Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Seth Brown' 'Bruce C. Noll' 'Tobias Schroeder' 'Vesela Ugrinova' _publ_contact_author_name 'Seth N. Brown' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Notre Dame Notre Dame Indiana 46556-5670 UNITED STATES OF AMERICA ; _publ_contact_author_email SETH.N.BROWN.114@ND.EDU _publ_section_title ; A Chelating \&s-Diketonate/Phenoxide Ligand and its Coordination Behavior Toward Titanium and Scandium ; data_ligand _database_code_depnum_ccdc_archive 'CCDC 281977' # Collected as bcn97 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; 1,3-Bis(2'-(3'',5''-di-tert-butyl-2''-hydroxystyryl)phenyl)- propane-1,3-dione ; _chemical_melting_point ? _chemical_formula_moiety 'C47 H56 O4' _chemical_formula_sum 'C47 H56 O4' _chemical_formula_weight 684.92 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' _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 9.1032(4) _cell_length_b 11.9561(5) _cell_length_c 18.4632(8) _cell_angle_alpha 104.741(2) _cell_angle_beta 96.902(3) _cell_angle_gamma 92.611(2) _cell_volume 1923.21(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5872 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 31.51 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9755 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_crystal_recrystallization_method ; Crystals grown by dissolving an oily sample of the compound in hexane and allowing to stand at room temperature. ; _diffrn_ambient_temperature 100(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 SMART Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41961 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9525 _reflns_number_gt 7190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.1014P)^2^+1.3218P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9525 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2032 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 O1 O 0.44677(19) 0.25209(15) 0.38850(10) 0.0455(4) Uani 1 1 d . . . O2 O 0.51316(18) 0.43934(15) 0.35832(10) 0.0426(4) Uani 1 1 d . . . O3 O 1.1314(3) 0.12690(18) 0.33411(13) 0.0304(7) Uani 0.647(5) 1 d P A 1 O31 O 0.6835(4) -0.1239(3) 0.2450(2) 0.0319(12) Uani 0.353(5) 1 d P A 2 H31 H 0.6396 -0.1697 0.2051 0.048 Uiso 0.353(5) 1 calc PR A 2 O4 O 1.1827(3) 0.72697(18) 0.72112(12) 0.0327(6) Uani 0.692(5) 1 d P B 1 O41 O 0.7671(6) 0.4375(5) 0.6466(3) 0.0509(19) Uani 0.308(5) 1 d P B 2 H41 H 0.7259 0.3893 0.6654 0.076 Uiso 0.308(5) 1 calc PR B 2 C1 C 0.5633(2) 0.27241(17) 0.43644(12) 0.0321(4) Uani 1 1 d . . . C2 C 0.6600(2) 0.37308(18) 0.44876(12) 0.0318(4) Uani 1 1 d . . . C3 C 0.6320(2) 0.45443(17) 0.40856(12) 0.0300(4) Uani 1 1 d . . . C4 C 0.7426(2) 0.07866(16) 0.38128(11) 0.0264(4) Uani 1 1 d . . . C5 C 0.8736(2) 0.04037(16) 0.36489(11) 0.0259(4) Uani 1 1 d . A . C6 C 0.8294(3) 0.59023(17) 0.55371(12) 0.0305(4) Uani 1 1 d . . . C7 C 0.9507(2) 0.60677(16) 0.60454(12) 0.0295(4) Uani 1 1 d . B . C11 C 0.6021(2) 0.18838(16) 0.48189(12) 0.0296(4) Uani 1 1 d . . . C12 C 0.6943(2) 0.10003(16) 0.45674(11) 0.0264(4) Uani 1 1 d . . . C13 C 0.7330(2) 0.02771(19) 0.50384(12) 0.0323(4) Uani 1 1 d . . . C14 C 0.6812(3) 0.0428(2) 0.57270(13) 0.0380(5) Uani 1 1 d . . . C15 C 0.5881(3) 0.1300(2) 0.59602(13) 0.0414(5) Uani 1 1 d . . . C16 C 0.5500(3) 0.2026(2) 0.55114(14) 0.0411(5) Uani 1 1 d . . . C21 C 0.7324(2) 0.55803(17) 0.41386(11) 0.0291(4) Uani 1 1 d . . . C22 C 0.8284(2) 0.61736(17) 0.47983(11) 0.0300(4) Uani 1 1 d . . . C23 C 0.9230(3) 0.71009(18) 0.47498(13) 0.0362(5) Uani 1 1 d . . . C24 C 0.9270(3) 0.74135(19) 0.40794(13) 0.0398(5) Uani 1 1 d . . . C25 C 0.8311(3) 0.68277(19) 0.34357(12) 0.0364(5) Uani 1 1 d . . . C26 C 0.7348(2) 0.59282(18) 0.34683(12) 0.0319(4) Uani 1 1 d . . . C31 C 0.9139(2) 0.00354(16) 0.28744(11) 0.0245(4) Uani 1 1 d . . . C32 C 1.0493(2) 0.04588(16) 0.27180(11) 0.0253(4) Uani 0.647(5) 1 d P A 1 C321 C 1.0493(2) 0.04588(16) 0.27180(11) 0.0253(4) Uani 0.353(5) 1 d P A 2 H321 H 1.1132 0.0997 0.3109 0.030 Uiso 0.353(5) 1 calc PR A 2 C33 C 1.0925(2) 0.01047(16) 0.19968(11) 0.0244(4) Uani 1 1 d . . . C34 C 0.9952(2) -0.07086(16) 0.14470(11) 0.0247(4) Uani 1 1 d . A . C35 C 0.8593(2) -0.11535(16) 0.15734(11) 0.0250(4) Uani 1 1 d . . . C36 C 0.8201(2) -0.07561(16) 0.23001(11) 0.0249(4) Uani 0.647(5) 1 d P A 1 H36 H 0.7275 -0.1032 0.2405 0.030 Uiso 0.647(5) 1 calc PR A 1 C361 C 0.8201(2) -0.07561(16) 0.23001(11) 0.0249(4) Uani 0.353(5) 1 d P A 2 C41 C 0.9660(2) 0.58829(16) 0.68068(11) 0.0268(4) Uani 1 1 d . . . C42 C 1.0828(2) 0.65011(16) 0.73490(12) 0.0284(4) Uani 0.692(5) 1 d P B 1 C421 C 1.0828(2) 0.65011(16) 0.73490(12) 0.0284(4) Uani 0.308(5) 1 d P B 2 H42 H 1.1477 0.7037 0.7214 0.034 Uiso 0.308(5) 1 calc PR B 2 C43 C 1.1065(2) 0.63539(16) 0.80756(11) 0.0292(4) Uani 1 1 d . . . C44 C 1.0086(2) 0.55634(17) 0.82492(11) 0.0285(4) Uani 1 1 d . B . C45 C 0.8909(2) 0.49244(17) 0.77344(11) 0.0286(4) Uani 1 1 d . . . C46 C 0.8719(2) 0.50953(17) 0.70119(11) 0.0286(4) Uani 0.692(5) 1 d P B 1 H46 H 0.7930 0.4666 0.6650 0.034 Uiso 0.692(5) 1 calc PR B 1 C461 C 0.8719(2) 0.50953(17) 0.70119(11) 0.0286(4) Uani 0.308(5) 1 d P B 2 C330 C 1.2386(2) 0.05930(16) 0.18138(11) 0.0268(4) Uani 1 1 d . A . C331 C 1.2391(3) 0.19220(18) 0.19503(14) 0.0374(5) Uani 1 1 d . . . H33A H 1.2253 0.2273 0.2476 0.056 Uiso 1 1 calc R A . H33B H 1.1582 0.2107 0.1610 0.056 Uiso 1 1 calc R . . H33C H 1.3342 0.2230 0.1852 0.056 Uiso 1 1 calc R . . C332 C 1.3725(2) 0.02879(18) 0.23076(12) 0.0319(4) Uani 1 1 d . . . H33D H 1.3629 0.0602 0.2843 0.048 Uiso 1 1 calc R A . H33E H 1.4646 0.0625 0.2197 0.048 Uiso 1 1 calc R . . H33F H 1.3747 -0.0557 0.2196 0.048 Uiso 1 1 calc R . . C333 C 1.2602(2) 0.00791(19) 0.09867(12) 0.0330(4) Uani 1 1 d . . . H33G H 1.3542 0.0410 0.0892 0.050 Uiso 1 1 calc R A . H33H H 1.1781 0.0264 0.0653 0.050 Uiso 1 1 calc R . . H33I H 1.2621 -0.0765 0.0887 0.050 Uiso 1 1 calc R . . C350 C 0.7544(2) -0.20300(17) 0.09522(11) 0.0289(4) Uani 1 1 d . A . C351 C 0.6128(3) -0.1454(2) 0.07657(14) 0.0458(6) Uani 1 1 d . . . H35A H 0.5665 -0.1183 0.1225 0.069 Uiso 1 1 calc R A . H35B H 0.5435 -0.2018 0.0385 0.069 Uiso 1 1 calc R . . H35C H 0.6379 -0.0793 0.0568 0.069 Uiso 1 1 calc R . . C352 C 0.7139(3) -0.3113(2) 0.12158(14) 0.0422(5) Uani 1 1 d . . . H35D H 0.6696 -0.2880 0.1685 0.063 Uiso 1 1 calc R A . H35E H 0.8037 -0.3507 0.1306 0.063 Uiso 1 1 calc R . . H35F H 0.6425 -0.3641 0.0824 0.063 Uiso 1 1 calc R . . C353 C 0.8233(3) -0.2439(2) 0.02248(12) 0.0376(5) Uani 1 1 d . . . H35G H 0.7527 -0.2996 -0.0153 0.056 Uiso 1 1 calc R A . H35H H 0.9142 -0.2811 0.0330 0.056 Uiso 1 1 calc R . . H35I H 0.8471 -0.1771 0.0031 0.056 Uiso 1 1 calc R . . C430 C 1.2347(2) 0.70162(18) 0.86768(13) 0.0380(5) Uani 