Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ekkehardt Hahn' 'Birgit Birkmann' 'Tania Pape' _publ_contact_author_name 'Ekkehardt Hahn' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Westfalische Wilhelms Universitat Muenster Corrensstrasse 36 Munster D-48149 GERMANY ; _publ_contact_author_email FEHAHN@UNI-MUENSTER.DE _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Self-assembly reactions with a bis(benzene-o-dithiolato) ligand ; data_sad _database_code_depnum_ccdc_archive 'CCDC 674837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H138 N12 O9 S12 Ti2' _chemical_formula_weight 2252.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.4943(9) _cell_length_b 37.4265(17) _cell_length_c 16.5461(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.488(3) _cell_angle_gamma 90.00 _cell_volume 11431.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent needles' _exptl_crystal_colour red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4752 _exptl_absorpt_coefficient_mu 3.717 _exptl_absorpt_correction_type multi-csan _exptl_absorpt_correction_T_min 0.3401 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports Maximum and minimum effective transmission: 1.000000 0.686142 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65493 _diffrn_reflns_av_R_equivalents 0.1748 _diffrn_reflns_av_sigmaI/netI 0.2060 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 67.50 _reflns_number_total 20313 _reflns_number_gt 6711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _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^)+(0.2000P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20313 _refine_ls_number_parameters 1291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2250 _refine_ls_R_factor_gt 0.1136 _refine_ls_wR_factor_ref 0.3764 _refine_ls_wR_factor_gt 0.2964 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _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 0.25213(9) 0.32678(5) 0.22233(13) 0.0500(5) Uani 1 1 d . . . Ti2 Ti 0.26620(8) 0.66779(5) 0.09523(13) 0.0499(6) Uani 1 1 d . . . S1A S 0.19258(14) 0.28585(7) 0.3078(2) 0.0597(8) Uani 1 1 d . . . S2A S 0.15927(13) 0.36675(7) 0.2714(2) 0.0612(9) Uani 1 1 d . . . S3A S 0.18726(14) 0.70635(8) 0.1628(2) 0.0723(10) Uani 1 1 d . . . S4A S 0.16125(13) 0.62817(7) 0.0989(2) 0.0720(10) Uani 1 1 d . . . O1A O -0.0178(7) 0.4120(3) 0.4189(10) 0.191(8) Uani 1 1 d . . . O2A O -0.0389(4) 0.5836(2) 0.1135(7) 0.104(4) Uani 1 1 d . . . N1A N 0.0796(5) 0.4236(3) 0.3555(7) 0.075(3) Uani 1 1 d . . . H1A H 0.1163 0.4147 0.3309 0.090 Uiso 1 1 calc R . . N2A N 0.0552(5) 0.5732(3) 0.2009(8) 0.083(4) Uani 1 1 d . . . H2A H 0.0882 0.5836 0.2334 0.100 Uiso 1 1 calc R . . C1A C 0.1187(5) 0.3079(3) 0.3490(8) 0.064(3) Uani 1 1 d . . . C2A C 0.1084(5) 0.3447(3) 0.3431(7) 0.058(3) Uani 1 1 d . . . C3A C 0.0532(6) 0.3612(3) 0.3848(8) 0.068(4) Uani 1 1 d . . . C4A C 0.0096(7) 0.3403(4) 0.4303(9) 0.095(5) Uani 1 1 d . . . H4A H -0.0269 0.3513 0.4597 0.115 Uiso 1 1 calc R . . C5A C 0.0179(7) 0.3033(4) 0.4342(10) 0.100(5) Uani 1 1 d . . . H5A H -0.0136 0.2892 0.4645 0.120 Uiso 1 1 calc R . . C6A C 0.0725(6) 0.2871(4) 0.3933(9) 0.089(5) Uani 1 1 d . . . H6A H 0.0785 0.2619 0.3955 0.107 Uiso 1 1 calc R . . C7A C 0.0359(6) 0.4008(4) 0.3877(10) 0.083(4) Uani 1 1 d . . . C8A C 0.0731(6) 0.4621(3) 0.3565(10) 0.076(4) Uani 1 1 d . . . C9A C 0.0740(7) 0.4807(4) 0.4251(11) 0.095(5) Uani 1 1 d . . . H9A1 H 0.0779 0.4682 0.4751 0.114 Uiso 1 1 calc R . . C10A C 0.0697(7) 0.5177(4) 0.4263(11) 0.091(5) Uani 1 1 d . . . H10D H 0.0719 0.5304 0.4760 0.109 Uiso 1 1 calc R . . C11A C 0.0619(7) 0.5357(4) 0.3529(12) 0.090(5) Uani 1 1 d . . . H11C H 0.0570 0.5609 0.3524 0.108 Uiso 1 1 calc R . . C12A C 0.0614(6) 0.5170(4) 0.2801(12) 0.075(4) Uani 1 1 d . . . C13A C 0.0640(6) 0.4796(3) 0.2795(10) 0.071(4) Uani 1 1 d . . . C14A C 0.0566(5) 0.4608(4) 0.2035(11) 0.077(4) Uani 1 1 d . . . H14D H 0.0590 0.4355 0.2035 0.092 Uiso 1 1 calc R . . C15A C 0.0459(6) 0.4787(4) 0.1303(10) 0.078(4) Uani 1 1 d . . . H15C H 0.0394 0.4660 0.0805 0.093 Uiso 1 1 calc R . . C16A C 0.0451(5) 0.5162(4) 0.1327(11) 0.082(5) Uani 1 1 d . . . H16D H 0.0392 0.5290 0.0832 0.098 Uiso 1 1 calc R . . C17A C 0.0526(6) 0.5350(4) 0.2038(13) 0.083(5) Uani 1 1 d . . . C18A C 0.0130(6) 0.5946(4) 0.1541(10) 0.089(5) Uani 1 1 d . . . C19A C 0.0258(5) 0.6342(3) 0.1621(9) 0.081(4) Uani 1 1 d . . . C20A C -0.0301(6) 0.6541(4) 0.1855(11) 0.113(6) Uani 1 1 d . . . H20D H -0.0754 0.6429 0.1926 0.135 Uiso 1 1 calc R . . C21A C -0.0231(7) 0.6897(5) 0.1990(12) 0.129(7) Uani 1 1 d . . . H21C H -0.0631 0.7033 0.2151 0.155 Uiso 1 1 calc R . . C22A C 0.0420(6) 0.7059(4) 0.1893(11) 0.106(6) Uani 1 1 d . . . H22D H 0.0468 0.7309 0.1982 0.127 Uiso 1 1 calc R . . C23A C 0.1020(6) 0.6860(3) 0.1661(9) 0.078(4) Uani 1 1 d . . . C24A C 0.0931(5) 0.6501(3) 0.1454(8) 0.070(4) Uani 1 1 d . . . S1B S 0.35530(13) 0.28864(7) 0.22578(19) 0.0549(8) Uani 1 1 d . . . S2B S 0.33475(14) 0.36482(7) 0.3043(2) 0.0595(8) Uani 1 1 d . . . S3B S 0.35743(12) 0.70650(7) 0.15740(18) 0.0498(7) Uani 1 1 d . . . S4B S 0.33411(15) 0.62390(8) 0.1772(2) 0.0702(10) Uani 1 1 d . . . O1B O 0.4335(4) 0.39729(19) 0.4834(5) 0.062(2) Uani 1 1 d . . . O2B O 0.4527(4) 0.57004(19) 0.2613(5) 0.063(2) Uani 1 1 d . . . N1B N 0.4914(4) 0.4158(2) 0.3717(6) 0.055(2) Uani 1 1 d . . . H1B H 0.5073 0.4081 0.3258 0.066 Uiso 1 1 calc R . . N2B N 0.4019(4) 0.5738(3) 0.3842(6) 0.065(3) Uani 1 1 d . . . H2B H 0.3908 0.5883 0.4234 0.078 Uiso 1 1 calc R . . C1B C 0.4189(5) 0.3055(3) 0.3007(7) 0.057(3) Uani 1 1 d . . . C2B C 0.4128(5) 0.3393(3) 0.3332(7) 0.049(3) Uani 1 1 d . . . C3B C 0.4650(5) 0.3521(3) 0.3867(7) 0.048(3) Uani 1 1 d . . . C4B C 0.5232(5) 0.3320(3) 0.4143(7) 0.055(3) Uani 1 1 d . . . H4B H 0.5582 0.3413 0.4530 0.066 Uiso 1 1 calc R . . C5B C 0.5298(6) 0.2978(3) 0.3846(8) 0.063(3) Uani 1 1 d . . . H5B H 0.5689 0.2831 0.4040 0.075 Uiso 1 1 calc R . . C6B C 0.4788(5) 0.2847(3) 0.3257(7) 0.058(3) Uani 1 1 d . . . H6B H 0.4850 0.2617 0.3029 0.069 Uiso 1 1 calc R . . C7B C 0.4608(5) 0.3906(3) 0.4192(8) 0.058(3) Uani 1 1 d . . . C8B C 0.5007(6) 0.4534(3) 0.3878(7) 0.058(3) Uani 1 1 d . . . C9B C 0.5683(5) 0.4664(3) 0.3916(7) 0.056(3) Uani 1 1 d . . . H9B1 H 0.6079 0.4504 0.3884 0.067 Uiso 1 1 calc R . . C10B C 0.5820(5) 0.5030(3) 0.4002(7) 0.062(3) Uani 1 1 d . . . H10E H 0.6305 0.5115 0.4048 0.075 Uiso 1 1 calc R . . C11B C 0.5250(5) 0.5269(3) 0.4021(7) 0.059(3) Uani 1 1 d . . . H11D H 0.5335 0.5519 0.4071 0.071 Uiso 1 1 calc R . . C12B C 0.4521(5) 0.5128(3) 0.3962(7) 0.054(3) Uani 1 1 d . . . C13B C 0.4404(5) 0.4756(3) 0.3943(8) 0.062(3) Uani 1 1 d . . . C14B C 0.3679(5) 0.4624(3) 0.3990(7) 0.059(3) Uani 1 1 d . . . H14E H 0.3585 0.4374 0.3978 0.071 Uiso 1 1 calc R . . C15B C 0.3125(5) 0.4864(3) 0.4054(7) 0.059(3) Uani 1 1 d . . . H15D H 0.2650 0.4778 0.4128 0.071 Uiso 1 1 calc R . . C16B C 0.3244(5) 0.5237(3) 0.4011(7) 0.062(3) Uani 1 1 d . . . H16E H 0.2850 0.5399 0.4023 0.074 Uiso 1 1 calc R . . C17B C 0.3916(5) 0.5358(3) 0.3952(8) 0.062(3) Uani 1 1 d . . . C18B C 0.4283(5) 0.5883(3) 0.3151(9) 0.066(4) Uani 1 1 d . . . C19B C 0.4284(5) 0.6286(3) 0.3105(8) 0.058(3) Uani 1 1 d . . . C20B C 0.4691(5) 0.6479(3) 0.3697(7) 0.059(3) Uani 1 1 d . . . H20E H 0.4940 0.6355 0.4132 0.071 Uiso 1 1 calc R . . C21B C 0.4734(5) 0.6847(3) 0.3655(8) 0.063(3) Uani 1 1 d . . . H21D H 0.5010 0.6975 0.4063 0.076 Uiso 1 1 calc R . . C22B C 0.4381(5) 0.7028(3) 0.3029(8) 0.058(3) Uani 1 1 d . . . H22E H 0.4421 0.7281 0.3005 0.069 Uiso 1 1 calc R . . C23B C 0.3968(4) 0.6850(3) 0.2430(7) 0.047(3) Uani 1 1 d . . . C24B C 0.3904(4) 0.6474(3) 0.2474(7) 0.049(3) Uani 1 1 d . . . S1C S 0.20914(14) 0.28983(7) 0.1108(2) 0.0574(8) Uani 1 1 d . . . S2C S 0.25402(14) 0.37128(7) 0.11507(19) 0.0550(7) Uani 1 1 d . . . S3C S 0.26222(15) 0.71013(8) -0.0124(2) 0.0667(9) Uani 1 1 d . . . S4C S 0.29970(19) 0.62902(8) -0.0165(2) 0.0748(10) Uani 1 1 d . . . O1C O 0.3045(3) 0.42055(18) -0.0210(4) 0.0520(19) Uani 1 1 d . . . O2C O 0.3980(4) 0.59434(19) -0.2486(5) 0.073(2) Uani 1 1 d . . . N1C N 0.3229(4) 0.5779(2) -0.1532(6) 0.057(2) Uani 1 1 d . . . H1C H 0.2979 0.5864 -0.1140 0.068 Uiso 1 1 calc R . . N2C N 0.1977(4) 0.4281(2) -0.0934(6) 