# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Ti(2)(OiPr)6(2) _database_code_depnum_ccdc_archive 'CCDC 921771' #TrackingRef 'NJC_Jones.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H108 N2 O8 Ti2' _chemical_formula_weight 1081.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 17.1370(12) _cell_length_b 11.4570(16) _cell_length_c 17.2330(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.355(5) _cell_angle_gamma 90.00 _cell_volume 3368.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12937 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26382 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5924 _reflns_number_gt 3651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0567P)^2^+2.2233P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5924 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti -0.05933(3) 0.84856(5) 0.23209(3) 0.03352(19) Uani 1 1 d . A . O1 O -0.11235(13) 0.8414(2) 0.31648(13) 0.0472(6) Uani 1 1 d . . . N1 N 0.01369(14) 0.8440(2) 0.13192(14) 0.0290(6) Uani 1 1 d . . . C1 C -0.1275(4) 0.8011(7) 0.3926(4) 0.0600(17) Uani 0.75 1 d P A 1 H1 H -0.1022 0.7232 0.4025 0.072 Uiso 0.75 1 calc PR A 1 O2 O 0.00866(11) 0.72332(18) 0.26489(12) 0.0322(5) Uani 1 1 d . . . C2 C -0.2119(9) 0.790(2) 0.3941(9) 0.110(6) Uani 0.75 1 d P A 1 H2A H -0.2366 0.8661 0.3852 0.165 Uiso 0.75 1 calc PR A 1 H2B H -0.2234 0.7596 0.4451 0.165 Uiso 0.75 1 calc PR A 1 H2C H -0.2323 0.7353 0.3532 0.165 Uiso 0.75 1 calc PR A 1 O3 O -0.14022(14) 0.8281(2) 0.15793(13) 0.0453(6) Uani 1 1 d . . . C3 C -0.0933(11) 0.8851(16) 0.4502(10) 0.136(7) Uani 0.75 1 d P A 1 H3A H -0.0366 0.8903 0.4467 0.204 Uiso 0.75 1 calc PR A 1 H3B H -0.1032 0.8593 0.5026 0.204 Uiso 0.75 1 calc PR A 1 H3C H -0.1171 0.9620 0.4399 0.204 Uiso 0.75 1 calc PR A 1 O4 O -0.02682(13) 0.9991(2) 0.24048(14) 0.0457(6) Uani 1 1 d . . . C4 C 0.06621(16) 0.6565(3) 0.24215(17) 0.0285(7) Uani 1 1 d . A . C5 C 0.09670(16) 0.6775(3) 0.17096(17) 0.0274(7) Uani 1 1 d . . . C6 C 0.15655(17) 0.6060(3) 0.14644(18) 0.0306(7) Uani 1 1 d . A . H6 H 0.1770 0.6222 0.0982 0.037 Uiso 1 1 calc R . . C7 C 0.18630(17) 0.5128(3) 0.19069(19) 0.0327(7) Uani 1 1 d . . . C8 C 0.15513(18) 0.4960(3) 0.26217(19) 0.0342(8) Uani 1 1 d . A . H8 H 0.1754 0.4329 0.2937 0.041 Uiso 1 1 calc R . . C9 C 0.09719(17) 0.5637(3) 0.29051(18) 0.0300(7) Uani 1 1 d . . . C10 C 0.06723(19) 0.5409(3) 0.37050(19) 0.0366(8) Uani 1 1 d . A . C11 C -0.02013(19) 0.5072(3) 0.3591(2) 0.0476(9) Uani 1 1 d . . . H11A H -0.0501 0.5708 0.3324 0.071 Uiso 1 1 calc R A . H11B H -0.0395 0.4933 0.4100 0.071 Uiso 1 1 calc R . . H11C H -0.0263 0.4361 0.3275 0.071 Uiso 1 1 calc R . . C12 C 0.0797(2) 0.6498(3) 0.42226(19) 0.0459(9) Uani 1 1 d . . . H12A H 0.0528 0.7165 0.3962 0.069 Uiso 1 1 calc R A . H12B H 0.1359 0.6665 0.4314 0.069 Uiso 1 1 calc R . . H12C H 0.0583 0.6357 0.4722 0.069 Uiso 1 1 calc R . . C13 C 0.1112(2) 0.4392(3) 0.4136(2) 0.0509(10) Uani 1 1 d . . . H13A H 0.0901 0.4265 0.4638 0.076 Uiso 1 1 calc R A . H13B H 0.1671 0.4583 0.4223 0.076 Uiso 1 1 calc R . . H13C H 0.1045 0.3682 0.3820 0.076 Uiso 1 1 calc R . . C14 C 0.24969(19) 0.4302(3) 0.1667(2) 0.0423(9) Uani 1 1 d . A . C15 C 0.2786(2) 0.4655(4) 0.0886(2) 0.0618(12) Uani 1 1 d . . . H15A H 0.3202 0.4121 0.0759 0.093 Uiso 1 1 calc R A . H15B H 0.2991 0.5453 0.0923 0.093 Uiso 1 1 calc R . . H15C H 0.2350 0.4617 0.0477 0.093 Uiso 1 1 calc R . . C16 C 0.3202(2) 0.4320(4) 0.2286(2) 0.0612(12) Uani 1 1 d . . . H16A H 0.3037 0.4052 0.2785 0.092 Uiso 1 1 calc R A . H16B H 0.3406 0.5118 0.2344 0.092 Uiso 1 1 calc R . . H16C H 0.3612 0.3804 0.2124 0.092 Uiso 1 1 calc R . . C17 C 0.2163(3) 0.3061(4) 0.1596(3) 0.0715(13) Uani 1 1 d . . . H17A H 0.1971 0.2830 0.2092 0.107 Uiso 1 1 calc R A . H17B H 0.2574 0.2519 0.1467 0.107 Uiso 1 1 calc R . . H17C H 0.1729 0.3039 0.1183 0.107 Uiso 1 1 calc R . . C18 C 0.06868(17) 0.7723(3) 0.12029(18) 0.0302(7) Uani 1 1 d . A . H18 H 0.0976(15) 0.782(2) 0.0736(17) 0.026(8) Uiso 1 1 d . . . C19 C -0.00582(18) 0.9352(3) 0.07187(18) 0.0335(8) Uani 1 1 d . A . H19 H -0.0495 0.9826 0.0903 0.040 Uiso 1 1 calc R . . C20 C -0.03645(19) 0.8830(3) -0.00642(19) 0.0378(8) Uani 1 1 d . . . H20A H -0.0814 0.8311 0.0005 0.045 Uiso 1 1 calc R A . H20B H 0.0052 0.8358 -0.0274 0.045 Uiso 1 1 calc R . . C21 C 0.06219(19) 1.0192(3) 0.06400(19) 0.0372(8) Uani 1 1 d . . . H21A H 0.1069 0.9762 0.0452 0.045 Uiso 1 1 calc R A . H21B H 0.0795 1.0533 0.1155 0.045 Uiso 1 1 calc R . . C22 C -0.2254(8) 0.846(2) 0.1506(11) 0.069(8) Uani 0.60 1 d P A 1 H22 H -0.2427 0.8638 0.2032 0.083 Uiso 0.60 1 calc PR A 1 C23 C -0.2648(10) 0.741(2) 0.1201(11) 0.122(8) Uani 0.60 1 d P A 1 H23A H -0.2556 0.6778 0.1579 0.183 Uiso 0.60 1 calc PR A 1 H23B H -0.2442 0.7192 0.0710 0.183 Uiso 0.60 1 calc PR A 1 H23C H -0.3212 0.7562 0.1108 0.183 Uiso 0.60 1 calc PR A 1 C24 C -0.2434(6) 0.9481(11) 0.0985(10) 0.146(6) Uani 0.60 1 d P A 1 H24A H -0.2997 0.9651 0.0957 0.219 Uiso 0.60 1 calc PR A 1 H24B H -0.2287 0.9301 0.0462 0.219 Uiso 0.60 1 calc PR A 1 H24C H -0.2138 1.0162 0.1192 0.219 Uiso 0.60 1 calc PR A 1 C25 C -0.0538(3) 1.1004(3) 0.2776(2) 0.0622(11) Uani 1 1 d . A . H25 H -0.1021 1.0778 0.3024 0.075 Uiso 1 1 calc R . . C26 C -0.0762(4) 1.1900(5) 0.2201(3) 0.123(2) Uani 1 1 d . . . H26A H -0.0291 1.2221 0.2000 0.185 Uiso 1 1 calc R A . H26B H -0.1044 1.2524 0.2445 0.185 Uiso 1 1 calc R . . H26C H -0.1102 1.1558 0.1771 0.185 Uiso 1 1 calc R . . C27 C 0.0043(4) 1.1374(5) 0.3397(4) 0.118(2) Uani 1 1 d . . . H27A H 0.0210 1.0700 0.3722 0.177 Uiso 1 1 calc R A . H27B H -0.0186 1.1966 0.3718 0.177 Uiso 1 1 calc R . . H27C H 0.0498 1.1705 0.3170 0.177 Uiso 1 1 calc R . . C28 C 0.4665(4) -0.0239(6) 0.5223(5) 0.156(5) Uani 1 1 d . . . H28A H 0.4179 -0.0269 0.4865 0.187 Uiso 1 1 calc R . . H28B H 0.4795 -0.1048 0.5393 0.187 Uiso 1 1 calc R . . C29 C 0.4516(5) 0.0471(6) 0.5920(5) 0.152(4) Uani 1 1 d . . . H29A H 0.4368 0.1272 0.5748 0.182 Uiso 1 1 calc R . . H29B H 0.5008 0.0524 0.6269 0.182 Uiso 1 1 calc R . . C30 C 0.3881(5) -0.0021(6) 0.6371(5) 0.144(3) Uani 1 1 d . . . H30A H 0.3387 -0.0043 0.6037 0.216 Uiso 1 1 calc R . . H30B H 0.3820 0.0473 0.6825 0.216 Uiso 1 1 calc R . . H30C H 0.4024 -0.0814 0.6545 0.216 Uiso 1 1 calc R . . C1' C -0.1497(11) 0.8686(18) 0.3854(10) 0.050(5) Uani 0.25 1 d P A 2 H1' H -0.1788 0.9442 0.3800 0.060 Uiso 0.25 1 calc PR A 2 C2' C -0.210(2) 0.755(6) 0.397(4) 0.13(2) Uani 0.25 1 d P A 2 H2'1 H -0.2625 0.7727 0.3716 0.189 Uiso 0.25 1 calc PR A 2 H2'2 H -0.2144 0.7429 0.4533 0.189 Uiso 0.25 1 calc PR A 2 H2'3 H -0.1897 0.6848 0.3747 0.189 Uiso 0.25 1 calc PR A 2 C3' C -0.0879(18) 0.868(3) 0.459(3) 0.053(8) Uani 0.25 1 d P A 2 H3'1 H -0.0465 0.8114 0.4518 0.080 Uiso 0.25 1 calc PR A 2 H3'2 H -0.1140 0.8467 0.5055 0.080 Uiso 0.25 1 calc PR A 2 H3'3 H -0.0648 0.9461 0.4667 0.080 Uiso 0.25 1 calc PR A 2 C22' C -0.2189(16) 0.829(3) 0.1605(17) 0.064(9) Uani 0.40 1 d P A 2 H22' H -0.2322 0.7806 0.2055 0.077 Uiso 0.40 1 calc PR A 2 C23' C -0.2554(11) 0.772(3) 0.0834(14) 0.101(9) Uani 0.40 1 d P A 2 H23D H -0.3127 0.7746 0.0816 0.151 Uiso 0.40 1 calc PR A 2 H23E H -0.2383 0.6903 0.0815 0.151 Uiso 0.40 1 calc PR A 2 H23F H -0.2382 0.8141 0.0386 0.151 Uiso 0.40 1 calc PR A 2 C24' C -0.2523(9) 0.9466(17) 0.1683(10) 0.096(5) Uani 0.40 1 d P A 2 H24D H -0.2347 0.9785 0.2198 0.143 Uiso 0.40 1 calc PR A 2 H24E H -0.3096 0.9417 0.1626 0.143 Uiso 0.40 1 calc PR A 2 H24F H -0.2348 0.9978 0.1278 0.143 Uiso 0.40 1 calc PR 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 0.0352(3) 0.0320(3) 0.0328(3) 0.0005(3) 0.0001(2) 0.0055(3) O1 0.0500(14) 0.0551(16) 0.0377(14) 0.0012(13) 0.0102(11) 0.0110(12) N1 0.0359(14) 0.0236(14) 0.0262(14) 0.0032(12) -0.0041(11) 0.0011(12) C1 0.074(4) 0.062(5) 0.047(4) 0.006(4) 0.020(3) 0.013(4) O2 0.0370(12) 0.0300(13) 0.0299(12) 0.0052(10) 0.0039(9) 0.0049(10) C2 0.115(11) 0.132(15) 0.090(8) 0.019(8) 0.050(7) -0.033(8) O3 0.0317(14) 0.0616(17) 0.0412(14) -0.0010(12) -0.0044(10) 0.0057(11) C3 0.176(14) 0.201(19) 0.031(6) -0.033(9) 0.014(7) -0.013(11) O4 0.0548(14) 