Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2007 ####################################################################### # # 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_graggo _database_code_depnum_ccdc_archive 'CCDC 652772' _database_code_depnum_ccdc_archive 'CCDC 652772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H90 Cl2 N4 O2 Ti2' _chemical_formula_weight 1126.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.4999(18) _cell_length_b 12.9944(16) _cell_length_c 17.350(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.761(5) _cell_angle_gamma 90.00 _cell_volume 2979.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9673 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 30.79 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8599 _exptl_absorpt_correction_T_max 0.9761 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX2 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 157240 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9104 _reflns_number_gt 7490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. The toluene molecule is disordered over a centre of symmetry. Its methyl hydrogen positions may be unreliable. The isopropyl carbons C28, C29 are disordered over two positions with occupation factors 0.84, 0.16. ; _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^)+(0.0373P)^2^+1.6762P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9104 _refine_ls_number_parameters 390 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.072 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.500904(15) 0.506360(15) 0.419883(11) 0.00960(5) Uani 1 1 d . . . Cl Cl 0.50563(2) 0.35292(2) 0.361473(18) 0.01952(7) Uani 1 1 d . . . O O 0.40882(6) 0.49367(7) 0.48570(5) 0.01401(16) Uani 1 1 d . . . N1 N 0.60679(7) 0.58878(7) 0.36820(5) 0.01131(17) Uani 1 1 d . . . N2 N 0.38929(7) 0.58586(7) 0.33851(5) 0.01150(17) Uani 1 1 d . . . C1 C 0.67386(10) 0.63863(10) 0.24990(7) 0.0191(2) Uani 1 1 d . . . H1A H 0.6994 0.7063 0.2696 0.029 Uiso 1 1 calc R . . H1B H 0.6478 0.6425 0.1930 0.029 Uiso 1 1 calc R . . H1C H 0.7289 0.5882 0.2609 0.029 Uiso 1 1 calc R . . C2 C 0.58967(9) 0.60612(8) 0.29034(7) 0.0126(2) Uani 1 1 d . . . C3 C 0.49396(9) 0.60102(9) 0.24153(6) 0.0135(2) Uani 1 1 d . . . H3 H 0.4920 0.5953 0.1867 0.016 Uiso 1 1 calc R . . C4 C 0.40088(9) 0.60333(9) 0.26437(6) 0.0127(2) Uani 1 1 d . . . C5 C 0.31163(10) 0.63237(10) 0.20014(7) 0.0185(2) Uani 1 1 d . . . H5A H 0.2609 0.5774 0.1939 0.028 Uiso 1 1 calc R . . H5B H 0.3344 0.6419 0.1505 0.028 Uiso 1 1 calc R . . H5C H 0.2818 0.6966 0.2144 0.028 Uiso 1 1 calc R . . C6 C 0.28873(9) 0.61302(9) 0.35028(7) 0.0130(2) Uani 1 1 d . . . C7 C 0.20778(9) 0.54352(9) 0.32883(7) 0.0150(2) Uani 1 1 d . . . C8 C 0.11051(10) 0.57842(10) 0.33128(8) 0.0200(2) Uani 1 1 d . . . H8 H 0.0552 0.5320 0.3190 0.024 Uiso 1 1 calc R . . C9 C 0.09280(10) 0.67890(11) 0.35116(8) 0.0211(3) Uani 1 1 d . . . H9 H 0.0257 0.7019 0.3499 0.025 Uiso 1 1 calc R . . C10 C 0.17341(10) 0.74551(10) 0.37287(8) 0.0188(2) Uani 1 1 d . . . H10 H 0.1611 0.8143 0.3869 0.023 Uiso 1 1 calc R . . C11 C 0.27262(9) 0.71382(9) 0.37469(7) 0.0155(2) Uani 1 1 d . . . C12 C 0.22113(9) 0.43396(9) 0.30223(7) 0.0160(2) Uani 1 1 d . . . H12 H 0.2905 0.4276 0.2907 0.019 Uiso 1 1 calc R . . C13 C 0.21289(11) 0.35939(10) 0.36835(8) 0.0228(3) Uani 1 1 d . . . H13A H 0.2634 0.3772 0.4155 0.034 Uiso 1 1 calc R . . H13B H 0.2250 0.2891 0.3520 0.034 Uiso 1 1 calc R . . H13C H 0.1450 0.3639 0.3801 0.034 Uiso 1 1 calc R . . C14 C 0.14385(11) 0.40362(11) 0.22771(8) 0.0231(3) Uani 1 1 d . . . H14A H 0.0758 0.4024 0.2394 0.035 Uiso 1 1 calc R . . H14B H 0.1605 0.3352 0.2102 0.035 Uiso 1 1 calc R . . H14C H 0.1459 0.4539 0.1860 0.035 Uiso 1 1 calc R . . C15 C 0.35870(10) 0.78983(10) 0.39969(8) 0.0198(2) Uani 1 1 d . . . H15 H 0.4229 0.7491 0.4116 0.024 Uiso 1 1 calc R . . C16 C 0.36765(18) 0.86378(16) 0.33466(11) 0.0535(6) Uani 1 1 d . . . H16A H 0.3826 0.8255 0.2897 0.080 Uiso 1 1 calc R . . H16B H 0.4224 0.9128 0.3536 0.080 Uiso 1 1 calc R . . H16C H 0.3038 0.9012 0.3183 0.080 Uiso 1 1 calc R . . C17 C 0.35085(13) 0.84813(13) 0.47425(10) 0.0349(4) Uani 1 1 d . . . H17A H 0.4095 0.8936 0.4892 0.052 Uiso 1 1 calc R . . H17B H 0.3493 