1 1 d . B . C431 C 1.2224(4) 0.8297(3) 0.88776(19) 0.0431(7) Uani 0.726(3) 1 d P B 1 H43A H 1.1235 0.8463 0.9016 0.065 Uiso 0.726(3) 1 calc PR B 1 H43B H 1.2377 0.8596 0.8443 0.065 Uiso 0.726(3) 1 calc PR B 1 H43C H 1.2979 0.8673 0.9306 0.065 Uiso 0.726(3) 1 calc PR B 1 C432 C 1.3814(3) 0.6635(3) 0.84524(18) 0.0388(7) Uani 0.726(3) 1 d P B 1 H43D H 1.3791 0.5787 0.8330 0.058 Uiso 0.726(3) 1 calc PR B 1 H43E H 1.4604 0.6972 0.8872 0.058 Uiso 0.726(3) 1 calc PR B 1 H43F H 1.4004 0.6898 0.8009 0.058 Uiso 0.726(3) 1 calc PR B 1 C433 C 1.2278(3) 0.6666(3) 0.94667(16) 0.0328(6) Uani 0.726(3) 1 d P B 1 H43G H 1.2356 0.5829 0.9384 0.049 Uiso 0.726(3) 1 calc PR B 1 H43H H 1.1334 0.6870 0.9651 0.049 Uiso 0.726(3) 1 calc PR B 1 H43I H 1.3102 0.7087 0.9843 0.049 Uiso 0.726(3) 1 calc PR B 1 C434 C 1.3462(11) 0.6308(7) 0.8814(5) 0.0431(7) Uani 0.274(3) 1 d P B 2 H43J H 1.3603 0.5759 0.8338 0.065 Uiso 0.274(3) 1 calc PR B 2 H43K H 1.3178 0.5878 0.9169 0.065 Uiso 0.274(3) 1 calc PR B 2 H43L H 1.4390 0.6787 0.9031 0.065 Uiso 0.274(3) 1 calc PR B 2 C435 C 1.1837(9) 0.7915(8) 0.9239(5) 0.0388(7) Uani 0.274(3) 1 d P B 2 H43M H 1.1039 0.8280 0.9001 0.058 Uiso 0.274(3) 1 calc PR B 2 H43N H 1.2660 0.8499 0.9480 0.058 Uiso 0.274(3) 1 calc PR B 2 H43O H 1.1461 0.7583 0.9621 0.058 Uiso 0.274(3) 1 calc PR B 2 C436 C 1.3315(9) 0.7921(7) 0.8201(4) 0.0328(6) Uani 0.274(3) 1 d P B 2 H43P H 1.2653 0.8485 0.8069 0.049 Uiso 0.274(3) 1 calc PR B 2 H43Q H 1.3618 0.7434 0.7739 0.049 Uiso 0.274(3) 1 calc PR B 2 H43R H 1.4196 0.8334 0.8537 0.049 Uiso 0.274(3) 1 calc PR B 2 C450 C 0.7925(3) 0.4010(2) 0.79432(14) 0.0400(5) Uani 1 1 d . B . C451 C 0.8134(5) 0.4116(3) 0.87843(18) 0.0786(11) Uani 1 1 d . . . H45A H 0.7486 0.3516 0.8891 0.118 Uiso 1 1 calc R B . H45B H 0.7879 0.4884 0.9055 0.118 Uiso 1 1 calc R . . H45C H 0.9171 0.4015 0.8952 0.118 Uiso 1 1 calc R . . C452 C 0.8389(3) 0.2793(2) 0.75554(18) 0.0525(7) Uani 1 1 d . . . H45D H 0.8269 0.2684 0.7007 0.079 Uiso 1 1 calc R B . H45E H 0.7761 0.2195 0.7676 0.079 Uiso 1 1 calc R . . H45F H 0.9430 0.2730 0.7739 0.079 Uiso 1 1 calc R . . C453 C 0.6295(3) 0.4047(3) 0.76329(19) 0.0568(8) Uani 1 1 d . . . H45G H 0.6206 0.3980 0.7089 0.085 Uiso 1 1 calc R B . H45H H 0.5934 0.4784 0.7890 0.085 Uiso 1 1 calc R . . H45I H 0.5701 0.3402 0.7721 0.085 Uiso 1 1 calc R . . H1 H 0.461(5) 0.354(4) 0.361(3) 0.120(16) Uiso 1 1 d . . . H30 H 1.215(5) 0.152(4) 0.326(2) 0.042(11) Uiso 0.647(5) 1 d P . . H40 H 1.146(5) 0.740(4) 0.681(3) 0.052(12) Uiso 0.692(5) 1 d P . . H2 H 0.747(3) 0.383(2) 0.4861(14) 0.032(6) Uiso 1 1 d . . . H4 H 0.671(3) 0.089(2) 0.3402(14) 0.036(6) Uiso 1 1 d . . . H5 H 0.947(2) 0.0366(19) 0.4070(13) 0.025(5) Uiso 1 1 d . . . H6 H 0.739(3) 0.563(2) 0.5660(14) 0.036(6) Uiso 1 1 d . . . H7 H 1.040(3) 0.633(2) 0.5913(14) 0.036(6) Uiso 1 1 d . . . H13 H 0.798(3) -0.034(2) 0.4876(15) 0.043(7) Uiso 1 1 d . . . H14 H 0.706(3) -0.007(3) 0.6039(16) 0.048(7) Uiso 1 1 d . . . H15 H 0.555(3) 0.138(2) 0.6449(16) 0.048(7) Uiso 1 1 d . . . H16 H 0.478(3) 0.274(3) 0.5675(17) 0.062(9) Uiso 1 1 d . . . H23 H 0.983(3) 0.753(3) 0.5170(17) 0.052(8) Uiso 1 1 d . . . H24 H 1.002(3) 0.796(2) 0.4058(15) 0.044(7) Uiso 1 1 d . . . H25 H 0.837(3) 0.705(2) 0.2995(14) 0.033(6) Uiso 1 1 d . . . H26 H 0.664(3) 0.550(2) 0.3003(16) 0.045(7) Uiso 1 1 d . . . H34 H 1.023(2) -0.093(2) 0.0971(13) 0.026(5) Uiso 1 1 d . . . H44 H 1.026(2) 0.546(2) 0.8762(13) 0.026(5) Uiso 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 O1 0.0379(9) 0.0356(9) 0.0564(10) 0.0052(7) -0.0034(8) 0.0006(7) O2 0.0366(9) 0.0362(9) 0.0516(10) 0.0098(7) -0.0052(7) 0.0081(7) O3 0.0281(12) 0.0215(11) 0.0357(13) -0.0021(8) 0.0033(9) -0.0011(8) O31 0.028(2) 0.029(2) 0.034(2) 0.0003(16) 0.0038(16) 0.0049(15) O4 0.0433(13) 0.0273(11) 0.0272(12) 0.0084(8) 0.0033(9) -0.0046(9) O41 0.045(3) 0.050(4) 0.052(4) 0.017(3) -0.014(3) -0.018(3) C1 0.0331(11) 0.0219(9) 0.0396(11) -0.0005(8) 0.0143(9) 0.0088(7) C2 0.0289(10) 0.0276(10) 0.0381(11) 0.0069(8) 0.0036(9) 0.0059(8) C3 0.0296(10) 0.0243(9) 0.0350(10) 0.0030(8) 0.0066(8) 0.0120(7) C4 0.0289(10) 0.0223(9) 0.0267(9) 0.0040(7) 0.0026(8) 0.0046(7) C5 0.0290(10) 0.0212(9) 0.0260(9) 0.0037(7) 0.0021(7) 0.0039(7) C6 0.0386(11) 0.0209(9) 0.0328(10) 0.0065(7) 0.0067(9) 0.0096(8) C7 0.0372(11) 0.0204(9) 0.0327(10) 0.0077(7) 0.0084(8) 0.0080(7) C11 0.0317(10) 0.0210(9) 0.0329(10) -0.0007(7) 0.0091(8) -0.0003(7) C12 0.0255(9) 0.0232(9) 0.0278(9) 0.0018(7) 0.0044(7) 0.0000(7) C13 0.0314(10) 0.0317(10) 0.0322(10) 0.0064(8) 0.0028(8) 0.0011(8) C14 0.0402(12) 0.0398(12) 0.0326(11) 0.0103(9) 0.0016(9) -0.0082(9) C15 0.0480(14) 0.0413(13) 0.0310(11) 0.0000(9) 0.0147(10) -0.0086(10) C16 0.0505(14) 0.0299(11) 0.0410(12) -0.0008(9) 0.0215(10) -0.0006(9) C21 0.0321(10) 0.0231(9) 0.0328(10) 0.0062(7) 0.0056(8) 0.0134(7) C22 0.0375(11) 0.0213(9) 0.0316(10) 0.0060(7) 0.0051(8) 0.0123(8) C23 0.0522(13) 0.0205(9) 0.0333(11) 0.0046(8) -0.0003(10) 0.0053(9) C24 0.0563(15) 0.0229(10) 0.0411(12) 0.0105(9) 0.0052(10) 0.0044(9) C25 0.0528(14) 0.0290(10) 0.0302(11) 0.0107(8) 0.0065(9) 0.0132(9) C26 0.0371(11) 0.0277(10) 0.0310(10) 0.0058(8) 0.0044(9) 0.0152(8) C31 0.0258(9) 0.0206(8) 0.0273(9) 0.0048(7) 0.0047(7) 0.0087(7) C32 0.0257(9) 0.0195(8) 0.0290(9) 0.0036(7) 0.0014(7) 0.0057(7) C321 0.0257(9) 0.0195(8) 0.0290(9) 0.0036(7) 0.0014(7) 0.0057(7) C33 0.0239(9) 0.0203(8) 0.0304(9) 0.0080(7) 0.0044(7) 0.0070(6) C34 0.0274(9) 0.0215(9) 0.0260(9) 0.0060(7) 0.0048(7) 0.0084(7) C35 0.0255(9) 0.0213(9) 0.0273(9) 0.0045(7) 0.0019(7) 0.0078(7) C36 0.0217(9) 0.0237(9) 0.0297(9) 0.0063(7) 0.0043(7) 0.0074(7) C361 0.0217(9) 0.0237(9) 0.0297(9) 0.0063(7) 0.0043(7) 0.0074(7) C41 0.0292(10) 0.0212(9) 0.0299(10) 0.0062(7) 0.0028(8) 0.0076(7) C42 0.0268(9) 0.0165(8) 0.0401(11) 0.0025(7) 0.0074(8) 0.0054(7) C421 0.0268(9) 0.0165(8) 0.0401(11) 0.0025(7) 0.0074(8) 0.0054(7) C43 0.0256(9) 0.0209(9) 0.0342(10) -0.0043(7) -0.0009(8) 0.0092(7) C44 0.0302(10) 0.0274(10) 0.0262(9) 0.0046(7) -0.0005(8) 0.0105(7) C45 0.0303(10) 0.0245(9) 0.0316(10) 0.0093(7) 0.0014(8) 0.0058(7) C46 0.0277(10) 0.0253(9) 0.0312(10) 0.0080(7) -0.0036(8) 0.0014(7) C461 0.0277(10) 0.0253(9) 0.0312(10) 0.0080(7) -0.0036(8) 0.0014(7) C330 0.0253(9) 0.0237(9) 0.0323(10) 0.0079(7) 0.0054(7) 0.0056(7) C331 0.0354(11) 0.0246(10) 0.0554(14) 0.0128(9) 0.0133(10) 0.0066(8) C332 0.0273(10) 0.0319(10) 0.0363(11) 0.0089(8) 0.0032(8) 0.0046(8) C333 0.0289(10) 0.0387(11) 0.0334(11) 0.0111(9) 0.0076(8) 0.0051(8) C350 0.0262(9) 0.0266(9) 0.0303(10) 0.0013(7) 0.0018(8) 0.0056(7) C351 0.0342(12) 0.0492(14) 0.0433(13) -0.0034(10) -0.0084(10) 0.0150(10) C352 0.0406(13) 0.0375(12) 0.0443(13) 0.0064(10) 0.0026(10) -0.0079(9) C353 0.0391(12) 0.0372(12) 0.0312(11) -0.0005(9) 