0.0321(14) 0.0500(16) -0.0059(11) 0.0049(12) 0.0050(11) C4 0.0286(16) 0.0248(17) 0.0313(17) 0.0015(14) -0.0012(13) -0.0027(13) C5 0.0301(16) 0.0251(18) 0.0259(17) 0.0035(13) -0.0029(13) -0.0022(12) C6 0.0333(17) 0.0304(18) 0.0281(18) 0.0024(15) 0.0037(13) -0.0007(14) C7 0.0339(17) 0.0313(19) 0.0321(18) 0.0038(15) -0.0018(14) 0.0027(14) C8 0.0397(18) 0.0278(19) 0.0341(19) 0.0071(15) -0.0020(14) 0.0013(14) C9 0.0333(17) 0.0265(18) 0.0292(18) 0.0054(14) -0.0027(13) -0.0017(13) C10 0.0464(19) 0.031(2) 0.0319(19) 0.0097(15) 0.0025(15) 0.0000(15) C11 0.047(2) 0.051(2) 0.046(2) 0.0150(18) 0.0080(17) -0.0088(17) C12 0.057(2) 0.047(2) 0.034(2) 0.0056(18) 0.0050(16) -0.0016(18) C13 0.063(2) 0.053(2) 0.038(2) 0.0193(18) 0.0088(18) 0.0088(19) C14 0.043(2) 0.038(2) 0.047(2) 0.0060(17) 0.0077(16) 0.0117(15) C15 0.056(2) 0.072(3) 0.060(3) 0.010(2) 0.018(2) 0.029(2) C16 0.044(2) 0.076(3) 0.063(3) 0.016(2) 0.0003(19) 0.023(2) C17 0.079(3) 0.046(3) 0.094(4) -0.010(2) 0.029(3) 0.012(2) C18 0.0344(17) 0.0320(19) 0.0239(18) 0.0025(14) 0.0013(14) -0.0034(14) C19 0.0417(18) 0.0265(18) 0.0313(18) 0.0065(14) -0.0021(14) 0.0068(14) C20 0.0467(19) 0.0277(19) 0.037(2) 0.0075(15) -0.0072(15) -0.0021(14) C21 0.0467(19) 0.0295(19) 0.0331(19) 0.0078(15) -0.0087(15) 0.0001(15) C22 0.009(5) 0.135(17) 0.061(10) 0.021(8) 0.001(5) 0.006(7) C23 0.059(7) 0.114(11) 0.19(2) -0.006(14) 0.012(11) -0.041(7) C24 0.073(7) 0.111(10) 0.241(17) 0.067(12) -0.047(10) 0.016(6) C25 0.087(3) 0.039(2) 0.059(3) -0.010(2) 0.002(2) 0.011(2) C26 0.201(7) 0.056(4) 0.106(5) -0.010(3) -0.022(5) 0.060(4) C27 0.139(5) 0.083(4) 0.124(5) -0.052(4) -0.037(4) 0.024(4) C28 0.197(10) 0.054(5) 0.185(10) -0.017(5) -0.149(9) 0.028(4) C29 0.186(8) 0.055(4) 0.190(8) -0.005(5) -0.112(7) 0.013(4) C30 0.154(7) 0.070(5) 0.190(8) 0.011(5) -0.086(6) 0.004(4) C1' 0.064(12) 0.048(13) 0.042(11) 0.009(9) 0.024(8) 0.009(9) C2' 0.040(16) 0.13(4) 0.20(4) 0.11(3) -0.011(18) -0.023(15) C3' 0.048(13) 0.051(14) 0.06(2) -0.002(13) 0.018(12) 0.016(10) C22' 0.080(18) 0.071(12) 0.036(9) -0.018(9) -0.028(8) 0.034(10) C23' 0.036(10) 0.16(3) 0.094(16) -0.032(15) -0.040(10) 0.002(11) C24' 0.057(8) 0.111(13) 0.118(13) 0.009(11) 0.003(9) 0.050(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.787(2) . ? Ti1 O3 1.811(2) . ? Ti1 O4 1.814(2) . ? Ti1 O2 1.901(2) . ? Ti1 N1 2.225(3) . ? O1 C1' 1.434(17) . ? O1 C1 1.436(7) . ? N1 C18 1.280(4) . ? N1 C19 1.487(4) . ? C1 C3 1.466(19) . ? C1 C2 1.455(16) . ? C1 H1 1.0000 . ? O2 C4 1.336(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C22' 1.35(3) . ? O3 C22 1.469(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C25 1.423(4) . ? C4 C5 1.398(4) . ? C4 C9 1.423(4) . ? C5 C6 1.408(4) . ? C5 C18 1.448(4) . ? C6 C7 1.381(4) . ? C6 H6 0.9500 . ? C7 C8 1.401(4) . ? C7 C14 1.527(4) . ? C8 C9 1.385(4) . ? C8 H8 0.9500 . ? C9 C10 1.538(4) . ? C10 C12 1.537(5) . ? C10 C13 1.540(5) . ? C10 C11 1.541(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.530(5) . ? C14 C17 1.534(5) . ? C14 C16 1.536(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 0.99(3) . ? C19 C20 1.524(4) . ? C19 C21 1.527(4) . ? C19 H19 1.0000 . ? C20 C21 1.534(4) 3_575 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C20 1.534(4) 3_575 ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.45(3) . ? C22 C24 1.49(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.453(6) . ? C25 C27 1.455(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.491(11) . ? C28 C28 1.541(16) 3_656 ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.505(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C1' C3' 1.58(5) . ? C1' C2' 1.69(6) . ? C1' H1' 1.0000 . ? C2' H2'1 0.9800 . ? C2' H2'2 0.9800 . ? C2' H2'3 0.9800 . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? C22' C24' 1.47(3) . ? C22' C23' 1.56(3) . ? C22' H22' 1.0000 . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 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 O1 Ti1 O3 98.89(11) . . ? O1 Ti1 O4 98.88(12) . . ? O3 Ti1 O4 112.85(11) . . ? O1 Ti1 O2 93.87(10) . . ? O3 Ti1 O2 121.34(11) . . ? O4 Ti1 O2 121.24(10) . . ? O1 Ti1 N1 174.63(10) . . ? O3 Ti1 N1 84.17(10) . . ? O4 Ti1 N1 83.88(10) . . ? O2 Ti1 N1 80.76(9) . . ? C1' O1 C1 35.1(7) . . ? C1' O1 Ti1 164.5(8) . . ? C1 O1 Ti1 155.0(3) . . ? C18 N1 C19 117.6(3) . . ? C18 N1 Ti1 127.7(2) . . ? C19 N1 Ti1 114.66(18) . . ? O1 C1 C3 108.2(9) . . ? O1 C1 C2 108.1(8) . . ? C3 C1 C2 112.4(11) . . ? O1 C1 H1 109.3 . . ? C3 C1 H1 109.3 . . ? C2 C1 H1 109.3 . . ? C4 O2 Ti1 142.58(19) . . ? C22' O3 C22 10(2) . . ? C22' O3 Ti1 132.4(11) . . ? C22 O3 Ti1 137.1(8) . . ? C25 O4 Ti1 134.5(3) . . ? O2 C4 C5 120.4(3) . . ? O2 C4 C9 120.1(3) . . ? C5 C4 C9 119.5(3) . . ? C4 C5 C6 120.4(3) . . ? C4 C5 C18 121.9(3) . . ? C6 C5 C18 117.8(3) . . ? C7 C6 C5 121.7(3) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 116.1(3) . . ? C6 C7 C14 124.4(3) . . ? C8 C7 C14 119.5(3) . . ? C9 C8 C7 125.3(3) . . ? C9 C8 H8 117.4 . . ? C7 C8 H8 117.4 . . ? C8 C9 C4 116.9(3) . . ? C8 C9 C10 122.1(3) . . ? C4 C9 C10 121.0(3) . . ? C12 C10 C9 110.0(3) . . ? C12 C10 C13 107.4(3) . . ? C9 C10 C13 111.8(3) . . ? C12 C10 C11 111.0(3) . . ? C9 C10 C11 109.3(3) . . ? C13 C10 C11 107.3(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C14 C15 111.8(3) . . ? C7 C14 C17 109.1(3) . . ? C15 C14 C17 108.9(3) . . ? C7 C14 C16 109.6(3) . . ? C15 C14 C16 108.0(3) . . ? C17 C14 C16 109.4(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C5 126.5(3) . . ? N1 C18 H18 119.2(16) . . ? C5 C18 H18 114.3(16) . . ? N1 C19 C20 112.1(3) . . ? N1 C19 C21 112.4(2) . . ? C20 C19 C21 111.8(3) . . ? N1 C19 H19 106.7 . . ? C20 C19 H19 106.7 . . ? C21 C19 H19 106.7 . . ? C19 C20 C21 109.9(3) . 3_575 ? C19 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 3_575 . ? C19 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 3_575 . ? H20A C20 H20B 108.2 . . ? C19 C21 C20 110.0(3) . 3_575 ? C19 C21 H21A 109.7 . . ? C20 C21 H21A 109.7 3_575 . ? C19 C21 H21B 109.7 . . ? C20 C21 H21B 109.7 3_575 . ? H21A C21 H21B 108.2 . . ? C23 C22 O3 109.8(16) . . ? C23 C22 C24 111.6(16) . . ? O3 C22 C24 108.2(11) . . ? C23 C22 H22 109.1 . . ? O3 C22 H22 109.1 . . ? C24 C22 H22 109.1 . . ? O4 C25 C26 110.2(4) . . ? O4 C25 C27 109.8(4) . . ? C26 C25 C27 114.5(5) . . ? O4 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C28 113.5(8) . 3_656 ? C29 C28 H28A 108.9 . . ? C28 C28 H28A 108.9 3_656 . ? C29 C28 H28B 108.9 . . ? C28 C28 H28B 108.9 3_656 . ? H28A C28 H28B 107.7 . . ? C28 C29 C30 113.5(6) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C1' C3' 110.5(16) . . ? O1 C1' C2' 105(3) . . ? C3' C1' C2' 106(2) . . ? O1 C1' H1' 111.6 . . ? C3' C1' H1' 111.6 . . ? C2' C1' H1' 111.6 . . ? C1' C2' H2'1 109.5 . . ? C1' C2' H2'2 109.5 . . ? H2'1 C2' H2'2 109.5 . . ? C1' C2' H2'3 109.5 . . ? H2'1 C2' H2'3 109.5 . . ? H2'2 C2' H2'3 109.5 . . ? C1' C3' H3'1 109.5 . . ? C1' C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C1' C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? O3 C22' C24' 114(2) . . ? O3 C22' C23' 106.8(18) . . ? C24' C22' C23' 110(3) . . ? O3 C22' H22' 108.7 . . ? C24' C22' H22' 108.7 . . ? C23' C22' H22' 108.7 . . ? C22' C23' H23D 109.5 . . ? C22' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C22' C24' H24D 109.5 . . ? C22' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.530 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.055 data_Al2Me4_2 _database_code_depnum_ccdc_archive 'CCDC 921772' #TrackingRef 'NJC_Jones.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H80 Al2 N2 O4' _chemical_formula_weight 803.10 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5690(10) _cell_length_b 11.6000(7) _cell_length_c 11.8190(13) _cell_angle_alpha 109.497(5) _cell_angle_beta 96.776(4) _cell_angle_gamma 93.635(5) _cell_volume 1220.