Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'M Bochmann' _publ_contact_author_address ; School of Chemical Sciences and Pharmacy University of East Anglia Norwich Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email M.BOCHMANN@UEA.AC.UK _publ_section_title ; Titanium, Zinc and Alkaline-Earth Metal Complexes Supported by Bulky O,N,N,O-Multidentate Ligands: Syntheses, Characterisation and Activity in Cyclic Ester Polymerisation ; loop_ _publ_author_name Y.Sarazin M.Bochmann R.H.Howard D.L.Hughes S.M.Humphrey #===END data_yanns3 _database_code_depnum_ccdc_archive 'CCDC 243644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 7' _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Ca F10 N2 O4, 2/3(C7 H8)' _chemical_formula_structural '[Ca(thf)2{OC6H3tBu-6-(CHNC6F5)-2}2].toluene' _chemical_formula_sum 'C46.67 H47.33 Ca F10 N2 O4' _chemical_formula_weight 930.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' #(no.148, hexagonal axes) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 28.728(4) _cell_length_b 28.728(4) _cell_length_c 13.871(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9914(3) _cell_formula_units_Z 9 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square prisms' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4350 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis-IIc' _diffrn_measurement_method 'image-plate oscillation photos' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18625 _diffrn_reflns_av_R_equivalents 0.1388 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.40 _reflns_number_total 4044 _reflns_number_gt 2177 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC R-Axis-II control software' _computing_cell_refinement 'DENZO/CELL (Otwinowski and Minor, 1985)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski and Minor, 1985)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _refine_special_details ; 1) There is disorder in the THF ligand, where one CH2 group is distributed equally over two sites; this was satisfactorily resolved and refined. A toluene solvent molecule is disordered about a three-fold symmetry axis; this has not been fully resolved, but seven carbon atoms, with site occupancies in the range of 0.16 to 0.45, were refined isotropically. There is (approximately) one-third of a toluene molecule in the asymmetric unit, i.e. two-thirds of a toluene molecule per Ca-complex molecule. 2) 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 'w = [\s^2^(Fo^2^)+(0.0686P)^2^]-1 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 4044 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 Ca Ca 0.5000 0.0000 0.5000 0.0384(2) Uani 1 2 d S . . O1 O 0.52801(8) 0.04597(8) 0.36298(12) 0.0386(5) Uani 1 1 d . . . C11 C 0.53664(11) 0.08948(11) 0.32180(19) 0.0355(7) Uani 1 1 d . . . C12 C 0.53375(11) 0.13078(11) 0.37492(19) 0.0378(7) Uani 1 1 d . . . C13 C 0.53976(13) 0.17684(12) 0.3288(2) 0.0469(8) Uani 1 1 d . . . H13 H 0.5370 0.2028 0.3642 0.056 Uiso 1 1 calc R . . C14 C 0.54962(13) 0.18383(13) 0.2324(2) 0.0498(8) Uani 1 1 d . . . H14 H 0.5523 0.2138 0.2016 0.060 Uiso 1 1 calc R . . C15 C 0.55564(12) 0.14572(12) 0.1804(2) 0.0448(8) Uani 1 1 d . . . H15 H 0.5636 0.1518 0.1151 0.054 Uiso 1 1 calc R . . C16 C 0.55033(11) 0.09944(11) 0.22090(18) 0.0357(7) Uani 1 1 d . . . C161 C 0.55904(11) 0.05974(12) 0.16241(19) 0.0394(7) Uani 1 1 d . . . C162 C 0.60333(12) 0.05232(13) 0.2073(2) 0.0458(8) Uani 1 1 d . . . H16A H 0.6083 0.0271 0.1697 0.069 Uiso 1 1 calc R . . H16B H 0.5934 0.0390 0.2719 0.069 Uiso 1 1 calc R . . H16C H 0.6362 0.0862 0.2086 0.069 Uiso 1 1 calc R . . C163 C 0.57648(14) 0.07931(13) 0.0586(2) 0.0523(8) Uani 1 1 d . . . H16D H 0.5815 0.0533 0.0239 0.079 Uiso 1 1 calc R . . H16E H 0.6096 0.1130 0.0596 0.079 Uiso 1 1 calc R . . H16F H 0.5492 0.0839 0.0274 0.079 Uiso 1 1 calc R . . C164 C 0.50736(12) 0.00544(12) 0.1560(2) 0.0470(8) Uani 1 1 d . . . H16G H 0.5138 -0.0190 0.1189 0.070 Uiso 1 1 calc R . . H16H H 0.4799 0.0099 0.1254 0.070 Uiso 1 1 calc R . . H16I H 0.4959 -0.0088 0.2197 0.070 Uiso 1 1 calc R . . C120 C 0.52675(11) 0.12974(12) 0.4768(2) 0.0421(7) Uani 1 1 d . . . H120 H 0.5296 0.1608 0.5036 0.051 Uiso 1 1 calc R . . N2 N 0.51696(9) 0.09163(10) 0.53702(15) 0.0404(6) Uani 1 1 d . . . C21 C 0.51632(12) 0.10523(12) 0.63563(19) 0.0414(7) Uani 1 1 d . . . C22 C 0.56289(13) 0.13486(15) 0.6865(2) 0.0584(9) Uani 1 1 d . . . F22 F 0.61028(8) 0.15286(11) 0.64293(15) 0.0952(8) Uani 1 1 d . . . C23 C 0.56241(15) 0.14624(16) 0.7833(2) 0.0627(10) Uani 1 1 d . . . F23 F 0.60846(9) 0.17443(11) 0.83105(15) 0.1022(9) Uani 1 1 d . . . C24 C 0.51456(15) 0.12937(14) 0.8285(2) 0.0520(9) Uani 1 1 d . . . F24 F 0.51375(9) 0.14062(8) 0.92228(12) 0.0701(6) Uani 1 1 d . . . C25 C 0.46813(14) 0.10045(13) 0.7794(2) 0.0482(8) Uani 1 1 d . . . F25 F 0.42084(8) 0.08399(8) 0.82387(13) 0.0714(6) Uani 1 1 d . . . C26 C 0.46911(13) 0.08800(12) 0.6842(2) 0.0428(7) Uani 1 1 d . . . F26 F 0.42238(7) 0.05809(7) 0.63748(12) 0.0562(5) Uani 1 1 d . . . O3 O 0.58864(8) 0.03178(9) 0.54928(15) 0.0550(6) Uani 1 1 d . B . C31 C 0.60623(13) 0.01364(15) 0.6298(2) 0.0623(10) Uani 1 1 d . B . H31A H 0.5873 -0.0253 0.6320 0.075 Uiso 1 1 calc R . . H31B H 0.5996 0.0269 0.6895 0.075 Uiso 1 1 calc R . . C32 C 0.66443(14) 0.03509(17) 0.6162(3) 0.0721(11) Uani 1 1 d . . . H32A H 0.6728 0.0063 0.6151 0.086 Uiso 0.50 1 calc PR A 1 H32B H 0.6849 0.0601 0.6672 0.086 Uiso 0.50 1 calc PR A 1 H32C H 0.6829 0.0421 0.6776 0.086 Uiso 0.50 1 calc PR A 2 H32D H 0.6712 0.0105 0.5792 0.086 Uiso 0.50 1 calc PR A 2 C33A C 0.6764(4) 0.0637(5) 0.5182(8) 0.089(3) Uani 0.50 1 d P B 1 H33A H 0.7095 0.0980 0.5216 0.107 Uiso 0.50 1 calc PR B 1 H33B H 0.6804 0.0420 0.4690 0.107 Uiso 0.50 1 calc PR B 1 C33B C 0.6807(4) 0.0838(4) 0.5645(7) 0.062(3) Uani 0.50 1 d P B 2 H33C H 0.7136 0.0944 0.5291 0.074 Uiso 0.50 1 calc PR B 2 H33D H 0.6865 0.1125 0.6082 0.074 Uiso 0.50 1 calc PR B 2 C34 C 0.63500(13) 0.07119(16) 0.4965(3) 0.0679(11) Uani 1 1 d . . . H34A H 0.6279 0.0668 0.4278 0.081 Uiso 0.50 1 calc PR B 1 H34B H 0.6434 0.1072 0.5146 0.081 Uiso 0.50 1 calc PR B 1 H34C H 0.6324 0.1030 0.4830 0.081 Uiso 0.50 1 calc PR B 2 H34D H 0.6392 0.0565 0.4363 0.081 Uiso 0.50 1 calc PR B 2 C51 C 0.9982(8) 0.0447(8) 0.2312(14) 0.142(6) Uiso 0.35 1 d P . . C52 C 1.0248(9) 0.0599(8) 0.3424(14) 0.142(7) Uiso 0.37 1 d P . . C53 C 0.9992(8) 0.0614(8) 0.3090(14) 0.156(6) Uiso 0.45 1 d P . . C54 C 0.993(3) 0.010(3) 0.3005(15) 0.156(12) Uiso 0.28 1 d P . . C55 C 0.978(2) 0.020(2) 0.363(3) 0.162(16) Uiso 0.17 1 d P . . C56 C 1.0000 0.0000 0.1754(17) 0.145(7) Uiso 0.57 3 d SP . . C57 C 1.0000 0.0000 0.0833(19) 0.165(9) Uiso 0.48 3 d SP . . 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 Ca 0.0354(5) 0.0458(5) 0.0308(4) 0.0052(4) 0.0006(4) 0.0180(4) O1 0.0456(12) 0.0411(12) 0.0307(10) 0.0047(9) 0.0029(9) 0.0228(10) C11 0.0324(16) 0.0393(17) 0.0346(16) 0.0013(14) -0.0033(13) 0.0178(14) C12 0.0394(17) 0.0412(17) 0.0325(15) -0.0007(13) -0.0009(13) 0.0197(14) C13 0.060(2) 0.0457(19) 0.0423(18) -0.0017(15) 0.0028(15) 0.0317(17) C14 0.067(2) 0.0450(19) 0.0416(18) 0.0066(15) -0.0018(16) 0.0308(17) C15 0.054(2) 0.0475(19) 0.0331(16) 0.0018(14) -0.0021(14) 0.0256(16) C16 0.0367(16) 0.0403(17) 0.0291(15) -0.0003(13) -0.0019(13) 0.0184(14) C161 0.0468(18) 0.0459(18) 0.0287(15) 0.0027(13) -0.0005(13) 0.0255(15) C162 0.0510(19) 0.055(2) 0.0374(16) 0.0052(15) 0.0030(14) 0.0310(17) C163 0.069(2) 0.065(2) 0.0305(16) 0.0012(15) 0.0016(15) 0.0390(19) C164 0.052(2) 0.0492(19) 0.0433(17) -0.0074(15) -0.0085(15) 0.0279(17) C120 0.0447(18) 0.0460(18) 0.0397(17) -0.0034(15) -0.0016(14) 0.0257(15) N2 0.0423(15) 0.0491(15) 0.0313(13) -0.0011(12) 0.0012(11) 0.0240(13) C21 0.0495(19) 0.0516(19) 0.0294(15) 0.0000(14) 0.0021(14) 0.0299(16) C22 0.045(2) 0.092(3) 0.0411(18) -0.0164(18) -0.0045(16) 0.0354(19) F22 0.0441(12) 0.163(2) 0.0609(13) -0.0430(14) -0.0077(10) 0.0385(14) C23 0.064(2) 0.091(3) 0.0435(19) -0.0217(19) -0.0189(19) 0.047(2) F23 0.0792(16) 0.173(3) 0.0594(14) -0.0513(16) -0.0306(12) 0.0665(17) C24 0.080(3) 0.068(2) 0.0279(17) -0.0036(16) 0.0001(17) 0.052(2) F24 0.1133(17) 0.0895(15) 0.0319(10) -0.0053(10) 0.0000(10) 0.0690(14) C25 0.062(2) 0.055(2) 0.0383(17) 0.0054(16) 0.0142(17) 0.0371(18) F25 0.0769(14) 0.0823(15) 0.0550(12) 0.0011(10) 0.0270(11) 0.0398(12) C26 0.049(2) 0.0474(18) 0.0378(17) 0.0008(15) 0.0012(15) 0.0289(17) F26 0.0455(11) 0.0643(12) 0.0509(11) -0.0003(9) 0.0068(9) 0.0216(10) O3 0.0339(12) 0.0679(15) 0.0527(13) 0.0197(11) -0.0019(10) 0.0176(11) C31 0.053(2) 0.072(2) 0.064(2) 0.0168(19) -0.0092(18) 0.0324(19) C32 0.059(2) 0.088(3) 0.076(3) -0.015(2) -0.019(2) 0.042(2) C33A 0.048(6) 0.130(11) 0.085(9) 0.024(7) 0.018(6) 0.043(7) C33B 0.028(4) 0.064(6) 0.069(7) -0.024(5) -0.002(4) 0.004(4) C34 0.038(2) 0.083(3) 0.059(2) 0.012(2) 0.0015(18) 0.013(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 Ca O1 2.2229(18) . ? Ca O1 2.2229(18) 10_656 ? Ca O3 2.3369(19) . ? Ca O3 2.3369(19) 10_656 ? Ca N2 2.479(2) . ? Ca N2 2.479(2) 10_656 ? O1 C11 1.281(3) . ? C11 C12 1.434(4) . ? C11 C16 1.443(4) . ? C12 C13 1.401(4) . ? C12 C120 1.426(4) . ? C13 C14 1.360(4) . ? C13 H13 0.9300 . ? C14 C15 1.392(4) . ? C14 H14 0.9300 . ? C15 C16 1.380(4) . ? C15 H15 0.9300 . ? C16 C161 1.519(4) . ? C161 C162 1.524(4) . ? C161 C164 1.526(4) . ? C161 C163 1.536(4) . ? C162 H16A 0.9600 . ? C162 H16B 0.9600 . ? C162 H16C 0.9600 . ? C163 H16D 0.9600 . ? C163 H16E 0.9600 . ? C163 H16F 0.9600 . ? C164 H16G 0.9600 . ? C164 H16H 0.9600 . ? C164 H16I 0.9600 . ? C120 N2 1.291(4) . ? C120 H120 0.9300 . ? N2 C21 1.425(3) . ? C21 C26 1.366(4) . ? C21 C22 1.369(4) . ? C22 F22 1.335(4) . ? C22 C23 1.383(4) . ? C23 F23 1.332(4) . ? C23 C24 1.361(5) . ? C24 F24 1.344(3) . ? C24 C25 1.351(4) . ? C25 F25 1.345(3) . ? C25 C26 1.372(4) . ? C26 F26 1.344(3) . ? O3 C31 1.427(3) . ? O3 C34 1.443(4) . ? C31 C32 1.477(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33B 1.426(12) . ? C32 C33A 1.536(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C32 H32D 0.9700 . ? C33A C34 1.344(12) . ? C33A H33A 0.9700 . ? C33A H33B 0.9700 . ? C33B C34 1.506(11) . ? C33B H33C 0.9700 . ? C33B H33D 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C34 H34D 0.9700 . ? C51 C53 1.18(2) . ? C51 C54 1.33(4) . ? C51 C56 1.52(2) . ? C51 C52 1.68(3) . ? C51 C54 1.73(7) 3_765 ? C51 C54 1.93(4) 2_645 ? C51 C55 1.94(5) . ? C52 C53 0.89(3) . ? C52 C55 1.29(6) . ? C52 C54 1.38(7) . ? C52 C55 1.43(5) 3_765 ? C52 C54 1.54(8) 3_765 ? C52 C54 2.01(4) 2_645 ? C53 C55 1.27(5) . ? C53 C54 1.39(5) . ? C53 C54 1.88(8) 3_765 ? C54 C54 0.75(6) 3_765 ? C54 C54 0.75(6) 2_645 ? C54 C55 1.06(4) . ? C54 C55 1.54(8) 3_765 ? C54 C52 1.54(8) 2_645 ? C54 C55 1.61(6) 2_645 ? C54 C51 1.73(7) 2_645 ? C54 C56 1.79(3) . ? C54 C53 1.88(8) 2_645 ? C55 C52 1.43(5) 2_645 ? C55 C54 1.54(8) 2_645 ? C55 C54 1.61(6) 3_765 ? C55 C55 1.81(8) 3_765 ? C55 C55 1.81(8) 2_645 ? C56 C57 1.28(3) . ? C56 C51 1.52(2) 3_765 ? C56 C51 1.52(2) 2_645 ? C56 C54 1.79(3) 3_765 ? C56 C54 1.79(3) 2_645 ? 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 Ca O1 180.0 . 10_656 ? O1 Ca O3 91.02(7) . . ? O1 Ca O3 88.98(7) 10_656 . ? O1 Ca O3 88.98(7) . 10_656 ? O1 Ca O3 91.02(7) 10_656 10_656 ? O3 Ca O3 180.0 . 10_656 ? O1 Ca N2 74.08(7) . . ? O1 Ca N2 105.91(7) 10_656 . ? O3 Ca N2 85.83(8) . . ? O3 Ca N2 94.17(8) 10_656 . ? O1 Ca N2 105.92(7) . 10_656 ? O1 Ca N2 74.09(7) 10_656 10_656 ? O3 Ca N2 94.17(8) . 10_656 ? O3 Ca N2 85.83(8) 10_656 10_656 ? N2 Ca N2 180.0 . 10_656 ? C11 O1 Ca 142.85(18) . . ? O1 C11 C12 121.0(2) . . ? O1 C11 C16 121.8(3) . . ? C12 C11 C16 117.2(2) . . ? C13 C12 C120 115.0(3) . . ? C13 C12 C11 121.1(3) . . ? C120 C12 C11 123.9(3) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 123.3(3) . . ? C16 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C15 C16 C11 118.3(3) . . ? C15 C16 C161 121.7(2) . . ? C11 C16 C161 120.0(2) . . ? C16 C161 C162 110.4(2) . . ? C16 C161 C164 110.9(2) . . ? C162 C161 C164 109.5(2) . . ? C16 C161 C163 111.8(2) . . ? C162 C161 C163 107.0(2) . . ? C164 C161 C163 107.0(2) . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C161 C164 H16G 109.5 . . ? C161 C164 H16H 109.5 . . ? H16G C164 H16H 109.5 . . ? C161 C164 H16I 109.5 . . ? H16G C164 H16I 109.5 . . ? H16H C164 H16I 109.5 . . ? N2 C120 C12 128.9(3) . . ? N2 C120 H120 115.6 . . ? C12 C120 H120 115.6 . . ? C120 N2 C21 114.5(2) . . ? C120 N2 Ca 127.60(19) . . ? C21 N2 Ca 117.86(18) . . ? C26 C21 C22 117.1(3) . . ? C26 C21 N2 121.4(3) . . ? C22 C21 N2 121.5(3) . . ? F22 C22 C21 119.8(3) . . ? F22 C22 C23 118.5(3) . . ? C21 C22 C23 121.7(3) . . ? F23 C23 C24 120.5(3) . . ? F23 C23 C22 120.1(3) . . ? C24 C23 C22 119.4(3) . . ? F24 C24 C25 120.4(3) . . ? F24 C24 C23 119.8(3) . . ? C25 C24 C23 119.9(3) . . ? F25 C25 C24 119.9(3) . . ? F25 C25 C26 119.9(3) . . ? C24 C25 C26 120.2(3) . . ? F26 C26 C21 119.2(3) . . ? F26 C26 C25 119.1(3) . . ? C21 C26 C25 121.7(3) . . ? C31 O3 C34 109.1(2) . . ? C31 O3 Ca 126.99(18) . . ? C34 O3 Ca 123.78(18) . . ? O3 C31 C32 106.3(3) . . ? O3 C31 H31A 110.5 . . ? C32 C31 H31A 110.5 . . ? O3 C31 H31B 110.5 . . ? C32 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? C33B C32 C31 102.7(5) . . ? C33B C32 C33A 32.3(5) . . ? C31 C32 C33A 103.9(5) . . ? C33B C32 H32A 136.8 . . ? C31 C32 H32A 111.0 . . ? C33A C32 H32A 111.0 . . ? C33B C32 H32B 82.0 . . ? C31 C32 H32B 111.0 . . ? C33A C32 H32B 111.0 . . ? H32A C32 H32B 109.0 . . ? C33B C32 H32C 111.2 . . ? C31 C32 H32C 111.2 . . ? C33A C32 H32C 135.5 . . ? H32A C32 H32C 81.2 . . ? H32B C32 H32C 30.6 . . ? C33B C32 H32D 111.2 . . ? C31 C32 H32D 111.2 . . ? C33A C32 H32D 81.3 . . ? H32A C32 H32D 31.1 . . ? H32B C32 H32D 131.1 . . ? H32C C32 H32D 109.1 . . ? C34 C33A C32 107.7(7) . . ? C34 C33A H33A 110.2 . . ? C32 C33A H33A 110.2 . . ? C34 C33A H33B 110.2 . . ? C32 C33A H33B 110.2 . . ? H33A C33A H33B 108.5 . . ? C32 C33B C34 105.1(6) . . ? C32 C33B H33C 110.7 . . ? C34 C33B H33C 110.7 . . ? C32 C33B H33D 110.7 . . ? C34 C33B H33D 110.7 . . ? H33C C33B H33D 108.8 . . ? C33A C34 O3 107.7(6) . . ? C33A C34 C33B 33.2(5) . . ? O3 C34 C33B 102.8(5) . . ? C33A C34 H34A 110.2 . . ? O3 C34 H34A 110.2 . . ? C33B C34 H34A 138.4 . . ? C33A C34 H34B 110.2 . . ? O3 C34 H34B 110.2 . . ? C33B C34 H34B 82.0 . . ? H34A C34 H34B 108.5 . . ? C33A C34 H34C 133.1 . . ? O3 C34 H34C 111.2 . . ? C33B C34 H34C 111.2 . . ? H34A C34 H34C 79.8 . . ? H34B C34 H34C 30.9 . . ? C33A C34 H34D 79.2 . . ? O3 C34 H34D 111.2 . . ? C33B C34 H34D 111.2 . . ? H34A C34 H34D 32.9 . . ? H34B C34 H34D 131.9 . . ? H34C C34 H34D 109.1 . . ? C53 C51 C54 67(2) . . ? C53 C51 C56 144(2) . . ? C54 C51 C56 77.3(19) . . ? C53 C51 C52 30.2(13) . . ? C54 C51 C52 53(3) . . ? C56 C51 C52 118.9(18) . . ? C53 C51 C54 78(2) . 3_765 ? C54 C51 C54 24(3) . 3_765 ? C56 C51 C54 66(2) . 3_765 ? C52 C51 C54 53.6(19) . 3_765 ? C53 C51 C54 83.4(17) . 2_645 ? C54 C51 C54 16.4(15) . 2_645 ? C56 C51 C54 61.1(16) . 2_645 ? C52 C51 C54 67.3(11) . 2_645 ? C54 C51 C54 22.9(17) 3_765 2_645 ? C53 C51 C55 39.5(18) . . ? C54 C51 C55 31(2) . . ? C56 C51 C55 107(2) . . ? C52 C51 C55 41.0(16) . . ? C54 C51 C55 51.7(15) 3_765 . ? C54 C51 C55 47(2) 2_645 . ? C53 C52 C55 69(3) . . ? C53 C52 C54 72(2) . . ? C55 C52 C54 47(2) . . ? C53 C52 C55 139(4) . 3_765 ? C55 C52 C55 83(4) . 3_765 ? C54 C52 C55 66(3) . 3_765 ? C53 C52 C54 98(3) . 3_765 ? C55 C52 C54 69(3) . 3_765 ? C54 C52 C54 29(3) . 3_765 ? C55 C52 C54 42(2) 3_765 3_765 ? C53 C52 C51 41.7(18) . . ? C55 C52 C51 80(3) . . ? C54 C52 C51 50.4(15) . . ? C55 C52 C51 106(2) 3_765 . ? C54 C52 C51 64.9(16) 3_765 . ? C53 C52 C54 86(3) . 2_645 ? C55 C52 C54 50(3) . 2_645 ? C54 C52 C54 14(3) . 2_645 ? C55 C52 C54 53(3) 3_765 2_645 ? C54 C52 C54 19(2) 3_765 2_645 ? C51 C52 C54 62.3(14) . 2_645 ? C52 C53 C51 108(3) . . ? C52 C53 C55 71(3) . . ? C51 C53 C55 105(3) . . ? C52 C53 C54 70(3) . . ? C51 C53 C54 61.8(15) . . ? C55 C53 C54 47(2) . . ? C52 C53 C54 54(2) . 3_765 ? C51 C53 C54 64.2(14) . 3_765 ? C55 C53 C54 57(2) . 3_765 ? C54 C53 C54 20(4) . 3_765 ? C54 C54 C54 59.99(3) 3_765 2_645 ? C54 C54 C55 124(6) 3_765 . ? C54 C54 C55 115(9) 2_645 . ? C54 C54 C51 109(9) 3_765 . ? C54 C54 C51 133.7(17) 2_645 . ? C55 C54 C51 108(5) . . ? C54 C54 C52 87(10) 3_765 . ? C54 C54 C52 140(8) 2_645 . ? C55 C54 C52 62(4) . . ? C51 C54 C52 77(4) . . ? C54 C54 C53 120(10) 3_765 . ? C54 C54 C53 175.1(14) 2_645 . ? C55 C54 C53 61(4) . . ? C51 C54 C53 51(2) . . ? C52 C54 C53 37.5(19) . . ? C54 C54 C55 39(5) 3_765 3_765 ? C54 C54 C55 81(8) 2_645 3_765 ? C55 C54 C55 86(5) . 3_765 ? C51 C54 C55 119(5) . 3_765 ? C52 C54 C55 58(3) . 3_765 ? C53 C54 C55 96(4) . 3_765 ? C54 C54 C52 118(9) 3_765 2_645 ? C54 C54 C52 63(10) 2_645 2_645 ? C55 C54 C52 64(5) . 2_645 ? C51 C54 C52 127(4) . 2_645 ? C52 C54 C52 125(2) . 2_645 ? C53 C54 C52 115(3) . 2_645 ? C55 C54 C52 112(3) 3_765 2_645 ? C54 C54 C55 71(8) 3_765 2_645 ? C54 C54 C55 33(3) 2_645 2_645 ? C55 C54 C55 83(5) . 2_645 ? C51 C54 C55 165(5) . 2_645 ? C52 C54 C55 118(3) . 2_645 ? C53 C54 C55 142(3) . 2_645 ? C55 C54 C55 70(3) 3_765 2_645 ? C52 C54 C55 48(2) 2_645 2_645 ? C54 C54 C51 93(8) 3_765 2_645 ? C54 C54 C51 47(7) 2_645 2_645 ? C55 C54 C51 123(8) . 2_645 ? C51 C54 C51 95(2) . 2_645 ? C52 C54 C51 171(3) . 2_645 ? C53 C54 C51 137(3) . 2_645 ? C55 C54 C51 126(3) 3_765 2_645 ? C52 C54 C51 61(3) 2_645 2_645 ? C55 C54 C51 71(3) 2_645 2_645 ? C54 C54 C56 77.8(10) 3_765 . ? C54 C54 C56 77.8(10) 2_645 . ? C55 C54 C56 158(5) . . ? C51 C54 C56 56.1(14) . . ? C52 C54 C56 121(4) . . ? C53 C54 C56 107(3) . . ? C55 C54 C56 114(3) 3_765 . ? C52 C54 C56 112(4) 2_645 . ? C55 C54 C56 111(3) 2_645 . ? C51 C54 C56 51.2(13) 2_645 . ? C54 C54 C53 100(10) 3_765 2_645 ? C54 C54 C53 40(10) 2_645 2_645 ? C55 C54 C53 91(6) . 2_645 ? C51 C54 C53 126(4) . 2_645 ? C52 C54 C53 151(3) . 2_645 ? C53 C54 C53 139(4) . 2_645 ? C55 C54 C53 112(3) 3_765 2_645 ? C52 C54 C53 27.8(15) 2_645 2_645 ? C55 C54 C53 42(2) 2_645 2_645 ? C51 C54 C53 37.6(16) 2_645 2_645 ? C56 C54 C53 89(2) . 2_645 ? C54 C55 C53 73(4) . . ? C54 C55 C52 71(5) . . ? C53 C55 C52 41(2) . . ? C54 C55 C52 75(6) . 2_645 ? C53 C55 C52 132(4) . 2_645 ? C52 C55 C52 145(4) . 2_645 ? C54 C55 C54 26(4) . 2_645 ? C53 C55 C54 99(3) . 2_645 ? C52 C55 C54 90(3) . 2_645 ? C52 C55 C54 55(2) 2_645 2_645 ? C54 C55 C54 23(3) . 3_765 ? C53 C55 C54 81(4) . 3_765 ? C52 C55 C54 63(3) . 3_765 ? C52 C55 C54 83(3) 2_645 3_765 ? C54 C55 C54 28(2) 2_645 3_765 ? C54 C55 C55 58(4) . 3_765 ? C53 C55 C55 88(4) . 3_765 ? C52 C55 C55 51(3) . 3_765 ? C52 C55 C55 104(3) 2_645 3_765 ? C54 C55 C55 57(3) 2_645 3_765 ? C54 C55 C55 35.5(15) 3_765 3_765 ? C54 C55 C55 62(4) . 2_645 ? C53 C55 C55 133(3) . 2_645 ? C52 C55 C55 110(3) . 2_645 ? C52 C55 C55 45(3) 2_645 2_645 ? C54 C55 C55 35.7(17) 2_645 2_645 ? C54 C55 C55 53(3) 3_765 2_645 ? C55 C55 C55 60.001(3) 3_765 2_645 ? C54 C55 C51 41(3) . . ? C53 C55 C51 36.0(17) . . ? C52 C55 C51 59(3) . . ? C52 C55 C51 98(3) 2_645 . ? C54 C55 C51 66.4(18) 2_645 . ? C54 C55 C51 58(2) 3_765 . ? C55 C55 C51 83(2) 3_765 . ? C55 C55 C51 102.1(15) 2_645 . ? C57 C56 C51 120.6(11) . 3_765 ? C57 C56 C51 120.6(11) . . ? C51 C56 C51 96.4(14) 3_765 . ? C57 C56 C51 120.6(11) . 2_645 ? C51 C56 C51 96.4(14) 3_765 2_645 ? C51 C56 C51 96.4(14) . 2_645 ? C57 C56 C54 165.9(11) . . ? C51 C56 C54 71(2) 3_765 . ? C51 C56 C54 46.5(16) . . ? C51 C56 C54 62(3) 2_645 . ? C57 C56 C54 165.9(11) . 3_765 ? C51 C56 C54 46.5(16) 3_765 3_765 ? C51 C56 C54 62(3) . 3_765 ? C51 C56 C54 71(2) 2_645 3_765 ? C54 C56 C54 24.3(19) . 3_765 ? C57 C56 C54 165.9(11) . 2_645 ? C51 C56 C54 62(3) 3_765 2_645 ? C51 C56 C54 71(2) . 2_645 ? C51 C56 C54 46.5(16) 2_645 2_645 ? C54 C56 C54 24.3(19) . 