0.0051(9) 0.0020(9) C430 0.0288(10) 0.0275(10) 0.0457(13) -0.0091(9) -0.0035(9) 0.0054(8) C431 0.058(2) 0.0240(14) 0.0398(16) 0.0008(12) -0.0053(14) 0.0012(12) C432 0.0281(14) 0.0516(18) 0.0305(14) 0.0002(13) 0.0043(11) -0.0005(12) C433 0.0319(14) 0.0361(14) 0.0272(13) 0.0046(10) 0.0002(10) -0.0006(10) C434 0.058(2) 0.0240(14) 0.0398(16) 0.0008(12) -0.0053(14) 0.0012(12) C435 0.0281(14) 0.0516(18) 0.0305(14) 0.0002(13) 0.0043(11) -0.0005(12) C436 0.0319(14) 0.0361(14) 0.0272(13) 0.0046(10) 0.0002(10) -0.0006(10) C450 0.0397(12) 0.0406(12) 0.0444(13) 0.0229(10) 0.0006(10) -0.0022(9) C451 0.121(3) 0.071(2) 0.0532(18) 0.0310(16) 0.0238(19) -0.010(2) C452 0.0415(13) 0.0353(13) 0.084(2) 0.0276(13) -0.0015(13) -0.0029(10) C453 0.0336(13) 0.0620(17) 0.091(2) 0.0430(16) 0.0215(13) 0.0114(11) _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 O1 C1 1.269(3) . y O1 H1 1.44(5) . ? O2 C3 1.311(3) . y O2 H1 1.12(5) . ? O3 C32 1.407(3) . ? O3 H30 0.85(5) . ? O31 H31 0.8400 . ? O4 C42 1.354(3) . ? O4 H40 0.84(5) . ? O41 H41 0.8400 . ? C1 C2 1.411(3) . y C1 C11 1.493(3) . ? C2 C3 1.381(3) . y C2 H2 0.96(2) . ? C3 C21 1.481(3) . ? C4 C5 1.338(3) . y C4 C12 1.475(3) . ? C4 H4 0.97(3) . ? C5 C31 1.481(3) . ? C5 H5 0.97(2) . ? C6 C7 1.333(3) . y C6 C22 1.479(3) . ? C6 H6 0.94(3) . ? C7 C41 1.469(3) . ? C7 H7 0.94(3) . ? C11 C16 1.390(3) . ? C11 C12 1.400(3) . ? C12 C13 1.402(3) . ? C13 C14 1.381(3) . ? C13 H13 0.98(3) . ? C14 C15 1.389(4) . ? C14 H14 0.95(3) . ? C15 C16 1.372(4) . ? C15 H15 0.97(3) . ? C16 H16 1.11(3) . ? C21 C26 1.405(3) . ? C21 C22 1.414(3) . ? C22 C23 1.400(3) . ? C23 C24 1.385(3) . ? C23 H23 0.91(3) . ? C24 C25 1.392(3) . ? C24 H24 0.93(3) . ? C25 C26 1.374(3) . ? C25 H25 0.92(2) . ? C26 H26 1.01(3) . ? C31 C36 1.395(3) . ? C31 C32 1.401(3) . ? C32 C33 1.400(3) . ? C33 C34 1.402(3) . ? C33 C330 1.536(3) . ? C34 C35 1.393(3) . ? C34 H34 0.92(2) . ? C35 C36 1.400(3) . ? C35 C350 1.536(3) . ? C36 H36 0.9500 . ? C41 C46 1.397(3) . ? C41 C42 1.406(3) . ? C42 C43 1.390(3) . ? C43 C44 1.391(3) . ? C43 C430 1.542(3) . ? C44 C45 1.395(3) . ? C44 H44 0.98(2) . ? C45 C46 1.392(3) . ? C45 C450 1.534(3) . ? C46 H46 0.9500 . ? C330 C333 1.534(3) . ? C330 C331 1.544(3) . ? C330 C332 1.547(3) . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C332 H33D 0.9800 . ? C332 H33E 0.9800 . ? C332 H33F 0.9800 . ? C333 H33G 0.9800 . ? C333 H33H 0.9800 . ? C333 H33I 0.9800 . ? C350 C353 1.527(3) . ? C350 C351 1.533(3) . ? C350 C352 1.539(3) . ? C351 H35A 0.9800 . ? C351 H35B 0.9800 . ? C351 H35C 0.9800 . ? C352 H35D 0.9800 . ? C352 H35E 0.9800 . ? C352 H35F 0.9800 . ? C353 H35G 0.9800 . ? C353 H35H 0.9800 . ? C353 H35I 0.9800 . ? C430 C434 1.392(9) . ? C430 C435 1.429(8) . ? C430 C431 1.494(4) . ? C430 C432 1.501(4) . ? C430 C433 1.624(4) . ? C430 C436 1.817(8) . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C432 H43D 0.9800 . ? C432 H43E 0.9800 . ? C432 H43F 0.9800 . ? C433 H43G 0.9800 . ? C433 H43H 0.9800 . ? C433 H43I 0.9800 . ? C434 H43J 0.9800 . ? C434 H43K 0.9800 . ? C434 H43L 0.9800 . ? C435 H43M 0.9800 . ? C435 H43N 0.9800 . ? C435 H43O 0.9800 . ? C436 H43P 0.9800 . ? C436 H43Q 0.9800 . ? C436 H43R 0.9800 . ? C450 C451 1.514(4) . ? C450 C453 1.533(3) . ? C450 C452 1.551(4) . ? C451 H45A 0.9800 . ? C451 H45B 0.9800 . ? C451 H45C 0.9800 . ? C452 H45D 0.9800 . ? C452 H45E 0.9800 . ? C452 H45F 0.9800 . ? C453 H45G 0.9800 . ? C453 H45H 0.9800 . ? C453 H45I 0.9800 . ? 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 C1 O1 H1 98.7(19) . . ? C3 O2 H1 103(2) . . ? C32 O3 H30 115(3) . . ? C42 O4 H40 105(3) . . ? O1 C1 C2 122.1(2) . . y O1 C1 C11 120.03(18) . . ? C2 C1 C11 117.84(19) . . ? C3 C2 C1 121.2(2) . . y C3 C2 H2 120.8(14) . . ? C1 C2 H2 118.0(14) . . ? O2 C3 C2 120.01(19) . . y O2 C3 C21 115.08(18) . . ? C2 C3 C21 124.80(19) . . ? C5 C4 C12 124.56(18) . . ? C5 C4 H4 118.2(15) . . ? C12 C4 H4 117.1(15) . . ? C4 C5 C31 124.48(18) . . ? C4 C5 H5 117.4(13) . . ? C31 C5 H5 118.1(13) . . ? C7 C6 C22 122.8(2) . . ? C7 C6 H6 118.8(15) . . ? C22 C6 H6 118.3(15) . . ? C6 C7 C41 128.5(2) . . ? C6 C7 H7 117.8(15) . . ? C41 C7 H7 113.7(15) . . ? C16 C11 C12 120.7(2) . . ? C16 C11 C1 118.63(19) . . ? C12 C11 C1 120.65(18) . . ? C11 C12 C13 117.91(18) . . ? C11 C12 C4 121.42(18) . . ? C13 C12 C4 120.57(18) . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13 119.9(15) . . ? C12 C13 H13 119.1(15) . . ? C13 C14 C15 120.1(2) . . ? C13 C14 H14 120.9(18) . . ? C15 C14 H14 119.0(17) . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 122.9(17) . . ? C14 C15 H15 117.2(17) . . ? C15 C16 C11 120.4(2) . . ? C15 C16 H16 122.9(16) . . ? C11 C16 H16 116.7(16) . . ? C26 C21 C22 119.87(19) . . ? C26 C21 C3 115.98(19) . . ? C22 C21 C3 124.06(18) . . ? C23 C22 C21 117.51(19) . . ? C23 C22 C6 118.71(19) . . ? C21 C22 C6 123.72(19) . . ? C24 C23 C22 121.9(2) . . ? C24 C23 H23 117.9(18) . . ? C22 C23 H23 120.1(18) . . ? C23 C24 C25 119.9(2) . . ? C23 C24 H24 118.5(17) . . ? C25 C24 H24 121.2(17) . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25 122.3(15) . . ? C24 C25 H25 118.2(15) . . ? C25 C26 C21 121.2(2) . . ? C25 C26 H26 120.1(15) . . ? C21 C26 H26 118.7(15) . . ? C36 C31 C32 119.34(17) . . ? C36 C31 C5 120.70(17) . . ? C32 C31 C5 119.93(17) . . ? C33 C32 C31 121.36(17) . . ? C33 C32 O3 125.14(18) . . ? C31 C32 O3 113.48(18) . . ? C32 C33 C34 116.73(17) . . ? C32 C33 C330 121.71(17) . . ? C34 C33 C330 121.56(17) . . ? C35 C34 C33 124.10(18) . . ? C35 C34 H34 119.6(14) . . ? C33 C34 H34 116.3(14) . . ? C34 C35 C36 116.91(17) . . ? C34 C35 C350 122.57(17) . . ? C36 C35 C350 120.52(17) . . ? C31 C36 C35 121.54(17) . . ? C31 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C46 C41 C42 118.29(18) . . ? C46 C41 C7 122.93(18) . . ? C42 C41 C7 118.75(18) . . ? O4 C42 C43 114.27(19) . . ? O4 C42 C41 123.6(2) . . ? C43 C42 C41 122.12(18) . . ? C42 C43 C44 117.03(17) . . ? C42 C43 C430 122.94(19) . . ? C44 C43 C430 120.02(19) . . ? C43 C44 C45 123.39(18) . . ? C43 C44 H44 117.0(13) . . ? C45 C44 H44 119.6(13) . . ? C46 C45 C44 117.60(18) . . ? C46 C45 C450 121.30(18) . . ? C44 C45 C450 120.98(18) . . ? C45 C46 C41 121.56(18) . . ? C45 C46 H46 119.2 . . ? C41 C46 H46 119.2 . . ? C333 C330 C33 111.85(16) . . ? C333 C330 C331 107.76(17) . . ? C33 C330 C331 110.02(16) . . ? C333 C330 C332 106.84(16) . . ? C33 C330 C332 110.34(15) . . ? C331 C330 C332 109.94(17) . . ? C330 C331 H33A 109.5 . . ? C330 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C330 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C330 C332 H33D 109.5 . . ? C330 C332 H33E 109.5 . . ? H33D C332 H33E 109.5 . . ? C330 C332 H33F 109.5 . . ? H33D C332 H33F 109.5 . . ? H33E C332 H33F 109.5 . . ? C330 C333 H33G 109.5 . . ? C330 C333 