0.057(3) Uani 1 1 d . . . H2C H 0.1608 0.4173 -0.1191 0.068 Uiso 1 1 calc R . . C1C C 0.2188(5) 0.3129(3) 0.0195(7) 0.044(3) Uani 1 1 d . . . C2C C 0.2342(4) 0.3501(2) 0.0212(6) 0.036(2) Uani 1 1 d . . . C3C C 0.2325(5) 0.3687(3) -0.0517(7) 0.049(3) Uani 1 1 d . . . C4C C 0.2191(5) 0.3513(3) -0.1244(8) 0.061(3) Uani 1 1 d . . . H4C H 0.2168 0.3646 -0.1733 0.073 Uiso 1 1 calc R . . C5C C 0.2090(5) 0.3145(3) -0.1274(8) 0.060(3) Uani 1 1 d . . . H5C H 0.2022 0.3026 -0.1780 0.072 Uiso 1 1 calc R . . C6C C 0.2090(5) 0.2952(3) -0.0554(8) 0.058(3) Uani 1 1 d . . . H6C H 0.2024 0.2700 -0.0568 0.070 Uiso 1 1 calc R . . C7C C 0.2481(5) 0.4084(3) -0.0531(6) 0.049(3) Uani 1 1 d . . . C8C C 0.2017(5) 0.4665(3) -0.0963(7) 0.058(3) Uani 1 1 d . . . C9C C 0.1463(5) 0.4858(3) -0.0652(8) 0.069(4) Uani 1 1 d . . . H9C H 0.1064 0.4736 -0.0446 0.083 Uiso 1 1 calc R . . C10C C 0.1483(5) 0.5233(3) -0.0637(8) 0.068(4) Uani 1 1 d . . . H10F H 0.1101 0.5362 -0.0414 0.081 Uiso 1 1 calc R . . C11C C 0.2046(5) 0.5409(3) -0.0939(7) 0.059(3) Uani 1 1 d . . . H11E H 0.2062 0.5663 -0.0911 0.071 Uiso 1 1 calc R . . C12C C 0.2611(5) 0.5222(3) -0.1297(7) 0.049(3) Uani 1 1 d . . . C13C C 0.2597(5) 0.4851(3) -0.1329(7) 0.051(3) Uani 1 1 d . . . C14C C 0.3141(5) 0.4661(3) -0.1707(6) 0.052(3) Uani 1 1 d . . . H14F H 0.3123 0.4407 -0.1733 0.063 Uiso 1 1 calc R . . C15C C 0.3692(5) 0.4841(3) -0.2034(7) 0.057(3) Uani 1 1 d . . . H15E H 0.4054 0.4714 -0.2299 0.069 Uiso 1 1 calc R . . C16C C 0.3724(6) 0.5216(3) -0.1979(7) 0.063(3) Uani 1 1 d . . . H16F H 0.4118 0.5339 -0.2197 0.076 Uiso 1 1 calc R . . C17C C 0.3214(5) 0.5404(3) -0.1626(6) 0.050(3) Uani 1 1 d . . . C18C C 0.3578(6) 0.6026(3) -0.1966(8) 0.058(3) Uani 1 1 d . . . C19C C 0.3450(5) 0.6412(3) -0.1744(8) 0.060(3) Uani 1 1 d . . . C20C C 0.3622(6) 0.6653(3) -0.2344(8) 0.064(3) Uani 1 1 d . . . H20F H 0.3833 0.6563 -0.2812 0.077 Uiso 1 1 calc R . . C21C C 0.3499(6) 0.7013(3) -0.2292(9) 0.078(4) Uani 1 1 d . . . H21E H 0.3611 0.7169 -0.2721 0.093 Uiso 1 1 calc R . . C22C C 0.3211(6) 0.7146(3) -0.1602(9) 0.073(4) Uani 1 1 d . . . H22F H 0.3129 0.7396 -0.1554 0.088 Uiso 1 1 calc R . . C23C C 0.3037(6) 0.6917(3) -0.0970(8) 0.066(3) Uani 1 1 d . . . C24C C 0.3161(5) 0.6552(3) -0.1018(8) 0.063(3) Uani 1 1 d . . . N2 N 0.2651(5) 0.3394(3) 0.5733(6) 0.070(3) Uani 1 1 d . . . C7 C 0.3388(6) 0.3536(3) 0.6061(8) 0.075(4) Uani 1 1 d . . . H7A H 0.3687 0.3331 0.6252 0.090 Uiso 1 1 calc R . . H7B H 0.3630 0.3647 0.5607 0.090 Uiso 1 1 calc R . . C8 C 0.3379(7) 0.3808(4) 0.6747(9) 0.093(5) Uani 1 1 d . . . H8A H 0.3153 0.4030 0.6544 0.140 Uiso 1 1 calc R . . H8B H 0.3877 0.3857 0.6954 0.140 Uiso 1 1 calc R . . H8C H 0.3102 0.3712 0.7184 0.140 Uiso 1 1 calc R . . C9 C 0.2136(6) 0.3700(4) 0.5529(9) 0.081(4) Uani 1 1 d . . . H9A H 0.2011 0.3814 0.6042 0.097 Uiso 1 1 calc R . . H9B H 0.1684 0.3600 0.5270 0.097 Uiso 1 1 calc R . . C10 C 0.2408(7) 0.3989(4) 0.4977(9) 0.091(4) Uani 1 1 d . . . H10A H 0.2839 0.4103 0.5238 0.136 Uiso 1 1 calc R . . H10B H 0.2028 0.4169 0.4875 0.136 Uiso 1 1 calc R . . H10C H 0.2531 0.3882 0.4463 0.136 Uiso 1 1 calc R . . C11 C 0.2744(6) 0.3192(3) 0.4957(8) 0.076(4) Uani 1 1 d . . . H11A H 0.2915 0.3361 0.4551 0.091 Uiso 1 1 calc R . . H11B H 0.2262 0.3104 0.4751 0.091 Uiso 1 1 calc R . . C12 C 0.3270(6) 0.2869(3) 0.5009(9) 0.084(4) Uani 1 1 d . . . H12A H 0.3771 0.2956 0.5046 0.125 Uiso 1 1 calc R . . H12B H 0.3190 0.2721 0.4524 0.125 Uiso 1 1 calc R . . H12C H 0.3182 0.2727 0.5491 0.125 Uiso 1 1 calc R . . C13 C 0.2356(7) 0.3175(4) 0.6380(9) 0.098(5) Uani 1 1 d . . . H13A H 0.2378 0.3318 0.6884 0.118 Uiso 1 1 calc R . . H13B H 0.2678 0.2966 0.6477 0.118 Uiso 1 1 calc R . . C14 C 0.1574(7) 0.3036(4) 0.6229(11) 0.111(6) Uani 1 1 d . . . H14A H 0.1242 0.3239 0.6157 0.167 Uiso 1 1 calc R . . H14B H 0.1441 0.2893 0.6694 0.167 Uiso 1 1 calc R . . H14C H 0.1542 0.2888 0.5740 0.167 Uiso 1 1 calc R . . N3 N 0.3303(4) 0.4957(2) 0.1400(6) 0.052(2) Uani 1 1 d . . . C15 C 0.3059(6) 0.5277(3) 0.1868(8) 0.069(4) Uani 1 1 d . . . H15A H 0.3455 0.5456 0.1897 0.083 Uiso 1 1 calc R . . H15B H 0.2979 0.5201 0.2429 0.083 Uiso 1 1 calc R . . C16 C 0.2368(6) 0.5456(3) 0.1509(10) 0.096(5) Uani 1 1 d . . . H16A H 0.2454 0.5552 0.0972 0.144 Uiso 1 1 calc R . . H16B H 0.2231 0.5651 0.1864 0.144 Uiso 1 1 calc R . . H16C H 0.1975 0.5280 0.1460 0.144 Uiso 1 1 calc R . . C17 C 0.3456(6) 0.5061(3) 0.0556(7) 0.062(3) Uani 1 1 d . . . H17A H 0.3009 0.5163 0.0290 0.074 Uiso 1 1 calc R . . H17B H 0.3575 0.4842 0.0255 0.074 Uiso 1 1 calc R . . C18 C 0.4081(6) 0.5335(3) 0.0480(9) 0.081(4) Uani 1 1 d . . . H18A H 0.3940 0.5565 0.0705 0.121 Uiso 1 1 calc R . . H18B H 0.4176 0.5365 -0.0092 0.121 Uiso 1 1 calc R . . H18C H 0.4519 0.5247 0.0779 0.121 Uiso 1 1 calc R . . C19 C 0.3964(5) 0.4818(3) 0.1885(8) 0.066(4) Uani 1 1 d . . . H19A H 0.3830 0.4762 0.2441 0.079 Uiso 1 1 calc R . . H19B H 0.4337 0.5009 0.1924 0.079 Uiso 1 1 calc R . . C20 C 0.4292(6) 0.4480(3) 0.1510(9) 0.085(4) Uani 1 1 d . . . H20A H 0.3906 0.4306 0.1379 0.127 Uiso 1 1 calc R . . H20B H 0.4652 0.4374 0.1898 0.127 Uiso 1 1 calc R . . H20C H 0.4525 0.4545 0.1014 0.127 Uiso 1 1 calc R . . C21 C 0.2703(5) 0.4675(3) 0.1339(8) 0.057(3) Uani 1 1 d . . . H21A H 0.2285 0.4777 0.1015 0.068 Uiso 1 1 calc R . . H21B H 0.2880 0.4469 0.1034 0.068 Uiso 1 1 calc R . . C22 C 0.2439(5) 0.4540(3) 0.2111(8) 0.063(3) Uani 1 1 d . . . H22A H 0.2839 0.4426 0.2429 0.094 Uiso 1 1 calc R . . H22B H 0.2051 0.4366 0.1995 0.094 Uiso 1 1 calc R . . H22C H 0.2251 0.4740 0.2419 0.094 Uiso 1 1 calc R . . N4 N 0.4593(4) 0.3347(2) 0.9765(6) 0.054(2) Uani 1 1 d . . . C23 C 0.5149(5) 0.3062(3) 1.0009(8) 0.067(4) Uani 1 1 d . . . H23A H 0.5375 0.2979 0.9516 0.080 Uiso 1 1 calc R . . H23B H 0.5534 0.3174 1.0366 0.080 Uiso 1 1 calc R . . C24 C 0.4864(6) 0.2742(3) 1.0438(8) 0.077(4) Uani 1 1 d . . . H24A H 0.4586 0.2821 1.0890 0.115 Uiso 1 1 calc R . . H24B H 0.5271 0.2593 1.0644 0.115 Uiso 1 1 calc R . . H24C H 0.4550 0.2602 1.0058 0.115 Uiso 1 1 calc R . . C25 C 0.4229(5) 0.3485(3) 1.0509(8) 0.074(4) Uani 1 1 d . . . H25A H 0.3915 0.3689 1.0339 0.089 Uiso 1 1 calc R . . H25B H 0.3910 0.3293 1.0696 0.089 Uiso 1 1 calc R . . C26 C 0.4716(6) 0.3602(3) 1.1214(8) 0.076(4) Uani 1 1 d . . . H26A H 0.4997 0.3397 1.1428 0.115 Uiso 1 1 calc R . . H26B H 0.4423 0.3699 1.1637 0.115 Uiso 1 1 calc R . . H26C H 0.5047 0.3787 1.1038 0.115 Uiso 1 1 calc R . . C27 C 0.5013(5) 0.3634(3) 0.9374(8) 0.063(3) Uani 1 1 d . . . H27A H 0.5275 0.3526 0.8930 0.075 Uiso 1 1 calc R . . H27B H 0.5381 0.3728 0.9779 0.075 Uiso 1 1 calc R . . C28 C 0.4563(6) 0.3943(3) 0.9033(8) 0.074(4) Uani 1 1 d . . . H28A H 0.4143 0.3850 0.8708 0.111 Uiso 1 1 calc R . . H28B H 0.4858 0.4091 0.8691 0.111 Uiso 1 1 calc R . . H28C H 0.4396 0.4088 0.9478 0.111 Uiso 1 1 calc R . . C29 C 0.4005(5) 0.3187(3) 0.9198(8) 0.066(3) Uani 1 1 d . . . H29A H 0.3597 0.3359 0.9140 0.079 Uiso 1 1 calc R . . H29B H 0.3821 0.2968 0.9452 0.079 Uiso 1 1 calc R . . C30 C 0.4236(7) 0.3092(3) 0.8355(9) 0.084(4) Uani 1 1 d . . . H30A H 0.4250 0.3309 0.8025 0.127 Uiso 1 1 calc R . . H30B H 0.3888 0.2923 0.8098 0.127 Uiso 1 1 calc R . . H30C H 0.4718 0.2982 0.8399 0.127 Uiso 1 1 calc R . . N10 N 0.1852(10) 0.6601(5) 0.3643(10) 0.151(6) Uani 1 1 d . . . O40 O 0.1609(9) 0.6030(4) 0.3149(10) 0.194(8) Uani 1 1 d . . . C42 C 0.1971(14) 0.6266(7) 0.3273(14) 0.158(9) Uani 1 1 d . . . C43 C 0.1103(14) 0.6704(12) 0.3939(19) 0.39(3) Uani 1 1 d . . . H43A H 0.0760 0.6740 0.3471 0.586 Uiso 1 1 calc . . . H43B H 0.1146 0.6925 0.4255 0.586 Uiso 1 1 calc . . . H43C H 0.0928 0.6512 0.4279 0.586 Uiso 1 1 calc . . . C44 C 0.2443(10) 0.6877(5) 0.3759(15) 0.168(10) Uani 1 1 d . . . H44A H 0.2898 0.6778 0.3583 0.252 Uiso 1 1 calc . . . H44B H 0.2504 0.6942 0.4333 0.252 Uiso 1 1 calc . . . H44C H 0.2312 0.7090 0.3438 0.252 Uiso 1 1 calc . . . N11 N 0.1544(6) 0.4774(5) 0.6856(8) 0.118(6) Uani 1 1 d . . . O41 O 0.1601(8) 0.4142(4) 0.7083(9) 0.153(6) Uani 1 1 d . . . C45 C 0.1192(8) 0.5100(6) 0.7092(11) 0.136(7) Uani 1 1 d . . . H45A H 0.1543 0.5251 0.7399 0.204 Uiso 1 1 calc . . . H45B H 0.0792 0.5042 0.7431 0.204 Uiso 1 1 calc . . . H45C H 0.1004 0.5228 0.6607 0.204 Uiso 1 1 calc . . . C46 C 0.2100(10) 0.4778(6) 