0.7990 0.5169 0.052 Uiso 1 1 calc R . . H17C H 0.2887 0.8893 0.4647 0.052 Uiso 1 1 calc R . . C18 C 0.70781(9) 0.61895(9) 0.40866(7) 0.0127(2) Uani 1 1 d . . . C19 C 0.78971(9) 0.55091(9) 0.41135(7) 0.0147(2) Uani 1 1 d . . . C20 C 0.88698(9) 0.58637(10) 0.44374(8) 0.0190(2) Uani 1 1 d . . . H20 H 0.9429 0.5410 0.4471 0.023 Uiso 1 1 calc R . . C21 C 0.90373(10) 0.68637(10) 0.47105(8) 0.0199(2) Uani 1 1 d . . . H21 H 0.9705 0.7094 0.4921 0.024 Uiso 1 1 calc R . . C22 C 0.82269(9) 0.75231(10) 0.46747(7) 0.0176(2) Uani 1 1 d . . . H22 H 0.8345 0.8209 0.4861 0.021 Uiso 1 1 calc R . . C23 C 0.72375(9) 0.72013(9) 0.43696(7) 0.0146(2) Uani 1 1 d . A . C24 C 0.77695(9) 0.44210(9) 0.37893(7) 0.0158(2) Uani 1 1 d . . . H24 H 0.7081 0.4363 0.3445 0.019 Uiso 1 1 calc R . . C25 C 0.85569(11) 0.41451(11) 0.32958(8) 0.0233(3) Uani 1 1 d . . . H25A H 0.8563 0.4679 0.2898 0.035 Uiso 1 1 calc R . . H25B H 0.8382 0.3482 0.3035 0.035 Uiso 1 1 calc R . . H25C H 0.9228 0.4099 0.3640 0.035 Uiso 1 1 calc R . . C26 C 0.78363(10) 0.36565(10) 0.44669(8) 0.0212(3) Uani 1 1 d . . . H26A H 0.8507 0.3702 0.4812 0.032 Uiso 1 1 calc R . . H26B H 0.7729 0.2957 0.4255 0.032 Uiso 1 1 calc R . . H26C H 0.7317 0.3820 0.4768 0.032 Uiso 1 1 calc R . . C27 C 0.63860(10) 0.79743(9) 0.43344(8) 0.0185(2) Uani 1 1 d DU . . H27 H 0.5736 0.7636 0.4080 0.022 Uiso 0.841(8) 1 calc PR A 1 H27' H 0.5772 0.7538 0.4317 0.022 Uiso 0.159(8) 1 calc PR A 2 C28 C 0.6298(2) 0.8329(2) 0.51510(11) 0.0242(5) Uani 0.841(8) 1 d PDU A 1 H28A H 0.6125 0.7741 0.5452 0.036 Uiso 0.841(8) 1 calc PR A 1 H28B H 0.5767 0.8853 0.5107 0.036 Uiso 0.841(8) 1 calc PR A 1 H28C H 0.6945 0.8622 0.5421 0.036 Uiso 0.841(8) 1 calc PR A 1 C29 C 0.65534(19) 0.89221(16) 0.38313(12) 0.0284(6) Uani 0.841(8) 1 d PDU A 1 H29A H 0.7200 0.9249 0.4063 0.043 Uiso 0.841(8) 1 calc PR A 1 H29B H 0.6002 0.9416 0.3820 0.043 Uiso 0.841(8) 1 calc PR A 1 H29C H 0.6564 0.8699 0.3293 0.043 Uiso 0.841(8) 1 calc PR A 1 C28' C 0.6502(12) 0.8573(12) 0.5126(8) 0.032(4) Uiso 0.159(8) 1 d PDU A 2 H28D H 0.6698 0.8094 0.5566 0.049 Uiso 0.159(8) 1 calc PR A 2 H28E H 0.5856 0.8898 0.5157 0.049 Uiso 0.159(8) 1 calc PR A 2 H28F H 0.7023 0.9103 0.5151 0.049 Uiso 0.159(8) 1 calc PR A 2 C29' C 0.6134(11) 0.8599(10) 0.3654(6) 0.032(3) Uiso 0.159(8) 1 d PDU A 2 H29D H 0.5580 0.9064 0.3707 0.048 Uiso 0.159(8) 1 calc PR A 2 H29E H 0.5920 0.8161 0.3189 0.048 Uiso 0.159(8) 1 calc PR A 2 H29F H 0.6726 0.9004 0.3594 0.048 Uiso 0.159(8) 1 calc PR A 2 C91 C 1.0059(6) 0.9319(9) 0.5631(8) 0.025(2) Uani 0.50 1 d PDU B -1 C92 C 0.9292(10) 1.0101(11) 0.5448(9) 0.030(2) Uani 0.50 1 d PDU B -1 H92 H 0.8803 1.0166 0.5769 0.036 Uiso 0.50 1 calc PR B -1 C93 C 0.9249(12) 1.0760(10) 0.4816(10) 0.037(3) Uani 0.50 1 d PDU B -1 H93 H 0.8742 1.1278 0.4710 0.045 Uiso 0.50 1 calc PR B -1 C94 C 0.9917(9) 1.0665(12) 0.4359(10) 0.050(3) Uani 0.50 1 d PDU B -1 H94 H 0.9865 1.1117 0.3922 0.059 Uiso 0.50 1 calc PR B -1 C95 C 1.0654(12) 0.9977(12) 0.4474(10) 0.039(3) Uani 0.50 1 d PDU B -1 H95 H 1.1113 0.9946 0.4126 0.047 Uiso 0.50 1 calc PR B -1 C96 C 1.0755(10) 0.9308(11) 0.5098(10) 0.036(2) Uani 0.50 1 d PDU B -1 H96 H 1.1295 0.8825 0.5181 0.043 Uiso 0.50 1 calc PR B -1 C97 C 1.0089(3) 0.8624(3) 0.6275(2) 0.0382(8) Uani 0.50 1 d PDU B -1 H97A H 0.9771 0.8948 0.6674 0.057 Uiso 0.50 1 calc PR B -1 H97B H 1.0793 0.8455 0.6508 0.057 Uiso 0.50 1 calc PR B -1 H97C H 0.9721 0.7993 0.6085 0.057 Uiso 0.50 1 calc PR B -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 Ti 0.01155(9) 0.00878(9) 0.00855(9) 0.00091(7) 0.00226(6) 0.00026(7) Cl 0.02789(16) 0.01141(12) 0.02008(14) -0.00338(10) 0.00682(11) -0.00035(11) O 0.0099(4) 0.0213(4) 0.0106(3) 0.0029(3) 0.0016(3) -0.0004(3) N1 0.0113(4) 0.0110(4) 0.0114(4) 0.0007(3) 0.0018(3) -0.0004(3) N2 0.0112(4) 0.0115(4) 0.0119(4) 0.0010(3) 0.0027(3) 0.0005(3) C1 0.0186(6) 0.0246(6) 0.0160(5) 0.0035(5) 0.0077(4) -0.0019(5) C2 0.0158(5) 0.0100(5) 0.0129(5) 0.0013(4) 0.0051(4) 0.0002(4) C3 0.0178(5) 0.0134(5) 0.0096(5) 0.0002(4) 0.0030(4) -0.0005(4) C4 0.0159(5) 0.0101(5) 0.0116(5) 0.0011(4) 0.0014(4) -0.0003(4) C5 0.0185(6) 0.0220(6) 0.0135(5) 0.0039(4) -0.0006(4) 0.0013(5) C6 0.0121(5) 0.0143(5) 0.0127(5) 0.0024(4) 0.0027(4) 0.0022(4) C7 0.0141(5) 0.0151(5) 0.0154(5) 