H33H 109.5 . . ? H33G C333 H33H 109.5 . . ? C330 C333 H33I 109.5 . . ? H33G C333 H33I 109.5 . . ? H33H C333 H33I 109.5 . . ? C353 C350 C351 107.92(18) . . ? C353 C350 C35 112.42(17) . . ? C351 C350 C35 108.94(16) . . ? C353 C350 C352 107.36(18) . . ? C351 C350 C352 109.47(19) . . ? C35 C350 C352 110.65(17) . . ? C350 C351 H35A 109.5 . . ? C350 C351 H35B 109.5 . . ? H35A C351 H35B 109.5 . . ? C350 C351 H35C 109.5 . . ? H35A C351 H35C 109.5 . . ? H35B C351 H35C 109.5 . . ? C350 C352 H35D 109.5 . . ? C350 C352 H35E 109.5 . . ? H35D C352 H35E 109.5 . . ? C350 C352 H35F 109.5 . . ? H35D C352 H35F 109.5 . . ? H35E C352 H35F 109.5 . . ? C350 C353 H35G 109.5 . . ? C350 C353 H35H 109.5 . . ? H35G C353 H35H 109.5 . . ? C350 C353 H35I 109.5 . . ? H35G C353 H35I 109.5 . . ? H35H C353 H35I 109.5 . . ? C434 C430 C435 125.1(6) . . ? C434 C430 C431 134.3(4) . . ? C435 C430 C431 39.4(4) . . ? C434 C430 C432 37.5(4) . . ? C435 C430 C432 137.1(4) . . ? C431 C430 C432 115.3(3) . . ? C434 C430 C43 112.5(4) . . ? C435 C430 C43 112.0(4) . . ? C431 C430 C43 112.2(2) . . ? C432 C430 C43 110.37(19) . . ? C434 C430 C433 68.1(5) . . ? C435 C430 C433 67.5(4) . . ? C431 C430 C433 104.3(2) . . ? C432 C430 C433 103.9(2) . . ? C43 C430 C433 110.25(19) . . ? C434 C430 C436 100.0(5) . . ? C435 C430 C436 98.5(5) . . ? C431 C430 C436 59.8(3) . . ? C432 C430 C436 64.0(3) . . ? C43 C430 C436 104.4(3) . . ? C433 C430 C436 145.3(3) . . ? C430 C431 H43A 109.5 . . ? C430 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C430 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C430 C432 H43D 109.5 . . ? C430 C432 H43E 109.5 . . ? H43D C432 H43E 109.5 . . ? C430 C432 H43F 109.5 . . ? H43D C432 H43F 109.5 . . ? H43E C432 H43F 109.5 . . ? C430 C433 H43G 109.5 . . ? C430 C433 H43H 109.5 . . ? H43G C433 H43H 109.5 . . ? C430 C433 H43I 109.5 . . ? H43G C433 H43I 109.5 . . ? H43H C433 H43I 109.5 . . ? C430 C434 H43J 109.5 . . ? C430 C434 H43K 109.5 . . ? H43J C434 H43K 109.5 . . ? C430 C434 H43L 109.5 . . ? H43J C434 H43L 109.5 . . ? H43K C434 H43L 109.5 . . ? C430 C435 H43M 109.5 . . ? C430 C435 H43N 109.5 . . ? H43M C435 H43N 109.5 . . ? C430 C435 H43O 109.5 . . ? H43M C435 H43O 109.5 . . ? H43N C435 H43O 109.5 . . ? C430 C436 H43P 109.5 . . ? C430 C436 H43Q 109.5 . . ? H43P C436 H43Q 109.5 . . ? C430 C436 H43R 109.5 . . ? H43P C436 H43R 109.5 . . ? H43Q C436 H43R 109.5 . . ? C451 C450 C453 111.9(3) . . ? C451 C450 C45 112.4(2) . . ? C453 C450 C45 110.68(18) . . ? C451 C450 C452 106.6(2) . . ? C453 C450 C452 106.7(2) . . ? C45 C450 C452 108.27(19) . . ? C450 C451 H45A 109.5 . . ? C450 C451 H45B 109.5 . . ? H45A C451 H45B 109.5 . . ? C450 C451 H45C 109.5 . . ? H45A C451 H45C 109.5 . . ? H45B C451 H45C 109.5 . . ? C450 C452 H45D 109.5 . . ? C450 C452 H45E 109.5 . . ? H45D C452 H45E 109.5 . . ? C450 C452 H45F 109.5 . . ? H45D C452 H45F 109.5 . . ? H45E C452 H45F 109.5 . . ? C450 C453 H45G 109.5 . . ? C450 C453 H45H 109.5 . . ? H45G C453 H45H 109.5 . . ? C450 C453 H45I 109.5 . . ? H45G C453 H45I 109.5 . . ? H45H C453 H45I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.773 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.068 data_halflig _database_code_depnum_ccdc_archive 'CCDC 281978' # Collected as bcn117 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis{1-[2'-(3'',5''-di-tert-butyl-2''-oxyphenethyl)phenyl]-3-p-tolylpropane- 1,3-dionato}titanium(IV) tetrakis (dichloromethane) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C64 H72 O6 Ti, 4 (CH2Cl2)' _chemical_formula_sum 'C68 H80 Cl8 O6 Ti' _chemical_formula_weight 1324.82 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' Cl Cl 0.1484 0.1585 '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 13.1693(5) _cell_length_b 14.4819(6) _cell_length_c 18.8272(8) _cell_angle_alpha 69.077(1) _cell_angle_beta 88.780(2) _cell_angle_gamma 89.507(2) _cell_volume 3353.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9118 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.17 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7826 _exptl_absorpt_correction_T_max 0.9429 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART Apex CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65373 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.33 _reflns_number_total 16402 _reflns_number_gt 12632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^)+(0.0520P)^2^+2.0464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16402 _refine_ls_number_parameters 1068 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Ti Ti 0.22221(2) 0.71570(2) 0.226032(15) 0.01228(7) Uani 1 1 d . . . O1 O 0.37344(9) 0.76067(8) 0.20930(6) 0.0155(2) Uani 1 1 d . . . O2 O 0.22089(8) 0.78615(8) 0.11659(6) 0.0142(2) Uani 1 1 d . . . O3 O 0.09563(8) 0.66389(8) 0.22788(6) 0.0143(2) Uani 1 1 d . . . O4 O 0.28230(9) 0.60190(8) 0.19701(6) 0.0157(2) Uani 1 1 d . . . O5 O 0.26640(9) 0.63029(8) 0.32586(6) 0.0150(2) Uani 1 1 d . . . O6 O 0.19374(9) 0.81682(8) 0.26031(6) 0.0150(2) Uani 1 1 d . . . C1 C 0.42997(12) 0.78408(11) 0.14932(9) 0.0145(3) Uani 1 1 d . . . C2 C 0.39193(13) 0.79877(12) 0.07648(9) 0.0162(3) Uani 1 1 d . . . H2 H 0.4343(17) 0.8092(16) 0.0362(12) 0.024(5) Uiso 1 1 d . . . C3 C 0.28901(13) 0.80095(11) 0.06307(9) 0.0145(3) Uani 1 1 d . . . C4 C 0.10704(13) 0.69131(12) 0.04121(9) 0.0159(3) Uani 1 1 d . . . H4A H 0.0768(15) 0.6450(14) 0.0208(10) 0.014(5) Uiso 1 1 d . . . H4B H 0.1514(15) 0.6580(15) 0.0766(11) 0.016(5) Uiso 1 1 d . . . C5 C 0.02035(13) 0.73340(12) 0.07718(9) 0.0159(3) Uani 1 1 d . . . H5A H 0.0469(15) 0.7862(15) 0.0936(11) 0.017(5) Uiso 1 1 d . . . H5B H -0.0290(16) 0.7654(15) 0.0404(11) 0.021(5) Uiso 1 1 d . . . C6 C 0.34503(12) 0.53336(12) 0.23108(9) 0.0151(3) Uani 1 1 d . . . C7 C 0.37905(13) 0.51526(12) 0.30535(9) 0.0170(3) Uani 1 1 d . . . H7 H 0.4294(16) 0.4643(15) 0.3270(11) 0.018(5) Uiso 1 1 d . . . C8 C 0.33286(12) 0.56109(12) 0.35130(9) 0.0150(3) Uani 1 1 d . . . C9 C 0.33317(13) 0.71053(13) 0.42831(9) 0.0174(3) Uani 1 1 d . . . H9A H 0.3705(15) 0.7459(15) 0.4552(11) 0.019(5) Uiso 1 1 d . . . H9B H 0.3640(15) 0.7305(14) 0.3770(11) 0.016(5) Uiso 1 1 d . . . C10 C 0.22149(13) 0.74595(12) 0.42224(9) 0.0163(3) Uani 1 1 d . . . H10A H 0.1962(14) 0.7382(14) 0.4717(11) 0.013(4) Uiso 1 1 d . . . H10B H 0.1821(15) 0.7048(14) 0.4040(10) 0.012(4) Uiso 1 1 d . . . C11 C 0.53996(12) 0.79577(12) 0.15955(9) 0.0152(3) Uani 1 1 d . . . C12 C 0.57884(14) 0.75899(14) 0.23297(10) 0.0201(3) Uani 1 1 d . . . H12 H 0.5323(17) 0.7283(16) 0.2748(12) 0.026(5) Uiso 1 1 d . . . C13 C 0.68036(14) 0.76960(14) 0.24494(10) 0.0224(4) Uani 1 1 d . . . H13 H 0.7055(17) 0.7446(17) 0.2937(13) 0.031(6) Uiso 1 1 d . . . C14 C 0.74732(13) 0.81726(13) 0.18455(10) 0.0194(3) Uani 1 1 d . . . C15 C 0.70861(14) 0.85291(14) 0.11145(10) 0.0217(4) Uani 1 1 d . . . H15 H 0.7527(18) 0.8849(17) 0.0708(13) 0.030(6) Uiso 1 1 d . . . C16 C 0.60670(14) 0.84282(13) 0.09884(10) 0.0200(3) Uani 1 1 d . . . H16 H 0.5828(16) 0.8702(16) 0.0468(12) 0.027(5) Uiso 1 1 d . . . C17 C 0.85649(14) 0.83223(16) 0.19863(12) 0.0247(4) Uani 1 1 d . . . H17A H 0.8870(19) 0.7732(19) 0.2316(14) 0.040(7) Uiso 1 1 d . . . H17B H 0.8950(19) 0.8540(19) 0.1551(14) 0.040(7) Uiso 1 1 d . . . H17C H 0.8607(18) 0.8809(19) 0.2210(13) 0.038(7) Uiso 1 1 d . . . C21 C 0.24781(13) 0.82147(12) -0.01412(9) 0.0153(3) Uani 1 1 d . . . C22 C 0.16146(13) 0.77043(12) -0.02326(9) 0.0161(3) Uani 1 1 d . . . C23 C 0.12456(14) 0.79392(14) -0.09655(9) 0.0193(3) Uani 1 1 d . . . H23 H 0.0716(16) 0.7608(15) -0.1027(11) 0.017(5) Uiso 1 1 d . . . C24 C 0.16933(15) 0.86659(14) -0.15886(10) 0.0229(4) Uani 1 1 d . . . H24 H 0.1433(18) 0.8789(17) -0.2041(13) 0.034(6) Uiso 1 1 d . . . C25 C 0.25345(15) 0.91676(14) -0.14950(10) 0.0225(4) Uani 1 1 d . . . H25 H 0.2847(16) 0.9646(16) -0.1879(12) 0.022(5) Uiso 1 1 d . . . C26 C 0.29375(14) 0.89332(13) -0.07744(9) 0.0189(3) Uani 1 1 d . . . H26 H 0.3510(16) 0.9281(15) -0.0718(11) 0.020(5) Uiso 1 1 d . . . C31 C 0.01163(12) 0.61810(12) 0.21566(9) 0.0141(3) Uani 1 1 d . . . C32 C -0.03090(13) 0.65353(12) 0.14264(9) 0.0156(3) Uani 1 1 d . . . C33 C -0.11960(13) 0.61131(13) 0.13003(9) 0.0176(3) Uani 1 1 d . . . H33 H -0.1434(17) 0.6378(16) 0.0798(12) 0.027(5) Uiso 1 1 d . . . C34 C -0.16944(13) 0.53452(12) 0.18708(9) 0.0168(3) Uani 1 1 d . . . C35 C -0.12424(13) 0.50012(13) 0.25812(9) 0.0165(3) Uani 1 1 d . . . H35 H -0.1562(16) 0.4463(16) 0.2978(11) 0.021(5) Uiso 1 1 d . . . C36 C -0.03472(12) 0.53796(12) 0.27496(9) 0.0146(3) Uani 1 1 d . . . C41 C 0.37770(12) 0.46917(12) 0.18835(9) 0.0159(3) Uani 1 1 d . . . C42 C 0.36888(14) 0.50385(13) 0.10928(10) 0.0207(4) Uani 1 1 d . . . H42 H 0.3424(15) 0.5696(15) 0.0834(11) 0.016(5) Uiso 1 1 d . . . C43 C 0.39961(15) 0.44562(14) 0.06819(10) 0.0237(4) Uani 1 1 d . . . H43 H 0.3920(17) 0.4708(17) 0.0126(13) 0.031(6) Uiso 1 1 d . . . C44 C 0.43826(14) 0.35084(14) 0.10476(10) 0.0229(4) Uani 1 1 d . . . C45 C 0.44503(15) 0.31591(14) 0.18351(10) 0.0234(4) Uani 1 1 d . . . H45 H 0.4688(17) 0.2500(18) 0.2088(12) 0.031(6) Uiso 1 1 d . . . C46 C 0.41567(14) 0.37415(13) 0.22503(10) 0.0199(3) Uani 1 1 d . . . H46 H 0.4234(15) 0.3477(15) 0.2793(11) 0.017(5) Uiso 1 1 d . . . C47 C 0.4722(2) 0.28758(18) 0.06003(13) 0.0343(5) Uani 1 1 d . . . H47A H 0.430(3) 0.226(3) 0.069(2) 0.098(13) Uiso 1 1 d . . . H47B H 0.535(3) 0.258(3) 0.076(2) 0.086(11) Uiso 1 1 d . . . H47C H 0.482(2) 0.320(2) 0.0096(18) 0.058(8) Uiso 1 1 d . . . C51 C 0.35119(12) 0.53058(13) 0.43408(9) 0.0166(3) Uani 1 1 d . . . C52 C 0.34562(13) 0.60048(13) 0.47051(9) 0.0168(3) Uani 1 1 d . . . C53 C 0.35608(14) 0.56567(14) 0.54948(9) 0.0213(4) Uani 1 1 d . . . H53 H 0.3538(17) 0.6165(16) 0.5738(12) 0.028(6) Uiso 1 1 d . . . C54 C 0.37140(15) 0.46622(14) 0.59114(10) 0.0243(4) Uani 1 1 d . . . H54 H 0.3759(16) 0.4434(16) 0.6470(12) 0.026(5) Uiso 1 1 d . . . C55 C 0.37919(15) 0.39847(14) 0.55453(10) 0.0242(4) Uani 1 1 d . . . H55 H 0.3914(17) 0.3294(17) 0.5808(12) 0.028(6) Uiso 1 1 d . . . C56 C 0.36901(14) 0.43060(13) 0.47648(10) 0.0203(4) Uani 1 1 d . . . H56 H 0.3692(17) 0.3811(17) 0.4522(12) 0.029(6) Uiso 1 1 d . . . C61 C 0.20054(12) 0.88596(12) 0.29355(9) 0.0143(3) Uani 1 1 d . . . C62 C 0.21175(12) 0.85388(12) 0.37312(9) 0.0155(3) Uani 1 1 d . . . C63 C 0.21758(13) 0.92407(13) 0.40795(9) 0.0172(3) Uani 1 1 d . . . H63 H 0.2242(16) 0.8986(15) 0.4611(12) 0.022(5) Uiso 1 1 d . . . C64 C 0.21259(13) 1.02504(13) 0.36713(9) 0.0173(3) Uani 1 1 d . . . C65 C 0.20073(13) 1.05424(13) 0.28849(9) 0.0175(3) Uani 1 1 d . . . H65 H 0.1939(17) 1.1195(17) 0.2602(12) 0.026(5) Uiso 1 1 d . . . C66 C 0.19455(12) 0.98839(12) 0.24953(9) 0.0155(3) Uani 1 1 d . . . C340 C -0.26680(13) 0.48931(13) 0.17120(10) 0.0189(3) Uani 1 1 d . . . C341 C -0.3206(2) 0.4241(3) 0.24428(14) 0.0480(7) Uani 1 1 d . . . H34A H -0.334(2) 0.467(2) 0.2705(18) 0.069(10) Uiso 1 1 d . . . H34B H -0.277(3) 0.369(3) 0.274(2) 0.096(12) Uiso 1 1 d . . . H34C H -0.383(2) 0.399(2) 0.2307(16) 0.058(8) Uiso 1 1 d . . . C342 C -0.34073(16) 0.57089(17) 0.12819(14) 0.0323(5) Uani 1 1 d . . . H34D H -0.4055(19) 0.5444(17) 0.1207(13) 0.034(6) Uiso 1 1 d . . . H34E H -0.354(2) 0.618(2) 0.1550(16) 0.061(8) Uiso 1 1 d . . . H34F H -0.315(2) 0.610(2) 0.0785(16) 0.047(7) Uiso 1 1 d . . . C343 C -0.24110(18) 0.4261(2) 0.12329(16) 0.0385(5) Uani 1 1 d . . . H34G H -0.198(2) 0.369(2) 0.1505(16) 0.061(9) Uiso 1 1 d . . . H34H H -0.306(2) 0.3962(19) 0.1141(14) 0.041(7) Uiso 1 1 d . . . H34I H -0.207(2) 0.470(2) 0.0745(17) 0.060(9) Uiso 1 1 d . . . C360 C 0.01175(13) 0.49131(12) 0.35410(9) 0.0159(3) Uani 1 1 d . . . C361 C -0.05380(15) 0.40753(14) 0.40862(10) 0.0212(4) Uani 1 1 d . . . H36A H -0.0604(16) 0.3536(16) 0.3900(12) 0.025(5) Uiso 1 1 d . . . H36B H -0.1160(18) 0.4303(16) 0.4177(12) 0.028(6) Uiso 1 1 d . . . H36C H -0.0183(16) 0.3808(15) 0.4579(12) 0.024(5) Uiso 1 1 d . . . C362 C 0.11503(14) 0.44522(13) 0.34604(10) 0.0185(3) Uani 1 1 d . . . H36D H 0.1458(17) 0.4252(17) 0.3939(13) 0.030(6) Uiso 1 1 d . . . H36E H 0.1044(16) 0.3876(16) 0.3320(11) 0.024(5) Uiso 1 1 d . . . H36F H 0.1579(16) 0.4914(15) 0.3084(11) 0.017(5) Uiso 1 1 d . . . C363 C 0.02273(15) 0.56944(14) 0.39116(10) 0.0205(4) Uani 1 1 d . . . H36G H -0.0468(17) 0.5922(16) 0.4027(12) 0.028(6) Uiso 1 1 d . . . H36H H 0.0591(17) 0.5387(16) 0.4388(12) 0.028(6) Uiso 1 1 d . . . H36I H 0.0627(16) 0.6275(15) 0.3592(11) 0.018(5) Uiso 1 1 d . . . C640 C 0.21498(14) 1.10163(13) 0.40607(9) 0.0198(3) Uani 1 1 d . . . C641 C 0.26949(18) 1.19590(15) 0.35593(12) 0.0291(4) Uani 1 1 d . . . H64A H 0.2737(19) 1.2435(19) 0.3835(14) 0.043(7) Uiso 1 1 d . . . H64B H 0.2320(18) 1.2302(18) 0.3093(14) 0.036(6) Uiso 1 1 d . . . H64C H 0.338(2) 1.1794(19) 0.3459(14) 0.044(7) Uiso 1 1 d . . . C642 C 0.27031(19) 1.06141(16) 0.48202(12) 0.0317(5) Uani 1 1 d . . . H64D H 0.2758(18) 1.1149(18) 0.5030(13) 0.034(6) Uiso 1 1 d . . . H64E H 0.2350(19) 1.0020(19) 0.5200(14) 0.037(6) Uiso 1 1 d . . . H64F H 0.3365(19) 1.0380(18) 0.4755(13) 0.034(6) Uiso 1 1 d . . . C643 C 0.10487(16) 1.12708(16) 0.42136(11) 0.0263(4) Uani 1 1 d . . . H64G H 0.1016(17) 1.1760(17) 0.4465(12) 0.028(6) Uiso 1 1 d . . . H64H H 0.0691(19) 1.0702(19) 0.4573(14) 0.040(7) Uiso 1 1 d . . . H64I H 0.0681(18) 1.1521(17) 0.3738(14) 0.035(6) Uiso 1 1 d . . . C660 C 0.18267(13) 1.02774(12) 0.16250(9) 0.0178(3) Uani 1 1 d . . . C661 C 0.17233(17) 1.14080(14) 0.12920(10) 0.0247(4) Uani 1 1 d . . . H66A H 0.1126(18) 1.1614(17) 0.1506(12) 0.030(6) Uiso 1 1 d . . . H66B H 0.2314(17) 1.1760(16) 0.1405(11) 0.023(5) Uiso 1 1 d . . . H66C H 0.1648(15) 1.1622(15) 0.0746(12) 0.020(5) Uiso 1 1 d . . . C662 C 0.27834(15) 1.00142(14) 0.12503(10) 0.0199(4) Uani 1 1 d . . . H66D H 0.2746(17) 1.0203(17) 0.0716(13) 0.030(6) Uiso 1 1 d . . . H66E H 0.3356(18) 1.0405(17) 0.1302(13) 0.033(6) Uiso 1 1 d . . . H66F H 0.2975(16) 0.9297(16) 0.1475(11) 0.020(5) Uiso 1 1 d . . . C663 C 0.08669(15) 0.98464(15) 0.14145(11) 0.0230(4) Uani 1 1 d . . . H66G H 0.0821(18) 1.0097(18) 0.0878(14) 0.035(6) Uiso 1 1 d . . . H66H H 0.0881(16) 0.9141(16) 0.1587(11) 0.020(5) Uiso 1 1 d . . . H66I H 0.0293(18) 1.0055(17) 0.1621(12) 0.029(6) Uiso 1 1 d . . . C71 C 0.68992(19) 0.1485(2) 0.33534(14) 0.0406(5) Uani 1 1 d . . . H71A H 0.676(2) 0.183(2) 0.2836(16) 0.051(8) Uiso 1 1 d . . . H71B H 0.688(2) 0.078(2) 0.3484(16) 0.061(9) Uiso 1 1 d . . . Cl11 Cl 0.59113(5) 0.17839(5) 0.38819(4) 0.04992(16) Uani 1 1 d . . . Cl12 Cl 0.81007(5) 0.18202(4) 0.35805(3) 0.04254(13) Uani 1 1 d . . . C72 C 0.0787(2) 0.41229(17) 0.15965(13) 0.0366(5) Uani 1 1 d . . . H72A H 0.028(2) 0.465(2) 0.1564(16) 0.058(8) Uiso 1 1 d . . . H72B H 0.143(3) 0.420(2) 0.1786(18) 0.074(10) Uiso 1 1 d . . . Cl21 Cl 0.02333(4) 0.30223(4) 0.22273(3) 0.03053(11) Uani 1 1 d . . . Cl22 Cl 0.09912(5) 0.40914(4) 0.06779(3) 0.04008(13) Uani 1 1 d . . . C73 C -0.04722(16) 0.82669(16) 0.38940(13) 0.0313(4) Uani 1 1 d . . . H73A H -0.002(2) 0.814(2) 0.4304(15) 0.050(8) Uiso 1 1 d . . . H73B H -0.0145(19) 0.8058(18) 0.3493(14) 0.041(7) Uiso 1 1 d . . . Cl31 Cl -0.07286(5) 0.95416(4) 0.35308(3) 0.03810(13) Uani 1 1 d . . . Cl32 Cl -0.15905(4) 0.75550(4) 0.42176(3) 0.03063(11) Uani 1 1 d . . . C74 C 0.45986(16) -0.06110(16) 0.30837(12) 0.0309(4) Uani 1 1 d . . . H74A H 0.399(2) -0.0423(18) 0.3307(13) 0.040(7) Uiso 1 1 d . . . H74B H 0.4511(19) -0.1141(19) 0.2888(14) 0.041(7) Uiso 1 1 d . . . Cl41 Cl 0.55147(5) -0.10412(5) 0.37998(4) 0.05217(17) Uani 1 1 d . . . Cl42 Cl 0.50421(5) 0.04415(4) 0.23375(3) 0.04487(14) 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 Ti 0.01235(14) 0.01317(14) 0.01154(13) -0.00469(10) 0.00045(10) -0.00081(11) O1 0.0139(6) 0.0173(6) 0.0147(5) -0.0050(4) 0.0011(4) -0.0010(5) O2 0.0138(6) 0.0155(5) 0.0128(5) -0.0046(4) 0.0011(4) -0.0014(4) O3 0.0124(6) 0.0167(6) 0.0144(5) -0.0063(4) -0.0002(4) -0.0024(4) O4 0.0163(6) 0.0152(6) 0.0158(5) -0.0061(4) 0.0004(4) 0.0010(5) O5 0.0149(6) 0.0157(6) 0.0135(5) -0.0041(4) 0.0007(4) 0.0000(4) O6 0.0160(6) 0.0158(6) 0.0139(5) -0.0062(4) 0.0005(4) -0.0013(5) C1 0.0149(8) 0.0118(7) 0.0169(7) -0.0055(6) 0.0015(6) -0.0001(6) C2 0.0149(8) 0.0185(8) 0.0153(7) -0.0065(6) 0.0032(6) -0.0007(6) C3 0.0179(8) 0.0119(7) 0.0132(7) -0.0040(6) 0.0016(6) -0.0001(6) C4 0.0171(8) 0.0162(8) 0.0150(7) -0.0061(6) -0.0018(6) -0.0014(7) C5 0.0147(8) 0.0162(8) 0.0154(7) -0.0037(6) -0.0017(6) 0.0000(6) C6 0.0111(8) 0.0152(8) 0.0178(7) -0.0045(6) 0.0032(6) -0.0027(6) C7 0.0154(8) 0.0174(8) 0.0170(7) -0.0048(6) -0.0002(6) 0.0016(7) C8 0.0123(8) 0.0149(8) 0.0165(7) -0.0038(6) -0.0002(6) -0.0033(6) C9 0.0174(8) 0.0185(8) 0.0158(7) -0.0053(6) -0.0005(6) -0.0032(7) C10 0.0179(8) 0.0174(8) 0.0140(7) -0.0060(6) 0.0031(6) -0.0043(7) C11 0.0142(8) 0.0139(7) 0.0181(7) -0.0065(6) 0.0006(6) 0.0006(6) C12 0.0162(8) 0.0244(9) 0.0182(8) -0.0060(7) 0.0013(6) -0.0011(7) C13 0.0188(9) 0.0294(10) 0.0178(8) -0.0068(7) -0.0023(7) -0.0006(7) C14 0.0151(8) 0.0221(9) 0.0241(8) -0.0122(7) 0.0008(6) -0.0006(7) C15 0.0177(9) 0.0249(9) 0.0215(8) -0.0073(7) 0.0052(7) -0.0054(7) C16 0.0191(9) 0.0223(9) 0.0168(8) -0.0047(7) 0.0007(6) -0.0015(7) C17 0.0142(9) 0.0337(11) 0.0300(10) -0.0162(9) -0.0003(7) -0.0020(8) C21 0.0160(8) 0.0163(8) 0.0140(7) -0.0061(6) 0.0006(6) 0.0024(6) C22 0.0169(8) 0.0166(8) 0.0154(7) -0.0066(6) 0.0006(6) 0.0026(6) C23 0.0190(9) 0.0230(9) 0.0175(8) -0.0091(7) -0.0026(6) 0.0001(7) C24 0.0262(10) 0.0286(10) 0.0128(7) -0.0062(7) -0.0027(7) 0.0051(8) C25 0.0255(10) 0.0224(9) 0.0151(8) -0.0015(7) 0.0033(7) 0.0008(7) C26 0.0187(9) 0.0193(8) 0.0174(8) -0.0053(6) 0.0019(6) -0.0002(7) C31 0.0120(8) 0.0152(8) 0.0169(7) -0.0079(6) 0.0002(6) -0.0004(6) C32 0.0152(8) 0.0157(8) 0.0160(7) -0.0056(6) 0.0008(6) 0.0007(6) C33 0.0163(8) 0.0194(8) 0.0166(7) -0.0057(6) -0.0017(6) 0.0015(7) C34 0.0130(8) 0.0188(8) 0.0202(8) -0.0090(6) 0.0000(6) -0.0007(6) C35 0.0152(8) 0.0172(8) 0.0174(7) -0.0066(6) 0.0022(6) -0.0014(6) C36 0.0146(8) 0.0147(7) 0.0150(7) -0.0060(6) 0.0011(6) -0.0002(6) C41 0.0119(8) 0.0174(8) 0.0188(7) -0.0069(6) 0.0023(6) -0.0020(6) C42 0.0217(9) 0.0209(9) 0.0197(8) -0.0076(7) -0.0007(7) 0.0037(7) C43 0.0252(10) 0.0283(10) 0.0196(8) -0.0110(7) -0.0014(7) 0.0054(8) C44 0.0222(9) 0.0247(9) 0.0254(9) -0.0134(7) 0.0007(7) 0.0027(7) C45 0.0264(10) 0.0189(9) 0.0251(9) -0.0079(7) -0.0004(7) 0.0044(7) C46 0.0197(9) 0.0205(9) 0.0194(8) -0.0071(7) 0.0014(6) 0.0015(7) C47 0.0460(14) 0.0319(11) 0.0300(11) -0.0176(9) -0.0003(9) 0.0142(10) C51 0.0132(8) 0.0202(8) 0.0146(7) -0.0040(6) -0.0001(6) -0.0014(6) C52 0.0127(8) 0.0196(8) 0.0161(7) -0.0039(6) -0.0010(6) -0.0019(6) C53 0.0221(9) 0.0246(9) 0.0165(8) -0.0063(7) -0.0025(6) -0.0009(7) C54 0.0250(10) 0.0283(10) 0.0159(8) -0.0032(7) -0.0035(7) 0.0008(8) C55 0.0244(10) 0.0218(9) 0.0207(8) -0.0007(7) -0.0027(7) 0.0022(8) C56 0.0189(9) 0.0210(9) 0.0195(8) -0.0053(7) -0.0008(6) 0.0011(7) C61 0.0100(7) 0.0176(8) 0.0170(7) -0.0085(6) 0.0023(6) -0.0013(6) C62 0.0127(8) 0.0181(8) 0.0166(7) -0.0072(6) 0.0024(6) -0.0018(6) C63 0.0173(8) 0.0210(8) 0.0144(7) -0.0078(6) 0.0018(6) -0.0013(7) C64 0.0148(8) 0.0206(8) 0.0189(8) -0.0102(7) 0.0015(6) -0.0010(7) C65 0.0183(9) 0.0145(8) 0.0201(8) -0.0068(6) 0.0001(6) 0.0012(7) C66 0.0127(8) 0.0184(8) 0.0154(7) -0.0062(6) 0.0011(6) -0.0004(6) C340 0.0141(8) 0.0219(9) 0.0216(8) -0.0087(7) -0.0016(6) -0.0025(7) C341 0.0342(13) 0.0694(19) 0.0294(11) -0.0032(12) -0.0041(10) -0.0302(13) C342 0.0188(10) 0.0296(11) 0.0498(13) -0.0151(10) -0.0123(9) 0.0021(8) C343 0.0224(11) 0.0438(13) 0.0669(16) -0.0409(13) -0.0052(11) -0.0007(10) C360 0.0155(8) 0.0173(8) 0.0143(7) -0.0050(6) 0.0002(6) -0.0025(6) C361 0.0219(9) 0.0219(9) 0.0162(8) -0.0025(7) 0.0008(7) -0.0062(7) C362 0.0186(9) 0.0185(8) 0.0170(8) -0.0046(7) -0.0016(7) -0.0007(7) C363 0.0237(9) 0.0230(9) 0.0166(8) -0.0093(7) 0.0021(7) -0.0045(8) C640 0.0226(9) 0.0198(8) 0.0194(8) -0.0100(7) -0.0004(7) -0.0005(7) C641 0.0360(12) 0.0241(10) 0.0321(10) -0.0161(8) 0.0050(9) -0.0074(9) C642 0.0446(13) 0.0273(10) 0.0302(10) -0.0181(9) -0.0135(9) 0.0063(10) C643 0.0280(10) 0.0287(10) 0.0281(10) -0.0176(8) 0.0034(8) 0.0017(8) C660 0.0211(9) 0.0169(8) 0.0153(7) -0.0055(6) -0.0018(6) 0.0021(7) C661 0.0354(11) 0.0187(9) 0.0190(8) -0.0053(7) -0.0039(8) 0.0055(8) C662 0.0243(10) 0.0189(9) 