0.6345(12) 0.171(10) Uani 1 1 d . . . H46A H 0.2069 0.4996 0.6015 0.256 Uiso 1 1 calc . . . H46B H 0.2065 0.4568 0.5992 0.256 Uiso 1 1 calc . . . H46C H 0.2564 0.4774 0.6665 0.256 Uiso 1 1 calc . . . C47 C 0.1339(12) 0.4427(7) 0.7207(16) 0.159(11) Uani 1 1 d . . . O66 O 0.3216(5) 0.6133(3) 0.5050(7) 0.068(4) Uani 0.687(14) 1 d P . . O66A O 0.7669(11) 0.3981(6) 0.4218(13) 0.058(8) Uani 0.313(14) 1 d P . . N51 N 0.9569(8) 0.3266(4) 0.1274(10) 0.110(2) Uiso 1 1 d . . . C51 C 0.9453(15) 0.3091(7) 0.0465(17) 0.110(2) Uiso 0.624(8) 1 d P A 1 H51A H 0.9492 0.3272 0.0035 0.132 Uiso 0.624(8) 1 calc PR A 1 H51B H 0.8957 0.2989 0.0412 0.132 Uiso 0.624(8) 1 calc PR A 1 C52 C 1.0000(14) 0.2794(7) 0.0345(17) 0.110(2) Uiso 0.624(8) 1 d P A 1 H52A H 0.9894 0.2680 -0.0182 0.165 Uiso 0.62 1 calc P A 1 H52B H 0.9970 0.2616 0.0775 0.165 Uiso 0.62 1 calc P A 1 H52C H 1.0490 0.2895 0.0364 0.165 Uiso 0.62 1 calc P A 1 C51A C 1.016(2) 0.2971(11) 0.164(3) 0.110(2) Uiso 0.376(8) 1 d P A 2 H51C H 1.0646 0.3086 0.1637 0.132 Uiso 0.376(8) 1 calc PR A 2 H51D H 1.0065 0.2935 0.2215 0.132 Uiso 0.376(8) 1 calc PR A 2 C52A C 1.024(2) 0.2630(12) 0.131(3) 0.110(2) Uiso 0.376(8) 1 d P A 2 H52D H 1.0118 0.2640 0.0721 0.165 Uiso 0.38 1 calc P A 2 H52E H 0.9914 0.2463 0.1558 0.165 Uiso 0.38 1 calc P A 2 H52F H 1.0742 0.2549 0.1403 0.165 Uiso 0.38 1 calc P A 2 C53 C 0.9512(14) 0.3059(7) 0.1965(17) 0.110(2) Uiso 0.624(8) 1 d P A 1 H53A H 0.9624 0.3207 0.2452 0.132 Uiso 0.624(8) 1 calc PR A 1 H53B H 0.9866 0.2861 0.1967 0.132 Uiso 0.624(8) 1 calc PR A 1 C53A C 0.894(2) 0.3069(12) 0.115(3) 0.110(2) Uiso 0.376(8) 1 d P A 4 H53C H 0.9009 0.2875 0.0759 0.132 Uiso 0.376(8) 1 calc PR A 4 H53D H 0.8541 0.3225 0.0925 0.132 Uiso 0.376(8) 1 calc PR A 4 C54 C 0.8711(9) 0.2902(4) 0.1988(11) 0.110(2) Uiso 1 1 d . . . H54A H 0.8675 0.2757 0.2478 0.165 Uiso 0.62 1 calc P A 1 H54B H 0.8604 0.2753 0.1510 0.165 Uiso 0.62 1 calc P A 1 H54C H 0.8363 0.3099 0.1992 0.165 Uiso 0.62 1 calc P A 1 H54D H 0.8971 0.2676 0.2089 0.165 Uiso 0.38 1 calc P A 4 H54E H 0.8188 0.2857 0.1961 0.165 Uiso 0.38 1 calc P A 4 H54F H 0.8837 0.3070 0.2430 0.165 Uiso 0.38 1 calc P A 4 C55 C 0.8907(14) 0.3566(7) 0.1197(16) 0.110(2) Uiso 0.624(8) 1 d P A 3 H55A H 0.8917 0.3692 0.0671 0.132 Uiso 0.624(8) 1 calc PR A 3 H55B H 0.8433 0.3444 0.1216 0.132 Uiso 0.624(8) 1 calc PR A 3 C55A C 0.963(2) 0.3546(11) 0.183(3) 0.110(2) Uiso 0.376(8) 1 d P A 5 H55C H 1.0073 0.3682 0.1738 0.132 Uiso 0.376(8) 1 calc PR A 5 H55D H 0.9690 0.3441 0.2382 0.132 Uiso 0.376(8) 1 calc PR A 5 C56 C 0.8985(9) 0.3814(5) 0.1826(11) 0.110(2) Uiso 1 1 d . . . H56A H 0.8596 0.3991 0.1768 0.165 Uiso 0.62 1 calc P A 3 H56B H 0.9455 0.3934 0.1808 0.165 Uiso 0.62 1 calc P A 3 H56C H 0.8960 0.3690 0.2346 0.165 Uiso 0.62 1 calc P A 3 H56D H 0.9128 0.4024 0.2151 0.165 Uiso 0.38 1 calc P A 5 H56E H 0.8568 0.3699 0.2055 0.165 Uiso 0.38 1 calc P A 5 H56F H 0.8855 0.3887 0.1268 0.165 Uiso 0.38 1 calc P A 5 C57 C 1.0256(14) 0.3463(7) 0.1285(17) 0.110(2) Uiso 0.624(8) 1 d P A 1 H57A H 1.0268 0.3620 0.1767 0.132 Uiso 0.624(8) 1 calc PR A 1 H57B H 1.0647 0.3285 0.1386 0.132 Uiso 0.624(8) 1 calc PR A 1 C57A C 0.987(2) 0.3353(12) 0.052(3) 0.110(2) Uiso 0.376(8) 1 d P A 2 H57C H 0.9469 0.3424 0.0124 0.132 Uiso 0.376(8) 1 calc PR A 2 H57D H 1.0103 0.3139 0.0305 0.132 Uiso 0.376(8) 1 calc PR A 2 C58 C 1.0468(9) 0.3684(4) 0.0615(11) 0.110(2) Uiso 1 1 d . . . H58A H 1.0926 0.3805 0.0768 0.165 Uiso 0.62 1 calc P A 1 H58B H 1.0091 0.3862 0.0485 0.165 Uiso 0.62 1 calc P A 1 H58C H 1.0529 0.3533 0.0140 0.165 Uiso 0.62 1 calc P A 1 H58D H 1.0921 0.3593 0.0878 0.165 Uiso 0.38 1 calc P A 2 H58E H 1.0276 0.3875 0.0945 0.165 Uiso 0.38 1 calc P A 2 H58F H 1.0561 0.3777 0.0078 0.165 Uiso 0.38 1 calc P A 2 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 0.0414(9) 0.0410(12) 0.0684(15) 0.0022(10) 0.0105(10) -0.0018(8) Ti2 0.0314(8) 0.0420(11) 0.0768(15) -0.0013(11) 0.0060(9) 0.0009(7) S1A 0.0564(15) 0.0458(17) 0.078(2) 0.0044(16) 0.0161(15) -0.0022(12) S2A 0.0513(14) 0.0410(16) 0.095(2) 0.0085(16) 0.0312(15) -0.0003(12) S3A 0.0466(14) 0.0492(18) 0.124(3) -0.0144(19) 0.0298(17) -0.0037(12) S4A 0.0370(12) 0.0428(17) 0.136(3) -0.0026(19) 0.0041(16) -0.0019(11) O1A 0.162(11) 0.091(9) 0.34(2) -0.008(10) 0.179(13) 0.009(8) O2A 0.054(5) 0.089(7) 0.165(11) 0.030(7) -0.019(6) -0.010(5) N1A 0.065(6) 0.067(7) 0.097(9) 0.004(6) 0.031(6) 0.018(5) N2A 0.041(5) 0.075(8) 0.136(11) 0.017(7) 0.018(6) 0.006(5) C1A 0.040(5) 0.066(8) 0.088(10) -0.005(7) 0.015(6) -0.009(5) C2A 0.037(5) 0.066(8) 0.070(9) 0.007(7) -0.001(5) -0.007(5) C3A 0.049(6) 0.064(8) 0.092(10) 0.003(7) 0.023(7) -0.001(5) C4A 0.071(8) 0.099(12) 0.122(14) 0.017(10) 0.046(9) 0.025(8) C5A 0.071(8) 0.092(12) 0.143(15) 0.042(11) 0.048(9) 0.006(8) C6A 0.059(7) 0.071(9) 0.138(14) 0.014(9) 0.025(8) 0.002(6) C7A 0.054(7) 0.076(10) 0.121(13) 0.008(9) 0.031(8) 0.003(6) C8A 0.072(8) 0.049(8) 0.108(13) 0.014(9) 0.024(8) 0.024(6) C9A 0.100(10) 0.064(10) 0.124(15) -0.014(10) 0.036(10) 0.008(8) C10A 0.087(9) 0.070(10) 0.116(14) 0.001(10) 0.008(9) 0.007(8) C11A 0.073(8) 0.055(9) 0.144(16) 0.014(11) 0.027(10) 0.019(7) C12A 0.052(6) 0.051(9) 0.126(14) 0.014(10) 0.029(8) 0.009(6) C13A 0.053(6) 0.051(8) 0.111(13) 0.005(9) 0.032(7) 0.010(6) C14A 0.043(6) 0.063(9) 0.129(14) -0.002(10) 0.030(8) 0.004(6) C15A 0.048(6) 0.090(11) 0.096(12) 0.006(9) 0.010(7) -0.001(7) C16A 0.041(6) 0.068(10) 0.139(15) 0.034(10) 0.031(8) 0.003(6) C17A 0.042(6) 0.061(10) 0.151(17) -0.004(11) 0.033(9) -0.002(6) C18A 0.032(6) 0.081(10) 0.151(15) 0.034(10) -0.023(7) -0.021(6) C19A 0.036(5) 0.063(9) 0.142(14) 0.024(9) -0.002(7) -0.007(5) C20A 0.023(5) 0.119(14) 0.196(19) 0.020(13) 0.005(8) -0.007(7) C21A 0.043(7) 0.110(14) 0.24(2) 0.008(15) 0.044(10) -0.007(8) C22A 0.059(7) 0.064(9) 0.201(19) -0.006(10) 0.049(10) 0.006(6) C23A 0.052(6) 0.067(9) 0.119(12) 0.000(8) 0.029(7) -0.005(6) C24A 0.036(5) 0.056(8) 0.117(12) 0.014(8) 0.009(6) 0.005(5) S1B 0.0485(13) 0.0409(16) 0.077(2) -0.0040(15) 0.0136(14) -0.0012(11) S2B 0.0498(14) 0.0444(17) 0.083(2) -0.0052(15) -0.0072(15) 0.0100(12) S3B 0.0339(11) 0.0397(15) 0.076(2) 0.0029(14) 0.0085(13) 0.0000(10) S4B 0.0617(16) 0.0425(17) 0.103(3) 0.0017(17) -0.0243(17) -0.0065(13) O1B 0.055(4) 0.059(5) 0.072(6) 0.003(4) 0.007(4) 0.003(4) O2B 0.051(4) 0.050(5) 0.088(7) -0.001(4) 0.017(4) 0.010(3) N1B 0.059(5) 0.046(6) 0.061(6) -0.001(5) 0.004(5) 0.000(4) N2B 0.055(5) 0.059(7) 0.082(8) -0.004(6) 0.023(5) -0.003(4) C1B 0.047(5) 0.039(6) 0.086(9) 0.004(6) 0.017(6) -0.001(5) C2B 0.043(5) 0.032(6) 0.072(8) 0.014(6) 0.017(6) 0.004(4) C3B 0.042(5) 0.039(6) 0.062(8) 0.011(6) 0.009(5) -0.001(4) C4B 0.047(6) 0.052(7) 0.065(8) 0.006(6) 0.014(6) 0.000(5) C5B 0.052(6) 0.061(8) 0.076(9) 0.008(7) 0.016(6) 0.010(6) C6B 0.059(6) 0.036(6) 0.080(9) -0.001(6) 0.021(7) -0.001(5) C7B 0.049(6) 0.055(8) 0.070(9) 0.000(7) 0.014(6) -0.007(5) C8B 0.058(6) 0.038(7) 0.077(9) 0.000(6) 0.004(6) 0.005(5) C9B 0.046(6) 0.047(7) 0.077(9) 0.001(6) 0.016(6) 0.002(5) C10B 0.043(5) 0.064(8) 0.081(9) 0.008(7) 0.011(6) 0.004(5) C11B 0.050(6) 0.054(7) 0.074(9) 0.002(6) 0.012(6) -0.005(5) C12B 0.039(5) 0.056(7) 0.068(8) 0.001(6) 0.008(5) 0.002(5) C13B 0.050(6) 0.057(8) 0.081(9) 0.008(7) 0.016(6) -0.004(5) C14B 0.042(5) 0.063(8) 0.073(9) 0.005(7) 0.003(6) 0.001(5) C15B 0.047(6) 0.055(7) 0.075(9) 0.007(6) 0.015(6) -0.012(5) C16B 0.046(6) 0.067(8) 0.073(9) 0.005(7) 0.011(6) -0.001(5) C17B 0.045(6) 0.056(8) 0.086(10) -0.001(7) 0.014(6) -0.005(5) C18B 0.032(5) 0.056(8) 0.111(12) -0.001(8) 0.004(6) 0.003(5) C19B 0.024(4) 0.051(7) 0.100(10) -0.011(7) 0.006(6) 0.004(4) C20B 0.042(5) 0.056(8) 0.077(9) -0.002(7) -0.002(6) 0.001(5) C21B 0.047(6) 0.052(8) 0.088(10) -0.016(7) -0.014(6) -0.008(5) C22B 0.038(5) 0.051(7) 0.085(9) -0.013(7) 0.015(6) 0.000(5) C23B 0.027(4) 0.045(6) 0.068(8) 0.002(6) 0.000(5) -0.002(4) C24B 0.025(4) 0.053(7) 0.070(8) -0.010(6) 0.009(5) -0.001(4) S1C 0.0546(14) 0.0435(16) 0.075(2) 0.0007(15) 0.0072(15) -0.0082(12) S2C 0.0559(14) 0.0418(16) 0.068(2) 0.0017(15) 0.0112(14) -0.0079(12) S3C 0.0635(16) 0.0479(18) 0.089(3) 0.0014(17) 0.0069(17) 0.0103(13) S4C 0.101(2) 0.0428(18) 0.083(2) 0.0018(17) 0.024(2) 0.0075(16) O1C 0.039(4) 0.058(5) 0.060(5) 0.004(4) 0.005(3) -0.004(3) O2C 0.092(5) 