) 0.0304(5) 0.0316(5) 0.0055(4) 0.0120(4) 0.0153(4) S4 0.0249(5) 0.0315(5) 0.0379(6) 0.0050(4) 0.0104(4) 0.0087(4) N1 0.0216(15) 0.0244(16) 0.0233(15) 0.0030(13) 0.0044(12) 0.0098(13) N2 0.038(2) 0.038(2) 0.054(2) -0.0057(18) 0.0147(18) 0.0038(17) N3 0.0264(17) 0.0369(19) 0.045(2) 0.0038(16) 0.0135(15) 0.0144(15) O1 0.0345(14) 0.0278(14) 0.0353(15) 0.0032(12) 0.0096(12) 0.0163(12) O2 0.095(3) 0.045(2) 0.060(2) 0.0184(17) 0.041(2) 0.027(2) O3 0.045(9) 0.109(9) 0.082(9) -0.040(8) 0.001(7) 0.039(8) O3' 0.128(11) 0.099(12) 0.21(2) -0.072(12) 0.112(13) -0.022(10) O4 0.087(11) 0.125(11) 0.086(11) 0.046(9) -0.012(8) 0.005(9) O4' 0.128(16) 0.029(7) 0.123(18) 0.008(8) -0.015(13) 0.027(8) O5 0.0257(13) 0.0302(14) 0.0264(13) 0.0006(11) 0.0075(11) 0.0108(11) O6 0.0440(17) 0.0363(16) 0.0515(18) 0.0095(14) 0.0185(14) 0.0229(14) O7 0.0285(14) 0.0276(14) 0.0407(16) 0.0027(12) 0.0146(12) 0.0084(12) O8 0.0316(16) 0.061(2) 0.0487(19) -0.0049(16) -0.0005(14) 0.0119(15) C1 0.032(2) 0.0240(19) 0.0266(19) 0.0100(16) 0.0133(16) 0.0120(16) C2 0.038(2) 0.030(2) 0.0247(19) 0.0108(16) 0.0106(17) 0.0178(18) C3 0.037(2) 0.045(2) 0.025(2) 0.0150(18) 0.0104(17) 0.025(2) C4 0.037(2) 0.039(2) 0.0228(19) 0.0068(17) 0.0026(17) 0.0146(19) C5 0.036(2) 0.036(2) 0.0213(19) 0.0071(16) 0.0111(16) 0.0188(18) C6 0.059(3) 0.028(2) 0.046(3) 0.0120(19) 0.025(2) 0.023(2) C7 0.043(3) 0.072(3) 0.047(3) 0.027(2) 0.015(2) 0.036(3) C8 0.045(3) 0.047(3) 0.034(2) 0.005(2) 0.003(2) 0.006(2) C9 0.053(3) 0.045(3) 0.039(2) -0.006(2) 0.018(2) 0.022(2) C10 0.036(2) 0.070(3) 0.046(3) 0.012(2) 0.017(2) 0.027(2) C11 0.045(3) 0.035(3) 0.059(3) 0.008(2) 0.014(2) -0.004(2) C12 0.0265(19) 0.037(2) 0.0254(19) 0.0019(17) 0.0023(16) 0.0135(17) C13 0.031(2) 0.053(3) 0.043(2) 0.015(2) 0.0068(19) 0.021(2) C14 0.041(2) 0.039(2) 0.032(2) -0.0072(18) -0.0002(18) 0.014(2) C15 0.036(2) 0.040(2) 0.032(2) 0.0131(18) 0.0073(17) 0.0185(19) C16 0.070(3) 0.046(3) 0.063(3) 0.003(3) 0.008(3) 0.042(3) C18 0.049(3) 0.051(3) 0.031(2) 0.007(2) 0.018(2) 0.024(2) C19 0.049(3) 0.038(3) 0.058(3) 0.012(2) 0.026(2) 0.012(2) F1 0.078(2) 0.087(2) 0.078(2) -0.0104(19) -0.0148(18) 0.057(2) F2 0.121(3) 0.052(2) 0.147(4) 0.010(2) 0.034(3) 0.062(2) F3 0.0591(19) 0.089(2) 0.084(2) 0.0149(19) 0.0329(17) 0.0448(18) F4 0.091(6) 0.038(4) 0.092(6) -0.008(4) 0.007(5) -0.013(4) F4' 0.051(4) 0.069(5) 0.127(8) -0.026(5) -0.001(4) -0.024(4) F5 0.104(8) 0.073(7) 0.115(7) 0.002(6) 0.044(6) 0.051(7) F5' 0.063(6) 0.076(5) 0.043(4) -0.005(4) -0.004(4) 0.012(5) F6 0.086(8) 0.105(11) 0.057(6) 0.038(6) 0.007(6) 0.006(6) F6' 0.068(12) 0.097(10) 0.143(16) -0.009(10) 0.012(9) 0.043(10) F7 0.0509(17) 0.069(2) 0.0406(15) -0.0100(14) 0.0108(13) 0.0052(15) F8 0.0567(17) 0.084(2) 0.0505(17) 0.0068(15) 0.0342(14) 0.0303(16) F9 0.097(2) 0.076(2) 0.0404(16) 0.0241(15) 0.0223(15) 0.0546(19) F10 0.088(2) 0.098(3) 0.098(3) 0.047(2) 0.068(2) 0.045(2) F11 0.087(2) 0.066(2) 0.082(2) 0.0367(18) 0.012(2) 0.0381(19) F12 0.149(4) 0.0318(16) 0.095(3) 0.0087(18) 0.056(3) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.754(3) . ? Si1 C10 1.846(4) . ? Si1 C11 1.854(5) . ? Si1 C1 1.872(4) . ? Si1 Ti1 2.9293(14) . ? Ti1 N1 1.907(3) . ? Ti1 O1 2.082(3) . ? Ti1 O5 2.135(2) . ? Ti1 O7 2.156(3) . ? Ti1 C1 2.272(4) . ? Ti1 C2 2.315(4) . ? Ti1 C5 2.359(4) . ? Ti1 C3 2.429(4) . ? Ti1 C4 2.438(4) . ? S1 O2 1.408(4) . ? S1 O1 1.451(3) . ? S1 N2 1.539(4) . ? S1 C16 1.838(5) . ? S2 C17' 0.967(14) . ? S2 S2' 1.313(4) . ? S2 F5' 1.425(11) . ? S2 O4 1.438(16) . ? S2 O3 1.46(2) . ? S2 F6' 1.58(2) . ? S2 N2 1.613(4) . ? S2 C17 1.854(13) . ? S2' C17 1.013(13) . ? S2' O4' 1.36(2) . ? S2' O3' 1.485(16) . ? S2' F5 1.520(10) . ? S2' F6 1.639(18) . ? S2' N2 1.647(5) . ? S2' C17' 1.797(14) . ? S3 O6 1.406(3) . ? S3 O5 1.453(3) . ? S3 N3 1.557(3) . ? S3 C18 1.837(4) . ? S4 O8 1.400(3) . ? S4 O7 1.451(3) . ? S4 N3 1.563(3) . ? S4 C19 1.820(5) . ? N1 C12 1.494(5) . ? O3 C17' 1.33(3) . ? O3' F5 0.88(2) . ? O3' C17 1.691(19) . ? O4 F5' 0.773(16) . ? O4 C17' 1.21(2) . ? O4' C17 1.11(2) . ? O4' F5 1.80(3) . ? C1 C5 1.422(5) . ? C1 C2 1.434(5) . ? C2 C3 1.407(6) . ? C2 C6 1.508(5) . ? C3 C4 1.431(6) . ? C3 C7 1.492(5) . ? C4 C5 1.411(6) . ? C4 C8 1.491(6) . ? C5 C9 1.509(5) . ? C12 C15 1.510(6) . ? C12 C13 1.528(5) . ? C12 C14 1.538(5) . ? C16 F3 1.302(6) . ? C16 F1 1.309(6) . ? C16 F2 1.310(6) . ? C17 F5 1.273(15) . ? C17 F4 1.315(14) . ? C17 F6 1.34(2) . ? C17 C17' 1.791(18) . ? C17' F6' 1.23(2) . ? C17' F4' 1.346(16) . ? C17' F5' 1.545(18) . ? C18 F8 1.303(5) . ? C18 F9 1.309(5) . ? C18 F7 1.319(5) . ? C19 F12 1.292(6) . ? C19 F10 1.311(5) . ? C19 F11 1.315(6) . ? F4 F4' 1.178(11) . ? 