2_645 ? C54 C56 C54 24.3(19) 3_765 2_645 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ca O1 C11 26.3(3) 10_656 . . . ? O3 Ca O1 C11 -98.9(3) . . . . ? O3 Ca O1 C11 81.1(3) 10_656 . . . ? N2 Ca O1 C11 -13.6(3) . . . . ? N2 Ca O1 C11 166.4(3) 10_656 . . . ? Ca O1 C11 C12 8.3(4) . . . . ? Ca O1 C11 C16 -172.56(19) . . . . ? O1 C11 C12 C13 -175.9(3) . . . . ? C16 C11 C12 C13 5.0(4) . . . . ? O1 C11 C12 C120 6.5(4) . . . . ? C16 C11 C12 C120 -172.6(3) . . . . ? C120 C12 C13 C14 176.4(3) . . . . ? C11 C12 C13 C14 -1.4(5) . . . . ? C12 C13 C14 C15 -2.3(5) . . . . ? C13 C14 C15 C16 2.3(5) . . . . ? C14 C15 C16 C11 1.5(4) . . . . ? C14 C15 C16 C161 -177.9(3) . . . . ? O1 C11 C16 C15 175.9(3) . . . . ? C12 C11 C16 C15 -4.9(4) . . . . ? O1 C11 C16 C161 -4.7(4) . . . . ? C12 C11 C16 C161 174.5(2) . . . . ? C15 C16 C161 C162 121.8(3) . . . . ? C11 C16 C161 C162 -57.6(3) . . . . ? C15 C16 C161 C164 -116.6(3) . . . . ? C11 C16 C161 C164 64.0(3) . . . . ? C15 C16 C161 C163 2.8(4) . . . . ? C11 C16 C161 C163 -176.6(2) . . . . ? C13 C12 C120 N2 175.2(3) . . . . ? C11 C12 C120 N2 -7.1(5) . . . . ? C12 C120 N2 C21 175.4(3) . . . . ? C12 C120 N2 Ca -4.4(4) . . . . ? O1 Ca N2 C120 10.1(2) . . . . ? O1 Ca N2 C120 -169.9(2) 10_656 . . . ? O3 Ca N2 C120 102.4(2) . . . . ? O3 Ca N2 C120 -77.6(2) 10_656 . . . ? N2 Ca N2 C120 -179(35) 10_656 . . . ? O1 Ca N2 C21 -169.6(2) . . . . ? O1 Ca N2 C21 10.4(2) 10_656 . . . ? O3 Ca N2 C21 -77.4(2) . . . . ? O3 Ca N2 C21 102.6(2) 10_656 . . . ? N2 Ca N2 C21 1(35) 10_656 . . . ? C120 N2 C21 C26 102.3(3) . . . . ? Ca N2 C21 C26 -77.9(3) . . . . ? C120 N2 C21 C22 -79.5(4) . . . . ? Ca N2 C21 C22 100.3(3) . . . . ? C26 C21 C22 F22 -179.9(3) . . . . ? N2 C21 C22 F22 1.8(5) . . . . ? C26 C21 C22 C23 1.0(5) . . . . ? N2 C21 C22 C23 -177.2(3) . . . . ? F22 C22 C23 F23 -0.2(6) . . . . ? C21 C22 C23 F23 178.9(3) . . . . ? F22 C22 C23 C24 178.4(3) . . . . ? C21 C22 C23 C24 -2.5(6) . . . . ? F23 C23 C24 F24 -0.9(5) . . . . ? C22 C23 C24 F24 -179.5(3) . . . . ? F23 C23 C24 C25 -179.5(3) . . . . ? C22 C23 C24 C25 1.9(5) . . . . ? F24 C24 C25 F25 1.7(5) . . . . ? C23 C24 C25 F25 -179.7(3) . . . . ? F24 C24 C25 C26 -178.5(3) . . . . ? C23 C24 C25 C26 0.1(5) . . . . ? C22 C21 C26 F26 -179.0(3) . . . . ? N2 C21 C26 F26 -0.7(4) . . . . ? C22 C21 C26 C25 1.1(5) . . . . ? N2 C21 C26 C25 179.3(3) . . . . ? F25 C25 C26 F26 -1.8(4) . . . . ? C24 C25 C26 F26 178.4(3) . . . . ? F25 C25 C26 C21 178.1(3) . . . . ? C24 C25 C26 C21 -1.7(5) . . . . ? O1 Ca O3 C31 -169.8(3) . . . . ? O1 Ca O3 C31 10.2(3) 10_656 . . . ? O3 Ca O3 C31 47(2) 10_656 . . . ? N2 Ca O3 C31 116.2(3) . . . . ? N2 Ca O3 C31 -63.8(3) 10_656 . . . ? O1 Ca O3 C34 5.3(3) . . . . ? O1 Ca O3 C34 -174.7(3) 10_656 . . . ? O3 Ca O3 C34 -138(2) 10_656 . . . ? N2 Ca O3 C34 -68.7(3) . . . . ? N2 Ca O3 C34 111.3(3) 10_656 . . . ? C34 O3 C31 C32 -10.3(4) . . . . ? Ca O3 C31 C32 165.4(2) . . . . ? O3 C31 C32 C33B 29.9(5) . . . . ? O3 C31 C32 C33A -3.2(6) . . . . ? C33B C32 C33A C34 -75.2(14) . . . . ? C31 C32 C33A C34 16.7(10) . . . . ? C31 C32 C33B C34 -37.5(6) . . . . ? C33A C32 C33B C34 58.4(10) . . . . ? C32 C33A C34 O3 -23.3(10) . . . . ? C32 C33A C34 C33B 63.1(11) . . . . ? C31 O3 C34 C33A 21.8(7) . . . . ? Ca O3 C34 C33A -154.1(6) . . . . ? C31 O3 C34 C33B -12.4(5) . . . . ? Ca O3 C34 C33B 171.7(4) . . . . ? C32 C33B C34 C33A -71.4(14) . . . . ? C32 C33B C34 O3 31.4(7) . . . . ? C54 C51 C52 C53 -109(4) . . . . ? C56 C51 C52 C53 -152(3) . . . . ? C54 C51 C52 C53 -140(4) 3_765 . . . ? C54 C51 C52 C53 -118(4) 2_645 . . . ? C55 C51 C52 C53 -69(3) . . . . ? C53 C51 C52 C55 69(3) . . . . ? C54 C51 C52 C55 -41(4) . . . . ? C56 C51 C52 C55 -84(3) . . . . ? C54 C51 C52 C55 -71(3) 3_765 . . . ? C54 C51 C52 C55 -50(4) 2_645 . . . ? C53 C51 C52 C54 109(4) . . . . ? C56 C51 C52 C54 -43(3) . . . . ? C54 C51 C52 C54 -30(4) 3_765 . . . ? C54 C51 C52 C54 -9(5) 2_645 . . . ? C55 C51 C52 C54 41(4) . . . . ? C53 C51 C52 C55 149(5) . . . 3_765 ? C54 C51 C52 C55 40(3) . . . 3_765 ? C56 C51 C52 C55 -3(3) . . . 3_765 ? C54 C51 C52 C55 9(3) 3_765 . . 3_765 ? C54 C51 C52 C55 31(3) 2_645 . . 3_765 ? C55 C51 C52 C55 80(4) . . . 3_765 ? C53 C51 C52 C54 140(4) . . . 3_765 ? C54 C51 C52 C54 30(4) . . . 3_765 ? C56 C51 C52 C54 -13(2) . . . 3_765 ? C54 C51 C52 C54 21(2) 2_645 . . 3_765 ? C55 C51 C52 C54 71(3) . . . 3_765 ? C53 C51 C52 C54 118(4) . . . 2_645 ? C54 C51 C52 C54 9(5) . . . 2_645 ? C56 C51 C52 C54 -34(3) . . . 2_645 ? C54 C51 C52 C54 -21(2) 3_765 . . 2_645 ? C55 C51 C52 C54 50(4) . . . 2_645 ? C55 C52 C53 C51 -100(3) . . . . ? C54 C52 C53 C51 -50(3) . . . . ? C55 C52 C53 C51 -48(7) 3_765 . . . ? C54 C52 C53 C51 -36(3) 3_765 . . . ? C54 C52 C53 C51 -51(3) 2_645 . . . ? C54 C52 C53 C55 50(2) . . . . ? C55 C52 C53 C55 51(6) 3_765 . . . ? C54 C52 C53 C55 63(3) 3_765 . . . ? C51 C52 C53 C55 100(3) . . . . ? C54 C52 C53 C55 48(3) 2_645 . . . ? C55 C52 C53 C54 -50(2) . . . . ? C55 C52 C53 C54 1(6) 3_765 . . . ? C54 C52 C53 C54 14(3) 3_765 . . . ? C51 C52 C53 C54 50(3) . . . . ? C54 C52 C53 C54 -1(3) 2_645 . . . ? C55 C52 C53 C54 -63(3) . . . 3_765 ? C54 C52 C53 C54 -14(3) . . . 3_765 ? C55 C52 C53 C54 -12(5) 3_765 . . 3_765 ? C51 C52 C53 C54 36(3) . . . 3_765 ? C54 C52 C53 C54 -15.0(13) 2_645 . . 3_765 ? C54 C51 C53 C52 55(4) . . . . ? C56 C51 C53 C52 44(5) . . . . ? C54 C51 C53 C52 32(3) 3_765 . . . ? C54 C51 C53 C52 55(3) 2_645 . . . ? C55 C51 C53 C52 74(3) . . . . ? C54 C51 C53 C55 -19(5) . . . . ? C56 C51 C53 C55 -31(5) . . . . ? C52 C51 C53 C55 -74(3) . . . . ? C54 C51 C53 C55 -42(3) 3_765 . . . ? C54 C51 C53 C55 -19(3) 2_645 . . . ? C56 C51 C53 C54 -11(4) . . . . ? C52 C51 C53 C54 -55(4) . . . . ? C54 C51 C53 C54 -23(5) 3_765 . . . ? C54 C51 C53 C54 0(5) 2_645 . . . ? C55 C51 C53 C54 19(5) . . . . ? C54 C51 C53 C54 23(5) . . . 3_765 ? C56 C51 C53 C54 12(3) . . . 3_765 ? C52 C51 C53 C54 -32(3) . . . 3_765 ? C54 C51 C53 C54 22.6(19) 2_645 . . 3_765 ? C55 C51 C53 C54 42(3) . . . 3_765 ? C53 C51 C54 C54 -113(10) . . . 3_765 ? C56 C51 C54 C54 60(9) . . . 3_765 ? C52 C51 C54 C54 -82(11) . . . 3_765 ? C54 C51 C54 C54 66(8) 2_645 . . 3_765 ? C55 C51 C54 C54 -137(16) . . . 3_765 ? C53 C51 C54 C54 -180(100) . . . 2_645 ? C56 C51 C54 C54 -7(17) . . . 2_645 ? C52 C51 C54 C54 -149(19) . . . 2_645 ? C54 C51 C54 C54 -66(8) 3_765 . . 2_645 ? C55 C51 C54 C54 156(23) . . . 2_645 ? C53 C51 C54 C55 24(6) . . . . ? C56 C51 C54 C55 -163(7) . . . . ? C52 C51 C54 C55 55(5) . . . . ? C54 C51 C54 C55 137(16) 3_765 . . . ? C54 C51 C54 C55 -156(23) 2_645 . . . ? C53 C51 C54 C52 -31.0(17) . . . . ? C56 C51 C54 C52 142(3) . . . . ? C54 C51 C54 C52 82(11) 3_765 . . . ? C54 C51 C54 C52 149(19) 2_645 . . . ? C55 C51 C54 C52 -55(5) . . . . ? C56 C51 C54 C53 173(3) . . . . ? C52 C51 C54 C53 31.0(17) . . . . ? C54 C51 C54 C53 113(10) 3_765 . . . ? C54 C51 C54 C53 180(100) 2_645 . . . ? C55 C51 C54 C53 -24(6) . . . . ? C53 C51 C54 C55 -72(3) . . . 3_765 ? C56 C51 C54 C55 101(3) . . . 3_765 ? C52 C51 C54 C55 -41(3) . . . 3_765 ? C54 C51 C54 C55 41(10) 3_765 . . 3_765 ? C54 C51 C54 C55 108(17) 2_645 . . 3_765 ? C55 C51 C54 C55 -96(7) . . . 3_765 ? C53 C51 C54 C52 94(3) . . . 2_645 ? C56 C51 C54 C52 -93(3) . . . 2_645 ? C52 C51 C54 C52 125(3) . . . 2_645 ? C54 C51 C54 C52 -153(11) 3_765 . . 2_645 ? C54 C51 C54 C52 -87(19) 2_645 . . 2_645 ? C55 C51 C54 C52 70(6) . . . 2_645 ? C53 C51 C54 C55 159(19) . . . 2_645 ? C56 C51 C54 C55 -28(18) . . . 2_645 ? C52 C51 C54 C55 -170(19) . . . 2_645 ? C54 C51 C54 C55 -88(13) 3_765 . . 2_645 ? C54 C51 C54 C55 -22(11) 2_645 . . 2_645 ? C55 C51 C54 C55 135(23) . . . 2_645 ? C53 C51 C54 C51 151(4) . . . 2_645 ? C56 C51 C54 C51 -35.6(14) . . . 2_645 ? C52 C51 C54 C51 -178(4) . . . 2_645 ? C54 C51 C54 C51 -95(8) 3_765 . . 2_645 ? C54 C51 C54 C51 -29(16) 2_645 . . 2_645 ? C55 C51 C54 C51 127(8) . . . 2_645 ? C53 C51 C54 C56 -173(3) . . . . ? C52 C51 C54 C56 -142(3) . . . . ? C54 C51 C54 C56 -60(9) 3_765 . . . ? C54 C51 C54 C56 7(17) 2_645 . . . ? C55 C51 C54 C56 163(7) . . . . ? C53 C51 C54 C53 128(4) . . . 2_645 ? C56 C51 C54 C53 -58(3) . . . 2_645 ? C52 C51 C54 C53 159(4) . . . 2_645 ? C54 C51 C54 C53 -118(8) 3_765 . . 2_645 ? C54 C51 C54 C53 -52(16) 2_645 . . 2_645 ? C55 C51 C54 C53 105(9) . . . 2_645 ? C53 C52 C54 C54 152(6) . . . 3_765 ? C55 C52 C54 C54 -131(5) . . . 3_765 ? C55 C52 C54 C54 -27(4) 3_765 . . 3_765 ? C51 C52 C54 C54 110(6) . . . 3_765 ? C54 C52 C54 C54 -34(9) 2_645 . . 3_765 ? C53 C52 C54 C54 -174(14) . . . 2_645 ? C55 C52 C54 C54 -97(13) . . . 2_645 ? C55 C52 C54 C54 7(13) 3_765 . . 2_645 ? C54 C52 C54 C54 34(9) 3_765 . . 2_645 ? C51 C52 C54 C54 145(14) . . . 2_645 ? C53 C52 C54 C55 -77(4) . . . . ? C55 C52 C54 C55 104(6) 3_765 . . . ? C54 C52 C54 C55 131(5) 3_765 . . . ? C51 C52 C54 C55 -118(5) . . . . ? C54 C52 C54 C55 97(13) 2_645 . . . ? C53 C52 C54 C51 41(2) . . . . ? C55 C52 C54 C51 118(5) . . . . ? C55 C52 C54 C51 -138(3) 3_765 . . . ? C54 C52 C54 C51 -110(6) 3_765 . . . ? C54 C52 C54 C51 -145(14) 2_645 . . . ? C55 C52 C54 C53 77(4) . . . . ? C55 C52 C54 C53 -179(4) 3_765 . . . ? C54 C52 C54 C53 -152(6) 3_765 . . . ? C51 C52 C54 C53 -41(2) . . . . ? C54 C52 C54 C53 174(14) 2_645 . . . ? C53 C52 C54 C55 179(4) . . . 3_765 ? C55 C52 C54 C55 -104(6) . . . 3_765 ? C54 C52 C54 C55 27(4) 3_765 . . 3_765 ? C51 C52 C54 C55 138(3) . . . 3_765 ? C54 C52 C54 C55 -7(13) 2_645 . . 3_765 ? C53 C52 C54 C52 -85(4) . . . 2_645 ? C55 C52 C54 C52 -8(4) . . . 2_645 ? C55 C52 C54 C52 96(4) 3_765 . . 2_645 ? C54 C52 C54 C52 124(4) 3_765 . . 2_645 ? C51 C52 C54 C52 -126(4) . . . 2_645 ? C54 C52 C54 C52 89(12) 2_645 . . 2_645 ? C53 C52 C54 C55 -141(4) . . . 2_645 ? C55 C52 C54 C55 -64(4) . . . 2_645 ? C55 C52 C54 C55 40(4) 3_765 . . 2_645 ? C54 C52 C54 C55 67(3) 3_765 . . 2_645 ? C51 C52 C54 C55 177(5) . . . 2_645 ? C54 C52 C54 C55 32(11) 2_645 . . 2_645 ? C53 C52 C54 C51 56(24) . . . 2_645 ? C55 C52 C54 C51 133(26) . . . 2_645 ? C55 C52 C54 C51 -123(24) 3_765 . . 2_645 ? C54 C52 C54 C51 -96(28) 3_765 . . 2_645 ? C51 C52 C54 C51 15(23) . . . 2_645 ? C54 C52 C54 C51 -130(35) 2_645 . . 2_645 ? C53 C52 C54 C56 78(3) . . . . ? C55 C52 C54 C56 155(5) . . . . ? C55 C52 C54 C56 -101(3) 3_765 . . . ? C54 C52 C54 C56 -74(6) 3_765 . . . ? C51 C52 C54 C56 36.2(19) . . . . ? C54 C52 C54 C56 -109(15) 2_645 . . . ? C53 C52 C54 C53 -103(6) . . . 2_645 ? C55 C52 C54 C53 -26(5) . . . 2_645 ? C55 C52 C54 C53 78(7) 3_765 . . 2_645 ? C54 C52 C54 C53 105(5) 3_765 . . 2_645 ? C51 C52 C54 C53 -144(8) . . . 2_645 ? C54 C52 C54 C53 71(10) 2_645 . . 2_645 ? C52 C53 C54 C54 -33(3) . . . 3_765 ? C51 C53 C54 C54 91(3) . . . 3_765 ? C55 C53 C54 C54 -115(4) . . . 3_765 ? C52 C53 C54 C54 55(100) . . . 2_645 ? C51 C53 C54 C54 179(100) . . . 2_645 ? C55 C53 C54 C54 -27(100) . . . 2_645 ? C54 C53 C54 C54 88(100) 3_765 . . 2_645 ? C52 C53 C54 C55 82(4) . . . . ? C51 C53 C54 C55 -154(6) . . . . ? C54 C53 C54 C55 115(4) 3_765 . . . ? C52 C53 C54 C51 -124(3) . . . . ? C55 C53 C54 C51 154(6) . . . . ? C54 C53 C54 C51 -91(3) 3_765 . . . ? C51 C53 C54 C52 124(3) . . . . ? C55 C53 C54 C52 -82(4) . . . . ? C54 C53 C54 C52 33(3) 3_765 . . . ? C52 C53 C54 C55 -1(3) . . . 3_765 ? C51 C53 C54 C55 124(4) . . . 3_765 ? C55 C53 C54 C55 -83(5) . . . 3_765 ? C54 C53 C54 C55 32.2(17) 3_765 . . 3_765 ? C52 C53 C54 C52 117(3) . . . 2_645 ? C51 C53 C54 C52 -119(4) . . . 2_645 ? C55 C53 C54 C52 35(4) . . . 2_645 ? C54 C53 C54 C52 150(2) 3_765 . . 2_645 ? C52 C53 C54 C55 64(8) . . . 2_645 ? C51 C53 C54 C55 -171(9) . . . 2_645 ? C55 C53 C54 C55 -18(7) . . . 2_645 ? C54 C53 C54 C55 97(7) 3_765 . . 2_645 ? C52 C53 C54 C51 -169(6) . . . 2_645 ? C51 C53 C54 C51 -45(5) . . . 2_645 ? C55 C53 C54 C51 109(9) . . . 2_645 ? C54 C53 C54 C51 -136(7) 3_765 . . 2_645 ? C52 C53 C54 C56 -119(4) . . . . ? C51 C53 C54 C56 6(2) . . . . ? C55 C53 C54 C56 160(7) . . . . ? C54 C53 C54 C56 -86(5) 3_765 . . . ? C52 C53 C54 C53 133(3) . . . 2_645 ? C51 C53 C54 C53 -103(4) . . . 2_645 ? C55 C53 C54 C53 51(5) . . . 2_645 ? C54 C53 C54 C53 166(4) 3_765 . . 2_645 ? C54 C54 C55 C53 108(16) 3_765 . . . ? C54 C54 C55 C53 178(13) 2_645 . . . ? C51 C54 C55 C53 -21(5) . . . . ? C52 C54 C55 C53 43(2) . . . . ? C55 C54 C55 C53 99(4) 3_765 . . . ? C52 C54 C55 C53 -144(3) 2_645 . . . ? C55 C54 C55 C53 169(4) 2_645 . . . ? C51 C54 C55 C53 -130(4) 2_645 . . . ? C56 C54 C55 C53 -61(20) . . . . ? C53 C54 C55 C53 -150(2) 2_645 . . . ? C54 C54 C55 C52 65(16) 3_765 . . . ? C54 C54 C55 C52 135(12) 2_645 . . . ? C51 C54 C55 C52 -64(6) . . . . ? C53 C54 C55 C52 -43(2) . . . . ? C55 C54 C55 C52 56(3) 3_765 . . . ? C52 C54 C55 C52 173(3) 2_645 . . . ? C55 C54 C55 C52 126(3) 2_645 . . . ? C51 C54 C55 C52 -172(3) 2_645 . . . ? C56 C54 C55 C52 -104(20) . . . . ? C53 C54 C55 C52 168(2) 2_645 . . . ? C54 C54 C55 C52 -108(15) 3_765 . . 2_645 ? C54 C54 C55 C52 -38(12) 2_645 . . 2_645 ? C51 C54 C55 C52 123(5) . . . 2_645 ? C52 C54 C55 C52 -173(3) . . . 2_645 ? C53 C54 C55 C52 144(3) . . . 2_645 ? C55 C54 C55 C52 -117(2) 3_765 . . 2_645 ? C55 C54 C55 C52 -47(3) 2_645 . . 2_645 ? C51 C54 C55 C52 15(4) 2_645 . . 2_645 ? C56 C54 C55 C52 83(20) . . . 2_645 ? C53 C54 C55 C52 -6(2) 2_645 . . 2_645 ? C54 C54 C55 C54 -69(4) 3_765 . . 2_645 ? C51 C54 C55 C54 161(17) . . . 2_645 ? C52 C54 C55 C54 -135(12) . . . 2_645 ? C53 C54 C55 C54 -178(13) . . . 2_645 ? C55 C54 C55 C54 -79(11) 3_765 . . 2_645 ? C52 C54 C55 C54 38(12) 2_645 . . 2_645 ? C55 C54 C55 C54 -8(11) 2_645 . . 2_645 ? C51 C54 C55 C54 53(13) 2_645 . . 2_645 ? C56 C54 C55 C54 121(31) . . . 2_645 ? C53 C54 C55 C54 33(11) 2_645 . . 2_645 ? C54 C54 C55 C54 69(4) 2_645 . . 3_765 ? C51 C54 C55 C54 -129(20) . . . 3_765 ? C52 C54 C55 C54 -65(16) . . . 3_765 ? C53 C54 C55 C54 -108(16) . . . 3_765 ? C55 C54 C55 C54 -10(14) 3_765 . . 3_765 ? C52 C54 C55 C54 108(15) 2_645 . . 3_765 ? C55 C54 C55 C54 61(14) 2_645 . . 3_765 ? C51 C54 C55 C54 122(16) 2_645 . . 3_765 ? C56 C54 C55 C54 -169(35) . . . 3_765 ? C53 C54 C55 C54 102(15) 2_645 . . 3_765 ? C54 C54 C55 C55 10(14) 3_765 . . 3_765 ? C54 C54 C55 C55 79(11) 2_645 . . 3_765 ? C51 C54 C55 C55 -120(6) . . . 3_765 ? C52 C54 C55 C55 -56(3) . . . 3_765 ? C53 C54 C55 C55 -99(4) . . . 3_765 ? C52 C54 C55 C55 117(2) 2_645 . . 3_765 ? C55 C54 C55 C55 71(2) 2_645 . . 3_765 ? C51 C54 C55 C55 132(5) 2_645 . . 3_765 ? C56 C54 C55 C55 -160(21) . . . 3_765 ? C53 C54 C55 C55 112(3) 2_645 . . 3_765 ? C54 C54 C55 C55 -61(14) 3_765 . . 2_645 ? C54 C54 C55 C55 8(11) 2_645 . . 2_645 ? C51 C54 C55 C55 170(7) . . . 2_645 ? C52 C54 C55 C55 -126(3) . . . 2_645 ? C53 C54 C55 C55 -169(4) . . . 2_645 ? C55 C54 C55 C55 -71(2) 3_765 . . 2_645 ? C52 C54 C55 C55 47(3) 2_645 . . 2_645 ? C51 C54 C55 C55 61(3) 2_645 . . 2_645 ? C56 C54 C55 C55 130(21) . . . 2_645 ? C53 C54 C55 C55 41(2) 2_645 . . 2_645 ? C54 C54 C55 C51 129(20) 3_765 . . . ? C54 C54 C55 C51 -161(17) 2_645 . . . ? C52 C54 C55 C51 64(6) . . . . ? C53 C54 C55 C51 21(5) . . . . ? C55 C54 C55 C51 120(6) 3_765 . . . ? C52 C54 C55 C51 -123(5) 2_645 . . . ? C55 C54 C55 C51 -170(7) 2_645 . . . ? C51 C54 C55 C51 -108(6) 2_645 . . . ? C56 C54 C55 C51 -40(16) . . . . ? C53 C54 C55 C51 -129(6) 2_645 . . . ? C52 C53 C55 C54 -81(5) . . . . ? C51 C53 C55 C54 24(5) . . . . ? C54 C53 C55 C54 -22(5) 3_765 . . . ? C51 C53 C55 C52 105(3) . . . . ? C54 C53 C55 C52 81(5) . . . . ? C54 C53 C55 C52 59(2) 3_765 . . . ? C52 C53 C55 C52 -130(6) . . . 2_645 ? C51 C53 C55 C52 -26(6) . . . 2_645 ? C54 C53 C55 C52 -49(6) . . . 2_645 ? C54 C53 C55 C52 -71(5) 3_765 . . 2_645 ? C52 C53 C55 C54 -80(3) . . . 2_645 ? C51 C53 C55 C54 25(4) . . . 2_645 ? C54 C53 C55 C54 1(6) . . . 2_645 ? C54 C53 C55 C54 -21(2) 3_765 . . 2_645 ? C52 C53 C55 C54 -59(2) . . . 3_765 ? C51 C53 C55 C54 46(3) . . . 3_765 ? C54 C53 C55 C54 22(5) . . . 3_765 ? C52 C53 C55 C55 -24(3) . . . 3_765 ? C51 C53 C55 C55 81(3) . . . 3_765 ? C54 C53 C55 C55 57(4) . . . 3_765 ? C54 C53 C55 C55 35.0(15) 3_765 . . 3_765 ? C52 C53 C55 C55 -68(5) . . . 2_645 ? C51 C53 C55 C55 37(6) . . . 2_645 ? C54 C53 C55 C55 13(4) . . . 2_645 ? C54 C53 C55 C55 -9(5) 3_765 . . 2_645 ? C52 C53 C55 C51 -105(3) . . . . ? C54 C53 C55 C51 -24(5) . . . . ? C54 C53 C55 C51 -46(3) 3_765 . . . ? C53 C52 C55 C54 85(3) . . . . ? C55 C52 C55 C54 -64(4) 3_765 . . . ? C54 C52 C55 C54 -23(3) 3_765 . . . ? C51 C52 C55 C54 43(3) . . . . ? C54 C52 C55 C54 -18(3) 2_645 . . . ? C54 C52 C55 C53 -85(3) . . . . ? C55 C52 C55 C53 -149(3) 3_765 . . . ? C54 C52 C55 C53 -108(3) 3_765 . . . ? C51 C52 C55 C53 -41.7(18) . . . . ? C54 C52 C55 C53 -104(3) 2_645 . . . ? C53 C52 C55 C52 97(7) . . . 2_645 ? C54 C52 C55 C52 12(6) . . . 2_645 ? C55 C52 C55 C52 -52(9) 3_765 . . 2_645 ? C54 C52 C55 C52 -12(7) 3_765 . . 2_645 ? C51 C52 C55 C52 55(7) . . . 2_645 ? C54 C52 C55 C52 -7(6) 2_645 . . 2_645 ? C53 C52 C55 C54 104(3) . . . 2_645 ? C54 C52 C55 C54 18(3) . . . 2_645 ? C55 C52 C55 C54 -45(4) 3_765 . . 2_645 ? C54 C52 C55 C54 -5(3) 3_765 . . 2_645 ? C51 C52 C55 C54 62(2) . . . 2_645 ? C53 C52 C55 C54 108(3) . . . 3_765 ? C54 C52 C55 C54 23(3) . . . 3_765 ? C55 C52 C55 C54 -40(3) 3_765 . . 3_765 ? C51 C52 C55 C54 66.8(17) . . . 3_765 ? C54 C52 C55 C54 5(3) 2_645 . . 3_765 ? C53 C52 C55 C55 149(3) . . . 3_765 ? C54 C52 C55 C55 64(4) . . . 3_765 ? C54 C52 C55 C55 40(3) 3_765 . . 3_765 ? C51 C52 C55 C55 107(2) . . . 3_765 ? C54 C52 C55 C55 45(4) 2_645 . . 3_765 ? C53 C52 C55 C55 134(3) . . . 2_645 ? C54 C52 C55 C55 49(3) . . . 2_645 ? C55 C52 C55 C55 -15(3) 3_765 . . 2_645 ? C54 C52 C55 C55 25.5(16) 3_765 . . 2_645 ? C51 C52 C55 C55 92.3(16) . . . 2_645 ? C54 C52 C55 C55 30(3) 2_645 . . 2_645 ? C53 C52 C55 C51 41.7(18) . . . . ? C54 C52 C55 C51 -43(3) . . . . ? C55 C52 C55 C51 -107(2) 3_765 . . . ? C54 C52 C55 C51 -66.8(17) 3_765 . . . ? C54 C52 C55 C51 -62(2) 2_645 . . . ? C53 C51 C55 C54 -144(9) . . . . ? C56 C51 C55 C54 17(8) . . . . ? C52 C51 C55 C54 -97(7) . . . . ? C54 C51 C55 C54 -21(9) 3_765 . . . ? C54 C51 C55 C54 9(9) 2_645 . . . ? C54 C51 C55 C53 144(9) . . . . ? C56 C51 C55 C53 162(3) . . . . ? C52 C51 C55 C53 47(3) . . . . ? C54 C51 C55 C53 123(4) 3_765 . . . ? C54 C51 C55 C53 153(4) 2_645 . . . ? C53 C51 C55 C52 -47(3) . . . . ? C54 C51 C55 C52 97(8) . . . . ? C56 C51 C55 C52 114(3) . . . . ? C54 C51 C55 C52 76(3) 3_765 . . . ? C54 C51 C55 C52 106(4) 2_645 . . . ? C53 C51 C55 C52 161(5) . . . 2_645 ? C54 C51 C55 C52 -55(7) . . . 2_645 ? C56 C51 C55 C52 -37(3) . . . 2_645 ? C52 C51 C55 C52 -152(4) . . . 2_645 ? C54 C51 C55 C52 -76(3) 3_765 . . 2_645 ? C54 C51 C55 C52 -46(3) 2_645 . . 2_645 ? C53 C51 C55 C54 -153(4) . . . 2_645 ? C54 C51 C55 C54 -9(9) . . . 2_645 ? C56 C51 C55 C54 9(3) . . . 2_645 ? C52 C51 C55 C54 -106(4) . . . 2_645 ? C54 C51 C55 C54 -30(2) 3_765 . . 2_645 ? C53 C51 C55 C54 -123(4) . . . 3_765 ? C54 C51 C55 C54 21(9) . . . 3_765 ? C56 C51 C55 C54 38(3) . . . 3_765 ? C52 C51 C55 C54 -76(3) . . . 3_765 ? C54 C51 C55 C54 30(2) 2_645 . . 3_765 ? C53 C51 C55 C55 -96(5) . . . 3_765 ? C54 C51 C55 C55 48(6) . . . 3_765 ? C56 C51 C55 C55 65(3) . . . 3_765 ? C52 C51 C55 C55 -49(3) . . . 3_765 ? C54 C51 C55 C55 27(3) 3_765 . . 3_765 ? C54 C51 C55 C55 57(3) 2_645 . . 3_765 ? C53 C51 C55 C55 -154(5) . . . 2_645 ? C54 C51 C55 C55 -9(6) . . . 2_645 ? C56 C51 C55 C55 8(4) . . . 2_645 ? C52 C51 C55 C55 -106(3) . . . 2_645 ? C54 C51 C55 C55 -30(3) 3_765 . . 2_645 ? C54 C51 C55 C55 0(4) 2_645 . . 2_645 ? C53 C51 C56 C57 -177(3) . . . . ? C54 C51 C56 C57 173(3) . . . . ? C52 C51 C56 C57 -153.2(12) . . . . ? C54 C51 C56 C57 -164.3(14) 3_765 . . . ? C54 C51 C56 C57 171(2) 2_645 . . . ? C55 C51 C56 C57 163.7(17) . . . . ? C53 C51 C56 C51 -45(3) . . . 3_765 ? C54 C51 C56 C51 -56(3) . . . 3_765 ? C52 C51 C56 C51 -21.8(18) . . . 3_765 ? C54 C51 C56 C51 -32.9(16) 3_765 . . 3_765 ? C54 C51 C56 C51 -58(3) 2_645 . . 3_765 ? C55 C51 C56 C51 -64.9(18) . . . 3_765 ? C53 C51 C56 C51 52(3) . . . 2_645 ? C54 C51 C56 C51 42(3) . . . 2_645 ? C52 C51 C56 C51 75.4(11) . . . 2_645 ? C54 C51 C56 C51 64.4(17) 3_765 . . 2_645 ? C54 C51 C56 C51 39(2) 2_645 . . 2_645 ? C55 C51 C56 C51 32(2) . . . 2_645 ? C53 C51 C56 C54 11(4) . . . . ? C52 C51 C56 C54 34(3) . . . . ? C54 C51 C56 C54 23(4) 3_765 . . . ? C54 C51 C56 C54 -2(5) 2_645 . . . ? C55 C51 C56 C54 -9(4) . . . . ? C53 C51 C56 C54 -12(3) . . . 3_765 ? C54 C51 C56 C54 -23(4) . . . 3_765 ? C52 C51 C56 C54 11.1(19) . . . 3_765 ? C54 C51 C56 C54 -25(2) 2_645 . . 3_765 ? C55 C51 C56 C54 -32.1(19) . . . 3_765 ? C53 C51 C56 C54 13(4) . . . 2_645 ? C54 C51 C56 C54 2(5) . . . 2_645 ? C52 C51 C56 C54 36(3) . . . 2_645 ? C54 C51 C56 C54 25(2) 3_765 . . 2_645 ? C55 C51 C56 C54 -7(3) . . . 2_645 ? C54 C54 C56 C57 -149.24(11) 3_765 . . . ? C54 C54 C56 C57 149.24(16) 2_645 . . . ? C55 C54 C56 C57 22(30) . . . . ? C51 C54 C56 C57 -26(12) . . . . ? C52 C54 C56 C57 -70(12) . . . . ? C53 C54 C56 C57 -31(14) . . . . ? C55 C54 C56 C57 -136(8) 3_765 . . . ? C52 C54 C56 C57 95(10) 2_645 . . . ? C55 C54 C56 C57 147(8) 2_645 . . . ? C51 C54 C56 C57 106(10) 2_645 . . . ? C53 C54 C56 C57 111(9) 2_645 . . . ? C54 C54 C56 C51 -4(9) 3_765 . . 3_765 ? C54 C54 C56 C51 -65(9) 2_645 . . 3_765 ? C55 C54 C56 C51 167(21) . . . 3_765 ? C51 C54 C56 C51 120(3) . . . 3_765 ? C52 C54 C56 C51 76(3) . . . 3_765 ? C53 C54 C56 C51 114(4) . . . 3_765 ? C55 C54 C56 C51 9(3) 3_765 . . 3_765 ? C52 C54 C56 C51 -120(2) 2_645 . . 3_765 ? C55 C54 C56 C51 -68(3) 2_645 . . 3_765 ? C51 C54 C56 C51 -108.4(8) 2_645 . . 3_765 ? C53 C54 C56 C51 -103.9(16) 2_645 . . 3_765 ? C54 C54 C56 C51 -123(12) 3_765 . . . ? C54 C54 C56 C51 175(12) 2_645 . . . ? C55 C54 C56 C51 48(19) . . . . ? C52 C54 C56 C51 -44(2) . . . . ? C53 C54 C56 C51 -5(2) . . . . ? C55 C54 C56 C51 -110(5) 3_765 . . . ? C52 C54 C56 C51 121(4) 2_645 . . . ? C55 C54 C56 C51 173(6) 2_645 . . . ? C51 C54 C56 C51 132(3) 2_645 . . . ? C53 C54 C56 C51 136(4) 2_645 . . . ? C54 C54 C56 C51 105(10) 3_765 . . 2_645 ? C54 C54 C56 C51 43(10) 2_645 . . 