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4852 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 24.11 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7936 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 24.16 _reflns_number_total 3792 _reflns_number_gt 2365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0878P)^2^+1.8602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3792 _refine_ls_number_parameters 261 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1313 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.012 _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 Al1 Al 0.27876(13) 0.48558(11) 0.76497(12) 0.0338(4) Uani 1 1 d . . . O1 O 0.4471(3) 0.5604(3) 0.7708(3) 0.0405(8) Uani 1 1 d . . . N1 N 0.2694(4) 0.5671(3) 0.9397(3) 0.0329(8) Uani 1 1 d . . . C1 C 0.1316(5) 0.5386(5) 0.6711(5) 0.0543(13) Uani 1 1 d . . . H1A H 0.1323 0.6281 0.7059 0.081 Uiso 1 1 calc R . . H1B H 0.0391 0.4987 0.6734 0.081 Uiso 1 1 calc R . . H1C H 0.1493 0.5158 0.5868 0.081 Uiso 1 1 calc R . . O2 O 0.2284(15) 0.8104(12) 0.2697(11) 0.117(4) Uiso 0.55 1 d PD A 1 C2 C 0.2933(6) 0.3091(4) 0.7149(5) 0.0538(14) Uani 1 1 d . . . H2A H 0.3602 0.2871 0.6564 0.081 Uiso 1 1 calc R . . H2B H 0.2000 0.2639 0.6771 0.081 Uiso 1 1 calc R . . H2C H 0.3269 0.2875 0.7861 0.081 Uiso 1 1 calc R . . C3 C 0.5212(4) 0.6605(4) 0.8525(4) 0.0332(10) Uani 1 1 d . . . C4 C 0.4820(4) 0.7101(4) 0.9690(4) 0.0317(10) Uani 1 1 d . . . C5 C 0.5572(4) 0.8183(4) 1.0538(4) 0.0325(10) Uani 1 1 d . . . H5 H 0.5295 0.8503 1.1319 0.039 Uiso 1 1 calc R . . C6 C 0.6706(4) 0.8795(4) 1.0269(4) 0.0315(10) Uani 1 1 d . . . C7 C 0.7090(4) 0.8246(4) 0.9113(4) 0.0349(10) Uani 1 1 d . . . H7 H 0.7890 0.8632 0.8921 0.042 Uiso 1 1 calc R . . C8 C 0.6391(4) 0.7186(4) 0.8231(4) 0.0340(10) Uani 1 1 d . . . C9 C 0.7522(4) 0.9974(4) 1.1180(4) 0.0372(10) Uani 1 1 d . . . C10 C 0.8816(5) 0.9650(4) 1.1859(5) 0.0530(13) Uani 1 1 d . . . H10A H 0.8502 0.9157 1.2332 0.079 Uiso 1 1 calc R . . H10B H 0.9379 1.0409 1.2407 0.079 Uiso 1 1 calc R . . H10C H 0.9394 0.9178 1.1274 0.079 Uiso 1 1 calc R . . C11 C 0.8049(5) 1.0845(4) 1.0537(4) 0.0477(12) Uani 1 1 d . . . H11A H 0.8787 1.0485 1.0064 0.072 Uiso 1 1 calc R . . H11B H 0.8437 1.1642 1.1146 0.072 Uiso 1 1 calc R . . H11C H 0.7256 1.0960 0.9994 0.072 Uiso 1 1 calc R . . C12 C 0.6594(5) 1.0699(4) 1.2086(5) 0.0535(14) Uani 1 1 d . . . H12A H 0.5734 1.0849 1.1641 0.080 Uiso 1 1 calc R . . H12B H 0.7122 1.1487 1.2604 0.080 Uiso 1 1 calc R . . H12C H 0.6334 1.0223 1.2591 0.080 Uiso 1 1 calc R . . C13 C 0.6842(4) 0.6669(4) 0.6964(4) 0.0379(11) Uani 1 1 d . . . C14 C 0.7163(5) 0.5331(4) 0.6704(4) 0.0475(12) Uani 1 1 d . . . H14A H 0.7919 0.5300 0.7326 0.071 Uiso 1 1 calc R . . H14B H 0.7467 0.5015 0.5904 0.071 Uiso 1 1 calc R . . H14C H 0.6309 0.4826 0.6717 0.071 Uiso 1 1 calc R . . C15 C 0.8181(5) 0.7410(5) 0.6860(5) 0.0527(13) Uani 1 1 d . . . H15A H 0.7996 0.8263 0.6993 0.079 Uiso 1 1 calc R . . H15B H 0.8443 0.7045 0.6049 0.079 Uiso 1 1 calc R . . H15C H 0.8958 0.7393 0.7472 0.079 Uiso 1 1 calc R . . C16 C 0.5647(5) 0.6739(5) 0.6004(4) 0.0498(13) Uani 1 1 d . . . H16A H 0.4772 0.6287 0.6059 0.075 Uiso 1 1 calc R . . H16B H 0.5910 0.6374 0.5193 0.075 Uiso 1 1 calc R . . H16C H 0.5497 0.7602 0.6148 0.075 Uiso 1 1 calc R . . C17 C 0.3621(5) 0.6571(4) 1.0058(4) 0.0358(10) Uani 1 1 d . . . H17 H 0.352(4) 0.701(3) 1.094(4) 0.029(10) Uiso 1 1 d . . . C18 C 0.1490(4) 0.5411(4) 1.0018(4) 0.0359(10) Uani 1 1 d . . . H18 H 0.1851 0.5626 1.0901 0.043 Uiso 1 1 calc R . . C19 C 0.0328(5) 0.6207(4) 0.9892(4) 0.0403(11) Uani 1 1 d . . . H19A H 0.0002 0.6042 0.9020 0.048 Uiso 1 1 calc R . . H19B H 0.0711 0.7085 1.0267 0.048 Uiso 1 1 calc R . . C20 C -0.0925(5) 0.5957(4) 1.0498(4) 0.0403(11) Uani 1 1 d . . . H20A H -0.1688 0.6454 1.0360 0.048 Uiso 1 1 calc R . . H20B H -0.0624 0.6202 1.1384 0.048 Uiso 1 1 calc R . . C21 C 0.282(3) 0.771(2) 0.3780(16) 0.219(12) Uiso 0.55 1 d PD A 1 H21A H 0.2590 0.6825 0.3634 0.263 Uiso 0.55 1 calc PR A 1 H21B H 0.3831 0.7983 0.4108 0.263 Uiso 0.55 1 calc PR A 1 C22 C 0.180(2) 0.8537(14) 0.4503(19) 0.135(7) Uiso 0.55 1 d PD A 1 H22A H 0.1951 0.8608 0.5368 0.162 Uiso 0.55 1 calc PR A 1 H22B H 0.0797 0.8227 0.4156 0.162 Uiso 0.55 1 calc PR A 1 C23 C 0.2222(17) 0.9771(11) 0.4345(12) 0.085(4) Uiso 0.55 1 d PD A 1 H23A H 0.1389 1.0225 0.4295 0.103 Uiso 0.55 1 calc PR A 1 H23B H 0.2942 1.0293 0.5026 0.103 Uiso 0.55 1 calc PR A 1 C24 C 0.2816(15) 0.9399(12) 0.3178(12) 0.086(4) Uiso 0.55 1 d P A 1 H24A H 0.2444 0.9844 0.2643 0.103 Uiso 0.55 1 calc PR A 1 H24B H 0.3863 0.9524 0.3313 0.103 Uiso 0.55 1 calc PR A 1 O2A O 0.3592(19) 0.8925(17) 0.3308(15) 0.154(6) Uiso 0.45 1 d PD B 2 C21A C 0.318(2) 0.9563(18) 0.4572(15) 0.119(7) Uiso 0.45 1 d PD B 2 H21C H 0.3271 1.0468 0.4779 0.143 Uiso 0.45 1 calc PR B 2 H21D H 0.3785 0.9360 0.5202 0.143 Uiso 0.45 1 calc PR B 2 C22A C 0.151(2) 0.9018(15) 0.4460(16) 0.098(6) Uiso 0.45 1 d PD B 2 H22C H 0.1269 0.8926 0.5220 0.118 Uiso 0.45 1 calc PR B 2 H22D H 0.0824 0.9496 0.4162 0.118 Uiso 0.45 1 calc PR B 2 C23A C 0.1678(15) 0.7785(11) 0.3487(12) 0.077(4) Uiso 0.45 1 d PD B 2 H23C H 0.0789 0.7450 0.2915 0.093 Uiso 0.45 1 calc PR B 2 H23D H 0.1954 0.7173 0.3864 0.093 Uiso 0.45 1 calc PR B 2 C24A C 0.2865(16) 0.8116(13) 0.2836(13) 0.057(4) Uiso 0.45 1 d PD B 2 H24C H 0.3425 0.7406 0.2602 0.069 Uiso 0.45 1 calc PR B 2 H24D H 0.2411 0.8202 0.2076 0.069 Uiso 0.45 1 calc PR B 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 Al1 0.0329(7) 0.0344(7) 0.0327(7) 0.0090(5) 0.0113(6) -0.0043(5) O1 0.0349(17) 0.0469(17) 0.0332(17) 0.0047(14) 0.0143(14) -0.0109(13) N1 0.031(2) 0.0348(19) 0.034(2) 0.0124(16) 0.0114(16) -0.0031(15) C1 0.047(3) 0.077(4) 0.042(3) 0.018(3) 0.016(2) 0.016(3) C2 0.069(4) 0.044(3) 0.048(3) 0.011(2) 0.024(3) 0.000(2) C3 0.029(2) 0.036(2) 0.031(2) 0.0082(19) 0.0039(19) -0.0053(18) C4 0.029(2) 0.033(2) 0.034(2) 0.0135(19) 0.0068(19) 0.0000(17) C5 0.031(2) 0.035(2) 0.030(2) 0.0089(18) 0.0088(19) -0.0017(18) C6 0.027(2) 0.036(2) 0.035(2) 0.0158(19) 0.0062(19) 0.0032(17) C7 0.028(2) 0.040(2) 0.038(3) 0.016(2) 0.008(2) -0.0009(18) C8 0.028(2) 0.042(2) 0.033(2) 0.014(2) 0.0100(19) -0.0010(18) C9 0.032(2) 0.037(2) 0.041(3) 0.013(2) 0.006(2) -0.0050(18) C10 0.045(3) 0.048(3) 0.060(3) 0.020(2) -0.011(3) -0.013(2) C11 0.056(3) 0.037(2) 0.049(3) 0.014(2) 0.012(2) -0.005(2) C12 0.051(3) 0.045(3) 0.052(3) 0.001(2) 0.019(3) -0.010(2) C13 0.029(2) 0.049(3) 0.032(2) 0.009(2) 0.0074(19) -0.0052(19) C14 0.041(3) 0.054(3) 0.041(3) 0.005(2) 0.013(2) 0.002(2) C15 0.042(3) 0.067(3) 0.044(3) 0.011(2) 0.020(2) -0.012(2) C16 0.047(3) 0.065(3) 0.039(3) 0.020(2) 0.010(2) -0.004(2) C17 0.035(3) 0.037(2) 0.034(3) 0.010(2) 0.009(2) -0.0020(19) C18 0.033(2) 0.043(2) 0.034(2) 0.015(2) 0.014(2) -0.0020(19) C19 0.042(3) 0.034(2) 0.047(3) 0.014(2) 0.019(2) -0.0041(19) C20 0.036(3) 0.038(2) 0.048(3) 0.014(2) 0.018(2) -0.0006(19) _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 Al1 O1 1.763(3) . ? Al1 C1 1.946(5) . ? Al1 C2 1.952(5) . ? Al1 N1 1.979(4) . ? O1 C3 1.331(5) . ? N1 C17 1.290(5) . ? N1 C18 1.504(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C24 1.450(17) . ? O2 C21 1.540(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.410(6) . ? C3 C8 1.414(6) . ? C4 C5 1.405(6) . ? C4 C17 1.446(6) . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? C6 C7 1.405(6) . ? C6 C9 1.524(6) . ? C7 C8 1.387(6) . ? C7 H7 0.9500 . ? C8 C13 1.541(6) . ? C9 C10 1.531(7) . ? C9 C12 1.537(6) . ? C9 C11 1.546(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.537(6) . ? C13 C16 1.539(7) . ? C13 C14 1.538(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17 1.02(4) . ? C18 C19 1.515(6) . ? C18 C20 1.532(6) 2_567 ? C18 H18 1.0000 . ? C19 C20 1.528(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C18 1.532(6) 2_567 ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.539(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.540(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.494(17) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O2A C24A 1.073(19) . ? O2A C21A 1.541(2) . ? C21A C22A 1.66(3) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.540(2) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A C24A 1.541(2) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C1 111.6(2) . . ? O1 Al1 C2 107.99(19) . . ? C1 Al1 C2 116.7(2) . . ? O1 Al1 N1 94.69(14) . . ? C1 Al1 N1 108.73(18) . . ? C2 Al1 N1 115.00(18) . . ? C3 O1 Al1 131.8(3) . . ? C17 N1 C18 115.0(3) . . ? C17 N1 Al1 120.6(3) . . ? C18 N1 Al1 124.0(3) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C24 O2 C21 100.2(14) . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 120.1(3) . . ? O1 C3 C8 120.4(4) . . ? C4 C3 C8 119.5(4) . . ? C5 C4 C3 120.1(4) . . ? C5 C4 C17 116.9(4) . . ? C3 C4 C17 122.9(4) . . ? C6 C5 C4 121.9(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 116.0(4) . . ? C5 C6 C9 122.3(4) . . ? C7 C6 C9 121.6(4) . . ? C8 C7 C6 125.0(4) . . ? C8 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? C7 C8 C3 117.4(4) . . ? C7 C8 C13 121.9(4) . . ? C3 C8 C13 120.7(4) . . ? C6 C9 C10 109.2(3) . . ? C6 C9 C12 111.7(4) . . ? C10 C9 C12 110.0(4) . . ? C6 C9 C11 111.2(4) . . ? C10 C9 C11 108.1(4) . . ? C12 C9 C11 106.4(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 107.7(4) . . ? C15 C13 C14 107.6(4) . . ? C16 C13 C14 110.4(4) . . ? C15 C13 C8 111.9(4) . . ? C16 C13 C8 109.2(3) . . ? C14 C13 C8 109.9(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C4 127.7(4) . . ? N1 C17 H17 119(2) . . ? C4 C17 H17 113(2) . . ? N1 C18 C19 109.8(3) . . ? N1 C18 C20 110.8(3) . 2_567 ? C19 C18 C20 111.1(4) . 2_567 ? N1 C18 H18 108.3 . . ? C19 C18 H18 108.3 . . ? C20 C18 H18 108.3 2_567 . ? C18 C19 C20 111.4(3) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C18 110.5(3) . 2_567 ? C19 C20 H20A 109.5 . . ? C18 C20 H20A 109.5 2_567 . ? C19 C20 H20B 109.5 . . ? C18 C20 H20B 109.5 2_567 . ? H20A C20 H20B 108.1 . . ? C22 C21 O2 88.0(12) . . ? C22 C21 H21A 114.0 . . ? O2 C21 H21A 114.0 . . ? C22 C21 H21B 114.0 . . ? O2 C21 H21B 114.0 . . ? H21A C21 H21B 111.2 . . ? C21 C22 C23 101.4(14) . . ? C21 C22 H22A 111.5 . . ? C23 C22 H22A 111.5 . . ? C21 C22 H22B 111.5 . . ? C23 C22 H22B 111.5 . . ? H22A C22 H22B 109.3 . . ? C24 C23 C22 103.6(11) . . ? C24 C23 H23A 111.0 . . ? C22 C23 H23A 111.0 . . ? C24 C23 H23B 111.0 . . ? C22 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? O2 C24 C23 99.7(10) . . ? O2 C24 H24A 111.8 . . ? C23 C24 H24A 111.8 . . ? O2 C24 H24B 111.8 . . ? C23 C24 H24B 111.8 . . ? H24A C24 H24B 109.6 . . ? C24A O2A C21A 109.1(16) . . ? O2A C21A C22A 104.7(14) . . ? O2A C21A H21C 110.8 . . ? C22A C21A H21C 110.8 . . ? O2A C21A H21D 110.8 . . ? C22A C21A H21D 110.8 . . ? H21C C21A H21D 108.9 . . ? C23A C22A C21A 93.0(11) . . ? C23A C22A H22C 113.1 . . ? C21A C22A H22C 113.1 . . ? C23A C22A H22D 113.1 . . ? C21A C22A H22D 113.1 . . ? H22C C22A H22D 110.5 . . ? C22A C23A C24A 103.9(11) . . ? C22A C23A H23C 111.0 . . ? C24A C23A H23C 111.0 . . ? C22A C23A H23D 111.0 . . ? C24A C23A H23D 111.0 . . ? H23C C23A H23D 109.0 . . ? O2A C24A C23A 118.7(15) . . ? O2A C24A H24C 107.6 . . ? C23A C24A H24C 107.6 . . ? O2A C24A H24D 107.6 . . ? C23A C24A H24D 107.6 . . ? H24C C24A H24D 107.1 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.490 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.070 data_Al2Me4_1 _database_code_depnum_ccdc_archive 'CCDC 921773' #TrackingRef 'NJC_Jones.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H52 Al2 N2 O2' _chemical_formula_weight 574.74 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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 6.4870(6) _cell_length_b 7.6680(7) _cell_length_c 17.3850(14) _cell_angle_alpha 98.515(5) _cell_angle_beta 90.729(5) _cell_angle_gamma 94.709(5) _cell_volume 852.08(13) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25443 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13796 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3854 _reflns_number_gt 3129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0585P)^2^+0.2854P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3854 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Al1 Al 0.18151(7) 0.21072(5) 0.65837(3) 0.02713(14) Uani 1 1 d . . . O1 O 0.29572(16) 0.26963(13) 0.75252(6) 0.0314(2) Uani 1 1 d . . . N1 N 0.26375(18) 0.44203(15) 0.62537(7) 0.0265(3) Uani 1 1 d . . . C1 C 0.3244(3) 0.0264(2) 0.59486(10) 0.0403(4) Uani 1 1 d . . . H1A H 0.4556 0.0785 0.5776 0.061 Uiso 1 1 calc R . . H1B H 0.2372 -0.0250 0.5494 0.061 Uiso 1 1 calc R . . H1C H 0.3518 -0.0664 0.6259 0.061 Uiso 1 1 calc R . . C2 C -0.1171(2) 0.1619(2) 0.66444(10) 0.0392(4) Uani 1 1 d . . . H2A H -0.1471 0.0534 0.6872 0.059 Uiso 1 1 calc R . . H2B H -0.1801 0.1468 0.6121 0.059 Uiso 1 1 calc R . . H2C H -0.1742 0.2610 0.6970 0.059 Uiso 1 1 calc R . . C3 C 0.4568(2) 0.38334(17) 0.77665(8) 0.0254(3) Uani 1 1 d . . . C4 C 0.5186(2) 0.52072(17) 0.73338(8) 0.0253(3) Uani 1 1 d . . . C5 C 0.6917(2) 0.64011(18) 0.75810(8) 0.0276(3) Uani 1 1 d . . . H5 H 0.7286 0.7338 0.7295 0.033 Uiso 1 1 calc R . . C6 C 0.8076(2) 0.62360(19) 0.82263(9) 0.0308(3) Uani 1 1 d . . . C7 C 0.7415(2) 0.48808(19) 0.86536(9) 0.0304(3) Uani 1 1 d . . . H7 H 0.8195 0.4776 0.9108 0.036 Uiso 1 1 calc R . . C8 C 0.5701(2) 0.36880(18) 0.84560(8) 0.0267(3) Uani 1 1 d . . . C9 C 0.5074(2) 0.22053(19) 0.89373(8) 0.0307(3) Uani 1 1 d . . . C10 C 0.6454(3) 0.2352(2) 0.96721(10) 0.0441(4) Uani 1 1 d . . . H10A H 0.7897 0.2254 0.9523 0.066 Uiso 1 1 calc R . . H10B H 0.6013 0.1398 0.9967 0.066 Uiso 1 1 calc R . . H10C H 0.6333 0.3498 0.9995 0.066 Uiso 1 1 calc R . . C11 C 0.2819(3) 0.2298(2) 0.91953(10) 0.0392(4) Uani 1 1 d . . . H11A H 0.2670 0.3450 0.9510 0.059 Uiso 1 1 calc R . . H11B H 0.2456 0.1354 0.9505 0.059 Uiso 1 1 calc R . . H11C H 0.1897 0.2151 0.8735 0.059 Uiso 1 1 calc R . . C12 C 0.5335(3) 0.0399(2) 0.84438(10) 0.0379(4) Uani 1 1 d . . . H12A H 0.4440 0.0254 0.7976 0.057 Uiso 1 1 calc R . . H12B H 0.4949 -0.0549 0.8749 0.057 Uiso 1 1 calc R . . H12C H 0.6780 0.0343 0.8292 0.057 Uiso 1 1 calc R . . C13 C 0.9990(3) 0.7449(2) 0.84832(11) 0.0455(4) Uani 1 1 d . . . H13A H 1.0221 0.8310 0.8123 0.068 Uiso 1 1 calc R . . H13B H 1.1188 0.6750 0.8486 0.068 Uiso 1 1 calc R . . H13C H 0.9804 0.8075 0.9008 0.068 Uiso 1 1 calc R . . C14 C 0.4103(2) 0.54615(18) 0.66358(8) 0.0261(3) Uani 1 1 d . . . H14 H 0.4510 0.6516 0.6431 0.031 Uiso 1 1 calc R . . C15 C 0.1714(2) 0.50349(18) 0.55696(8) 0.0273(3) Uani 1 1 d . . . H15 H 0.2702 0.5964 0.5398 0.033 Uiso 1 1 calc R . . C16 C 0.1330(2) 0.35150(19) 0.48972(8) 0.0301(3) Uani 1 1 d . . . H16A H 0.0427 0.2549 0.5069 0.036 Uiso 1 1 calc R . . H16B H 0.2661 0.3043 0.4739 0.036 Uiso 1 1 calc R . . C17 C 0.0302(2) 0.4141(2) 0.42009(8) 0.0306(3) Uani 1 1 d . . . H17A H 0.1263 0.5026 0.3998 0.037 Uiso 1 1 calc R . . H17B H 0.0006 0.3124 0.3782 0.037 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 Al1 0.0279(2) 0.0242(2) 0.0288(2) 0.00577(17) -0.00539(17) -0.00282(16) O1 0.0347(6) 0.0281(5) 0.0309(5) 0.0091(4) -0.0079(4) -0.0081(4) N1 0.0286(6) 0.0263(6) 0.0249(6) 0.0055(5) -0.0035(5) 0.0009(5) C1 0.0408(9) 0.0333(8) 0.0453(10) 0.0010(7) -0.0058(7) 0.0033(7) C2 0.0318(8) 0.0438(9) 0.0416(9) 0.0098(7) -0.0018(7) -0.0044(7) C3 0.0278(7) 0.0217(6) 0.0256(7) 0.0020(5) -0.0016(5) -0.0004(5) C4 0.0279(7) 0.0221(6) 0.0255(7) 0.0030(5) -0.0022(5) 0.0014(5) C5 0.0300(7) 0.0226(6) 0.0300(7) 0.0053(6) -0.0004(6) -0.0015(5) C6 0.0312(8) 0.0281(7) 0.0317(8) 0.0032(6) -0.0046(6) -0.0028(6) C7 0.0334(8) 0.0300(7) 0.0269(7) 0.0032(6) -0.0074(6) 0.0008(6) C8 0.0323(7) 0.0238(6) 0.0240(7) 0.0041(5) -0.0008(6) 0.0014(5) C9 0.0396(8) 0.0265(7) 0.0261(7) 0.0073(6) -0.0043(6) -0.0021(6) C10 0.0612(11) 0.0388(9) 0.0330(9) 0.0149(7) -0.0128(8) -0.0073(8) C11 0.0490(10) 0.0357(8) 0.0331(8) 0.0086(7) 0.0057(7) -0.0025(7) C12 0.0523(10) 0.0262(7) 0.0361(8) 0.0085(6) -0.0019(7) 0.0027(7) C13 0.0420(10) 0.0443(9) 0.0484(10) 0.0127(8) -0.0154(8) -0.0155(7) C14 0.0292(7) 0.0223(6) 0.0274(7) 0.0061(5) -0.0009(6) 0.0012(5) C15 0.0304(7) 0.0268(7) 0.0257(7) 0.0086(5) -0.0045(6) 0.0007(5) C16 0.0336(8) 0.0308(7) 0.0264(7) 0.0042(6) -0.0028(6) 0.0058(6) C17 0.0358(8) 0.0321(7) 0.0241(7) 0.0038(6) -0.0029(6) 0.0055(6) _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 