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 N1 Si1 C10 114.36(19) . . ? N1 Si1 C11 115.1(2) . . ? C10 Si1 C11 107.9(2) . . ? N1 Si1 C1 89.01(15) . . ? C10 Si1 C1 114.36(19) . . ? C11 Si1 C1 115.4(2) . . ? N1 Si1 Ti1 38.70(9) . . ? C10 Si1 Ti1 119.65(17) . . ? C11 Si1 Ti1 131.91(17) . . ? C1 Si1 Ti1 50.85(12) . . ? N1 Ti1 O1 91.80(11) . . ? N1 Ti1 O5 90.18(11) . . ? O1 Ti1 O5 137.61(11) . . ? N1 Ti1 O7 142.46(12) . . ? O1 Ti1 O7 77.70(10) . . ? O5 Ti1 O7 75.30(10) . . ? N1 Ti1 C1 74.39(13) . . ? O1 Ti1 C1 106.23(12) . . ? O5 Ti1 C1 115.02(11) . . ? O7 Ti1 C1 143.12(12) . . ? N1 Ti1 C2 91.29(13) . . ? O1 Ti1 C2 138.90(12) . . ? O5 Ti1 C2 83.34(12) . . ? O7 Ti1 C2 120.28(12) . . ? C1 Ti1 C2 36.42(13) . . ? N1 Ti1 C5 99.50(13) . . ? O1 Ti1 C5 80.57(12) . . ? O5 Ti1 C5 140.59(12) . . ? O7 Ti1 C5 113.78(12) . . ? C1 Ti1 C5 35.70(13) . . ? C2 Ti1 C5 58.52(13) . . ? N1 Ti1 C3 125.64(14) . . ? O1 Ti1 C3 125.10(12) . . ? O5 Ti1 C3 86.19(11) . . ? O7 Ti1 C3 88.36(13) . . ? C1 Ti1 C3 58.85(13) . . ? C2 Ti1 C3 34.40(14) . . ? C5 Ti1 C3 57.16(13) . . ? N1 Ti1 C4 131.80(14) . . ? O1 Ti1 C4 91.27(12) . . ? O5 Ti1 C4 117.86(12) . . ? O7 Ti1 C4 84.88(13) . . ? C1 Ti1 C4 58.66(14) . . ? C2 Ti1 C4 57.61(14) . . ? C5 Ti1 C4 34.15(13) . . ? C3 Ti1 C4 34.19(13) . . ? N1 Ti1 Si1 35.09(9) . . ? O1 Ti1 Si1 96.57(8) . . ? O5 Ti1 Si1 108.64(7) . . ? O7 Ti1 Si1 174.08(7) . . ? C1 Ti1 Si1 39.73(9) . . ? C2 Ti1 Si1 65.10(10) . . ? C5 Ti1 Si1 66.19(10) . . ? C3 Ti1 Si1 96.25(10) . . ? C4 Ti1 Si1 96.83(10) . . ? O2 S1 O1 115.77(18) . . ? O2 S1 N2 120.0(2) . . ? O1 S1 N2 108.7(2) . . ? O2 S1 C16 107.2(3) . . ? O1 S1 C16 100.5(2) . . ? N2 S1 C16 101.8(2) . . ? C17' S2 S2' 102.9(8) . . ? C17' S2 F5' 77.9(9) . . ? S2' S2 F5' 114.2(5) . . ? C17' S2 O4 56.6(10) . . ? S2' S2 O4 136.3(9) . . ? F5' S2 O4 31.3(6) . . ? C17' S2 O3 62.6(13) . . ? S2' S2 O3 113.4(13) . . ? F5' S2 O3 123.1(10) . . ? O4 S2 O3 91.8(11) . . ? C17' S2 F6' 51.2(10) . . ? S2' S2 F6' 124.6(11) . . ? F5' S2 F6' 106.8(9) . . ? O4 S2 F6' 75.4(11) . . ? O3 S2 F6' 16.5(14) . . ? C17' S2 N2 167.6(9) . . ? S2' S2 N2 67.6(2) . . ? F5' S2 N2 112.9(4) . . ? O4 S2 N2 135.8(7) . . ? O3 S2 N2 112.7(8) . . ? F6' S2 N2 126.7(8) . . ? C17' S2 C17 71.1(9) . . ? S2' S2 C17 31.9(4) . . ? F5' S2 C17 105.2(6) . . ? O4 S2 C17 112.9(9) . . ? O3 S2 C17 99.1(15) . . ? F6' S2 C17 103.2(12) . . ? N2 S2 C17 99.3(4) . . ? C17 S2' S2 104.9(7) . . ? C17 S2' O4' 53.3(11) . . ? S2 S2' O4' 133.1(12) . . ? C17 S2' O3' 82.9(9) . . ? S2 S2' O3' 105.5(11) . . ? O4' S2' O3' 110.8(13) . . ? C17 S2' F5 56.2(7) . . ? S2 S2' F5 129.0(5) . . ? O4' S2' F5 77.2(11) . . ? O3' S2' F5 34.1(8) . . ? C17 S2' F6 54.6(11) . . ? S2 S2' F6 120.4(9) . . ? O4' S2' F6 13.2(18) . . ? O3' S2' F6 122.5(11) . . ? F5 S2' F6 88.4(8) . . ? C17 S2' N2 168.5(7) . . ? S2 S2' N2 64.9(2) . . ? O4' S2' N2 129.0(10) . . ? O3' S2' N2 104.6(7) . . ? F5 S2' N2 134.0(5) . . ? F6 S2' N2 124.6(7) . . ? C17 S2' C17' 73.3(8) . . ? S2 S2' C17' 31.6(4) . . ? O4' S2' C17' 109.8(13) . . ? O3' S2' C17' 102.7(10) . . ? F5 S2' C17' 109.7(7) . . ? F6 S2' C17' 99.7(10) . . ? N2 S2' C17' 96.2(5) . . ? O6 S3 O5 116.84(17) . . ? O6 S3 N3 112.23(18) . . ? O5 S3 N3 114.17(16) . . ? O6 S3 C18 104.37(19) . . ? O5 S3 C18 103.29(17) . . ? N3 S3 C18 104.1(2) . . ? O8 S4 O7 117.38(18) . . ? O8 S4 N3 111.62(19) . . ? O7 S4 N3 113.38(17) . . ? O8 S4 C19 106.0(2) . . ? O7 S4 C19 104.2(2) . . ? N3 S4 C19 102.5(2) . . ? C12 N1 Si1 128.5(2) . . ? C12 N1 Ti1 125.2(2) . . ? Si1 N1 Ti1 106.21(15) . . ? S1 N2 S2 131.4(3) . . ? S1 N2 S2' 117.0(3) . . ? S2 N2 S2' 47.51(17) . . ? S3 N3 S4 126.1(2) . . ? S1 O1 Ti1 151.53(18) . . ? C17' O3 S2 40.2(9) . . ? F5 O3' S2' 75.1(16) . . ? F5 O3' C17 47.5(12) . . ? S2' O3' C17 36.5(5) . . ? F5' O4 C17' 100(2) . . ? F5' O4 S2 73.3(17) . . ? C17' O4 S2 41.7(8) . . ? C17 O4' S2' 47.3(11) . . ? C17 O4' F5 44.5(12) . . ? S2' O4' F5 55.5(10) . . ? S3 O5 Ti1 142.11(15) . . ? S4 O7 Ti1 142.58(16) . . ? C5 C1 C2 106.3(3) . . ? C5 C1 Si1 124.8(3) . . ? C2 C1 Si1 119.8(3) . . ? C5 C1 Ti1 75.5(2) . . ? C2 C1 Ti1 73.4(2) . . ? Si1 C1 Ti1 89.42(15) . . ? C3 C2 C1 109.0(3) . . ? C3 C2 C6 124.8(3) . . ? C1 C2 C6 126.1(4) . . ? C3 C2 Ti1 77.2(2) . . ? C1 C2 Ti1 70.1(2) . . ? C6 C2 Ti1 120.5(3) . . ? C2 C3 C4 107.8(3) . . ? C2 C3 C7 127.1(4) . . ? C4 C3 C7 124.8(4) . . ? C2 C3 Ti1 68.4(2) . . ? C4 C3 Ti1 73.3(2) . . ? C7 C3 Ti1 129.4(3) . . ? C5 C4 C3 107.5(4) . . ? C5 C4 C8 127.2(4) . . ? C3 C4 C8 125.1(4) . . ? C5 C4 Ti1 69.9(2) . . ? C3 C4 Ti1 72.6(2) . . ? C8 C4 Ti1 127.5(3) . . ? C4 C5 C1 109.4(3) . . ? C4 C5 C9 122.7(4) . . ? C1 C5 C9 127.8(4) . . ? C4 C5 Ti1 76.0(2) . . ? C1 C5 Ti1 68.8(2) . . ? C9 C5 Ti1 125.0(3) . . ? N1 C12 C15 110.4(3) . . ? N1 C12 C13 109.9(3) . . ? C15 C12 C13 109.7(3) . . ? N1 C12 C14 107.5(3) . . ? C15 C12 C14 110.4(3) . . ? C13 C12 C14 109.0(3) . . ? F3 C16 F1 109.7(5) . . ? F3 C16 F2 109.3(4) . . ? F1 C16 F2 108.4(4) . . ? F3 C16 S1 110.9(3) . . ? F1 C16 S1 109.1(3) . . ? F2 C16 S1 109.4(4) . . ? S2' C17 O4' 79.4(14) . . ? S2' C17 F5 82.5(10) . . ? O4' C17 F5 98.0(19) . . ? S2' C17 F4 151.6(13) . . ? O4' C17 F4 122.2(18) . . ? F5 C17 F4 109.6(12) . . ? S2' C17 F6 87.3(13) . . ? O4' C17 F6 18(2) . . ? F5 C17 F6 115.2(15) . . ? F4 C17 F6 108.8(13) . . ? S2' C17 O3' 60.6(8) . . ? O4' C17 O3' 112(2) . . ? F5 C17 O3' 30.7(8) . . ? F4 C17 O3' 117.8(11) . . ? F6 C17 O3' 129.3(15) . . ? S2' C17 C17' 73.9(9) . . ? O4' C17 C17' 125.2(14) . . ? F5 C17 C17' 124.0(12) . . ? F4 C17 C17' 78.2(9) . . ? F6 C17 C17' 113.5(13) . . ? O3' C17 C17' 95.2(12) . . ? S2' C17 S2 43.2(5) . . ? O4' C17 S2 109.0(11) . . ? F5 C17 S2 108.4(9) . . ? F4 C17 S2 108.6(9) . . ? F6 C17 S2 106.0(11) . . ? O3' C17 S2 77.8(9) . . ? C17' C17 S2 30.7(5) . . ? S2 C17' O4 81.7(12) . . ? S2 C17' F6' 91.0(15) . . ? O4 C17' F6' 98(2) . . ? S2 C17' O3 77.2(15) . . ? O4 C17' O3 110(2) . . ? F6' C17' O3 19.8(15) . . ? S2 C17' F4' 151.0(14) . . ? O4 C17' F4' 108.3(14) . . ? F6' C17' F4' 113.5(18) . . ? O3 C17' F4' 121.6(18) . . ? S2 C17' F5' 64.4(9) . . ? O4 C17' F5' 29.6(10) . . ? F6' C17' F5' 120.3(19) . . ? O3 C17' F5' 124(2) . . ? F4' C17' F5' 111.3(11) . . ? S2 C17' C17 78.2(9) . . ? O4 C17' C17 131.9(14) . . ? F6' C17' C17 125.1(16) . . ? O3 C17' C17 