2_645 ? C55 C54 C56 C51 -84(21) . . . 2_645 ? C51 C54 C56 C51 -132(3) . . . 2_645 ? C52 C54 C56 C51 -176(4) . . . 2_645 ? C53 C54 C56 C51 -137(4) . . . 2_645 ? C55 C54 C56 C51 118(4) 3_765 . . 2_645 ? C52 C54 C56 C51 -11.4(18) 2_645 . . 2_645 ? C55 C54 C56 C51 41(3) 2_645 . . 2_645 ? C53 C54 C56 C51 4.5(13) 2_645 . . 2_645 ? C54 C54 C56 C54 -61.5(2) 2_645 . . 3_765 ? C55 C54 C56 C54 171(30) . . . 3_765 ? C51 C54 C56 C54 123(12) . . . 3_765 ? C52 C54 C56 C54 80(12) . . . 3_765 ? C53 C54 C56 C54 118(14) . . . 3_765 ? C55 C54 C56 C54 13(8) 3_765 . . 3_765 ? C52 C54 C56 C54 -116(10) 2_645 . . 3_765 ? C55 C54 C56 C54 -64(8) 2_645 . . 3_765 ? C51 C54 C56 C54 -105(10) 2_645 . . 3_765 ? C53 C54 C56 C54 -100(9) 2_645 . . 3_765 ? C54 C54 C56 C54 61.5(2) 3_765 . . 2_645 ? C55 C54 C56 C54 -127(30) . . . 2_645 ? C51 C54 C56 C54 -175(12) . . . 2_645 ? C52 C54 C56 C54 141(12) . . . 2_645 ? C53 C54 C56 C54 179(14) . . . 2_645 ? C55 C54 C56 C54 75(8) 3_765 . . 2_645 ? C52 C54 C56 C54 -55(10) 2_645 . . 2_645 ? C55 C54 C56 C54 -2(8) 2_645 . . 2_645 ? C51 C54 C56 C54 -43(10) 2_645 . . 2_645 ? C53 C54 C56 C54 -39(9) 2_645 . . 2_645 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.643 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.063 data_yanns4 _database_code_depnum_ccdc_archive 'CCDC 243645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 1-Ca' _chemical_melting_point ? _chemical_formula_moiety 'C68 H108 Ca2 N4 O4, C4 H10 O' _chemical_formula_structural '[{Ca(N{CH2C6H2O-2,tBu2-3,5}2{CH2CH2NMe2})}2].Et2O' _chemical_formula_sum 'C72 H118 Ca2 N4 O5' _chemical_formula_weight 1199.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Ca Ca 0.2030 0.3060 '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 #(no. 2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7184(2) _cell_length_b 14.4919(2) _cell_length_c 27.3095(5) _cell_angle_alpha 104.7170(10) _cell_angle_beta 90.0640(10) _cell_angle_gamma 105.4130(10) _cell_volume 3576.51(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements SORTAV (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 31350 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.05 _reflns_number_total 12430 _reflns_number_gt 8912 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) Disorder was identified in the t-butyl group of C(151) where there are two orientations of the three methyl groups, and in the CH2NMe2 groups of both ligands. In all cases, the disorder was resolved and the partial atoms were refined separately and successfully. 2) 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^)+(0.0445P)^2^+1.9043P] 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 12430 _refine_ls_number_parameters 832 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Ca1 Ca 0.60134(5) 0.09673(3) 0.309007(17) 0.02881(13) Uani 1 1 d . B . Ca2 Ca 0.52328(5) -0.06529(3) 0.188720(17) 0.02969(13) Uani 1 1 d . B . N1 N 0.82422(19) 0.21474(14) 0.29121(7) 0.0288(4) Uani 1 1 d . B . C1 C 0.9494(2) 0.18770(18) 0.30978(8) 0.0328(5) Uani 1 1 d . . . H1A H 1.0364 0.2357 0.3056 0.039 Uiso 1 1 calc R . . H1B H 0.9514 0.1234 0.2885 0.039 Uiso 1 1 calc R . . C11 C 0.9499(2) 0.18337(18) 0.36432(8) 0.0315(5) Uani 1 1 d . A . C12 C 0.8506(2) 0.10401(17) 0.37711(8) 0.0304(5) Uani 1 1 d . . . O12 O 0.75530(17) 0.03898(12) 0.34139(6) 0.0361(4) Uani 1 1 d . . . C13 C 0.8538(2) 0.09807(17) 0.42837(8) 0.0304(5) Uani 1 1 d . . . C131 C 0.7469(2) 0.01360(18) 0.44437(9) 0.0342(6) Uani 1 1 d . . . C132 C 0.5929(3) 0.0185(2) 0.43532(11) 0.0484(7) Uani 1 1 d . . . H13A H 0.5834 0.0819 0.4541 0.073 Uiso 1 1 calc R . . H13B H 0.5270 -0.0330 0.4464 0.073 Uiso 1 1 calc R . . H13C H 0.5722 0.0098 0.3998 0.073 Uiso 1 1 calc R . . C133 C 0.7600(3) -0.08787(19) 0.41397(9) 0.0417(6) Uani 1 1 d . . . H13D H 0.6918 -0.1393 0.4244 0.063 Uiso 1 1 calc R . . H13E H 0.8549 -0.0925 0.4201 0.063 Uiso 1 1 calc R . . H13F H 0.7416 -0.0953 0.3784 0.063 Uiso 1 1 calc R . . C134 C 0.7699(3) 0.0189(2) 0.50058(9) 0.0445(7) Uani 1 1 d . . . H13G H 0.7619 0.0816 0.5210 0.067 Uiso 1 1 calc R . . H13H H 0.8634 0.0123 0.5071 0.067 Uiso 1 1 calc R . . H13I H 0.6987 -0.0339 0.5089 0.067 Uiso 1 1 calc R . . C14 C 0.9536(2) 0.17251(19) 0.46315(9) 0.0365(6) Uani 1 1 d . . . H14 H 0.9556 0.1687 0.4966 0.044 Uiso 1 1 calc R . . C15 C 1.0509(2) 0.25247(19) 0.45154(9) 0.0362(6) Uani 1 1 d . A . C151 C 1.1544(3) 0.3329(2) 0.49262(10) 0.0539(8) Uani 1 1 d . . . C152 C 1.0909(9) 0.3650(6) 0.5376(3) 0.089(3) Uani 0.604(7) 1 d P A 1 H15A H 1.1617 0.4147 0.5617 0.133 Uiso 0.604(7) 1 calc PR A 1 H15B H 1.0515 0.3097 0.5514 0.133 Uiso 0.604(7) 1 calc PR A 1 H15C H 1.0159 0.3925 0.5304 0.133 Uiso 0.604(7) 1 calc PR A 1 C153 C 1.2732(6) 0.2794(5) 0.5050(2) 0.077(2) Uani 0.604(7) 1 d P A 1 H15D H 1.3200 0.2591 0.4748 0.115 Uiso 0.604(7) 1 calc PR A 1 H15E H 1.2269 0.2223 0.5165 0.115 Uiso 0.604(7) 1 calc PR A 1 H15F H 1.3429 0.3252 0.5309 0.115 Uiso 0.604(7) 1 calc PR A 1 C154 C 1.2432(7) 0.4172(4) 0.4719(2) 0.0631(19) Uani 0.604(7) 1 d P A 1 H15G H 1.2827 0.3898 0.4412 0.095 Uiso 0.604(7) 1 calc PR A 1 H15H H 1.3194 0.4587 0.4967 0.095 Uiso 0.604(7) 1 calc PR A 1 H15I H 1.1831 0.4560 0.4650 0.095 Uiso 0.604(7) 1 calc PR A 1 C155 C 1.0795(11) 0.4312(6) 0.5009(3) 0.081(4) Uani 0.396(7) 1 d P A 2 H15J H 0.9800 0.4093 0.5066 0.121 Uiso 0.396(7) 1 calc PR A 2 H15K H 1.0888 0.4553 0.4711 0.121 Uiso 0.396(7) 1 calc PR A 2 H15L H 1.1282 0.4835 0.5297 0.121 Uiso 0.396(7) 1 calc PR A 2 C156 C 1.1310(13) 0.3171(9) 0.5485(4) 0.072(3) Uani 0.396(7) 1 d P A 2 H15M H 1.0304 0.2983 0.5530 0.108 Uiso 0.396(7) 1 calc PR A 2 H15N H 1.1766 0.3779 0.5734 0.108 Uiso 0.396(7) 1 calc PR A 2 H15O H 1.1720 0.2658 0.5523 0.108 Uiso 0.396(7) 1 calc PR A 2 C157 C 1.2908(10) 0.3645(11) 0.4832(4) 0.101(6) Uani 0.396(7) 1 d P A 2 H15P H 1.3421 0.4148 0.5122 0.152 Uiso 0.396(7) 1 calc PR A 2 H15Q H 1.2962 0.3916 0.4544 0.152 Uiso 0.396(7) 1 calc PR A 2 H15R H 1.3326 0.3099 0.4761 0.152 Uiso 0.396(7) 1 calc PR A 2 C16 C 1.0480(2) 0.25465(18) 0.40098(9) 0.0340(6) Uani 1 1 d . . . H16 H 1.1136 0.3054 0.3914 0.041 Uiso 1 1 calc R A . C2 C 0.8317(2) 0.19975(18) 0.23507(8) 0.0303(5) Uani 1 1 d . . . H2A H 0.8291 0.1310 0.2200 0.036 Uiso 1 1 calc R . . H2B H 0.9236 0.2403 0.2290 0.036 Uiso 1 1 calc R . . C21 C 0.7161(2) 0.22345(17) 0.20743(8) 0.0296(5) Uani 1 1 d . . . C22 C 0.5725(2) 0.16842(16) 0.20537(8) 0.0282(5) Uani 1 1 d . . . O22 O 0.53838(16) 0.09636(11) 0.22968(5) 0.0294(4) Uani 1 1 d . . . C23 C 0.4668(2) 0.18898(17) 0.17726(8) 0.0313(5) Uani 1 1 d . . . C231 C 0.3073(3) 0.13568(19) 0.17647(9) 0.0366(6) Uani 1 1 d . . . C232 C 0.2560(3) 0.1585(2) 0.23022(9) 0.0471(7) Uani 1 1 d . . . H23A H 0.2746 0.2289 0.2436 0.071 Uiso 1 1 calc R . . H23B H 0.3061 0.1330 0.2517 0.071 Uiso 1 1 calc R . . H23C H 0.1551 0.1277 0.2290 0.071 Uiso 1 1 calc R . . C233 C 0.2759(3) 0.0227(2) 0.15565(10) 0.0459(7) Uani 1 1 d . . . H23D H 0.1753 -0.0076 0.1559 0.069 Uiso 1 1 calc R . . H23E H 0.3285 -0.0023 0.1766 0.069 Uiso 1 1 calc R . . H23F H 0.3043 0.0073 0.1215 0.069 Uiso 1 1 calc R . . C234 C 0.2136(3) 0.1695(2) 0.14336(11) 0.0536(8) Uani 1 1 d . . . H23G H 0.2301 0.2401 0.1550 0.080 Uiso 1 1 calc R . . H23H H 0.1147 0.1374 0.1456 0.080 Uiso 1 1 calc R . . H23I H 0.2374 0.1521 0.1087 0.080 Uiso 1 1 calc R . . C24 C 0.5126(3) 0.25908(18) 0.15001(8) 0.0356(6) Uani 1 1 d . . . H24 H 0.4440 0.2718 0.1309 0.043 Uiso 1 1 calc R . . C25 C 0.6552(3) 0.31155(17) 0.14970(9) 0.0344(6) Uani 1 1 d . . . C251 C 0.6936(3) 0.38403(19) 0.11614(9) 0.0405(6) Uani 1 1 d . . . C252 C 0.8537(3) 0.4336(2) 0.11994(11) 0.0549(8) Uani 1 1 d . . . H25A H 0.8733 0.4782 0.0986 0.082 Uiso 1 1 calc R . . H25B H 0.9037 0.3839 0.1092 0.082 Uiso 1 1 calc R . . H25C H 0.8850 0.4700 0.1545 0.082 Uiso 1 1 calc R . . C253 C 0.6470(3) 0.3269(2) 0.06019(9) 0.0510(7) Uani 1 1 d . . . H25D H 0.6712 0.3719 0.0391 0.076 Uiso 1 1 calc R . . H25E H 0.5454 0.2971 0.0566 0.076 Uiso 1 1 calc R . . H25F H 0.6953 0.2760 0.0500 0.076 Uiso 1 1 calc R . . C254 C 0.6149(4) 0.4644(2) 0.13219(11) 0.0566(8) Uani 1 1 d . . . H25G H 0.6393 0.5098 0.1113 0.085 Uiso 1 1 calc R . . H25H H 0.6426 0.4997 0.1671 0.085 Uiso 1 1 calc R . . H25I H 0.5135 0.4340 0.1282 0.085 Uiso 1 1 calc R . . C26 C 0.7548(3) 0.29387(17) 0.17976(8) 0.0335(6) Uani 1 1 d . . . H26 H 0.8502 0.3300 0.1816 0.040 Uiso 1 1 calc R . . C3 C 0.8296(3) 0.31894(18) 0.31651(9) 0.0366(6) Uani 1 1 d . . . H3A H 0.8752 0.3607 0.2951 0.044 Uiso 0.567(6) 1 calc PR B 1 H3B H 0.8883 0.3397 0.3482 0.044 Uiso 0.567(6) 1 calc PR B 1 H3C H 0.9287 0.3584 0.3213 0.044 Uiso 0.433(6) 1 calc PR B 2 H3D H 0.7794 0.3438 0.2943 0.044 Uiso 0.433(6) 1 calc PR B 2 C31 C 0.6829(5) 0.3347(3) 0.32743(16) 0.0384(14) Uani 0.567(6) 1 d P B 1 H31A H 0.6939 0.4040 0.3443 0.046 Uiso 0.567(6) 1 calc PR B 1 H31B H 0.6261 0.3187 0.2956 0.046 Uiso 0.567(6) 1 calc PR B 1 N32 N 0.6052(2) 0.27111(16) 0.36044(8) 0.0459(6) Uani 1 1 d . . . C33 C 0.4525(7) 0.2881(5) 0.3604(2) 0.0532(16) Uani 0.567(6) 1 d P B 1 H33A H 0.4140 0.2733 0.3260 0.080 Uiso 0.567(6) 1 calc PR B 1 H33B H 0.4592 0.3560 0.3773 0.080 Uiso 0.567(6) 1 calc PR B 1 H33C H 0.3909 0.2453 0.3778 0.080 Uiso 0.567(6) 1 calc PR B 1 C34 C 0.6617(8) 0.2964(5) 0.4097(2) 0.0531(17) Uani 0.567(6) 1 d P B 1 H34A H 0.6060 0.2516 0.4274 0.080 Uiso 0.567(6) 1 calc PR B 1 H34B H 0.6600 0.3630 0.4262 0.080 Uiso 0.567(6) 1 calc PR B 1 H34C H 0.7587 0.2923 0.4099 0.080 Uiso 0.567(6) 1 calc PR B 1 C31A C 0.7668(7) 0.3329(4) 0.3660(2) 0.0414(19) Uani 0.433(6) 1 d P B 2 H31C H 0.7740 0.4027 0.3801 0.050 Uiso 0.433(6) 1 calc PR B 2 H31D H 0.8200 0.3122 0.3893 0.050 Uiso 0.433(6) 1 calc PR B 2 C33A C 0.5185(10) 0.3097(6) 0.3403(4) 0.064(2) Uani 0.433(6) 1 d P B 2 H33D H 0.4221 0.2684 0.3379 0.096 Uiso 0.433(6) 1 calc PR B 2 H33E H 0.5460 0.3141 0.3071 0.096 Uiso 0.433(6) 1 calc PR B 2 H33F H 0.5241 0.3749 0.3614 0.096 Uiso 0.433(6) 1 calc PR B 2 C34A C 0.5802(12) 0.2739(7) 0.4173(3) 0.062(3) Uani 0.433(6) 1 d P B 2 H34D H 0.6462 0.2453 0.4302 0.093 Uiso 0.433(6) 1 calc PR B 2 H34E H 0.4839 0.2366 0.4198 0.093 Uiso 0.433(6) 1 calc PR B 2 H34F H 0.5951 0.3414 0.4368 0.093 Uiso 0.433(6) 1 calc PR B 2 N4 N 0.6230(2) -0.19856(14) 0.20390(7) 0.0300(4) Uani 1 1 d . B . C4 C 0.7678(3) -0.1863(2) 0.18349(9) 0.0373(6) Uani 1 1 d . . . H4A H 0.8029 -0.2415 0.1864 0.045 Uiso 1 1 calc R . . H4B H 0.8325 -0.1261 0.2046 0.045 Uiso 1 1 calc R . . C41 C 0.7732(2) -0.18094(18) 0.12884(9) 0.0338(6) Uani 1 1 d . . . C42 C 0.7544(2) -0.09474(17) 0.11748(9) 0.0312(5) Uani 1 1 d . . . O42 O 0.72587(17) -0.02458(12) 0.15440(6) 0.0365(4) Uani 1 1 d . . . C43 C 0.7630(2) -0.08814(17) 0.06636(8) 0.0295(5) Uani 1 1 d . . . C431 C 0.7464(2) 0.00412(17) 0.05210(8) 0.0306(5) Uani 1 1 d . . . C432 C 0.5995(3) 0.0203(2) 0.06481(10) 0.0417(6) Uani 1 1 d . . . H43A H 0.5913 0.0786 0.0558 0.063 Uiso 1 1 calc R . . H43B H 0.5895 0.0286 0.1005 0.063 Uiso 1 1 calc R . . H43C H 0.5256 -0.0363 0.0461 0.063 Uiso 1 1 calc R . . C433 C 0.7604(3) -0.00344(19) -0.00469(9) 0.0397(6) Uani 1 1 d . . . H43D H 0.7493 0.0558 -0.0118 0.060 Uiso 1 1 calc R . . H43E H 0.6876 -0.0598 -0.0242 0.060 Uiso 1 1 calc R . . H43F H 0.8530 -0.0111 -0.0136 0.060 Uiso 1 1 calc R . . C434 C 0.8627(3) 0.09586(19) 0.08142(10) 0.0428(6) Uani 1 1 d . . . H43G H 0.8513 0.1534 0.0725 0.064 Uiso 1 1 calc R . . H43H H 0.9552 0.0874 0.0730 0.064 Uiso 1 1 calc R . . H43I H 0.8545 0.1043 0.1172 0.064 Uiso 1 1 calc R . . C44 C 0.7858(2) -0.16921(17) 0.02999(8) 0.0311(5) Uani 1 1 d . . . H44 H 0.7901 -0.1654 -0.0035 0.037 Uiso 1 1 calc R . . C45 C 0.8025(2) -0.25490(17) 0.04028(8) 0.0308(5) Uani 1 1 d . . . C451 C 0.8222(3) -0.34309(18) -0.00087(9) 0.0366(6) Uani 1 1 d . . . C452 C 0.8212(3) -0.3269(2) -0.05399(9) 0.0449(7) Uani 1 1 d . . . H45A H 0.8344 -0.3842 -0.0783 0.067 Uiso 1 1 calc R . . H45B H 0.8974 -0.2696 -0.0549 0.067 Uiso 1 1 calc R . . H45C H 0.7313 -0.3167 -0.0622 0.067 Uiso 1 1 calc R . . C453 C 0.9632(4) -0.3635(3) 0.01019(11) 0.0748(11) Uani 1 1 d . . . H45D H 0.9659 -0.3736 0.0436 0.112 Uiso 1 1 calc R . . H45E H 1.0413 -0.3079 0.0084 0.112 Uiso 1 1 calc R . . H45F H 0.9715 -0.4219 -0.0144 0.112 Uiso 1 1 calc R . . C454 C 0.6971(4) -0.4340(2) -0.00166(12) 0.0752(11) Uani 1 1 d . . . H45G H 0.6937 -0.4465 0.0313 0.113 Uiso 1 1 calc R . . H45H H 0.7102 -0.4907 -0.0264 0.113 Uiso 1 1 calc R . . H45I H 0.6091 -0.4217 -0.0103 0.113 Uiso 1 1 calc R . . C46 C 0.7989(2) -0.25750(18) 0.09096(9) 0.0348(6) Uani 1 1 d . . . H46 H 0.8142 -0.3122 0.0997 0.042 Uiso 1 1 calc R . . C5 C 0.6452(2) -0.18628(18) 0.25977(8) 0.0308(5) Uani 1 1 d . . . H5A H 0.7076 -0.1204 0.2748 0.037 Uiso 1 1 calc R . . H5B H 0.6951 -0.2335 0.2644 0.037 Uiso 1 1 calc R . . C51 C 0.5123(2) -0.19976(17) 0.28890(8) 0.0292(5) Uani 1 1 d . . . C52 C 0.4267(2) -0.13462(16) 0.29291(8) 0.0269(5) Uani 1 1 d . B . O52 O 0.46142(15) -0.06160(11) 0.26911(5) 0.0293(4) Uani 1 1 d . . . C53 C 0.3059(2) -0.14586(17) 0.32250(8) 0.0297(5) Uani 1 1 d . . . C531 C 0.2023(2) -0.08122(18) 0.32535(9) 0.0331(5) Uani 1 1 d . B . C532 C 0.1316(3) -0.0975(2) 0.27219(9) 0.0431(6) Uani 1 1 d . . . H53A H 0.0674 -0.0567 0.2744 0.065 Uiso 1 1 calc R B . H53B H 0.0793 -0.1660 0.2593 0.065 Uiso 1 1 calc R . . H53C H 0.2042 -0.0799 0.2498 0.065 Uiso 1 1 calc R . . C533 C 0.2785(3) 0.02989(19) 0.34608(10) 0.0454(7) Uani 1 1 d . . . H53D H 0.2104 0.0676 0.3472 0.068 Uiso 1 1 calc R B . H53E H 0.3519 0.0496 0.3243 0.068 Uiso 1 1 calc R . . H53F H 0.3208 0.0419 0.3797 0.068 Uiso 1 1 calc R . . C534 C 0.0805(3) -0.1059(2) 0.35936(10) 0.0480(7) Uani 1 1 d . . . H53G H 0.0192 -0.0635 0.3598 0.072 Uiso 1 1 calc R B . H53H H 0.1195 -0.0957 0.3932 0.072 Uiso 1 1 calc R . . H53I H 0.0262 -0.1739 0.3464 0.072 Uiso 1 1 calc R . . C54 C 0.2847(2) -0.21791(17) 0.34910(8) 0.0327(5) Uani 1 1 d . B . H54 H 0.2079 -0.2241 0.3694 0.039 Uiso 1 1 calc R . . C55 C 0.3712(3) -0.28156(17) 0.34732(9) 0.0337(6) Uani 1 1 d . . . C551 C 0.3417(3) -0.35618(19) 0.38002(9) 0.0413(6) Uani 1 1 d . B . C552 C 0.4461(3) -0.4195(2) 0.37151(12) 0.0620(9) Uani 1 1 d . . . H55A H 0.5422 -0.3773 0.3793 0.093 Uiso 1 1 calc R B . H55B H 0.4351 -0.4575 0.3367 0.093 Uiso 1 1 calc R . . H55C H 0.4268 -0.4636 0.3931 0.093 Uiso 1 1 calc R . . C553 C 0.1888(3) -0.4241(2) 0.36768(11) 0.0565(8) Uani 1 1 d . . . H55D H 0.1223 -0.3846 0.3732 0.085 Uiso 1 1 calc R B . H55E H 0.1705 -0.4683 0.3893 0.085 Uiso 1 1 calc R . . H55F H 0.1777 -0.4621 0.3328 0.085 Uiso 1 1 calc R . . C554 C 0.3572(3) -0.2991(2) 0.43620(10) 0.0526(7) Uani 1 1 d . . . H55G H 0.2908 -0.2594 0.4422 0.079 Uiso 1 1 calc R B . H55H H 0.4530 -0.2568 0.4449 0.079 Uiso 1 1 calc R . . H55I H 0.3374 -0.3452 0.4567 0.079 Uiso 1 1 calc R . . C56 C 0.4832(3) -0.27157(17) 0.31580(9) 0.0341(6) Uani 1 1 d . B . H56 H 0.5408 -0.3145 0.3125 0.041 Uiso 1 1 calc R . . C6 C 0.5248(3) -0.29686(18) 0.17915(10) 0.0430(6) Uani 1 1 d . . . H6A H 0.4545 -0.3146 0.2028 0.052 Uiso 0.588(6) 1 calc PR C 1 H6B H 0.5796 -0.3452 0.1730 0.052 Uiso 0.588(6) 1 calc PR C 1 H6C H 0.5640 -0.3250 0.1480 0.052 Uiso 0.412(6) 1 calc PR C 2 H6D H 0.5216 -0.3401 0.2013 0.052 Uiso 0.412(6) 1 calc PR C 2 C61 C 0.4467(5) -0.3059(3) 0.13005(16) 0.0425(14) Uani 0.588(6) 1 d P B 1 H61A H 0.3801 -0.3715 0.1190 0.051 Uiso 0.588(6) 1 calc PR C 1 H61B H 0.5152 -0.2995 0.1045 0.051 Uiso 0.588(6) 1 calc PR C 1 N62 N 0.3658(2) -0.22957(16) 0.13364(8) 0.0417(5) Uani 1 1 d . . . C63 C 0.3404(8) -0.2287(5) 0.0781(2) 0.0559(17) Uani 0.588(6) 1 d P B 1 H63A H 0.4308 -0.2076 0.0644 0.084 Uiso 0.588(6) 1 calc PR C 1 H63B H 0.2845 -0.1837 0.0768 0.084 Uiso 0.588(6) 1 calc PR C 1 H63C H 0.2901 -0.2943 0.0585 0.084 Uiso 0.588(6) 1 calc PR C 1 C64 C 0.2328(8) -0.2555(6) 0.1539(3) 0.0522(17) Uani 0.588(6) 1 d P B 1 H64A H 0.1857 -0.2044 0.1556 0.078 Uiso 0.588(6) 1 calc PR C 1 H64B H 0.2469 -0.2628 0.1873 0.078 Uiso 0.588(6) 1 calc PR C 1 H64C H 0.1748 -0.3171 0.1325 0.078 Uiso 0.588(6) 1 calc PR C 1 C61A C 0.3830(7) -0.2964(5) 0.1674(2) 0.041(2) Uani 0.412(6) 1 d P B 2 H61C H 0.3403 -0.2761 0.1990 0.049 Uiso 0.412(6) 1 calc PR C 2 H61D H 0.3288 -0.3639 0.1507 0.049 Uiso 0.412(6) 1 calc PR C 2 C63A C 0.4032(10) -0.2579(7) 0.0844(3) 0.050(2) Uani 0.412(6) 1 d P B 2 H63D H 0.5040 -0.2519 0.0846 0.076 Uiso 0.412(6) 1 calc PR C 2 H63E H 0.3807 -0.2158 0.0653 0.076 Uiso 0.412(6) 1 calc PR C 2 H63F H 0.3509 -0.3255 0.0690 0.076 Uiso 0.412(6) 1 calc PR C 2 C64A C 0.2038(11) -0.2337(9) 0.1354(4) 0.058(3) Uani 0.412(6) 1 d P B 2 H64D H 0.1822 -0.2116 0.1700 0.087 Uiso 0.412(6) 1 calc PR C 2 H64E H 0.1470 -0.3007 0.1211 0.087 Uiso 0.412(6) 1 calc PR C 2 H64F H 0.1826 -0.1915 0.1162 0.087 Uiso 0.412(6) 1 calc PR C 2 C71 C 0.2060(4) 0.4476(3) 0.21352(16) 0.1022(14) Uani 1 1 d . . . H71A H 0.2958 0.4614 0.1985 0.153 Uiso 1 1 calc R . . H71B H 0.1379 0.3937 0.1903 0.153 Uiso 1 1 calc R . . H71C H 0.2188 0.4297 0.2444 0.153 Uiso 1 1 calc R . . C72 C 0.1522(4) 0.5376(3) 0.22495(13) 0.0798(11) Uani 1 1 d . . . H72A H 0.2205 0.5924 0.2484 0.096 Uiso 1 1 calc R . . H72B H 0.1403 0.5567 0.1940 0.096 Uiso 1 1 calc R . . O73 O 0.0192(2) 0.51550(14) 0.24676(7) 0.0591(5) Uani 1 1 d . . . C74 C -0.0387(4) 0.5982(2) 0.26033(13) 0.0761(11) Uani 1 1 d . . . H74A H -0.0594 0.6174 0.2302 0.091 Uiso 1 1 calc R . . H74B H 0.0298 0.6542 0.2830 0.091 Uiso 1 1 calc R . . C75 C -0.1726(5) 0.5697(3) 0.28602(16) 0.0932(12) Uani 1 1 d . . . H75A H -0.2119 0.6253 0.2960 0.140 Uiso 1 1 calc R . . H75B H -0.1515 0.5499 0.3155 0.140 Uiso 1 1 calc R . . H75C H -0.2408 0.5154 0.2631 0.140 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 Ca1 0.0340(3) 0.0308(3) 0.0228(2) 0.0074(2) 0.00484(19) 0.0105(2) Ca2 0.0345(3) 0.0327(3) 0.0229(2) 0.0066(2) 0.0026(2) 0.0116(2) N1 0.0345(11) 0.0312(11) 0.0222(10) 0.0064(8) 0.0019(8) 0.0122(9) C1 0.0318(13) 0.0392(14) 0.0291(13) 0.0125(11) 0.0032(10) 0.0090(11) C11 0.0302(12) 0.0415(14) 0.0256(12) 0.0117(11) 0.0021(10) 0.0120(11) C12 0.0298(12) 0.0361(14) 0.0275(12) 0.0086(11) -0.0001(10) 0.0125(11) O12 0.0405(10) 0.0377(10) 0.0292(9) 0.0112(8) -0.0042(7) 0.0068(8) C13 0.0297(12) 0.0372(14) 0.0277(13) 0.0113(11) 0.0018(10) 0.0121(11) C131 0.0328(13) 0.0445(15) 0.0279(13) 0.0142(11) 0.0044(10) 0.0108(11) C132 0.0348(14) 0.0629(19) 0.0553(18) 0.0272(15) 0.0105(13) 0.0155(13) C133 0.0426(15) 0.0458(16) 0.0399(15) 0.0190(13) 0.0093(12) 0.0101(12) C134 0.0455(15) 0.0570(18) 0.0371(15) 0.0224(13) 0.0112(12) 0.0149(13) C14 0.0382(14) 0.0501(16) 0.0253(13) 0.0138(12) 0.0012(11) 0.0158(12) C15 0.0350(13) 0.0424(15) 0.0316(14) 0.0109(12) -0.0026(11) 0.0102(12) C151 0.0555(18) 0.0595(19) 0.0347(16) 0.0150(14) -0.0118(13) -0.0065(15) C152 0.092(6) 0.078(6) 0.049(4) -0.016(4) 0.021(4) -0.023(4) C153 0.071(4) 0.071(4) 0.082(4) 0.024(3) -0.043(3) 0.005(3) C154 0.071(4) 0.050(4) 0.051(3) 0.012(3) -0.025(3) -0.012(3) C155 0.107(8) 0.052(6) 0.068(6) -0.007(5) -0.035(5) 0.018(5) C156 0.096(8) 0.068(8) 0.039(5) 0.005(5) -0.026(5) 0.010(6) C157 0.053(6) 0.151(15) 0.045(6) -0.015(8) -0.001(5) -0.026(7) C16 0.0294(13) 0.0392(15) 0.0359(14) 0.0161(12) 0.0014(11) 0.0076(11) C2 0.0319(12) 0.0354(14) 0.0252(12) 0.0110(10) 0.0044(10) 0.0090(11) C21 0.0380(13) 0.0304(13) 0.0233(12) 0.0068(10) 0.0039(10) 0.0146(11) C22 0.0388(13) 0.0293(13) 0.0208(11) 0.0073(10) 0.0076(10) 0.0158(11) O22 0.0343(9) 0.0318(9) 0.0266(8) 0.0123(7) 0.0049(7) 0.0125(7) C23 0.0390(13) 0.0367(14) 0.0233(12) 0.0087(11) 0.0037(10) 0.0186(11) C231 0.0354(13) 0.0502(16) 0.0311(13) 0.0134(12) 0.0035(11) 0.0210(12) C232 0.0455(16) 0.068(2) 0.0384(15) 0.0176(14) 0.0129(12) 0.0298(14) C233 0.0343(14) 0.0548(18) 0.0469(16) 0.0119(14) 0.0044(12) 0.0108(13) C234 0.0442(16) 0.078(2) 0.0508(17) 0.0278(16) 0.0027(13) 0.0280(15) C24 0.0480(15) 0.0423(15) 0.0250(13) 0.0112(11) 0.0031(11) 0.0247(12) C25 0.0499(16) 0.0309(14) 0.0259(13) 0.0096(11) 0.0067(11) 0.0151(12) C251 0.0609(17) 0.0388(15) 0.0302(14) 0.0164(12) 0.0103(12) 0.0207(13) C252 0.073(2) 0.0535(18) 0.0458(17) 0.0295(15) 0.0094(15) 0.0136(16) C253 0.078(2) 0.0529(18) 0.0312(14) 0.0198(13) 0.0098(14) 0.0249(16) C254 0.094(2) 0.0477(18) 0.0451(17) 0.0240(14) 0.0194(16) 0.0366(17) C26 0.0421(14) 0.0321(14) 0.0277(13) 0.0091(11) 0.0076(11) 0.0112(11) C3 0.0430(14) 0.0329(14) 0.0321(13) 0.0066(11) 0.0021(11) 0.0092(11) C31 0.052(3) 0.035(3) 0.032(3) 0.009(2) 0.008(2) 0.019(2) N32 0.0561(14) 0.0387(13) 0.0415(14) 0.0055(11) 0.0191(11) 0.0154(11) C33 0.051(4) 0.051(4) 0.058(4) 0.001(3) 0.016(3) 0.025(3) C34 0.073(5) 0.051(4) 0.040(3) 0.011(3) 0.021(3) 0.026(4) C31A 0.060(4) 0.034(3) 0.031(3) 0.004(3) 0.002(3) 0.020(3) C33A 0.056(6) 0.059(5) 0.075(6) -0.001(5) 0.001(4) 0.028(5) C34A 0.088(7) 0.049(5) 0.043(5) 0.000(4) 0.029(5) 0.021(5) N4 0.0369(11) 0.0325(11) 0.0218(10) 0.0068(8) 0.0043(8) 0.0119(9) C4 0.0409(14) 0.0496(16) 