0.047(5) 0.086(7) -0.002(5) 0.054(5) -0.015(4) N1C 0.048(4) 0.044(6) 0.080(7) -0.008(5) 0.023(5) -0.006(4) N2C 0.037(4) 0.055(6) 0.077(7) 0.008(5) -0.013(4) -0.016(4) C1C 0.039(5) 0.033(6) 0.061(7) 0.012(5) 0.005(5) -0.003(4) C2C 0.038(5) 0.030(5) 0.042(6) -0.005(5) 0.001(4) -0.001(4) C3C 0.032(5) 0.049(7) 0.067(8) -0.002(6) 0.014(5) -0.004(4) C4C 0.045(6) 0.052(7) 0.087(10) -0.001(7) 0.012(6) -0.011(5) C5C 0.047(6) 0.063(8) 0.071(9) 0.000(7) 0.004(6) -0.003(5) C6C 0.043(5) 0.052(7) 0.080(9) -0.030(7) 0.000(6) -0.010(5) C7C 0.029(5) 0.067(8) 0.050(7) 0.015(6) 0.005(5) -0.002(5) C8C 0.042(5) 0.056(8) 0.075(9) 0.009(6) -0.011(6) -0.007(5) C9C 0.035(5) 0.065(8) 0.108(11) 0.011(8) 0.003(6) -0.005(5) C10C 0.038(5) 0.070(9) 0.096(11) -0.001(8) 0.014(6) 0.012(5) C11C 0.047(6) 0.062(8) 0.070(9) 0.007(6) 0.010(6) 0.001(5) C12C 0.038(5) 0.055(7) 0.053(7) 0.005(6) 0.000(5) 0.001(5) C13C 0.036(5) 0.055(7) 0.062(8) 0.003(6) 0.003(5) -0.003(5) C14C 0.058(6) 0.047(7) 0.051(7) -0.004(6) -0.004(6) 0.004(5) C15C 0.057(6) 0.052(7) 0.066(8) 0.007(6) 0.028(6) 0.001(5) C16C 0.055(6) 0.059(8) 0.078(9) -0.002(7) 0.023(6) -0.001(5) C17C 0.050(6) 0.055(7) 0.044(7) -0.007(6) -0.003(5) 0.002(5) C18C 0.051(6) 0.048(7) 0.074(9) 0.000(6) 0.002(6) -0.002(5) C19C 0.045(5) 0.055(8) 0.083(10) 0.004(7) 0.020(6) 0.003(5) C20C 0.066(7) 0.051(8) 0.078(9) -0.002(7) 0.023(7) -0.010(6) C21C 0.080(8) 0.068(10) 0.089(11) 0.002(8) 0.033(8) 0.008(7) C22C 0.079(8) 0.034(7) 0.107(12) 0.006(7) 0.018(8) -0.004(6) C23C 0.055(6) 0.049(7) 0.096(11) 0.008(7) 0.024(7) 0.001(5) C24C 0.049(6) 0.052(7) 0.087(10) 0.029(7) -0.001(6) 0.001(5) N2 0.053(5) 0.085(8) 0.075(8) -0.009(6) 0.017(5) 0.010(5) C7 0.060(7) 0.083(10) 0.083(10) -0.009(8) 0.010(7) 0.000(6) C8 0.074(8) 0.115(12) 0.090(11) -0.022(10) 0.000(8) -0.004(8) C9 0.057(7) 0.090(11) 0.096(11) -0.013(9) 0.010(7) 0.007(7) C10 0.089(9) 0.085(11) 0.099(12) -0.006(9) 0.016(9) 0.018(8) C11 0.066(7) 0.101(11) 0.062(9) -0.025(8) 0.019(7) 0.011(7) C12 0.071(8) 0.062(9) 0.119(13) -0.015(8) 0.018(8) -0.001(6) C13 0.092(10) 0.094(11) 0.115(13) 0.014(10) 0.052(10) -0.017(8) C14 0.079(9) 0.082(11) 0.176(18) -0.012(11) 0.041(11) 0.001(8) N3 0.035(4) 0.045(5) 0.076(7) -0.006(5) 0.004(4) -0.003(4) C15 0.057(6) 0.043(7) 0.110(11) -0.004(7) 0.015(7) -0.011(5) C16 0.053(7) 0.046(8) 0.188(17) -0.042(9) -0.003(9) 0.003(6) C17 0.063(7) 0.060(8) 0.064(8) 0.011(7) 0.013(6) -0.009(6) C18 0.068(7) 0.071(9) 0.105(12) 0.018(8) 0.020(8) -0.007(6) C19 0.038(5) 0.059(8) 0.099(11) 0.015(7) -0.006(6) 0.001(5) C20 0.054(7) 0.066(9) 0.133(14) 0.018(9) -0.002(8) 0.011(6) C21 0.044(5) 0.035(6) 0.091(10) -0.001(6) 0.005(6) -0.009(4) C22 0.038(5) 0.059(8) 0.093(10) -0.002(7) 0.009(6) -0.009(5) N4 0.035(4) 0.049(6) 0.078(7) 0.001(5) 0.018(4) 0.003(4) C23 0.046(6) 0.063(8) 0.095(10) 0.010(7) 0.026(6) 0.014(5) C24 0.064(7) 0.049(8) 0.120(12) 0.010(8) 0.018(8) 0.006(6) C25 0.044(6) 0.053(8) 0.128(13) -0.001(8) 0.035(7) 0.010(5) C26 0.053(6) 0.066(9) 0.108(12) -0.010(8) -0.010(7) 0.008(6) C27 0.046(5) 0.055(7) 0.091(10) 0.003(7) 0.030(6) 0.000(5) C28 0.066(7) 0.058(8) 0.101(11) 0.016(8) 0.030(7) 0.000(6) C29 0.049(6) 0.056(8) 0.094(10) -0.002(7) 0.022(7) 0.003(5) C30 0.075(8) 0.074(10) 0.106(12) -0.011(9) 0.016(8) 0.021(7) N10 0.178(16) 0.157(16) 0.124(14) -0.007(13) 0.055(12) -0.027(14) O40 0.238(16) 0.162(14) 0.177(15) 0.017(11) -0.028(12) -0.149(13) C42 0.23(3) 0.13(2) 0.116(18) -0.011(16) 0.032(17) -0.057(19) C43 0.15(2) 0.80(8) 0.23(3) 0.25(4) 0.13(2) 0.21(3) C44 0.108(13) 0.114(16) 0.28(3) 0.040(17) 0.031(16) -0.041(12) N11 0.046(6) 0.211(17) 0.096(11) -0.051(11) -0.007(6) 0.044(8) O41 0.160(12) 0.142(13) 0.155(13) -0.045(11) -0.005(9) 0.058(10) C45 0.069(9) 0.23(2) 0.112(15) -0.003(15) 0.005(10) 0.034(12) C46 0.120(14) 0.28(3) 0.114(16) -0.051(17) 0.007(13) 0.093(16) C47 0.143(19) 0.122(19) 0.20(3) 0.041(19) -0.077(18) -0.042(15) O66 0.064(7) 0.042(7) 0.095(10) -0.003(6) -0.006(6) -0.001(5) O66A 0.059(14) 0.069(18) 0.048(16) 0.027(13) 0.012(12) 0.025(12) _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 S1B 2.381(3) . ? Ti1 S1A 2.397(3) . ? Ti1 S1C 2.403(4) . ? Ti1 S2C 2.436(3) . ? Ti1 S2B 2.439(3) . ? Ti1 S2A 2.453(3) . ? Ti2 S3A 2.380(3) . ? Ti2 S3C 2.381(4) . ? Ti2 S3B 2.407(3) . ? Ti2 S4B 2.430(3) . ? Ti2 S4A 2.446(3) . ? Ti2 S4C 2.459(4) . ? S1A C1A 1.769(11) . ? S2A C2A 1.763(11) . ? S3A C23A 1.756(11) . ? S4A C24A 1.724(11) . ? O1A C7A 1.220(14) . ? O2A C18A 1.211(14) . ? N1A C7A 1.311(14) . ? N1A C8A 1.444(14) . ? N2A C18A 1.333(15) . ? N2A C17A 1.429(15) . ? C1A C2A 1.392(15) . ? C1A C6A 1.397(16) . ? C2A C3A 1.409(15) . ? C3A C4A 1.380(16) . ? C3A C7A 1.517(16) . ? C4A C5A 1.396(18) . ? C5A C6A 1.389(17) . ? C8A C9A 1.331(19) . ? C8A C13A 1.434(18) . ? C9A C10A 1.386(17) . ? C10A C11A 1.387(19) . ? C11A C12A 1.39(2) . ? C12A C13A 1.400(16) . ? C12A C17A 1.43(2) . ? C13A C14A 1.439(18) . ? C14A C15A 1.387(17) . ? C15A C16A 1.405(17) . ? C16A C17A 1.372(19) . ? C18A C19A 1.508(16) . ? C19A C20A 1.348(17) . ? C19A C24A 1.421(14) . ? C20A C21A 1.357(19) . ? C21A C22A 1.365(16) . ? C22A C23A 1.410(15) . ? C23A C24A 1.395(16) . ? S1B C1B 1.772(12) . ? S2B C2B 1.772(9) . ? S3B C23B 1.750(11) . ? S4B C24B 1.749(10) . ? O1B C7B 1.231(13) . ? O2B C18B 1.230(14) . ? N1B C7B 1.372(13) . ? N1B C8B 1.442(12) . ? N2B C18B 1.381(15) . ? N2B C17B 1.449(13) . ? C1B C2B 1.383(14) . ? C1B C6B 1.395(14) . ? C2B C3B 1.356(14) . ? C3B C4B 1.369(13) . ? C3B C7B 1.541(14) . ? C4B C5B 1.378(14) . ? C5B C6B 1.402(15) . ? C8B C9B 1.340(13) . ? C8B C13B 1.399(14) . ? C9B C10B 1.399(14) . ? C10B C11B 1.384(13) . ? C11B C12B 1.445(13) . ? C12B C17B 1.410(14) . ? C12B C13B 1.411(14) . ? C13B C14B 1.434(13) . ? C14B C15B 1.373(14) . ? C15B C16B 1.416(14) . ? C16B C17B 1.331(13) . ? C18B C19B 1.512(14) . ? C19B C20B 1.397(14) . ? C19B C24B 1.409(15) . ? C20B C21B 1.382(14) . ? C21B C22B 1.369(15) . ? C22B C23B 1.386(14) . ? C23B C24B 1.414(13) . ? S1C C1C 1.757(10) . ? S2C C2C 1.762(10) . ? S3C C23C 1.777(12) . ? S4C C24C 1.760(12) . ? O1C C7C 1.228(11) . ? O2C C18C 1.211(12) . ? N1C C18C 1.357(13) . ? N1C C17C 1.411(12) . ? N2C C7C 1.334(12) . ? N2C C8C 1.441(13) . ? C1C C6C 1.408(14) . ? C1C C2C 1.423(12) . ? C2C C3C 1.389(13) . ? C3C C4C 1.376(15) . ? C3C C7C 1.517(14) . ? C4C C5C 1.390(14) . ? C5C C6C 1.393(15) . ? C8C C9C 1.377(15) . ? C8C C13C 1.442(14) . ? C9C C10C 1.402(14) . ? C10C C11C 1.354(14) . ? C11C C12C 1.416(14) . ? C12C C13C 1.389(14) . ? C12C C17C 1.443(13) . ? C13C C14C 1.411(13) . ? C14C C15C 1.362(13) . ? C15C C16C 1.407(14) . ? C16C C17C 1.340(13) . ? C18C C19C 1.512(15) . ? C19C C20C 1.392(15) . ? C19C C24C 1.444(16) . ? C20C C21C 1.372(15) . ? C21C C22C 1.382(16) . ? C22C C23C 1.404(16) . ? C23C C24C 1.388(15) . ? N2 C13 1.481(15) . ? N2 C11 1.510(14) . ? N2 C9 1.515(14) . ? N2 C7 1.530(14) . ? C7 C8 1.525(16) . ? C9 C10 1.519(16) . ? C11 C12 1.549(15) . ? C13 C14 1.542(17) . ? N3 C17 1.494(13) . ? N3 C15 1.511(13) . ? N3 C19 1.512(12) . ? N3 C21 1.528(11) . ? C15 C16 1.532(15) . ? C17 C18 1.555(14) . ? C19 C20 1.551(15) . ? C21 C22 1.484(15) . ? N4 C27 1.494(12) . ? N4 C29 1.516(13) . ? N4 C23 1.519(12) . ? N4 C25 1.528(14) . ? C23 C24 1.506(14) . ? C25 C26 1.496(16) . ? C27 C28 1.515(14) . ? C29 C30 1.526(16) . ? N10 C42 1.42(2) . ? N10 C44 1.51(2) . ? N10 C43 1.55(3) . ? O40 C42 1.12(2) . ? N11 C46 1.37(2) . ? N11 C45 1.45(2) . ? N11 C47 1.48(2) . ? O41 C47 1.19(2) . ? N51 C53A 1.39(4) . ? N51 C53 1.39(3) . ? N51 C55A 1.40(4) . ? N51 C57A 1.43(4) . ? N51 C57 1.47(3) . ? N51 C51 1.49(3) . ? N51 C51A 1.65(4) . ? N51 C55 1.66(3) . ? C51 C52 1.52(3) . ? C51A C52A 1.40(5) . ? C53 C54 1.60(3) . ? C53A C54 1.60(4) . ? C55 C56 1.39(3) . ? C55A C56 1.55(4) . ? C57 C58 1.46(3) . ? C57A C58 1.67(4) . ? 