107.7(15) . . ? F4' C17' C17 75.0(9) . . ? F5' C17' C17 103.1(9) . . ? S2 C17' S2' 45.4(6) . . ? O4 C17' S2' 114.8(12) . . ? F6' C17' S2' 114.4(12) . . ? O3 C17' S2' 94.7(11) . . ? F4' C17' S2' 107.4(9) . . ? F5' C17' S2' 86.6(7) . . ? C17 C17' S2' 32.8(5) . . ? F8 C18 F9 109.1(4) . . ? F8 C18 F7 109.4(3) . . ? F9 C18 F7 109.0(4) . . ? F8 C18 S3 110.0(3) . . ? F9 C18 S3 111.0(3) . . ? F7 C18 S3 108.3(3) . . ? F12 C19 F10 109.6(4) . . ? F12 C19 F11 107.1(4) . . ? F10 C19 F11 107.8(4) . . ? F12 C19 S4 111.5(4) . . ? F10 C19 S4 110.3(4) . . ? F11 C19 S4 110.4(3) . . ? F4' F4 C17 102.3(9) . . ? F4 F4' C17' 104.1(9) . . ? O3' F5 C17 101.7(16) . . ? O3' F5 S2' 70.8(13) . . ? C17 F5 S2' 41.4(7) . . ? O3' F5 O4' 117.3(17) . . ? C17 F5 O4' 37.5(11) . . ? S2' F5 O4' 47.3(6) . . ? O4 F5' S2 75.3(17) . . ? O4 F5' C17' 50.7(18) . . ? S2 F5' C17' 37.7(6) . . ? C17 F6 S2' 38.1(8) . . ? C17' F6' S2 37.7(10) . . ? _refine_diff_density_max 0.463 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.074 data_ccd645 _database_code_depnum_ccdc_archive 'CCDC 255446' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 F12 N2 O8 Ru S4' _chemical_formula_weight 795.58 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.760(5) _cell_length_b 14.354(6) _cell_length_c 17.295(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.438(9) _cell_angle_gamma 90.00 _cell_volume 2642(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.7128 _exptl_absorpt_correction_T_max 0.8193 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 with SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ' >2' _diffrn_reflns_number 16298 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.35 _reflns_number_total 4681 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0723P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4681 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0879 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 1.559 _refine_ls_restrained_S_all 1.559 _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 Ru1 Ru -0.00326(5) 0.12295(3) 0.22854(3) 0.02531(19) Uani 1 1 d . . . S1 S 0.10014(16) 0.28969(11) 0.30185(9) 0.0305(4) Uani 1 1 d . . . S2 S -0.14019(18) 0.34761(12) 0.22402(11) 0.0390(4) Uani 1 1 d . . . S3 S 0.14675(18) 0.15905(12) 0.07132(10) 0.0342(4) Uani 1 1 d . . . S4 S 0.16798(17) 0.25351(12) -0.06648(10) 0.0350(4) Uani 1 1 d . . . O1 O 0.1571(4) 0.1983(3) 0.3006(3) 0.0342(11) Uani 1 1 d . . . O2 O 0.1685(5) 0.3693(3) 0.2845(3) 0.0454(13) Uani 1 1 d . . . O3 O -0.2592(5) 0.3038(4) 0.2140(3) 0.0499(14) Uani 1 1 d . . . O4 O -0.1149(6) 0.4300(4) 0.2683(4) 0.0569(15) Uani 1 1 d . . . O5 O 0.0890(5) 0.1863(3) 0.1392(3) 0.0374(11) Uani 1 1 d . . . O6 O 0.1004(6) 0.0769(4) 0.0319(3) 0.0564(16) Uani 1 1 d . . . O7 O 0.2025(5) 0.1682(4) -0.0998(3) 0.0490(13) Uani 1 1 d . . . O8 O 0.2306(5) 0.3372(4) -0.0810(3) 0.0495(14) Uani 1 1 d . . . N1 N -0.0344(5) 0.2688(4) 0.2515(3) 0.0290(12) Uani 1 1 d . . . N2 N 0.1590(6) 0.2497(4) 0.0243(3) 0.0359(13) Uani 1 1 d . . . F1 F 0.0353(7) 0.3867(4) 0.4186(3) 0.0813(18) Uani 1 1 d . . . F2 F 0.1815(5) 0.2882(5) 0.4497(3) 0.0837(19) Uani 1 1 d . . . F3 F -0.0084(5) 0.2427(4) 0.4224(3) 0.0672(15) Uani 1 1 d . . . F4 F 0.0025(5) 0.4040(4) 0.1232(3) 0.0666(14) Uani 1 1 d . . . F5 F -0.1354(5) 0.3027(4) 0.0775(3) 0.0644(14) Uani 1 1 d . . . F6 F -0.1915(5) 0.4442(4) 0.0975(3) 0.0756(17) Uani 1 1 d . . . F7 F 0.3773(6) 0.1139(5) 0.0608(4) 0.095(2) Uani 1 1 d . . . F8 F 0.3577(5) 0.2026(5) 0.1587(3) 0.0827(18) Uani 1 1 d . . . F9 F 0.3068(6) 0.0594(4) 0.1617(4) 0.097(2) Uani 1 1 d . . . F10 F -0.0400(5) 0.3493(5) -0.0820(4) 0.0821(17) Uani 1 1 d . . . F11 F -0.0677(5) 0.2017(5) -0.0939(4) 0.0869(19) Uani 1 1 d . . . F12 F -0.0030(7) 0.2790(6) -0.1858(3) 0.117(3) Uani 1 1 d . . . C1 C 0.0035(7) 0.0044(4) 0.3077(4) 0.0322(15) Uani 1 1 d . . . C2 C 0.0293(7) -0.0261(4) 0.2324(4) 0.0344(16) Uani 1 1 d . . . H2 H 0.1017 -0.0603 0.2291 0.041 Uiso 1 1 calc R . . C3 C -0.0517(7) -0.0056(5) 0.1653(4) 0.0379(17) Uani 1 1 d . . . H3 H -0.0327 -0.0268 0.1175 0.046 Uiso 1 1 calc R . . C4 C -0.1642(7) 0.0473(5) 0.1666(4) 0.0379(17) Uani 1 1 d . . . C5 C -0.1886(6) 0.0764(5) 0.2410(4) 0.0350(16) Uani 1 1 d . . . H5 H -0.2608 0.1110 0.2442 0.042 Uiso 1 1 calc R . . C6 C -0.1087(7) 0.0555(5) 0.3097(4) 0.0340(15) Uani 1 1 d . . . H6 H -0.1293 0.0753 0.3574 0.041 Uiso 1 1 calc R . . C7 C 0.0899(7) -0.0120(5) 0.3831(4) 0.0411(17) Uani 1 1 d . . . H7 H 0.0857 0.0435 0.4156 0.049 Uiso 1 1 calc R . . C8 C 0.0340(9) -0.0934(7) 0.4248(5) 0.060(2) Uani 1 1 d . . . H8A H -0.0522 -0.0803 0.4289 0.090 Uiso 1 1 calc R . . H8B H 0.0807 -0.1012 0.4761 0.090 Uiso 1 1 calc R . . H8C H 0.0388 -0.1496 0.3952 0.090 Uiso 1 1 calc R . . C9 C 0.2244(8) -0.0268(7) 0.3751(5) 0.059(2) Uani 1 1 d . . . H9A H 0.2722 -0.0365 0.4259 0.089 Uiso 1 1 calc R . . H9B H 0.2558 0.0270 0.3514 0.089 Uiso 1 1 calc R . . H9C H 0.2319 -0.0805 0.3430 0.089 Uiso 1 1 calc R . . C10 C -0.2477(8) 0.0727(6) 0.0932(5) 0.052(2) Uani 1 1 d . . . H10A H -0.2148 0.0468 0.0493 0.078 Uiso 1 1 calc R . . H10B H -0.2517 0.1393 0.0883 0.078 Uiso 1 1 calc R . . H10C H -0.3304 0.0485 0.0948 0.078 Uiso 1 1 calc R . . C11 C 0.0747(8) 0.3031(6) 0.4052(4) 0.0444(19) Uani 1 1 d . . . C12 C -0.1119(8) 0.3759(6) 0.1233(5) 0.052(2) Uani 1 1 d . . . C13 C 0.3085(9) 0.1316(6) 0.1172(6) 0.059(2) Uani 1 1 d . . . C14 C 0.0044(9) 0.2740(8) -0.1095(6) 