0.0286(13) 0.0135(12) 0.0084(11) 0.0213(12) C41 0.0374(13) 0.0435(15) 0.0263(12) 0.0121(11) 0.0081(10) 0.0180(11) C42 0.0286(12) 0.0370(14) 0.0291(13) 0.0072(11) 0.0079(10) 0.0125(11) O42 0.0452(10) 0.0364(10) 0.0283(9) 0.0053(8) 0.0115(7) 0.0148(8) C43 0.0271(12) 0.0353(14) 0.0274(12) 0.0083(10) 0.0045(10) 0.0107(10) C431 0.0307(12) 0.0340(14) 0.0296(13) 0.0104(11) 0.0052(10) 0.0113(10) C432 0.0383(14) 0.0475(16) 0.0437(15) 0.0141(13) 0.0066(12) 0.0175(12) C433 0.0476(15) 0.0430(15) 0.0364(14) 0.0165(12) 0.0065(12) 0.0199(12) C434 0.0397(14) 0.0440(16) 0.0431(15) 0.0127(13) 0.0066(12) 0.0078(12) C44 0.0326(13) 0.0394(14) 0.0225(12) 0.0090(11) 0.0051(10) 0.0111(11) C45 0.0324(13) 0.0333(14) 0.0284(13) 0.0082(11) 0.0072(10) 0.0117(11) C451 0.0518(15) 0.0375(15) 0.0255(13) 0.0087(11) 0.0095(11) 0.0204(12) C452 0.0645(18) 0.0439(16) 0.0289(14) 0.0066(12) 0.0099(12) 0.0224(14) C453 0.102(3) 0.102(3) 0.0402(17) 0.0038(18) 0.0077(17) 0.076(2) C454 0.124(3) 0.0421(19) 0.0457(19) 0.0101(15) 0.0216(19) 0.0019(19) C46 0.0398(14) 0.0416(15) 0.0312(13) 0.0136(11) 0.0113(11) 0.0212(12) C5 0.0361(13) 0.0371(14) 0.0243(12) 0.0094(10) 0.0052(10) 0.0176(11) C51 0.0319(12) 0.0314(13) 0.0240(12) 0.0078(10) 0.0036(10) 0.0074(10) C52 0.0307(12) 0.0279(13) 0.0211(11) 0.0071(10) 0.0008(9) 0.0060(10) O52 0.0336(9) 0.0304(9) 0.0266(8) 0.0100(7) 0.0060(7) 0.0110(7) C53 0.0296(12) 0.0325(13) 0.0258(12) 0.0074(10) 0.0026(10) 0.0072(10) C531 0.0313(13) 0.0402(14) 0.0298(13) 0.0101(11) 0.0061(10) 0.0124(11) C532 0.0390(14) 0.0555(18) 0.0374(15) 0.0148(13) 0.0001(12) 0.0152(13) C533 0.0420(15) 0.0453(16) 0.0502(17) 0.0056(13) 0.0040(12) 0.0209(13) C534 0.0439(15) 0.0648(19) 0.0453(16) 0.0220(14) 0.0182(13) 0.0244(14) C54 0.0323(13) 0.0374(14) 0.0282(13) 0.0106(11) 0.0066(10) 0.0076(11) C55 0.0392(14) 0.0312(14) 0.0307(13) 0.0107(11) 0.0055(11) 0.0072(11) C551 0.0510(16) 0.0421(16) 0.0362(14) 0.0188(12) 0.0114(12) 0.0139(13) C552 0.083(2) 0.059(2) 0.068(2) 0.0434(17) 0.0275(17) 0.0353(17) C553 0.068(2) 0.0477(18) 0.0542(18) 0.0271(15) 0.0066(15) 0.0032(15) C554 0.0674(19) 0.0569(19) 0.0383(16) 0.0252(14) 0.0072(14) 0.0132(15) C56 0.0400(14) 0.0332(14) 0.0314(13) 0.0087(11) 0.0053(11) 0.0137(11) C6 0.0591(17) 0.0330(15) 0.0361(15) 0.0032(12) 0.0017(13) 0.0168(13) C61 0.051(3) 0.045(3) 0.027(3) 0.001(2) 0.003(2) 0.013(2) N62 0.0415(13) 0.0415(13) 0.0373(12) 0.0062(10) -0.0053(10) 0.0072(10) C63 0.064(4) 0.059(4) 0.035(3) 0.011(3) -0.007(3) 0.002(3) C64 0.048(4) 0.050(4) 0.056(5) 0.009(3) 0.005(3) 0.014(3) C61A 0.044(4) 0.038(4) 0.033(4) 0.004(3) 0.004(3) 0.006(3) C63A 0.064(6) 0.047(5) 0.028(4) 0.002(3) -0.004(4) 0.002(4) C64A 0.045(5) 0.059(7) 0.061(7) 0.001(5) -0.009(5) 0.012(4) C71 0.085(3) 0.112(4) 0.091(3) 0.005(3) 0.031(2) 0.016(3) C72 0.082(3) 0.081(3) 0.053(2) 0.0193(19) 0.0031(18) -0.020(2) O73 0.0746(14) 0.0442(12) 0.0510(12) 0.0138(10) 0.0030(11) 0.0029(11) C74 0.118(3) 0.0419(19) 0.066(2) 0.0140(17) -0.016(2) 0.018(2) C75 0.112(3) 0.086(3) 0.096(3) 0.022(2) 0.012(3) 0.055(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 Ca1 O12 2.1817(16) . ? Ca1 O22 2.2488(15) . ? Ca1 O52 2.3170(16) . ? Ca1 N1 2.5115(19) . ? Ca1 N32 2.551(2) . ? Ca1 Ca2 3.4653(6) . ? Ca2 O42 2.1842(16) . ? Ca2 O52 2.2682(15) . ? Ca2 O22 2.2904(15) . ? Ca2 N4 2.4981(19) . ? Ca2 N62 2.552(2) . ? N1 C3 1.479(3) . ? N1 C1 1.498(3) . ? N1 C2 1.498(3) . ? C1 C11 1.507(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C11 C16 1.388(3) . ? C11 C12 1.411(3) . ? C12 O12 1.328(3) . ? C12 C13 1.425(3) . ? C13 C14 1.389(3) . ? C13 C131 1.538(3) . ? C131 C134 1.530(3) . ? C131 C133 1.532(3) . ? C131 C132 1.540(3) . ? C132 H13A 0.9600 . ? C132 H13B 0.9600 . ? C132 H13C 0.9600 . ? C133 H13D 0.9600 . ? C133 H13E 0.9600 . ? C133 H13F 0.9600 . ? C134 H13G 0.9600 . ? C134 H13H 0.9600 . ? C134 H13I 0.9600 . ? C14 C15 1.394(3) . ? C14 H14 0.9300 . ? C15 C16 1.390(3) . ? C15 C151 1.529(4) . ? C151 C157 1.331(9) . ? C151 C152 1.404(7) . ? C151 C154 1.532(6) . ? C151 C156 1.606(10) . ? C151 C153 1.630(6) . ? C151 C155 1.731(9) . ? C152 H15A 0.9600 . ? C152 H15B 0.9600 . ? C152 H15C 0.9600 . ? C153 H15D 0.9600 . ? C153 H15E 0.9600 . ? C153 H15F 0.9600 . ? C154 H15G 0.9600 . ? C154 H15H 0.9600 . ? C154 H15I 0.9600 . ? C155 H15J 0.9600 . ? C155 H15K 0.9600 . ? C155 H15L 0.9600 . ? C156 H15M 0.9600 . ? C156 H15N 0.9600 . ? C156 H15O 0.9600 . ? C157 H15P 0.9600 . ? C157 H15Q 0.9600 . ? C157 H15R 0.9600 . ? C16 H16 0.9300 . ? C2 C21 1.511(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C21 C26 1.394(3) . ? C21 C22 1.404(3) . ? C22 O22 1.345(3) . ? C22 C23 1.418(3) . ? C23 C24 1.389(3) . ? C23 C231 1.535(3) . ? C231 C234 1.532(3) . ? C231 C232 1.535(3) . ? C231 C233 1.536(4) . ? C232 H23A 0.9600 . ? C232 H23B 0.9600 . ? C232 H23C 0.9600 . ? C233 H23D 0.9600 . ? C233 H23E 0.9600 . ? C233 H23F 0.9600 . ? C234 H23G 0.9600 . ? C234 H23H 0.9600 . ? C234 H23I 0.9600 . ? C24 C25 1.394(3) . ? C24 H24 0.9300 . ? C25 C26 1.383(3) . ? C25 C251 1.537(3) . ? C251 C252 1.522(4) . ? C251 C254 1.532(4) . ? C251 C253 1.543(3) . ? C252 H25A 0.9600 . ? C252 H25B 0.9600 . ? C252 H25C 0.9600 . ? C253 H25D 0.9600 . ? C253 H25E 0.9600 . ? C253 H25F 0.9600 . ? C254 H25G 0.9600 . ? C254 H25H 0.9600 . ? C254 H25I 0.9600 . ? C26 H26 0.9300 . ? C3 C31A 1.473(6) . ? C3 C31 1.521(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C31 N32 1.512(5) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? N32 C33A 1.315(8) . ? N32 C34 1.374(7) . ? N32 C34A 1.563(8) . ? N32 C33 1.567(6) . ? N32 C31A 1.574(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C31A H31C 0.9700 . ? C31A H31D 0.9700 . ? C33A H33D 0.9600 . ? C33A H33E 0.9600 . ? C33A H33F 0.9600 . ? C34A H34D 0.9600 . ? C34A H34E 0.9600 . ? C34A H34F 0.9600 . ? N4 C6 1.478(3) . ? N4 C4 1.497(3) . ? N4 C5 1.499(3) . ? C4 C41 1.514(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C41 C46 1.389(3) . ? C41 C42 1.417(3) . ? C42 O42 1.325(3) . ? C42 C43 1.425(3) . ? C43 C44 1.401(3) . ? C43 C431 1.531(3) . ? C431 C434 1.531(3) . ? C431 C432 1.533(3) . ? C431 C433 1.536(3) . ? C432 H43A 0.9600 . ? C432 H43B 0.9600 . ? C432 H43C 0.9600 . ? C433 H43D 0.9600 . ? C433 H43E 0.9600 . ? C433 H43F 0.9600 . ? C434 H43G 0.9600 . ? C434 H43H 0.9600 . ? C434 H43I 0.9600 . ? C44 C45 1.390(3) . ? C44 H44 0.9300 . ? C45 C46 1.394(3) . ? C45 C451 1.528(3) . ? C451 C453 1.522(4) . ? C451 C452 1.528(3) . ? C451 C454 1.533(4) . ? C452 H45A 0.9600 . ? C452 H45B 0.9600 . ? C452 H45C 0.9600 . ? C453 H45D 0.9600 . ? C453 H45E 0.9600 . ? C453 H45F 0.9600 . ? C454 H45G 0.9600 . ? C454 H45H 0.9600 . ? C454 H45I 0.9600 . ? C46 H46 0.9300 . ? C5 C51 1.512(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C51 C56 1.391(3) . ? C51 C52 1.401(3) . ? C52 O52 1.348(3) . ? C52 C53 1.423(3) . ? C53 C54 1.390(3) . ? C53 C531 1.537(3) . ? C531 C534 1.529(3) . ? C531 C533 1.538(3) . ? C531 C532 1.540(3) . ? C532 H53A 0.9600 . ? C532 H53B 0.9600 . ? C532 H53C 0.9600 . ? C533 H53D 0.9600 . ? C533 H53E 0.9600 . ? C533 H53F 0.9600 . ? C534 H53G 0.9600 . ? C534 H53H 0.9600 . ? C534 H53I 0.9600 . ? C54 C55 1.396(3) . ? C54 H54 0.9300 . ? C55 C56 1.388(3) . ? C55 C551 1.541(3) . ? C551 C552 1.520(4) . ? C551 C553 1.531(4) . ? C551 C554 1.533(4) . ? C552 H55A 0.9600 . ? C552 H55B 0.9600 . ? C552 H55C 0.9600 . ? C553 H55D 0.9600 . ? C553 H55E 0.9600 . ? C553 H55F 0.9600 . ? C554 H55G 0.9600 . ? C554 H55H 0.9600 . ? C554 H55I 0.9600 . ? C56 H56 0.9300 . ? C6 C61A 1.417(7) . ? C6 C61 1.499(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C61 N62 1.503(5) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? N62 C63A 1.382(8) . ? N62 C64 1.402(8) . ? N62 C61A 1.534(7) . ? N62 C63 1.540(6) . ? N62 C64A 1.560(11) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C61A H61C 0.9700 . ? C61A H61D 0.9700 . ? C63A H63D 0.9600 . ? C63A H63E 0.9600 . ? C63A H63F 0.9600 . ? C64A H64D 0.9600 . ? C64A H64E 0.9600 . ? C64A H64F 0.9600 . ? C71 C72 1.492(5) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 O73 1.417(4) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? O73 C74 1.423(4) . ? C74 C75 1.490(5) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? 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 O12 Ca1 O22 134.13(6) . . ? O12 Ca1 O52 92.05(6) . . ? O22 Ca1 O52 72.56(5) . . ? O12 Ca1 N1 82.74(6) . . ? O22 Ca1 N1 80.37(6) . . ? O52 Ca1 N1 136.32(6) . . ? O12 Ca1 N32 112.01(7) . . ? O22 Ca1 N32 102.84(7) . . ? O52 Ca1 N32 146.39(7) . . ? N1 Ca1 N32 72.32(6) . . ? O12 Ca1 Ca2 101.25(4) . . ? O22 Ca1 Ca2 40.68(4) . . ? O52 Ca1 Ca2 40.38(4) . . ? N1 Ca1 Ca2 98.06(4) . . ? N32 Ca1 Ca2 143.38(6) . . ? O42 Ca2 O52 134.39(6) . . ? O42 Ca2 O22 92.73(6) . . ? O52 Ca2 O22 72.71(5) . . ? O42 Ca2 N4 82.46(6) . . ? O52 Ca2 N4 80.13(6) . . ? O22 Ca2 N4 136.43(6) . . ? O42 Ca2 N62 109.52(6) . . ? O52 Ca2 N62 105.19(6) . . ? O22 Ca2 N62 146.34(6) . . ? N4 Ca2 N62 73.28(7) . . ? O42 Ca2 Ca1 101.33(4) . . ? O52 Ca2 Ca1 41.44(4) . . ? O22 Ca2 Ca1 39.79(4) . . ? N4 Ca2 Ca1 98.59(4) . . ? N62 Ca2 Ca1 146.41(5) . . ? C3 N1 C1 110.80(18) . . ? C3 N1 C2 110.71(17) . . ? C1 N1 C2 106.83(16) . . ? C3 N1 Ca1 111.34(13) . . ? C1 N1 Ca1 107.34(13) . . ? C2 N1 Ca1 109.67(13) . . ? N1 C1 C11 115.23(18) . . ? N1 C1 H1A 108.5 . . ? C11 C1 H1A 108.5 . . ? N1 C1 H1B 108.5 . . ? C11 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C16 C11 C12 120.7(2) . . ? C16 C11 C1 120.8(2) . . ? C12 C11 C1 118.5(2) . . ? O12 C12 C11 119.0(2) . . ? O12 C12 C13 122.3(2) . . ? C11 C12 C13 118.6(2) . . ? C12 O12 Ca1 116.30(14) . . ? C14 C13 C12 117.6(2) . . ? C14 C13 C131 121.7(2) . . ? C12 C13 C131 120.7(2) . . ? C134 C131 C133 107.0(2) . . ? C134 C131 C13 112.7(2) . . ? C133 C131 C13 110.99(18) . . ? C134 C131 C132 107.3(2) . . ? C133 C131 C132 108.7(2) . . ? C13 C131 C132 109.9(2) . . ? C131 C132 H13A 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C131 C133 H13D 109.5 . . ? C131 C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? H13D C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? C131 C134 H13G 109.5 . . ? C131 C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? C131 C134 H13I 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? C13 C14 C15 124.7(2) . . ? C13 C14 H14 117.6 . . ? C15 C14 H14 117.6 . . ? C16 C15 C14 116.3(2) . . ? C16 C15 C151 122.4(2) . . ? C14 C15 C151 121.3(2) . . ? C157 C151 C152 127.1(5) . . ? C157 C151 C15 119.1(5) . . ? C152 C151 C15 113.9(4) . . ? C157 C151 C154 44.2(7) . . ? C152 C151 C154 114.2(5) . . ? C15 C151 C154 112.2(3) . . ? C157 C151 C156 114.5(7) . . ? C152 C151 C156 37.4(5) . . ? C15 C151 C156 113.0(4) . . ? C154 C151 C156 134.3(5) . . ? C157 C151 C153 58.6(8) . . ? C152 C151 C153 108.5(5) . . ? C15 C151 C153 104.0(3) . . ? C154 C151 C153 102.8(4) . . ? C156 C151 C153 72.9(5) . . ? C157 C151 C155 108.2(8) . . ? C152 C151 C155 59.2(5) . . ? C15 C151 C155 102.1(3) . . ? C154 C151 C155 67.2(5) . . ? C156 C151 C155 96.4(6) . . ? C153 C151 C155 153.9(4) . . ? C151 C152 H15A 109.5 . . ? C151 C152 H15B 109.5 . . ? H15A C152 H15B 109.5 . . ? C151 C152 H15C 109.5 . . ? H15A C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? C151 C153 H15D 109.5 . . ? C151 C153 H15E 109.5 . . ? H15D C153 H15E 109.5 . . ? C151 C153 H15F 109.5 . . ? H15D C153 H15F 109.5 . . ? H15E C153 H15F 109.5 . . ? C151 C154 H15G 109.5 . . ? C151 C154 H15H 109.5 . . ? H15G C154 H15H 109.5 . . ? C151 C154 H15I 109.5 . . ? H15G C154 H15I 109.5 . . ? H15H C154 H15I 109.5 . . ? C151 C155 H15J 109.5 . . ? C151 C155 H15K 109.5 . . ? H15J C155 H15K 109.5 . . ? C151 C155 H15L 109.5 . . ? H15J C155 H15L 109.5 . . ? H15K C155 H15L 109.5 . . ? C151 C156 H15M 109.5 . . ? C151 C156 H15N 109.5 . . ? H15M C156 H15N 109.5 . . ? C151 C156 H15O 109.5 . . ? H15M C156 H15O 109.5 . . ? H15N C156 H15O 109.5 . . ? C151 C157 H15P 109.5 . . ? C151 C157 H15Q 109.5 . . ? H15P C157 H15Q 109.5 . . ? C151 C157 H15R 109.5 . . ? H15P C157 H15R 109.5 . . ? H15Q C157 H15R 109.5 . . ? C11 C16 C15 122.0(2) . . ? C11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? N1 C2 C21 116.79(18) . . ? N1 C2 H2A 108.1 . . ? C21 C2 H2A 108.1 . . ? N1 C2 H2B 108.1 . . ? C21 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C26 C21 C22 119.9(2) . . ? C26 C21 C2 119.3(2) . . ? C22 C21 C2 120.5(2) . . ? O22 C22 C21 119.19(19) . . ? O22 C22 C23 121.3(2) . . ? C21 C22 C23 119.5(2) . . ? C22 O22 Ca1 130.73(13) . . ? C22 O22 Ca2 121.35(12) . . ? Ca1 O22 Ca2 99.53(6) . . ? C24 C23 C22 117.7(2) . . ? C24 C23 C231 120.7(2) . . ? C22 C23 C231 121.6(2) . . ? C234 C231 C23 112.3(2) . . ? C234 C231 C232 106.6(2) . . ? C23 C231 C232 110.2(2) . . ? C234 C231 C233 106.6(2) . . ? C23 C231 C233 112.23(19) . . ? C232 C231 C233 108.7(2) . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C231 C233 H23D 109.5 . . ? C231 C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? H23D C233 H23F 109.5 . . ? H23E C233 H23F 109.5 . . ? C231 C234 H23G 109.5 . . ? C231 C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C231 C234 H23I 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C23 C24 C25 123.8(2) . . ? C23 C24 H24 118.1 . . ? C25 C24 H24 118.1 . . ? C26 C25 C24 117.1(2) . . ? C26 C25 C251 123.8(2) . . ? C24 C25 C251 119.1(2) . . ? C252 C251 C254 108.9(2) . . ? C252 C251 C25 112.0(2) . . ? C254 C251 C25 109.5(2) . . ? C252 C251 C253 108.0(2) . . ? C254 C251 C253 109.1(2) . . ? C25 C251 C253 109.3(2) . . ? C251 C252 H25A 109.5 . . ? C251 C252 H25B 109.5 . . ? H25A C252 H25B 109.5 . . ? C251 C252 H25C 109.5 . . ? H25A C252 H25C 109.5 . . ? H25B C252 H25C 109.5 . . ? C251 C253 H25D 109.5 . . ? C251 C253 H25E 109.5 . . ? H25D C253 H25E 109.5 . . ? C251 C253 H25F 109.5 . . ? H25D C253 H25F 109.5 . . ? H25E C253 H25F 109.5 . . ? C251 C254 H25G 109.5 . . ? C251 C254 H25H 109.5 . . ? H25G C254 H25H 109.5 . . ? C251 C254 H25I 109.5 . . ? H25G C254 H25I 109.5 . . ? H25H C254 H25I 109.5 . . ? C25 C26 C21 121.9(2) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? C31A C3 N1 114.3(3) . . ? C31A C3 C31 53.2(3) . . ? N1 C3 C31 113.4(2) . . ? C31A C3 H3A 136.8 . . ? N1 C3 H3A 108.9 . . ? C31 C3 H3A 108.9 . . ? C31A C3 H3B 58.2 . . ? N1 C3 H3B 108.9 . . ? C31 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C31A C3 H3C 108.7 . . ? N1 C3 H3C 108.7 . . ? C31 C3 H3C 138.0 . . ? H3A C3 H3C 55.0 . . ? H3B C3 H3C 55.4 . . ? C31A C3 H3D 108.7 . . ? N1 C3 H3D 108.7 . . ? C31 C3 H3D 58.5 . . ? H3A C3 H3D 55.0 . . ? H3B C3 H3D 142.2 . . ? H3C C3 H3D 107.6 . . ? N32 C31 C3 111.7(3) . . ? N32 C31 H31A 109.3 . . ? C3 C31 H31A 109.3 . . ? N32 C31 H31B 109.3 . . ? C3 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C33A N32 C34 128.9(5) . . ? C33A N32 C31 68.6(5) . . ? C34 N32 C31 115.7(4) . . ? C33A N32 C34A 112.7(6) . . ? C34 N32 C34A 31.6(4) . . ? C31 N32 C34A 141.5(4) . . ? C33A N32 C33 34.6(4) . . ? C34 N32 C33 109.0(4) . . ? C31 N32 C33 102.8(3) . . ? C34A N32 C33 82.8(4) . . ? C33A N32 C31A 113.8(5) . . ? C34 N32 C31A 68.6(4) . . ? C31 N32 C31A 51.5(3) . . ? C34A N32 C31A 99.9(5) . . ? C33 N32 C31A 139.3(4) . . ? C33A N32 Ca1 113.3(4) . . ? C34 N32 Ca1 114.8(3) . . ? C31 N32 Ca1 102.33(19) . . ? C34A N32 Ca1 110.9(3) . . ? C33 N32 Ca1 111.6(2) . . ? C31A N32 Ca1 105.2(2) . . ? N32 C33 H33A 109.5 . . ? N32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C3 C31A N32 110.9(4) . . ? C3 C31A H31C 109.5 . . ? N32 C31A H31C 109.5 . . ? C3 C31A H31D 109.5 . . ? N32 C31A H31D 109.5 . . ? H31C C31A H31D 108.0 . . ? N32 C33A H33D 109.5 . . ? N32 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? N32 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? N32 C34A H34D 109.5 . . ? N32 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? N32 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C6 N4 C4 111.50(18) . . ? C6 N4 C5 110.61(18) . . ? C4 N4 C5 106.49(16) . . ? C6 N4 Ca2 109.70(14) . . ? C4 N4 Ca2 108.30(13) . . ? C5 N4 Ca2 110.17(13) . . ? N4 C4 C41 115.28(19) . . ? N4 C4 H4A 108.5 . . ? C41 C4 H4A 108.5 . . ? N4 C4 H4B 108.5 . . ? C41 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C46 C41 C42 120.8(2) . . ? C46 C41 C4 120.9(2) . . ? C42 C41 C4 118.3(2) . . ? O42 C42 C41 119.0(2) . . ? O42 C42 C43 122.5(2) . . ? C41 C42 C43 118.6(2) . . ? C42 O42 Ca2 116.48(14) . . ? C44 C43 C42 117.5(2) . . ? C44 C43 C431 121.7(2) . . ? C42 C43 C431 120.8(2) . . ? C43 C431 C434 109.91(19) . . ? C43 C431 C432 110.72(19) . . ? C434 C431 C432 108.75(19) . . ? C43 C431 C433 112.45(19) . . ? C434 C431 C433 107.34(19) . . ? C432 C431 C433 107.52(19) . . ? C431 C432 H43A 109.5 . . ? C431 C432 H43B 109.5 . . ? H43A C432 H43B 109.5 . . ? C431 C432 H43C 109.5 . . ? H43A C432 H43C 109.5 . . ? H43B C432 H43C 109.5 . . ? C431 C433 H43D 109.5 . . ? C431 C433 H43E 109.5 . . ? H43D C433 H43E 109.5 . . ? C431 C433 H43F 109.5 . . ? H43D C433 H43F 109.5 . . ? H43E C433 H43F 109.5 . . ? C431 C434 H43G 109.5 . . ? C431 C434 H43H 109.5 . . ? H43G C434 H43H 109.5 . . ? C431 C434 H43I 109.5 . . ? H43G C434 H43I 109.5 . . ? H43H C434 H43I 109.5 . . ? C45 C44 C43 124.8(2) . . ? C45 C44 H44 117.6 . . ? C43 C44 H44 117.6 . . ? C44 C45 C46 116.3(2) . . ? C44 C45 C451 123.0(2) . . ? C46 C45 C451 120.6(2) . . ? C453 C451 C452 108.3(2) . . ? C453 C451 C45 110.0(2) . . ? C452 C451 C45 112.9(2) . . ? C453 C451 C454 110.0(3) . . ? C452 C451 C454 106.9(2) . . ? C45 C451 C454 108.5(2) . . ? C451 C452 H45A 109.5 . . ? C451 C452 H45B 109.5 . . ? H45A C452 H45B 109.5 . . ? C451 C452 H45C 109.5 . . ? H45A C452 H45C 109.5 . . ? H45B C452 H45C 109.5 . . ? C451 C453 H45D 109.5 . . ? C451 C453 H45E 109.5 . . ? H45D C453 H45E 109.5 . . ? C451 C453 H45F 109.5 . . ? H45D C453 H45F 109.5 . . ? H45E C453 H45F 109.5 . . ? C451 C454 H45G 109.5 . . ? C451 C454 H45H 109.5 . . ? H45G C454 H45H 109.5 . . ? C451 C454 H45I 109.5 . . ? H45G C454 H45I 109.5 . . ? H45H C454 H45I 109.5 . . ? C41 C46 C45 122.0(2) . . ? C41 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? N4 C5 C51 116.57(18) . . ? N4 C5 H5A 108.1 . . ? C51 C5 H5A 108.1 . . ? N4 C5 H5B 108.1 . . ? C51 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C56 C51 C52 119.9(2) . . ? C56 C51 C5 119.3(2) . . ? C52 C51 C5 120.5(2) . . ? O52 C52 C51 119.23(19) . . ? O52 C52 C53 121.2(2) . . ? C51 C52 C53 119.5(2) . . ? C52 O52 Ca2 130.66(13) . . ? C52 O52 Ca1 122.50(13) . . ? Ca2 O52 Ca1 98.18(6) . . ? C54 C53 C52 117.4(2) . . ? C54 C53 C531 120.8(2) . . ? C52 C53 C531 121.8(2) . . ? C534 C531 C53 112.9(2) . . ? C534 C531 C533 106.8(2) . . ? C53 C531 C533 112.05(19) . . ? C534 C531 C532 106.5(2) . . ? C53 C531 C532 110.10(19) . . ? C533 C531 C532 108.2(2) . . ? C531 C532 H53A 109.5 . . ? C531 C532 H53B 109.5 . . ? H53A C532 H53B 109.5 . . ? C531 C532 H53C 109.5 . . ? H53A C532 H53C 109.5 . . ? H53B C532 H53C 109.5 . . ? C531 C533 H53D 109.5 . . ? C531 C533 H53E 109.5 . . ? H53D C533 H53E 109.5 . . ? C531 C533 H53F 109.5 . . ? H53D C533 H53F 109.5 . . ? H53E C533 H53F 109.5 . . ? C531 C534 H53G 109.5 . . ? C531 C534 H53H 109.5 . . ? H53G C534 H53H 109.5 . . ? C531 C534 H53I 109.5 . . ? H53G C534 H53I 109.5 . . ? H53H C534 H53I 109.5 . . ? C53 C54 C55 124.3(2) . . ? C53 C54 H54 117.8 . . ? C55 C54 H54 117.8 . . ? C56 C55 C54 116.3(2) . . ? C56 C55 C551 123.6(2) . . ? C54 C55 C551 120.1(2) . . ? C552 C551 C553 109.0(2) . . ? C552 C551 C554 108.7(2) . . ? C553 C551 C554 108.2(2) . . ? C552 C551 C55 111.5(2) . . ? C553 C551 C55 110.3(2) . . ? C554 C551 C55 109.1(2) . . ? C551 C552 H55A 109.5 . . ? C551 C552 H55B 109.5 . . ? H55A C552 H55B 109.5 . . ? C551 C552 H55C 109.5 . . ? H55A C552 H55C 109.5 . . ? H55B C552 H55C 109.5 . . ? C551 C553 H55D 109.5 . . ? C551 C553 H55E 109.5 . . ? H55D C553 H55E 109.5 . . ? C551 C553 H55F 109.5 . . ? H55D C553 H55F 109.5 . . ? H55E C553 H55F 109.5 . . ? C551 C554 H55G 109.5 . . ? C551 C554 H55H 109.5 . . ? H55G C554 H55H 109.5 . . ? C551 C554 H55I 109.5 . . ? H55G C554 H55I 109.5 . . ? H55H C554 H55I 109.5 . . ? C55 C56 C51 122.4(2) . . ? C55 C56 H56 118.8 . . ? C51 C56 H56 118.8 . . ? C61A C6 N4 115.0(3) . . ? C61A C6 C61 48.1(3) . . ? N4 C6 C61 116.5(3) . . ? C61A C6 H6A 63.2 . . ? N4 C6 H6A 108.2 . . ? C61 C6 H6A 108.2 . . ? C61A C6 H6B 136.6 . . ? N4 C6 H6B 108.2 . . ? C61 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C61A C6 H6C 108.5 . . ? N4 C6 H6C 108.5 . . ? C61 C6 H6C 62.6 . . ? H6A C6 H6C 142.0 . . ? H6B C6 H6C 51.1 . . ? C61A C6 H6D 108.5 . . ? N4 C6 H6D 108.5 . . ? C61 C6 H6D 134.8 . . ? H6A C6 H6D 50.5 . . ? H6B C6 H6D 59.0 . . ? H6C C6 H6D 107.5 . . ? C6 C61 N62 113.4(3) . . ? C6 C61 H61A 108.9 . . ? N62 C61 H61A 108.9 . . ? C6 C61 H61B 108.9 . . ? N62 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C63A N62 C64 129.7(5) . . ? C63A N62 C61 71.0(5) . . ? C64 N62 C61 112.6(4) . . ? C63A N62 C61A 115.2(5) . . ? C64 N62 C61A 74.7(4) . . ? C61 N62 C61A 46.1(3) . . ? C63A