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 S1B Ti1 S1A 89.94(11) . . ? S1B Ti1 S1C 84.29(11) . . ? S1A Ti1 S1C 86.72(12) . . ? S1B Ti1 S2C 112.36(12) . . ? S1A Ti1 S2C 153.39(12) . . ? S1C Ti1 S2C 81.52(12) . . ? S1B Ti1 S2B 82.11(10) . . ? S1A Ti1 S2B 109.87(14) . . ? S1C Ti1 S2B 158.43(13) . . ? S2C Ti1 S2B 88.26(11) . . ? S1B Ti1 S2A 159.06(15) . . ? S1A Ti1 S2A 80.70(11) . . ? S1C Ti1 S2A 113.57(12) . . ? S2C Ti1 S2A 82.28(11) . . ? S2B Ti1 S2A 83.54(11) . . ? S3A Ti2 S3C 87.47(13) . . ? S3A Ti2 S3B 82.43(11) . . ? S3C Ti2 S3B 84.71(12) . . ? S3A Ti2 S4B 117.30(15) . . ? S3C Ti2 S4B 149.13(13) . . ? S3B Ti2 S4B 81.00(11) . . ? S3A Ti2 S4A 81.12(11) . . ? S3C Ti2 S4A 115.68(13) . . ? S3B Ti2 S4A 153.00(15) . . ? S4B Ti2 S4A 87.73(12) . . ? S3A Ti2 S4C 154.29(15) . . ? S3C Ti2 S4C 80.12(13) . . ? S3B Ti2 S4C 118.32(12) . . ? S4B Ti2 S4C 82.83(13) . . ? S4A Ti2 S4C 84.12(13) . . ? C1A S1A Ti1 108.8(4) . . ? C2A S2A Ti1 110.5(4) . . ? C23A S3A Ti2 109.2(4) . . ? C24A S4A Ti2 109.0(4) . . ? C7A N1A C8A 126.2(10) . . ? C18A N2A C17A 126.9(13) . . ? C2A C1A C6A 120.3(11) . . ? C2A C1A S1A 122.7(8) . . ? C6A C1A S1A 116.9(10) . . ? C1A C2A C3A 119.9(10) . . ? C1A C2A S2A 115.7(9) . . ? C3A C2A S2A 123.8(9) . . ? C4A C3A C2A 118.9(12) . . ? C4A C3A C7A 113.9(11) . . ? C2A C3A C7A 127.2(11) . . ? C3A C4A C5A 121.5(12) . . ? C6A C5A C4A 119.5(12) . . ? C5A C6A C1A 119.8(13) . . ? O1A C7A N1A 119.1(13) . . ? O1A C7A C3A 121.8(12) . . ? N1A C7A C3A 119.2(11) . . ? C9A C8A C13A 120.8(13) . . ? C9A C8A N1A 122.4(15) . . ? C13A C8A N1A 116.7(13) . . ? C8A C9A C10A 122.5(17) . . ? C9A C10A C11A 118.4(16) . . ? C10A C11A C12A 120.5(14) . . ? C11A C12A C13A 120.7(15) . . ? C11A C12A C17A 121.3(14) . . ? C13A C12A C17A 117.9(16) . . ? C12A C13A C8A 116.9(15) . . ? C12A C13A C14A 119.5(15) . . ? C8A C13A C14A 123.6(13) . . ? C15A C14A C13A 122.0(13) . . ? C14A C15A C16A 117.2(15) . . ? C17A C16A C15A 122.5(15) . . ? C16A C17A N2A 119.1(17) . . ? C16A C17A C12A 120.9(14) . . ? N2A C17A C12A 119.9(16) . . ? O2A C18A N2A 122.3(13) . . ? O2A C18A C19A 119.9(12) . . ? N2A C18A C19A 117.3(12) . . ? C20A C19A C24A 121.5(12) . . ? C20A C19A C18A 116.7(11) . . ? C24A C19A C18A 121.8(11) . . ? C19A C20A C21A 121.4(12) . . ? C20A C21A C22A 119.6(13) . . ? C21A C22A C23A 120.7(13) . . ? C24A C23A C22A 119.6(10) . . ? C24A C23A S3A 120.3(8) . . ? C22A C23A S3A 120.1(10) . . ? C23A C24A C19A 116.5(11) . . ? C23A C24A S4A 119.3(8) . . ? C19A C24A S4A 124.2(10) . . ? C1B S1B Ti1 107.5(4) . . ? C2B S2B Ti1 108.0(4) . . ? C23B S3B Ti2 108.4(3) . . ? C24B S4B Ti2 107.3(4) . . ? C7B N1B C8B 128.0(10) . . ? C18B N2B C17B 123.1(10) . . ? C2B C1B C6B 118.4(10) . . ? C2B C1B S1B 122.1(8) . . ? C6B C1B S1B 119.4(9) . . ? C3B C2B C1B 120.3(9) . . ? C3B C2B S2B 121.5(8) . . ? C1B C2B S2B 118.2(8) . . ? C2B C3B C4B 122.5(10) . . ? C2B C3B C7B 120.5(9) . . ? C4B C3B C7B 117.0(10) . . ? C3B C4B C5B 118.5(11) . . ? C4B C5B C6B 120.0(10) . . ? C1B C6B C5B 120.1(10) . . ? O1B C7B N1B 124.0(11) . . ? O1B C7B C3B 121.6(10) . . ? N1B C7B C3B 114.4(10) . . ? C9B C8B C13B 121.8(10) . . ? C9B C8B N1B 117.6(9) . . ? C13B C8B N1B 120.4(9) . . ? C8B C9B C10B 121.5(10) . . ? C11B C10B C9B 120.1(10) . . ? C10B C11B C12B 118.2(10) . . ? C17B C12B C13B 118.8(9) . . ? C17B C12B C11B 121.0(10) . . ? C13B C12B C11B 120.2(9) . . ? C8B C13B C12B 117.7(9) . . ? C8B C13B C14B 123.5(11) . . ? C12B C13B C14B 118.7(10) . . ? C15B C14B C13B 118.9(11) . . ? C14B C15B C16B 121.5(9) . . ? C17B C16B C15B 119.2(10) . . ? C16B C17B C12B 122.4(11) . . ? C16B C17B N2B 118.3(10) . . ? C12B C17B N2B 119.3(9) . . ? O2B C18B N2B 123.0(11) . . ? O2B C18B C19B 121.1(12) . . ? N2B C18B C19B 115.8(11) . . ? C20B C19B C24B 119.1(10) . . ? C20B C19B C18B 118.7(11) . . ? C24B C19B C18B 122.1(10) . . ? C21B C20B C19B 120.5(11) . . ? C22B C21B C20B 120.4(11) . . ? C21B C22B C23B 121.2(10) . . ? C22B C23B C24B 119.2(10) . . ? C22B C23B S3B 122.7(8) . . ? C24B C23B S3B 117.9(8) . . ? C19B C24B C23B 119.6(10) . . ? C19B C24B S4B 119.5(8) . . ? C23B C24B S4B 120.9(9) . . ? C1C S1C Ti1 109.3(4) . . ? C2C S2C Ti1 108.9(3) . . ? C23C S3C Ti2 109.6(4) . . ? C24C S4C Ti2 109.7(5) . . ? C18C N1C C17C 128.8(10) . . ? C7C N2C C8C 122.1(8) . . ? C6C C1C C2C 119.6(10) . . ? C6C C1C S1C 120.7(8) . . ? C2C C1C S1C 119.7(8) . . ? C3C C2C C1C 118.6(9) . . ? C3C C2C S2C 122.3(8) . . ? C1C C2C S2C 119.1(8) . . ? C4C C3C C2C 121.1(10) . . ? C4C C3C C7C 118.3(10) . . ? C2C C3C C7C 120.6(10) . . ? C3C C4C C5C 121.0(12) . . ? C4C C5C C6C 119.4(12) . . ? C5C C6C C1C 120.1(11) . . ? O1C C7C N2C 124.2(10) . . ? O1C C7C C3C 120.9(9) . . ? N2C C7C C3C 114.9(9) . . ? C9C C8C N2C 118.1(9) . . ? C9C C8C C13C 119.5(10) . . ? N2C C8C C13C 122.5(10) . . ? C8C C9C C10C 120.8(10) . . ? C11C C10C C9C 120.0(10) . . ? C10C C11C C12C 121.1(11) . . ? C13C C12C C11C 119.8(9) . . ? C13C C12C C17C 118.1(9) . . ? C11C C12C C17C 122.1(10) . . ? C12C C13C C14C 120.7(9) . . ? C12C C13C C8C 118.6(9) . . ? C14C C13C C8C 120.7(10) . . ? C15C C14C C13C 119.8(10) . . ? C14C C15C C16C 119.9(10) . . ? C17C C16C C15C 121.6(10) . . ? C16C C17C N1C 124.1(10) . . ? C16C C17C C12C 119.9(10) . . ? N1C C17C C12C 116.0(9) . . ? O2C C18C N1C 122.2(10) . . ? O2C C18C C19C 121.9(10) . . ? N1C C18C C19C 115.9(10) . . ? C20C C19C C24C 118.0(11) . . ? C20C C19C C18C 113.6(11) . . ? C24C C19C C18C 128.4(11) . . ? C21C C20C C19C 123.2(12) . . ? C20C C21C C22C 118.6(13) . . ? C21C C22C C23C 120.8(12) . . ? C24C C23C C22C 120.9(12) . . ? C24C C23C S3C 120.5(10) . . ? C22C C23C S3C 118.6(9) . . ? C23C C24C C19C 118.4(11) . . ? C23C C24C S4C 117.8(10) . . ? C19C C24C S4C 123.8(9) . . ? C13 N2 C11 113.7(11) . . ? C13 N2 C9 109.0(9) . . ? C11 N2 C9 107.0(10) . . ? C13 N2 C7 107.3(10) . . ? C11 N2 C7 109.4(9) . . ? C9 N2 C7 110.5(10) . . ? C8 C7 N2 116.5(10) . . ? N2 C9 C10 116.5(10) . . ? N2 C11 C12 116.5(11) . . ? N2 C13 C14 116.9(13) . . ? C17 N3 C15 110.6(9) . . ? C17 N3 C19 113.0(8) . . ? C15 N3 C19 104.8(9) . . ? C17 N3 C21 107.2(8) . . ? C15 N3 C21 110.1(8) . . ? C19 N3 C21 111.1(8) . . ? N3 C15 C16 114.6(10) . . ? N3 C17 C18 115.6(10) . . ? N3 C19 C20 113.0(10) . . ? C22 C21 N3 116.9(9) . . ? C27 N4 C29 112.9(9) . . ? C27 N4 C23 104.9(7) . . ? C29 N4 C23 109.6(8) . . ? C27 N4 C25 111.9(8) . . ? C29 N4 C25 107.2(8) . . ? C23 N4 C25 110.2(9) . . ? C24 C23 N4 115.8(8) . . ? C26 C25 N4 117.0(9) . . ? N4 C27 C28 114.9(8) . . ? N4 C29 C30 115.3(9) . . ? C42 N10 C44 122.0(19) . . ? C42 N10 C43 121(3) . . ? C44 N10 C43 117(2) . . ? O40 C42 N10 132(3) . . ? C46 N11 C45 121.5(19) . . ? C46 N11 C47 118.2(18) . . ? C45 N11 C47 120.2(18) . . ? O41 C47 N11 127(3) . . ? C53A N51 C53 74(2) . . ? C53A N51 C55A 122(3) . . ? C53 N51 C55A 83(2) . . ? C53A N51 C57A 111(3) . . ? C53 N51 C57A 154(2) . . ? C55A N51 C57A 113(3) . . ? C53A N51 C57 172(3) . . ? C53 N51 C57 112.2(19) . . ? C55A N51 C57 65(2) . . ? C57A N51 C57 61(2) . . ? C53A N51 C51 64(2) . . ? C53 N51 C51 119(2) . . ? C55A N51 C51 157(3) . . ? C57A N51 C51 50.3(19) . . ? C57 N51 C51 108.0(19) . . ? C53A N51 C51A 104(3) . . ? C53 N51 C51A 53.7(18) . . ? C55A N51 C51A 104(3) . . ? C57A N51 C51A 101(3) . . ? C57 N51 C51A 76.9(19) . . ? C51 N51 C51A 95(2) . . ? C53A N51 C55 75(2) . . ? C53 N51 C55 110.3(18) . . ? C55A N51 C55 65(2) . . ? C57A N51 C55 96(2) . . ? C57 N51 C55 107.1(16) . . ? C51 N51 C55 99.4(16) . . ? C51A N51 C55 163(2) . . ? N51 C51 C52 112(2) . . ? C52A C51A N51 123(4) . . ? N51 C53 C54 110.0(19) . . ? N51 C53A C54 110(3) . . ? C53A C54 C53 62.9(19) . . ? C56 C55 N51 110.4(19) . . ? N51 C55A C56 117(3) . . ? C55 C56 C55A 68(2) . . ? C58 C57 N51 123(2) . . ? N51 C57A C58 112(3) . . ? C57 C58 C57A 56.1(18) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.267 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.133 # Attachment '[Ph4As]4[Ti2_B_3].cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 674838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C176 H142 As4 N6 O8 S12 Ti2' _chemical_formula_weight 3249.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 '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 19.4830(8) _cell_length_b 13.8938(6) _cell_length_c 28.3429(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.625(2) _cell_angle_gamma 90.00 _cell_volume 7423.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 3.