0.063(2) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0228(3) 0.0268(3) 0.0277(3) -0.0005(2) 0.0083(2) -0.0011(2) S1 0.0271(9) 0.0321(9) 0.0334(9) -0.0046(6) 0.0079(7) -0.0048(7) S2 0.0320(10) 0.0366(9) 0.0511(11) 0.0005(8) 0.0146(8) 0.0078(7) S3 0.0392(10) 0.0324(9) 0.0346(9) -0.0017(7) 0.0175(8) -0.0046(7) S4 0.0307(10) 0.0432(10) 0.0330(9) 0.0031(7) 0.0105(7) -0.0066(8) O1 0.023(2) 0.038(3) 0.042(3) -0.002(2) 0.004(2) -0.001(2) O2 0.042(3) 0.037(3) 0.060(3) -0.007(2) 0.018(3) -0.008(2) O3 0.021(3) 0.065(4) 0.066(4) 0.006(3) 0.015(2) 0.004(2) O4 0.056(4) 0.040(3) 0.077(4) -0.005(3) 0.017(3) 0.013(3) O5 0.047(3) 0.033(2) 0.036(3) -0.002(2) 0.022(2) -0.007(2) O6 0.086(5) 0.040(3) 0.052(3) -0.014(2) 0.036(3) -0.028(3) O7 0.054(4) 0.055(3) 0.041(3) -0.005(2) 0.018(3) -0.007(3) O8 0.050(3) 0.052(3) 0.051(3) 0.011(2) 0.021(3) -0.008(3) N1 0.026(3) 0.026(3) 0.036(3) -0.004(2) 0.008(2) -0.004(2) N2 0.044(4) 0.035(3) 0.030(3) -0.003(2) 0.011(3) -0.005(3) F1 0.125(6) 0.060(3) 0.066(3) -0.018(3) 0.037(3) 0.010(3) F2 0.050(3) 0.157(6) 0.040(3) -0.027(3) -0.005(2) 0.004(3) F3 0.078(4) 0.085(4) 0.044(3) -0.008(2) 0.028(3) -0.028(3) F4 0.042(3) 0.079(4) 0.081(4) 0.027(3) 0.019(2) -0.003(3) F5 0.072(4) 0.077(4) 0.044(3) -0.002(2) 0.008(2) 0.004(3) F6 0.069(4) 0.076(4) 0.085(4) 0.041(3) 0.020(3) 0.031(3) F7 0.058(4) 0.133(6) 0.102(5) 0.018(4) 0.044(3) 0.036(4) F8 0.057(4) 0.113(5) 0.072(4) 0.013(3) -0.012(3) -0.013(3) F9 0.089(5) 0.086(4) 0.121(5) 0.061(4) 0.034(4) 0.032(4) F10 0.055(4) 0.096(5) 0.096(4) 0.018(3) 0.013(3) 0.029(3) F11 0.034(3) 0.110(5) 0.116(5) -0.009(4) 0.008(3) -0.017(3) F12 0.081(5) 0.222(9) 0.043(3) 0.018(4) -0.012(3) 0.010(5) C1 0.034(4) 0.023(3) 0.041(4) 0.003(3) 0.011(3) -0.002(3) C2 0.037(4) 0.023(3) 0.046(4) 0.000(3) 0.016(3) 0.004(3) C3 0.052(5) 0.030(4) 0.034(4) -0.006(3) 0.015(3) -0.012(3) C4 0.039(4) 0.038(4) 0.036(4) 0.005(3) 0.001(3) -0.016(3) C5 0.020(4) 0.033(4) 0.054(4) 0.002(3) 0.012(3) -0.006(3) C6 0.032(4) 0.039(4) 0.036(4) 0.004(3) 0.023(3) -0.004(3) C7 0.040(4) 0.048(4) 0.038(4) 0.002(3) 0.012(3) 0.009(3) C8 0.055(6) 0.073(6) 0.052(5) 0.030(4) 0.010(4) 0.015(5) C9 0.042(5) 0.079(6) 0.055(5) 0.009(4) 0.004(4) 0.009(5) C10 0.049(5) 0.055(5) 0.049(5) 0.003(4) -0.003(4) -0.012(4) C11 0.042(5) 0.056(5) 0.037(4) -0.011(3) 0.012(3) -0.011(4) C12 0.037(5) 0.056(5) 0.064(5) 0.025(4) 0.011(4) 0.008(4) C13 0.049(5) 0.059(5) 0.073(6) 0.028(5) 0.026(5) 0.019(5) C14 0.041(5) 0.086(7) 0.061(6) 0.003(5) 0.002(4) 0.005(5) _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 Ru1 C5 2.143(7) . ? Ru1 O5 2.156(5) . ? Ru1 C6 2.159(6) . ? Ru1 N1 2.166(5) . ? Ru1 C2 2.168(6) . ? Ru1 C3 2.170(7) . ? Ru1 C1 2.179(6) . ? Ru1 C4 2.186(7) . ? Ru1 O1 2.251(4) . ? Ru1 S1 2.8566(19) . ? S1 O2 1.415(5) . ? S1 O1 1.449(5) . ? S1 N1 1.604(6) . ? S1 C11 1.858(8) . ? S2 O3 1.414(6) . ? S2 O4 1.414(6) . ? S2 N1 1.625(6) . ? S2 C12 1.857(9) . ? S3 O6 1.416(5) . ? S3 O5 1.459(5) . ? S3 N2 1.550(6) . ? S3 C13 1.846(9) . ? S4 O8 1.417(5) . ? S4 O7 1.425(6) . ? S4 N2 1.589(6) . ? S4 C14 1.832(9) . ? F1 C11 1.306(9) . ? F2 C11 1.303(9) . ? F3 C11 1.310(9) . ? F4 C12 1.295(10) . ? F5 C12 1.318(10) . ? F6 C12 1.335(9) . ? F7 C13 1.332(11) . ? F8 C13 1.313(11) . ? F9 C13 1.293(9) . ? F10 C14 1.299(11) . ? F11 C14 1.347(11) . ? F12 C14 1.312(11) . ? C1 C6 1.418(10) . ? C1 C2 1.438(10) . ? C1 C7 1.505(10) . ? C2 C3 1.378(10) . ? C3 C4 1.431(11) . ? C4 C5 1.413(10) . ? C4 C10 1.489(10) . ? C5 C6 1.393(10) . ? C7 C9 1.489(11) . ? C7 C8 1.540(11) . ? 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 C5 Ru1 O5 137.4(2) . . ? C5 Ru1 C6 37.8(3) . . ? O5 Ru1 C6 174.8(2) . . ? C5 Ru1 N1 96.4(2) . . ? O5 Ru1 N1 79.88(19) . . ? C6 Ru1 N1 101.8(2) . . ? C5 Ru1 C2 80.7(3) . . ? O5 Ru1 C2 110.4(2) . . ? C6 Ru1 C2 68.6(3) . . ? N1 Ru1 C2 167.7(2) . . ? C5 Ru1 C3 68.1(3) . . ? O5 Ru1 C3 95.7(2) . . ? C6 Ru1 C3 80.6(3) . . ? N1 Ru1 C3 151.9(2) . . ? C2 Ru1 C3 37.0(3) . . ? C5 Ru1 C1 68.9(3) . . ? O5 Ru1 C1 143.4(2) . . ? C6 Ru1 C1 38.2(3) . . ? N1 Ru1 C1 129.2(2) . . ? C2 Ru1 C1 38.6(3) . . ? C3 Ru1 C1 68.7(3) . . ? C5 Ru1 C4 38.1(3) . . ? O5 Ru1 C4 105.8(2) . . ? C6 Ru1 C4 69.0(3) . . ? N1 Ru1 C4 115.9(3) . . ? C2 Ru1 C4 68.7(3) . . ? C3 Ru1 C4 38.4(3) . . ? C1 Ru1 C4 82.6(3) . . ? C5 Ru1 O1 138.0(2) . . ? O5 Ru1 O1 78.40(18) . . ? C6 Ru1 O1 106.8(2) . . ? N1 Ru1 O1 63.94(19) . . ? C2 Ru1 O1 110.5(2) . . ? C3 Ru1 O1 142.7(2) . . ? C1 Ru1 O1 94.3(2) . . ? C4 Ru1 O1 175.8(2) . . ? C5 Ru1 S1 121.60(19) . . ? O5 Ru1 S1 76.99(13) . . ? C6 Ru1 S1 107.15(19) . . ? N1 Ru1 S1 33.85(15) . . ? C2 Ru1 S1 139.70(19) . . ? C3 Ru1 S1 170.3(2) . . ? C1 Ru1 S1 113.62(18) . . ? C4 Ru1 S1 149.6(2) . . ? O1 Ru1 S1 30.10(12) . . ? O2 S1 O1 119.6(3) . . ? O2 S1 N1 119.5(3) . . ? O1 S1 N1 99.9(3) . . ? O2 S1 C11 106.0(3) . . ? O1 S1 C11 103.3(3) . . ? N1 S1 C11 107.0(3) . . ? O2 S1 Ru1 139.8(2) . . ? O1 S1 Ru1 51.17(18) . . ? N1 S1 Ru1 48.77(19) . . ? C11 S1 Ru1 114.3(3) . . ? O3 S2 O4 122.5(4) . . ? O3 S2 N1 108.0(3) . . ? O4 S2 N1 110.7(3) . . ? O3 S2 C12 104.6(4) . . ? O4 S2 C12 106.3(4) . . ? N1 S2 C12 102.9(3) . . ? O6 S3 O5 116.6(3) . . ? O6 S3 N2 119.9(3) . . ? O5 S3 N2 106.0(3) . . ? O6 S3 C13 105.8(4) . . ? O5 S3 C13 101.4(4) . . ? N2 S3 C13 104.9(4) . . ? O8 S4 O7 119.8(3) . . ? O8 S4 N2 107.7(3) . . ? O7 S4 N2 115.3(3) . . ? O8 S4 C14 104.2(4) . . ? O7 S4 C14 105.4(4) . . ? N2 S4 C14 102.3(4) . . ? S1 O1 Ru1 98.7(2) . . ? S3 O5 Ru1 139.3(3) . . ? S1 N1 S2 