N62 C63 34.0(4) . . ? C64 N62 C63 108.7(4) . . ? C61 N62 C63 104.0(3) . . ? C61A N62 C63 143.1(4) . . ? C63A N62 C64A 111.7(6) . . ? C64 N62 C64A 28.7(4) . . ? C61 N62 C64A 133.5(5) . . ? C61A N62 C64A 102.9(5) . . ? C63 N62 C64A 83.1(5) . . ? C63A N62 Ca2 115.8(4) . . ? C64 N62 Ca2 110.6(3) . . ? C61 N62 Ca2 107.35(19) . . ? C61A N62 Ca2 98.3(2) . . ? C63 N62 Ca2 113.4(3) . . ? C64A N62 Ca2 111.6(4) . . ? N62 C63 H63A 109.5 . . ? N62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N62 C64 H64A 109.5 . . ? N62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C6 C61A N62 116.4(4) . . ? C6 C61A H61C 108.2 . . ? N62 C61A H61C 108.2 . . ? C6 C61A H61D 108.2 . . ? N62 C61A H61D 108.2 . . ? H61C C61A H61D 107.3 . . ? N62 C63A H63D 109.5 . . ? N62 C63A H63E 109.5 . . ? H63D C63A H63E 109.5 . . ? N62 C63A H63F 109.5 . . ? H63D C63A H63F 109.5 . . ? H63E C63A H63F 109.5 . . ? N62 C64A H64D 109.5 . . ? N62 C64A H64E 109.5 . . ? H64D C64A H64E 109.5 . . ? N62 C64A H64F 109.5 . . ? H64D C64A H64F 109.5 . . ? H64E C64A H64F 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O73 C72 C71 108.6(3) . . ? O73 C72 H72A 110.0 . . ? C71 C72 H72A 110.0 . . ? O73 C72 H72B 110.0 . . ? C71 C72 H72B 110.0 . . ? H72A C72 H72B 108.3 . . ? C72 O73 C74 112.7(3) . . ? O73 C74 C75 108.6(3) . . ? O73 C74 H74A 110.0 . . ? C75 C74 H74A 110.0 . . ? O73 C74 H74B 110.0 . . ? C75 C74 H74B 110.0 . . ? H74A C74 H74B 108.4 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Ca1 Ca2 O42 -68.54(6) . . . . ? O22 Ca1 Ca2 O42 80.52(7) . . . . ? O52 Ca1 Ca2 O42 -148.31(7) . . . . ? N1 Ca1 Ca2 O42 15.61(6) . . . . ? N32 Ca1 Ca2 O42 86.72(10) . . . . ? O12 Ca1 Ca2 O52 79.77(7) . . . . ? O22 Ca1 Ca2 O52 -131.17(8) . . . . ? N1 Ca1 Ca2 O52 163.92(7) . . . . ? N32 Ca1 Ca2 O52 -124.97(10) . . . . ? O12 Ca1 Ca2 O22 -149.05(7) . . . . ? O52 Ca1 Ca2 O22 131.17(8) . . . . ? N1 Ca1 Ca2 O22 -64.91(7) . . . . ? N32 Ca1 Ca2 O22 6.21(10) . . . . ? O12 Ca1 Ca2 N4 15.43(6) . . . . ? O22 Ca1 Ca2 N4 164.49(7) . . . . ? O52 Ca1 Ca2 N4 -64.34(7) . . . . ? N1 Ca1 Ca2 N4 99.58(6) . . . . ? N32 Ca1 Ca2 N4 170.69(10) . . . . ? O12 Ca1 Ca2 N62 88.06(10) . . . . ? O22 Ca1 Ca2 N62 -122.88(11) . . . . ? O52 Ca1 Ca2 N62 8.29(11) . . . . ? N1 Ca1 Ca2 N62 172.21(10) . . . . ? N32 Ca1 Ca2 N62 -116.68(12) . . . . ? O12 Ca1 N1 C3 -120.31(14) . . . . ? O22 Ca1 N1 C3 102.51(14) . . . . ? O52 Ca1 N1 C3 154.35(13) . . . . ? N32 Ca1 N1 C3 -4.39(14) . . . . ? Ca2 Ca1 N1 C3 139.29(13) . . . . ? O12 Ca1 N1 C1 1.12(13) . . . . ? O22 Ca1 N1 C1 -136.06(13) . . . . ? O52 Ca1 N1 C1 -84.22(15) . . . . ? N32 Ca1 N1 C1 117.04(14) . . . . ? Ca2 Ca1 N1 C1 -99.28(12) . . . . ? O12 Ca1 N1 C2 116.82(14) . . . . ? O22 Ca1 N1 C2 -20.37(13) . . . . ? O52 Ca1 N1 C2 31.48(17) . . . . ? N32 Ca1 N1 C2 -127.26(15) . . . . ? Ca2 Ca1 N1 C2 16.42(13) . . . . ? C3 N1 C1 C11 67.9(2) . . . . ? C2 N1 C1 C11 -171.47(19) . . . . ? Ca1 N1 C1 C11 -53.9(2) . . . . ? N1 C1 C11 C16 -109.5(2) . . . . ? N1 C1 C11 C12 71.9(3) . . . . ? C16 C11 C12 O12 177.8(2) . . . . ? C1 C11 C12 O12 -3.5(3) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? C1 C11 C12 C13 178.1(2) . . . . ? C11 C12 O12 Ca1 -63.8(2) . . . . ? C13 C12 O12 Ca1 114.5(2) . . . . ? O22 Ca1 O12 C12 124.41(15) . . . . ? O52 Ca1 O12 C12 -168.11(15) . . . . ? N1 Ca1 O12 C12 55.43(15) . . . . ? N32 Ca1 O12 C12 -12.13(16) . . . . ? Ca2 Ca1 O12 C12 152.25(14) . . . . ? O12 C12 C13 C14 -177.1(2) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? O12 C12 C13 C131 1.1(3) . . . . ? C11 C12 C13 C131 179.4(2) . . . . ? C14 C13 C131 C134 -3.2(3) . . . . ? C12 C13 C131 C134 178.7(2) . . . . ? C14 C13 C131 C133 -123.2(2) . . . . ? C12 C13 C131 C133 58.7(3) . . . . ? C14 C13 C131 C132 116.5(2) . . . . ? C12 C13 C131 C132 -61.6(3) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C131 C13 C14 C15 -178.3(2) . . . . ? C13 C14 C15 C16 -1.7(4) . . . . ? C13 C14 C15 C151 178.2(2) . . . . ? C16 C15 C151 C157 -44.6(10) . . . . ? C14 C15 C151 C157 135.5(9) . . . . ? C16 C15 C151 C152 135.8(5) . . . . ? C14 C15 C151 C152 -44.1(6) . . . . ? C16 C15 C151 C154 4.2(5) . . . . ? C14 C15 C151 C154 -175.7(4) . . . . ? C16 C15 C151 C156 176.7(5) . . . . ? C14 C15 C151 C156 -3.2(6) . . . . ? C16 C15 C151 C153 -106.2(4) . . . . ? C14 C15 C151 C153 73.9(4) . . . . ? C16 C15 C151 C155 74.3(5) . . . . ? C14 C15 C151 C155 -105.6(4) . . . . ? C12 C11 C16 C15 -1.4(4) . . . . ? C1 C11 C16 C15 -180.0(2) . . . . ? C14 C15 C16 C11 2.4(3) . . . . ? C151 C15 C16 C11 -177.5(2) . . . . ? C3 N1 C2 C21 -58.7(2) . . . . ? C1 N1 C2 C21 -179.40(19) . . . . ? Ca1 N1 C2 C21 64.6(2) . . . . ? N1 C2 C21 C26 122.1(2) . . . . ? N1 C2 C21 C22 -64.2(3) . . . . ? C26 C21 C22 O22 175.78(19) . . . . ? C2 C21 C22 O22 2.1(3) . . . . ? C26 C21 C22 C23 -3.4(3) . . . . ? C2 C21 C22 C23 -177.11(19) . . . . ? C21 C22 O22 Ca1 47.5(3) . . . . ? C23 C22 O22 Ca1 -133.28(18) . . . . ? C21 C22 O22 Ca2 -93.8(2) . . . . ? C23 C22 O22 Ca2 85.4(2) . . . . ? O12 Ca1 O22 C22 -102.58(18) . . . . ? O52 Ca1 O22 C22 -177.96(18) . . . . ? N1 Ca1 O22 C22 -32.65(17) . . . . ? N32 Ca1 O22 C22 36.57(18) . . . . ? Ca2 Ca1 O22 C22 -147.22(19) . . . . ? O12 Ca1 O22 Ca2 44.64(10) . . . . ? O52 Ca1 O22 Ca2 -30.74(5) . . . . ? N1 Ca1 O22 Ca2 114.57(6) . . . . ? N32 Ca1 O22 Ca2 -176.21(6) . . . . ? O42 Ca2 O22 C22 46.80(16) . . . . ? O52 Ca2 O22 C22 -177.26(16) . . . . ? N4 Ca2 O22 C22 128.72(15) . . . . ? N62 Ca2 O22 C22 -85.67(19) . . . . ? Ca1 Ca2 O22 C22 151.29(18) . . . . ? O42 Ca2 O22 Ca1 -104.49(6) . . . . ? O52 Ca2 O22 Ca1 31.45(5) . . . . ? N4 Ca2 O22 Ca1 -22.56(10) . . . . ? N62 Ca2 O22 Ca1 123.05(11) . . . . ? O22 C22 C23 C24 -174.98(19) . . . . ? C21 C22 C23 C24 4.2(3) . . . . ? O22 C22 C23 C231 4.7(3) . . . . ? C21 C22 C23 C231 -176.1(2) . . . . ? C24 C23 C231 C234 0.0(3) . . . . ? C22 C23 C231 C234 -179.7(2) . . . . ? C24 C23 C231 C232 -118.7(2) . . . . ? C22 C23 C231 C232 61.7(3) . . . . ? C24 C23 C231 C233 120.1(2) . . . . ? C22 C23 C231 C233 -59.6(3) . . . . ? C22 C23 C24 C25 -1.5(3) . . . . ? C231 C23 C24 C25 178.8(2) . . . . ? C23 C24 C25 C26 -2.1(3) . . . . ? C23 C24 C25 C251 177.3(2) . . . . ? C26 C25 C251 C252 0.1(3) . . . . ? C24 C25 C251 C252 -179.2(2) . . . . ? C26 C25 C251 C254 -120.8(3) . . . . ? C24 C25 C251 C254 59.9(3) . . . . ? C26 C25 C251 C253 119.7(3) . . . . ? C24 C25 C251 C253 -59.6(3) . . . . ? C24 C25 C26 C21 2.9(3) . . . . ? C251 C25 C26 C21 -176.4(2) . . . . ? C22 C21 C26 C25 -0.3(3) . . . . ? C2 C21 C26 C25 173.5(2) . . . . ? C1 N1 C3 C31A -85.0(3) . . . . ? C2 N1 C3 C31A 156.7(3) . . . . ? Ca1 N1 C3 C31A 34.4(3) . . . . ? C1 N1 C3 C31 -143.6(2) . . . . ? C2 N1 C3 C31 98.1(3) . . . . ? Ca1 N1 C3 C31 -24.2(3) . . . . ? C31A C3 C31 N32 -45.5(4) . . . . ? N1 C3 C31 N32 58.2(4) . . . . ? C3 C31 N32 C33A -167.1(5) . . . . ? C3 C31 N32 C34 68.8(4) . . . . ? C3 C31 N32 C34A 92.9(7) . . . . ? C3 C31 N32 C33 -172.6(3) . . . . ? C3 C31 N32 C31A 43.1(3) . . . . ? C3 C31 N32 Ca1 -56.7(3) . . . . ? O12 Ca1 N32 C33A 176.8(5) . . . . ? O22 Ca1 N32 C33A 27.2(5) . . . . ? O52 Ca1 N32 C33A -50.6(6) . . . . ? N1 Ca1 N32 C33A 102.5(5) . . . . ? Ca2 Ca1 N32 C33A 23.0(6) . . . . ? O12 Ca1 N32 C34 -21.1(4) . . . . ? O22 Ca1 N32 C34 -170.7(4) . . . . ? O52 Ca1 N32 C34 111.5(4) . . . . ? N1 Ca1 N32 C34 -95.4(4) . . . . ? Ca2 Ca1 N32 C34 -174.9(3) . . . . ? O12 Ca1 N32 C31 105.0(2) . . . . ? O22 Ca1 N32 C31 -44.6(2) . . . . ? O52 Ca1 N32 C31 -122.4(2) . . . . ? N1 Ca1 N32 C31 30.7(2) . . . . ? Ca2 Ca1 N32 C31 -48.8(2) . . . . ? O12 Ca1 N32 C34A -55.3(5) . . . . ? O22 Ca1 N32 C34A 155.1(4) . . . . ? O52 Ca1 N32 C34A 77.4(5) . . . . ? N1 Ca1 N32 C34A -129.5(5) . . . . ? Ca2 Ca1 N32 C34A 151.0(4) . . . . ? O12 Ca1 N32 C33 -145.8(3) . . . . ? O22 Ca1 N32 C33 64.7(3) . . . . ? O52 Ca1 N32 C33 -13.1(4) . . . . ? N1 Ca1 N32 C33 140.0(3) . . . . ? Ca2 Ca1 N32 C33 60.5(3) . . . . ? O12 Ca1 N32 C31A 51.9(3) . . . . ? O22 Ca1 N32 C31A -97.7(3) . . . . ? O52 Ca1 N32 C31A -175.4(2) . . . . ? N1 Ca1 N32 C31A -22.3(2) . . . . ? Ca2 Ca1 N32 C31A -101.8(3) . . . . ? N1 C3 C31A N32 -58.9(5) . . . . ? C31 C3 C31A N32 43.0(3) . . . . ? C33A N32 C31A C3 -75.3(6) . . . . ? C34 N32 C31A C3 160.4(5) . . . . ? C31 N32 C31A C3 -44.6(3) . . . . ? C34A N32 C31A C3 164.3(5) . . . . ? C33 N32 C31A C3 -105.1(6) . . . . ? Ca1 N32 C31A C3 49.3(4) . . . . ? O42 Ca2 N4 C6 -121.41(15) . . . . ? O52 Ca2 N4 C6 100.93(15) . . . . ? O22 Ca2 N4 C6 152.57(13) . . . . ? N62 Ca2 N4 C6 -8.35(14) . . . . ? Ca1 Ca2 N4 C6 138.19(14) . . . . ? O42 Ca2 N4 C4 0.49(13) . . . . ? O52 Ca2 N4 C4 -137.17(14) . . . . ? O22 Ca2 N4 C4 -85.53(15) . . . . ? N62 Ca2 N4 C4 113.55(14) . . . . ? Ca1 Ca2 N4 C4 -99.91(13) . . . . ? O42 Ca2 N4 C5 116.60(14) . . . . ? O52 Ca2 N4 C5 -21.07(13) . . . . ? O22 Ca2 N4 C5 30.58(17) . . . . ? N62 Ca2 N4 C5 -130.34(15) . . . . ? Ca1 Ca2 N4 C5 16.20(14) . . . . ? C6 N4 C4 C41 67.9(3) . . . . ? C5 N4 C4 C41 -171.4(2) . . . . ? Ca2 N4 C4 C41 -52.9(2) . . . . ? N4 C4 C41 C46 -110.7(3) . . . . ? N4 C4 C41 C42 70.7(3) . . . . ? C46 C41 C42 O42 178.0(2) . . . . ? C4 C41 C42 O42 -3.3(3) . . . . ? C46 C41 C42 C43 -0.2(3) . . . . ? C4 C41 C42 C43 178.4(2) . . . . ? C41 C42 O42 Ca2 -64.2(2) . . . . ? C43 C42 O42 Ca2 114.0(2) . . . . ? O52 Ca2 O42 C42 124.30(15) . . . . ? O22 Ca2 O42 C42 -167.39(16) . . . . ? N4 Ca2 O42 C42 56.11(16) . . . . ? N62 Ca2 O42 C42 -13.11(17) . . . . ? Ca1 Ca2 O42 C42 153.41(15) . . . . ? O42 C42 C43 C44 -176.5(2) . . . . ? C41 C42 C43 C44 1.7(3) . . . . ? O42 C42 C43 C431 3.0(3) . . . . ? C41 C42 C43 C431 -178.8(2) . . . . ? C44 C43 C431 C434 -120.6(2) . . . . ? C42 C43 C431 C434 60.0(3) . . . . ? C44 C43 C431 C432 119.3(2) . . . . ? C42 C43 C431 C432 -60.2(3) . . . . ? C44 C43 C431 C433 -1.0(3) . . . . ? C42 C43 C431 C433 179.5(2) . . . . ? C42 C43 C44 C45 -0.9(3) . . . . ? C431 C43 C44 C45 179.7(2) . . . . ? C43 C44 C45 C46 -1.4(3) . . . . ? C43 C44 C45 C451 177.9(2) . . . . ? C44 C45 C451 C453 121.1(3) . . . . ? C46 C45 C451 C453 -59.6(3) . . . . ? C44 C45 C451 C452 -0.1(3) . . . . ? C46 C45 C451 C452 179.2(2) . . . . ? C44 C45 C451 C454 -118.5(3) . . . . ? C46 C45 C451 C454 60.8(3) . . . . ? C42 C41 C46 C45 -2.3(4) . . . . ? C4 C41 C46 C45 179.1(2) . . . . ? C44 C45 C46 C41 3.0(3) . . . . ? C451 C45 C46 C41 -176.3(2) . . . . ? C6 N4 C5 C51 -56.2(3) . . . . ? C4 N4 C5 C51 -177.5(2) . . . . ? Ca2 N4 C5 C51 65.2(2) . . . . ? N4 C5 C51 C56 122.0(2) . . . . ? N4 C5 C51 C52 -64.1(3) . . . . ? C56 C51 C52 O52 176.0(2) . . . . ? C5 C51 C52 O52 2.1(3) . . . . ? C56 C51 C52 C53 -3.2(3) . . . . ? C5 C51 C52 C53 -177.0(2) . . . . ? C51 C52 O52 Ca2 46.8(3) . . . . ? C53 C52 O52 Ca2 -134.01(17) . . . . ? C51 C52 O52 Ca1 -93.5(2) . . . . ? C53 C52 O52 Ca1 85.7(2) . . . . ? O42 Ca2 O52 C52 -100.90(18) . . . . ? O22 Ca2 O52 C52 -177.32(18) . . . . ? N4 Ca2 O52 C52 -31.80(17) . . . . ? N62 Ca2 O52 C52 37.73(18) . . . . ? Ca1 Ca2 O52 C52 -147.02(19) . . . . ? O42 Ca2 O52 Ca1 46.12(10) . . . . ? O22 Ca2 O52 Ca1 -30.30(5) . . . . ? N4 Ca2 O52 Ca1 115.22(6) . . . . ? N62 Ca2 O52 Ca1 -175.26(6) . . . . ? O12 Ca1 O52 C52 45.66(15) . . . . ? O22 Ca1 O52 C52 -178.37(16) . . . . ? N1 Ca1 O52 C52 127.28(15) . . . . ? N32 Ca1 O52 C52 -91.34(19) . . . . ? Ca2 Ca1 O52 C52 150.68(18) . . . . ? O12 Ca1 O52 Ca2 -105.03(6) . . . . ? O22 Ca1 O52 Ca2 30.95(5) . . . . ? N1 Ca1 O52 Ca2 -23.40(10) . . . . ? N32 Ca1 O52 Ca2 117.97(11) . . . . ? O52 C52 C53 C54 -174.80(19) . . . . ? C51 C52 C53 C54 4.4(3) . . . . ? O52 C52 C53 C531 5.1(3) . . . . ? C51 C52 C53 C531 -175.8(2) . . . . ? C54 C53 C531 C534 -0.1(3) . . . . ? C52 C53 C531 C534 -179.9(2) . . . . ? C54 C53 C531 C533 120.6(2) . . . . ? C52 C53 C531 C533 -59.3(3) . . . . ? C54 C53 C531 C532 -118.9(2) . . . . ? C52 C53 C531 C532 61.2(3) . . . . ? C52 C53 C54 C55 -2.2(3) . . . . ? C531 C53 C54 C55 178.0(2) . . . . ? C53 C54 C55 C56 -1.3(4) . . . . ? C53 C54 C55 C551 177.6(2) . . . . ? C56 C55 C551 C552 -2.4(4) . . . . ? C54 C55 C551 C552 178.8(2) . . . . ? C56 C55 C551 C553 -123.8(3) . . . . ? C54 C55 C551 C553 57.5(3) . . . . ? C56 C55 C551 C554 117.6(3) . . . . ? C54 C55 C551 C554 -61.2(3) . . . . ? C54 C55 C56 C51 2.6(3) . . . . ? C551 C55 C56 C51 -176.2(2) . . . . ? C52 C51 C56 C55 -0.4(3) . . . . ? C5 C51 C56 C55 173.5(2) . . . . ? C4 N4 C6 C61A -139.1(3) . . . . ? C5 N4 C6 C61A 102.6(4) . . . . ? Ca2 N4 C6 C61A -19.2(4) . . . . ? C4 N4 C6 C61 -85.4(3) . . . . ? C5 N4 C6 C61 156.3(3) . . . . ? Ca2 N4 C6 C61 34.6(3) . . . . ? C61A C6 C61 N62 47.0(4) . . . . ? N4 C6 C61 N62 -53.8(4) . . . . ? C6 C61 N62 C63A 152.5(5) . . . . ? C6 C61 N62 C64 -81.5(5) . . . . ? C6 C61 N62 C61A -44.3(4) . . . . ? C6 C61 N62 C63 161.0(4) . . . . ? C6 C61 N62 C64A -105.3(7) . . . . ? C6 C61 N62 Ca2 40.5(4) . . . . ? O42 Ca2 N62 C63A -17.8(5) . . . . ? O52 Ca2 N62 C63A -167.8(5) . . . . ? O22 Ca2 N62 C63A 110.7(5) . . . . ? N4 Ca2 N62 C63A -93.3(5) . . . . ? Ca1 Ca2 N62 C63A -173.4(5) . . . . ? O42 Ca2 N62 C64 -177.8(3) . . . . ? O52 Ca2 N62 C64 32.3(3) . . . . ? O22 Ca2 N62 C64 -49.2(4) . . . . ? N4 Ca2 N62 C64 106.8(3) . . . . ? Ca1 Ca2 N62 C64 26.6(4) . . . . ? O42 Ca2 N62 C61 59.0(2) . . . . ? O52 Ca2 N62 C61 -91.0(2) . . . . ? O22 Ca2 N62 C61 -172.5(2) . . . . ? N4 Ca2 N62 C61 -16.5(2) . . . . ? Ca1 Ca2 N62 C61 -96.6(2) . . . . ? O42 Ca2 N62 C61A 105.5(3) . . . . ? O52 Ca2 N62 C61A -44.5(3) . . . . ? O22 Ca2 N62 C61A -126.0(3) . . . . ? N4 Ca2 N62 C61A 30.1(3) . . . . ? Ca1 Ca2 N62 C61A -50.1(3) . . . . ? O42 Ca2 N62 C63 -55.3(3) . . . . ? O52 Ca2 N62 C63 154.8(3) . . . . ? O22 Ca2 N62 C63 73.3(4) . . . . ? N4 Ca2 N62 C63 -130.7(3) . . . . ? Ca1 Ca2 N62 C63 149.1(3) . . . . ? O42 Ca2 N62 C64A -147.0(5) . . . . ? O52 Ca2 N62 C64A 63.1(5) . . . . ? O22 Ca2 N62 C64A -18.5(5) . . . . ? N4 Ca2 N62 C64A 137.6(5) . . . . ? Ca1 Ca2 N62 C64A 57.4(5) . . . . ? N4 C6 C61A N62 56.7(5) . . . . ? C61 C6 C61A N62 -47.3(4) . . . . ? C63A N62 C61A C6 66.7(6) . . . . ? C64 N62 C61A C6 -166.2(6) . . . . ? C61 N62 C61A C6 49.2(4) . . . . ? C63 N62 C61A C6 92.8(7) . . . . ? C64A N62 C61A C6 -171.5(6) . . . . ? Ca2 N62 C61A C6 -57.0(4) . . . . ? C71 C72 O73 C74 178.3(3) . . . . ? C72 O73 C74 C75 -176.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.269 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.048 #===END data_ruthh2a _database_code_depnum_ccdc_archive 'CCDC 281712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 2-Ti' _chemical_melting_point ? _chemical_formula_moiety 'C34 H56 N2 O4 Ti' _chemical_formula_structural '[Ti {N(CH2C6H2O-2,tBu-3,Me-5)2(CH2CH2NMe2)} (OiPr)2]' _chemical_formula_sum 'C34 H56 N2 O4 Ti' _chemical_formula_weight 604.71 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 orthorhombic _symmetry_space_group_name_H-M Pbcn #(no. 69) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.9796(4) _cell_length_b 16.7107(3) _cell_length_c 22.3627(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6718.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'cube-like block' _exptl_crystal_colour 'very pale yellow,' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements SORTAV (Blessing, 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 34498 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5924 _reflns_number_gt 4482 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+5.1289P] 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 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.62126(2) 0.22994(2) 0.547161(17) 0.02200(13) Uani 1 1 d . A . N1 N 0.69643(11) 0.11764(11) 0.53276(8) 0.0229(4) Uani 1 1 d . . . C1 C 0.71793(13) 0.11232(14) 0.46836(10) 0.0245(5) Uani 1 1 d . . . H1A H 0.7540 0.0679 0.4639 0.029 Uiso 1 1 calc R . . H1B H 0.7440 0.1624 0.4574 0.029 Uiso 1 1 calc R . . C11 C 0.65580(13) 0.09932(14) 0.42420(10) 0.0233(5) Uani 1 1 d . . . C12 C 0.59167(13) 0.14688(13) 0.42591(10) 0.0222(5) Uani 1 1 d . . . O12 O 0.58148(9) 0.19716(9) 0.47218(7) 0.0252(4) Uani 1 1 d . . . C13 C 0.53926(13) 0.14299(14) 0.37853(10) 0.0243(5) Uani 1 1 d . . . C131 C 0.47286(14) 0.20064(15) 0.37466(11) 0.0291(6) Uani 1 1 d . . . C132 C 0.42299(16) 0.19512(19) 0.43014(12) 0.0435(7) Uani 1 1 d . . . H13A H 0.4527 0.2056 0.4660 0.065 Uiso 1 1 calc R . . H13B H 0.4013 0.1414 0.4326 0.065 Uiso 1 1 calc R . . H13C H 0.3831 0.2348 0.4272 0.065 Uiso 1 1 calc R . . C133 C 0.50281(18) 0.28596(16) 0.36811(15) 0.0523(8) Uani 1 1 d . . . H13D H 0.5354 0.2984 0.4020 0.078 Uiso 1 1 calc R . . H13E H 0.4612 0.3238 0.3674 0.078 Uiso 1 1 calc R . . H13F H 0.5310 0.2904 0.3308 0.078 Uiso 1 1 calc R . . C134 C 0.42286(16) 0.18356(18) 0.32087(12) 0.0412(7) Uani 1 1 d . . . H13G H 0.4027 0.1293 0.3241 0.062 Uiso 1 1 calc R . . H13H H 0.4520 0.1883 0.2840 0.062 Uiso 1 1 calc R . . H13I H 0.3819 0.2222 0.3201 0.062 Uiso 1 1 calc R . . C14 C 0.55350(14) 0.08739(14) 0.33317(10) 0.0263(5) Uani 1 1 d . . . H14 H 0.5182 0.0829 0.3017 0.032 Uiso 1 1 calc R . . C15 C 0.61600(14) 0.03828(14) 0.33106(10) 0.0260(5) Uani 1 1 d . . . C151 C 0.62967(15) -0.01834(16) 0.27974(11) 0.0335(6) Uani 1 1 d . . . H15A H 0.5857 -0.0198 0.2539 0.050 Uiso 1 1 calc R . . H15B H 0.6395 -0.0721 0.2954 0.050 Uiso 1 1 calc R . . H15C H 0.6727 0.0001 0.2566 0.050 Uiso 1 1 calc R . . C16 C 0.66676(13) 0.04533(14) 0.37748(10) 0.0252(5) Uani 1 1 d . . . H16 H 0.7100 0.0126 0.3774 0.030 Uiso 1 1 calc R . . C2 C 0.76835(13) 0.12960(15) 0.56518(10) 0.0281(6) Uani 1 1 d . . . H2A H 0.7928 0.1776 0.5482 0.034 Uiso 1 1 calc R . . H2B H 0.8007 0.0832 0.5562 0.034 Uiso 1 1 calc R . . C21 C 0.76591(14) 0.13957(14) 0.63207(10) 0.0265(5) Uani 1 1 d . . . C22 C 0.72121(13) 0.19935(14) 0.65723(10) 0.0254(5) Uani 1 1 d . . . O22 O 0.67003(9) 0.23519(10) 0.62248(7) 0.0265(4) Uani 1 1 d . . . C23 C 0.73099(14) 0.22180(15) 0.71788(10) 0.0292(6) Uani 1 1 d . . . C231 C 0.69401(15) 0.29719(15) 0.74351(11) 0.0345(6) Uani 1 1 d . . . C232 C 0.60872(16) 0.29279(18) 0.74178(13) 0.0437(7) Uani 1 1 d . . . H23A H 0.5918 0.2468 0.7654 0.066 Uiso 1 1 calc R . . H23B H 0.5921 0.2867 0.7003 0.066 Uiso 1 1 calc R . . H23C H 0.5878 0.3421 0.7586 0.066 Uiso 1 1 calc R . . C233 C 0.72005(17) 0.36957(16) 0.70639(13) 0.0437(7) Uani 1 1 d . . . H23D H 0.6971 0.4184 0.7221 0.066 Uiso 1 1 calc R . . H23E H 0.7053 0.3622 0.6646 0.066 Uiso 1 1 calc R . . H23F H 0.7743 0.3742 0.7089 0.066 Uiso 1 1 calc R . . C234 C 0.7165(2) 0.3122(2) 0.80878(13) 0.0549(9) Uani 1 1 d . . . H23G H 0.7006 0.2669 0.8335 0.082 Uiso 1 1 calc R . . H23H H 0.6926 0.3612 0.8232 0.082 Uiso 1 1 calc R . . H23I H 0.7706 0.3180 0.8113 0.082 Uiso 1 1 calc R . . C24 C 0.78092(15) 0.17627(15) 0.75142(11) 0.0335(6) Uani 1 1 d . . . H24 H 0.7871 0.1893 0.7925 0.040 Uiso 1 1 calc R . . C25 C 0.82192(15) 0.11329(15) 0.72842(11) 0.0335(6) Uani 1 1 d . . . C251 C 0.87535(19) 0.06624(18) 0.76736(13) 0.0522(8) Uani 1 1 d . . . H25A H 0.9039 0.1032 0.7924 0.078 Uiso 1 1 calc R . . H25B H 0.9095 0.0357 0.7419 0.078 Uiso 1 1 calc R . . H25C H 0.8472 0.0294 0.7929 0.078 Uiso 1 1 calc R . . C26 C 0.81482(14) 0.09649(15) 0.66782(11) 0.0313(6) Uani 1 1 d . . . H26 H 0.8438 0.0549 0.6506 0.038 Uiso 1 1 calc R . . C3 C 0.65974(14) 0.04212(14) 0.55145(10) 0.0272(5) Uani 1 1 d . . . H3A H 0.6981 0.0023 0.5624 0.033 Uiso 1 1 calc R . . H3B H 0.6308 0.0203 0.5175 0.033 Uiso 1 1 calc R . . C31 C 0.60855(15) 0.05573(15) 0.60412(11) 0.0306(6) Uani 1 1 d . . . H31A H 0.5813 0.0057 0.6131 0.037 Uiso 1 1 calc R . . H31B H 0.6384 0.0701 0.6397 0.037 Uiso 1 1 calc R . . N32 N 0.55482(11) 0.12038(12) 0.59140(8) 0.0271(5) Uani 1 1 d . . . C33 C 0.49415(15) 0.08980(17) 0.55306(12) 0.0378(7) Uani 1 1 d . . . H33A H 0.4593 0.1333 0.5442 0.057 Uiso 1 1 calc R . . H33B H 0.4679 0.0467 0.5739 0.057 Uiso 1 1 calc R . . H33C H 0.5151 0.0692 0.5156 0.057 Uiso 1 1 calc R . . C34 C 0.52107(17) 0.14487(17) 0.64884(12) 0.0420(7) Uani 1 1 d . . . H34A H 0.4856 0.1884 0.6418 0.063 Uiso 1 1 calc R . . H34B H 0.5602 0.1633 0.6761 0.063 Uiso 1 1 calc R . . H34C H 0.4951 0.0992 0.6667 0.063 Uiso 1 1 calc R . . O4 O 0.54434(10) 0.29480(10) 0.56515(7) 0.0318(4) Uani 1 1 d . . . C41 C 0.5003(2) 0.3554(3) 0.5907(3) 0.0441(17) Uani 0.739(12) 1 d P A 1 H41 H 0.4863 0.3366 0.6316 0.053 Uiso 0.739(12) 1 calc PR A 1 C42 C 0.5451(2) 0.4311(2) 0.5988(2) 0.0778(12) Uani 1 1 d . . . H42A H 0.5916 0.4186 0.6197 0.117 Uiso 1 1 calc R A 1 H42B H 0.5164 0.4696 0.6224 0.117 Uiso 1 1 calc R A 1 H42C H 0.5564 0.4542 0.5596 0.117 Uiso 1 1 calc R A 1 C43 C 0.4316(2) 0.3675(2) 0.5583(2) 0.0931(15) Uani 1 1 d . . . H43A H 0.4066 0.3159 0.5527 0.140 Uiso 1 1 calc R A 1 H43B H 0.4426 0.3912 0.5191 0.140 Uiso 1 1 calc R A 1 H43C H 0.3993 0.4035 0.5810 0.140 Uiso 1 1 calc R A 1 C41A C 0.5079(6) 0.3695(6) 0.5546(8) 0.030(3) Uiso 0.261(12) 1 d P A 2 H41A H 0.5209 0.3866 0.5130 0.036 Uiso 0.261(12) 1 calc PR A 2 O5 O 0.69154(10) 0.29372(10) 0.51183(7) 0.0305(4) Uani 1 