Al1 O1 1.7683(11) . ? Al1 C2 1.9498(17) . ? Al1 C1 1.9636(17) . ? Al1 N1 1.9782(12) . ? O1 C3 1.3264(16) . ? N1 C14 1.2981(18) . ? N1 C15 1.4798(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.4174(19) . ? C3 C8 1.4212(19) . ? C4 C5 1.4092(19) . ? C4 C14 1.4404(19) . ? C5 C6 1.370(2) . ? C5 H5 0.9500 . ? C6 C7 1.407(2) . ? C6 C13 1.510(2) . ? C7 C8 1.386(2) . ? C7 H7 0.9500 . ? C8 C9 1.5403(19) . ? C9 C10 1.536(2) . ? C9 C11 1.540(2) . ? C9 C12 1.541(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14 0.9500 . ? C15 C16 1.526(2) . ? C15 C17 1.531(2) 2_566 ? C15 H15 1.0000 . ? C16 C17 1.5312(19) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C15 1.531(2) 2_566 ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C2 110.62(7) . . ? O1 Al1 C1 111.98(7) . . ? C2 Al1 C1 115.49(8) . . ? O1 Al1 N1 94.38(5) . . ? C2 Al1 N1 113.43(7) . . ? C1 Al1 N1 109.05(7) . . ? C3 O1 Al1 129.69(9) . . ? C14 N1 C15 116.84(12) . . ? C14 N1 Al1 119.50(10) . . ? C15 N1 Al1 123.63(9) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C4 120.08(12) . . ? O1 C3 C8 120.72(12) . . ? C4 C3 C8 119.20(12) . . ? C5 C4 C3 120.29(12) . . ? C5 C4 C14 117.06(12) . . ? C3 C4 C14 122.65(12) . . ? C6 C5 C4 121.26(13) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 117.41(13) . . ? C5 C6 C13 122.28(14) . . ? C7 C6 C13 120.31(14) . . ? C8 C7 C6 124.41(13) . . ? C8 C7 H7 117.8 . . ? C6 C7 H7 117.8 . . ? C7 C8 C3 117.35(12) . . ? C7 C8 C9 122.15(12) . . ? C3 C8 C9 120.46(12) . . ? C10 C9 C11 107.79(13) . . ? C10 C9 C8 111.38(12) . . ? C11 C9 C8 110.73(12) . . ? C10 C9 C12 107.65(13) . . ? C11 C9 C12 110.08(13) . . ? C8 C9 C12 109.16(12) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C13 H13A 109.5 . . ? C6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C4 127.66(13) . . ? N1 C14 H14 116.2 . . ? C4 C14 H14 116.2 . . ? N1 C15 C16 110.92(11) . . ? N1 C15 C17 109.48(11) . 2_566 ? C16 C15 C17 110.79(12) . 2_566 ? N1 C15 H15 108.5 . . ? C16 C15 H15 108.5 . . ? C17 C15 H15 108.5 2_566 . ? C15 C16 C17 110.75(12) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C15 C17 C16 111.17(12) 2_566 . ? C15 C17 H17A 109.4 2_566 . ? C16 C17 H17A 109.4 . . ? C15 C17 H17B 109.4 2_566 . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.238 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.052 data_Ti2(OiPr)6(1) _database_code_depnum_ccdc_archive 'CCDC 921774' #TrackingRef 'NJC_Jones.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H41 N O4 Ti' _chemical_formula_weight 455.48 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.4230(2) _cell_length_b 22.8100(5) _cell_length_c 12.5010(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.6170(10) _cell_angle_gamma 90.00 _cell_volume 2701.97(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6227 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8753 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'multi-scan Sortav (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39062 _diffrn_reflns_av_R_equivalents 0.1081 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6195 _reflns_number_gt 4785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+1.1489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6195 _refine_ls_number_parameters 323 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0892 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1912 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _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 0.87948(5) -0.122212(19) 0.64544(4) 0.03490(17) Uani 1 1 d . A . O1 O 0.9749(2) -0.18788(8) 0.64773(18) 0.0481(5) Uani 1 1 d . . . N1 N 0.7779(2) -0.03872(9) 0.66020(17) 0.0345(4) Uani 1 1 d . . . C1 C 1.0948(6) -0.2253(2) 0.7023(5) 0.0625(12) Uani 0.70 1 d P A 1 H1 H 1.1673 -0.2043 0.7712 0.075 Uiso 0.70 1 calc PR A 1 O2 O 1.02894(18) -0.09026(7) 0.77999(16) 0.0387(4) Uani 1 1 d . . . C2 C 1.048(2) -0.2781(5) 0.7453(13) 0.115(6) Uani 0.70 1 d P A 1 H2A H 0.9950 -0.2662 0.7905 0.173 Uiso 0.70 1 calc PR A 1 H2B H 1.1308 -0.3010 0.7957 0.173 Uiso 0.70 1 calc PR A 1 H2C H 0.9877 -0.3020 0.6780 0.173 Uiso 0.70 1 calc PR A 1 O3 O 0.8512(2) -0.09490(9) 0.50173(17) 0.0473(5) Uani 1 1 d . . . C3 C 1.1529(11) -0.2350(5) 0.6124(10) 0.120(4) Uani 0.70 1 d P A 1 H3A H 1.0783 -0.2503 0.5399 0.179 Uiso 0.70 1 calc PR A 1 H3B H 1.2307 -0.2632 0.6428 0.179 Uiso 0.70 1 calc PR A 1 H3C H 1.1876 -0.1977 0.5955 0.179 Uiso 0.70 1 calc PR A 1 O4 O 0.7219(2) -0.15537(8) 0.64915(17) 0.0467(5) Uani 1 1 d . . . C4 C 1.0683(2) -0.04215(10) 0.8460(2) 0.0311(5) Uani 1 1 d . A . C5 C 0.9730(2) 0.00450(10) 0.8270(2) 0.0311(5) Uani 1 1 d . . . C6 C 1.0155(2) 0.05537(10) 0.8966(2) 0.0330(5) Uani 1 1 d . A . H6 H 0.9501 0.0865 0.8833 0.040 Uiso 1 1 calc R . . C7 C 1.1502(3) 0.06091(11) 0.9835(2) 0.0338(5) Uani 1 1 d . . . C8 C 1.2421(2) 0.01386(11) 1.0016(2) 0.0349(5) Uani 1 1 d . A . H8 H 1.3347 0.0173 1.0622 0.042 Uiso 1 1 calc R . . C9 C 1.2073(2) -0.03780(10) 0.9368(2) 0.0329(5) Uani 1 1 d . . . C10 C 1.1979(3) 0.11612(12) 1.0569(3) 0.0456(6) Uani 1 1 d . A . H10A H 1.2520 0.1406 1.0261 0.068 Uiso 1 1 calc R . . H10B H 1.2573 0.1056 1.1388 0.068 Uiso 1 1 calc R . . H10C H 1.1151 0.1379 1.0534 0.068 Uiso 1 1 calc R . . C11 C 1.3128(3) -0.08794(11) 0.9592(2) 0.0387(6) Uani 1 1 d . A . C12 C 1.4532(3) -0.07619(14) 1.0652(3) 0.0511(7) Uani 1 1 d . . . H12A H 1.4950 -0.0400 1.0520 0.077 Uiso 1 1 calc R A . H12B H 1.5179 -0.1090 1.0749 0.077 Uiso 1 1 calc R . . H12C H 1.4364 -0.0721 1.1364 0.077 Uiso 1 1 calc R . . C13 C 1.2524(3) -0.14483(13) 0.9879(3) 0.0537(7) Uani 1 1 d . . . H13A H 1.2378 -0.1391 1.0598 0.081 Uiso 1 1 calc R A . H13B H 1.3190 -0.1771 0.9997 0.081 Uiso 1 1 calc R . . H13C H 1.1621 -0.1543 0.9225 0.081 Uiso 1 1 calc R . . C14 C 1.3449(3) -0.09599(14) 0.8509(3) 0.0483(7) Uani 1 1 d . . . H14A H 1.2568 -0.1035 0.7815 0.072 Uiso 1 1 calc R A . H14B H 1.4090 -0.1293 0.8637 0.072 Uiso 1 1 calc R . . H14C H 1.3892 -0.0603 0.8383 0.072 Uiso 1 1 calc R . . C15 C 0.8310(2) 0.00279(11) 0.7348(2) 0.0344(5) Uani 1 1 d . A . H15 H 0.7718 0.0354 0.7291 0.041 Uiso 1 1 calc R . . C16 C 0.6327(2) -0.03040(12) 0.5672(2) 0.0376(5) Uani 1 1 d . . . H16 H 0.6085 -0.0669 0.5186 0.045 Uiso 1 1 calc R . . C17 C 0.6261(3) 0.02000(13) 0.4843(2) 0.0423(6) Uani 1 1 d . . . H17A H 0.6969 0.0136 0.4518 0.051 Uiso 1 1 calc R A . H17B H 0.6487 0.0574 0.5285 0.051 Uiso 1 1 calc R . . C18 C 0.4784(3) 0.02370(13) 0.3834(2) 0.0414(6) Uani 1 1 d . . . H18A H 0.4736 0.0577 0.3326 0.050 Uiso 1 1 calc R . . H18B H 0.4592 -0.0123 0.3348 0.050 Uiso 1 1 calc R . . C19 C 0.8999(17) -0.1141(8) 0.4167(17) 0.030(5) Uiso 0.30 1 d PD A 1 H19 H 0.9116 -0.1576 0.4242 0.035 Uiso 0.30 1 calc PR A 1 C21 C 1.034(4) -0.089(2) 0.436(4) 0.136(14) Uiso 0.30 1 d P A 1 H21A H 1.0363 -0.0480 0.4565 0.204 Uiso 0.30 1 calc PR A 1 H21B H 1.0492 -0.0931 0.3634 0.204 Uiso 0.30 1 calc PR A 1 H21C H 1.1092 -0.1105 0.4996 0.204 Uiso 0.30 1 calc PR A 1 C22 C 0.6493(7) -0.2091(4) 0.6102(7) 0.0519(17) Uani 0.70 1 d P A 1 H22 H 0.7177 -0.2368 0.5999 0.062 Uiso 0.70 1 calc PR A 1 C23 C 0.6162(9) -0.2342(3) 0.7094(6) 0.084(2) Uani 0.70 1 d P A 1 H23A H 0.7043 -0.2404 0.7794 0.127 Uiso 0.70 1 calc PR A 1 H23B H 0.5666 -0.2716 0.6843 0.127 Uiso 0.70 1 calc PR A 1 H23C H 0.5563 -0.2065 0.7280 0.127 Uiso 0.70 1 calc PR A 1 C24 C 0.5294(9) -0.2032(4) 0.4931(6) 0.107(3) Uani 0.70 1 d P A 1 H24A H 0.4553 -0.1792 0.5003 0.160 Uiso 0.70 1 calc PR A 1 H24B H 0.4917 -0.2421 0.4631 0.160 Uiso 0.70 1 calc PR A 1 H24C H 0.5620 -0.1842 0.4386 0.160 Uiso 0.70 1 calc PR A 1 C1' C 1.0438(12) -0.2415(5) 0.6385(11) 0.051(2) Uiso 0.30 1 d PD A 2 H1' H 0.9879 -0.2610 0.5613 0.061 Uiso 0.30 1 calc PR A 2 C3' C 1.1942(15) -0.2281(11) 0.651(2) 0.076(6) Uiso 0.30 1 d PD A 2 H2'1 H 1.2528 -0.2156 0.7317 0.114 Uiso 0.30 1 calc PR A 2 H2'2 H 1.1906 -0.1967 0.5962 0.114 Uiso 0.30 1 calc PR A 2 H2'3 H 1.2348 -0.2634 0.6328 0.114 Uiso 0.30 1 calc PR A 2 C23' C 0.5557(17) -0.2163(7) 0.6792(15) 0.073(5) Uiso 0.30 1 d PD A 2 H23D H 0.4750 -0.1943 0.6229 0.109 Uiso 0.30 1 calc PR A 2 H23E