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2790 _exptl_absorpt_correction_T_max 0.8256 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports Maximum and minimum effective transmission: 1.000000 0.577419 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'goebel mirror' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40787 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 65.00 _reflns_number_total 12508 _reflns_number_gt 7902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _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^)+(0.0977P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12508 _refine_ls_number_parameters 939 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _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 0.09241(5) 0.94710(7) 0.29715(3) 0.0235(2) Uani 1 1 d . . . S1 S 0.14085(7) 0.81900(10) 0.25733(5) 0.0318(3) Uani 1 1 d . . . S2 S 0.06041(7) 0.81073(9) 0.34038(5) 0.0303(3) Uani 1 1 d . . . S3 S 0.18403(7) 1.04886(10) 0.27947(5) 0.0319(3) Uani 1 1 d . . . S4 S 0.15548(7) 0.99058(9) 0.37893(5) 0.0261(3) Uani 1 1 d . . . S5 S 0.00509(7) 0.96618(10) 0.22015(5) 0.0300(3) Uani 1 1 d . . . S6 S 0.00950(6) 1.05155(9) 0.32185(4) 0.0251(3) Uani 1 1 d . . . N1 N 0.0884(3) 0.6841(3) 0.43085(16) 0.0358(12) Uani 1 1 d . . . H1 H 0.1002 0.7390 0.4196 0.043 Uiso 1 1 calc R . . N2 N 0.1098(3) 1.1119(4) 0.45430(18) 0.0598(16) Uani 1 1 d . . . H2 H 0.0968 1.0758 0.4280 0.072 Uiso 1 1 calc R . . N3 N -0.1053(2) 1.1291(3) 0.36660(16) 0.0334(11) Uani 1 1 d . . . H3 H -0.0731 1.0848 0.3666 0.040 Uiso 1 1 calc R . . O1 O 0.0773(3) 0.5254(3) 0.41604(16) 0.0568(13) Uani 1 1 d . . . O2 O 0.1830(2) 1.2335(3) 0.48642(15) 0.0583(13) Uani 1 1 d . . . O3 O -0.17136(19) 1.2482(3) 0.32413(13) 0.0351(9) Uani 1 1 d . . . C1 C 0.1353(3) 0.7105(4) 0.28812(18) 0.0254(12) Uani 1 1 d . . . C2 C 0.1052(2) 0.7078(4) 0.32859(18) 0.0248(12) Uani 1 1 d . . . C3 C 0.1082(3) 0.6208(4) 0.35503(18) 0.0265(12) Uani 1 1 d . . . C4 C 0.1359(3) 0.5388(4) 0.3382(2) 0.0314(13) Uani 1 1 d . . . H4 H 0.1379 0.4801 0.3557 0.038 Uiso 1 1 calc R . . C5 C 0.1607(3) 0.5411(4) 0.2965(2) 0.0366(14) Uani 1 1 d . . . H5 H 0.1770 0.4837 0.2848 0.044 Uiso 1 1 calc R . . C6 C 0.1618(3) 0.6265(4) 0.27213(19) 0.0327(13) Uani 1 1 d . . . H6 H 0.1805 0.6283 0.2443 0.039 Uiso 1 1 calc R . . C7 C 0.0878(3) 0.6074(4) 0.4023(2) 0.0325(13) Uani 1 1 d . . . C8 C 0.0724(3) 0.6886(4) 0.4770(2) 0.0412(15) Uani 1 1 d . . . C9 C 0.0283(3) 0.6305(4) 0.4916(2) 0.0379(14) Uani 1 1 d . . . H9 H 0.0099 0.5768 0.4716 0.045 Uiso 1 1 calc R . . C10 C 0.0070(3) 0.6434(4) 0.5349(2) 0.0396(15) Uani 1 1 d . . . H10 H -0.0272 0.6018 0.5427 0.047 Uiso 1 1 calc R . . C11 C 0.0365(3) 0.7171(5) 0.5659(2) 0.0481(17) Uani 1 1 d . . . H11 H 0.0204 0.7281 0.5944 0.058 Uiso 1 1 calc R . . C12 C 0.0908(3) 0.7773(4) 0.5560(2) 0.0414(15) Uani 1 1 d . . . C13 C 0.1112(3) 0.7613(4) 0.5116(2) 0.0379(14) Uani 1 1 d . . . C14 C 0.1646(4) 0.8221(5) 0.5013(3) 0.0545(18) Uani 1 1 d . . . H14 H 0.1784 0.8129 0.4718 0.065 Uiso 1 1 calc R . . C15 C 0.1955(3) 0.8906(6) 0.5315(2) 0.065(2) Uani 1 1 d . . . H15 H 0.2303 0.9305 0.5232 0.078 Uiso 1 1 calc R . . C16 C 0.1988(2) 1.1325(4) 0.32734(19) 0.0273(12) Uani 1 1 d . . . C17 C 0.1816(2) 1.1105(4) 0.37176(19) 0.0281(12) Uani 1 1 d . . . C18 C 0.1867(3) 1.1827(4) 0.4075(2) 0.0329(13) Uani 1 1 d . . . C19 C 0.2132(3) 1.2718(4) 0.3995(2) 0.0420(15) Uani 1 1 d . . . H19 H 0.2171 1.3207 0.4234 0.050 Uiso 1 1 calc R . . C20 C 0.2343(3) 1.2915(4) 0.3574(2) 0.0443(16) Uani 1 1 d . . . H20 H 0.2541 1.3525 0.3533 0.053 Uiso 1 1 calc R . . C21 C 0.2265(3) 1.2227(4) 0.3214(2) 0.0364(14) Uani 1 1 d . . . H21 H 0.2402 1.2370 0.2923 0.044 Uiso 1 1 calc R . . C22 C 0.1613(3) 1.1758(4) 0.4539(2) 0.0374(14) Uani 1 1 d . . . C23 C 0.0719(4) 1.0932(6) 0.4920(3) 0.064(2) Uani 1 1 d . . . C24 C 0.0738(3) 1.1486(5) 0.5276(2) 0.0516(17) Uani 1 1 d . . . H24 H 0.1037 1.2036 0.5319 0.062 Uiso 1 1 calc R . . C25 C 0.0321(4) 1.1303(5) 0.5615(2) 0.0516(18) Uani 1 1 d . . . H25 H 0.0346 1.1733 0.5880 0.062 Uiso 1 1 calc R . . C26 C 0.0213(4) 1.0096(6) 0.4827(3) 0.067(2) Uani 1 1 d . . . C27 C 0.0081(5) 0.9422(6) 0.4432(3) 0.085(3) Uani 1 1 d . . . H27 H 0.0318 0.9531 0.4182 0.102 Uiso 1 1 calc R . . C28 C -0.0619(3) 1.0463(4) 0.22664(19) 0.0280(12) Uani 1 1 d . . . C29 C -0.0629(2) 1.0814(3) 0.27336(18) 0.0231(11) Uani 1 1 d . . . C30 C -0.1194(3) 1.1408(4) 0.27791(18) 0.0248(12) Uani 1 1 d . . . C31 C -0.1715(3) 1.1659(4) 0.2362(2) 0.0326(13) Uani 1 1 d . . . H31 H -0.2090 1.2076 0.2389 0.039 Uiso 1 1 calc R . . C32 C -0.1695(3) 1.1311(4) 0.19090(19) 0.0344(13) Uani 1 1 d . . . H32 H -0.2058 1.1483 0.1629 0.041 Uiso 1 1 calc R . . C33 C -0.1153(3) 1.0717(4) 0.18619(19) 0.0320(13) Uani 1 1 d . . . H33 H -0.1144 1.0477 0.1549 0.038 Uiso 1 1 calc R . . C34 C -0.1329(3) 1.1781(4) 0.32466(19) 0.0264(12) Uani 1 1 d . . . C35 C -0.1261(3) 1.1461(5) 0.4112(2) 0.0390(15) Uani 1 1 d . . . C36 C -0.1770(3) 1.0950(5) 0.4238(2) 0.060(2) Uani 1 1 d . . . H36 H -0.2016 1.0473 0.4019 0.071 Uiso 1 1 calc R . . As1 As 0.63894(3) 0.98280(4) 0.23244(2) 0.02787(17) Uani 1 1 d . . . C41 C 0.7302(3) 0.9321(4) 0.26423(19) 0.0276(12) Uani 1 1 d . . . C42 C 0.7800(3) 0.9115(4) 0.2390(2) 0.0324(13) Uani 1 1 d . . . H42 H 0.7688 0.9192 0.2046 0.039 Uiso 1 1 calc R . . C43 C 0.8470(3) 0.8793(4) 0.2640(2) 0.0344(14) Uani 1 1 d . . . H43 H 0.8816 0.8649 0.2467 0.041 Uiso 1 1 calc R . . C44 C 0.8626(3) 0.8685(4) 0.3131(2) 0.0392(15) Uani 1 1 d . . . H44 H 0.9087 0.8477 0.3301 0.047 Uiso 1 1 calc R . . C45 C 0.8129(3) 0.8870(4) 0.3389(2) 0.0432(15) Uani 1 1 d . . . H45 H 0.8241 0.8780 0.3733 0.052 Uiso 1 1 calc R . . C46 C 0.7455(3) 0.9193(4) 0.3138(2) 0.0380(14) Uani 1 1 d . . . H46 H 0.7105 0.9323 0.3309 0.046 Uiso 1 1 calc R . . C47 C 0.6212(3) 1.0888(4) 0.27070(19) 0.0297(13) Uani 1 1 d . . . C48 C 0.5507(3) 1.1163(4) 0.2656(2) 0.0419(15) Uani 1 1 d . . . H48 H 0.5130 1.0824 0.2443 0.050 Uiso 1 1 calc R . . C49 C 0.5371(3) 1.1942(5) 0.2923(2) 0.0494(17) Uani 1 1 d . . . H49 H 0.4897 1.2162 0.2882 0.059 Uiso 1 1 calc R . . C50 C 0.5913(3) 1.2397(4) 0.3247(2) 0.0461(16) Uani 1 1 d . . . H50 H 0.5809 1.2908 0.3441 0.055 Uiso 1 1 calc R . . C51 C 0.6611(3) 1.2125(4) 0.3297(2) 0.0441(16) Uani 1 1 d . . . H51 H 0.6986 1.2451 0.3519 0.053 Uiso 1 1 calc R . . C52 C 0.6756(3) 1.1375(4) 0.3019(2) 0.0341(13) Uani 1 1 d . . . H52 H 0.7233 1.1193 0.3044 0.041 Uiso 1 1 calc R . . C53 C 0.5641(3) 0.8923(4) 0.23015(19) 0.0272(12) Uani 1 1 d . . . C54 C 0.5134(3) 0.8745(4) 0.1882(2) 0.0329(13) Uani 1 1 d . . . H54 H 0.5150 0.9056 0.1587 0.039 Uiso 1 1 calc R . . C55 C 0.4596(3) 0.8106(4) 0.1893(2) 0.0385(14) Uani 1 1 d . . . H55 H 0.4249 0.7959 0.1601 0.046 Uiso 1 1 calc R . . C56 C 0.4556(3) 0.7677(4) 0.2323(2) 0.0393(15) Uani 1 1 d . . . H56 H 0.4178 0.7249 0.2329 0.047 Uiso 1 1 calc R . . C57 C 0.5062(3) 0.7873(4) 0.2740(2) 0.0423(15) Uani 1 1 d . . . H57 H 0.5035 0.7579 0.3037 0.051 Uiso 1 1 calc R . . C58 C 0.5614(3) 0.8490(4) 0.2737(2) 0.0391(15) Uani 1 1 d . . . H58 H 0.5969 0.8617 0.3028 0.047 Uiso 1 1 calc R . . C59 C 0.6395(3) 1.0263(4) 0.1688(2) 0.0317(13) Uani 1 1 d . . . C60 C 0.6480(3) 0.9616(4) 0.1336(2) 0.0394(15) Uani 1 1 d . . . H60 H 0.6513 0.8945 0.1404 0.047 Uiso 1 1 calc R . . C61 C 0.6517(3) 0.9957(5) 0.0885(2) 0.0471(17) Uani 1 1 d . . . H61 H 0.6581 0.9518 0.0643 0.057 Uiso 1 1 calc R . . C62 C 0.6462(3) 1.0912(5) 0.0784(2) 0.0449(16) Uani 1 1 d . . . H62 H 0.6492 1.1140 0.0474 0.054 Uiso 1 1 calc R . . C63 C 0.6362(4) 1.1544(4) 0.1128(2) 0.0486(17) Uani 1 1 d . . . H63 H 0.6318 1.2211 0.1052 0.058 Uiso 1 1 calc R . . C64 C 0.6326(3) 1.1237(4) 0.1582(2) 0.0412(15) Uani 1 1 d . . . H64 H 0.6254 1.1684 0.1819 0.049 Uiso 1 1 calc R . . As2 As 0.93028(3) 0.17420(5) 0.03669(2) 0.03788(19) Uani 1 1 d . . . C71 C 0.9022(3) 0.2871(4) 0.0668(2) 0.0370(14) Uani 1 1 d . . . C72 C 0.8313(3) 0.3074(5) 0.0605(2) 0.0471(16) Uani 1 1 d . . . H72 H 0.7961 0.2616 0.0460 0.056 Uiso 1 1 calc R . . C73 C 0.8120(4) 0.3957(5) 0.0757(2) 0.0536(18) Uani 1 1 d . . . H73 H 0.7634 0.4121 0.0705 0.064 Uiso 1 1 calc R . . C74 C 0.8642(4) 0.4601(5) 0.0987(3) 0.0567(19) Uani 1 1 d . . . H74 H 0.8511 0.5199 0.1101 0.068 Uiso 1 1 calc R . . C75 C 0.9347(4) 0.4381(5) 0.1051(2) 0.0546(18) Uani 1 1 d . . . H75 H 0.9698 0.4834 0.1205 0.066 Uiso 1 1 calc R . . C76 C 0.9554(4) 0.3511(4) 0.0894(2) 0.0472(16) Uani 1 1 d . . . H76 H 1.0041 0.3356 0.0939 0.057 Uiso 1 1 calc R . . C77 C 1.0256(3) 0.1423(4) 0.0711(2) 0.0406(15) Uani 1 1 d . . . C78 C 1.0790(3) 0.1477(5) 0.0485(2) 