1 d . . . C51 C 0.70172(15) 0.32894(15) 0.45471(10) 0.0310(6) Uani 1 1 d . A . H51 H 0.6827 0.2913 0.4235 0.037 Uiso 1 1 calc R . . C52 C 0.65829(17) 0.40629(17) 0.45123(13) 0.0451(7) Uani 1 1 d . . . H52A H 0.6054 0.3954 0.4581 0.068 Uiso 1 1 calc R A . H52B H 0.6648 0.4302 0.4116 0.068 Uiso 1 1 calc R . . H52C H 0.6765 0.4434 0.4818 0.068 Uiso 1 1 calc R . . C53 C 0.78414(15) 0.34242(18) 0.44469(12) 0.0408(7) Uani 1 1 d . . . H53A H 0.8105 0.2912 0.4473 0.061 Uiso 1 1 calc R A . H53B H 0.8033 0.3790 0.4753 0.061 Uiso 1 1 calc R . . H53C H 0.7920 0.3658 0.4050 0.061 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 0.0232(2) 0.0202(2) 0.0226(2) -0.00134(16) 0.00012(17) -0.00050(18) N1 0.0217(11) 0.0233(11) 0.0237(10) 0.0003(8) -0.0010(8) -0.0027(8) C1 0.0241(13) 0.0250(13) 0.0244(12) -0.0013(10) 0.0015(9) 0.0013(11) C11 0.0261(13) 0.0229(13) 0.0210(12) 0.0027(9) 0.0018(9) -0.0022(11) C12 0.0251(13) 0.0216(12) 0.0197(12) 0.0005(9) 0.0012(9) -0.0023(10) O12 0.0268(9) 0.0240(9) 0.0249(8) -0.0035(7) -0.0031(7) 0.0035(7) C13 0.0252(13) 0.0254(13) 0.0222(12) 0.0028(9) 0.0010(10) -0.0015(10) C131 0.0263(14) 0.0304(14) 0.0305(13) -0.0005(10) -0.0052(10) 0.0012(11) C132 0.0329(16) 0.0563(19) 0.0414(16) -0.0035(14) 0.0019(12) 0.0165(14) C133 0.0476(19) 0.0320(16) 0.077(2) 0.0087(15) -0.0232(16) 0.0030(15) C134 0.0348(16) 0.0494(18) 0.0395(16) -0.0051(13) -0.0104(12) 0.0110(14) C14 0.0291(14) 0.0296(14) 0.0202(12) 0.0018(10) -0.0018(10) -0.0047(11) C15 0.0295(14) 0.0262(13) 0.0222(12) 0.0008(9) 0.0040(10) -0.0027(11) C151 0.0351(16) 0.0376(16) 0.0277(13) -0.0059(11) 0.0021(11) -0.0023(12) C16 0.0257(13) 0.0228(13) 0.0271(13) 0.0032(10) 0.0044(10) 0.0011(11) C2 0.0234(13) 0.0314(14) 0.0295(13) -0.0026(10) -0.0022(10) 0.0027(11) C21 0.0280(14) 0.0258(13) 0.0258(13) -0.0013(10) -0.0042(10) -0.0042(11) C22 0.0270(13) 0.0241(13) 0.0252(13) 0.0005(10) -0.0016(10) -0.0073(11) O22 0.0264(9) 0.0282(9) 0.0248(9) -0.0028(7) -0.0026(7) 0.0004(8) C23 0.0311(14) 0.0292(14) 0.0273(13) -0.0021(10) -0.0010(11) -0.0094(11) C231 0.0387(16) 0.0345(15) 0.0304(14) -0.0078(11) -0.0023(11) -0.0033(12) C232 0.0389(17) 0.0505(18) 0.0418(16) -0.0140(13) 0.0084(13) -0.0059(14) C233 0.0419(17) 0.0310(16) 0.0582(18) -0.0094(13) 0.0065(14) -0.0015(14) C234 0.065(2) 0.058(2) 0.0412(17) -0.0232(15) -0.0126(15) 0.0053(18) C24 0.0447(17) 0.0318(14) 0.0241(13) 0.0001(11) -0.0056(11) -0.0119(13) C25 0.0382(16) 0.0275(14) 0.0348(15) 0.0036(11) -0.0130(11) -0.0066(12) C251 0.066(2) 0.0448(18) 0.0452(18) -0.0051(14) -0.0267(15) 0.0072(16) C26 0.0327(15) 0.0252(14) 0.0359(15) -0.0019(11) -0.0076(11) -0.0005(11) C3 0.0311(14) 0.0202(13) 0.0302(13) 0.0017(10) -0.0013(10) -0.0001(11) C31 0.0380(15) 0.0256(13) 0.0282(13) 0.0034(10) -0.0008(11) -0.0064(12) N32 0.0268(11) 0.0256(11) 0.0289(11) -0.0007(8) 0.0019(8) -0.0029(9) C33 0.0326(15) 0.0382(16) 0.0427(16) 0.0058(12) -0.0047(12) -0.0137(13) C34 0.0449(18) 0.0423(17) 0.0387(16) -0.0023(12) 0.0175(13) -0.0089(14) O4 0.0305(10) 0.0286(10) 0.0361(10) -0.0072(7) 0.0014(8) 0.0059(8) C41 0.043(3) 0.037(2) 0.052(4) -0.014(2) 0.000(2) 0.0112(19) C42 0.064(2) 0.045(2) 0.125(3) -0.037(2) -0.023(2) 0.0102(19) C43 0.044(2) 0.061(3) 0.174(5) -0.036(3) -0.023(3) 0.020(2) O5 0.0342(10) 0.0293(10) 0.0281(9) 0.0028(7) 0.0009(7) -0.0071(8) C51 0.0393(16) 0.0264(14) 0.0272(13) 0.0034(10) -0.0005(11) -0.0061(12) C52 0.0461(18) 0.0358(17) 0.0533(18) 0.0062(13) -0.0051(14) -0.0025(14) C53 0.0384(16) 0.0414(17) 0.0426(16) 0.0064(12) 0.0080(12) -0.0061(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 O4 1.8025(17) . ? Ti O5 1.8321(17) . ? Ti O22 1.9009(15) . ? Ti O12 1.9034(15) . ? Ti N1 2.335(2) . ? Ti N32 2.400(2) . ? N1 C3 1.484(3) . ? N1 C1 1.494(3) . ? N1 C2 1.496(3) . ? C1 C11 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C11 C16 1.394(3) . ? C11 C12 1.401(3) . ? C12 O12 1.346(3) . ? C12 C13 1.419(3) . ? C13 C14 1.399(3) . ? C13 C131 1.536(3) . ? C131 C134 1.529(3) . ? C131 C133 1.531(4) . ? C131 C132 1.534(4) . ? C132 H13A 0.9800 . ? C132 H13B 0.9800 . ? C132 H13C 0.9800 . ? C133 H13D 0.9800 . ? C133 H13E 0.9800 . ? C133 H13F 0.9800 . ? C134 H13G 0.9800 . ? C134 H13H 0.9800 . ? C134 H13I 0.9800 . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.387(3) . ? C15 C151 1.508(3) . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C16 H16 0.9500 . ? C2 C21 1.506(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C21 C26 1.390(3) . ? C21 C22 1.400(3) . ? C22 O22 1.345(3) . ? C22 C23 1.418(3) . ? C23 C24 1.395(4) . ? C23 C231 1.535(4) . ? C231 C234 1.535(4) . ? C231 C232 1.536(4) . ? C231 C233 1.540(4) . ? C232 H23A 0.9800 . ? C232 H23B 0.9800 . ? C232 H23C 0.9800 . ? C233 H23D 0.9800 . ? C233 H23E 0.9800 . ? C233 H23F 0.9800 . ? C234 H23G 0.9800 . ? C234 H23H 0.9800 . ? C234 H23I 0.9800 . ? C24 C25 1.384(4) . ? C24 H24 0.9500 . ? C25 C26 1.390(3) . ? C25 C251 1.516(4) . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C26 H26 0.9500 . ? C3 C31 1.512(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C31 N32 1.477(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N32 C34 1.478(3) . ? N32 C33 1.478(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O4 C41 1.407(4) . ? O4 C41A 1.429(11) . ? C41 C43 1.446(6) . ? C41 C42 1.510(5) . ? C41 H41 1.0000 . ? C42 C41A 1.577(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C41A 1.374(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C41A H41A 1.0000 . ? O5 C51 1.418(3) . ? C51 C52 1.512(4) . ? C51 C53 1.516(4) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 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 O4 Ti O5 106.00(8) . . ? O4 Ti O22 97.37(7) . . ? O5 Ti O22 92.12(7) . . ? O4 Ti O12 94.67(7) . . ? O5 Ti O12 92.68(7) . . ? O22 Ti O12 165.27(7) . . ? O4 Ti N1 163.36(8) . . ? O5 Ti N1 90.51(7) . . ? O22 Ti N1 83.82(7) . . ? O12 Ti N1 82.23(7) . . ? O4 Ti N32 89.13(7) . . ? O5 Ti N32 164.79(8) . . ? O22 Ti N32 84.24(7) . . ? O12 Ti N32 87.51(7) . . ? N1 Ti N32 74.44(7) . . ? C3 N1 C1 109.62(17) . . ? C3 N1 C2 111.19(18) . . ? C1 N1 C2 104.57(17) . . ? C3 N1 Ti 112.79(14) . . ? C1 N1 Ti 109.30(13) . . ? C2 N1 Ti 109.04(14) . . ? N1 C1 C11 116.66(19) . . ? N1 C1 H1A 108.1 . . ? C11 C1 H1A 108.1 . . ? N1 C1 H1B 108.1 . . ? C11 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C16 C11 C12 120.3(2) . . ? C16 C11 C1 118.7(2) . . ? C12 C11 C1 120.7(2) . . ? O12 C12 C11 119.2(2) . . ? O12 C12 C13 120.8(2) . . ? C11 C12 C13 120.0(2) . . ? C12 O12 Ti 143.71(15) . . ? C14 C13 C12 116.7(2) . . ? C14 C13 C131 121.2(2) . . ? C12 C13 C131 122.0(2) . . ? C134 C131 C133 107.8(2) . . ? C134 C131 C132 106.3(2) . . ? C133 C131 C132 109.8(2) . . ? C134 C131 C13 112.6(2) . . ? C133 C131 C13 108.4(2) . . ? C132 C131 C13 111.8(2) . . ? C131 C132 H13A 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C131 C133 H13D 109.5 . . ? C131 C133 H13E 109.5 . . ? H13D C133 H13E 109.5 . . ? C131 C133 H13F 109.5 . . ? H13D C133 H13F 109.5 . . ? H13E C133 H13F 109.5 . . ? C131 C134 H13G 109.5 . . ? C131 C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? C131 C134 H13I 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? C15 C14 C13 124.3(2) . . ? C15 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C16 C15 C14 117.1(2) . . ? C16 C15 C151 121.0(2) . . ? C14 C15 C151 121.8(2) . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C15 C16 C11 121.5(2) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? N1 C2 C21 118.1(2) . . ? N1 C2 H2A 107.8 . . ? C21 C2 H2A 107.8 . . ? N1 C2 H2B 107.8 . . ? C21 C2 H2B 107.8 . . ? H2A C2 H2B 107.1 . . ? C26 C21 C22 120.1(2) . . ? C26 C21 C2 119.7(2) . . ? C22 C21 C2 119.7(2) . . ? O22 C22 C21 118.6(2) . . ? O22 C22 C23 121.3(2) . . ? C21 C22 C23 120.1(2) . . ? C22 O22 Ti 143.80(15) . . ? C24 C23 C22 116.7(2) . . ? C24 C23 C231 121.7(2) . . ? C22 C23 C231 121.3(2) . . ? C234 C231 C23 112.0(2) . . ? C234 C231 C232 107.1(2) . . ? C23 C231 C232 112.6(2) . . ? C234 C231 C233 107.7(2) . . ? C23 C231 C233 108.2(2) . . ? C232 C231 C233 109.1(2) . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C231 C233 H23D 109.5 . . ? C231 C233 H23E 109.5 . . ? H23D C233 H23E 109.5 . . ? C231 C233 H23F 109.5 . . ? H23D C233 H23F 109.5 . . ? H23E C233 H23F 109.5 . . ? C231 C234 H23G 109.5 . . ? C231 C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C231 C234 H23I 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C25 C24 C23 123.9(2) . . ? C25 C24 H24 118.1 . . ? C23 C24 H24 118.1 . . ? C24 C25 C26 117.8(2) . . ? C24 C25 C251 121.2(2) . . ? C26 C25 C251 120.9(2) . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C21 C26 C25 121.0(2) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? N1 C3 C31 111.22(19) . . ? N1 C3 H3A 109.4 . . ? C31 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C31 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N32 C31 C3 110.97(19) . . ? N32 C31 H31A 109.4 . . ? C3 C31 H31A 109.4 . . ? N32 C31 H31B 109.4 . . ? C3 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 N32 C34 107.67(19) . . ? C31 N32 C33 109.97(19) . . ? C34 N32 C33 107.3(2) . . ? C31 N32 Ti 108.18(14) . . ? C34 N32 Ti 110.57(15) . . ? C33 N32 Ti 113.07(15) . . ? N32 C33 H33A 109.5 . . ? N32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 O4 C41A 35.0(5) . . ? C41 O4 Ti 162.8(2) . . ? C41A O4 Ti 147.1(6) . . ? O4 C41 C43 112.2(4) . . ? O4 C41 C42 110.6(4) . . ? C43 C41 C42 113.5(4) . . ? O4 C41 H41 106.7 . . ? C43 C41 H41 106.7 . . ? C42 C41 H41 106.7 . . ? C41 C42 C41A 32.0(4) . . ? C41 C42 H42A 109.5 . . ? C41A C42 H42A 121.4 . . ? C41 C42 H42B 109.5 . . ? C41A C42 H42B 122.9 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? C41A C42 H42C 77.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41A C43 C41 35.1(5) . . ? C41A C43 H43A 118.1 . . ? C41 C43 H43A 109.5 . . ? C41A C43 H43B 74.8 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41A C43 H43C 127.6 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C43 C41A O4 115.3(9) . . ? C43 C41A C42 113.7(9) . . ? O4 C41A C42 105.8(8) . . ? C43 C41A H41A 107.2 . . ? O4 C41A H41A 107.2 . . ? C42 C41A H41A 107.2 . . ? C51 O5 Ti 135.95(15) . . ? O5 C51 C52 109.5(2) . . ? O5 C51 C53 108.7(2) . . ? C52 C51 C53 111.7(2) . . ? O5 C51 H51 108.9 . . ? C52 C51 H51 108.9 . . ? C53 C51 H51 108.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ti N1 C3 -2.8(3) . . . . ? O5 Ti N1 C3 -175.63(15) . . . . ? O22 Ti N1 C3 92.29(15) . . . . ? O12 Ti N1 C3 -83.00(15) . . . . ? N32 Ti N1 C3 6.57(14) . . . . ? O4 Ti N1 C1 119.4(3) . . . . ? O5 Ti N1 C1 -53.42(14) . . . . ? O22 Ti N1 C1 -145.50(15) . . . . ? O12 Ti N1 C1 39.22(14) . . . . ? N32 Ti N1 C1 128.78(15) . . . . ? O4 Ti N1 C2 -126.8(3) . . . . ? O5 Ti N1 C2 60.33(14) . . . . ? O22 Ti N1 C2 -31.75(14) . . . . ? O12 Ti N1 C2 152.97(15) . . . . ? N32 Ti N1 C2 -117.46(15) . . . . ? C3 N1 C1 C11 60.2(3) . . . . ? C2 N1 C1 C11 179.5(2) . . . . ? Ti N1 C1 C11 -63.9(2) . . . . ? N1 C1 C11 C16 -137.9(2) . . . . ? N1 C1 C11 C12 49.2(3) . . . . ? C16 C11 C12 O12 178.4(2) . . . . ? C1 C11 C12 O12 -8.8(3) . . . . ? C16 C11 C12 C13 -3.0(3) . . . . ? C1 C11 C12 C13 169.7(2) . . . . ? C11 C12 O12 Ti -5.1(4) . . . . ? C13 C12 O12 Ti 176.33(17) . . . . ? O4 Ti O12 C12 -173.4(2) . . . . ? O5 Ti O12 C12 80.3(2) . . . . ? O22 Ti O12 C12 -28.6(4) . . . . ? N1 Ti O12 C12 -9.9(2) . . . . ? N32 Ti O12 C12 -84.5(2) . . . . ? O12 C12 C13 C14 -178.3(2) . . . . ? C11 C12 C13 C14 3.1(3) . . . . ? O12 C12 C13 C131 5.7(3) . . . . ? C11 C12 C13 C131 -172.8(2) . . . . ? C14 C13 C131 C134 5.9(3) . . . . ? C12 C13 C131 C134 -178.4(2) . . . . ? C14 C13 C131 C133 -113.3(3) . . . . ? C12 C13 C131 C133 62.5(3) . . . . ? C14 C13 C131 C132 125.5(2) . . . . ? C12 C13 C131 C132 -58.7(3) . . . . ? C12 C13 C14 C15 -1.9(3) . . . . ? C131 C13 C14 C15 174.1(2) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C13 C14 C15 C151 -177.7(2) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? C151 C15 C16 C11 178.0(2) . . . . ? C12 C11 C16 C15 1.4(3) . . . . ? C1 C11 C16 C15 -171.4(2) . . . . ? C3 N1 C2 C21 -63.4(3) . . . . ? C1 N1 C2 C21 178.4(2) . . . . ? Ti N1 C2 C21 61.6(2) . . . . ? N1 C2 C21 C26 133.1(2) . . . . ? N1 C2 C21 C22 -55.0(3) . . . . ? C26 C21 C22 O22 -174.4(2) . . . . ? C2 C21 C22 O22 13.7(3) . . . . ? C26 C21 C22 C23 6.5(4) . . . . ? C2 C21 C22 C23 -165.4(2) . . . . ? C21 C22 O22 Ti 10.5(4) . . . . ? C23 C22 O22 Ti -170.35(18) . . . . ? O4 Ti O22 C22 162.9(2) . . . . ? O5 Ti O22 C22 -90.6(3) . . . . ? O12 Ti O22 C22 18.3(5) . . . . ? N1 Ti O22 C22 -0.3(2) . . . . ? N32 Ti O22 C22 74.6(3) . . . . ? O22 C22 C23 C24 174.6(2) . . . . ? C21 C22 C23 C24 -6.3(3) . . . . ? O22 C22 C23 C231 -11.0(4) . . . . ? C21 C22 C23 C231 168.1(2) . . . . ? C24 C23 C231 C234 -2.2(4) . . . . ? C22 C23 C231 C234 -176.4(2) . . . . ? C24 C23 C231 C232 -123.0(3) . . . . ? C22 C23 C231 C232 62.8(3) . . . . ? C24 C23 C231 C233 116.3(3) . . . . ? C22 C23 C231 C233 -57.8(3) . . . . ? C22 C23 C24 C25 1.9(4) . . . . ? C231 C23 C24 C25 -172.5(2) . . . . ? C23 C24 C25 C26 2.5(4) . . . . ? C23 C24 C25 C251 179.9(3) . . . . ? C22 C21 C26 C25 -1.9(4) . . . . ? C2 C21 C26 C25 169.9(2) . . . . ? C24 C25 C26 C21 -2.5(4) . . . . ? C251 C25 C26 C21 -180.0(3) . . . . ? C1 N1 C3 C31 -155.03(19) . . . . ? C2 N1 C3 C31 89.8(2) . . . . ? Ti N1 C3 C31 -33.0(2) . . . . ? N1 C3 C31 N32 53.7(3) . . . . ? C3 C31 N32 C34 -165.1(2) . . . . ? C3 C31 N32 C33 78.4(2) . . . . ? C3 C31 N32 Ti -45.6(2) . . . . ? O4 Ti N32 C31 -161.97(15) . . . . ? O5 Ti N32 C31 12.3(3) . . . . ? O22 Ti N32 C31 -64.47(14) . . . . ? O12 Ti N32 C31 103.32(14) . . . . ? N1 Ti N32 C31 20.69(14) . . . . ? O4 Ti N32 C34 -44.31(17) . . . . ? O5 Ti N32 C34 129.9(3) . . . . ? O22 Ti N32 C34 53.20(17) . . . . ? O12 Ti N32 C34 -139.02(17) . . . . ? N1 Ti N32 C34 138.36(18) . . . . ? O4 Ti N32 C33 75.98(17) . . . . ? O5 Ti N32 C33 -109.8(3) . . . . ? O22 Ti N32 C33 173.48(17) . . . . ? O12 Ti N32 C33 -18.73(17) . . . . ? N1 Ti N32 C33 -101.35(17) . . . . ? O5 Ti O4 C41 -65.3(11) . . . . ? O22 Ti O4 C41 29.1(11) . . . . ? O12 Ti O4 C41 -159.4(11) . . . . ? N1 Ti O4 C41 122.2(11) . . . . ? N32 Ti O4 C41 113.2(11) . . . . ? O5 Ti O4 C41A 18.6(10) . . . . ? O22 Ti O4 C41A 113.0(10) . . . . ? O12 Ti O4 C41A -75.5(10) . . . . ? N1 Ti O4 C41A -154.0(10) . . . . ? N32 Ti O4 C41A -163.0(10) . . . . ? C41A O4 C41 C43 57.2(8) . . . . ? Ti O4 C41 C43 166.9(7) . . . . ? C41A O4 C41 C42 -70.5(9) . . . . ? Ti O4 C41 C42 39.1(14) . . . . ? O4 C41 C42 C41A 67.7(8) . . . . ? C43 C41 C42 C41A -59.4(9) . . . . ? O4 C41 C43 C41A -60.8(8) . . . . ? C42 C41 C43 C41A 65.5(9) . . . . ? C41 C43 C41A O4 61.6(10) . . . . ? C41 C43 C41A C42 -60.8(10) . . . . ? C41 O4 C41A C43 -65.0(11) . . . . ? Ti O4 C41A C43 145.8(6) . . . . ? C41 O4 C41A C42 61.5(9) . . . . ? Ti O4 C41A C42 -87.7(14) . . . . ? C41 C42 C41A C43 65.1(11) . . . . ? C41 C42 C41A O4 -62.4(9) . . . . ? O4 Ti O5 C51 -77.3(2) . . . . ? O22 Ti O5 C51 -175.5(2) . . . . ? O12 Ti O5 C51 18.4(2) . . . . ? N1 Ti O5 C51 100.6(2) . . . . ? N32 Ti O5 C51 108.7(3) . . . . ? Ti O5 C51 C52 83.3(3) . . . . ? Ti O5 C51 C53 -154.40(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.282 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.073 #===END data_ua0430 _database_code_depnum_ccdc_archive 'CCDC 281713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex 8' _chemical_melting_point ? _chemical_formula_moiety 'C42 H72 N2 Na O6 Ti' _chemical_formula_structural '[Ti {N(CH2C6H2O-2,tBu-3,Me-5)2(CH2CH2NMe2)} (OiPr)2 Na (THF)2]' _chemical_formula_sum 'C42 H72 N2 Na O6 Ti' _chemical_formula_weight 771.91 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.4176(4) _cell_length_b 15.6454(3) _cell_length_c 29.5745(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.3821(7) _cell_angle_gamma 90.00 _cell_volume 10168.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 120849 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description blocks _exptl_crystal_colour 'red/green, dichroic' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 0.215 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 1.079 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 42735 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 21.00 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.983 _reflns_number_total 10744 _reflns_number_gt 6107 _reflns_threshold_expression I>2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10744 _refine_ls_number_parameters 937 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1458 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2549 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.690 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.067 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_1 Ti 0.37467(5) 0.06424(7) 0.23475(4) 0.0323(4) Uani 1 1 d . . . O1_1 O 0.39014(19) 0.0747(3) 0.30391(14) 0.0388(12) Uani 1 1 d . . . N1_1 N 0.4130(2) 0.2047(3) 0.23778(16) 0.0318(13) Uani 1 1 d . . . C1_1 C 0.4798(3) 0.2090(4) 0.2414(2) 0.0373(18) Uani 1 1 d . . . H1A_1 H 0.4960 0.2593 0.2602 0.045 Uiso 1 1 calc R . . H1B_1 H 0.4890 0.2164 0.2102 0.045 Uiso 1 1 calc R . . Na1_1 Na 0.25110(12) 0.11455(18) 0.15788(9) 0.0533(8) Uani 1 1 d . . . O2_1 O 0.35290(18) 0.0870(3) 0.16427(14) 0.0371(11) Uani 1 1 d . . . N2_1 N 0.4831(2) 0.0515(4) 0.2402(2) 0.0442(16) Uani 1 1 d . . . C2_1 C 0.5106(3) 0.1304(6) 0.2629(3) 0.082(3) Uani 1 1 d . . . H2A_1 H 0.5542 0.1325 0.2609 0.098 Uiso 1 1 calc R . . H2B_1 H 0.5082 0.1289 0.2959 0.098 Uiso 1 1 calc R . . O3_1 O 0.37128(19) -0.0522(3) 0.22949(14) 0.0446(13) Uani 1 1 d . . . C3_1 C 0.5086(4) -0.0152(6) 0.2735(3) 0.096(3) Uani 1 1 d . . . H3A_1 H 0.5526 -0.0192 0.2751 0.144 Uiso 1 1 calc R . . H3B_1 H 0.4895 -0.0702 0.2635 0.144 Uiso 1 1 calc R . . H3C_1 H 0.5006 -0.0007 0.3039 0.144 Uiso 1 1 calc R . . O4_1 O 0.29078(18) 0.1103(3) 0.23156(14) 0.0359(11) Uani 1 1 d . . . C4_1 C 0.5004(4) 0.0300(7) 0.1976(3) 0.109(4) Uani 1 1 d . . . H4A_1 H 0.5448 0.0262 0.2023 0.164 Uiso 1 1 calc R . . H4B_1 H 0.4858 0.0742 0.1746 0.164 Uiso 1 1 calc R . . H4C_1 H 0.4825 -0.0252 0.1867 0.164 Uiso 1 1 calc R . . C5_1 C 0.3945(3) 0.2483(4) 0.2780(2) 0.0359(17) Uani 1 1 d . . . H5A_1 H 0.3497 0.2444 0.2741 0.043 Uiso 1 1 calc R . . H5B_1 H 0.4050 0.3096 0.2769 0.043 Uiso 1 1 calc R . . O5_1 O 0.2278(2) 0.2404(4) 0.11724(19) 0.0711(16) Uani 1 1 d . . . C6_1 C 0.4224(3) 0.2148(4) 0.3260(2) 0.0343(17) Uani 1 1 d . . . O6_1 O 0.1607(2) 0.0483(4) 0.12842(17) 0.0739(17) Uani 1 1 d . . . C7_1 C 0.4141(3) 0.1286(4) 0.3366(2) 0.0322(17) Uani 1 1 d . . . C8_1 C 0.4305(3) 0.1020(4) 0.3834(2) 0.0371(18) Uani 1 1 d . . . C9_1 C 0.4569(3) 0.1615(5) 0.4158(2) 0.051(2) Uani 1 1 d . . . H9_1 H 0.4692 0.1436 0.4469 0.062 Uiso 1 1 calc R . . C10_1 C 0.4663(3) 0.2473(6) 0.4049(2) 0.055(2) Uani 1 1 d . . . C11_1 C 0.4501(3) 0.2721(4) 0.3599(2) 0.0452(19) Uani 1 1 d . . . H11_1 H 0.4577 0.3291 0.3515 0.054 Uiso 1 1 calc R . . C12_1 C 0.4135(3) 0.0124(4) 0.3980(2) 0.046(2) Uani 1 1 d . . . C13_1 C 0.3443(4) 0.0006(5) 0.3880(3) 0.074(3) Uani 1 1 d . . . H13A_1 H 0.3282 0.0105 0.3551 0.111 Uiso 1 1 calc R . . H13B_1 H 0.3260 0.0415 0.4064 0.111 Uiso 1 1 calc R . . H13C_1 H 0.3345 -0.0578 0.3961 0.111 Uiso 1 1 calc R . . C14_1 C 0.4368(4) -0.0034(5) 0.4497(2) 0.064(2) Uani 1 1 d . . . H14A_1 H 0.4192 0.0391 0.4676 0.097 Uiso 1 1 calc R . . H14B_1 H 0.4813 0.0014 0.4569 0.097 Uiso 1 1 calc R . . H14C_1 H 0.4249 -0.0608 0.4578 0.097 Uiso 1 1 calc R . . C15_1 C 0.4422(4) -0.0577(5) 0.3722(3) 0.068(3) Uani 1 1 d . . . H15A_1 H 0.4285 -0.0503 0.3389 0.102 Uiso 1 1 calc R . . H15B_1 H 0.4296 -0.1141 0.3813 0.102 Uiso 1 1 calc R . . H15C_1 H 0.4866 -0.0532 0.3801 0.102 Uiso 1 1 calc R . . C16_1 C 0.4950(4) 0.3103(5) 0.4428(3) 0.085(3) Uani 1 1 d . . . H16A_1 H 0.4985 0.3667 0.4291 0.128 Uiso 1 1 calc R . . H16B_1 H 0.5356 0.2899 0.4574 0.128 Uiso 1 1 calc R . . H16C_1 H 0.4694 0.3144 0.4660 0.128 Uiso 1 1 calc R . . C17_1 C 0.3813(3) 0.2514(4) 0.19557(19) 0.0341(17) Uani 1 1 d . . . H17A_1 H 0.3370 0.2488 0.1947 0.041 Uiso 1 1 calc R . . H17B_1 H 0.3934 0.3123 0.1989 0.041 Uiso 1 1 calc R . . C18_1 C 0.3925(3) 0.2210(4) 0.1510(2) 0.0358(17) Uani 1 1 d . . . C19_1 C 0.3752(3) 0.1376(4) 0.1355(2) 0.0329(17) Uani 1 1 d . . . C20_1 C 0.3791(3) 0.1104(4) 0.0909(2) 0.0409(19) Uani 1 1 d . . . C21_1 C 0.3990(3) 0.1721(5) 0.0623(2) 0.0400(19) Uani 1 1 d . . . H21_1 H 0.4008 0.1555 0.0317 0.048 Uiso 1 1 calc R . . C22_1 C 0.4159(3) 0.2545(5) 0.0754(2) 0.0421(18) Uani 1 1 d . . . C23_1 C 0.4124(3) 0.2771(5) 0.1204(2) 0.048(2) Uani 1 1 d . . . H23_1 H 0.4240 0.3333 0.1307 0.057 Uiso 1 1 calc R . . C24_1 C 0.3592(3) 0.0210(4) 0.0723(2) 0.0434(19) Uani 1 1 d . . . C25_1 C 0.3925(4) -0.0471(4) 0.1040(3) 0.062(2) Uani 1 1 d . . . H25A_1 H 0.3851 -0.0386 0.1353 0.092 Uiso 1 1 