0.0022(4) 0.0024(4) 0.0004(4) C8 0.0144(6) 0.0207(6) 0.0249(6) 0.0006(5) 0.0041(5) -0.0014(5) C9 0.0145(6) 0.0233(6) 0.0260(6) 0.0013(5) 0.0055(5) 0.0046(5) C10 0.0188(6) 0.0156(5) 0.0229(6) 0.0010(5) 0.0062(5) 0.0045(5) C11 0.0157(5) 0.0134(5) 0.0177(5) 0.0018(4) 0.0044(4) 0.0012(4) C12 0.0151(5) 0.0148(5) 0.0172(5) 0.0001(4) 0.0009(4) -0.0011(4) C13 0.0294(7) 0.0168(6) 0.0210(6) 0.0028(5) 0.0025(5) -0.0020(5) C14 0.0229(7) 0.0223(6) 0.0213(6) -0.0021(5) -0.0022(5) -0.0013(5) C15 0.0166(6) 0.0139(5) 0.0301(6) -0.0025(5) 0.0078(5) 0.0000(4) C16 0.0773(15) 0.0506(11) 0.0313(9) 0.0061(8) 0.0082(9) -0.0425(11) C17 0.0382(9) 0.0345(8) 0.0333(8) -0.0121(7) 0.0103(7) -0.0159(7) C18 0.0112(5) 0.0141(5) 0.0126(5) 0.0015(4) 0.0020(4) -0.0017(4) C19 0.0144(5) 0.0144(5) 0.0157(5) 0.0006(4) 0.0038(4) 0.0004(4) C20 0.0135(5) 0.0199(6) 0.0232(6) -0.0007(5) 0.0030(4) 0.0012(4) C21 0.0134(5) 0.0225(6) 0.0231(6) -0.0018(5) 0.0018(5) -0.0038(5) C22 0.0167(6) 0.0155(5) 0.0203(6) -0.0010(4) 0.0029(4) -0.0037(4) C23 0.0147(5) 0.0132(5) 0.0158(5) 0.0014(4) 0.0026(4) -0.0003(4) C24 0.0144(5) 0.0145(5) 0.0189(5) -0.0010(4) 0.0040(4) 0.0010(4) C25 0.0221(6) 0.0218(6) 0.0281(7) -0.0042(5) 0.0102(5) 0.0012(5) C26 0.0232(6) 0.0165(6) 0.0241(6) 0.0027(5) 0.0051(5) 0.0018(5) C27 0.0152(6) 0.0133(5) 0.0252(6) -0.0012(4) 0.0003(5) 0.0007(4) C28 0.0256(11) 0.0221(10) 0.0273(9) 0.0019(7) 0.0113(7) 0.0061(9) C29 0.0328(12) 0.0210(9) 0.0314(10) 0.0111(7) 0.0061(8) 0.0064(8) C91 0.018(3) 0.017(4) 0.038(5) -0.011(3) 0.003(3) 0.001(3) C92 0.022(3) 0.021(3) 0.048(5) -0.012(3) 0.008(3) 0.004(2) C93 0.042(5) 0.014(3) 0.051(5) -0.002(3) -0.001(3) 0.003(3) C94 0.066(7) 0.034(6) 0.045(7) -0.017(5) 0.004(5) -0.020(5) C95 0.049(6) 0.029(4) 0.042(4) -0.013(3) 0.016(4) -0.010(4) C96 0.024(4) 0.038(6) 0.049(4) -0.020(4) 0.014(3) -0.003(3) C97 0.044(2) 0.0297(16) 0.0336(16) -0.0062(13) -0.0093(14) -0.0054(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O 1.8316(8) 3_666 ? Ti O 1.8589(8) . ? Ti N2 2.1127(10) . ? Ti N1 2.1253(10) . ? Ti Cl 2.2434(4) . ? Ti Ti 2.7900(5) 3_666 ? O Ti 1.8316(8) 3_666 ? N1 C2 1.3422(14) . ? N1 C18 1.4547(15) . ? N2 C4 1.3464(14) . ? N2 C6 1.4568(15) . ? C1 C2 1.5125(16) . ? C2 C3 1.3946(16) . ? C3 C4 1.3928(16) . ? C4 C5 1.5128(16) . ? C6 C11 1.4070(16) . ? C6 C7 1.4080(17) . ? C7 C8 1.3981(17) . ? C7 C12 1.5187(17) . ? C8 C9 1.3837(19) . ? C9 C10 1.3814(19) . ? C10 C11 1.3954(17) . ? C11 C15 1.5193(17) . ? C12 C13 1.5230(17) . ? C12 C14 1.5380(17) . ? C15 C16 1.506(2) . ? C15 C17 1.521(2) . ? C18 C23 1.4046(16) . ? C18 C19 1.4090(16) . ? C19 C20 1.3970(17) . ? C19 C24 1.5185(17) . ? C20 C21 1.3858(18) . ? C21 C22 1.3811(18) . ? C22 C23 1.3967(17) . ? C23 C27 1.5184(17) . ? C24 C26 1.5277(17) . ? C24 C25 1.5371(17) . ? C27 C29' 1.416(9) . ? C27 C28 1.517(2) . ? C27 C29 1.552(2) . ? C27 C28' 1.557(12) . ? C91 C97 1.431(14) . ? C91 C92 1.439(14) . ? C91 C96 1.446(15) . ? C92 C93 1.384(9) . ? C93 C94 1.322(16) . ? C94 C95 1.321(16) . ? C95 C96 1.374(10) . ? 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 O Ti O 81.78(4) 3_666 . ? O Ti N2 148.39(4) 3_666 . ? O Ti N2 88.78(4) . . ? O Ti N1 89.73(4) 3_666 . ? O Ti N1 153.56(4) . . ? N2 Ti N1 85.47(4) . . ? O Ti Cl 109.19(3) 3_666 . ? O Ti Cl 106.43(3) . . ? N2 Ti Cl 102.41(3) . . ? N1 Ti Cl 100.01(3) . . ? O Ti Ti 41.26(3) 3_666 3_666 ? O Ti Ti 40.52(3) . 3_666 ? N2 Ti Ti 123.02(3) . 3_666 ? N1 Ti Ti 126.41(3) . 3_666 ? Cl Ti Ti 113.846(14) . 3_666 ? Ti O Ti 98.22(4) 3_666 . ? C2 N1 C18 113.12(9) . . ? C2 N1 Ti 121.10(8) . . ? C18 N1 Ti 125.25(7) . . ? C4 N2 C6 112.71(9) . . ? C4 N2 Ti 120.99(8) . . ? C6 N2 Ti 125.65(7) . . ? N1 C2 C3 123.45(10) . . ? N1 C2 C1 121.48(11) . . ? C3 C2 C1 114.99(10) . . ? C4 C3 C2 127.17(10) . . ? N2 C4 C3 123.74(10) . . ? N2 C4 C5 121.04(10) . . ? C3 C4 C5 115.16(10) . . ? C11 C6 C7 121.16(11) . . ? C11 C6 N2 118.25(10) . . ? C7 C6 N2 120.19(10) . . ? C8 C7 C6 117.85(11) . . ? C8 C7 C12 118.93(11) . . ? C6 C7 C12 123.22(11) . . ? C9 C8 C7 121.65(12) . . ? C10 C9 C8 119.52(12) . . ? C9 C10 C11 121.36(12) . . ? C10 C11 C6 118.32(11) . . ? C10 C11 C15 119.30(11) . . ? C6 C11 C15 122.34(11) . . ? C7 C12 C13 109.64(10) . . ? C7 C12 C14 113.18(10) . . ? C13 C12 C14 109.20(11) . . ? C16 C15 C11 