124.5(3) . . ? S1 N1 Ru1 97.4(3) . . ? S2 N1 Ru1 137.7(3) . . ? S3 N2 S4 124.7(4) . . ? C6 C1 C2 117.2(6) . . ? C6 C1 C7 118.7(6) . . ? C2 C1 C7 124.1(6) . . ? C6 C1 Ru1 70.1(4) . . ? C2 C1 Ru1 70.3(4) . . ? C7 C1 Ru1 128.8(5) . . ? C3 C2 C1 121.1(7) . . ? C3 C2 Ru1 71.6(4) . . ? C1 C2 Ru1 71.1(3) . . ? C2 C3 C4 122.1(6) . . ? C2 C3 Ru1 71.4(4) . . ? C4 C3 Ru1 71.5(4) . . ? C5 C4 C3 116.3(6) . . ? C5 C4 C10 122.2(7) . . ? C3 C4 C10 121.5(7) . . ? C5 C4 Ru1 69.3(4) . . ? C3 C4 Ru1 70.2(4) . . ? C10 C4 Ru1 129.1(5) . . ? C6 C5 C4 122.6(7) . . ? C6 C5 Ru1 71.7(4) . . ? C4 C5 Ru1 72.6(4) . . ? C5 C6 C1 120.8(6) . . ? C5 C6 Ru1 70.5(4) . . ? C1 C6 Ru1 71.7(4) . . ? C9 C7 C1 115.3(6) . . ? C9 C7 C8 112.7(7) . . ? C1 C7 C8 106.9(6) . . ? F2 C11 F1 109.1(7) . . ? F2 C11 F3 109.3(7) . . ? F1 C11 F3 108.5(7) . . ? F2 C11 S1 108.0(5) . . ? F1 C11 S1 111.3(6) . . ? F3 C11 S1 110.6(5) . . ? F4 C12 F5 110.3(8) . . ? F4 C12 F6 109.5(7) . . ? F5 C12 F6 109.1(7) . . ? F4 C12 S2 110.9(6) . . ? F5 C12 S2 110.3(5) . . ? F6 C12 S2 106.8(6) . . ? F9 C13 F8 109.6(9) . . ? F9 C13 F7 109.9(8) . . ? F8 C13 F7 109.1(8) . . ? F9 C13 S3 109.4(7) . . ? F8 C13 S3 110.4(6) . . ? F7 C13 S3 108.5(7) . . ? F10 C14 F12 110.5(9) . . ? F10 C14 F11 108.4(8) . . ? F12 C14 F11 107.0(8) . . ? F10 C14 S4 111.6(7) . . ? F12 C14 S4 109.3(7) . . ? F11 C14 S4 110.0(7) . . ? _refine_diff_density_max 1.874 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.145 data_ccd570 _database_code_depnum_ccdc_archive 'CCDC 255447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 F6 Fe N O6 S2' _chemical_formula_weight 457.11 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' F F 0.0171 0.0103 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 32 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 9.1524(14) _cell_length_b 9.1524(14) _cell_length_c 31.283(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2269.4(7) _cell_formula_units_Z 6 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'multifaceted block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 1.371 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.5775 _exptl_absorpt_correction_T_max 0.7257 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 with SMART 1k CCD' _diffrn_measurement_method ' \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 12400 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 23.24 _reflns_number_total 2177 _reflns_number_gt 2135 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0565P)^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 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 0.05(3) _refine_ls_number_reflns 2177 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.689 _refine_ls_restrained_S_all 1.689 _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 Fe1 Fe 0.09716(8) 0.74095(8) 0.08875(2) 0.0357(2) Uani 1 1 d . . . S1 S 0.02386(16) 0.36955(15) 0.11948(4) 0.0415(3) Uani 1 1 d . . . S2 S 0.19426(15) 0.48531(16) 0.04187(4) 0.0414(3) Uani 1 1 d . . . N1 N 0.0997(5) 0.5154(5) 0.08277(11) 0.0347(8) Uani 1 1 d . . . O1 O 0.4427(6) 0.9656(6) 0.06015(18) 0.0896(17) Uani 1 1 d . . . O2 O 0.1979(6) 0.8097(6) 0.17865(12) 0.0700(11) Uani 1 1 d . . . O3 O 0.0001(5) 0.4412(4) 0.15737(11) 0.0632(11) Uani 1 1 d . . . O4 O 0.1085(5) 0.2751(5) 0.12187(12) 0.0560(10) Uani 1 1 d . . . O5 O 0.1187(5) 0.3142(5) 0.02930(12) 0.0625(10) Uani 1 1 d . . . O6 O 0.2297(5) 0.6152(5) 0.01164(9) 0.0509(9) Uani 1 1 d . . . C1 C -0.0635(8) 0.8353(8) 0.1018(2) 0.0600(15) Uani 1 1 d . . . H1 H -0.0648 0.8877 0.1272 0.072 Uiso 1 1 calc R . . C2 C 0.0358(8) 0.9160(8) 0.0659(2) 0.0680(17) Uani 1 1 d . . . H2 H 0.1130 1.0307 0.0634 0.082 Uiso 1 1 calc R . . C3 C -0.0025(7) 0.7923(8) 0.03443(18) 0.0622(16) Uani 1 1 d . . . H3 H 0.0444 0.8106 0.0072 0.075 Uiso 1 1 calc R . . C4 C -0.1224(6) 0.6382(7) 0.05115(16) 0.0498(12) Uani 1 1 d . . . H4 H -0.1701 0.5353 0.0369 0.060 Uiso 1 1 calc R . . C5 C -0.1603(7) 0.6631(7) 0.09317(18) 0.0493(12) Uani 1 1 d . . . H5 H -0.2357 0.5802 0.1117 0.059 Uiso 1 1 calc R . . C6 C 0.3109(7) 0.8737(7) 0.07146(18) 0.0557(14) Uani 1 1 d . . . C7 C 0.1582(7) 0.7743(6) 0.14418(17) 0.0484(12) Uani 1 1 d . . . C8 C -0.1947(7) 0.2151(6) 0.10231(19) 0.0509(13) Uani 1 1 d . . . C9 C 0.4095(8) 0.5418(9) 0.06289(19) 0.0640(17) Uani 1 1 d . . . F1 F -0.1962(5) 0.1385(7) 0.06753(16) 0.117(2) Uani 1 1 d . . . F2 F -0.2842(5) 0.2820(5) 0.0963(2) 0.122(2) Uani 1 1 d . . . F3 F -0.2637(7) 0.1020(6) 0.13108(16) 0.127(2) Uani 1 1 d . . . F4 F 0.5217(5) 0.6356(9) 0.03470(14) 0.123(2) Uani 1 1 d . . . F5 F 0.4421(5) 0.6311(7) 0.09779(13) 0.0976(15) Uani 1 1 d . . . F6 F 0.4200(6) 0.4095(7) 0.07115(18) 0.1109(17) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0362(4) 0.0326(4) 0.0357(4) 0.0009(3) -0.0025(3) 0.0153(3) S1 0.0505(7) 0.0382(6) 0.0344(6) 0.0052(5) 0.0010(5) 0.0212(6) S2 0.0441(7) 0.0593(8) 0.0295(6) -0.0001(5) 0.0006(5) 0.0324(6) N1 0.036(2) 0.036(2) 0.0308(19) 0.0001(15) 0.0042(16) 0.0163(16) O1 0.041(2) 0.070(3) 0.115(4) 0.033(3) 0.006(2) -0.004(2) O2 0.083(3) 0.065(3) 0.047(2) -0.0180(19) -0.021(2) 0.026(2) O3 0.097(3) 0.051(2) 0.0310(17) 0.0038(16) 0.0104(19) 0.029(2) O4 0.060(2) 0.057(2) 0.059(2) 0.0084(18) -0.0094(18) 0.0345(19) O5 0.082(3) 0.067(2) 0.054(2) -0.0152(19) 0.000(2) 0.049(2) O6 0.056(2) 0.082(3) 0.0245(15) 0.0127(16) 0.0070(15) 0.0424(19) C1 0.071(4) 0.064(4) 0.066(4) -0.007(3) 0.001(3) 0.049(3) C2 0.073(4) 0.049(3) 