calc R . . H25B_1 H 0.4363 -0.0430 0.1045 0.092 Uiso 1 1 calc R . . H25C_1 H 0.3778 -0.1037 0.0928 0.092 Uiso 1 1 calc R . . C26_1 C 0.3721(3) 0.0047(5) 0.0234(2) 0.058(2) Uani 1 1 d . . . H26A_1 H 0.4158 0.0110 0.0241 0.088 Uiso 1 1 calc R . . H26B_1 H 0.3494 0.0461 0.0017 0.088 Uiso 1 1 calc R . . H26C_1 H 0.3593 -0.0534 0.0135 0.088 Uiso 1 1 calc R . . C27_1 C 0.2903(3) 0.0106(5) 0.0689(3) 0.062(2) Uani 1 1 d . . . H27A_1 H 0.2802 0.0203 0.0993 0.094 Uiso 1 1 calc R . . H27B_1 H 0.2781 -0.0473 0.0584 0.094 Uiso 1 1 calc R . . H27C_1 H 0.2686 0.0523 0.0469 0.094 Uiso 1 1 calc R . . C28_1 C 0.4345(4) 0.3172(5) 0.0430(2) 0.063(2) Uani 1 1 d . . . H28A_1 H 0.4448 0.3717 0.0589 0.095 Uiso 1 1 calc R . . H28B_1 H 0.4008 0.3259 0.0167 0.095 Uiso 1 1 calc R . . H28C_1 H 0.4700 0.2953 0.0320 0.095 Uiso 1 1 calc R . . C29_1 C 0.3584(3) -0.1400(5) 0.2214(3) 0.057(2) Uani 1 1 d . . . H29A_1 H 0.3880 -0.1619 0.2030 0.068 Uiso 1 1 calc R . . C30_1 C 0.3677(3) -0.1915(5) 0.2649(3) 0.070(3) Uani 1 1 d . . . H30A_1 H 0.4093 -0.1834 0.2821 0.104 Uiso 1 1 calc R . . H30B_1 H 0.3610 -0.2521 0.2572 0.104 Uiso 1 1 calc R . . H30C_1 H 0.3388 -0.1728 0.2838 0.104 Uiso 1 1 calc R . . C31_1 C 0.2960(3) -0.1496(5) 0.1919(3) 0.076(3) Uani 1 1 d . . . H31A_1 H 0.2932 -0.1152 0.1638 0.114 Uiso 1 1 calc R . . H31B_1 H 0.2654 -0.1300 0.2090 0.114 Uiso 1 1 calc R . . H31C_1 H 0.2887 -0.2098 0.1834 0.114 Uiso 1 1 calc R . . C32_1 C 0.2573(3) 0.1135(4) 0.2665(2) 0.0377(18) Uani 1 1 d . . . H32A_1 H 0.2855 0.1292 0.2959 0.045 Uiso 1 1 calc R . . C33_1 C 0.2081(3) 0.1827(5) 0.2556(3) 0.065(2) Uani 1 1 d . . . H33A_1 H 0.2272 0.2378 0.2517 0.097 Uiso 1 1 calc R . . H33B_1 H 0.1860 0.1866 0.2810 0.097 Uiso 1 1 calc R . . H33C_1 H 0.1796 0.1678 0.2271 0.097 Uiso 1 1 calc R . . C34_1 C 0.2290(3) 0.0264(5) 0.2732(3) 0.063(2) Uani 1 1 d . . . H34A_1 H 0.2612 -0.0166 0.2807 0.095 Uiso 1 1 calc R . . H34B_1 H 0.2010 0.0100 0.2447 0.095 Uiso 1 1 calc R . . H34C_1 H 0.2066 0.0301 0.2985 0.095 Uiso 1 1 calc R . . C35_1 C 0.2148(5) 0.3204(9) 0.1381(4) 0.116(4) Uani 1 1 d . . . H35A_1 H 0.2362 0.3227 0.1707 0.139 Uiso 1 1 calc R . . H35B_1 H 0.1706 0.3259 0.1370 0.139 Uiso 1 1 calc R . . C36_1 C 0.2358(10) 0.3890(9) 0.1119(6) 0.231(11) Uani 1 1 d . . . H36A_1 H 0.2065 0.4371 0.1077 0.277 Uiso 1 1 calc R . . H36B_1 H 0.2759 0.4104 0.1280 0.277 Uiso 1 1 calc R . . C37_1 C 0.2401(7) 0.3524(9) 0.0682(5) 0.165(6) Uani 1 1 d . . . H37A_1 H 0.2785 0.3707 0.0593 0.199 Uiso 1 1 calc R . . H37B_1 H 0.2057 0.3721 0.0441 0.199 Uiso 1 1 calc R . . C38_1 C 0.2388(4) 0.2591(6) 0.0719(3) 0.083(3) Uani 1 1 d . . . H38A_1 H 0.2059 0.2350 0.0479 0.100 Uiso 1 1 calc R . . H38B_1 H 0.2781 0.2344 0.0679 0.100 Uiso 1 1 calc R . . C39_1 C 0.1171(4) 0.0851(7) 0.0934(4) 0.112(4) Uani 1 1 d . . . H39A_1 H 0.1340 0.0919 0.0651 0.134 Uiso 1 1 calc R . . H39B_1 H 0.1055 0.1422 0.1032 0.134 Uiso 1 1 calc R . . C40_1 C 0.0634(4) 0.0286(6) 0.0841(3) 0.085(3) Uani 1 1 d . . . H40A_1 H 0.0496 0.0194 0.0506 0.102 Uiso 1 1 calc R . . H40B_1 H 0.0294 0.0534 0.0968 0.102 Uiso 1 1 calc R . . C41_1 C 0.0852(5) -0.0556(6) 0.1086(4) 0.096(3) Uani 1 1 d . . . H41A_1 H 0.0571 -0.0744 0.1286 0.116 Uiso 1 1 calc R . . H41B_1 H 0.0880 -0.1012 0.0859 0.116 Uiso 1 1 calc R . . C42_1 C 0.1426(5) -0.0365(7) 0.1349(4) 0.130(5) Uani 1 1 d . . . H42A_1 H 0.1729 -0.0763 0.1264 0.156 Uiso 1 1 calc R . . H42B_1 H 0.1420 -0.0455 0.1679 0.156 Uiso 1 1 calc R . . Ti1_2 Ti 0.12933(5) 0.56464(7) 0.27395(4) 0.0367(4) Uani 1 1 d . . . O1_2 O 0.11524(19) 0.5556(3) 0.20518(15) 0.0442(12) Uani 1 1 d . . . N1_2 N 0.0881(2) 0.4255(3) 0.26939(17) 0.0339(14) Uani 1 1 d . . . C1_2 C 0.0210(3) 0.4245(4) 0.2623(2) 0.0400(18) Uani 1 1 d . . . H1A_2 H 0.0050 0.3821 0.2381 0.048 Uiso 1 1 calc R . . H1B_2 H 0.0090 0.4056 0.2912 0.048 Uiso 1 1 calc R . . O2_2 O 0.14849(19) 0.5415(3) 0.34476(14) 0.0394(12) Uani 1 1 d . . . N2_2 N 0.0213(2) 0.5821(3) 0.2677(2) 0.0469(16) Uani 1 1 d . . . C2_2 C -0.0056(4) 0.5021(7) 0.2497(7) 0.235(10) Uani 1 1 d . . . H2A_2 H -0.0468 0.5001 0.2570 0.282 Uiso 1 1 calc R . . H2B_2 H -0.0113 0.5056 0.2157 0.282 Uiso 1 1 calc R . . Na1_2 Na 0.25058(11) 0.51212(18) 0.35303(9) 0.0532(8) Uani 1 1 d . . . O3_2 O 0.1351(2) 0.6804(3) 0.27952(16) 0.0503(13) Uani 1 1 d . . . C3_2 C -0.0037(4) 0.6448(8) 0.2328(3) 0.131(5) Uani 1 1 d . . . H3A_2 H -0.0476 0.6500 0.2312 0.196 Uiso 1 1 calc R . . H3B_2 H 0.0039 0.6263 0.2028 0.196 Uiso 1 1 calc R . . H3C_2 H 0.0158 0.7003 0.2409 0.196 Uiso 1 1 calc R . . O4_2 O 0.21282(18) 0.5162(3) 0.27823(15) 0.0413(12) Uani 1 1 d . . . C4_2 C 0.0053(4) 0.6100(9) 0.3094(3) 0.153(6) Uani 1 1 d . . . H4A_2 H -0.0390 0.6157 0.3049 0.229 Uiso 1 1 calc R . . H4B_2 H 0.0244 0.6654 0.3184 0.229 Uiso 1 1 calc R . . H4C_2 H 0.0194 0.5680 0.3338 0.229 Uiso 1 1 calc R . . O5_2 O 0.2685(3) 0.3845(4) 0.3930(2) 0.0773(17) Uani 1 1 d . . . C5_2 C 0.1080(3) 0.3828(4) 0.2304(2) 0.0444(19) Uani 1 1 d . . . H5A_2 H 0.0965 0.3218 0.2311 0.053 Uiso 1 1 calc R . . H5B_2 H 0.1530 0.3852 0.2362 0.053 Uiso 1 1 calc R . . C6_2 C 0.0850(3) 0.4149(4) 0.1821(2) 0.0373(18) Uani 1 1 d . . . O6_2 O 0.3440(2) 0.5766(4) 0.37780(19) 0.0779(17) Uani 1 1 d . . . C7_2 C 0.0944(3) 0.5017(5) 0.1711(3) 0.0427(19) Uani 1 1 d . . . C8_2 C 0.0821(3) 0.5262(5) 0.1239(2) 0.0428(19) Uani 1 1 d . . . C9_2 C 0.0582(3) 0.4647(5) 0.0914(2) 0.053(2) Uani 1 1 d . . . H9_2 H 0.0498 0.4812 0.0599 0.064 Uiso 1 1 calc R . . C10_2 C 0.0458(3) 0.3809(5) 0.1019(3) 0.049(2) Uani 1 1 d . . . C11_2 C 0.0597(3) 0.3577(5) 0.1483(2) 0.0453(19) Uani 1 1 d . . . H11_2 H 0.0515 0.3010 0.1568 0.054 Uiso 1 1 calc R . . C12_2 C 0.0992(4) 0.6167(5) 0.1103(3) 0.057(2) Uani 1 1 d . . . C13_2 C 0.0819(5) 0.6309(5) 0.0575(3) 0.090(3) Uani 1 1 d . . . H13A_2 H 0.1038 0.5897 0.0418 0.135 Uiso 1 1 calc R . . H13B_2 H 0.0930 0.6891 0.0501 0.135 Uiso 1 1 calc R . . H13C_2 H 0.0380 0.6228 0.0471 0.135 Uiso 1 1 calc R . . C14_2 C 0.1678(4) 0.6301(6) 0.1251(3) 0.094(3) Uani 1 1 d . . . H14A_2 H 0.1799 0.6214 0.1585 0.141 Uiso 1 1 calc R . . H14B_2 H 0.1782 0.6884 0.1174 0.141 Uiso 1 1 calc R . . H14C_2 H 0.1892 0.5891 0.1090 0.141 Uiso 1 1 calc R . . C15_2 C 0.0643(4) 0.6835(4) 0.1325(3) 0.071(3) Uani 1 1 d . . . H15A_2 H 0.0735 0.6763 0.1661 0.106 Uiso 1 1 calc R . . H15B_2 H 0.0205 0.6761 0.1210 0.106 Uiso 1 1 calc R . . H15C_2 H 0.0765 0.7408 0.1246 0.106 Uiso 1 1 calc R . . C16_2 C 0.0196(4) 0.3196(5) 0.0640(2) 0.068(2) Uani 1 1 d . . . H16A_2 H 0.0136 0.3492 0.0342 0.101 Uiso 1 1 calc R . . H16B_2 H -0.0196 0.2981 0.0691 0.101 Uiso 1 1 calc R . . H16C_2 H 0.0477 0.2717 0.0639 0.101 Uiso 1 1 calc R . . C17_2 C 0.1149(3) 0.3767(4) 0.3116(2) 0.0366(18) Uani 1 1 d . . . H17A_2 H 0.1596 0.3746 0.3138 0.044 Uiso 1 1 calc R . . H17B_2 H 0.0997 0.3172 0.3076 0.044 Uiso 1 1 calc R . . C18_2 C 0.1030(3) 0.4093(4) 0.3570(2) 0.0356(17) Uani 1 1 d . . . C19_2 C 0.1233(3) 0.4918(4) 0.3723(2) 0.0345(17) Uani 1 1 d . . . C20_2 C 0.1196(3) 0.5181(4) 0.4177(3) 0.0438(19) Uani 1 1 d . . . C21_2 C 0.0940(3) 0.4595(5) 0.4448(2) 0.049(2) Uani 1 1 d . . . H21_2 H 0.0910 0.4759 0.4752 0.059 Uiso 1 1 calc R . . C22_2 C 0.0728(3) 0.3782(5) 0.4290(3) 0.050(2) Uani 1 1 d . . . C23_2 C 0.0778(3) 0.3548(5) 0.3849(2) 0.0429(19) Uani 1 1 d . . . H23_2 H 0.0637 0.3002 0.3735 0.052 Uiso 1 1 calc R . . C24_2 C 0.1437(3) 0.6062(5) 0.4371(3) 0.053(2) Uani 1 1 d . . . C25_2 C 0.1343(4) 0.6197(5) 0.4874(3) 0.079(3) Uani 1 1 d . . . H25A_2 H 0.0908 0.6176 0.4880 0.118 Uiso 1 1 calc R . . H25B_2 H 0.1508 0.6755 0.4987 0.118 Uiso 1 1 calc R . . H25C_2 H 0.1555 0.5745 0.5073 0.118 Uiso 1 1 calc R . . C26_2 C 0.2131(3) 0.6108(5) 0.4390(3) 0.069(3) Uani 1 1 d . . . H26A_2 H 0.2212 0.6028 0.4079 0.104 Uiso 1 1 calc R . . H26B_2 H 0.2335 0.5657 0.4593 0.104 Uiso 1 1 calc R . . H26C_2 H 0.2284 0.6667 0.4509 0.104 Uiso 1 1 calc R . . C27_2 C 0.1130(4) 0.6784(5) 0.4076(3) 0.075(3) Uani 1 1 d . . . H27A_2 H 0.1190 0.6710 0.3759 0.113 Uiso 1 1 calc R . . H27B_2 H 0.1307 0.7329 0.4198 0.113 Uiso 1 1 calc R . . H27C_2 H 0.0694 0.6781 0.4079 0.113 Uiso 1 1 calc R . . C28_2 C 0.0470(4) 0.3199(5) 0.4612(2) 0.071(3) Uani 1 1 d . . . H28A_2 H 0.0339 0.2661 0.4454 0.106 Uiso 1 1 calc R . . H28B_2 H 0.0121 0.3477 0.4705 0.106 Uiso 1 1 calc R . . H28C_2 H 0.0784 0.3081 0.4886 0.106 Uiso 1 1 calc R . . C29_2 C 0.1476(4) 0.7657(5) 0.2866(3) 0.079(3) Uani 1 1 d . . . H29_2 H 0.1165 0.7858 0.3043 0.094 Uiso 1 1 calc R . . C30_2 C 0.1351(4) 0.8175(5) 0.2438(3) 0.091(3) Uani 1 1 d . . . H30A_2 H 0.0944 0.8040 0.2263 0.136 Uiso 1 1 calc R . . H30B_2 H 0.1655 0.8044 0.2251 0.136 Uiso 1 1 calc R . . H30C_2 H 0.1373 0.8783 0.2518 0.136 Uiso 1 1 calc R . . C31_2 C 0.2074(4) 0.7803(5) 0.3191(3) 0.083(3) Uani 1 1 d . . . H31A_2 H 0.2098 0.7438 0.3464 0.125 Uiso 1 1 calc R . . H31B_2 H 0.2106 0.8404 0.3287 0.125 Uiso 1 1 calc R . . H31C_2 H 0.2409 0.7662 0.3036 0.125 Uiso 1 1 calc R . . C32_2 C 0.2472(3) 0.5140(4) 0.2438(2) 0.0413(18) Uani 1 1 d . . . H32_2 H 0.2194 0.5006 0.2139 0.050 Uiso 1 1 calc R . . C33_2 C 0.2786(3) 0.5976(4) 0.2387(3) 0.064(2) Uani 1 1 d . . . H33A_2 H 0.2481 0.6432 0.2318 0.097 Uiso 1 1 calc R . . H33B_2 H 0.3009 0.5931 0.2134 0.097 Uiso 1 1 calc R . . H33C_2 H 0.3071 0.6109 0.2674 0.097 Uiso 1 1 calc R . . C34_2 C 0.2943(3) 0.4415(5) 0.2547(3) 0.067(2) Uani 1 1 d . . . H34A_2 H 0.2733 0.3873 0.2572 0.101 Uiso 1 1 calc R . . H34B_2 H 0.3222 0.4536 0.2839 0.101 Uiso 1 1 calc R . . H34C_2 H 0.3174 0.4373 0.2299 0.101 Uiso 1 1 calc R . . C35_2 C 0.2949(6) 0.3138(8) 0.3726(4) 0.121(4) Uani 1 1 d . . . H35A_2 H 0.2726 0.3046 0.3406 0.146 Uiso 1 1 calc R . . H35B_2 H 0.3379 0.3264 0.3717 0.146 Uiso 1 1 calc R . . C36_2 C 0.2914(8) 0.2400(9) 0.3990(6) 0.201(8) Uani 1 1 d . . . H36A_2 H 0.3313 0.2106 0.4060 0.241 Uiso 1 1 calc R . . H36B_2 H 0.2607 0.1999 0.3822 0.241 Uiso 1 1 calc R . . C37_2 C 0.2738(7) 0.2692(7) 0.4415(4) 0.145(5) Uani 1 1 d . . . H37A_2 H 0.3099 0.2723 0.4669 0.174 Uiso 1 1 calc R . . H37B_2 H 0.2439 0.2295 0.4506 0.174 Uiso 1 1 calc R . . C38_2 C 0.2470(4) 0.3541(6) 0.4313(3) 0.076(3) Uani 1 1 d . . . H38A_2 H 0.2021 0.3504 0.4244 0.091 Uiso 1 1 calc R . . H38B_2 H 0.2596 0.3927 0.4580 0.091 Uiso 1 1 calc R . . C39_2 C 0.3614(6) 0.6645(7) 0.3774(5) 0.157(6) Uani 1 1 d . . . H39A_2 H 0.3564 0.6843 0.3451 0.189 Uiso 1 1 calc R . . H39B_2 H 0.3340 0.6991 0.3927 0.189 Uiso 1 1 calc R . . C40_2 C 0.4219(5) 0.6777(7) 0.4001(5) 0.155(6) Uani 1 1 d . . . H40A_2 H 0.4244 0.7241 0.4232 0.186 Uiso 1 1 calc R . . H40B_2 H 0.4477 0.6929 0.3778 0.186 Uiso 1 1 calc R . . C41_2 C 0.4411(4) 0.5958(8) 0.4227(3) 0.108(4) Uani 1 1 d . . . H41A_2 H 0.4407 0.5993 0.4560 0.130 Uiso 1 1 calc R . . H41B_2 H 0.4829 0.5815 0.4190 0.130 Uiso 1 1 calc R . . C42_2 C 0.3964(4) 0.5281(6) 0.3998(3) 0.080(3) Uani 1 1 d . . . H42A_2 H 0.4136 0.4950 0.3768 0.096 Uiso 1 1 calc R . . H42B_2 H 0.3858 0.4882 0.4230 0.096 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_1 0.0378(7) 0.0246(8) 0.0339(8) -0.0015(6) 0.0059(6) -0.0004(6) O1_1 0.057(3) 0.027(3) 0.030(3) 0.001(2) 0.004(2) -0.001(2) N1_1 0.033(3) 0.033(3) 0.031(3) 0.000(3) 0.010(3) 0.008(3) C1_1 0.039(4) 0.029(4) 0.042(4) 0.002(3) 0.006(3) 0.001(3) Na1_1 0.0491(17) 0.066(2) 0.0416(17) 0.0054(14) 0.0004(13) -0.0040(14) O2_1 0.046(3) 0.031(3) 0.035(3) -0.004(2) 0.011(2) -0.005(2) N2_1 0.035(3) 0.040(4) 0.059(4) -0.007(3) 0.011(3) 0.002(3) C2_1 0.043(5) 0.083(7) 0.121(8) -0.016(6) 0.018(5) -0.006(5) O3_1 0.057(3) 0.023(3) 0.051(3) -0.006(2) 0.003(2) -0.004(2) C3_1 0.057(6) 0.135(9) 0.098(7) 0.050(7) 0.020(5) 0.034(6) O4_1 0.038(3) 0.035(3) 0.037(3) 0.002(2) 0.013(2) -0.001(2) C4_1 0.056(6) 0.202(12) 0.069(7) -0.028(7) 0.009(5) 0.036(7) C5_1 0.050(4) 0.026(4) 0.039(4) -0.007(3) 0.024(3) -0.006(3) O5_1 0.065(4) 0.086(5) 0.065(4) 0.013(4) 0.016(3) 0.016(3) C6_1 0.044(4) 0.033(5) 0.029(4) -0.001(4) 0.013(3) -0.002(3) O6_1 0.057(3) 0.089(5) 0.065(4) 0.014(3) -0.012(3) -0.009(3) C7_1 0.038(4) 0.039(5) 0.020(4) -0.001(4) 0.006(3) -0.001(3) C8_1 0.043(4) 0.030(4) 0.039(5) -0.009(4) 0.010(3) 0.006(3) C9_1 0.062(5) 0.059(6) 0.031(4) -0.004(4) 0.007(4) -0.009(4) C10_1 0.055(5) 0.076(7) 0.037(5) -0.023(5) 0.015(4) -0.018(4) C11_1 0.065(5) 0.041(5) 0.033(5) -0.008(4) 0.019(4) -0.014(4) C12_1 0.061(5) 0.041(5) 0.034(4) -0.001(4) 0.001(4) 0.008(4) C13_1 0.075(6) 0.062(6) 0.081(6) 0.026(5) 0.004(5) -0.018(5) C14_1 0.092(6) 0.058(5) 0.040(5) 0.006(4) 0.004(4) 0.005(5) C15_1 0.106(7) 0.043(5) 0.053(5) 0.005(4) 0.010(5) 0.025(5) C16_1 0.122(8) 0.080(7) 0.053(5) -0.030(5) 0.015(5) -0.054(6) C17_1 0.049(4) 0.024(4) 0.027(4) -0.003(3) 0.002(3) 0.002(3) C18_1 0.042(4) 0.029(5) 0.037(4) 0.004(4) 0.009(3) -0.001(3) C19_1 0.033(4) 0.042(5) 0.029(4) 0.004(4) 0.019(3) 0.005(3) C20_1 0.029(4) 0.052(5) 0.042(5) 0.010(4) 0.005(3) 0.002(3) C21_1 0.041(4) 0.046(5) 0.032(4) -0.010(4) 0.005(3) 0.017(4) C22_1 0.044(4) 0.055(6) 0.030(5) 0.013(4) 0.013(3) -0.003(4) C23_1 0.049(5) 0.049(5) 0.040(5) 0.006(4) -0.002(4) 0.000(4) C24_1 0.055(5) 0.039(5) 0.040(4) -0.016(4) 0.015(4) -0.003(4) C25_1 0.086(6) 0.037(5) 0.063(5) -0.011(4) 0.017(5) 0.009(4) C26_1 0.069(5) 0.058(5) 0.051(5) -0.012(4) 0.018(4) -0.007(4) C27_1 0.077(6) 0.061(6) 0.053(5) -0.020(4) 0.022(4) -0.016(4) C28_1 0.085(6) 0.073(6) 0.033(4) 0.003(4) 0.014(4) -0.016(5) C29_1 0.053(5) 0.047(5) 0.065(5) -0.010(4) 0.000(4) -0.015(4) C30_1 0.068(6) 0.042(5) 0.096(7) 0.018(5) 0.009(5) -0.009(4) C31_1 0.071(6) 0.065(6) 0.082(6) 0.008(5) -0.011(5) -0.023(5) C32_1 0.035(4) 0.037(4) 0.044(4) -0.002(4) 0.016(4) -0.003(3) C33_1 0.064(5) 0.057(5) 0.079(6) 0.003(5) 0.029(4) 0.017(4) C34_1 0.072(6) 0.052(5) 0.075(6) 0.011(4) 0.035(5) -0.011(4) C35_1 0.125(9) 0.152(12) 0.078(7) -0.002(8) 0.035(7) 0.078(9) C36_1 0.47(3) 0.087(11) 0.189(17) 0.022(12) 0.19(2) 0.081(15) C37_1 0.258(18) 0.106(11) 0.158(13) 0.062(10) 0.101(12) 0.070(11) C38_1 0.105(7) 0.085(8) 0.064(6) 0.011(6) 0.027(5) 0.030(6) C39_1 0.077(7) 0.113(9) 0.125(9) 0.037(7) -0.032(7) -0.003(7) C40_1 0.056(6) 0.120(9) 0.074(6) 0.002(6) 0.001(5) -0.017(6) C41_1 0.097(8) 0.067(7) 0.121(9) -0.004(6) 0.011(7) -0.025(6) C42_1 0.115(9) 0.087(8) 0.158(11) 0.048(8) -0.047(8) -0.043(7) Ti1_2 0.0385(8) 0.0270(8) 0.0452(8) 0.0023(6) 0.0096(6) 0.0023(6) O1_2 0.053(3) 0.035(3) 0.043(3) 0.002(2) 0.003(2) 0.002(2) N1_2 0.037(4) 0.028(3) 0.036(3) 0.004(3) 0.005(3) 0.004(3) C1_2 0.036(4) 0.044(5) 0.041(4) 0.004(4) 0.008(3) 0.000(4) O2_2 0.043(3) 0.035(3) 0.043(3) 0.003(2) 0.015(2) -0.002(2) N2_2 0.047(4) 0.029(4) 0.068(4) -0.003(3) 0.018(3) 0.004(3) C2_2 0.036(6) 0.057(8) 0.60(3) -0.018(13) 0.027(11) -0.002(6) Na1_2 0.0441(16) 0.061(2) 0.0532(18) 0.0031(15) 0.0059(14) -0.0015(14) O3_2 0.061(3) 0.022(3) 0.071(3) -0.001(2) 0.021(3) -0.006(2) C3_2 0.062(6) 0.226(14) 0.104(8) 0.093(9) 0.016(6) 0.055(7) O4_2 0.037(3) 0.038(3) 0.051(3) -0.001(2) 0.015(2) -0.002(2) C4_2 0.056(6) 0.316(19) 0.084(8) -0.056(10) 0.010(6) 0.074(9) O5_2 0.073(4) 0.068(4) 0.094(5) 0.010(4) 0.023(3) 0.019(3) C5_2 0.052(5) 0.030(4) 0.051(5) 0.003(4) 0.007(4) -0.001(3) C6_2 0.037(4) 0.034(5) 0.043(5) -0.004(4) 0.011(3) 0.001(3) O6_2 0.062(4) 0.084(5) 0.081(4) 0.000(3) -0.002(3) -0.009(3) C7_2 0.030(4) 0.039(5) 0.058(5) 0.008(4) 0.007(4) 0.001(3) C8_2 0.041(4) 0.055(5) 0.035(4) 0.009(4) 0.014(3) 0.004(4) C9_2 0.063(5) 0.059(6) 0.036(5) 0.007(4) 0.005(4) -0.003(4) C10_2 0.059(5) 0.046(5) 0.047(5) -0.003(4) 0.019(4) -0.001(4) C11_2 0.052(5) 0.042(5) 0.048(5) 0.002(4) 0.024(4) -0.004(4) C12_2 0.083(6) 0.036(5) 0.057(5) 0.020(4) 0.026(4) 0.002(4) C13_2 0.148(9) 0.066(6) 0.067(6) 0.025(5) 0.047(6) 0.012(6) C14_2 0.074(7) 0.074(7) 0.129(9) 0.037(6) 0.007(6) -0.022(5) C15_2 0.116(7) 0.033(5) 0.062(5) 0.010(4) 0.014(5) 0.016(5) C16_2 0.094(6) 0.076(6) 0.036(5) 0.000(4) 0.018(4) -0.015(5) C17_2 0.044(4) 0.020(4) 0.044(4) 0.007(3) 0.007(3) 0.000(3) C18_2 0.041(4) 0.022(4) 0.045(5) 0.002(4) 0.010(4) -0.001(3) C19_2 0.030(4) 0.036(5) 0.039(5) 0.004(4) 0.011(3) 0.002(3) C20_2 0.033(4) 0.048(5) 0.048(5) 0.003(4) 0.004(4) 0.006(4) C21_2 0.040(4) 0.073(6) 0.034(4) -0.002(4) 0.008(4) -0.003(4) C22_2 0.049(5) 0.045(5) 0.049(5) 0.010(4) -0.004(4) -0.016(4) C23_2 0.047(4) 0.043(5) 0.037(5) 0.000(4) 0.002(4) -0.012(4) C24_2 0.063(5) 0.043(5) 0.056(5) -0.019(4) 0.015(4) -0.011(4) C25_2 0.105(7) 0.078(7) 0.064(6) -0.019(5) 0.044(5) -0.019(5) C26_2 0.059(5) 0.068(6) 0.076(6) -0.034(5) 0.000(4) -0.013(4) C27_2 0.099(7) 0.044(5) 0.080(6) 0.000(5) 0.010(5) 0.012(5) C28_2 0.097(7) 0.071(6) 0.046(5) 0.012(5) 0.017(5) -0.016(5) C29_2 0.088(7) 0.047(6) 0.094(7) 0.014(5) 0.002(5) -0.006(5) C30_2 0.085(7) 0.045(6) 0.138(9) 0.041(6) 0.013(6) -0.006(5) C31_2 0.076(6) 0.056(6) 0.111(7) 0.003(5) 0.001(6) -0.013(5) C32_2 0.043(4) 0.039(5) 0.046(5) -0.001(4) 0.017(4) 0.001(4) C33_2 0.071(5) 0.038(5) 0.091(6) 0.000(4) 0.033(5) -0.010(4) C34_2 0.061(5) 0.059(6) 0.088(6) -0.002(5) 0.030(5) 0.003(4) C35_2 0.167(11) 0.109(10) 0.107(9) 0.024(8) 0.074(8) 0.062(9) C36_2 0.35(2) 0.114(12) 0.193(15) 0.057(12) 0.184(16) 0.105(13) C37_2 0.223(15) 0.087(9) 0.128(11) 0.040(8) 0.045(10) 0.047(9) C38_2 0.087(7) 0.084(7) 0.058(6) 0.007(5) 0.018(5) 0.015(5) C39_2 0.134(11) 0.063(8) 0.233(15) 0.031(8) -0.067(10) -0.015(7) C40_2 0.062(7) 0.096(9) 0.276(17) 0.021(10) -0.042(9) -0.019(6) C41_2 0.051(6) 0.172(12) 0.090(7) 0.017(8) -0.014(5) -0.029(7) C42_2 0.053(6) 0.103(8) 0.083(7) 0.015(6) 0.012(5) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1_1 O3_1 1.828(4) . ? Ti1_1 O4_1 1.999(4) . ? Ti1_1 O1_1 2.013(4) . ? Ti1_1 O2_1 2.076(4) . ? Ti1_1 N1_1 2.354(5) . ? Ti1_1 N2_1 2.413(5) . ? Ti1_1 Na1_1 3.313(3) . ? O1_1 C7_1 1.314(7) . ? N1_1 C1_1 1.483(8) . ? N1_1 C17_1 1.499(7) . ? N1_1 C5_1 1.500(7) . ? C1_1 C2_1 1.490(10) . ? C1_1 H1A_1 0.9900 . ? C1_1 H1B_1 0.9900 . ? Na1_1 O4_1 2.186(4) . ? Na1_1 O6_1 2.291(6) . ? Na1_1 O2_1 2.293(5) . ? Na1_1 O5_1 2.312(6) . ? Na1_1 C19_1 3.006(7) . ? O2_1 C19_1 1.330(7) . ? N2_1 C4_1 1.430(10) . ? N2_1 C3_1 1.469(9) . ? N2_1 C2_1 1.480(9) . ? C2_1 H2A_1 0.9900 . ? C2_1 H2B_1 0.9900 . ? O3_1 C29_1 1.414(8) . ? C3_1 H3A_1 0.9800 . ? C3_1 H3B_1 0.9800 . ? C3_1 H3C_1 0.9800 . ? O4_1 C32_1 1.392(7) . ? C4_1 H4A_1 0.9800 . ? C4_1 H4B_1 0.9800 . ? C4_1 H4C_1 0.9800 . ? C5_1 C6_1 1.525(8) . ? C5_1 H5A_1 0.9900 . ? C5_1 H5B_1 0.9900 . ? O5_1 C38_1 1.440(9) . ? O5_1 C35_1 1.450(11) . ? C6_1 C11_1 1.395(8) . ? C6_1 C7_1 1.405(8) . ? O6_1 C39_1 1.398(9) . ? O6_1 C42_1 1.411(10) . ? C7_1 C8_1 1.423(8) . ? C8_1 C9_1 1.382(9) . ? C8_1 C12_1 1.536(9) . ? C9_1 C10_1 1.407(10) . ? C9_1 H9_1 0.9500 . ? C10_1 C11_1 1.365(9) . ? C10_1 C16_1 1.535(9) . ? C11_1 H11_1 0.9500 . ? C12_1 C13_1 1.531(10) . ? C12_1 C14_1 1.536(9) . ? C12_1 C15_1 1.546(9) . ? C13_1 H13A_1 0.9800 . ? C13_1 H13B_1 0.9800 . ? C13_1 H13C_1 0.9800 . ? C14_1 H14A_1 0.9800 . ? C14_1 H14B_1 0.9800 . ? C14_1 H14C_1 0.9800 . ? C15_1 H15A_1 0.9800 . ? C15_1 H15B_1 0.9800 . ? C15_1 H15C_1 0.9800 . ? C16_1 H16A_1 0.9800 . ? C16_1 H16B_1 0.9800 . ? C16_1 H16C_1 0.9800 . ? C17_1 C18_1 1.468(8) . ? C17_1 H17A_1 0.9900 . ? C17_1 H17B_1 0.9900 . ? C18_1 C23_1 1.395(9) . ? C18_1 C19_1 1.412(9) . ? C19_1 C20_1 1.404(9) . ? C20_1 C21_1 1.412(9) . ? C20_1 C24_1 1.537(9) . ? C21_1 C22_1 1.379(9) . ? C21_1 H21_1 0.9500 . ? C22_1 C23_1 1.395(9) . ? C22_1 C28_1 1.486(9) . ? C23_1 H23_1 0.9500 . ? C24_1 C25_1 1.516(9) . ? C24_1 C27_1 1.535(9) . ? C24_1 C26_1 1.551(9) . ? C25_1 H25A_1 0.9800 . ? C25_1 H25B_1 0.9800 . ? C25_1 H25C_1 0.9800 . ? C26_1 H26A_1 0.9800 . ? C26_1 H26B_1 0.9800 . ? C26_1 H26C_1 0.9800 . ? C27_1 H27A_1 0.9800 . ? C27_1 H27B_1 0.9800 . ? C27_1 H27C_1 0.9800 . ? C28_1 H28A_1 0.9800 . ? C28_1 H28B_1 0.9800 . ? C28_1 H28C_1 0.9800 . ? C29_1 C30_1 1.496(10) . ? C29_1 C31_1 1.504(9) . ? C29_1 H29A_1 1.0000 . ? C30_1 H30A_1 0.9800 . ? C30_1 H30B_1 0.9800 . ? C30_1 H30C_1 0.9800 . ? C31_1 H31A_1 0.9800 . ? C31_1 H31B_1 0.9800 . ? C31_1 H31C_1 0.9800 . ? C32_1 C34_1 1.533(9) . ? C32_1 C33_1 1.535(9) . ? C32_1 H32A_1 1.0000 . ? C33_1 H33A_1 0.9800 . ? C33_1 H33B_1 0.9800 . ? C33_1 H33C_1 0.9800 . ? C34_1 H34A_1 0.9800 . ? C34_1 H34B_1 0.9800 . ? C34_1 H34C_1 0.9800 . ? C35_1 C36_1 1.455(16) . ? C35_1 H35A_1 0.9900 . ? C35_1 H35B_1 0.9900 . ? C36_1 C37_1 1.435(17) . ? C36_1 H36A_1 0.9900 . ? C36_1 H36B_1 0.9900 . ? C37_1 C38_1 1.464(13) . ? C37_1 H37A_1 0.9900 . ? C37_1 H37B_1 0.9900 . ? C38_1 H38A_1 0.9900 . ? C38_1 H38B_1 0.9900 . ? C39_1 C40_1 1.476(11) . ? C39_1 H39A_1 0.9900 . ? C39_1 H39B_1 0.9900 . ? C40_1 C41_1 1.536(11) . ? C40_1 H40A_1 0.9900 . ? C40_1 H40B_1 0.9900 . ? C41_1 C42_1 1.398(11) . ? C41_1 H41A_1 0.9900 . ? C41_1 H41B_1 0.9900 . ? C42_1 H42A_1 0.9900 . ? C42_1 H42B_1 0.9900 . ? Ti1_2 O3_2 1.821(4) . ? Ti1_2 O4_2 2.000(4) . ? Ti1_2 O1_2 2.001(5) . ? Ti1_2 O2_2 2.085(4) . ? Ti1_2 N1_2 2.359(5) . ? Ti1_2 N2_2 2.409(6) . ? Ti1_2 Na1_2 3.320(3) . ? O1_2 C7_2 