111.99(12) . . ? C16 C15 C17 110.45(13) . . ? C11 C15 C17 112.63(11) . . ? C23 C18 C19 120.83(11) . . ? C23 C18 N1 118.86(10) . . ? C19 C18 N1 119.94(10) . . ? C20 C19 C18 118.25(11) . . ? C20 C19 C24 118.84(11) . . ? C18 C19 C24 122.89(11) . . ? C21 C20 C19 121.41(12) . . ? C22 C21 C20 119.60(12) . . ? C21 C22 C23 121.26(12) . . ? C22 C23 C18 118.64(11) . . ? C22 C23 C27 118.35(11) . . ? C18 C23 C27 122.98(11) . . ? C19 C24 C26 109.64(10) . . ? C19 C24 C25 112.61(10) . . ? C26 C24 C25 109.75(10) . . ? C29' C27 C28 123.6(5) . . ? C29' C27 C23 117.7(5) . . ? C28 C27 C23 111.46(12) . . ? C29' C27 C29 27.7(6) . . ? C28 C27 C29 109.40(14) . . ? C23 C27 C29 110.59(12) . . ? C29' C27 C28' 114.4(7) . . ? C28 C27 C28' 15.9(6) . . ? C23 C27 C28' 110.8(6) . . ? C29 C27 C28' 95.7(6) . . ? C97 C91 C92 121.5(9) . . ? C97 C91 C96 125.1(8) . . ? C92 C91 C96 113.4(14) . . ? C93 C92 C91 121.6(13) . . ? C94 C93 C92 119.6(14) . . ? C95 C94 C93 124(2) . . ? C94 C95 C96 119.9(16) . . ? C95 C96 C91 121.6(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.598 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.056 ####################################################################### # # 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_goega _database_code_depnum_ccdc_archive 'CCDC 652773' _database_code_depnum_ccdc_archive 'CCDC 652773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H98 N4 O2 Ti2' _chemical_formula_weight 1171.36 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 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.7080(17) _cell_length_b 20.4316(18) _cell_length_c 9.0082(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.296(4) _cell_angle_gamma 90.00 _cell_volume 3229.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7150 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.80 _exptl_crystal_description tablet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.296 _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 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20806 _diffrn_reflns_av_R_equivalents 0.1551 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3406 _reflns_number_gt 2283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.1051P)^2^+10.0013P] 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 3406 _refine_ls_number_parameters 177 _refine_ls_number_restraints 141 _refine_ls_R_factor_all 0.1165 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2132 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.43348(5) 0.0000 0.53427(11) 0.0108(3) Uani 1 2 d S . . O O 0.5000 0.05967(16) 0.5000 0.0144(8) Uani 1 2 d S . . N N 0.34287(17) 0.07074(14) 0.4689(3) 0.0135(7) Uani 1 1 d U . . C1 C 0.4595(3) 0.0000 0.7797(6) 0.0192(12) Uani 1 2 d S . . H1A H 0.4748 -0.0441 0.8212 0.023 Uiso 0.50 1 calc PR . . H1B H 0.4146 0.0136 0.8041 0.023 Uiso 0.50 1 calc PR . . H1C H 0.5015 0.0306 0.8288 0.023 Uiso 0.50 1 calc PR . . C2 C 0.2797(2) 0.06116(18) 0.5039(4) 0.0157(8) Uani 1 1 d U . . C3 C 0.2557(3) 0.0000 0.5357(6) 0.0166(11) Uani 1 2 d SU . . H3 H 0.2183 0.0000 0.5852 0.020 Uiso 1 2 calc SR . . C4 C 0.2283(2) 0.1179(2) 0.5065(5) 0.0251(9) Uani 1 1 d U . . H4A H 0.2556 0.1481 0.5919 0.030 Uiso 1 1 calc R . . H4B H 0.1827 0.1014 0.5242 0.030 Uiso 1 1 calc R . . H4C H 0.2132 0.1410 0.4049 0.030 Uiso 1 1 calc R . . C11 C 0.3503(2) 0.13594(18) 0.4110(4) 0.0157(8) Uani 1 1 d U . . C12 C 0.3789(2) 0.18761(18) 0.5169(5) 0.0173(8) Uani 1 1 d U . . C13 C 0.3815(2) 0.24987(18) 0.4548(5) 0.0221(9) Uani 1 1 d U . . H13 H 0.4025 0.2852 0.5250 0.027 Uiso 1 1 calc R . . C14 C 0.3544(2) 0.2612(2) 0.2943(5) 0.0242(9) Uani 1 1 d U . . H14 H 0.3557 0.3041 0.2547 0.029 Uiso 1 1 calc R . . C15 C 0.3251(2) 0.20984(19) 0.1903(5) 0.0223(9) Uani 1 1 d U . . H15 H 0.3059 0.2180 0.0797 0.027 Uiso 1 1 calc R . . C16 C 0.3232(2) 0.14650(19) 0.2455(5) 0.0206(9) Uani 1 1 d U . . C17 C 0.4061(2) 0.17898(19) 0.6945(5) 0.0195(8) Uani 1 1 d U . . H17 H 0.3879 0.1354 0.7174 0.023 Uiso 1 1 calc R . . C18 C 0.3742(3) 0.2317(2) 0.7765(5) 0.0256(9) Uani 1 1 d U . . H18A H 0.3935 0.2242 0.8911 0.038 Uiso 1 1 calc R . . H18B H 0.3184 0.2295 0.7368 0.038 Uiso 1 1 calc R . . H18C H 0.3904 0.2750 0.7539 0.038 Uiso 1 1 calc R . . C19 C 0.4926(2) 0.1792(2) 0.7629(5) 