0.097(5) 0.010(3) -0.009(4) 0.042(3) C3 0.063(4) 0.092(5) 0.052(3) 0.033(3) 0.012(3) 0.055(4) C4 0.051(3) 0.062(3) 0.051(3) -0.013(3) -0.017(2) 0.039(3) C5 0.046(3) 0.059(3) 0.050(3) 0.009(2) 0.002(2) 0.032(3) C6 0.049(3) 0.044(3) 0.061(3) 0.009(3) -0.009(3) 0.014(3) C7 0.049(3) 0.035(3) 0.053(3) -0.007(2) -0.012(2) 0.015(2) C8 0.043(3) 0.035(3) 0.068(3) 0.007(3) 0.008(2) 0.013(2) C9 0.057(3) 0.103(5) 0.053(3) 0.031(3) 0.014(3) 0.055(4) F1 0.057(2) 0.146(4) 0.107(3) -0.068(3) -0.010(2) 0.021(3) F2 0.048(2) 0.052(2) 0.258(6) 0.012(3) -0.009(3) 0.0189(19) F3 0.108(4) 0.079(3) 0.106(3) 0.051(3) -0.008(3) -0.019(3) F4 0.061(2) 0.226(6) 0.098(3) 0.081(4) 0.036(2) 0.083(3) F5 0.064(2) 0.152(4) 0.075(3) -0.008(3) -0.026(2) 0.053(3) F6 0.084(3) 0.131(4) 0.155(4) 0.031(3) -0.003(3) 0.082(3) _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 Fe1 C6 1.794(6) . ? Fe1 C7 1.801(5) . ? Fe1 C2 2.072(6) . ? Fe1 N1 2.084(4) . ? Fe1 C1 2.085(5) . ? Fe1 C3 2.090(5) . ? Fe1 C5 2.097(5) . ? Fe1 C4 2.101(5) . ? S1 O4 1.422(4) . ? S1 O3 1.423(4) . ? S1 N1 1.630(4) . ? S1 C8 1.861(5) . ? S2 O5 1.415(4) . ? S2 O6 1.424(4) . ? S2 N1 1.643(4) . ? S2 C9 1.887(6) . ? O1 C6 1.129(7) . ? O2 C7 1.132(6) . ? C1 C5 1.395(8) . ? C1 C2 1.401(9) . ? C2 C3 1.407(9) . ? C3 C4 1.385(8) . ? C4 C5 1.407(8) . ? C8 F2 1.258(7) . ? C8 F3 1.275(6) . ? C8 F1 1.291(7) . ? C9 F6 1.287(8) . ? C9 F4 1.299(7) . ? C9 F5 1.306(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Fe1 C7 92.0(3) . . ? C6 Fe1 C2 89.9(3) . . ? C7 Fe1 C2 112.4(3) . . ? C6 Fe1 N1 95.5(2) . . ? C7 Fe1 N1 95.64(19) . . ? C2 Fe1 N1 151.2(2) . . ? C6 Fe1 C1 122.3(3) . . ? C7 Fe1 C1 87.9(2) . . ? C2 Fe1 C1 39.4(2) . . ? N1 Fe1 C1 141.9(2) . . ? C6 Fe1 C3 93.1(2) . . ? C7 Fe1 C3 151.4(2) . . ? C2 Fe1 C3 39.5(2) . . ? N1 Fe1 C3 111.8(2) . . ? C1 Fe1 C3 65.8(2) . . ? C6 Fe1 C5 155.4(2) . . ? C7 Fe1 C5 101.2(2) . . ? C2 Fe1 C5 66.0(2) . . ? N1 Fe1 C5 103.68(19) . . ? C1 Fe1 C5 39.0(2) . . ? C3 Fe1 C5 65.7(2) . . ? C6 Fe1 C4 127.5(2) . . ? C7 Fe1 C4 139.6(2) . . ? C2 Fe1 C4 65.5(2) . . ? N1 Fe1 C4 89.33(18) . . ? C1 Fe1 C4 65.2(2) . . ? C3 Fe1 C4 38.6(2) . . ? C5 Fe1 C4 39.1(2) . . ? O4 S1 O3 119.4(2) . . ? O4 S1 N1 113.4(2) . . ? O3 S1 N1 108.1(2) . . ? O4 S1 C8 105.0(2) . . ? O3 S1 C8 103.7(3) . . ? N1 S1 C8 106.0(2) . . ? O5 S2 O6 121.4(2) . . ? O5 S2 N1 113.3(2) . . ? O6 S2 N1 107.2(2) . . ? O5 S2 C9 105.4(3) . . ? O6 S2 C9 103.4(2) . . ? N1 S2 C9 104.4(2) . . ? S1 N1 S2 117.1(2) . . ? S1 N1 Fe1 122.5(2) . . ? S2 N1 Fe1 120.2(2) . . ? C5 C1 C2 108.5(5) . . ? C5 C1 Fe1 71.0(3) . . ? C2 C1 Fe1 69.8(3) . . ? C1 C2 C3 107.6(5) . . ? C1 C2 Fe1 70.8(3) . . ? C3 C2 Fe1 70.9(3) . . ? C4 C3 C2 107.9(5) . . ? C4 C3 Fe1 71.2(3) . . ? C2 C3 Fe1 69.6(3) . . ? C3 C4 C5 108.8(5) . . ? C3 C4 Fe1 70.3(3) . . ? C5 C4 Fe1 70.3(3) . . ? C1 C5 C4 107.2(5) . . ? C1 C5 Fe1 70.0(3) . . ? C4 C5 Fe1 70.6(3) . . ? O1 C6 Fe1 175.3(6) . . ? O2 C7 Fe1 173.6(5) . . ? F2 C8 F3 108.8(6) . . ? F2 C8 F1 107.8(6) . . ? F3 C8 F1 106.7(5) . . ? F2 C8 S1 112.8(4) . . ? F3 C8 S1 108.7(4) . . ? F1 C8 S1 111.8(4) . . ? F6 C9 F4 110.6(6) . . ? F6 C9 F5 108.7(5) . . ? F4 C9 F5 107.2(7) . . ? F6 C9 S2 111.7(5) . . ? F4 C9 S2 108.4(4) . . ? F5 C9 S2 110.1(4) . . ? _refine_diff_density_max 0.477 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.074 data_ccd588 _database_code_depnum_ccdc_archive 'CCDC 255448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 F12 N2 O8 S4 Ti' _chemical_formula_weight 738.38 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.862(3) _cell_length_b 10.505(3) _cell_length_c 12.736(4) _cell_angle_alpha 94.226(5) _cell_angle_beta 109.178(4) _cell_angle_gamma 92.533(5) _cell_volume 1239.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square slab' _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 0.9374 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4 with SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 6429 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 23.22 _reflns_number_total 3305 _reflns_number_gt 2877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (v. 4.202, Siemens 1996)' _computing_cell_refinement 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_data_reduction 'Bruker SAINT (v. 5.00, Bruker 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHEXTL (v. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. One of the NTf ligands was disordered at a low level. The atom S2 was refined in two positions, S2 and S2', with variable site occupancies tied to 1.0. The final refinement yielded a s.o.f. of 0.807(5) for S2 and 0.192(5) for S2'. ; _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^)+(0.0847P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3305 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 1.407 _refine_ls_restrained_S_all 1.407 _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 0.30118(7) 0.18026(7) 0.23337(6) 0.0293(3) Uani 1 1 d . . . S1 S 0.31023(12) 0.50502(11) 0.22402(10) 0.0432(3) Uani 1 1 d . . . S2 S 0.1068(2) 0.65587(17) 0.27048(14) 0.0582(7) Uani 0.807(5) 1 d P . . S2' S 0.2063(7) 0.6409(7) 0.3653(6) 0.052(3) Uani 0.193(5) 1 d P . . S3 S 0.60317(11) 0.15519(11) 0.15825(9) 0.0361(3) Uani 1 1 d . . . S4 S 0.76406(11) -0.01689(12) 0.30125(10) 0.0431(3) Uani 1 1 d . . . O1 O 0.3167(3) 0.3673(3) 0.1998(3) 0.0471(8) Uani 1 1 d . . . O2 O 0.4349(4) 0.5700(4) 0.3034(3) 0.0689(11) Uani 1 1 d . . . O3 O 0.2206(5) 0.7586(4) 