0.0153(8) -0.0046(6) 0.0030(7) -0.0013(7) C663 0.0221(10) 0.0245(10) 0.0241(9) -0.0105(7) -0.0072(7) 0.0050(8) C71 0.0396(14) 0.0441(14) 0.0395(12) -0.0163(11) -0.0012(10) -0.0122(11) Cl11 0.0421(3) 0.0477(4) 0.0513(3) -0.0074(3) 0.0059(3) -0.0020(3) Cl12 0.0396(3) 0.0427(3) 0.0446(3) -0.0143(2) -0.0011(2) -0.0111(2) C72 0.0470(14) 0.0343(12) 0.0351(11) -0.0208(9) 0.0053(10) -0.0088(11) Cl21 0.0418(3) 0.0268(2) 0.0256(2) -0.01233(18) -0.00532(19) 0.0038(2) Cl22 0.0595(4) 0.0327(3) 0.0298(2) -0.0135(2) 0.0022(2) -0.0060(3) C73 0.0232(10) 0.0345(11) 0.0374(11) -0.0141(9) -0.0013(9) 0.0004(9) Cl31 0.0446(3) 0.0316(3) 0.0363(3) -0.0101(2) 0.0023(2) -0.0009(2) Cl32 0.0251(2) 0.0345(3) 0.0370(2) -0.0186(2) 0.00118(19) -0.0016(2) C74 0.0238(10) 0.0279(10) 0.0386(11) -0.0091(9) 0.0019(8) -0.0054(8) Cl41 0.0526(4) 0.0374(3) 0.0565(4) -0.0030(3) -0.0234(3) -0.0098(3) Cl42 0.0376(3) 0.0365(3) 0.0480(3) 0.0007(2) -0.0020(2) -0.0142(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 Ti O3 1.8284(12) . y Ti O6 1.8322(11) . y Ti O5 1.9429(11) . y Ti O2 1.9459(11) . y Ti O4 2.0599(11) . y Ti O1 2.0831(12) . y O1 C1 1.2805(19) . ? O2 C3 1.2948(19) . ? O3 C31 1.360(2) . ? O4 C6 1.2778(19) . ? O5 C8 1.2882(19) . ? O6 C61 1.3615(19) . ? C1 C2 1.413(2) . ? C1 C11 1.484(2) . ? C2 C3 1.382(2) . ? C2 H2 0.90(2) . ? C3 C21 1.489(2) . ? C4 C22 1.511(2) . ? C4 C5 1.544(2) . ? C4 H4A 0.98(2) . ? C4 H4B 0.89(2) . ? C5 C32 1.507(2) . ? C5 H5A 0.99(2) . ? C5 H5B 0.95(2) . ? C6 C7 1.410(2) . ? C6 C41 1.486(2) . ? C7 C8 1.393(2) . ? C7 H7 0.97(2) . ? C8 C51 1.485(2) . ? C9 C52 1.515(2) . ? C9 C10 1.546(2) . ? C9 H9A 0.98(2) . ? C9 H9B 0.984(19) . ? C10 C62 1.511(2) . ? C10 H10A 0.950(19) . ? C10 H10B 0.95(2) . ? C11 C16 1.398(2) . ? C11 C12 1.399(2) . ? C12 C13 1.379(3) . ? C12 H12 0.96(2) . ? C13 C14 1.398(2) . ? C13 H13 0.93(2) . ? C14 C15 1.392(2) . ? C14 C17 1.499(3) . ? C15 C16 1.386(3) . ? C15 H15 0.93(2) . ? C16 H16 0.97(2) . ? C17 H17A 0.95(3) . ? C17 H17B 0.91(3) . ? C17 H17C 0.94(3) . ? C21 C26 1.401(2) . ? C21 C22 1.408(2) . ? C22 C23 1.395(2) . ? C23 C24 1.390(3) . ? C23 H23 0.88(2) . ? C24 C25 1.378(3) . ? C24 H24 0.88(2) . ? C25 C26 1.391(2) . ? C25 H25 0.90(2) . ? C26 H26 0.94(2) . ? C31 C32 1.411(2) . ? C31 C36 1.423(2) . ? C32 C33 1.386(2) . ? C33 C34 1.397(2) . ? C33 H33 0.94(2) . ? C34 C35 1.394(2) . ? C34 C340 1.527(2) . ? C35 C36 1.394(2) . ? C35 H35 0.96(2) . ? C36 C360 1.537(2) . ? C41 C46 1.394(2) . ? C41 C42 1.398(2) . ? C42 C43 1.386(2) . ? C42 H42 0.97(2) . ? C43 C44 1.395(3) . ? C43 H43 0.98(2) . ? C44 C45 1.390(3) . ? C44 C47 1.509(2) . ? C45 C46 1.387(2) . ? C45 H45 0.95(2) . ? C46 H46 0.962(19) . ? C47 H47A 1.01(4) . ? C47 H47B 0.94(4) . ? C47 H47C 0.90(3) . ? C51 C56 1.402(2) . ? C51 C52 1.412(2) . ? C52 C53 1.399(2) . ? C53 C54 1.387(3) . ? C53 H53 1.00(2) . ? C54 C55 1.388(3) . ? C54 H54 0.99(2) . ? C55 C56 1.383(2) . ? C55 H55 0.96(2) . ? C56 H56 0.98(2) . ? C61 C62 1.412(2) . ? C61 C66 1.420(2) . ? C62 C63 1.396(2) . ? C63 C64 1.390(2) . ? C63 H63 0.94(2) . ? C64 C65 1.399(2) . ? C64 C640 1.533(2) . ? C65 C66 1.399(2) . ? C65 H65 0.91(2) . ? C66 C660 1.542(2) . ? C340 C341 1.526(3) . ? C340 C342 1.526(3) . ? C340 C343 1.529(3) . ? C341 H34A 0.94(3) . ? C341 H34B 0.98(4) . ? C341 H34C 0.98(3) . ? C342 H34D 0.97(3) . ? C342 H34E 0.99(3) . ? C342 H34F 0.96(3) . ? C343 H34G 0.98(3) . ? C343 H34H 1.00(3) . ? C343 H34I 1.01(3) . ? C360 C363 1.536(2) . ? C360 C361 1.537(2) . ? C360 C362 1.538(2) . ? C361 H36A 0.97(2) . ? C361 H36B 0.92(2) . ? C361 H36C 0.99(2) . ? C362 H36D 0.94(2) . ? C362 H36E 0.97(2) . ? C362 H36F 0.96(2) . ? C363 H36G 1.02(2) . ? C363 H36H 0.98(2) . ? C363 H36I 0.99(2) . ? C640 C641 1.529(3) . ? C640 C642 1.535(3) . ? C640 C643 1.540(3) . ? C641 H64A 1.00(3) . ? C641 H64B 0.98(2) . ? C641 H64C 0.97(3) . ? C642 H64D 0.99(2) . ? C642 H64E 1.01(3) . ? C642 H64F 0.95(2) . ? C643 H64G 0.98(2) . ? C643 H64H 0.98(3) . ? C643 H64I 0.98(2) . ? C660 C663 1.535(3) . ? C660 C661 1.536(2) . ? C660 C662 1.541(2) . ? C661 H66A 0.97(2) . ? C661 H66B 1.00(2) . ? C661 H66C 0.97(2) . ? C662 H66D 0.95(2) . ? C662 H66E 0.97(3) . ? C662 H66F 1.00(2) . ? C663 H66G 0.95(2) . ? C663 H66H 0.95(2) . ? C663 H66I 0.94(2) . ? C71 Cl12 1.764(3) . ? C71 Cl11 1.765(3) . ? C71 H71A 0.94(3) . ? C71 H71B 0.97(3) . ? C72 Cl22 1.761(2) . ? C72 Cl21 1.765(2) . ? C72 H72A 1.00(3) . ? C72 H72B 0.95(3) . ? C73 Cl31 1.757(2) . ? C73 Cl32 1.773(2) . ? C73 H73A 0.95(3) . ? C73 H73B 1.00(2) . ? C74 Cl42 1.758(2) . ? C74 Cl41 1.766(2) . ? C74 H74A 0.97(3) . ? C74 H74B 0.97(3) . ? 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 O3 Ti O6 101.15(5) . . y O3 Ti O5 98.88(5) . . y O6 Ti O5 91.84(5) . . y O3 Ti O2 92.98(5) . . y O6 Ti O2 100.65(5) . . y O5 Ti O2 160.81(5) . . y O3 Ti O4 89.05(5) . . y O6 Ti O4 168.46(5) . . y O5 Ti O4 81.16(5) . . y O2 Ti O4 84.03(4) . . y O3 Ti O1 168.83(5) . . y O6 Ti O1 89.37(5) . . y O5 Ti O1 84.39(5) . . y O2 Ti O1 81.27(5) . . y O4 Ti O1 80.87(5) . . y C1 O1 Ti 130.03(11) . . ? C3 O2 Ti 133.16(10) . . ? C31 O3 Ti 165.86(10) . . y C6 O4 Ti 131.32(10) . . ? C8 O5 Ti 135.71(10) . . ? C61 O6 Ti 163.25(11) . . y O1 C1 C2 123.04(15) . . ? O1 C1 C11 116.45(14) . . ? C2 C1 C11 120.51(14) . . ? C3 C2 C1 122.08(15) . . ? C3 C2 H2 117.0(14) . . ? C1 C2 H2 120.9(14) . . ? O2 C3 C2 122.57(14) . . ? O2 C3 C21 114.79(14) . . ? C2 C3 C21 122.63(14) . . ? C22 C4 C5 112.60(13) . . ? C22 C4 H4A 108.1(11) . . ? C5 C4 H4A 107.5(11) . . ? C22 C4 H4B 110.0(13) . . ? C5 C4 H4B 110.4(12) . . ? H4A C4 H4B 108.1(17) . . ? C32 C5 C4 111.60(13) . . ? C32 C5 H5A 110.9(11) . . ? C4 C5 H5A 109.9(11) . . ? C32 C5 H5B 108.9(13) . . ? C4 C5 H5B 110.6(12) . . ? H5A C5 H5B 104.7(16) . . ? O4 C6 C7 123.59(14) . . ? O4 C6 C41 115.44(14) . . ? C7 C6 C41 120.92(14) . . ? C8 C7 C6 120.88(15) . . ? C8 C7 H7 119.2(11) . . ? C6 C7 H7 119.5(11) . . ? O5 C8 C7 122.31(14) . . ? O5 C8 C51 114.50(14) . . ? C7 C8 C51 123.09(14) . . ? C52 C9 C10 113.74(14) . . ? C52 C9 H9A 108.5(12) . . ? C10 C9 H9A 108.0(12) . . ? C52 C9 H9B 110.9(11) . . ? C10 C9 H9B 109.2(11) . . ? H9A C9 H9B 106.2(16) . . ? C62 C10 C9 111.91(14) . . ? C62 C10 H10A 107.7(11) . . ? C9 C10 H10A 108.8(11) . . ? C62 C10 H10B 112.0(11) . . ? C9 C10 H10B 108.9(11) . . ? H10A C10 H10B 107.5(16) . . ? C16 C11 C12 118.28(16) . . ? C16 C11 C1 122.80(15) . . ? C12 C11 C1 118.91(15) . . ? C13 C12 C11 120.65(16) . . ? C13 C12 H12 121.3(13) . . ? C11 C12 H12 118.0(13) . . ? C12 C13 C14 121.34(16) . . ? C12 C13 H13 120.0(14) . . ? C14 C13 H13 118.6(14) . . ? C15 C14 C13 117.88(16) . . ? C15 C14 C17 121.26(17) . . ? C13 C14 C17 120.83(16) . . ? C16 C15 C14 121.22(16) . . ? C16 C15 H15 120.2(14) . . ? C14 C15 H15 118.5(14) . . ? C15 C16 C11 120.62(16) . . ? C15 C16 