0.0247(9) Uani 1 1 d U . . H19A H 0.5093 0.1736 0.8779 0.037 Uiso 1 1 calc R . . H19B H 0.5118 0.2209 0.7382 0.037 Uiso 1 1 calc R . . H19C H 0.5124 0.1432 0.7166 0.037 Uiso 1 1 calc R . . C20 C 0.2887(3) 0.0922(2) 0.1287(5) 0.0344(11) Uani 1 1 d U . . H20 H 0.3063 0.0497 0.1844 0.041 Uiso 1 1 calc R . . C21 C 0.2033(4) 0.0937(4) 0.0774(7) 0.082(3) Uani 1 1 d U . . H21A H 0.1819 0.0582 0.0017 0.123 Uiso 1 1 calc R . . H21B H 0.1845 0.1358 0.0270 0.123 Uiso 1 1 calc R . . H21C H 0.1878 0.0880 0.1699 0.123 Uiso 1 1 calc R . . C22 C 0.3133(3) 0.0939(3) -0.0146(6) 0.0479(14) Uani 1 1 d U . . H22A H 0.2891 0.0578 -0.0859 0.072 Uiso 1 1 calc R . . H22B H 0.3689 0.0893 0.0196 0.072 Uiso 1 1 calc R . . H22C H 0.2980 0.1356 -0.0701 0.072 Uiso 1 1 calc R . . C91 C -0.0051(7) 0.0335(5) 0.2502(13) 0.081(4) Uiso 0.50 1 d PGU A -1 C92 C 0.0427(6) -0.0076(7) 0.2042(12) 0.124(5) Uiso 0.50 1 d PGU A -1 H92 H 0.0791 0.0104 0.1639 0.149 Uiso 0.50 1 calc PR A -1 C93 C 0.0372(7) -0.0751(6) 0.2173(15) 0.143(9) Uiso 0.50 1 d PGU A -1 H93 H 0.0699 -0.1032 0.1859 0.172 Uiso 0.50 1 calc PR A -1 C94 C -0.0160(8) -0.1014(4) 0.2763(16) 0.086(5) Uiso 0.50 1 d PGU A -1 H94 H -0.0197 -0.1475 0.2853 0.103 Uiso 0.50 1 calc PR A -1 C95 C -0.0638(6) -0.0603(6) 0.3223(13) 0.129(7) Uiso 0.50 1 d PGU A -1 H95 H -0.1002 -0.0784 0.3626 0.155 Uiso 0.50 1 calc PR A -1 C96 C -0.0584(6) 0.0071(6) 0.3092(13) 0.129(5) Uiso 0.50 1 d PGU A -1 H96 H -0.0910 0.0352 0.3406 0.155 Uiso 0.50 1 calc PR A -1 C97 C 0.0033(14) 0.1076(12) 0.205(3) 0.124(7) Uiso 0.50 1 d PU 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 Ti 0.0156(5) 0.0086(5) 0.0107(5) 0.000 0.0076(4) 0.000 O 0.0201(19) 0.0066(17) 0.0202(19) 0.000 0.0116(16) 0.000 N 0.0162(16) 0.0100(15) 0.0153(16) 0.0012(12) 0.0068(13) -0.0012(12) C1 0.028(3) 0.014(3) 0.021(3) 0.000 0.015(2) 0.000 C2 0.0181(19) 0.0159(19) 0.0133(18) 0.0003(15) 0.0057(15) 0.0013(15) C3 0.020(3) 0.018(3) 0.017(3) 0.000 0.012(2) 0.000 C4 0.028(2) 0.017(2) 0.037(2) 0.0019(18) 0.020(2) 0.0037(17) C11 0.0161(19) 0.0121(18) 0.0214(19) 0.0049(14) 0.0096(16) 0.0032(14) C12 0.0186(19) 0.0127(18) 0.026(2) 0.0029(15) 0.0144(16) 0.0024(15) C13 0.034(2) 0.0101(19) 0.030(2) -0.0012(16) 0.0201(19) 0.0012(16) C14 0.033(2) 0.0143(19) 0.034(2) 0.0083(17) 0.022(2) 0.0071(17) C15 0.027(2) 0.024(2) 0.019(2) 0.0100(16) 0.0115(17) 0.0083(17) C16 0.025(2) 0.018(2) 0.0187(19) 0.0015(15) 0.0079(17) 0.0025(16) C17 0.026(2) 0.0138(19) 0.022(2) -0.0002(15) 0.0137(17) -0.0021(16) C18 0.033(2) 0.022(2) 0.028(2) 0.0005(18) 0.0178(19) 0.0032(18) C19 0.025(2) 0.027(2) 0.023(2) -0.0056(17) 0.0099(18) -0.0009(18) C20 0.054(3) 0.026(2) 0.017(2) 0.0063(17) 0.004(2) -0.009(2) C21 0.063(4) 0.140(7) 0.044(4) -0.031(4) 0.019(3) -0.064(4) C22 0.063(4) 0.045(3) 0.038(3) -0.015(2) 0.020(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O 1.843(2) 5_656 ? Ti O 1.843(2) . ? Ti C1 2.092(5) . ? Ti N 2.149(3) . ? Ti N 2.149(3) 6 ? Ti Ti 2.7643(18) 5_656 ? O Ti 1.843(2) 5_656 ? N C2 1.339(5) . ? N C11 1.455(5) . ? C2 C3 1.391(4) . ? C2 C4 1.512(5) . ? C3 C2 1.391(4) 6 ? C11 C12 1.399(5) . ? C11 C16 1.415(5) . ? C12 C13 1.397(5) . ? C12 C17 1.511(5) . ? C13 C14 1.376(6) . ? C14 C15 1.386(6) . ? C15 C16 1.391(5) . ? C16 C20 1.511(6) . ? C17 C19 1.519(6) . ? C17 C18 1.539(5) . ? C20 C21 1.502(8) . ? C20 C22 1.514(7) . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 C97 1.59(2) . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? 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 O Ti O 82.83(16) 5_656 . ? O Ti C1 104.69(12) 5_656 . ? O Ti C1 104.69(12) . . ? O Ti N 155.98(9) 5_656 . ? O Ti N 91.35(11) . . ? C1 Ti N 99.33(14) . . ? O Ti N 91.35(11) 5_656 6 ? O Ti N 155.98(9) . 6 ? C1 Ti N 99.33(14) . 6 ? N Ti N 84.54(16) . 6 ? O Ti Ti 41.42(8) 5_656 5_656 ? O Ti Ti 41.41(8) . 5_656 ? C1 Ti Ti 109.76(16) . 5_656 ? N Ti Ti 128.66(8) . 