0.0562(19) Uani 1 1 d . . . H78 H 1.0696 0.1620 0.0146 0.067 Uiso 1 1 calc R . . C79 C 1.1484(4) 0.1318(6) 0.0762(3) 0.072(2) Uani 1 1 d . . . H79 H 1.1865 0.1355 0.0610 0.086 Uiso 1 1 calc R . . C80 C 1.1621(4) 0.1108(6) 0.1251(3) 0.073(2) Uani 1 1 d . . . H80 H 1.2095 0.1002 0.1434 0.088 Uiso 1 1 calc R . . C81 C 1.1075(4) 0.1051(5) 0.1476(3) 0.062(2) Uani 1 1 d . . . H81 H 1.1172 0.0905 0.1814 0.074 Uiso 1 1 calc R . . C82 C 1.0385(3) 0.1208(5) 0.1211(2) 0.0483(17) Uani 1 1 d . . . H82 H 1.0005 0.1172 0.1364 0.058 Uiso 1 1 calc R . . C83 C 0.8679(3) 0.0663(4) 0.0353(2) 0.0409(15) Uani 1 1 d . . . C84 C 0.8940(4) -0.0194(5) 0.0603(2) 0.0485(17) Uani 1 1 d . . . H84 H 0.9417 -0.0242 0.0793 0.058 Uiso 1 1 calc R . . C85 C 0.8467(4) -0.0977(5) 0.0559(3) 0.0584(19) Uani 1 1 d . . . H85 H 0.8620 -0.1566 0.0723 0.070 Uiso 1 1 calc R . . C86 C 0.7786(4) -0.0884(5) 0.0280(3) 0.0592(19) Uani 1 1 d . . . H86 H 0.7469 -0.1412 0.0255 0.071 Uiso 1 1 calc R . . C87 C 0.7553(4) -0.0058(5) 0.0038(3) 0.0550(18) Uani 1 1 d . . . H87 H 0.7079 -0.0018 -0.0156 0.066 Uiso 1 1 calc R . . C88 C 0.7994(3) 0.0721(5) 0.0072(2) 0.0494(17) Uani 1 1 d . . . H88 H 0.7828 0.1297 -0.0099 0.059 Uiso 1 1 calc R . . C89 C 0.9261(3) 0.2093(5) -0.0299(2) 0.0424(15) Uani 1 1 d . . . C90 C 0.9297(3) 0.1386(6) -0.0629(2) 0.0569(19) Uani 1 1 d . . . H90 H 0.9348 0.0730 -0.0533 0.068 Uiso 1 1 calc R . . C91 C 0.9257(3) 0.1656(6) -0.1112(2) 0.060(2) Uani 1 1 d . . . H91 H 0.9299 0.1184 -0.1345 0.073 Uiso 1 1 calc R . . C92 C 0.9155(4) 0.2608(6) -0.1247(3) 0.067(2) Uani 1 1 d . . . H92 H 0.9122 0.2785 -0.1576 0.080 Uiso 1 1 calc R . . C93 C 0.9099(4) 0.3320(6) -0.0909(3) 0.069(2) Uani 1 1 d . . . H93 H 0.9024 0.3975 -0.1006 0.083 Uiso 1 1 calc R . . C94 C 0.9156(4) 0.3045(5) -0.0429(3) 0.065(2) Uani 1 1 d . . . H94 H 0.9122 0.3514 -0.0191 0.078 Uiso 1 1 calc R . . O4 O 0.1239(3) 0.3971(4) 0.0954(2) 0.0885(18) Uani 1 1 d . . . C95 C 0.1778(4) 0.3895(8) 0.1410(3) 0.104(3) Uani 1 1 d . . . H95A H 0.2067 0.4490 0.1465 0.125 Uiso 1 1 calc R . . H95B H 0.2096 0.3347 0.1394 0.125 Uiso 1 1 calc R . . C96 C 0.1440(4) 0.3750(7) 0.1824(3) 0.104(3) Uani 1 1 d . . . H96A H 0.1119 0.4288 0.1835 0.156 Uiso 1 1 calc R . . H96B H 0.1808 0.3720 0.2131 0.156 Uiso 1 1 calc R . . H96C H 0.1170 0.3147 0.1776 0.156 Uiso 1 1 calc R . . C97 C 0.1543(4) 0.4107(8) 0.0552(3) 0.098(3) Uani 1 1 d . . . H97A H 0.1870 0.3570 0.0535 0.118 Uiso 1 1 calc R . . H97B H 0.1816 0.4715 0.0592 0.118 Uiso 1 1 calc R . . C98 C 0.0967(5) 0.4144(7) 0.0097(3) 0.118(4) Uani 1 1 d . . . H98A H 0.0713 0.3528 0.0050 0.177 Uiso 1 1 calc R . . H98B H 0.1170 0.4265 -0.0180 0.177 Uiso 1 1 calc R . . H98C H 0.0636 0.4662 0.0120 0.177 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 0.0261(5) 0.0267(5) 0.0204(5) -0.0013(4) 0.0108(4) 0.0013(4) S1 0.0414(8) 0.0317(8) 0.0288(8) -0.0011(6) 0.0212(6) 0.0050(6) S2 0.0390(8) 0.0252(7) 0.0338(8) -0.0010(6) 0.0223(6) 0.0029(6) S3 0.0314(7) 0.0402(8) 0.0275(8) -0.0007(6) 0.0140(6) -0.0048(6) S4 0.0260(7) 0.0310(7) 0.0225(7) -0.0005(6) 0.0081(5) 0.0017(6) S5 0.0325(7) 0.0387(8) 0.0208(7) -0.0060(6) 0.0101(6) 0.0015(6) S6 0.0261(7) 0.0293(7) 0.0198(7) -0.0038(5) 0.0057(5) 0.0025(6) N1 0.066(3) 0.022(2) 0.027(3) -0.003(2) 0.025(2) -0.010(2) N2 0.085(4) 0.067(4) 0.035(3) -0.027(3) 0.030(3) -0.025(3) N3 0.039(3) 0.035(3) 0.027(3) -0.002(2) 0.010(2) 0.010(2) O1 0.106(4) 0.027(2) 0.052(3) -0.005(2) 0.047(3) -0.009(2) O2 0.052(3) 0.078(3) 0.042(3) -0.032(3) 0.008(2) -0.016(2) O3 0.040(2) 0.034(2) 0.033(2) -0.0008(18) 0.0123(18) 0.0065(19) C1 0.025(3) 0.030(3) 0.021(3) -0.003(2) 0.005(2) 0.003(2) C2 0.022(3) 0.030(3) 0.023(3) -0.007(2) 0.007(2) -0.002(2) C3 0.030(3) 0.027(3) 0.023(3) -0.005(2) 0.006(2) -0.002(2) C4 0.035(3) 0.026(3) 0.034(3) -0.001(2) 0.010(3) 0.002(2) C5 0.041(3) 0.036(4) 0.033(4) -0.011(3) 0.010(3) 0.010(3) C6 0.036(3) 0.040(3) 0.024(3) -0.003(3) 0.011(2) 0.006(3) C7 0.038(3) 0.030(3) 0.030(3) 0.002(3) 0.010(3) -0.001(3) C8 0.065(4) 0.028(3) 0.038(4) -0.003(3) 0.028(3) -0.004(3) C9 0.055(4) 0.031(3) 0.029(3) -0.003(3) 0.013(3) -0.012(3) C10 0.043(4) 0.049(4) 0.025(3) 0.008(3) 0.005(3) -0.026(3) C11 0.053(4) 0.058(4) 0.038(4) 0.014(3) 0.022(3) 0.013(3) C12 0.049(4) 0.041(4) 0.036(4) 0.008(3) 0.015(3) 0.004(3) C13 0.037(3) 0.041(4) 0.037(4) 0.005(3) 0.012(3) 0.004(3) C14 0.061(5) 0.049(4) 0.064(5) -0.005(4) 0.035(4) -0.002(4) C15 0.051(4) 0.098(6) 0.059(5) -0.053(4) 0.038(4) -0.038(4) C16 0.017(3) 0.032(3) 0.032(3) 0.002(3) 0.005(2) 0.000(2) C17 0.017(3) 0.033(3) 0.034(3) -0.002(3) 0.004(2) 0.001(2) C18 0.022(3) 0.036(3) 0.035(4) -0.006(3) -0.003(2) 0.002(2) C19 0.035(3) 0.037(4) 0.048(4) -0.010(3) -0.002(3) -0.003(3) C20 0.026(3) 0.032(3) 0.067(5) -0.001(3) -0.004(3) -0.005(3) C21 0.024(3) 0.043(4) 0.042(4) 0.008(3) 0.008(3) -0.004(3) C22 0.032(3) 0.051(4) 0.024(3) -0.014(3) -0.005(2) 0.001(3) C23 0.061(5) 0.084(6) 0.051(5) -0.037(4) 0.023(4) -0.008(4) C24 0.049(4) 0.053(4) 0.052(5) -0.003(4) 0.010(3) -0.004(3) C25 0.087(5) 0.044(4) 0.022(4) -0.006(3) 0.009(3) -0.025(4) C26 0.071(5) 0.075(5) 0.059(5) 0.012(4) 0.026(4) 0.029(4) C27 0.148(9) 0.071(6) 0.030(5) -0.006(4) 0.011(5) 0.010(6) C28 0.031(3) 0.029(3) 0.024(3) -0.001(2) 0.009(2) -0.004(2) C29 0.022(3) 0.021(3) 0.027(3) -0.003(2) 0.008(2) -0.005(2) C30 0.023(3) 0.026(3) 0.025(3) -0.006(2) 0.004(2) -0.007(2) C31 0.031(3) 0.031(3) 0.036(4) -0.001(3) 0.010(3) 0.001(2) C32 0.034(3) 0.043(3) 0.022(3) 0.001(3) 0.001(2) 0.005(3) C33 0.037(3) 0.038(3) 0.021(3) -0.002(3) 0.006(2) -0.002(3) C34 0.020(3) 0.029(3) 0.030(3) -0.007(3) 0.007(2) -0.003(2) C35 0.033(3) 0.061(4) 0.022(3) 0.007(3) 0.006(2) -0.008(3) C36 0.054(4) 0.078(5) 0.047(4) -0.022(4) 0.013(3) -0.016(4) As1 0.0251(3) 0.0316(3) 0.0260(4) -0.0002(3) 0.0047(2) -0.0015(3) C41 0.034(3) 0.024(3) 0.022(3) -0.002(2) 0.002(2) -0.002(2) C42 0.035(3) 0.033(3) 0.032(3) 0.003(3) 0.014(3) -0.003(3) C43 0.032(3) 0.030(3) 0.046(4) -0.002(3) 0.020(3) -0.002(3) C44 0.029(3) 0.033(3) 0.052(4) -0.002(3) 0.003(3) 0.008(3) C45 0.046(4) 0.047(4) 0.031(4) 0.002(3) 0.001(3) 0.012(3) C46 0.035(3) 0.045(4) 0.036(4) -0.006(3) 0.013(3) 0.000(3) C47 0.033(3) 0.029(3) 0.030(3) 0.003(2) 0.013(2) 0.000(2) C48 0.037(3) 0.050(4) 0.037(4) -0.006(3) 0.007(3) 0.011(3) C49 0.033(4) 0.071(5) 0.043(4) -0.003(4) 0.007(3) 0.013(3) C50 0.056(4) 0.046(4) 0.037(4) -0.009(3) 0.012(3) 0.014(3) C51 0.050(4) 0.037(4) 0.044(4) -0.003(3) 0.008(3) -0.009(3) C52 0.032(3) 0.033(3) 0.039(4) -0.005(3) 0.011(3) -0.002(3) C53 0.025(3) 0.028(3) 0.028(3) -0.006(2) 0.006(2) -0.005(2) C54 0.029(3) 0.036(3) 0.033(3) 0.000(3) 0.007(2) 0.003(3) C55 0.026(3) 0.045(4) 0.039(4) -0.010(3) -0.002(3) 0.002(3) C56 0.030(3) 0.033(3) 0.059(4) -0.007(3) 0.017(3) -0.005(3) C57 0.040(4) 0.047(4) 0.044(4) 0.000(3) 0.018(3) -0.008(3) C58 0.037(3) 0.049(4) 0.030(4) -0.001(3) 0.006(3) -0.007(3) C59 0.022(3) 0.041(3) 0.030(3) -0.003(3) 0.001(2) -0.006(3) C60 0.048(4) 0.034(3) 0.037(4) -0.002(3) 0.014(3) -0.005(3) C61 0.049(4) 0.063(5) 0.033(4) -0.002(3) 0.018(3) -0.004(3) C62 0.050(4) 0.055(4) 0.029(4) 0.011(3) 0.008(3) -0.004(3) C63 0.078(5) 0.031(4) 0.039(4) 0.010(3) 0.020(3) 0.001(3) C64 0.055(4) 0.033(3) 0.033(4) 0.005(3) 0.007(3) 0.005(3) As2 0.0405(4) 0.0467(4) 0.0265(4) 0.0021(3) 0.0086(3) 0.0072(3) C71 0.042(4) 0.043(4) 0.025(3) 0.001(3) 0.007(3) 0.010(3) C72 0.043(4) 0.065(5) 0.034(4) -0.005(3) 0.010(3) 0.006(3) C73 0.054(4) 0.061(5) 0.052(5) 0.006(4) 0.023(4) 0.015(4) C74 0.079(5) 0.047(4) 0.054(5) 0.007(4) 0.035(4) 0.018(4) C75 0.071(5) 0.051(4) 0.047(4) -0.006(3) 0.025(4) -0.005(4) C76 0.057(4) 0.050(4) 0.040(4) 0.000(3) 0.021(3) 0.002(3) C77 0.035(3) 0.055(4) 0.030(4) 0.002(3) 0.005(3) 0.011(3) C78 0.047(4) 0.081(5) 0.041(4) 0.002(4) 0.013(3) 0.017(4) C79 0.047(4) 0.113(7) 0.056(5) 0.001(5) 0.013(4) 0.020(4) C80 0.049(5) 0.107(7) 0.053(5) -0.001(5) -0.005(4) 0.023(5) C81 0.062(5) 0.077(5) 0.039(4) 0.009(4) 0.000(4) 0.009(4) C82 0.048(4) 0.060(4) 0.037(4) 0.003(3) 0.010(3) 0.012(3) C83 0.057(4) 0.041(4) 0.026(3) -0.001(3) 0.013(3) 0.004(3) C84 0.058(4) 0.059(4) 0.032(4) -0.004(3) 0.016(3) 0.012(4) C85 0.090(6) 0.046(4) 0.047(5) 0.001(3) 0.034(4) -0.004(4) C86 0.061(5) 0.065(5) 0.056(5) -0.016(4) 0.021(4) -0.017(4) C87 0.050(4) 0.058(5) 