0.3134(4) 0.0915(15) Uani 1 1 d . . . O4 O -0.0334(6) 0.6726(7) 0.2048(5) 0.156(3) Uani 1 1 d . . . O5 O 0.5044(3) 0.1621(3) 0.2226(2) 0.0391(7) Uani 1 1 d . . . O6 O 0.5430(3) 0.1634(3) 0.0417(3) 0.0476(8) Uani 1 1 d . . . O7 O 0.7265(4) 0.0438(3) 0.3908(3) 0.0552(9) Uani 1 1 d . . . O8 O 0.9083(3) -0.0461(4) 0.3181(3) 0.0630(10) Uani 1 1 d . . . N1 N 0.1624(5) 0.5231(4) 0.2341(4) 0.0622(12) Uani 1 1 d . . . N2 N 0.7060(4) 0.0466(4) 0.1853(3) 0.0440(9) Uani 1 1 d . . . F1 F 0.1969(6) 0.4950(4) 0.0081(3) 0.1198(17) Uani 1 1 d . . . F2 F 0.2682(4) 0.6827(3) 0.0870(3) 0.0758(10) Uani 1 1 d . . . F3 F 0.4189(5) 0.5513(4) 0.0692(4) 0.1164(17) Uani 1 1 d . . . F4 F 0.0304(4) 0.7090(4) 0.4449(3) 0.0849(11) Uani 1 1 d . . . F5 F -0.0164(5) 0.5137(4) 0.3773(4) 0.1187(18) Uani 1 1 d . . . F6 F 0.2104(6) 0.5805(4) 0.4688(3) 0.1233(18) Uani 1 1 d . . . F7 F 0.8182(3) 0.3122(3) 0.1657(3) 0.0674(9) Uani 1 1 d . . . F8 F 0.6448(4) 0.4036(3) 0.1932(4) 0.0921(13) Uani 1 1 d . . . F9 F 0.7844(4) 0.3034(4) 0.3214(3) 0.0950(13) Uani 1 1 d . . . F10 F 0.5193(3) -0.1518(3) 0.2420(3) 0.0712(9) Uani 1 1 d . . . F11 F 0.6989(3) -0.2402(3) 0.3519(3) 0.0702(9) Uani 1 1 d . . . F12 F 0.6737(3) -0.2365(3) 0.1788(3) 0.0658(8) Uani 1 1 d . . . C1 C 0.0655(5) 0.0948(5) 0.1398(4) 0.0481(12) Uani 1 1 d . . . H1 H -0.0015 0.0972 0.1768 0.058 Uiso 1 1 calc R . . C2 C 0.1594(5) -0.0031(5) 0.1390(4) 0.0489(12) Uani 1 1 d . . . H2 H 0.1648 -0.0770 0.1756 0.059 Uiso 1 1 calc R . . C3 C 0.2424(5) 0.0302(5) 0.0738(4) 0.0504(13) Uani 1 1 d . . . H3 H 0.3118 -0.0181 0.0587 0.060 Uiso 1 1 calc R . . C4 C 0.2033(5) 0.1482(5) 0.0355(4) 0.0490(13) Uani 1 1 d . . . H4 H 0.2436 0.1935 -0.0084 0.059 Uiso 1 1 calc R . . C5 C 0.0928(5) 0.1872(5) 0.0743(4) 0.0515(13) Uani 1 1 d . . . H5 H 0.0456 0.2619 0.0590 0.062 Uiso 1 1 calc R . . C6 C 0.3613(6) 0.2840(5) 0.4173(4) 0.0579(15) Uani 1 1 d . . . H6 H 0.3866 0.3714 0.4323 0.069 Uiso 1 1 calc R . . C7 C 0.4534(5) 0.1881(6) 0.4222(4) 0.0518(14) Uani 1 1 d . . . H7 H 0.5528 0.1998 0.4414 0.062 Uiso 1 1 calc R . . C8 C 0.3740(6) 0.0720(5) 0.3942(4) 0.0534(13) Uani 1 1 d . . . H8 H 0.4104 -0.0075 0.3889 0.064 Uiso 1 1 calc R . . C9 C 0.2326(6) 0.0936(6) 0.3753(4) 0.0588(15) Uani 1 1 d . . . H9 H 0.1569 0.0311 0.3586 0.071 Uiso 1 1 calc R . . C10 C 0.2216(5) 0.2243(6) 0.3853(4) 0.0599(16) Uani 1 1 d . . . H10 H 0.1369 0.2655 0.3730 0.072 Uiso 1 1 calc R . . C11 C 0.2961(7) 0.5600(5) 0.0864(5) 0.0600(14) Uani 1 1 d . . . C12 C 0.0710(8) 0.6123(6) 0.3930(6) 0.083(2) Uani 1 1 d . . . C13 C 0.7200(5) 0.3039(5) 0.2143(4) 0.0498(13) Uani 1 1 d . . . C14 C 0.6580(5) -0.1717(5) 0.2654(4) 0.0489(12) Uani 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0301(4) 0.0274(5) 0.0290(4) 0.0002(3) 0.0089(3) -0.0003(3) S1 0.0555(7) 0.0308(7) 0.0438(7) 0.0027(5) 0.0179(6) -0.0016(5) S2 0.0800(14) 0.0485(12) 0.0508(12) 0.0073(8) 0.0252(10) 0.0221(9) S2' 0.059(4) 0.043(5) 0.055(5) -0.008(3) 0.024(4) 0.002(3) S3 0.0346(6) 0.0399(7) 0.0336(6) 0.0030(5) 0.0114(5) 0.0005(5) S4 0.0356(6) 0.0480(8) 0.0446(7) 0.0089(6) 0.0110(5) 0.0026(5) O1 0.070(2) 0.0257(19) 0.0492(19) 0.0008(15) 0.0245(16) 0.0053(15) O2 0.071(2) 0.049(2) 0.069(3) 0.0070(19) 0.0023(19) -0.0131(18) O3 0.127(4) 0.031(2) 0.143(4) 0.002(2) 0.083(3) -0.004(2) O4 0.131(5) 0.144(6) 0.137(5) -0.038(4) -0.031(4) 0.090(5) O5 0.0315(14) 0.046(2) 0.0400(17) 0.0070(14) 0.0113(13) 0.0033(13) O6 0.0481(17) 0.058(2) 0.0377(18) 0.0097(15) 0.0149(14) 0.0054(15) O7 0.062(2) 0.058(2) 0.041(2) 0.0041(16) 0.0114(16) 0.0073(17) O8 0.0390(17) 0.066(3) 0.085(3) 0.023(2) 0.0180(17) 0.0096(17) N1 0.076(3) 0.038(3) 0.085(3) 0.002(2) 0.044(3) 0.004(2) N2 0.045(2) 0.044(3) 0.047(2) 0.0021(18) 0.0207(18) 0.0048(17) F1 0.201(5) 0.078(3) 0.048(2) 0.0104(19) 0.003(3) -0.041(3) F2 0.111(3) 0.047(2) 0.075(2) 0.0258(17) 0.035(2) 0.0127(18) F3 0.163(4) 0.111(3) 0.133(4) 0.060(3) 0.112(3) 0.055(3) F4 0.114(3) 0.079(3) 0.070(2) -0.0082(19) 0.042(2) 0.022(2) F5 0.141(4) 0.098(4) 0.139(4) -0.039(3) 0.097(3) -0.064(3) F6 0.207(5) 0.103(3) 0.059(2) 0.018(2) 0.032(3) 0.073(3) F7 0.0577(17) 0.065(2) 0.086(2) 0.0019(17) 0.0359(17) -0.0159(15) F8 0.077(2) 0.042(2) 0.164(4) -0.001(2) 0.052(2) 0.0008(17) F9 0.123(3) 0.091(3) 0.049(2) -0.0081(18) 0.0090(19) -0.059(2) F10 0.0443(16) 0.066(2) 0.100(3) 0.0003(18) 0.0221(16) -0.0097(14) F11 0.087(2) 0.060(2) 0.059(2) 0.0244(16) 0.0175(16) -0.0080(16) F12 0.086(2) 0.050(2) 0.061(2) -0.0014(16) 0.0250(17) -0.0012(16) C1 0.034(2) 0.064(4) 0.040(3) -0.007(2) 0.008(2) -0.005(2) C2 0.052(3) 0.042(3) 0.039(3) -0.004(2) 0.001(2) -0.016(2) C3 0.049(3) 0.051(4) 0.042(3) -0.025(2) 0.009(2) -0.005(2) C4 0.046(3) 0.065(4) 0.030(2) -0.001(2) 0.007(2) -0.013(2) C5 0.042(3) 0.056(3) 0.042(3) 0.006(2) -0.005(2) 0.001(2) C6 0.099(4) 0.040(3) 0.028(3) -0.010(2) 0.019(3) -0.010(3) C7 0.043(3) 0.077(4) 0.028(3) 0.002(2) 0.003(2) -0.008(3) C8 0.076(4) 0.051(4) 0.032(3) 0.012(2) 0.013(2) 0.013(3) C9 0.062(3) 0.077(5) 0.035(3) 0.009(3) 0.015(2) -0.023(3) C10 0.055(3) 0.097(5) 0.035(3) 0.012(3) 0.020(2) 0.031(3) C11 0.084(4) 0.046(4) 0.054(3) 0.008(3) 0.028(3) 0.001(3) C12 0.125(6) 0.053(4) 0.088(5) -0.018(4) 0.068(5) -0.007(4) C13 0.052(3) 0.044(3) 0.055(3) 0.006(2) 0.021(3) -0.005(2) C14 0.048(3) 0.053(3) 0.050(3) 0.007(3) 0.021(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 2.051(3) . ? Ti1 O5 2.069(3) . ? Ti1 C2 2.329(5) . ? Ti1 C8 2.335(5) . ? Ti1 C1 2.338(4) . ? Ti1 C10 2.339(5) . ? Ti1 