5_656 ? N Ti Ti 128.66(8) 6 5_656 ? Ti O Ti 97.17(16) 5_656 . ? C2 N C11 114.8(3) . . ? C2 N Ti 120.9(2) . . ? C11 N Ti 123.4(2) . . ? N C2 C3 123.7(4) . . ? N C2 C4 120.6(3) . . ? C3 C2 C4 115.7(3) . . ? C2 C3 C2 127.9(5) 6 . ? C12 C11 C16 121.1(3) . . ? C12 C11 N 120.5(3) . . ? C16 C11 N 118.3(3) . . ? C13 C12 C11 118.2(4) . . ? C13 C12 C17 119.0(3) . . ? C11 C12 C17 122.9(3) . . ? C14 C13 C12 121.5(4) . . ? C13 C14 C15 119.9(4) . . ? C14 C15 C16 121.0(4) . . ? C15 C16 C11 118.3(4) . . ? C15 C16 C20 119.5(4) . . ? C11 C16 C20 122.1(3) . . ? C12 C17 C19 110.4(3) . . ? C12 C17 C18 112.5(3) . . ? C19 C17 C18 109.8(3) . . ? C21 C20 C16 110.6(4) . . ? C21 C20 C22 110.0(4) . . ? C16 C20 C22 113.2(4) . . ? C92 C91 C96 120.0 . . ? C92 C91 C97 111.7(14) . . ? C96 C91 C97 127.9(14) . . ? C93 C92 C91 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C96 C95 C94 120.0 . . ? C95 C96 C91 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.939 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.113 ####################################################################### # # 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_niki _database_code_depnum_ccdc_archive 'CCDC 652774' _database_code_depnum_ccdc_archive 'CCDC 652774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H102 N4 O2 Ti2' _chemical_formula_weight 1079.32 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 Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9759(11) _cell_length_b 13.0850(16) _cell_length_c 13.5178(16) _cell_angle_alpha 88.349(4) _cell_angle_beta 79.207(4) _cell_angle_gamma 80.387(4) _cell_volume 1537.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5405 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 30.44 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 0.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7794 _exptl_absorpt_correction_T_max 0.9141 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32303 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9307 _reflns_number_gt 7219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0907P)^2^+1.0318P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9307 _refine_ls_number_parameters 330 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.55572(3) 0.09029(2) 0.51297(2) 0.01652(9) Uani 1 1 d . . . O O 0.47625(15) -0.01251(10) 0.59108(9) 0.0217(3) Uani 1 1 d . . . N1 N 0.54485(16) 0.22791(11) 0.42113(11) 0.0175(3) Uani 1 1 d . . . N2 N 0.49636(16) 0.19764(11) 0.63797(11) 0.0183(3) Uani 1 1 d . . . C1 C 0.7919(2) 0.05571(17) 0.50765(16) 0.0286(4) Uani 1 1 d . . . H1A H 0.8138 0.0022 0.5576 0.034 Uiso 1 1 calc R . . H1B H 0.8303 0.1183 0.5226 0.034 Uiso 1 1 calc R . . H1C H 0.8430 0.0303 0.4403 0.034 Uiso 1 1 calc R . . C2 C 0.6395(2) 0.39375(15) 0.37053(15) 0.0280(4) Uani 1 1 d . . . H2A H 0.7322 0.3664 0.3220 0.034 Uiso 1 1 calc R . . H2B H 0.6580 0.4537 0.4055 0.034 Uiso 1 1 calc R . . H2C H 0.5537 0.4150 0.3350 0.034 Uiso 1 1 calc R . . C3 C 0.6002(2) 0.31040(13) 0.44655(13) 0.0192(3) Uani 1 1 d . . . C4 C 0.6217(2) 0.32892(14) 0.54387(14) 0.0221(3) Uani 1 1 d . . . H4 H 0.6868 0.3779 0.5495 0.026 Uiso 1 1 calc R . . C5 C 0.5589(2) 0.28414(14) 0.63380(13) 0.0206(3) Uani 1 1 d . . . C6 C 0.5594(3) 0.34300(16) 0.72887(15) 0.0307(4) Uani 1 1 d . . . H6A H 0.4532 0.3662 0.7632 0.037 Uiso 1 1 calc R . . H6B H 0.6105 0.4033 0.7112 0.037 Uiso 1 1 calc R . . H6C H 0.6146 0.2975 0.7737 0.037 Uiso 1 1 calc R . . C11 C 0.4116(2) 0.17540(14) 0.73675(13) 0.0205(3) Uani 1 1 d . . . C12 C 0.4895(2) 0.12481(14) 0.80987(13) 0.0218(3) Uani 1 1 d . . . C13 C 0.4040(2) 0.11054(17) 0.90533(14) 0.0282(4) Uani 1 1 d . . . H13 H 0.4548 0.0753 0.9552 0.034 Uiso 1 1 calc R . . C14 C 0.2477(2) 0.14627(18) 0.92929(15) 0.0309(4) Uani 1 1 d . . . H14 H 0.1922 0.1363 0.9950 0.037 Uiso 1 1 calc R . . C15 C 0.1731(2) 0.19658(17) 0.85671(15) 0.0302(4) Uani 1 1 d . . . H15 H 0.0657 0.2211 0.8730 0.036 Uiso 1 1 calc R . . C16 C 0.2526(2) 0.21218(16) 0.75984(14) 0.0269(4) Uani 1 1 d . . . C17 C 0.6622(2) 0.08730(15) 0.78970(14) 0.0234(4) Uani 1 1 d . . . H17 H 0.7081 0.1202 0.7261 0.028 Uiso 1 1 calc R . . C18 C 0.7387(3) 0.11704(18) 0.87495(16) 0.0311(4) Uani 1 1 d . . . H18A H 0.7120 0.1920 0.8868 0.037 Uiso 1 1 calc R . . H18B H 0.8506 0.0979 0.8558 0.037 Uiso 1 1 calc R . . H18C H 0.7023 0.0802 0.9366 0.037 Uiso 1 1 calc R . . C19 C 0.6962(3) -0.02989(16) 0.77523(17) 0.0317(4) Uani 1 1 d . . . H19A H 0.6586 -0.0637 0.8385 0.038 Uiso 1 1 calc R . . H19B H 0.8074 -0.0523 0.7555 0.038 Uiso 1 1 calc R . . H19C H 0.6445 -0.0491 0.7224 0.038 Uiso 1 1 calc R . . C20 C 0.1664(3) 0.2719(2) 0.68403(18) 