H16 118.3(13) . . ? C11 C16 H16 121.1(13) . . ? C14 C17 H17A 112.1(16) . . ? C14 C17 H17B 112.9(16) . . ? H17A C17 H17B 107(2) . . ? C14 C17 H17C 109.2(15) . . ? H17A C17 H17C 108(2) . . ? H17B C17 H17C 107(2) . . ? C26 C21 C22 120.06(15) . . ? C26 C21 C3 119.85(16) . . ? C22 C21 C3 120.07(14) . . ? C23 C22 C21 117.83(16) . . ? C23 C22 C4 118.10(16) . . ? C21 C22 C4 124.07(14) . . ? C24 C23 C22 121.79(18) . . ? C24 C23 H23 120.1(13) . . ? C22 C23 H23 118.1(13) . . ? C25 C24 C23 120.12(16) . . ? C25 C24 H24 121.3(16) . . ? C23 C24 H24 118.5(16) . . ? C24 C25 C26 119.52(17) . . ? C24 C25 H25 123.4(14) . . ? C26 C25 H25 117.1(14) . . ? C25 C26 C21 120.64(18) . . ? C25 C26 H26 118.7(12) . . ? C21 C26 H26 120.6(12) . . ? O3 C31 C32 118.40(14) . . ? O3 C31 C36 121.48(14) . . ? C32 C31 C36 120.10(15) . . ? C33 C32 C31 119.34(15) . . ? C33 C32 C5 119.21(14) . . ? C31 C32 C5 121.41(15) . . ? C32 C33 C34 122.57(15) . . ? C32 C33 H33 115.0(14) . . ? C34 C33 H33 122.4(14) . . ? C35 C34 C33 116.52(16) . . ? C35 C34 C340 122.20(15) . . ? C33 C34 C340 121.26(15) . . ? C36 C35 C34 124.25(16) . . ? C36 C35 H35 117.7(12) . . ? C34 C35 H35 118.0(12) . . ? C35 C36 C31 117.17(14) . . ? C35 C36 C360 120.16(14) . . ? C31 C36 C360 122.65(15) . . ? C46 C41 C42 118.69(15) . . ? C46 C41 C6 121.85(14) . . ? C42 C41 C6 119.46(14) . . ? C43 C42 C41 120.48(16) . . ? C43 C42 H42 120.2(11) . . ? C41 C42 H42 119.3(11) . . ? C42 C43 C44 120.87(16) . . ? C42 C43 H43 119.5(13) . . ? C44 C43 H43 119.6(13) . . ? C45 C44 C43 118.45(16) . . ? C45 C44 C47 120.63(17) . . ? C43 C44 C47 120.92(17) . . ? C46 C45 C44 121.07(16) . . ? C46 C45 H45 120.4(13) . . ? C44 C45 H45 118.6(13) . . ? C45 C46 C41 120.42(16) . . ? C45 C46 H46 118.2(12) . . ? C41 C46 H46 121.3(12) . . ? C44 C47 H47A 115(2) . . ? C44 C47 H47B 112(2) . . ? H47A C47 H47B 99(3) . . ? C44 C47 H47C 115.7(19) . . ? H47A C47 H47C 110(3) . . ? H47B C47 H47C 103(3) . . ? C56 C51 C52 120.23(15) . . ? C56 C51 C8 119.23(15) . . ? C52 C51 C8 120.46(14) . . ? C53 C52 C51 117.60(15) . . ? C53 C52 C9 118.87(15) . . ? C51 C52 C9 123.48(14) . . ? C54 C53 C52 121.71(17) . . ? C54 C53 H53 122.0(12) . . ? C52 C53 H53 116.2(12) . . ? C53 C54 C55 120.20(16) . . ? C53 C54 H54 120.0(13) . . ? C55 C54 H54 119.8(13) . . ? C56 C55 C54 119.43(17) . . ? C56 C55 H55 117.5(13) . . ? C54 C55 H55 123.1(13) . . ? C55 C56 C51 120.79(17) . . ? C55 C56 H56 118.2(13) . . ? C51 C56 H56 120.8(13) . . ? O6 C61 C62 118.71(14) . . ? O6 C61 C66 120.89(14) . . ? C62 C61 C66 120.39(14) . . ? C63 C62 C61 119.21(15) . . ? C63 C62 C10 118.29(14) . . ? C61 C62 C10 122.46(14) . . ? C64 C63 C62 122.39(15) . . ? C64 C63 H63 121.9(13) . . ? C62 C63 H63 115.7(13) . . ? C63 C64 C65 116.90(15) . . ? C63 C64 C640 122.12(14) . . ? C65 C64 C640 120.91(15) . . ? C64 C65 C66 124.02(16) . . ? C64 C65 H65 119.5(13) . . ? C66 C65 H65 116.5(13) . . ? C65 C66 C61 117.07(14) . . ? C65 C66 C660 120.24(15) . . ? C61 C66 C660 122.68(14) . . ? C341 C340 C342 107.55(19) . . ? C341 C340 C34 112.06(15) . . ? C342 C340 C34 110.09(15) . . ? C341 C340 C343 108.4(2) . . ? C342 C340 C343 109.33(17) . . ? C34 C340 C343 109.37(15) . . ? C340 C341 H34A 104(2) . . ? C340 C341 H34B 112(2) . . ? H34A C341 H34B 111(3) . . ? C340 C341 H34C 108.4(16) . . ? H34A C341 H34C 112(3) . . ? H34B C341 H34C 110(3) . . ? C340 C342 H34D 112.0(14) . . ? C340 C342 H34E 112.0(17) . . ? H34D C342 H34E 108(2) . . ? C340 C342 H34F 112.2(16) . . ? H34D C342 H34F 106(2) . . ? H34E C342 H34F 106(2) . . ? C340 C343 H34G 112.1(17) . . ? C340 C343 H34H 108.2(14) . . ? H34G C343 H34H 105(2) . . ? C340 C343 H34I 108.4(17) . . ? H34G C343 H34I 111(2) . . ? H34H C343 H34I 112(2) . . ? C363 C360 C361 106.96(14) . . ? C363 C360 C36 110.22(13) . . ? C361 C360 C36 112.71(14) . . ? C363 C360 C362 111.34(14) . . ? C361 C360 C362 106.61(14) . . ? C36 C360 C362 108.96(13) . . ? C360 C361 H36A 111.2(13) . . ? C360 C361 H36B 111.5(14) . . ? H36A C361 H36B 111.4(19) . . ? C360 C361 H36C 107.8(13) . . ? H36A C361 H36C 107.1(17) . . ? H36B C361 H36C 107.6(18) . . ? C360 C362 H36D 107.1(13) . . ? C360 C362 H36E 109.4(13) . . ? H36D C362 H36E 109.3(18) . . ? C360 C362 H36F 111.6(12) . . ? H36D C362 H36F 110.0(18) . . ? H36E C362 H36F 109.3(17) . . ? C360 C363 H36G 110.3(13) . . ? C360 C363 H36H 107.7(13) . . ? H36G C363 H36H 109.3(17) . . ? C360 C363 H36I 112.7(11) . . ? H36G C363 H36I 109.3(17) . . ? H36H C363 H36I 107.5(18) . . ? C641 C640 C64 111.16(14) . . ? C641 C640 C642 107.77(17) . . ? C64 C640 C642 111.38(14) . . ? C641 C640 C643 109.21(16) . . ? C64 C640 C643 108.48(15) . . ? C642 C640 C643 108.79(16) . . ? C640 C641 H64A 110.0(15) . . ? C640 C641 H64B 111.5(15) . . ? H64A C641 H64B 106.2(19) . . ? C640 C641 H64C 108.9(15) . . ? H64A C641 H64C 107(2) . . ? H64B C641 H64C 113(2) . . ? C640 C642 H64D 108.9(13) . . ? C640 C642 H64E 112.4(14) . . ? H64D C642 H64E 110.3(19) . . ? C640 C642 H64F 111.1(14) . . ? H64D C642 H64F 110(2) . . ? H64E C642 H64F 104(2) . . ? C640 C643 H64G 112.2(13) . . ? C640 C643 H64H 112.1(15) . . ? H64G C643 H64H 103.2(19) . . ? C640 C643 H64I 110.1(14) . . ? H64G C643 H64I 109.4(18) . . ? H64H C643 H64I 110(2) . . ? C663 C660 C661 107.08(15) . . ? C663 C660 C662 111.26(14) . . ? C661 C660 C662 106.62(15) . . ? C663 C660 C66 110.18(14) . . ? C661 C660 C66 112.33(14) . . ? C662 C660 C66 109.32(13) . . ? C660 C661 H66A 110.0(14) . . ? C660 C661 H66B 113.2(12) . . ? H66A C661 H66B 106.6(18) . . ? C660 C661 H66C 109.5(12) . . ? H66A C661 H66C 108.2(18) . . ? H66B C661 H66C 109.2(17) . . ? C660 C662 H66D 113.8(13) . . ? C660 C662 H66E 109.7(13) . . ? H66D C662 H66E 101.9(19) . . ? C660 C662 H66F 113.4(12) . . ? H66D C662 H66F 109.2(17) . . ? H66E C662 H66F 108.1(18) . . ? C660 C663 H66G 108.0(15) . . ? C660 C663 H66H 112.5(12) . . ? H66G C663 H66H 108.7(18) . . ? C660 C663 H66I 109.5(14) . . ? H66G C663 H66I 108.5(19) . . ? H66H C663 H66I 109.6(18) . . ? Cl12 C71 Cl11 111.91(14) . . ? Cl12 C71 H71A 110.5(17) . . ? Cl11 C71 H71A 106.5(17) . . ? Cl12 C71 H71B 108.9(18) . . ? Cl11 C71 H71B 106.7(18) . . ? H71A C71 H71B 112(2) . . ? Cl22 C72 Cl21 112.36(12) . . ? Cl22 C72 H72A 108.4(16) . . ? Cl21 C72 H72A 105.1(17) . . ? Cl22 C72 H72B 107.2(19) . . ? Cl21 C72 H72B 108(2) . . ? H72A C72 H72B 116(3) . . ? Cl31 C73 Cl32 112.11(11) . . ? Cl31 C73 H73A 108.1(17) . . ? Cl32 C73 H73A 109.4(17) . . ? Cl31 C73 H73B 110.2(14) . . ? Cl32 C73 H73B 107.8(15) . . ? H73A C73 H73B 109(2) . . ? Cl42 C74 Cl41 110.75(12) . . ? Cl42 C74 H74A 108.0(14) . . ? Cl41 C74 H74A 108.0(14) . . ? Cl42 C74 H74B 108.5(15) . . ? Cl41 C74 H74B 105.7(15) . . ? H74A C74 H74B 116(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.827 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.059