H 0.5886 -0.1978 0.7568 0.109 Uiso 0.30 1 calc PR A 2 H23F H 0.5269 -0.2567 0.6841 0.109 Uiso 0.30 1 calc PR A 2 C24' C 0.597(2) -0.2275(10) 0.5050(16) 0.106(7) Uiso 0.30 1 d PD A 2 H24D H 0.5818 -0.2697 0.4908 0.160 Uiso 0.30 1 calc PR A 2 H24E H 0.6535 -0.2126 0.4648 0.160 Uiso 0.30 1 calc PR A 2 H24F H 0.5057 -0.2073 0.4748 0.160 Uiso 0.30 1 calc PR A 2 C22' C 0.6756(18) -0.2163(12) 0.6380(15) 0.065(7) Uiso 0.30 1 d PD A 2 H22' H 0.7529 -0.2449 0.6802 0.078 Uiso 0.30 1 calc PR A 2 C2' C 1.061(3) -0.2832(11) 0.7406(18) 0.065(6) Uiso 0.30 1 d PD A 2 H2'4 H 1.1358 -0.3118 0.7508 0.097 Uiso 0.30 1 calc PR A 2 H2'5 H 0.9723 -0.3039 0.7227 0.097 Uiso 0.30 1 calc PR A 2 H2'6 H 1.0872 -0.2605 0.8132 0.097 Uiso 0.30 1 calc PR A 2 C19' C 0.8884(8) -0.1120(6) 0.4093(10) 0.060(4) Uani 0.70 1 d PD A 2 H19' H 0.8937 -0.1558 0.4067 0.071 Uiso 0.70 1 calc PR A 2 C20' C 0.7850(13) -0.0901(7) 0.2967(9) 0.152(6) Uani 0.70 1 d P A 2 H20A H 0.6913 -0.1052 0.2826 0.229 Uiso 0.70 1 calc PR A 2 H20B H 0.8106 -0.1033 0.2335 0.229 Uiso 0.70 1 calc PR A 2 H20C H 0.7838 -0.0472 0.2982 0.229 Uiso 0.70 1 calc PR A 2 C21' C 1.0341(6) -0.0853(4) 0.4357(6) 0.0470(16) Uani 0.70 1 d PD A 2 H21D H 1.0258 -0.0425 0.4289 0.071 Uiso 0.70 1 calc PR A 2 H21E H 1.0688 -0.1004 0.3792 0.071 Uiso 0.70 1 calc PR A 2 H21F H 1.1003 -0.0959 0.5157 0.071 Uiso 0.70 1 calc PR A 2 C20 C 0.7816(18) -0.1009(5) 0.2945(14) 0.040(3) Uiso 0.30 1 d PD A 1 H20D H 0.6948 -0.1209 0.2867 0.060 Uiso 0.30 1 calc PR A 1 H20E H 0.8097 -0.1150 0.2333 0.060 Uiso 0.30 1 calc PR A 1 H20F H 0.7649 -0.0586 0.2859 0.060 Uiso 0.30 1 calc PR A 1 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 0.0262(3) 0.0419(3) 0.0334(3) -0.00252(17) 0.00937(19) -0.00336(17) O1 0.0410(11) 0.0453(10) 0.0521(12) -0.0049(8) 0.0136(9) 0.0025(8) N1 0.0200(9) 0.0468(11) 0.0329(10) 0.0037(8) 0.0073(8) -0.0001(8) C1 0.050(3) 0.055(3) 0.073(3) -0.005(2) 0.015(3) 0.014(2) O2 0.0271(9) 0.0394(9) 0.0422(10) -0.0025(7) 0.0072(7) 0.0015(7) C2 0.126(10) 0.047(4) 0.143(10) 0.027(5) 0.026(6) 0.019(4) O3 0.0389(11) 0.0651(12) 0.0377(10) 0.0029(9) 0.0159(8) 0.0050(9) C3 0.111(7) 0.132(8) 0.129(10) -0.004(7) 0.064(8) 0.065(7) O4 0.0388(11) 0.0503(11) 0.0510(11) -0.0092(8) 0.0188(9) -0.0134(8) C4 0.0233(11) 0.0374(11) 0.0308(12) 0.0021(9) 0.0093(9) -0.0015(9) C5 0.0214(11) 0.0408(12) 0.0295(11) 0.0045(9) 0.0090(9) 0.0014(9) C6 0.0277(12) 0.0377(12) 0.0332(12) 0.0040(9) 0.0122(10) 0.0035(9) C7 0.0310(12) 0.0409(12) 0.0287(11) 0.0012(9) 0.0117(10) -0.0019(10) C8 0.0219(11) 0.0491(13) 0.0299(12) 0.0036(10) 0.0070(9) -0.0016(10) C9 0.0222(11) 0.0417(12) 0.0322(12) 0.0043(9) 0.0087(9) 0.0005(9) C10 0.0426(16) 0.0489(14) 0.0384(14) -0.0059(11) 0.0098(12) -0.0007(12) C11 0.0220(12) 0.0471(13) 0.0383(13) 0.0011(11) 0.0041(10) 0.0058(10) C12 0.0278(14) 0.0643(18) 0.0459(16) -0.0008(13) 0.0002(11) 0.0124(12) C13 0.0426(16) 0.0460(15) 0.0624(19) 0.0114(13) 0.0117(14) 0.0102(13) C14 0.0315(14) 0.0594(17) 0.0492(16) -0.0057(13) 0.0121(12) 0.0082(12) C15 0.0244(12) 0.0407(12) 0.0365(13) 0.0054(10) 0.0111(10) 0.0042(9) C16 0.0197(11) 0.0512(14) 0.0354(13) 0.0020(11) 0.0051(9) 0.0000(10) C17 0.0204(12) 0.0631(16) 0.0392(14) 0.0084(12) 0.0082(10) -0.0018(11) C18 0.0207(12) 0.0645(16) 0.0351(13) 0.0103(11) 0.0077(10) 0.0011(11) C22 0.041(3) 0.046(3) 0.060(4) -0.012(3) 0.014(3) -0.021(3) C23 0.103(6) 0.062(4) 0.091(5) 0.000(3) 0.044(4) -0.034(4) C24 0.102(6) 0.092(5) 0.081(4) -0.017(4) -0.006(4) -0.056(5) C19' 0.042(4) 0.095(7) 0.040(4) -0.009(2) 0.015(3) -0.012(3) C20' 0.051(4) 0.360(18) 0.038(3) 0.032(7) 0.011(3) 0.038(7) C21' 0.031(2) 0.066(3) 0.046(3) 0.0037(19) 0.0187(18) -0.0080(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7915(19) . ? Ti1 O3 1.8059(19) . ? Ti1 O4 1.8264(19) . ? Ti1 O2 1.8985(17) . ? Ti1 N1 2.224(2) . ? O1 C1 1.430(5) . ? O1 C1' 1.447(11) . ? N1 C15 1.282(3) . ? N1 C16 1.487(3) . ? C1 C2 1.482(12) . ? C1 C3 1.499(10) . ? C1 H1 1.0000 . ? O2 C4 1.331(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C19' 1.418(14) . ? O3 C19 1.42(2) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C22 1.417(7) . ? O4 C22' 1.46(3) . ? C4 C5 1.406(3) . ? C4 C9 1.424(3) . ? C5 C6 1.406(3) . ? C5 C15 1.449(3) . ? C6 C7 1.377(3) . ? C6 H6 0.9500 . ? C7 C8 1.393(3) . ? C7 C10 1.515(4) . ? C8 C9 1.390(3) . ? C8 H8 0.9500 . ? C9 C11 1.529(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.534(4) . ? C11 C14 1.536(4) . ? C11 C13 1.548(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 0.9500 . ? C16 C18 1.531(4) 3_656 ? C16 C17 1.530(4) . ? C16 H16 1.0000 . ? C17 C18 1.533(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C16 1.531(4) 3_656 ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C21 1.43(3) . ? C19 C20 1.541(5) . ? C19 H19 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.483(10) . ? C22 C23 1.529(9) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C1' C3' 1.540(5) . ? C1' C2' 1.541(5) . ? C1' H1' 1.0000 . ? C3' H2'1 0.9800 . ? C3' H2'2 0.9800 . ? C3' H2'3 0.9800 . ? C23' C22' 1.538(5) . ? C23' H23D 0.9800 . ? C23' H23E 0.9800 . ? C23' H23F 0.9800 . ? C24' C22' 1.538(5) . ? C24' H24D 0.9800 . ? C24' H24E 0.9800 . ? C24' H24F 0.9800 . ? C22' H22' 1.0000 . ? C2' H2'4 0.9800 . ? C2' H2'5 0.9800 . ? C2' H2'6 0.9800 . ? C19' C20' 1.459(10) . ? C19' C21' 1.539(5) . ? C19' H19' 1.0000 . ? C20' H20A 0.9800 . ? C20' H20B 0.9800 . ? C20' H20C 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 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 O1 Ti1 O3 99.42(9) . . ? O1 Ti1 O4 98.77(9) . . ? O3 Ti1 O4 113.10(9) . . ? O1 Ti1 O2 93.54(8) . . ? O3 Ti1 O2 118.85(9) . . ? O4 Ti1 O2 123.45(9) . . ? O1 Ti1 N1 174.29(8) . . ? O3 Ti1 N1 84.33(8) . . ? O4 Ti1 N1 83.58(8) . . ? O2 Ti1 N1 80.86(7) . . ? C1 O1 C1' 33.9(4) . . ? C1 O1 Ti1 151.1(3) . . ? C1' O1 Ti1 174.9(5) . . ? C15 N1 C16 117.7(2) . . ? C15 N1 Ti1 128.08(16) . . ? C16 N1 Ti1 114.13(15) . . ? O1 C1 C2 107.7(7) . . ? O1 C1 C3 106.0(5) . . ? C2 C1 C3 116.6(9) . . ? O1 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? C3 C1 H1 108.7 . . ? C4 O2 Ti1 142.47(15) . . ? C19' O3 C19 5.1(10) . . ? C19' O3 Ti1 136.8(5) . . ? C19 O3 Ti1 132.5(7) . . ? C22 O4 C22' 15.0(9) . . ? C22 O4 Ti1 135.0(3) . . ? C22' O4 Ti1 131.1(7) . . ? O2 C4 C5 120.4(2) . . ? O2 C4 C9 120.0(2) . . ? C5 C4 C9 119.6(2) . . ? C6 C5 C4 120.1(2) . . ? C6 C5 C15 117.9(2) . . ? C4 C5 C15 122.0(2) . . ? C7 C6 C5 121.2(2) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 117.6(2) . . ? C6 C7 C10 121.6(2) . . ? C8 C7 C10 120.8(2) . . ? C9 C8 C7 124.3(2) . . ? C9 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? C8 C9 C4 117.1(2) . . ? C8 C9 C11 122.3(2) . . ? C4 C9 C11 120.6(2) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 112.4(2) . . ? C9 C11 C14 109.4(2) . . ? C12 C11 C14 107.6(2) . . ? C9 C11 C13 109.8(2) . . ? C12 C11 C13 106.3(2) . . ? C14 C11 C13 111.3(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C5 126.0(2) . . ? N1 C15 H15 117.0 . . ? C5 C15 H15 117.0 . . ? N1 C16 C18 113.0(2) . 3_656 ? N1 C16 C17 111.7(2) . . ? C18 C16 C17 111.7(2) 3_656 . ? N1 C16 H16 106.6 . . ? C18 C16 H16 106.6 3_656 . ? C17 C16 H16 106.6 . . ? C16 C17 C18 110.2(2) . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C16 C18 C17 110.1(2) 3_656 . ? C16 C18 H18A 109.6 3_656 . ? C17 C18 H18A 109.6 . . ? C16 C18 H18B 109.6 3_656 . ? C17 C18 H18B 109.6 . . ? H18A C18 H18B 108.2 . . ? O3 C19 C21 113(2) . . ? O3 C19 C20 107.0(14) . . ? C21 C19 C20 114(2) . . ? O3 C19 H19 107.6 . . ? C21 C19 H19 107.6 . . ? C20 C19 H19 107.6 . . ? O4 C22 C24 111.7(7) . . ? O4 C22 C23 108.3(5) . . ? C24 C22 C23 116.9(6) . . ? O4 C22 H22 106.5 . . ? C24 C22 H22 106.5 . . ? C23 C22 H22 106.5 . . ? O1 C1' C3' 110.0(12) . . ? O1 C1' C2' 110.4(13) . . ? C3' C1' C2' 105.9(16) . . ? O1 C1' H1' 110.2 . . ? C3' C1' H1' 110.2 . . ? C2' C1' H1' 110.2 . . ? C1' C3' H2'1 109.5 . . ? C1' C3' H2'2 109.5 . . ? H2'1 C3' H2'2 109.5 . . ? C1' C3' H2'3 109.5 . . ? H2'1 C3' H2'3 109.5 . . ? H2'2 C3' H2'3 109.5 . . ? C22' C23' H23D 109.5 . . ? C22' C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C22' C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C22' C24' H24D 109.5 . . ? C22' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? O4 C22' C24' 105.6(17) . . ? O4 C22' C23' 104.5(16) . . ? C24' C22' C23' 102.7(15) . . ? O4 C22' H22' 114.3 . . ? C24' C22' H22' 114.3 . . ? C23' C22' H22' 114.3 . . ? C1' C2' H2'4 109.5 . . ? C1' C2' H2'5 109.5 . . ? H2'4 C2' H2'5 109.5 . . ? C1' C2' H2'6 109.5 . . ? H2'4 C2' H2'6 109.5 . . ? H2'5 C2' H2'6 109.5 . . ? O3 C19' C20' 110.5(10) . . ? O3 C19' C21' 107.2(8) . . ? C20' C19' C21' 109.7(9) . . ? O3 C19' H19' 109.8 . . ? C20' C19' H19' 109.8 . . ? C21' C19' H19' 109.8 . . ? C19' C20' H20A 109.5 . . ? C19' C20' H20B 109.5 . . ? H20A C20' H20B 109.5 . . ? C19' C20' H20C 109.5 . . ? H20A C20' H20C 109.5 . . ? H20B C20' H20C 109.5 . . ? C19' C21' H21D 109.5 . . ? C19' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.901 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.090 data_Ti2(OiPr)6(3) _database_code_depnum_ccdc_archive 'CCDC 921775' #TrackingRef 'NJC_Jones.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H49 Cl2 N O4 Ti' _chemical_formula_weight 726.60 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 8.8350(2) _cell_length_b 10.7560(3) _cell_length_c 20.4880(7) _cell_angle_alpha 95.5030(10) _cell_angle_beta 90.5850(10) _cell_angle_gamma 97.9200(10) _cell_volume 1918.96(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 52709 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25157 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.07 _reflns_number_total 6767 _reflns_number_gt 5380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0490P)^2^+1.9483P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6767 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 1.10520(5) 0.39214(4) 0.28673(2) 0.02330(14) Uani 1 1 d . . . Cl1 Cl 1.45021(14) 0.18215(11) 0.47790(6) 0.0767(3) Uani 1 1 d . . . O1 O 1.1989(2) 0.43375(17) 0.21372(9) 0.0307(4) Uani 1 1 d . . . N1 N 0.9855(2) 0.34012(19) 0.37809(10) 0.0241(5) Uani 1 1 d . . . C1 C 1.2537(3) 0.4682(3) 0.15241(13) 0.0316(6) Uani 1 1 d . . . H1 H 1.3027 0.3970 0.1308 0.038 Uiso 1 1 calc R . . Cl2 Cl 1.1544(2) 0.03570(12) 0.44274(9) 0.1181(6) Uani 1 1 d . . . O2 O 0.98582(19) 0.23945(16) 0.25268(8) 0.0257(4) Uani 1 1 d . . . C2 C 1.3729(4) 0.5835(3) 0.16191(16) 0.0465(8) Uani 1 1 d . . . H2A H 1.3261 0.6552 0.1816 0.070 Uiso 1 1 calc R . . H2B H 1.4147 0.6029 0.1193 0.070 Uiso 1 1 calc R . . H2C H 1.4554 0.5674 0.1909 0.070 Uiso 1 1 calc R . . O3 O 1.2750(2) 0.38905(17) 0.33895(9) 0.0298(4) Uani 1 1 d . . . C3 C 1.1191(4) 0.4869(3) 0.10958(14) 0.0408(7) Uani 1 1 d . . . H3A H 1.0427 0.4112 0.1070 0.061 Uiso 1 1 calc R . . H3B H 1.1543 0.5018 0.0654 0.061 Uiso 1 1 calc R . . H3C H 1.0733 0.5596 0.1286 0.061 Uiso 1 1 calc R . . O4 O 1.0110(2) 0.53112(17) 0.30337(9) 0.0350(5) Uani 1 1 d . . . C4 C 0.8817(3) 0.1470(2) 0.26955(12) 0.0233(5) Uani 1 1 d . . . C5 C 0.8342(3) 0.1431(2) 0.33467(12) 0.0248(5) Uani 1 1 d . . . C6 C 0.7261(3) 0.0432(2) 0.35121(13) 0.0271(6) Uani 1 1 d . . . H6 H 0.6955 0.0410 0.3954 0.033 Uiso 1 1 calc R . . C7 C 0.6636(3) -0.0517(2) 0.30475(13) 0.0262(6) Uani 1 1 d . . . C8 C 0.7113(3) -0.0453(2) 0.23995(12) 0.0237(5) Uani 1 1 d . . . H8 H 0.6681 -0.1097 0.2075 0.028 Uiso 1 1 calc R . . C9 C 0.8186(3) 0.0505(2) 0.22089(12) 0.0219(5) Uani 1 1 d . . . C10 C 0.5498(3) -0.1603(3) 0.32345(14) 0.0338(6) Uani 1 1 d . . . H10A H 0.6035 -0.2179 0.3463 0.051 Uiso 1 1 calc R . . H10B H 0.4985 -0.2057 0.2838 0.051 Uiso 1 1 calc R . . H10C H 0.4738 -0.1275 0.3524 0.051 Uiso 1 1 calc R . . C11 C 0.8797(3) 0.0514(2) 0.15008(12) 0.0230(5) Uani 1 1 d . . . C12 C 0.8105(3) -0.0704(2) 0.10750(12) 0.0237(5) Uani 1 1 d . . . C13 C 0.6621(3) -0.0796(3) 0.08109(13) 0.0293(6) Uani 1 1 d . . . H13 H 0.6063 -0.0105 0.0893 0.035 Uiso 1 1 calc R . . C14 C 0.5948(3) -0.1866(3) 0.04344(14) 0.0339(6) Uani 1 1 d . . . H14 H 0.4941 -0.1901 0.0261 0.041 Uiso 1 1 calc R . . C15 C 0.6729(3) -0.2888(3) 0.03082(13) 0.0329(6) Uani 1 1 d . . . H15 H 0.6267 -0.3625 0.0049 0.039 Uiso 1 1 calc R . . C16 C 0.8192(3) -0.2821(3) 0.05650(14) 0.0355(6) Uani 1 1 d . . . H16 H 0.8740 -0.3517 0.0481 0.043 Uiso 1 1 calc R . . C17 C 0.8868(3) -0.1746(2) 0.09445(13) 0.0301(6) Uani 1 1 d . . . H17 H 0.9874 -0.1721 0.1119 0.036 Uiso 1 1 calc R . . C18 C 0.8318(3) 0.1628(2) 0.11608(12) 0.0232(5) Uani 1 1 d . . . C19 C 0.7521(3) 0.2540(2) 0.14817(13) 0.0262(6) Uani 1 1 d . . . H19 H 0.7325 0.2521 0.1936 0.031 Uiso 1 1 calc R . . C20 C 0.7013(3) 0.3475(2) 0.11439(14) 0.0293(6) Uani 1 1 d . . . H20 H 0.6473 0.4084 0.1370 0.035 Uiso 1 1 calc R . . C21 C 0.7287(3) 0.3525(2) 0.04852(14) 0.0316(6) Uani 1 1 d . . . H21 H 0.6949 0.4169 0.0258 0.038 Uiso 1 1 calc R . . C22 C 0.8062(3) 0.2622(3) 0.01571(13) 0.0309(6) Uani 1 1 d . . . H22 H 0.8251 0.2646 -0.0297 0.037 Uiso 1 1 calc R . . C23 C 0.8559(3) 0.1687(2) 0.04903(13) 0.0274(6) Uani 1 1 d . . . H23 H 0.9076 0.1071 0.0258 0.033 Uiso 1 1 calc R . . C24 C 1.0563(3) 0.0574(2) 0.15657(12) 0.0240(5) Uani 1 1 d . . . C25 C 1.1601(3) 0.1269(2) 0.11919(13) 0.0289(6) Uani 1 1 d . . . H25 H 1.1240 0.1725 0.0862 0.035 Uiso 1 1 calc R . . C26 C 1.3174(3) 0.1306(3) 0.12946(15) 0.0361(7) Uani 1 1 d . . . H26 H 1.3870 0.1790 0.1035 0.043 Uiso 1 1 calc R . . C27 C 1.3724(3) 0.0649(3) 0.17682(15) 0.0388(7) Uani 1 1 d . . . H27 H 1.4793 0.0697 0.1845 0.047 Uiso 1 1 calc R . . C28 C 1.2708(3) -0.0079(3) 0.21289(15) 0.0386(7) Uani 1 1 d . . . H28 H 1.3079 -0.0555 0.2448 0.046 Uiso 1 1 calc R . . C29 C 1.1148(3) -0.0121(3) 0.20277(13) 0.0318(6) Uani 1 1 d . . . H29 H 1.0461 -0.0634 0.2278 0.038 Uiso 1 1 calc R . . C30 C 0.8896(3) 0.2421(2) 0.38595(12) 0.0261(6) Uani 1 1 d . . . H30 H 0.8519 0.2336 0.4288 0.031 Uiso 1 1 calc R . . C31 C 1.0179(3) 0.4377(2) 0.43472(12) 0.0251(5) Uani 1 1 d . . . H31 H 1.0970 0.5047 0.4203 0.030 Uiso 1 1 calc R . . C32 C 0.8764(3) 0.5005(2) 0.45162(13) 0.0276(6) Uani 1 1 d . . . H32A H 0.8368 0.5316 0.4118 0.033 Uiso 1 1 calc R . . H32B H 0.7957 0.4377 0.4672 0.033 Uiso 1 1 calc R . . C33 C 0.9149(3) 0.6107(2) 0.50484(13) 0.0281(6) Uani 1 1 d . . . H33A H 0.8214 0.6480 0.5167 0.034 Uiso 1 1 calc R . . H33B H 0.9898 0.6768 0.4883 0.034 Uiso 1 1 calc R . . C34 C 1.4259(3) 0.4561(3) 0.33560(14) 0.0335(6) Uani 1 1 d . . . H34 H 1.4239 0.5205 0.3036 0.040 Uiso 1 1 calc R . . C35 C 1.5338(4) 0.3658(4) 0.3113(2) 0.0565(9) Uani 1 1 d . . . H35A H 1.5417 0.3051 0.3435 0.085 Uiso 1 1 calc R . . H35B H 1.6350 0.4129 0.3053 0.085 Uiso 1 1 calc R . . H35C H 1.4949 0.3206 0.2694 0.085 Uiso 1 1 calc R . . C36 C 1.4717(4) 0.5236(3) 0.40216(16) 0.0463(8) Uani 1 1 d . . . H36A H 1.3990 0.5820 0.4150 0.069 Uiso 1 1 calc R . . H36B H 1.5745 0.5709 0.4004 0.069 Uiso 1 1 calc R . . H36C H 1.4715 0.4618 0.4344 0.069 Uiso 1 1 calc R . . C37 C 1.0038(4) 0.6497(2) 0.27945(14) 0.0354(7) Uani 1 1 d . . . H37 H 1.0870 0.6659 0.2473 0.042 Uiso 1 1 calc R . . C38 C 0.8517(4) 0.6442(4) 0.2451(2) 0.0586(10) Uani 1 1 d . . . H38A H 0.8414 0.5770 0.2088 0.088 Uiso 1 1 calc R . . H38B H 0.8448 0.7252 0.2279 0.088 Uiso 1 1 calc R . . H38C H 0.7697 0.6267 0.2761 0.088 Uiso 1 1 calc R . . C39 C 1.0280(7) 0.7510(3) 0.33624(18) 0.0776(14) Uani 1 1 d . . . H39A H 0.9484 0.7344 0.3685 0.116 Uiso 1 1 calc R . . H39B H 1.0228 0.8334 0.3203 0.116 Uiso 1 1 calc R . . H39C H 1.1286 0.7510 0.3569 0.116 Uiso 1 1 calc R . . C40 C 1.3161(6) 0.1282(4) 0.4142(2) 0.0760(13) Uani 1 1 d . . . H40A H 1.3642 0.0775 0.3795 0.091 Uiso 1 1 calc R . . H40B H 1.2838 0.2014 0.3948 0.091 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 0.0236(2) 0.0253(2) 0.0205(3) 0.00196(17) 0.00052(18) 0.00149(18) Cl1 0.0808(7) 0.0883(8) 0.0642(7) 0.0053(5) -0.0025(5) 0.0246(6) O1 0.0315(10) 0.0345(10) 0.0245(10) 0.0045(8) 0.0024(8) -0.0023(8) N1 0.0234(11) 0.0276(11) 0.0211(11) -0.0007(8) -0.0007(9) 0.0049(9) C1 0.0359(15) 0.0346(15) 0.0242(14) 0.0052(11) 0.0097(12) 0.0019(12) Cl2 0.1344(13) 0.0581(7) 0.1538(15) 0.0096(8) -0.0441(11) -0.0109(8) O2 0.0270(9) 0.0277(9) 