1.327(8) . ? N1_2 C5_2 1.476(8) . ? N1_2 C1_2 1.477(8) . ? N1_2 C17_2 1.486(7) . ? C1_2 C2_2 1.371(12) . ? C1_2 H1A_2 0.9900 . ? C1_2 H1B_2 0.9900 . ? O2_2 C19_2 1.330(7) . ? O2_2 Na1_2 2.300(5) . ? N2_2 C4_2 1.420(10) . ? N2_2 C2_2 1.445(12) . ? N2_2 C3_2 1.452(10) . ? C2_2 H2A_2 0.9900 . ? C2_2 H2B_2 0.9900 . ? Na1_2 O4_2 2.208(5) . ? Na1_2 O6_2 2.310(6) . ? Na1_2 O5_2 2.315(6) . ? Na1_2 C19_2 3.034(7) . ? O3_2 C29_2 1.371(9) . ? C3_2 H3A_2 0.9800 . ? C3_2 H3B_2 0.9800 . ? C3_2 H3C_2 0.9800 . ? O4_2 C32_2 1.393(8) . ? C4_2 H4A_2 0.9800 . ? C4_2 H4B_2 0.9800 . ? C4_2 H4C_2 0.9800 . ? O5_2 C38_2 1.399(9) . ? O5_2 C35_2 1.443(10) . ? C5_2 C6_2 1.505(8) . ? C5_2 H5A_2 0.9900 . ? C5_2 H5B_2 0.9900 . ? C6_2 C11_2 1.377(9) . ? C6_2 C7_2 1.422(9) . ? O6_2 C39_2 1.431(10) . ? O6_2 C42_2 1.441(9) . ? C7_2 C8_2 1.421(9) . ? C8_2 C9_2 1.389(9) . ? C8_2 C12_2 1.540(10) . ? C9_2 C10_2 1.389(10) . ? C9_2 H9_2 0.9500 . ? C10_2 C11_2 1.391(9) . ? C10_2 C16_2 1.504(9) . ? C11_2 H11_2 0.9500 . ? C12_2 C14_2 1.528(11) . ? C12_2 C15_2 1.528(10) . ? C12_2 C13_2 1.550(10) . ? C13_2 H13A_2 0.9800 . ? C13_2 H13B_2 0.9800 . ? C13_2 H13C_2 0.9800 . ? C14_2 H14A_2 0.9800 . ? C14_2 H14B_2 0.9800 . ? C14_2 H14C_2 0.9800 . ? C15_2 H15A_2 0.9800 . ? C15_2 H15B_2 0.9800 . ? C15_2 H15C_2 0.9800 . ? C16_2 H16A_2 0.9800 . ? C16_2 H16B_2 0.9800 . ? C16_2 H16C_2 0.9800 . ? C17_2 C18_2 1.507(9) . ? C17_2 H17A_2 0.9900 . ? C17_2 H17B_2 0.9900 . ? C18_2 C23_2 1.382(9) . ? C18_2 C19_2 1.414(9) . ? C19_2 C20_2 1.421(9) . ? C20_2 C21_2 1.412(9) . ? C20_2 C24_2 1.548(9) . ? C21_2 C22_2 1.406(9) . ? C21_2 H21_2 0.9500 . ? C22_2 C23_2 1.379(9) . ? C22_2 C28_2 1.514(10) . ? C23_2 H23_2 0.9500 . ? C24_2 C27_2 1.508(10) . ? C24_2 C26_2 1.546(10) . ? C24_2 C25_2 1.558(10) . ? C25_2 H25A_2 0.9800 . ? C25_2 H25B_2 0.9800 . ? C25_2 H25C_2 0.9800 . ? C26_2 H26A_2 0.9800 . ? C26_2 H26B_2 0.9800 . ? C26_2 H26C_2 0.9800 . ? C27_2 H27A_2 0.9800 . ? C27_2 H27B_2 0.9800 . ? C27_2 H27C_2 0.9800 . ? C28_2 H28A_2 0.9800 . ? C28_2 H28B_2 0.9800 . ? C28_2 H28C_2 0.9800 . ? C29_2 C30_2 1.480(11) . ? C29_2 C31_2 1.506(10) . ? C29_2 H29_2 1.0000 . ? C30_2 H30A_2 0.9800 . ? C30_2 H30B_2 0.9800 . ? C30_2 H30C_2 0.9800 . ? C31_2 H31A_2 0.9800 . ? C31_2 H31B_2 0.9800 . ? C31_2 H31C_2 0.9800 . ? C32_2 C33_2 1.507(9) . ? C32_2 C34_2 1.539(9) . ? C32_2 H32_2 1.0000 . ? C33_2 H33A_2 0.9800 . ? C33_2 H33B_2 0.9800 . ? C33_2 H33C_2 0.9800 . ? C34_2 H34A_2 0.9800 . ? C34_2 H34B_2 0.9800 . ? C34_2 H34C_2 0.9800 . ? C35_2 C36_2 1.405(14) . ? C35_2 H35A_2 0.9900 . ? C35_2 H35B_2 0.9900 . ? C36_2 C37_2 1.462(14) . ? C36_2 H36A_2 0.9900 . ? C36_2 H36B_2 0.9900 . ? C37_2 C38_2 1.465(12) . ? C37_2 H37A_2 0.9900 . ? C37_2 H37B_2 0.9900 . ? C38_2 H38A_2 0.9900 . ? C38_2 H38B_2 0.9900 . ? C39_2 C40_2 1.404(12) . ? C39_2 H39A_2 0.9900 . ? C39_2 H39B_2 0.9900 . ? C40_2 C41_2 1.469(13) . ? C40_2 H40A_2 0.9900 . ? C40_2 H40B_2 0.9900 . ? C41_2 C42_2 1.522(11) . ? C41_2 H41A_2 0.9900 . ? C41_2 H41B_2 0.9900 . ? C42_2 H42A_2 0.9900 . ? C42_2 H42B_2 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 O3_1 Ti1_1 O4_1 109.41(18) . . ? O3_1 Ti1_1 O1_1 99.42(18) . . ? O4_1 Ti1_1 O1_1 89.44(17) . . ? O3_1 Ti1_1 O2_1 95.04(17) . . ? O4_1 Ti1_1 O2_1 81.85(17) . . ? O1_1 Ti1_1 O2_1 164.97(17) . . ? O3_1 Ti1_1 N1_1 160.34(19) . . ? O4_1 Ti1_1 N1_1 89.88(17) . . ? O1_1 Ti1_1 N1_1 84.07(17) . . ? O2_1 Ti1_1 N1_1 83.68(16) . . ? O3_1 Ti1_1 N2_1 87.01(19) . . ? O4_1 Ti1_1 N2_1 163.57(18) . . ? O1_1 Ti1_1 N2_1 88.23(19) . . ? O2_1 Ti1_1 N2_1 96.65(19) . . ? N1_1 Ti1_1 N2_1 73.70(18) . . ? O3_1 Ti1_1 Na1_1 99.40(13) . . ? O4_1 Ti1_1 Na1_1 39.69(13) . . ? O1_1 Ti1_1 Na1_1 129.13(14) . . ? O2_1 Ti1_1 Na1_1 43.20(13) . . ? N1_1 Ti1_1 Na1_1 93.08(12) . . ? N2_1 Ti1_1 Na1_1 139.53(16) . . ? C7_1 O1_1 Ti1_1 139.8(4) . . ? C1_1 N1_1 C17_1 110.1(5) . . ? C1_1 N1_1 C5_1 110.8(4) . . ? C17_1 N1_1 C5_1 106.2(4) . . ? C1_1 N1_1 Ti1_1 113.7(3) . . ? C17_1 N1_1 Ti1_1 108.3(3) . . ? C5_1 N1_1 Ti1_1 107.4(4) . . ? N1_1 C1_1 C2_1 111.7(5) . . ? N1_1 C1_1 H1A_1 109.3 . . ? C2_1 C1_1 H1A_1 109.3 . . ? N1_1 C1_1 H1B_1 109.3 . . ? C2_1 C1_1 H1B_1 109.3 . . ? H1A_1 C1_1 H1B_1 107.9 . . ? O4_1 Na1_1 O6_1 121.4(2) . . ? O4_1 Na1_1 O2_1 73.12(17) . . ? O6_1 Na1_1 O2_1 137.5(2) . . ? O4_1 Na1_1 O5_1 123.3(2) . . ? O6_1 Na1_1 O5_1 95.5(2) . . ? O2_1 Na1_1 O5_1 108.8(2) . . ? O4_1 Na1_1 C19_1 90.63(18) . . ? O6_1 Na1_1 C19_1 139.3(2) . . ? O2_1 Na1_1 C19_1 24.71(15) . . ? O5_1 Na1_1 C19_1 84.7(2) . . ? O4_1 Na1_1 Ti1_1 35.72(12) . . ? O6_1 Na1_1 Ti1_1 135.30(17) . . ? O2_1 Na1_1 Ti1_1 38.29(11) . . ? O5_1 Na1_1 Ti1_1 129.15(16) . . ? C19_1 Na1_1 Ti1_1 59.66(13) . . ? C19_1 O2_1 Ti1_1 134.5(4) . . ? C19_1 O2_1 Na1_1 109.2(3) . . ? Ti1_1 O2_1 Na1_1 98.5(2) . . ? C4_1 N2_1 C3_1 106.6(7) . . ? C4_1 N2_1 C2_1 115.7(7) . . ? C3_1 N2_1 C2_1 102.6(6) . . ? C4_1 N2_1 Ti1_1 113.9(4) . . ? C3_1 N2_1 Ti1_1 110.9(5) . . ? C2_1 N2_1 Ti1_1 106.6(4) . . ? N2_1 C2_1 C1_1 112.3(6) . . ? N2_1 C2_1 H2A_1 109.2 . . ? C1_1 C2_1 H2A_1 109.2 . . ? N2_1 C2_1 H2B_1 109.2 . . ? C1_1 C2_1 H2B_1 109.2 . . ? H2A_1 C2_1 H2B_1 107.9 . . ? C29_1 O3_1 Ti1_1 170.3(4) . . ? N2_1 C3_1 H3A_1 109.5 . . ? N2_1 C3_1 H3B_1 109.5 . . ? H3A_1 C3_1 H3B_1 109.5 . . ? N2_1 C3_1 H3C_1 109.5 . . ? H3A_1 C3_1 H3C_1 109.5 . . ? H3B_1 C3_1 H3C_1 109.5 . . ? C32_1 O4_1 Ti1_1 128.1(4) . . ? C32_1 O4_1 Na1_1 124.5(4) . . ? Ti1_1 O4_1 Na1_1 104.6(2) . . ? N2_1 C4_1 H4A_1 109.5 . . ? N2_1 C4_1 H4B_1 109.5 . . ? H4A_1 C4_1 H4B_1 109.5 . . ? N2_1 C4_1 H4C_1 109.5 . . ? H4A_1 C4_1 H4C_1 109.5 . . ? H4B_1 C4_1 H4C_1 109.5 . . ? N1_1 C5_1 C6_1 117.1(5) . . ? N1_1 C5_1 H5A_1 108.0 . . ? C6_1 C5_1 H5A_1 108.0 . . ? N1_1 C5_1 H5B_1 108.0 . . ? C6_1 C5_1 H5B_1 108.0 . . ? H5A_1 C5_1 H5B_1 107.3 . . ? C38_1 O5_1 C35_1 107.8(7) . . ? C38_1 O5_1 Na1_1 126.5(5) . . ? C35_1 O5_1 Na1_1 123.9(6) . . ? C11_1 C6_1 C7_1 121.0(6) . . ? C11_1 C6_1 C5_1 119.3(6) . . ? C7_1 C6_1 C5_1 119.3(5) . . ? C39_1 O6_1 C42_1 108.1(6) . . ? C39_1 O6_1 Na1_1 122.1(5) . . ? C42_1 O6_1 Na1_1 129.0(5) . . ? O1_1 C7_1 C6_1 120.2(5) . . ? O1_1 C7_1 C8_1 121.2(6) . . ? C6_1 C7_1 C8_1 118.6(6) . . ? C9_1 C8_1 C7_1 118.0(6) . . ? C9_1 C8_1 C12_1 121.1(6) . . ? C7_1 C8_1 C12_1 120.6(6) . . ? C8_1 C9_1 C10_1 123.2(6) . . ? C8_1 C9_1 H9_1 118.4 . . ? C10_1 C9_1 H9_1 118.4 . . ? C11_1 C10_1 C9_1 118.1(6) . . ? C11_1 C10_1 C16_1 121.5(7) . . ? C9_1 C10_1 C16_1 120.4(7) . . ? C10_1 C11_1 C6_1 120.9(7) . . ? C10_1 C11_1 H11_1 119.6 . . ? C6_1 C11_1 H11_1 119.6 . . ? C13_1 C12_1 C14_1 107.8(6) . . ? C13_1 C12_1 C8_1 110.7(5) . . ? C14_1 C12_1 C8_1 111.8(5) . . ? C13_1 C12_1 C15_1 108.8(6) . . ? C14_1 C12_1 C15_1 106.5(6) . . ? C8_1 C12_1 C15_1 111.0(6) . . ? C12_1 C13_1 H13A_1 109.5 . . ? C12_1 C13_1 H13B_1 109.5 . . ? H13A_1 C13_1 H13B_1 109.5 . . ? C12_1 C13_1 H13C_1 109.5 . . ? H13A_1 C13_1 H13C_1 109.5 . . ? H13B_1 C13_1 H13C_1 109.5 . . ? C12_1 C14_1 H14A_1 109.5 . . ? C12_1 C14_1 H14B_1 109.5 . . ? H14A_1 C14_1 H14B_1 109.5 . . ? C12_1 C14_1 H14C_1 109.5 . . ? H14A_1 C14_1 H14C_1 109.5 . . ? H14B_1 C14_1 H14C_1 109.5 . . ? C12_1 C15_1 H15A_1 109.5 . . ? C12_1 C15_1 H15B_1 109.5 . . ? H15A_1 C15_1 H15B_1 109.5 . . ? C12_1 C15_1 H15C_1 109.5 . . ? H15A_1 C15_1 H15C_1 109.5 . . ? H15B_1 C15_1 H15C_1 109.5 . . ? C10_1 C16_1 H16A_1 109.5 . . ? C10_1 C16_1 H16B_1 109.5 . . ? H16A_1 C16_1 H16B_1 109.5 . . ? C10_1 C16_1 H16C_1 109.5 . . ? H16A_1 C16_1 H16C_1 109.5 . . ? H16B_1 C16_1 H16C_1 109.5 . . ? C18_1 C17_1 N1_1 116.9(5) . . ? C18_1 C17_1 H17A_1 108.1 . . ? N1_1 C17_1 H17A_1 108.1 . . ? C18_1 C17_1 H17B_1 108.1 . . ? N1_1 C17_1 H17B_1 108.1 . . ? H17A_1 C17_1 H17B_1 107.3 . . ? C23_1 C18_1 C19_1 118.2(6) . . ? C23_1 C18_1 C17_1 120.8(6) . . ? C19_1 C18_1 C17_1 120.5(6) . . ? O2_1 C19_1 C20_1 121.5(6) . . ? O2_1 C19_1 C18_1 117.1(6) . . ? C20_1 C19_1 C18_1 121.4(6) . . ? O2_1 C19_1 Na1_1 46.1(3) . . ? C20_1 C19_1 Na1_1 113.8(4) . . ? C18_1 C19_1 Na1_1 104.2(4) . . ? C19_1 C20_1 C21_1 116.2(6) . . ? C19_1 C20_1 C24_1 122.9(6) . . ? C21_1 C20_1 C24_1 120.8(6) . . ? C22_1 C21_1 C20_1 125.0(6) . . ? C22_1 C21_1 H21_1 117.5 . . ? C20_1 C21_1 H21_1 117.5 . . ? C21_1 C22_1 C23_1 116.1(6) . . ? C21_1 C22_1 C28_1 122.2(7) . . ? C23_1 C22_1 C28_1 121.7(7) . . ? C22_1 C23_1 C18_1 123.1(7) . . ? C22_1 C23_1 H23_1 118.4 . . ? C18_1 C23_1 H23_1 118.4 . . ? C25_1 C24_1 C27_1 109.5(6) . . ? C25_1 C24_1 C20_1 110.2(5) . . ? C27_1 C24_1 C20_1 109.7(6) . . ? C25_1 C24_1 C26_1 107.5(6) . . ? C27_1 C24_1 C26_1 107.0(5) . . ? C20_1 C24_1 C26_1 112.9(6) . . ? C24_1 C25_1 H25A_1 109.5 . . ? C24_1 C25_1 H25B_1 109.5 . . ? H25A_1 C25_1 H25B_1 109.5 . . ? C24_1 C25_1 H25C_1 109.5 . . ? H25A_1 C25_1 H25C_1 109.5 . . ? H25B_1 C25_1 H25C_1 109.5 . . ? C24_1 C26_1 H26A_1 109.5 . . ? C24_1 C26_1 H26B_1 109.5 . . ? H26A_1 C26_1 H26B_1 109.5 . . ? C24_1 C26_1 H26C_1 109.5 . . ? H26A_1 C26_1 H26C_1 109.5 . . ? H26B_1 C26_1 H26C_1 109.5 . . ? C24_1 C27_1 H27A_1 109.5 . . ? C24_1 C27_1 H27B_1 109.5 . . ? H27A_1 C27_1 H27B_1 109.5 . . ? C24_1 C27_1 H27C_1 109.5 . . ? H27A_1 C27_1 H27C_1 109.5 . . ? H27B_1 C27_1 H27C_1 109.5 . . ? C22_1 C28_1 H28A_1 109.5 . . ? C22_1 C28_1 H28B_1 109.5 . . ? H28A_1 C28_1 H28B_1 109.5 . . ? C22_1 C28_1 H28C_1 109.5 . . ? H28A_1 C28_1 H28C_1 109.5 . . ? H28B_1 C28_1 H28C_1 109.5 . . ? O3_1 C29_1 C30_1 112.9(6) . . ? O3_1 C29_1 C31_1 109.3(6) . . ? C30_1 C29_1 C31_1 113.6(7) . . ? O3_1 C29_1 H29A_1 106.9 . . ? C30_1 C29_1 H29A_1 106.9 . . ? C31_1 C29_1 H29A_1 106.9 . . ? C29_1 C30_1 H30A_1 109.5 . . ? C29_1 C30_1 H30B_1 109.5 . . ? H30A_1 C30_1 H30B_1 109.5 . . ? C29_1 C30_1 H30C_1 109.5 . . ? H30A_1 C30_1 H30C_1 109.5 . . ? H30B_1 C30_1 H30C_1 109.5 . . ? C29_1 C31_1 H31A_1 109.5 . . ? C29_1 C31_1 H31B_1 109.5 . . ? H31A_1 C31_1 H31B_1 109.5 . . ? C29_1 C31_1 H31C_1 109.5 . . ? H31A_1 C31_1 H31C_1 109.5 . . ? H31B_1 C31_1 H31C_1 109.5 . . ? O4_1 C32_1 C34_1 111.3(6) . . ? O4_1 C32_1 C33_1 109.8(5) . . ? C34_1 C32_1 C33_1 110.8(6) . . ? O4_1 C32_1 H32A_1 108.3 . . ? C34_1 C32_1 H32A_1 108.3 . . ? C33_1 C32_1 H32A_1 108.3 . . ? C32_1 C33_1 H33A_1 109.5 . . ? C32_1 C33_1 H33B_1 109.5 . . ? H33A_1 C33_1 H33B_1 109.5 . . ? C32_1 C33_1 H33C_1 109.5 . . ? H33A_1 C33_1 H33C_1 109.5 . . ? H33B_1 C33_1 H33C_1 109.5 . . ? C32_1 C34_1 H34A_1 109.5 . . ? C32_1 C34_1 H34B_1 109.5 . . ? H34A_1 C34_1 H34B_1 109.5 . . ? C32_1 C34_1 H34C_1 109.5 . . ? H34A_1 C34_1 H34C_1 109.5 . . ? H34B_1 C34_1 H34C_1 109.5 . . ? O5_1 C35_1 C36_1 107.3(9) . . ? O5_1 C35_1 H35A_1 110.3 . . ? C36_1 C35_1 H35A_1 110.3 . . ? O5_1 C35_1 H35B_1 110.3 . . ? C36_1 C35_1 H35B_1 110.3 . . ? H35A_1 C35_1 H35B_1 108.5 . . ? C37_1 C36_1 C35_1 105.7(12) . . ? C37_1 C36_1 H36A_1 110.6 . . ? C35_1 C36_1 H36A_1 110.6 . . ? C37_1 C36_1 H36B_1 110.6 . . ? C35_1 C36_1 H36B_1 110.6 . . ? H36A_1 C36_1 H36B_1 108.7 . . ? C36_1 C37_1 C38_1 108.9(11) . . ? C36_1 C37_1 H37A_1 109.9 . . ? C38_1 C37_1 H37A_1 109.9 . . ? C36_1 C37_1 H37B_1 109.9 . . ? C38_1 C37_1 H37B_1 109.9 . . ? H37A_1 C37_1 H37B_1 108.3 . . ? O5_1 C38_1 C37_1 106.5(8) . . ? O5_1 C38_1 H38A_1 110.4 . . ? C37_1 C38_1 H38A_1 110.4 . . ? O5_1 C38_1 H38B_1 110.4 . . ? C37_1 C38_1 H38B_1 110.4 . . ? H38A_1 C38_1 H38B_1 108.6 . . ? O6_1 C39_1 C40_1 108.4(8) . . ? O6_1 C39_1 H39A_1 110.0 . . ? C40_1 C39_1 H39A_1 110.0 . . ? O6_1 C39_1 H39B_1 110.0 . . ? C40_1 C39_1 H39B_1 110.0 . . ? H39A_1 C39_1 H39B_1 108.4 . . ? C39_1 C40_1 C41_1 104.6(7) . . ? C39_1 C40_1 H40A_1 110.8 . . ? C41_1 C40_1 H40A_1 110.8 . . ? C39_1 C40_1 H40B_1 110.8 . . ? C41_1 C40_1 H40B_1 110.8 . . ? H40A_1 C40_1 H40B_1 108.9 . . ? C42_1 C41_1 C40_1 104.6(7) . . ? C42_1 C41_1 H41A_1 110.8 . . ? C40_1 C41_1 H41A_1 110.8 . . ? C42_1 C41_1 H41B_1 110.8 . . ? C40_1 C41_1 H41B_1 110.8 . . ? H41A_1 C41_1 H41B_1 108.9 . . ? C41_1 C42_1 O6_1 112.4(8) . . ? C41_1 C42_1 H42A_1 109.1 . . ? O6_1 C42_1 H42A_1 109.1 . . ? C41_1 C42_1 H42B_1 109.1 . . ? O6_1 C42_1 H42B_1 109.1 . . ? H42A_1 C42_1 H42B_1 107.8 . . ? O3_2 Ti1_2 O4_2 108.80(19) . . ? O3_2 Ti1_2 O1_2 99.0(2) . . ? O4_2 Ti1_2 O1_2 89.75(18) . . ? O3_2 Ti1_2 O2_2 94.86(19) . . ? O4_2 Ti1_2 O2_2 82.30(18) . . ? O1_2 Ti1_2 O2_2 165.65(18) . . ? O3_2 Ti1_2 N1_2 160.6(2) . . ? O4_2 Ti1_2 N1_2 90.31(17) . . ? O1_2 Ti1_2 N1_2 83.97(18) . . ? O2_2 Ti1_2 N1_2 84.14(17) . . ? O3_2 Ti1_2 N2_2 86.9(2) . . ? O4_2 Ti1_2 N2_2 164.25(18) . . ? O1_2 Ti1_2 N2_2 88.58(19) . . ? O2_2 Ti1_2 N2_2 95.83(19) . . ? N1_2 Ti1_2 N2_2 73.95(18) . . ? O3_2 Ti1_2 Na1_2 98.55(15) . . ? O4_2 Ti1_2 Na1_2 40.17(14) . . ? O1_2 Ti1_2 Na1_2 129.91(14) . . ? O2_2 Ti1_2 Na1_2 43.26(13) . . ? N1_2 Ti1_2 Na1_2 93.96(12) . . ? N2_2 Ti1_2 Na1_2 138.89(16) . . ? C7_2 O1_2 Ti1_2 141.2(4) . . ? C5_2 N1_2 C1_2 109.9(5) . . ? C5_2 N1_2 C17_2 106.9(5) . . ? C1_2 N1_2 C17_2 110.3(5) . . ? C5_2 N1_2 Ti1_2 106.6(4) . . ? C1_2 N1_2 Ti1_2 113.2(4) . . ? C17_2 N1_2 Ti1_2 109.7(3) . . ? C2_2 C1_2 N1_2 113.9(6) . . ? C2_2 C1_2 H1A_2 108.8 . . ? N1_2 C1_2 H1A_2 108.8 . . ? C2_2 C1_2 H1B_2 108.8 . . ? N1_2 C1_2 H1B_2 108.8 . . ? H1A_2 C1_2 H1B_2 107.7 . . ? C19_2 O2_2 Ti1_2 133.6(4) . . ? C19_2 O2_2 Na1_2 110.5(3) . . ? Ti1_2 O2_2 Na1_2 98.3(2) . . ? C4_2 N2_2 C2_2 115.3(10) . . ? C4_2 N2_2 C3_2 106.4(8) . . ? C2_2 N2_2 C3_2 104.4(9) . . ? C4_2 N2_2 Ti1_2 113.0(5) . . ? C2_2 N2_2 Ti1_2 105.7(5) . . ? C3_2 N2_2 Ti1_2 111.8(5) . . ? C1_2 C2_2 N2_2 122.7(10) . . ? C1_2 C2_2 H2A_2 106.7 . . ? N2_2 C2_2 H2A_2 106.7 . . ? C1_2 C2_2 H2B_2 106.7 . . ? N2_2 C2_2 H2B_2 106.7 . . ? H2A_2 C2_2 H2B_2 106.6 . . ? O4_2 Na1_2 O2_2 73.19(17) . . ? O4_2 Na1_2 O6_2 116.7(2) . . ? O2_2 Na1_2 O6_2 140.1(2) . . ? O4_2 Na1_2 O5_2 122.0(2) . . ? O2_2 Na1_2 O5_2 107.2(2) . . ? O6_2 Na1_2 O5_2 99.2(2) . . ? O4_2 Na1_2 C19_2 90.16(18) . . ? O2_2 Na1_2 C19_2 24.24(15) . . ? O6_2 Na1_2 C19_2 144.4(2) . . ? O5_2 Na1_2 C19_2 83.6(2) . . ? O4_2 Na1_2 Ti1_2 35.74(12) . . ? O2_2 Na1_2 Ti1_2 38.41(12) . . ? O6_2 Na1_2 Ti1_2 132.88(18) . . ? O5_2 Na1_2 Ti1_2 127.48(17) . . ? C19_2 Na1_2 Ti1_2 59.29(13) . . ? C29_2 O3_2 Ti1_2 172.2(5) . . ? N2_2 C3_2 H3A_2 109.5 . . ? N2_2 C3_2 H3B_2 109.5 . . ? H3A_2 C3_2 H3B_2 109.5 . . ? N2_2 C3_2 H3C_2 109.5 . . ? H3A_2 C3_2 H3C_2 109.5 . . ? H3B_2 C3_2 H3C_2 109.5 . . ? C32_2 O4_2 Ti1_2 127.6(4) . . ? C32_2 O4_2 Na1_2 124.9(4) . . ? Ti1_2 O4_2 Na1_2 104.1(2) . . ? N2_2 C4_2 H4A_2 109.5 . . ? N2_2 C4_2 H4B_2 109.5 . . ? H4A_2 C4_2 H4B_2 109.5 . . ? N2_2 C4_2 H4C_2 109.5 . . ? H4A_2 C4_2 H4C_2 109.5 . . ? H4B_2 C4_2 H4C_2 109.5 . . ? C38_2 O5_2 C35_2 108.3(7) . . ? C38_2 O5_2 Na1_2 130.9(5) . . ? C35_2 O5_2 Na1_2 119.4(6) . . ? N1_2 C5_2 C6_2 119.4(5) . . ? N1_2 C5_2 H5A_2 107.5 . . ? C6_2 C5_2 H5A_2 107.5 . . ? N1_2 C5_2 H5B_2 107.5 . . ? C6_2 C5_2 H5B_2 107.5 . . ? H5A_2 C5_2 H5B_2 107.0 . . ? C11_2 C6_2 C7_2 120.8(6) . . ? C11_2 C6_2 C5_2 119.2(6) . . ? C7_2 C6_2 C5_2 119.8(6) . . ? C39_2 O6_2 C42_2 108.1(6) . . ? C39_2 O6_2 Na1_2 130.4(6) . . ? C42_2 O6_2 Na1_2 121.4(5) . . ? O1_2 C7_2 C8_2 123.1(6) . . ? O1_2 C7_2 C6_2 118.6(6) . . ? C8_2 C7_2 C6_2 118.3(7) . . ? C9_2 C8_2 C7_2 117.7(7) . . ? C9_2 C8_2 C12_2 122.6(6) . . ? C7_2 C8_2 C12_2 119.6(6) . . ? C10_2 C9_2 C8_2 124.5(7) . . ? C10_2 C9_2 H9_2 117.7 . . ? C8_2 C9_2 H9_2 117.7 . . ? C9_2 C10_2 C11_2 116.8(7) . . ? C9_2 C10_2 C16_2 120.0(7) . . ? C11_2 C10_2 C16_2 123.2(7) . . ? C6_2 C11_2 C10_2 121.8(7) . . ? C6_2 C11_2 H11_2 119.1 . . ? C10_2 C11_2 H11_2 119.1 . . ? C14_2 C12_2 C15_2 110.8(7) . . ? C14_2 C12_2 C8_2 109.8(6) . . ? C15_2 C12_2 C8_2 110.1(6) . . ? C14_2 C12_2 C13_2 107.8(7) . . ? C15_2 C12_2 C13_2 106.7(6) . . ? C8_2 C12_2 C13_2 111.6(6) . . ? C12_2 C13_2 H13A_2 109.5 . . ? C12_2 C13_2 H13B_2 109.5 . . ? H13A_2 C13_2 H13B_2 109.5 . . ? C12_2 C13_2 H13C_2 109.5 . . ? H13A_2 C13_2 H13C_2 109.5 . . ? H13B_2 C13_2 H13C_2 109.5 . . ? C12_2 C14_2 H14A_2 109.5 . . ? C12_2 C14_2 H14B_2 109.5 . . ? H14A_2 C14_2 H14B_2 109.5 . . ? C12_2 C14_2 H14C_2 109.5 . . ? H14A_2 C14_2 H14C_2 109.5 . . ? H14B_2 C14_2 H14C_2 109.5 . . ? C12_2 C15_2 H15A_2 109.5 . . ? C12_2 C15_2 H15B_2 109.5 . . ? H15A_2 C15_2 H15B_2 109.5 . . ? C12_2 C15_2 H15C_2 109.5 . . ? H15A_2 C15_2 H15C_2 109.5 . . ? H15B_2 C15_2 H15C_2 109.5 . . ? C10_2 C16_2 H16A_2 109.5 . . ? C10_2 C16_2 H16B_2 109.5 . . ? H16A_2 C16_2 H16B_2 109.5 . . ? C10_2 C16_2 H16C_2 109.5 . . ? H16A_2 C16_2 H16C_2 109.5 . . ? H16B_2 C16_2 H16C_2 109.5 . . ? N1_2 C17_2 C18_2 117.5(5) . . ? N1_2 C17_2 H17A_2 107.9 . . ? C18_2 C17_2 H17A_2 107.9 . . ? N1_2 C17_2 H17B_2 107.9 . . ? C18_2 C17_2 H17B_2 107.9 . . ? H17A_2 C17_2 H17B_2 107.2 . . ? C23_2 C18_2 C19_2 120.9(7) . . ? C23_2 C18_2 C17_2 119.3(6) . . ? C19_2 C18_2 C17_2 119.5(6) . . ? O2_2 C19_2 C18_2 119.0(6) . . ? O2_2 C19_2 C20_2 121.4(6) . . ? C18_2 C19_2 C20_2 119.5(6) . . ? O2_2 C19_2 Na1_2 45.2(3) . . ? C18_2 C19_2 Na1_2 106.9(4) . . ? C20_2 C19_2 Na1_2 112.4(4) . . ? C21_2 C20_2 C19_2 117.0(6) . . ? C21_2 C20_2 C24_2 121.2(7) . . ? C19_2 C20_2 C24_2 121.8(7) . . ? C22_2 C21_2 C20_2 123.2(7) . . ? C22_2 C21_2 H21_2 118.4 . . ? C20_2 C21_2 H21_2 118.4 . . ? C23_2 C22_2 C21_2 117.9(7) . . ? C23_2 C22_2 C28_2 123.2(7) . . ? C21_2 C22_2 C28_2 118.8(7) . . ? C22_2 C23_2 C18_2 121.4(6) . . ? C22_2 C23_2 H23_2 119.3 . . ? C18_2 C23_2 H23_2 119.3 . . ? C27_2 C24_2 C26_2 109.1(7) . . ? C27_2 C24_2 C20_2 111.4(6) . . ? C26_2 C24_2 C20_2 109.3(6) . . ? C27_2 C24_2 C25_2 108.6(6) . . ? C26_2 C24_2 C25_2 106.5(6) . . ? C20_2 C24_2 C25_2 111.8(6) . . ? C24_2 C25_2 H25A_2 109.5 . . ? C24_2 C25_2 H25B_2 109.5 . . ? H25A_2 C25_2 H25B_2 109.5 . . ? C24_2 C25_2 H25C_2 109.5 . . ? H25A_2 C25_2 H25C_2 109.5 . . ? H25B_2 C25_2 H25C_2 109.5 . . ? C24_2 C26_2 H26A_2 109.5 . . ? C24_2 C26_2 H26B_2 109.5 . . ? H26A_2 C26_2 H26B_2 109.5 . . ? C24_2 C26_2 H26C_2 109.5 . . ? H26A_2 C26_2 H26C_2 109.5 . . ? H26B_2 C26_2 H26C_2 109.5 . . ? C24_2 C27_2 H27A_2 109.5 . . ? C24_2 C27_2 H27B_2 109.5 . . ? H27A_2 C27_2 H27B_2 109.5 . . ? C24_2 C27_2 H27C_2 109.5 . . ? H27A_2 C27_2 H27C_2 109.5 . . ? H27B_2 C27_2 H27C_2 109.5 . . ? C22_2 C28_2 H28A_2 109.5 . . ? C22_2 C28_2 H28B_2 109.5 . . ? H28A_2 C28_2 H28B_2 109.5 . . ? C22_2 C28_2 H28C_2 109.5 . . ? H28A_2 C28_2 H28C_2 109.5 . . ? H28B_2 C28_2 H28C_2 109.5 . . ? O3_2 C29_2 C30_2 113.8(7) . . ? O3_2 C29_2 C31_2 111.9(6) . . ? C30_2 C29_2 C31_2 117.2(8) . . ? O3_2 C29_2 H29_2 104.0 . . ? C30_2 C29_2 H29_2 104.0 . . ? C31_2 C29_2 H29_2 104.0 . . ? C29_2 C30_2 H30A_2 109.5 . . ? C29_2 C30_2 H30B_2 109.5 . . ? H30A_2 C30_2 H30B_2 109.5 . . ? C29_2 C30_2 H30C_2 109.5 . . ? H30A_2 C30_2 H30C_2 109.5 . . ? H30B_2 C30_2 H30C_2 109.5 . . ? C29_2 C31_2 H31A_2 109.5 . . ? C29_2 C31_2 H31B_2 109.5 . . ? H31A_2 C31_2 H31B_2 109.5 . . ? C29_2 C31_2 H31C_2 109.5 . . ? H31A_2 C31_2 H31C_2 109.5 . . ? H31B_2 C31_2 H31C_2 109.5 . . ? O4_2 C32_2 C33_2 112.9(6) . . ? O4_2 C32_2 C34_2 108.8(6) . . ? C33_2 C32_2 C34_2 110.3(6) . . ? O4_2 C32_2 H32_2 108.3 . . ? C33_2 C32_2 H32_2 108.3 . . ? C34_2 C32_2 H32_2 108.3 . . ? C32_2 C33_2 H33A_2 109.5 . . ? C32_2 C33_2 H33B_2 109.5 . . ? H33A_2 C33_2 H33B_2 109.5 . . ? C32_2 C33_2 H33C_2 109.5 . . ? H33A_2 C33_2 H33C_2 109.5 . . ? H33B_2 C33_2 H33C_2 109.5 . . ? C32_2 C34_2 H34A_2 109.5 . . ? C32_2 C34_2 H34B_2 109.5 . . ? H34A_2 C34_2 H34B_2 109.5 . . ? C32_2 C34_2 H34C_2 109.5 . . ? H34A_2 C34_2 H34C_2 109.5 . . ? H34B_2 C34_2 H34C_2 109.5 . . ? C36_2 C35_2 O5_2 108.9(9) . . ? C36_2 C35_2 H35A_2 109.9 . . ? O5_2 C35_2 H35A_2 109.9 . . ? C36_2 C35_2 H35B_2 109.9 . . ? O5_2 C35_2 H35B_2 109.9 . . ? H35A_2 C35_2 H35B_2 108.3 . . ? C35_2 C36_2 C37_2 106.0(11) . . ? C35_2 C36_2 H36A_2 110.5 . . ? C37_2 C36_2 H36A_2 110.5 . . ? C35_2 C36_2 H36B_2 110.5 . . ? C37_2 C36_2 H36B_2 110.5 . . ? H36A_2 C36_2 H36B_2 108.7 . . ? C36_2 C37_2 C38_2 106.0(10) . . ? C36_2 C37_2 H37A_2 110.5 . . ? C38_2 C37_2 H37A_2 110.5 . . ? C36_2 C37_2 H37B_2 110.5 . . ? C38_2 C37_2 H37B_2 110.5 . . ? H37A_2 C37_2 H37B_2 108.7 . . ? O5_2 C38_2 C37_2 106.4(9) . . ? O5_2 C38_2 H38A_2 110.5 . . ? C37_2 C38_2 H38A_2 110.5 . . ? O5_2 C38_2 H38B_2 110.5 . . ? C37_2 C38_2 H38B_2 110.5 . . ? H38A_2 C38_2 H38B_2 108.6 . . ? C40_2 C39_2 O6_2 112.1(8) . . ? C40_2 C39_2 H39A_2 109.2 . . ? O6_2 C39_2 H39A_2 109.2 . . ? C40_2 C39_2 H39B_2 109.2 . . ? O6_2 C39_2 H39B_2 109.2 . . ? H39A_2 C39_2 H39B_2 107.9 . . ? C39_2 C40_2 C41_2 104.9(9) . . ? C39_2 C40_2 H40A_2 110.8 . . ? C41_2 C40_2 H40A_2 110.8 . . ? C39_2 C40_2 H40B_2 110.8 . . ? C41_2 C40_2 H40B_2 110.8 . . ? H40A_2 C40_2 H40B_2 108.8 . . ? C40_2 C41_2 C42_2 107.3(7) . . ? C40_2 C41_2 H41A_2 110.3 . . ? C42_2 C41_2 H41A_2 110.3 . . ? C40_2 C41_2 H41B_2 110.3 . . ? C42_2 C41_2 H41B_2 110.3 . . ? H41A_2 C41_2 H41B_2 108.5 . . ? O6_2 C42_2 C41_2 103.9(7) . . ? O6_2 C42_2 H42A_2 111.0 . . ? C41_2 C42_2 H42A_2 111.0 . . ? O6_2 C42_2 H42B_2 111.0 . . ? C41_2 C42_2 H42B_2 111.0 . . ? H42A_2 C42_2 H42B_2 109.0 . . ? #===END