C9 2.355(5) . ? Ti1 C3 2.372(4) . ? Ti1 C7 2.373(4) . ? Ti1 C5 2.374(4) . ? Ti1 C4 2.376(4) . ? Ti1 C6 2.384(5) . ? S1 O2 1.417(4) . ? S1 O1 1.465(3) . ? S1 N1 1.524(4) . ? S1 C11 1.850(5) . ? S2 S2' 1.308(7) . ? S2 O4 1.387(5) . ? S2 O3 1.458(5) . ? S2 N1 1.612(5) . ? S2 C12 1.794(7) . ? S2' O3 1.467(8) . ? S2' F6 1.494(8) . ? S2' C12 1.511(9) . ? S2' N1 1.919(8) . ? S3 O6 1.417(3) . ? S3 O5 1.466(3) . ? S3 N2 1.543(4) . ? S3 C13 1.847(5) . ? S4 O8 1.419(3) . ? S4 O7 1.427(4) . ? S4 N2 1.605(4) . ? S4 C14 1.837(5) . ? F1 C11 1.271(7) . ? F2 C11 1.330(6) . ? F3 C11 1.305(7) . ? F4 C12 1.319(7) . ? F5 C12 1.278(7) . ? F6 C12 1.466(9) . ? F7 C13 1.313(5) . ? F8 C13 1.303(6) . ? F9 C13 1.302(6) . ? F10 C14 1.331(5) . ? F11 C14 1.321(6) . ? F12 C14 1.309(6) . ? C1 C5 1.398(7) . ? C1 C2 1.415(7) . ? C2 C3 1.395(7) . ? C3 C4 1.389(7) . ? C4 C5 1.402(7) . ? C6 C7 1.377(7) . ? C6 C10 1.405(8) . ? C7 C8 1.376(8) . ? C8 C9 1.368(7) . ? C9 C10 1.382(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O5 88.37(12) . . ? O1 Ti1 C2 134.88(16) . . ? O5 Ti1 C2 107.14(16) . . ? O1 Ti1 C8 135.06(17) . . ? O5 Ti1 C8 87.82(16) . . ? C2 Ti1 C8 88.65(19) . . ? O1 Ti1 C1 108.52(16) . . ? O5 Ti1 C1 138.26(15) . . ? C2 Ti1 C1 35.31(18) . . ? C8 Ti1 C1 103.76(19) . . ? O1 Ti1 C10 95.34(19) . . ? O5 Ti1 C10 132.19(15) . . ? C2 Ti1 C10 103.4(2) . . ? C8 Ti1 C10 56.92(19) . . ? C1 Ti1 C10 85.21(19) . . ? O1 Ti1 C9 129.58(18) . . ? O5 Ti1 C9 121.68(16) . . ? C2 Ti1 C9 77.88(19) . . ? C8 Ti1 C9 33.91(18) . . ? C1 Ti1 C9 76.67(17) . . ? C10 Ti1 C9 34.3(2) . . ? O1 Ti1 C3 114.14(17) . . ? O5 Ti1 C3 80.38(14) . . ? C2 Ti1 C3 34.52(17) . . ? C8 Ti1 C3 109.3(2) . . ? C1 Ti1 C3 57.89(16) . . ? C10 Ti1 C3 137.8(2) . . ? C9 Ti1 C3 110.4(2) . . ? O1 Ti1 C7 102.15(17) . . ? O5 Ti1 C7 76.02(14) . . ? C2 Ti1 C7 122.50(19) . . ? C8 Ti1 C7 33.99(19) . . ? C1 Ti1 C7 132.81(16) . . ? C10 Ti1 C7 56.56(17) . . ? C9 Ti1 C7 56.14(17) . . ? C3 Ti1 C7 135.7(2) . . ? O1 Ti1 C5 78.34(16) . . ? O5 Ti1 C5 122.86(15) . . ? C2 Ti1 C5 57.45(19) . . ? C8 Ti1 C5 138.26(19) . . ? C1 Ti1 C5 34.51(18) . . ? C10 Ti1 C5 104.47(18) . . ? C9 Ti1 C5 108.73(18) . . ? C3 Ti1 C5 56.95(18) . . ? C7 Ti1 C5 161.03(18) . . ? O1 Ti1 C4 81.74(17) . . ? O5 Ti1 C4 89.13(14) . . ? C2 Ti1 C4 57.18(18) . . ? C8 Ti1 C4 142.9(2) . . ? C1 Ti1 C4 57.58(16) . . ? C10 Ti1 C4 138.61(17) . . ? C9 Ti1 C4 132.17(17) . . ? C3 Ti1 C4 34.03(18) . . ? C7 Ti1 C4 164.44(18) . . ? C5 Ti1 C4 34.33(17) . . ? O1 Ti1 C6 80.21(16) . . ? O5 Ti1 C6 100.56(17) . . ? C2 Ti1 C6 134.44(18) . . ? C8 Ti1 C6 56.66(19) . . ? C1 Ti1 C6 119.46(19) . . ? C10 Ti1 C6 34.59(19) . . ? C9 Ti1 C6 56.75(19) . . ? C3 Ti1 C6 165.65(19) . . ? C7 Ti1 C6 33.66(18) . . ? C5 Ti1 C6 130.3(2) . . ? C4 Ti1 C6 159.2(2) . . ? O2 S1 O1 116.2(2) . . ? O2 S1 N1 120.3(3) . . ? O1 S1 N1 106.5(2) . . ? O2 S1 C11 107.2(3) . . ? O1 S1 C11 99.8(2) . . ? N1 S1 C11 104.2(3) . . ? S2' S2 O4 153.2(4) . . ? S2' S2 O3 63.8(4) . . ? O4 S2 O3 124.5(4) . . ? S2' S2 N1 81.4(3) . . ? O4 S2 N1 112.2(3) . . ? O3 S2 N1 113.4(3) . . ? S2' S2 C12 55.7(4) . . ? O4 S2 C12 98.3(4) . . ? O3 S2 C12 103.6(3) . . ? N1 S2 C12 99.5(3) . . ? S2 S2' O3 63.1(4) . . ? S2 S2' F6 135.4(6) . . ? O3 S2' F6 147.6(6) . . ? S2 S2' C12 78.7(5) . . ? O3 S2' C12 118.9(6) . . ? F6 S2' C12 58.4(4) . . ? S2 S2' N1 56.2(3) . . ? O3 S2' N1 97.7(4) . . ? F6 S2' N1 114.6(5) . . ? C12 S2' N1 98.1(4) . . ? O6 S3 O5 116.92(18) . . ? O6 S3 N2 111.8(2) . . ? O5 S3 N2 114.47(19) . . ? O6 S3 C13 105.6(2) . . ? O5 S3 C13 101.5(2) . . ? N2 S3 C13 104.8(2) . . ? O8 S4 O7 120.1(2) . . ? O8 S4 N2 107.9(2) . . ? O7 S4 N2 115.1(2) . . ? O8 S4 C14 105.5(2) . . ? O7 S4 C14 104.9(2) . . ? N2 S4 C14 101.2(2) . . ? S1 O1 Ti1 152.8(2) . . ? S2 O3 S2' 53.1(3) . . ? S3 O5 Ti1 151.45(19) . . ? S1 N1 S2 126.0(3) . . ? S1 N1 S2' 102.7(3) . . ? S2 N1 S2' 42.4(2) . . ? S3 N2 S4 127.1(2) . . ? C12 F6 S2' 61.4(4) . . ? C5 C1 C2 106.9(4) . . ? C5 C1 Ti1 74.1(3) . . ? C2 C1 Ti1 72.0(2) . . ? C3 C2 C1 108.4(5) . . ? C3 C2 Ti1 74.4(3) . . ? C1 C2 Ti1 72.7(3) . . ? C4 C3 C2 108.0(4) . . ? C4 C3 Ti1 73.2(3) . . ? C2 C3 Ti1 71.1(3) . . ? C3 C4 C5 108.3(4) . . ? C3 C4 Ti1 72.8(3) . . ? C5 C4 Ti1 72.7(3) . . ? C1 C5 C4 108.4(5) . . ? C1 C5 Ti1 71.3(3) . . ? C4 C5 Ti1 72.9(3) . . ? C7 C6 C10 106.8(5) . . ? C7 C6 Ti1 72.8(3) . . ? C10 C6 Ti1 71.0(3) . . ? C8 C7 C6 108.8(4) . . ? C8 C7 Ti1 71.5(3) . . ? C6 C7 Ti1 73.6(3) . . ? C9 C8 C7 108.3(5) . . ? C9 C8 Ti1 73.8(3) . . ? C7 C8 Ti1 74.5(3) . . ? C8 C9 C10 108.2(5) . . ? C8 C9 Ti1 72.3(3) . . ? C10 C9 Ti1 72.3(3) . . ? C9 C10 C6 107.8(5) . . ? C9 C10 Ti1 73.5(3) . . ? C6 C10 Ti1 74.4(3) . . ? F1 C11 F3 109.9(5) . . ? F1 C11 F2 109.5(5) . . ? F3 C11 F2 107.6(4) . . ? F1 C11 S1 111.3(4) . . ? F3 C11 S1 109.8(4) . . ? F2 C11 S1 108.7(4) . . ? F5 C12 F4 110.6(5) . . ? F5 C12 F6 107.0(6) . . ? F4 C12 F6 106.4(5) . . ? F5 C12 S2' 134.4(6) . . ? F4 C12 S2' 115.0(6) . . ? F6 C12 S2' 60.2(4) . . ? F5 C12 S2 114.9(5) . . ? F4 C12 S2 112.4(5) . . ? F6 C12 S2 104.9(4) . . ? S2' C12 S2 45.6(3) . . ? F9 C13 F8 110.3(5) . . ? F9 C13 F7 108.6(4) . . ? F8 C13 F7 107.6(4) . . ? F9 C13 S3 110.2(3) . . ? F8 C13 S3 110.4(3) . . ? F7 C13 S3 109.6(4) . . ? F12 C14 F11 108.9(4) . . ? F12 C14 F10 108.2(4) . . ? F11 C14 F10 109.1(4) . . ? F12 C14 S4 112.4(3) . . ? F11 C14 S4 109.0(3) . . ? F10 C14 S4 109.1(4) . . ? _refine_diff_density_max 0.725 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.090