0.0207(9) 0.0008(7) 0.0021(7) -0.0011(7) C2 0.0471(19) 0.0492(19) 0.0401(18) 0.0099(14) 0.0110(15) -0.0092(15) O3 0.0246(9) 0.0363(10) 0.0281(10) 0.0055(8) -0.0002(8) 0.0006(8) C3 0.0467(18) 0.0488(18) 0.0265(16) 0.0077(13) 0.0011(13) 0.0025(14) O4 0.0453(12) 0.0299(10) 0.0326(11) 0.0077(8) 0.0049(9) 0.0118(9) C4 0.0218(12) 0.0263(13) 0.0221(13) 0.0038(10) 0.0021(10) 0.0033(10) C5 0.0247(13) 0.0276(13) 0.0222(13) 0.0008(10) 0.0001(10) 0.0048(10) C6 0.0283(14) 0.0314(14) 0.0219(13) 0.0046(10) 0.0052(11) 0.0034(11) C7 0.0254(13) 0.0269(13) 0.0270(14) 0.0048(10) 0.0033(11) 0.0044(11) C8 0.0234(13) 0.0254(13) 0.0222(13) -0.0008(10) -0.0019(10) 0.0051(10) C9 0.0209(12) 0.0250(13) 0.0207(13) 0.0019(10) 0.0009(10) 0.0066(10) C10 0.0362(15) 0.0319(15) 0.0321(16) 0.0051(11) 0.0052(12) -0.0009(12) C11 0.0235(13) 0.0244(13) 0.0210(13) -0.0008(10) 0.0012(10) 0.0047(10) C12 0.0256(13) 0.0272(13) 0.0176(12) 0.0008(10) 0.0036(10) 0.0016(10) C13 0.0268(14) 0.0316(14) 0.0287(15) 0.0001(11) 0.0007(11) 0.0029(11) C14 0.0296(14) 0.0377(16) 0.0311(15) -0.0025(12) -0.0025(12) -0.0023(12) C15 0.0366(16) 0.0300(14) 0.0285(15) -0.0050(11) 0.0021(12) -0.0024(12) C16 0.0388(16) 0.0295(15) 0.0374(17) -0.0029(12) 0.0035(13) 0.0065(12) C17 0.0275(14) 0.0319(14) 0.0308(15) -0.0007(11) 0.0018(11) 0.0062(11) C18 0.0202(12) 0.0245(13) 0.0239(13) 0.0016(10) 0.0001(10) -0.0002(10) C19 0.0228(13) 0.0300(14) 0.0249(14) 0.0016(10) 0.0011(10) 0.0015(11) C20 0.0244(13) 0.0272(14) 0.0364(16) 0.0012(11) -0.0016(11) 0.0055(11) C21 0.0284(14) 0.0288(14) 0.0380(17) 0.0071(11) -0.0056(12) 0.0033(11) C22 0.0296(14) 0.0378(15) 0.0254(14) 0.0066(11) 0.0002(11) 0.0022(12) C23 0.0257(13) 0.0296(14) 0.0271(14) 0.0023(11) 0.0010(11) 0.0048(11) C24 0.0226(13) 0.0271(13) 0.0218(13) -0.0019(10) 0.0005(10) 0.0052(10) C25 0.0251(13) 0.0340(15) 0.0286(14) 0.0058(11) 0.0027(11) 0.0062(11) C26 0.0231(14) 0.0406(16) 0.0452(18) 0.0079(13) 0.0079(12) 0.0038(12) C27 0.0212(14) 0.0519(18) 0.0445(18) 0.0036(14) 0.0014(12) 0.0105(13) C28 0.0309(15) 0.0508(18) 0.0380(17) 0.0107(13) -0.0022(13) 0.0148(13) C29 0.0296(14) 0.0381(15) 0.0293(15) 0.0064(12) 0.0036(12) 0.0077(12) C30 0.0292(14) 0.0328(14) 0.0169(13) 0.0024(10) 0.0045(10) 0.0055(11) C31 0.0263(13) 0.0278(13) 0.0200(13) -0.0022(10) 0.0023(10) 0.0023(10) C32 0.0286(14) 0.0324(14) 0.0215(13) -0.0021(10) -0.0016(10) 0.0064(11) C33 0.0293(14) 0.0308(14) 0.0244(14) -0.0019(11) -0.0007(11) 0.0087(11) C34 0.0243(14) 0.0415(16) 0.0334(16) 0.0061(12) -0.0003(12) -0.0017(12) C35 0.0322(17) 0.067(2) 0.067(2) -0.0092(18) 0.0105(16) 0.0060(16) C36 0.0332(16) 0.054(2) 0.047(2) -0.0051(15) -0.0073(14) -0.0016(14) C37 0.0509(18) 0.0263(14) 0.0309(16) 0.0067(11) 0.0064(13) 0.0090(13) C38 0.060(2) 0.057(2) 0.066(2) 0.0197(18) 0.0017(19) 0.0217(18) C39 0.158(5) 0.0326(19) 0.040(2) 0.0045(15) -0.002(2) 0.005(2) C40 0.111(4) 0.060(2) 0.059(3) -0.0070(19) -0.005(2) 0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.7815(18) . ? Ti1 O4 1.8149(18) . ? Ti1 O3 1.8394(18) . ? Ti1 O2 1.8932(17) . ? Ti1 N1 2.239(2) . ? Cl1 C40 1.754(5) . ? O1 C1 1.415(3) . ? N1 C30 1.282(3) . ? N1 C31 1.485(3) . ? C1 C2 1.509(4) . ? C1 C3 1.518(4) . ? C1 H1 1.0000 . ? Cl2 C40 1.764(5) . ? O2 C4 1.332(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O3 C34 1.432(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C37 1.418(3) . ? C4 C5 1.405(4) . ? C4 C9 1.419(3) . ? C5 C6 1.405(4) . ? C5 C30 1.452(4) . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.402(4) . ? C7 C10 1.514(4) . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C11 1.553(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.549(3) . ? C11 C18 1.548(3) . ? C11 C24 1.556(3) . ? C12 C17 1.392(4) . ? C12 C13 1.400(4) . ? C13 C14 1.380(4) . ? C13 H13 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.380(4) . ? C15 H15 0.9500 . ? C16 C17 1.388(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.398(4) . ? C18 C19 1.402(3) . ? C19 C20 1.394(4) . ? C19 H19 0.9500 . ? C20 C21 1.378(4) . ? C20 H20 0.9500 . ? C21 C22 1.389(4) . ? C21 H21 0.9500 . ? C22 C23 1.385(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.386(4) . ? C24 C29 1.398(4) . ? C25 C26 1.398(4) . ? C25 H25 0.9500 . ? C26 C27 1.376(4) . ? C26 H26 0.9500 . ? C27 C28 1.377(4) . ? C27 H27 0.9500 . ? C28 C29 1.386(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.528(4) . ? C31 C33 1.533(4) 2_766 ? C31 H31 1.0000 . ? C32 C33 1.531(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C31 1.533(4) 2_766 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.507(4) . ? C34 C36 1.506(4) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.502(5) . ? C37 C39 1.508(4) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti1 O4 98.26(9) . . ? O1 Ti1 O3 98.77(8) . . ? O4 Ti1 O3 114.68(9) . . ? O1 Ti1 O2 99.01(8) . . ? O4 Ti1 O2 118.41(9) . . ? O3 Ti1 O2 120.18(8) . . ? O1 Ti1 N1 179.48(8) . . ? O4 Ti1 N1 81.43(8) . . ? O3 Ti1 N1 81.74(8) . . ? O2 Ti1 N1 80.79(7) . . ? C1 O1 Ti1 172.38(18) . . ? C30 N1 C31 117.8(2) . . ? C30 N1 Ti1 128.42(17) . . ? C31 N1 Ti1 113.70(15) . . ? O1 C1 C2 110.4(2) . . ? O1 C1 C3 108.8(2) . . ? C2 C1 C3 112.8(2) . . ? O1 C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? C3 C1 H1 108.2 . . ? C4 O2 Ti1 142.27(16) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C34 O3 Ti1 129.42(16) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C37 O4 Ti1 140.13(18) . . ? O2 C4 C5 121.2(2) . . ? O2 C4 C9 119.3(2) . . ? C5 C4 C9 119.6(2) . . ? C4 C5 C6 119.9(2) . . ? C4 C5 C30 122.0(2) . . ? C6 C5 C30 118.1(2) . . ? C7 C6 C5 121.5(2) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 117.7(2) . . ? C6 C7 C10 121.0(2) . . ? C8 C7 C10 121.3(2) . . ? C9 C8 C7 123.3(2) . . ? C9 C8 H8 118.4 . . ? C7 C8 H8 118.4 . . ? C8 C9 C4 118.0(2) . . ? C8 C9 C11 122.9(2) . . ? C4 C9 C11 119.0(2) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 110.32(19) . . ? C12 C11 C18 106.3(2) . . ? C9 C11 C18 111.20(19) . . ? C12 C11 C24 110.18(19) . . ? C9 C11 C24 106.20(19) . . ? C18 C11 C24 112.7(2) . . ? C17 C12 C13 116.9(2) . . ? C17 C12 C11 123.6(2) . . ? C13 C12 C11 119.5(2) . . ? C14 C13 C12 121.6(3) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 118.9(3) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 121.4(3) . . ? C16 C17 H17 119.3 . . ? C12 C17 H17 119.3 . . ? C23 C18 C19 117.3(2) . . ? C23 C18 C11 119.6(2) . . ? C19 C18 C11 122.8(2) . . ? C20 C19 C18 121.0(2) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 120.6(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.3(2) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 121.6(2) . . ? C22 C23 H23 119.2 . . ? C18 C23 H23 119.2 . . ? C25 C24 C29 117.5(2) . . ? C25 C24 C11 124.3(2) . . ? C29 C24 C11 118.2(2) . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 119.4(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 120.2(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 121.4(3) . . ? C28 C29 H29 119.3 . . ? C24 C29 H29 119.3 . . ? N1 C30 C5 125.3(2) . . ? N1 C30 H30 117.4 . . ? C5 C30 H30 117.4 . . ? N1 C31 C32 110.9(2) . . ? N1 C31 C33 113.8(2) . 2_766 ? C32 C31 C33 111.5(2) . 2_766 ? N1 C31 H31 106.7 . . ? C32 C31 H31 106.7 . . ? C33 C31 H31 106.7 2_766 . ? C33 C32 C31 110.7(2) . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C31 109.0(2) . 2_766 ? C32 C33 H33A 109.9 . . ? C31 C33 H33A 109.9 2_766 . ? C32 C33 H33B 109.9 . . ? C31 C33 H33B 109.9 2_766 . ? H33A C33 H33B 108.3 . . ? O3 C34 C35 109.6(2) . . ? O3 C34 C36 108.6(2) . . ? C35 C34 C36 113.0(3) . . ? O3 C34 H34 108.5 . . ? C35 C34 H34 108.5 . . ? C36 C34 H34 108.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O4 C37 C38 108.2(3) . . ? O4 C37 C39 108.8(2) . . ? C38 C37 C39 112.6(3) . . ? O4 C37 H37 109.1 . . ? C38 C37 H37 109.1 . . ? C39 C37 H37 109.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Cl1 C40 Cl2 111.4(2) . . ? Cl1 C40 H40A 109.4 . . ? Cl2 C40 H40A 109.4 . . ? Cl1 C40 H40B 109.4 . . ? Cl2 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.579 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.055