0.0425(6) Uani 1 1 d . . . H20 H 0.2391 0.2729 0.6183 0.051 Uiso 1 1 calc R . . C21 C 0.0327(4) 0.2242(3) 0.6675(3) 0.0770(12) Uani 1 1 d . . . H21A H 0.0695 0.1534 0.6418 0.092 Uiso 1 1 calc R . . H21B H -0.0194 0.2655 0.6186 0.092 Uiso 1 1 calc R . . H21C H -0.0393 0.2223 0.7315 0.092 Uiso 1 1 calc R . . C22 C 0.1077(6) 0.3855(3) 0.7207(4) 0.1003(16) Uani 1 1 d . . . H22A H 0.0823 0.4290 0.6639 0.120 Uiso 1 1 calc R . . H22B H 0.1880 0.4115 0.7480 0.120 Uiso 1 1 calc R . . H22C H 0.0157 0.3878 0.7732 0.120 Uiso 1 1 calc R . . C31 C 0.5067(2) 0.23295(13) 0.32132(13) 0.0198(3) Uani 1 1 d . . . C32 C 0.6223(2) 0.20690(15) 0.23601(14) 0.0239(4) Uani 1 1 d . . . C33 C 0.5821(3) 0.22018(18) 0.14108(15) 0.0322(4) Uani 1 1 d . . . H33 H 0.6586 0.2014 0.0829 0.039 Uiso 1 1 calc R . . C34 C 0.4337(3) 0.26004(18) 0.12956(15) 0.0337(5) Uani 1 1 d . . . H34 H 0.4093 0.2701 0.0642 0.040 Uiso 1 1 calc R . . C35 C 0.3206(2) 0.28520(16) 0.21415(16) 0.0291(4) Uani 1 1 d . . . H35 H 0.2188 0.3128 0.2061 0.035 Uiso 1 1 calc R . . C36 C 0.3538(2) 0.27070(14) 0.31077(14) 0.0220(3) Uani 1 1 d . . . C37 C 0.7886(2) 0.16578(16) 0.24254(15) 0.0266(4) Uani 1 1 d . . . H37 H 0.8028 0.1783 0.3125 0.032 Uiso 1 1 calc R . . C38 C 0.9025(3) 0.2204(2) 0.16920(18) 0.0387(5) Uani 1 1 d . . . H38A H 0.8969 0.2043 0.0998 0.046 Uiso 1 1 calc R . . H38B H 1.0071 0.1963 0.1810 0.046 Uiso 1 1 calc R . . H38C H 0.8762 0.2955 0.1800 0.046 Uiso 1 1 calc R . . C39 C 0.8245(3) 0.04927(19) 0.2233(2) 0.0397(5) Uani 1 1 d . . . H39A H 0.7510 0.0149 0.2698 0.048 Uiso 1 1 calc R . . H39B H 0.9290 0.0227 0.2338 0.048 Uiso 1 1 calc R . . H39C H 0.8165 0.0353 0.1538 0.048 Uiso 1 1 calc R . . C40 C 0.2274(2) 0.30004(17) 0.40166(16) 0.0284(4) Uani 1 1 d . . . H40 H 0.2583 0.2573 0.4593 0.034 Uiso 1 1 calc R . . C41 C 0.2129(4) 0.4125(2) 0.4312(3) 0.0641(9) Uani 1 1 d . . . H41A H 0.3096 0.4246 0.4488 0.077 Uiso 1 1 calc R . . H41B H 0.1294 0.4287 0.4894 0.077 Uiso 1 1 calc R . . H41C H 0.1902 0.4571 0.3746 0.077 Uiso 1 1 calc R . . C42 C 0.0717(3) 0.2757(3) 0.3893(2) 0.0574(8) Uani 1 1 d . . . H42A H -0.0011 0.2885 0.4531 0.069 Uiso 1 1 calc R . . H42B H 0.0828 0.2028 0.3699 0.069 Uiso 1 1 calc R . . H42C H 0.0333 0.3202 0.3368 0.069 Uiso 1 1 calc R . . C97 C 0.3728(15) 0.5254(12) 0.0180(12) 0.315(8) Uiso 1 1 d D . . H97A H 0.4575 0.5231 -0.0399 0.378 Uiso 1 1 calc R . . H97B H 0.3993 0.4705 0.0655 0.378 Uiso 1 1 calc R . . H97C H 0.3552 0.5930 0.0514 0.378 Uiso 1 1 calc R . . C98 C 0.2354(15) 0.5103(11) -0.0161(9) 0.243(5) Uiso 1 1 d D . . H98A H 0.2768 0.4457 -0.0552 0.291 Uiso 1 1 calc R . . H98B H 0.2333 0.5651 -0.0681 0.291 Uiso 1 1 calc R . . C99 C 0.0715(18) 0.5008(16) 0.0036(14) 0.319(9) Uiso 1 1 d D . . H99A H 0.0878 0.4306 0.0331 0.382 Uiso 1 1 calc R . . H99B H 0.0448 0.5467 0.0635 0.382 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 Ti 0.01744(15) 0.01604(15) 0.01646(15) -0.00019(11) -0.00311(10) -0.00383(10) O 0.0311(7) 0.0206(6) 0.0147(5) 0.0004(5) -0.0037(5) -0.0087(5) N1 0.0200(7) 0.0173(6) 0.0160(6) -0.0001(5) -0.0038(5) -0.0045(5) N2 0.0206(7) 0.0186(7) 0.0152(6) 0.0007(5) -0.0023(5) -0.0036(5) C1 0.0222(8) 0.0329(10) 0.0307(10) -0.0019(8) -0.0057(7) -0.0030(7) C2 0.0393(11) 0.0219(9) 0.0245(9) 0.0031(7) -0.0041(8) -0.0127(8) C3 0.0207(8) 0.0179(7) 0.0186(7) 0.0006(6) -0.0019(6) -0.0046(6) C4 0.0253(8) 0.0205(8) 0.0225(8) -0.0014(7) -0.0052(7) -0.0086(6) C5 0.0235(8) 0.0190(8) 0.0196(8) -0.0013(6) -0.0056(6) -0.0023(6) C6 0.0478(12) 0.0243(9) 0.0222(9) -0.0037(8) -0.0078(8) -0.0105(8) C11 0.0240(8) 0.0206(8) 0.0161(7) -0.0014(6) -0.0013(6) -0.0037(6) C12 0.0258(8) 0.0209(8) 0.0185(8) -0.0011(7) -0.0029(6) -0.0047(6) C13 0.0322(10) 0.0333(10) 0.0185(8) 0.0043(8) -0.0040(7) -0.0053(8) C14 0.0329(10) 0.0388(11) 0.0178(8) 0.0009(8) 0.0037(7) -0.0067(8) C15 0.0259(9) 0.0368(11) 0.0238(9) -0.0008(8) 0.0021(7) -0.0007(8) C16 0.0242(9) 0.0320(10) 0.0222(8) 0.0019(8) -0.0019(7) -0.0015(7) C17 0.0248(8) 0.0257(9) 0.0203(8) 0.0006(7) -0.0059(7) -0.0039(7) C18 0.0331(10) 0.0368(11) 0.0261(9) -0.0027(8) -0.0104(8) -0.0079(8) C19 0.0338(10) 0.0265(10) 0.0362(11) -0.0024(8) -0.0131(8) -0.0008(8) C20 0.0247(10) 0.0648(16) 0.0307(11) 0.0158(11) -0.0001(8) 0.0051(10) C21 0.077(2) 0.093(3) 0.080(2) 