0.057(5) -0.008(4) 0.013(3) -0.005(4) C88 0.044(4) 0.054(4) 0.048(4) 0.003(3) 0.006(3) 0.006(3) C89 0.040(4) 0.061(4) 0.025(3) 0.002(3) 0.006(3) -0.001(3) C90 0.057(4) 0.081(5) 0.033(4) 0.005(4) 0.014(3) 0.028(4) C91 0.051(4) 0.098(6) 0.029(4) -0.006(4) 0.005(3) 0.018(4) C92 0.058(5) 0.102(7) 0.041(5) 0.010(5) 0.014(4) -0.008(5) C93 0.096(6) 0.077(6) 0.035(4) 0.006(4) 0.020(4) -0.016(5) C94 0.102(6) 0.048(4) 0.044(5) 0.001(3) 0.017(4) -0.021(4) O4 0.061(3) 0.135(5) 0.069(4) -0.005(4) 0.015(3) -0.030(3) C95 0.067(6) 0.181(10) 0.061(6) -0.018(6) 0.010(5) -0.048(6) C96 0.080(6) 0.161(9) 0.082(7) -0.042(6) 0.041(5) -0.055(6) C97 0.070(6) 0.147(9) 0.082(7) -0.001(6) 0.025(5) -0.030(6) C98 0.132(9) 0.140(9) 0.068(7) 0.036(6) 0.001(6) -0.026(7) _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 S6 2.4035(15) . ? Ti1 S4 2.4104(15) . ? Ti1 S5 2.4191(16) . ? Ti1 S2 2.4221(16) . ? Ti1 S1 2.4229(15) . ? Ti1 S3 2.4266(15) . ? S1 C1 1.759(5) . ? S2 C2 1.750(5) . ? S3 C16 1.754(5) . ? S4 C17 1.769(5) . ? S5 C28 1.761(5) . ? S6 C29 1.752(5) . ? N1 C7 1.337(6) . ? N1 C8 1.419(7) . ? N2 C22 1.342(7) . ? N2 C23 1.467(8) . ? N3 C34 1.357(6) . ? N3 C35 1.440(7) . ? O1 C7 1.237(6) . ? O2 C22 1.213(6) . ? O3 C34 1.227(6) . ? C1 C6 1.397(7) . ? C1 C2 1.415(7) . ? C2 C3 1.416(7) . ? C3 C4 1.396(7) . ? C3 C7 1.503(7) . ? C4 C5 1.385(7) . ? C5 C6 1.376(7) . ? C8 C9 1.320(7) . ? C8 C13 1.476(8) . ? C9 C10 1.402(7) . ? C10 C11 1.376(8) . ? C11 C12 1.431(8) . ? C12 C13 1.432(8) . ? C12 C35 1.466(8) 3_576 ? C13 C14 1.426(8) . ? C14 C15 1.320(8) . ? C15 C36 1.417(8) 3_576 ? C16 C21 1.391(7) . ? C16 C17 1.415(7) . ? C17 C18 1.412(7) . ? C18 C19 1.383(8) . ? C18 C22 1.521(8) . ? C19 C20 1.383(8) . ? C20 C21 1.378(8) . ? C23 C24 1.261(8) . ? C23 C26 1.504(11) . ? C24 C25 1.431(8) . ? C25 C27 1.262(10) 3_576 ? C26 C27 1.431(11) . ? C26 C26 1.460(13) 3_576 ? C27 C25 1.262(10) 3_576 ? C28 C33 1.385(7) . ? C28 C29 1.415(7) . ? C29 C30 1.408(7) . ? C30 C31 1.395(7) . ? C30 C34 1.506(7) . ? C31 C32 1.381(7) . ? C32 C33 1.373(7) . ? C35 C36 1.340(8) . ? C35 C12 1.466(8) 3_576 ? C36 C15 1.417(8) 3_576 ? As1 C59 1.905(5) . ? As1 C47 1.912(5) . ? As1 C41 1.913(5) . ? As1 C53 1.914(5) . ? C41 C46 1.371(7) . ? C41 C42 1.373(7) . ? C42 C43 1.392(7) . ? C43 C44 1.357(8) . ? C44 C45 1.377(8) . ? C45 C46 1.400(7) . ? C47 C52 1.375(7) . ? C47 C48 1.398(7) . ? C48 C49 1.385(8) . ? C49 C50 1.366(8) . ? C50 C51 1.385(8) . ? C51 C52 1.376(7) . ? C53 C54 1.363(7) . ? C53 C58 1.386(7) . ? C54 C55 1.380(7) . ? C55 C56 1.376(8) . ? C56 C57 1.361(8) . ? C57 C58 1.376(7) . ? C59 C60 1.383(7) . ? C59 C64 1.385(7) . ? C60 C61 1.383(8) . ? C61 C62 1.356(8) . ? C62 C63 1.361(8) . ? C63 C64 1.376(8) . ? As2 C77 1.918(6) . ? As2 C83 1.925(6) . ? As2 C71 1.930(6) . ? As2 C89 1.930(6) . ? C71 C72 1.377(8) . ? C71 C76 1.394(8) . ? C72 C73 1.382(8) . ? C73 C74 1.387(9) . ? C74 C75 1.374(9) . ? C75 C76 1.382(8) . ? C77 C78 1.356(8) . ? C77 C82 1.408(8) . ? C78 C79 1.399(9) . ? C79 C80 1.375(10) . ? C80 C81 1.375(9) . ? C81 C82 1.381(8) . ? C83 C88 1.373(8) . ? C83 C84 1.413(8) . ? C84 C85 1.412(9) . ? C85 C86 1.368(9) . ? C86 C87 1.355(9) . ? C87 C88 1.370(8) . ? C89 C90 1.370(8) . ? C89 C94 1.375(9) . ? C90 C91 1.402(9) . ? C91 C92 1.378(10) . ? C92 C93 1.400(10) . ? C93 C94 1.392(9) . ? O4 C97 1.424(9) . ? O4 C95 1.449(9) . ? C95 C96 1.497(10) . ? C97 C98 1.480(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 S6 Ti1 S4 77.61(5) . . ? S6 Ti1 S5 79.95(5) . . ? S4 Ti1 S5 155.75(6) . . ? S6 Ti1 S2 92.70(5) . . ? S4 Ti1 S2 80.98(5) . . ? S5 Ti1 S2 109.27(6) . . ? S6 Ti1 S1 161.58(6) . . ? S4 Ti1 S1 117.91(6) . . ? S5 Ti1 S1 85.88(5) . . ? S2 Ti1 S1 80.87(5) . . ? S6 Ti1 S3 106.97(6) . . ? S4 Ti1 S3 80.19(5) . . ? S5 Ti1 S3 97.83(6) . . ? S2 Ti1 S3 148.98(6) . . ? S1 Ti1 S3 86.47(5) . . ? C1 S1 Ti1 108.58(17) . . ? C2 S2 Ti1 109.75(17) . . ? C16 S3 Ti1 102.23(17) . . ? C17 S4 Ti1 102.54(18) . . ? C28 S5 Ti1 110.26(18) . . ? C29 S6 Ti1 112.41(17) . . ? C7 N1 C8 128.4(5) . . ? C22 N2 C23 129.6(5) . . ? C34 N3 C35 123.3(5) . . ? C6 C1 C2 120.2(5) . . ? C6 C1 S1 118.8(4) . . ? C2 C1 S1 121.0(4) . . ? C1 C2 C3 118.8(5) . . ? C1 C2 S2 117.5(4) . . ? C3 C2 S2 123.5(4) . . ? C4 C3 C2 119.0(5) . . ? C4 C3 C7 114.5(5) . . ? C2 C3 C7 126.4(5) . . ? C5 C4 C3 121.3(5) . . ? C6 C5 C4 120.2(5) . . ? C5 C6 C1 120.2(5) . . ? O1 C7 N1 121.4(5) . . ? O1 C7 C3 119.8(5) . . ? N1 C7 C3 118.5(5) . . ? C9 C8 N1 125.0(5) . . ? C9 C8 C13 118.3(5) . . ? N1 C8 C13 116.6(5) . . ? C8 C9 C10 123.8(5) . . ? C11 C10 C9 119.1(5) . . ? C10 C11 C12 121.3(6) . . ? C11 C12 C13 117.7(6) . . ? C11 C12 C35 123.6(5) . 3_576 ? C13 C12 C35 118.8(5) . 3_576 ? C14 C13 C12 117.8(6) . . ? C14 C13 C8 123.2(5) . . ? C12 C13 C8 118.8(5) . . ? C15 C14 C13 122.1(6) . . ? C14 C15 C36 120.3(6) . 3_576 ? C21 C16 C17 119.2(5) . . ? C21 C16 S3 119.8(4) . . ? C17 C16 S3 121.0(4) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 S4 123.8(4) . . ? C16 C17 S4 116.4(4) . . ? C19 C18 C17 118.6(5) . . ? C19 C18 C22 114.6(5) . . ? C17 C18 C22 126.6(5) . . ? C18 C19 C20 121.6(6) . . ? C21 C20 C19 120.0(6) . . ? C20 C21 C16 120.7(5) . . ? O2 C22 N2 123.3(6) . . ? O2 C22 C18 119.1(6) . . ? N2 C22 C18 117.1(5) . . ? C24 C23 N2 123.7(7) . . ? C24 C23 C26 119.9(7) . . ? N2 C23 C26 115.9(5) . . ? C23 C24 C25 121.5(7) . . ? C27 C25 C24 120.8(7) 3_576 . ? C27 C26 C26 112.7(10) . 3_576 ? C27 C26 C23 128.5(7) . . ? C26 C26 C23 118.7(9) 3_576 . ? C25 C27 C26 126.1(8) 3_576 . ? C33 C28 C29 120.2(5) . . ? C33 C28 S5 119.7(4) . . ? C29 C28 S5 120.0(4) . . ? C30 C29 C28 118.8(5) . . ? C30 C29 S6 124.1(4) . . ? C28 C29 S6 117.0(4) . . ? C31 C30 C29 119.2(5) . . ? C31 C30 C34 114.1(5) . . ? C29 C30 C34 126.6(5) . . ? C32 C31 C30 121.0(5) . . ? C33 C32 C31 120.3(5) . . ? C32 C33 C28 120.5(5) . . ? O3 C34 N3 120.9(5) . . ? O3 C34 C30 120.3(5) . . ? N3 C34 C30 118.6(5) . . ? C36 C35 N3 122.6(6) . . ? C36 C35 C12 118.4(5) . 3_576 ? N3 C35 C12 119.0(5) . 3_576 ? C35 C36 C15 122.4(6) . 3_576 ? C59 As1 C47 109.7(2) . . ? C59 As1 C41 109.6(2) . . ? C47 As1 C41 107.2(2) . . ? C59 As1 C53 111.3(2) . . ? C47 As1 C53 106.3(2) . . ? C41 As1 C53 112.5(2) . . ? C46 C41 C42 120.4(5) . . ? C46 C41 As1 117.8(4) . . ? C42 C41 As1 121.8(4) . . ? C41 C42 C43 119.9(5) . . ? C44 C43 C42 119.7(5) . . ? C43 C44 C45 121.3(5) . . ? C44 C45 C46 118.9(6) . . ? C41 C46 C45 119.8(5) . . ? C52 C47 C48 120.6(5) . . ? C52 C47 As1 121.6(4) . . ? C48 C47 As1 117.8(4) . . ? C49 C48 C47 118.4(6) . . ? C50 C49 C48 120.4(6) . . ? C49 C50 C51 121.0(6) . . ? C52 C51 C50 119.0(6) . . ? C47 C52 C51 120.3(5) . . ? C54 C53 C58 121.0(5) . . ? C54 C53 As1 121.8(4) . . ? C58 C53 As1 117.1(4) . . ? C53 C54 C55 119.0(5) . . ? C56 C55 C54 120.8(5) . . ? C57 C56 C55 119.5(5) . . ? C56 C57 C58 120.9(6) . . ? C57 C58 C53 118.8(5) . . ? C60 C59 C64 120.1(5) . . ? C60 C59 As1 120.4(4) . . ? C64 C59 As1 119.4(4) . . ? C61 C60 C59 119.2(6) . . ? C62 C61 C60 120.7(6) . . ? C61 C62 C63 119.9(6) . . ? C62 C63 C64 121.4(6) . . ? C63 C64 C59 118.7(6) . . ? C77 As2 C83 110.8(3) . . ? C77 As2 C71 108.0(3) . . ? C83 As2 C71 113.2(2) . . ? C77 As2 C89 110.6(2) . . ? C83 As2 C89 107.9(3) . . ? C71 As2 C89 106.3(3) . . ? C72 C71 C76 122.3(6) . . ? C72 C71 As2 119.8(5) . . ? C76 C71 As2 117.4(4) . . ? C71 C72 C73 118.9(6) . . ? C72 C73 C74 119.6(6) . . ? C75 C74 C73 120.5(6) . . ? C74 C75 C76 121.0(7) . . ? C75 C76 C71 117.5(6) . . ? C78 C77 C82 121.6(6) . . ? C78 C77 As2 120.4(5) . . ? C82 C77 As2 117.8(4) . . ? C77 C78 C79 118.3(6) . . ? C80 C79 C78 121.0(7) . . ? C79 C80 C81 120.3(7) . . ? C80 C81 C82 120.0(7) . . ? C81 C82 C77 118.9(6) . . ? C88 C83 C84 121.0(6) . . ? C88 C83 As2 118.8(5) . . ? C84 C83 As2 120.0(5) . . ? C85 C84 C83 117.4(6) . . ? C86 C85 C84 119.6(7) . . ? C87 C86 C85 121.7(7) . . ? C86 C87 C88 120.6(7) . . ? C87 C88 C83 119.6(6) . . ? C90 C89 C94 122.5(6) . . ? C90 C89 As2 119.3(5) . . ? C94 C89 As2 118.2(5) . . ? C89 C90 C91 118.3(7) . . ? C92 C91 C90 119.8(7) . . ? C91 C92 C93 121.2(7) . . ? C94 C93 C92 118.3(7) . . ? C89 C94 C93 119.7(7) . . ? C97 O4 C95 111.7(6) . . ? O4 C95 C96 110.2(7) . . ? O4 C97 C98 109.0(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.155 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.109