0.030(2) -0.056(2) -0.027(2) C22 0.118(4) 0.058(2) 0.128(4) 0.035(3) -0.057(3) 0.008(2) C31 0.0255(8) 0.0177(7) 0.0179(7) 0.0010(6) -0.0061(6) -0.0058(6) C32 0.0273(9) 0.0271(9) 0.0186(8) -0.0011(7) -0.0032(7) -0.0092(7) C33 0.0379(11) 0.0424(12) 0.0181(8) 0.0002(8) -0.0030(7) -0.0138(9) C34 0.0443(12) 0.0406(12) 0.0215(9) 0.0059(9) -0.0132(8) -0.0150(10) C35 0.0344(10) 0.0286(10) 0.0283(9) 0.0053(8) -0.0151(8) -0.0071(8) C36 0.0262(8) 0.0191(8) 0.0219(8) 0.0012(7) -0.0073(7) -0.0038(6) C37 0.0240(9) 0.0338(10) 0.0214(8) -0.0024(8) 0.0001(7) -0.0069(7) C38 0.0324(11) 0.0513(14) 0.0321(11) 0.0014(10) 0.0033(8) -0.0168(10) C39 0.0319(11) 0.0370(12) 0.0459(13) -0.0076(10) 0.0030(9) -0.0031(9) C40 0.0230(9) 0.0329(10) 0.0285(9) -0.0032(8) -0.0088(7) 0.0028(7) C41 0.0502(16) 0.0440(16) 0.089(3) -0.0266(16) 0.0050(16) 0.0014(13) C42 0.0362(13) 0.088(2) 0.0494(16) -0.0191(16) 0.0027(11) -0.0225(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O 1.8410(13) . ? Ti O 1.8514(13) 2_656 ? Ti C1 2.0808(19) . ? Ti N1 2.1568(14) . ? Ti N2 2.1591(15) . ? Ti Ti 2.7703(7) 2_656 ? O Ti 1.8514(13) 2_656 ? N1 C3 1.339(2) . ? N1 C31 1.450(2) . ? N2 C5 1.340(2) . ? N2 C11 1.455(2) . ? C2 C3 1.516(2) . ? C3 C4 1.398(2) . ? C4 C5 1.397(2) . ? C5 C6 1.518(3) . ? C11 C12 1.403(2) . ? C11 C16 1.407(3) . ? C12 C13 1.397(3) . ? C12 C17 1.522(3) . ? C13 C14 1.383(3) . ? C14 C15 1.380(3) . ? C15 C16 1.396(3) . ? C16 C20 1.519(3) . ? C17 C19 1.524(3) . ? C17 C18 1.537(3) . ? C20 C21 1.496(4) . ? C20 C22 1.554(5) . ? C31 C32 1.407(3) . ? C31 C36 1.411(3) . ? C32 C33 1.395(3) . ? C32 C37 1.518(3) . ? C33 C34 1.383(3) . ? C34 C35 1.386(3) . ? C35 C36 1.394(3) . ? C36 C40 1.518(3) . ? C37 C39 1.524(3) . ? C37 C38 1.537(3) . ? C40 C41 1.514(4) . ? C40 C42 1.524(3) . ? C97 C98 1.439(12) . ? C98 C99 1.471(12) . ? C99 C99 1.31(3) 2_565 ? 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 O Ti O 82.77(6) . 2_656 ? O Ti C1 104.89(7) . . ? O Ti C1 103.81(7) 2_656 . ? O Ti N1 155.27(6) . . ? O Ti N1 91.04(6) 2_656 . ? C1 Ti N1 99.83(7) . . ? O Ti N2 91.83(6) . . ? O Ti N2 157.27(6) 2_656 . ? C1 Ti N2 98.91(7) . . ? N1 Ti N2 84.69(6) . . ? O Ti Ti 41.53(4) . 2_656 ? O Ti Ti 41.25(4) 2_656 2_656 ? C1 Ti Ti 109.29(6) . 2_656 ? N1 Ti Ti 128.01(4) . 2_656 ? N2 Ti Ti 129.61(4) . 2_656 ? Ti O Ti 97.23(6) . 2_656 ? C3 N1 C31 114.58(14) . . ? C3 N1 Ti 120.31(11) . . ? C31 N1 Ti 124.14(11) . . ? C5 N2 C11 114.55(15) . . ? C5 N2 Ti 120.36(12) . . ? C11 N2 Ti 124.20(11) . . ? N1 C3 C4 123.81(15) . . ? N1 C3 C2 121.45(16) . . ? C4 C3 C2 114.71(16) . . ? C5 C4 C3 127.85(16) . . ? N2 C5 C4 123.56(16) . . ? N2 C5 C6 121.07(16) . . ? C4 C5 C6 115.31(16) . . ? C12 C11 C16 120.74(16) . . ? C12 C11 N2 120.33(16) . . ? C16 C11 N2 118.76(16) . . ? C13 C12 C11 118.09(17) . . ? C13 C12 C17 119.22(16) . . ? C11 C12 C17 122.67(16) . . ? C14 C13 C12 121.89(18) . . ? C15 C14 C13 119.25(17) . . ? C14 C15 C16 121.28(19) . . ? C15 C16 C11 118.73(18) . . ? C15 C16 C20 119.18(18) . . ? C11 C16 C20 122.04(17) . . ? C12 C17 C19 110.17(16) . . ? C12 C17 C18 112.22(16) . . ? C19 C17 C18 109.48(16) . . ? C21 C20 C16 112.4(2) . . ? C21 C20 C22 109.0(3) . . ? C16 C20 C22 109.8(3) . . ? C32 C31 C36 120.62(16) . . ? C32 C31 N1 120.37(16) . . ? C36 C31 N1 118.89(16) . . ? C33 C32 C31 118.35(18) . . ? C33 C32 C37 118.60(17) . . ? C31 C32 C37 123.04(16) . . ? C34 C33 C32 121.62(19) . . ? C33 C34 C35 119.49(18) . . ? C34 C35 C36 121.16(19) . . ? C35 C36 C31 118.70(18) . . ? C35 C36 C40 119.71(17) . . ? C31 C36 C40 121.54(16) . . ? C32 C37 C39 110.29(17) . . ? C32 C37 C38 112.62(18) . . ? C39 C37 C38 109.83(18) . . ? C41 C40 C36 111.9(2) . . ? C41 C40 C42 110.3(2) . . ? C36 C40 C42 113.68(19) . . ? C97 C98 C99 151.3(15) . . ? C99 C99 C98 165(3) 2_565 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.151 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.079 #============================================================================= # end of cif data for "niki" (compound 9b) #============================================================================= #============================================================================= # end of cif file #=============================================================================